Preliminary Design of Vanillin Production Plant From Black Liquor

Table of Content Table of Content ...................................................................................................... i CHAPTER 1 ........................................................................................................... 1 INTRODUCTION .................................................................................................. 1 1.1 1.2 1.3 1.3.1 1.3.2 1.3.3 Plant Development Background.............................................................. 1 Plant Development Goal ......................................................................... 7 Plant Development Analysis ................................................................... 8 Raw Material Analysis ...................................................................... 8 Location Analysis ........................................................................... 12 Market & Capacity Analysis .......................................................... 16

CHAPTER 2 ......................................................................................................... 23 PROCESS DESIGN .............................................................................................. 23 2.1 2.2 Process Technology Selection ................................................................ 23 Process Description ................................................................................ 26 Type Of Process .............................................................................. 26 BFD and Description ...................................................................... 30 PFD and Description ....................................................................... 32

2.2.1 2.2.2 2.2.3

CHAPTER 3 ......................................................................................................... 36 MASS AND ENERGY BALANCE ..................................................................... 36 3.1 Mass Balance.......................................................................................... 36 Overall Mass Balance ..................................................................... 36 Mass Balance Process Units ........................................................... 37

3.1.1 3.1.2 3.2

Energy Balance ...................................................................................... 40

CHAPTER 4 ......................................................................................................... 45 UTILITIES ............................................................................................................ 45 4.1 Water Utility ........................................................................................... 45 Water Utility Classification ............................................................ 45

4.1.1 4.2 4.3

Electric Utility ........................................................................................ 46 Steam Utility .......................................................................................... 48

BAB 5 ................................................................................................................... 49

Preliminary Design of Vanillin Production Plant From Black Liquor

SIZING ................................................................................................................. 49 5.1 Vessel .......................................................................................................... 49 5.1.1 5.1.2 5.1.3 5.1.4 5.1.5 5.1.6 5.1.7 5.1.8 5.2 Black Liquor Storage Tank (S-101) ................................................ 49 Acidification Tank (V-101) ............................................................ 50 Acidification Tank (V-102) ............................................................ 51 Blending Tank (V-103) ................................................................... 53 Lignin Slurry Storage (S-102)......................................................... 54 Waste Storage (S-103) .................................................................... 55 H2SO4 Storage (S-104) ................................................................... 56 NaOH Storage (S-105) .................................................................... 57

Filtration ................................................................................................. 58 Plate and Frame Filter (PF-101)...................................................... 58 Plate and Frame Filter (PF-102)...................................................... 59

5.2.1 5.2.2 5.3

Pump....................................................................................................... 60 Black Liquor Pump (P-101) ............................................................ 60 Black Liquor Acidification pump (P-102) ...................................... 60 Lignin Acidification Pump (P-103) ................................................ 61 Lignin Solution Pump (P-104) ........................................................ 62 Lignin Solution Pump (P-105) ........................................................ 63 Vanillin Slurry Pump (P-106) ......................................................... 63 Vanillin Solution Pump (P-107) ..................................................... 64 Water Pump (P-109) ....................................................................... 65

5.3.1 5.3.2 5.3.3 5.3.4 5.3.5 5.3.6 5.3.7 5.3.8 5.4

Conveyor ................................................................................................ 66

5.5 Bubble Column Reactor .............................................................................. 67 5.6 Ultrafiltration ............................................................................................... 68 5.7 Spray Dryer ................................................................................................. 69 5.8 Heat Exchanger .......................................................................................... 70 5.8.1 Heat Exchanger HE-101 ....................................................................... 70 5.8.2 Heat Exchanger HE-102 ....................................................................... 70 CHAPTER 6 ......................................................................................................... 71 PROCESS CONTROL ......................................................................................... 71 6.1 Process Control Instrumentation ............................................................ 71

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Preliminary Design of Vanillin Production Plant From Black Liquor

6.2 6.3 6.4 6.5 6.6 6.7 6.8

Process Control on Raw Material Storage Tank .................................... 71 Process Control on Heat Exchanger ....................................................... 72 Process Control on Reboiler ................................................................... 72 Process Control on Black Liquor Treatment Vessel .............................. 72 Process Control on Acidification Vessel and Lignin Solution Vessel ... 73 Process Control on Oxidation Reactor ................................................... 74 Process Control on Spray Dryer ............................................................. 76

CHAPTER 7 ......................................................................................................... 82 PLANT LAYOUT AND PIPING DESIGN ......................................................... 82 CHAPTER 8 ......................................................................................................... 86 HEALTH, SAFETY, AND ENVIRONMENT MANAGEMENT ....................... 86 8. 1 8. 2 Health Aspects ........................................................................................ 87 Safety Aspects ........................................................................................ 87 Hazard Identification and Risk Assessment (HIRA) ...................... 87

8.2.1

8.2.3 Hazard Operability Study (HAZOP) of Vanillin Plant....................... 94 8. 3. Environmental Aspects .......................................................................... 99

8. 3. 1. Liquid Waste ...................................................................................... 99 8. 3. 2. Solid Waste ........................................................................................ 99 8. 3. 3. Waste Gas .......................................................................................... 99 8. 4. Risk Management ................................................................................... 99

8.4.1. Personal Protection Equipment.......................................................... 100 8.4.2. Fire extinguisher ................................................................................ 105 8.4.3. MSDS (Material Safety Data Sheet).................................................. 107 8.5. Quality Control in Vanillin Plant ............................................................. 107 CHAPTER 9 ....................................................................................................... 108 ECONOMIC ANALYSIS .................................................................................. 108 9.1 Plant Cost Estimation ................................................................................ 108 9.2 Annual Operating Costs ....................................................................... 113 Raw Material Costs ....................................................................... 113 Operating Labor Costs ................................................................ 115 Utilities Costs ................................................................................ 116 Total Direct Costs ......................................................................... 117

9.2.1 9.2.2 9.2.3 9.2.4

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Preliminary Design of Vanillin Production Plant From Black Liquor

9.2.5 9.2.6 9.2.7 9.2.8 9.2.9 9.3 9.4

Total Fixed Costs .......................................................................... 117 Plant Overhead .............................................................................. 117 Total Manufacturing Cost ............................................................. 117 Expenses Cost ............................................................................... 118 Total Operating Cost ..................................................................... 118

Equity ................................................................................................... 119 Investment feasibility Analysis ............................................................ 120 Cash Flow ..................................................................................... 120 IRR ................................................................................................ 122

9.5.1 9.5.2

9.5.3 Net Present Value (NPV).................................................................... 124 9.5.4 Pay Back Period .................................................................................. 125 9.5.5Break Event Point (BEP) ..................................................................... 125 9.5.6 Sensitivity Analysis ............................................................................ 126 APPENDIX ......................................................................................................... 129 1. Vessel ....................................................................................................... 129 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 2. Black Liquor Storage Tank (S-101) ................................................. 129 Acidification Tank (V-101) ............................................................. 130 Acidification Tank (V-102) .............................................................. 132 Blending Tank ( V-103).................................................................... 133 Lignin Slurry Storage (S-102) .......................................................... 135 Waste Storage (S-103) ...................................................................... 137 H2SO4 Storage (S-104)..................................................................... 138 NaOH Storage (S-105) ..................................................................... 140

Plate and Frame Filter .............................................................................. 141 2.1 2.2 Plate and Frame Filter (PF-101) ....................................................... 141 Plate and Frame Filter (PF-102) ....................................................... 143

Pump ........................................................................................................ 144 3.1 3.2 3.3 3.4 3.5 Black Liquor Pump (P-101)&(P-102) .............................................. 144 Black Liquor Acidification Pump (P-102) ....................................... 146 Lignin Acidification Pump (P-103) .................................................. 148 Lignin Solution Pump (P-104) ......................................................... 150 Lignin Solution Pump (P-105) ......................................................... 152

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Preliminary Design of Vanillin Production Plant From Black Liquor

3.6 3.7 3.8 4 5 6 7.

Vanillin Slurry Pump (P-106)........................................................... 154 Vanillin Solution Pump (P-107) ....................................................... 156 Water Pump (P-108) ......................................................................... 158

Bubble Column Reactor ........................................................................... 161 Ultrafiltrasi ............................................................................................... 163 Spray Dryer .............................................................................................. 165 Material Safety Data Sheet (MSDS) ........................................................ 171

REFERENCE ...................................................................................................... 174

Preliminary Design of Vanillin Production Plant From Black Liquor

CHAPTER 1 INTRODUCTION 1.1 Plant Development Background Vanillin (4-hydroxy-3-methoxybenzaldehyde)

is

the

major

flavor

constituent of vanilla. This organic compound possesses the aldehydic, etheric and
phenolic functional groups, and its molecular formula is C8H8O3 corresponding to a molecular weight of 152.15 (Washburn, 2003). The chemical structure and geometry of vanillin are presented in Figure 1.1. Some relevant physical properties of vanillin are shown in Table 1.1.

Figure 1.1. Chemical structure (a) and geometry (b) of vanillin molecule.

Vanillin occurs widely in nature, especially in the cured beans of the tropical Vanilla orchids. It is the major component among about 200 other flavor compounds found in these beans (Walton et al., 2003). Isolated vanillin occurs in the form of white needle-like crystalline powder with a pleasant aromatic vanilla odor and an intensively sweet taste, which are the main reasons for its widespread demand.
Table 1.1. Physical properties of vanillin.

Preliminary Design of Vanillin Production Plant From Black Liquor

Vanillin has a wide range of applications in food industry as a flavor agent and in perfumery as an additive. Other applications are as chemical precursor in the pharmaceutical industry, ripening agent, antifoaming agent in lubrication oils, brightener in zinc coating baths, vulcanization inhibitor, and starting material for insecticides and herbicides (Mathias, 1993; Villar et al., 1997). There are around 150 varieties of vanilla, but only two of them are grown commercially Bourbon and Tahitian vanilla (McGregor, 2005). Vanilla has it origins on Mesoamerican Mexico, with this country dominating the world production until the late 19th century. Since then, the focus of development was shifted to the former French colonies, in particular Madagascar, Comoros, Reunion and Tahiti. Nowadays, vanilla is grown on numerous countries, with data from 2005 indicating that Madagascar was the largest producer, accounted for around 60% of the world production, followed by Indonesia and China, with 23% and 10%, respectively. Looking at the last 20 years, the vanilla production has oscillated between 1200 and 4000 tonnes, with a world consumption varying from 1800 to 3000 tonnes (McGregor, 2005). The natural vanilla market is characterized by very volatile prices. Normally the price pattern of vanilla is made up of high peaks and prolonged periods of relatively low prices. These prices have been particularly sensitive to events affecting a single country Madagascar. From 1989 to 1995, the vanilla market was regulated by the Univanille cartel, an alliance of vanilla exporters. The major buyers and producers, principally Madagascar, met annually to determine demand and export pricing. In Figure 1.2 is schematically shown the evolution on the market prices of natural vanilla, since the early 1990s to the first half of 2005.

Preliminary Design of Vanillin Production Plant From Black Liquor

Figure 1.2. Evolution of natural vanilla prices since the early 1990s to 2005 (Jaeger (2005 )

Vanilla does not consist of vanillin alone, but contain several tens of aromatic compounds. For example, the vanilla world trade in 2001 (2300 tonnes) represents less than 50 tonnes of natural vanillin (Loeillet, 2003), which only constitutes a yield around 2%. Historically, the production of vanillin was its direct extraction from vanilla beans. However, according to the constantly increasing markets, new chemicals routes were developed. Synthetic vanillin became widely used and competition of markets is longstanding and turns more fierce when prices of natural vanilla rockets. Vanillin was first produced by Haarmann and Reimer in the late 1800s, using guaiacol from phenol. This was the main route for more than 40 years, until it was discovered that vanillin could be produced from lignin present in the waste liquor of pulp and paper industry. The commercial production of vanillin from lignin started in 1937. This process become the dominant one for many years, with 80% supply ratio of the synthetic vanillin market (Triumph Venture Capital, 2004). However, in the 1980s some changes in the processes of pulp and paper

Preliminary Design of Vanillin Production Plant From Black Liquor

industry led to a decrease in the available raw material required by the vanillin plants. The traditional calcium sulphite pulping process produced huge amounts of disposable effluents, that combined with the growing public awareness on environmental issues were leading to unsustainable waste treatment costs. These mills started to close, or were converted to new technology that allowed the recycling of the waste liquors for chemical recovery and thus making these byproducts streams not available for vanillin production. Since 1993, only Borregaard was producing vanillin from lignin. Nowadays the synthesis of vanillin from guaiacol accounts for 85% of the world supply, with the remaining 15% being produced from lignin (Triumph Venture Capital, 2004b). Commercial users can choose between natural vanilla (very expensive and used only in niche markets), synthetic vanillin and artificial vanilla flavor (ethyl vanillin). Synthetic vanillin is a cost effective alternative to vanilla and is increasingly substituting the natural product. It not only substitutes vanilla, but also supplements adulterated vanillin extracts. Global demand for synthetic vanillin currently is around 16000 tonnes per year. But guaiacol is petroleum derivatives and it has been limited. Natural "vanilla extract" is a mixture of several hundred different compounds in addition to vanillin. Artificialvanilla flavoring is a solution of pure vanillin, usually of synthetic origin. Because of the scarcity and expense ofnatural vanilla extract, there has long been interest in the synthetic preparation of its predominant component. The first commercial synthesis of vanillin start with the more readily available natural compound eugenol today, artificial vanillin is made from either guaiacol or from lignin, a constituent of wood which is a byproduct of the pulp industry, Lignin based artificial vanilla flavoring is alleged to have a richer flavor profile than oil based flavoring; the difference is due to the presence of acetovanillone in the ligninderived product. Rhodia SA dominates the world vanillin market using the catecholguaiacol process. Rhodia entered the USA vanillin market in 1986 with the purchase of the Monsanto plant. This plant was subsequently closed down in 1991. In November 1993, Rhodia purchased the ITT Rayonier vanillin business and immediately closed the plant. After that, their main target has been China.

Preliminary Design of Vanillin Production Plant From Black Liquor

Borregaard (Norway), the second largest vanillin producer, is the only remaining producer of lignin. The company also has guaiacol vanillin and ethyl vanillin production capacity as it acquired Eurovanillin in 1995 (Triumph Venture Capital, 2004). Borregaard mainly supplies the European market and its lignin vanillin production is almost exclusively for large costumers under long-term contracts. Lignin based vanillin is in high demand in certain market sectors, particularly the perfume industry, European chocolate manufacturers, and the Japanese market, and as such tends to command a price premium. The price of lignin vanillin is consistently maintained at about $1.00 to $2.00 per kg above that of guaiacol based vanillin (Triumph Venture Capital, 2004b). The ethyl vanillin price follows the same basic trend as the vanillin price. It is maintained at about twice that of vanillin, but as it has about three times the flavour intensity of vanillin there is a cost saving associated with substituting vanillin with ethyl vanillin. The main source of pure lignin is the pulp and paper industry, where nowadays the Kraft process prevails with approximately 80% of the world chemical pulp production (Ullmanns Encyclopedia, 2003). A by-product stream of this process, known as black liquor, contains typically 30 to 34% of lignin in dry solid weight basis. This stream is burned to provide energy for mill operations, and to facilitate the recovery of pulping chemicals. Due to the complex energetic integration of the Kraft process, an expansion in the production of pulp implies a revamp in the burners. An alternative plant design to the burners revamp will be a utilization of the increased amount of black liquor in the production of high-added value products and the elimination of a production bottleneck at the recovery boiler (Axelsson et al., 2006). In this work, the focus is on the production of synthetic vanillin from lignin obtained from black liquor. A flow sheet of a process to produce synthetic vanillin from lignin in a pulp and paper industrial unit is proposed in Figure 1.2. A portion of the byproduct stream, black liquor, is processed to extract lignin. This extraction can be done by the traditional acidification/precipitation followed by separation, or using an improved method similar to one developed by a Swedish group and known as LignoBoost (hman et al., 2006). After obtaining purified lignin, the subsequent

Preliminary Design of Vanillin Production Plant From Black Liquor

process is based on three main steps studied in LSRE. The first step consists on the alkaline lignin oxidation in a bubble column reactor, which is the main subject of this thesis. Then, the mixture obtained in the reaction passes through a membrane ultrafiltration process where the bigger molecules of degraded lignin are retained. Sodium vanillate (salt of vanillin) and other low molecular weight species goes to the permeate stream (Zabkova, 2006). Finally, the permeate containing smaller molecules and excess NaOH flows through a packed bed on acid resin in H+ form, in order to convert the sodium vanillate into vanillin (Zabkova et al., 2007). This ion exchange step is accompanied by neutralization reaction resulting in a lower pH for the product exit stream. In order to have a reference point for the results to achieve, it is important to refer a study developed in South Africa that revealed a benchmark final vanillin concentration was 4.2 g/l, for a production process based on Kraft black liquors (Triumph Venture Capital, 2004a). A process which final product has a concentration below this value should not be very competitive in the present scenario of the synthetic vanillin market.

Figure 1.3. Flow sheet of a process for vanillin production integrated in a pulp and paper mill (Zabkova, 2006).

Preliminary Design of Vanillin Production Plant From Black Liquor

In the wide scope of the forestry activities the black liquor is obtained as a by-product of the pulp and paper industry. For this reason, this work deals with this industry. Pulp and paper industries are unquestionably of great relevance to the Indonesia economy. In fact Badan Pusat Statistik (BPS) noted that pulp export from January until September 2011 had increased by 72,37% from 1,05 juta tonne to 1,81 million tonne. Indonesia take 9th place in the world in pulp production. The total of pulp industry is 13 units, where 6 units is in Sumatera. The production capacity is for about 6,5 million tonne pulp per year. Black liquor is the main raw material for vanillin making from lignin. Black liquor is obtained from one of the biggest pulp and paper industry in Indonesia that loctaing in Riau, PT Riau Andalan Pulp & Paper. The available side product capacity of pulp is 4.920.000 m3/year. Because of the large side production of black liquor, PT Riau Andalan concern to process the black liquor beside to use it as fuel. Therefore, PT Riau Andalan Pulp & Paper decide to make Vanillin Plant based on lignin that use black liquor as the raw material. By see the ability of black liquor production and the excellence compared to China in product shipping cost, the vanillin product from this plant can compete with competitive price with good margin profit. Beside to fulfill the needs of vanillin demand in Indonesia, the development of this plant will also create new job opportunity, expand the vanillin export, and give contribution for local communities. This is the first vanillin plant from lignin in Indonesia, it is expected to increase confidence and independence of this nation to apply knowledge and technology in real life. 1.2 Plant Development Goal Market increase, raise in energy prices and high volatility in natural vanilla

prices are a strong driving force to have a deeper understanding of alternative methods to produce vanillin. Vanillin obtained from lignin can employ a lowvalue fuel to produce a high-added value and also represents a green process, since it is biomass-based. The guaiacol process to produce vanillin employs benzene obtained from a non-renewable source (petroleum). Within this context, the objective of this plant is to design the plant of vanillin production from lignin and its implementation in

Preliminary Design of Vanillin Production Plant From Black Liquor

Indonesia. The source of lignin should be black liquor from pulp and paper industries using the Kraft process. In this work it was used lignin from softwood Pinus spp., kindly supplied by PT Riau Andalan Pulp and Paper. The target of vanillin production per day is 4500 kg or 1750 ton per year. Needs of vanillin in Indonesia until this plant design was done is still filled with synthetic vanillin imported from China. This vanillin factory has a useful life 20 years. We assume that vanillin needs always grow every years according to projections import data we have collected. Until 2022 the vanillin needs of Indonesia is still below 1750 ton / year. Thats way until that year this plant can fulfill all of vanillin needs in Indonesia. Otherwise, in 2035 vanillin needs of Indonesia can reach 12000 ton / year, and we predict that there will be another vanillin plant from lignin to fulfill needs of vanillin, but with keeping the best quality of vanillin this plant wont lose the customer. 1.3 1.3.1 Plant Development Analysis Raw Material Analysis Vanillin (4-hydroxy-3-methoxybenzaldehyde) is organoleptically the

characteristic aroma component of the cured vanilla pod, where it contributes to about 2% (w/w) of the dry matter (Priefert, H., Rabenhorst, J., & Steinbchel, A., 2001). It is used in a broad range of flavors for foods, confectionery, and beverages (approximately 60%), as a fragrance ingredient in perfumes and cosmetics (approximately 33%), and for pharmaceuticals (approximately 7%). From the annual consumption of the world flavor market, only about 0.2% originates from botanical sources (Krings and Berger 1998). There are 2 types of commercially available vanillin. The first one is a natural vanillin extracted from the vanillin pods and the second type is a pure vanillin chemically synthesized from various chemical substrates. The price of the chemically synthesized nature-identical vanillin is very low (about US$15 kg1), compared to the price of cured vanilla pods [between US$30 kg1 and US$120 kg1 (actual price)], which usually contain about 2% (w/w) vanillin. The high price of natural vanillin is mainly due to the limited availability of vanilla pods depending on climate-associated fluctuations of harvest yields, economical and political

Preliminary Design of Vanillin Production Plant From Black Liquor

decisions, and last but not least to the labor-intensive cultivation, pollination, harvesting and curing of vanilla pods. Vanillin can be produced from phenolic compounds such as phenolic stibenes, guaiacol, lignin, isoeugenol, eugenol, ferulic acid, vanillic acid, aromatic amino acid, sugar beet pulp, wheat straw and biomass substances (Vaithanomsat, P., & Apiwatanapiwat, W. , 2009). The main portion is produced by chemical synthesis from guaiacol and lignin (Priefert, H., Rabenhorst, J., & Steinbchel, A., 2001). 1. Guaiacol Guaiacol is one of the raw material to produce vanillin which is derived from petroleum. Rhone-Poulenc is the Worlds largest producer of vanillin and ethyl vanillin with a $60m turnover in these two products. The company has concentrated on the guaiacol route. Production facilities are situated in Saint Frons (France), which has been in operation since 1978 and in Baton Rouge, Louisiana (USA), which was commissioned over a two-year period ending in mid-1992. Combined capacities for vanillin and ethyl vanillin are estimated to be 3 000t and 5 000t respectively. Ube Industries in Japan also use the guaiacol route to vanillin and ethyl vanillin. The company recently expanded their 1 000t manufacturing facility by 400t and are understood to produce more or less equal volumes of both vanillin and ethyl vanillin. Chinese producers are thought to produce only vanillin, mostly via the guaiacol route (total capacity 2 000t). Rhodia acquired in 2000 the existing business of the Chinese company Xuebao Fine Chemicals Co. Ltd, one of the most recent vanillin plant at that time. Rhodia shares its experience in vanillin manufacture about environmental problem, involved higher toxicity of the raw materials (guaiacol), unfavourable ecobalance (3 to 5 more tars and COD Chemical Oxygen Demand, and 5 times more VOC - Volatile Organic Compounds, 1/3 of which benzene), non compliance with environmental standards, high health & safety risks and unacceptable standards for a flavor. Therefore, many manufacturers are trying to produce vanillin with raw materials that are environmentally friendly and renewable, likes lignin.

Preliminary Design of Vanillin Production Plant From Black Liquor

2. Lignin The term lignin is derived from the Latin word for wood lignum. Lignin is a major constituent in structural cell walls of all higher vascular land plants. Its polyphenolic structure is well known for its role in woody biomass to give resistance to biological and chemical degradation. Lignin is third component macromolecule of wood associated kovalen with cellulose and hemicellulose. At this time and future, the application of lignin has prospect. Lignin commercially can be used as binder, filler, surfactant, polymer product, disperser and others chemical raw, especially benzene derivate.

Figure 1.4 Sustainable industrial wood biorefinery operated by Borregaard, Norway (2010).

Lignin is a renewable raw material that could potentially be used as a raw material in the manufacture of vanillin. This sustainable resource is to be used within the biobased economy which is expected in the years to come to gradually take a larger share compared to the fossil-based economy. The biobased economy is not just the implementation of innovative technologies using renewable resources, but it will be a real transition with a broad and high impact on society at different levels (Langeveld and Sanders 2010). The use of lignin as a raw material has the advantage in terms of availability of raw material is abundant, especially in Indonesia. Lignin is an organic compound produced by woody plants and Indonesia are rich of it. One of lignin source which has abundant availability in Indonesia are oil palm empty fruit bunches (PEFB). At present and for the future, Indonesia is one of the largest palm oil producing country in the world that automatically as well as the world's largest producer of PEFB. However, in the manufacture of vanillin, PEFB

10

Preliminary Design of Vanillin Production Plant From Black Liquor

ineffective if used as a raw material because of the process is not possible. Initial pre-treatment to get lignin from PEFB not support passage of vanillin plant. This is because the process of getting lignin is too complicated and a lot of equipment needed. Moreover, until now there has been none of plant that utilizes PEFB as raw materials in Indonesia. Another alternative that can be used as raw material is black liquor. Black liquor is the waste produced by the pulp and paper plant. Black liquor availability is very abundant in Indonesia because Indonesia is one of the largest paper producers in Southeast Asia. Therefore, black liquor can be used as renewable raw materials in the vanillin manufacture. PT. Riau Andalan Pulp and Paper is a pulp and paper plant that produced black liquor in Indonesia. The plant can produce 4.92 million tons of black liquor per year. 10% of black liquor produced by this plant can support the needs of vanillin for 20 years. Not only that, the processing of black liquor into lignin is much more economical compared with the processing of PEFB into lignin. Based on the explanation above, it was concluded that the raw materials used to produce lignin vanillin was obtained from black liquor.

Table1.2 Analysis of Selection Raw Material

No 1

Considerations Factor Raw material availability

PEFB 5

Black Liquor 4

Distance traveled raw materials

Substances in the material and the quality of the products

Materials processing efficiency

Material prices

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Preliminary Design of Vanillin Production Plant From Black Liquor

1.3.2

Location Analysis

1.3.2.1 Raw Material Availability Aspect Raw material availability aspect is the most influence aspect to decide the location of the plant that we want to build. Relating to this aspect, plant construction must near with the source of raw material to minimize the transportation cost and also avoid production obstacle due to raw material supply. Main raw material of vanillin plant is black liquor as waste of pulp and paper production plant. In Indonesia, The biggest pulp and paper industry is Riau Andalan Paper and Pulp (RAPP) with production capacity about two million tonnes a year. As one of the largest integrated pulp and paper mill in the world, black liquor as the waste production is so much, around 4.920.000 m3 a year. RAPP locates in PangkalanKerinci village, Langgam sub-district, Pelalawan Regency, Riau, Sumatra. Based on black liquor availability, we choose to build our plant in Pelalawan Regency, Riau near RAPP plant. Actually, the black liquor of this plant is used to production methanol as renewable energy and reduced consumption of fossil fuel for their plant. On the other side, total mass of black liquor that we need per day is 1000.5 tonnes or just about 0.007% from the total black liquor waste production per day from RAPP. Therefore, we sure that RAPP will give the black liquor as our raw material plant. Figure 1.5, 1.6, and 1.7 show the location of RAPP and also location of vanillin plant that we want to build in Riau. 1.3.2.2 Utility Needs Availability Aspect The utility needs for vanillin plant is water, electricity, and fuel. The water need is obtained PDAM and Kampar Kiri River near the plant. Meanwhile energy fuel resource is obtained from Pertamina RU II Dumai which is distributed through piping.Te electricity need is obtained from PLTA.

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Preliminary Design of Vanillin Production Plant From Black Liquor

Vanillin Plant Riau Andalan Pulp & Paper (Sumber Black Liquor)

Figure 1.5. Location of raw material avaibility and plant building Source: BadanKoordinasi Survey danPemetaanNasional, 2002

Vanillin Plant

Riau Andalan Pulp & Paper (Sumber Black Liquor)

Figure 1.6. Location of raw material avaibility and plant building Source : googlemap.com

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Preliminary Design of Vanillin Production Plant From Black Liquor

Vanillin Plant

Riau Andalan Pulp & Paper (Sumber Black Liquor)

Figure 1.7. Location of raw material avaibility and plant building Source : googlemap.com

1.3.2.3 Product Marketting Aspect Our consumer is food companies especially milk, chocolate, and ice cream industy. Most of that company locates in Cikarang industrial area.Some of the biggest company are Unilever, Nestle, Diamond, and Campina.Vanillin product will be distributed via land and sea transportation.Based on market place above, vanillin plant in Pekanbaru, Riau is not too strategic because far from food company target. We need more cost to distribute vanillin product. However, if we compare with choosing to build vanillin plant near the market target, cost for distribute vanillin product from Riau to Cikarang is lower than cost for deliver raw material from riau to Cikarang.

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Preliminary Design of Vanillin Production Plant From Black Liquor

1.3.2.4 Transportation Aspect Transportation in our plant is need to support our process production plant, mainly for supply the supporting material and distribution the vanillin to the target marketing. From the figure 1.4.3, we can looked that our plant is near with east main road Jambi-Riau. Our plant also near with the Kampar Kiri River. For, the air transport, our plant is near with the Sultan SyarifKasim II Airport in Pekanbaru. Therefore, from the transportation aspect, our plant location is strategic. 1.3.2.5 Social and Environment Aspect 1. Geographic Aspect Pelalawan regency is one of ten regency in Riau Province and located at 00o46,24 LU - 00o24,34 LS dan 101o 30,37-103o21,36 BT.Pelalawan has area about 13.256,7 km2danborders to the following area. a. North : Siak regency b. South :IndragiriHuluand Indragiri Hilirregency c. West : Kampar danIndragiriHulurengency d. East :Karimun, Kepulauan Riau province, Bengkalis regency Pelalawan regency topography consist of lowland and hill, which the lowland is about 93% from total area of Pelalawan Regency. Ground characteristic from certain parts are organic ground and acidic with brackish ground water. The humidity and temperature quite high. In general, Pelalawan regency is suitable use for plant construction because the ground structur is flat, not bumpy, and near with water resource. 2. Social Aspect The number of residents in regency Pelalawan based on survey in 2009 (BPS, 2009) is 280.197, consist of 145.442 are men (51,54%) and 134.775 are women (48,46%). Majority residents are moslem (257.447 people) and the others are Protestan, Katolik, Hindu, and Budha. 3. Labor Aspect The occupation of Pelalawan regency residents is quite diverse. There are businessman, farmer, fisherman, labor, and others. The

15

Preliminary Design of Vanillin Production Plant From Black Liquor

availability of labor is quite big due to Riau province have many Industry and residents. Therefore we can quite easily get the labor. 1.3.3 Market & Capacity Analysis Vanillin is a versatile, well-established aroma chemical used mostly as a

flavourcompound. The total world market is estimated at 10,500 tons per annum. Themajor applications are in the manufacture of chocolate and ice cream, with smallerquantities used in baked goods and confectionery. Vanillin can also be used as a fragrance and fixative in perfumes, cosmetics and other fragrance mixtures. It is alsoused as a pharmaceutical intermediate.Commercial users can choose between natural vanilla (very expensive and used onlyin niche markets), nature-identical vanillin (guaiacol or lignin vanillin), and artificialvanilla flavour (ethyl vanillin).

Figure 1.8 Vanillin Use for Flavour Market Source : www.nedlac.org.za/media/5959/industry.pdf

Natural vanilla flavouring, produced from the pod of the vanilla orchid by extraction of the aroma compounds with ethanol, constitutes less than 5% of the world market. Natural vanilla contains both vanillin and a range ofother aroma chemicals, which in total are responsible for the full flavour of true vanilla. Natural vanilla is considerably more expensive than synthetic vanillin by afactor of 10. Synthetic vanillin is produced on a commercial scale using two distinct technologies.Vanillin produced by the different process routes has different flavour profiles.Consumer preference ultimately drives demand for the different vanillin products. Incertain applications, particularly the perfume industry, 16

Preliminary Design of Vanillin Production Plant From Black Liquor

European chocolate manufacturers, and the Japanese market, lignin vanillin is preferred over guaiacolvanillin. As is the case with most aroma chemicals used in the flavour industry,companies are reluctant to change from current suppliers as the organoleptic profilewill also change. The world demand for vanillin in its major applications is as follows: The world demand for vanillin in its major applications is as follows: Table 1.3 Vanillin World Demand Applications

Source : www.nedlac.org.za/media/5959/industry.pdf

Vanillin is a mature market, and the market is growing steadily, anticipated to be 23% over the next few years. Flavour and fragrance applications continue to expandin line with demographics and increases with disposable income. As a result, thegrowth in consumption of vanillin in flavour and fragrance products is growing at 4%in developing nations, in comparison to 2% in developed regions.Vanillin for many years was used as an intermediate for 2,3,5-trimethoxybenzaldehyde, which itself is an intermediate for the drug trimethoprim.This product is now however manufactured almost exclusively in China using thecheaper gallic acid route. In the 1980s the use of vanillin as a pharmaceuticalintermediate in the production of drugs such as L-methyl dopa declined. It has nowlevelled to approximately 10% of total vanillin demand. In Europe, the use of vanillinas a pharmaceutical intermediate appears to be captive to Rhodia. The globaldemand for vanillin is estimated as follows:

17

Preliminary Design of Vanillin Production Plant From Black Liquor

Tabel 1.4 World Demands for Vanillin

Source : www.nedlac.org.za/media/5959/industry.pdf

The high cost of production and natural vanillin causes the industries of vanillin consumer (foods and drinks, pharmaceuticals, and perfumes) in Indonesia prefer to choose using synthetic vanillin which is imported from other countries. Based on literature that we have learned, there is several reasons Indonesia has to import synthetic vanillin. Firstly, in agricultural areas that producing vanilla beans such as Jawa Tengah, Jawa Timur, Bali, Nusa Tenggara Timur, Sulawesi Utara, Lampung, and Sumatra are found the pest of vanillin called Busuk Batang Vanili (BBV). It is the primary diseases and became one of problems in Indonesias vanillin production since 1960 (Soetono 1962; Hadisutrisno et al. 1967; Risfaheri et al. 1998). BBV has destroyed vanilla plants in production areas so it causes loosing of billions of rupiahs every years. The loss that caused by BBV in 1991 is predicted almost Rp 32 billions (Untung, 1992). The damage of vanillin plants caused by BBV In Bali is almost 80% (Sedhana, 1996). The consequences are the cost of vanillin natural is so much expensive and not sold in Indonesias markets so the natural vanillin products is exported to many countries. In the other hand, vanillin needs in Indonesia is fulfilled by synthetic vanillin product import that much cheaper. Literally, the good or bad market qualities from vanillin commodities, is not only determined by the vanilla qualities. There is many things that determine the vanillin quality markets, they are farmer, collector, wholesaler, processor, importir and also the marketing models that used in market systems. This case also causes synthetic vanilin cost that imported by Indonesia is so expensive. Price
of natural vanillin producton the marketis 3-4 times the price of synthetic vanillin. Price

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Preliminary Design of Vanillin Production Plant From Black Liquor

of natural vanilla extract U.S.$ 30-60 per gallon, while the priceof synthetic vanillin U.S.$10-15 pergallon(Schultz, 2005, referenced inMelawati2006).

Synthetic vanillin prodution is predicted about 3000 tonnes per year, whereas the global market demand of synthetic vanillin reaches 3500 tonnes. Along with the development of food and drink and pharmaceutical industries, the demand of synthetic vanillin will always increase with velocity 8-9% per year with the market target in USA 27 %, Eropa 45 %, Asia 21 % and others 7 %. For saving the foreign exchange and decreasing the dependence of vanillin import, so the production of synthetic vanillin with efficien process technology and high quality product is needed. This indicates that the vanillin market in Indonesia is big enough. In the future, we predict that the interest of people in Indonesia for the products such as ice cream, chocolate and the others semi-luxury foods FMCG owns like Walls, Campina, Diamond, Nestle and others will increase too. Moreover, today, the cake factories in big cities have increased so big. This case is supported with three reasons. Firstly, the facts that the economic growth is stable enough and will increase straightly. It will effect the amounts of middle class people in Indonesia which has high purchasing power is increased too. Finally, the semi-luxury food products that contains vanilla will be more affordable and demand will increase continously. Secondly, the aggresiveness of large FMCG campanies in Indonesia causes their volume increases continously.
As a result, demand forvanillaas one of theraw materialswould be even greater . The last reasonis that Indonesiais havingstyle trendsof consumerismwhere the need forfood and beverageis notanymorelimited tostaplefoods anddrinksbut also thesemi-luxury foods and drinksthat tendimpulsive. Wetried tomap thelocation ofplant semi-luxuryfood and beverage productsthat wil be our prospective customers. Someof these companiesare listed in Table 1.5 below.

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table 1.5 FMCG Companies

No

Companies

Products Ice Creams : Magnum, Paddle Pop,

1 Wall's

Vienetta, Cornetto, Buavita, etc Ice Creams: Concerto, Hula-Hula,

2 Campina 3 Diamond 4 PT IndoMeiji Diary Food 5 PT Ceres 6 PT Cadbury Indonesia

Tropicana, Bazooka, etc Ice Creams Ice Creams Chocolates Chocolates Coffees (Nescafe), Milk (Milo,

7 PT Nestl Indonesia

Carnation), Candies (FOXS)

Needs of vanillin in Indonesia until this plant design was done is still filled with synthetic vanillin imported from China. This vanillin factory has a useful life 20 years. We assumed that vanillin neededs always grow every years according to projections import data we have collected. Thus the amount of vanila needed each year until 2035 (according to the useful life on the plant) can be calculated.
Table 1.6 Vanillin Needs in Indonesia

Code

Commodity

2007

2008

2009

2010

2011

Trend

291241 Vanillin (4-hydroxy-3- 2,413.8 3,320.5 3,165.4 4,564.1 3,873 13.47 methoxybenzaldehyde)

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Preliminary Design of Vanillin Production Plant From Black Liquor

6000 5000 4000 3000 2000 1000 0 2006.5 2007 2007.5 2008 2008.5 2009 2009.5 2010 y = 4E-133e0.1559x R = 0.8783 2010.5 2011 2011.5

Figure 1.9 Curve Vanillin Needs in Indonesia

Prediction and calculation needs vanillin until 2035 are shown in Table 1.7 below.
Table 1.7 Value of Imported Vanillin in 2015-2035

Indonesian Years Imported Vanillin (ton) 2011 2012 2013 2014 2015 2016 2017 2018 2019 2020 2021 2022 288 336 393 459 537 627 733 857 1001 1170 1367 1598 2023 2024 2025 2026 2027 2028 2029 2030 2031 2032 2033 2034 2035 Years

Indonesian Imported Vanillin (ton) 1868 2183 2551 2981 3484 4072 4759 5562 6501 7597 8879 10377 12128

Vanillin factory will be built in 2013-2015 and began operating in 2015. The factory is designed to meet 53% requirement of vanilla in 2025. Because
production in 2015-2035 produced about 4.5 tons per day. Amount of excess vanillin

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Preliminary Design of Vanillin Production Plant From Black Liquor

which we produce will be exported to Australia so the factory will not be lossin the beginning of the operation. The production capacity of the factory is shown in the table 1.8 below.
Table 1.8 Production Capacity 2015-2035

Years 2013 2014 2015 2016 2017 2018 2019 2020 2021 2022 2023 2024 2025 2026 2027 2028 2029 2030 2031 2032 2033 2034 2035

Demand of Vanillin in Indonesia (ton) 393 459 537 627 733 857 1001 1170 1367 1598 1868 2183 2551 2981 3484 4072 4759 5562 6501 7597 8879 10377 12128

Plant Production Capacity (ton) Building Plant Building Plant 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350 1350

Excess of Production (ton)

813 723 617 493 349 180

Thus, the plant design for the production of synthetic vanillin from lignin can bedone, because the assessment can be realized technically and financially feasible. Feasibility is a projection that could change if the price of raw material or product prices fluctuate, so it is recommended to do innovation processes to reduce production costs and still prioritize the qualities of synthetic vanillin.

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Preliminary Design of Vanillin Production Plant From Black Liquor

CHAPTER 2 PROCESS DESIGN 2.1 Process Technology Selection In the manufacture of vanillin, a process that is needed is a method of decision LignoBoost. Lignin from black liquor and high temperature oxidation process in a reactor that will produce vanillin. In addition to the method above methods, other ways that are often used in the making of the balck liquor lignin, which Organosolv method using alcohol. Organosolv method is the technology used to convert biomass into compounds lignosellulosic the compound cellulose, lignin, and hemicellulose (Mosier et al., 2005). These technologies include enzymatic fractionating by cellulases and chemical hydrolysis by hot water treatment, steam explosion, ammonia fiber explosion, dilute or concentrated acid hydrolysis, alkaline treatment and organosolv processes. While Organosolv process itself means the use of ethanol in the pre-treatment process in biorefinery useful to recover the desired multiple lignin products. While LignoBoost is a method of making lignin extraction from black liquor using a compact cake or pellets and products can be used for biofuels or raw material for the chemical industry. LignoBoost works in conjunction with evaporation. It all starts with being precipitated lignin from the black liquor by lowering the pH with CO2. The precipitate is then dewatered using a filter press. LignoBoost then overcomes conventional sodium filtering and separation problems by redissolving the lignin in spent wash water and acid. The resulting slurry is dewatered and washed once again, with acidified wash water, to produce virtually pure lignin cakes. The lignin can be exported or, after the final drying, be used as fuel in the lime kiln.

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Preliminary Design of Vanillin Production Plant From Black Liquor

Figure 2.1 Proses Lignoboost

Table 2.1 Scoring Process of Lignin Production

Parameter Organosolv Process LignoBoost Process

Retention Time (30%) 1 4

Process Handling (10%) 1 3

Cost (40%) 3 1

Concentration Obtained (20%) 1 4

Total 1.8 2.7

Retention time is the length of time used in the process of making lignin. The greater nilainy, means less time spent in the process. Conversely, the more time spent, indicating the smaller value given. In the references we get, the time used to process more than one day Organosolv in a single batch. Meanwhile, LignoBoost Process only requires 4 hours in a single batch. Handling Process is how easy the process was done. In a reference point that we get, Organosolv mixing process using the process at every stage of the process used to be done so that the guard is large enough. Meanwhile, LignoBoost Process conducted in a reactor so that maintenance is done not so great. Cost is

24

Preliminary Design of Vanillin Production Plant From Black Liquor

how inexpensive process. Process Organosolv use only simple tools are used so the cost is not expensive. Otherways, LignoBoost Process using a mixing tank used so the cost is very expensive. Obtained Concentration is how much product. With a very high price, LignoBoost Process can use the tank so that the results can be produced very much. The next process is the process of making lignin into vanillin. In the manufacture of vanillin tool used is oxidation reactor. Reactor oxidation can be used in a continuous or batch mode. Continuous process is usually done to reduce the area of the plant so that the plant will be used more efficiently. In contrast, batch processes are used to meet the needs of the production of very large so the existing plant will be larger wide area.
Table 2.2 Scoring process in Oxidation Reactor

Process Parameter Time (30%) Batch System Continous System 2

Process Handling (10%) 2

Cost (20%)

Concentration Obtained (30%) 3

Mass Transfer (10%) 3 2.4 Total

2.2

According to the tables above our team will choose is a batch process Because of five parameters. Parameters that we choose is big factor in building a plant. There are Process time, process handling, cost, consentration obatained, and mass transfer. If the value of retention time is high, it means retention time of that process happen in not a long time. Otherwise we if the retention time is low, it means we need a long time in the process. In a batch system, process time need 12 hours a day. While in Continuous System, it takes time in one process can not be calculated Because every second of BCR will produce. If the value of the cost is high, it means the process is cheap and if low, it means the process is expensive. Batch system is more expensive than continuous process Because in batch system, the area will be very huge to cover capacity of the plant. If the value of concentration obtained is high, it means we have a big

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Preliminary Design of Vanillin Production Plant From Black Liquor

product in that process, and if low it means the product is small amount. Batch system will produce until 0871 amounted to 0.7 g / L, while, for the continuous process is 0.56 until 0.67 g / L. Mass transfer describe the amount of movement of a substance that will the make the process efficient. High value is big mass transfer, low mass transfer value is small. Batch system will result in a greater mass transfer due to the mass of those who dwell in the reactor. 2.2 2.2.1 Process Description Type Of Process In vanillin production process, there are two primary stages to

producevanillin from black liquor. Black liquor contains typically 30 to 34% of lignin in dry solid weight basis. Lignin should be extracted from black liquor with LignoBosstprocess and continued with conversion of lignin to vanillin.

Figure 2.2 Diagram of vanillin production process

2.2.1.1

Lignin Extraction from Black Liquor LignoBoost is a complete system that extracts ligninfrom Kraft black

liquor.LignoBoost works in conjunction with evaporation.In the LignoBoost process, a stream of black liquor is taken from the black liquor evaporation plant (Fig. 2.2), then lignin is precipitated by acidification (the preferred acid is CO 2) and filtered (chamber press filter 1, Fig. 2.2).Instead of washing lignin immediately after filtration, as in traditional processes, the filter cake is redispersed and acidified (cake re-slurry, Fig. 2.2). The resulting slurry is then

26

Preliminary Design of Vanillin Production Plant From Black Liquor

filtered and washed by means of displacement washing (chamber press filter 2, Fig. 2.2). When the filter cake is re-dispersed in a liquid, at pH level and temperature values approximately equal to those of the final washing liquor, the concentration gradients during the washing stage will be low. The change in the pH level, most of the change in ionic strength and any change in lignin solubility will then take place in the slurry, and not in the filter cake or in the filter medium during washing.The filtrate fromchamber press filter 2 (filtration, washingand dewatering stages) should be recycled tothe weak black liquor. The resulting slurry is once again dewatered and washed, with acidified wash water, to produce virtually pure lignin cakes.In some cases, thisfiltrate can be also used for washing theunbleached or oxygen delignified pulp.The LignoBoost process therefore makesit possible to extract lignin efficiently fromthe black liquor in kraft mills. The majoradvantages, compared to the previoustechnology, are the following:the filter area and the volume of acidicwashing water can be kept at lowervalues, resulting in lower investmentcosts,the addition of sulfuric acid can be alsokept at a lower level, resulting in loweroperational costs,the yield of lignin is higher, the lignin has a lower ash and carbohydrate content, the lignin has a higher content of dry solids.

Figure 2.3General layout of the LignoBoost lignin removal process (post-treatment, drying and pulverizingare excluded)

2.2.1.2 Lignin Oxidation in Batch Process Production of vanillin lignin based must be made in alkaline conditions. Alkaline conditions is made to achieve a very high pH nearing pH 14, in addition 27

Preliminary Design of Vanillin Production Plant From Black Liquor

to high temperature conditions also are 1500C and 10 bar.The purpose of this process is to break the bond position of alpha-and beta-carbon of fenilpropane and breaking bonds in the carbon chain in the phenyl propane propanoid. Lignin oxidation process in batch mode formed in a jacketed reactor with controlled temperature and pressure. The reactor is under stirring and oxygen was fed to the reactor. LigninLingoboost outcome enter into a reactor that has a temperature operating conditions of 1500C and pressure of 10 bar.Alkaline conditions created by inserting NaOH pH 14 into reactor first. Then lignin lignoboost enter to the input process. After that, the solution oxidaze with O2 gas 50% N2 50%.Lignin reaction occurred with O2 being described at the beginning of the bond that ties will occur. NaOH will react also with lignin to form Sodium Vanilate.Sodium Vanilate is salt vanillin mixed with Na+ ions. In addition it also produced some of the content of impurity content to be separated. Lignin is not transformed to Sodium Vanilate 100% m. 2.2.1.3 Membrane Ultrafiltration Separation In the filtration process, the tool used is membrane ultrafikasi. Membraneultrafikasi used has a large cut-off membrane of 15 kDa, or about 1.6 nm and the pressure used is 0-4 bar. Vanillin has large molecules 152 Da MW, making vanillin will pass with the existing pores. This process begins with the entry of sodium vanilate and other impurities. This process aims to separate Sodium vanilate with other impurities by using the principle of molecular size difference. Sodiumvanilate is outflow and by product is lignin and impurities. Lignin obtained from the by-product will in turn go back to the oxidation tank to re reacted with O2. 2.2.1.4. Spray Dryer Spray drying is a method of producing a dry powder from a liquid or

slurry by rapidly drying with a hot gas. This is the preferred method of drying of many thermally-sensitive materials such as foods and pharmaceuticals. A consistent particle size distribution is a reason for spray drying some industrial products such as catalysts. Air is the heated drying medium; however, if the liquid

28

Preliminary Design of Vanillin Production Plant From Black Liquor

is a flammable solvent such as ethanol or the product is oxygen-sensitive then nitrogen is used. All spray dryers use some type of atomizer or spray nozzle to disperse the liquid or slurry into a controlled drop size spray. The most common of these are rotary disks and single-fluid high pressure swirl nozzles. Alternatively, for some applications two-fluid or ultrasonic nozzles are used. Depending on the process needs, drop sizes from 10 to 500 m can be achieved with the appropriate choices. The most common applications are in the 100 to 200 m diameter range. The dry powder is often free-flowing The most common spray dryers are called single effect as there is only one drying air on the top of the drying. In most cases the air is blown in co-current of the sprayed liquid. The powders obtained with such type of dryers are fine with a lot of dusts and a poor flowability. In order to reduce the dusts and increase the flowability of the powders, there is since over 20 years a new generation of spray dryers called multiple effect spray dryers. Instead of drying the liquid in one stage, the drying is done through two steps: one at the top (as per single effect) and one or an integrated static bed at the bottom of the chamber. The fine powders generated by the first stage drying can be recycled in continuous flow either at the top of the chamber (around the sprayed liquid) or at the bottom inside the integrated fluidized bed. The drying of the powder can be finalized on an external vibrating fluidized bed. The hot drying gas can be passed as a co-current or counter-current flow to the atomiser direction. The co-current flow enables the particles to have a lower residence time within the system and the particle separator (typically a cyclone device) operates more efficiently. The counter-current flow method enables a greater residence time of the particles in the chamber and usually is paired with a fluidized bed system.

29

Preliminary Design of Vanillin Production Plant From Black Liquor

2.2.2 BFD and Description

CO2

H2SO4

NaOH

Black Liquor Lignin Extraction (LignoBoost) Lignin Lignin Oxidation

Vanillin + Others Filtration

Vanillin Solution Drying

Powdered Vanillin

O2, N2 (50%,50%) Waste Liquor

VANILLIN PLANT FROM LIGNIN BLOCK FLOW DIAGRAM Drawn By : Checked By : Revised By : Darwing No. : Note : Date : Date : Without Scale A4

Figure 2.4 Block Flow Diagram Vanillin Plant from Lignin

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Preliminary Design of Vanillin Production Plant From Black Liquor

Two main process in Vanillin Plant from Lignin is lignin extraction from black liquor and vanillin oxidation from lignin itself. From this BFD the raw material, which is black liquor is treated with acid. lignin is precipitated by acidification (the preferred acid is CO2) and filtered. Instead of washing lignin immediately after filtration, as in traditional processes, the filter cake is redispersed and acidified (using H2SO4). The resulting slurry is then filtered and washed by means of displacement washing. After the slurry is filtered, the next process is blending with NaOH to make a base condition of solution before entering bubble column reactor. In bubble column reactor there will be oxidation reaction between lignin and oxygen. It will result the vanillin solution and the other compounds. To get vanillin, this solution must be separated using ultrafiltration, so the other compounds can be impeded at filter, and the filtrate contains only vanillin. The vanillin solution from ultrafiltration must be dried using spray dryer before it will be packed and distributed.

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Preliminary Design of Vanillin Production Plant From Black Liquor

2.2.3 PFD and Description

P-101 Black Liquor Pump S-101 BL Storage P-102 BL Pump V-101 BL Solid Treatment Vessel CS-101 Oxidation Reactor P-103 Slurry Pump PF-101 Plate & Frame Filter P-111 NaOH Pump P-104 Slurry Pump F-102 Air Blower V-102 Acidification Vessel P-105 Slurry Pump P-106 Slurry Pump P-107 Filtrate Pump PF-102 Plate & Frame Filter SR-101 Crusher P-108 Water Pump V-103 Lignin Solution Vessel P-109 H2SO4 Solution Pump H-101 Heat Exchanger Water P-110 5 Water P-108 7 Lean Liquor C-101 O2 and N2 Compressor UF-101 Membrane Ultrafiltration H-102 Heat Exchanger SD-101 Spray Dryer 10 H-103 Heat Exchanger B-103 Steam Reboiler

Black Liquor From pulp ind P-101

2 4 S-101 V-101 P-102 3 P-103 PF-101 6 C-101 V-102 9 P-107 PF-102

12

Alkali Sulfat + Liq Acid

CO2

F-101 8 H2SO4 C-102 P-109 11 19 25 H-101 13 NaOH P-111 V-103 14 P-104 V-104 P-106 CS-101 O2 and N2 16 26 27 Air H-102 F-101 24 28 30 Powder Vanillin 15 P-105 H-103 20 UF-101 21 P-107 SD-101 29 Air 17 18 22 Others N2

Steam

Water

23

B-101

VANILLIN PLANT FROM LIGNIN PROCESS FLOW DIAGRAM Drawn By : Checked By Revised By : Drawing No : Notes : Group 6 Date : Date : Without Scale A4

Figure 2.5 Process Flow Diagram Vanillin Plant from Lignin

32

Preliminary Design of Vanillin Production Plant From Black Liquor

The main process of this plant consists of LignoBoost process which is the lignin separation process from black liquor, and the core of this plant is vanillin oxidation from lignin extract from LignoBoost process. The LignoBoost process is started from black liquor solid separation from black liquor in V-101 until the filtration process of black liquor solid so the lignin is separated from black liquor solid. Otherwise the vanillin oxidation process is started while solid lignin resulted by filtration F-102 entering the blending storage V-103 and NaOH is also added in that storage, oxidation in bubble column reactor, ultrafiltration, until drying process of vanillin to be vanillin powder in spray dryer. From the PFD it can be seen that the black liquor from PT Riau Andalan Pulp and Paper flowing through the pipe and pumped by P-101 pump to the black liquor storage S-101. And then the black liquor is kept until the batch is started. The black liquor than is pumped through P-102 pump to be precipitated in black liquor treatment vessel V-101, CO2 is added to the storage. The slurry from V-101 is pumped to press chamber filter (Plate and frame) PF-101, and water is pumped by P-108 as washing eluent in filtration. As the result, solid black liquor is impeded above the filter as a cake. Then cake is brought using conveyor C-101 to Acidification vessel V-102 to be re-dispersed so the lignin can be extracted. It needs H2SO4 as an acid liquid at pH 4 to extract that lignin. When the filter cake is re-dispersed in a liquid, at pH level and temperature values approximately equal to those of the final washing liquor, the concentration gradients during the washing stage will be low. The change in the pH level, most of the change in ionic strength and any change in lignin solubility will then take place in the slurry, and not in the filter cake or in the filter medium during washing. From V-102 the extract is pumped by P-107 to press chamber filter (Plate and frame) PF-102, and water is pumped by P-110 as washing eluent in filtration. The lignin is in the cake then is brought to blending storage V-103 with NaOH by conveyor C-102. In blending storage lignin is dissolved in NaOH before it is added to bubble column reactor. NaOH will give a base condition as the optimum condition in this reaction. Before entering bubble column reactor, the lignin solution is pumped by P-105 pump. During the process, the lignin solution is heated to increase the temperature through the heat exchanger HE-101, the heat

33

Preliminary Design of Vanillin Production Plant From Black Liquor

exchanger agent is steam from boiler B-101 at 220oC. The output temperature of lignin slurry is 170oC and then it enter the bubble column reactor CS-101. The operation condition of bubble column reactor itself is 170oC and 10 bar pressure. In BCR lignin is reacted with O2 resulting vanillin and other compounds. The reaction can be explained below. Lignin oxidation : 0.5 L + 1.56 O2 V + 114 X Vanillin oxidation : V + O2 D
Stoichiometry 1 Conversion 70%

Lignin Oxidation : 0.5 L + 1.56 O2 --> V + 114 X Initial (mol) Change (mol) Remaining (mol) 2350.242 10781.25 -1645.17 -7332.75 4700.483 705.0725 3448.496 4700.483 Stoichiometry 2 Vanilin Oxidation : V + O2 --> Product Initial (mol) Change (mol) Remaining (mol) 4700.483 3448.496 -3290.34 -3290.34 3290.338 1410.145 158.1582 3290.338 massa 500592.048 gram 0.50059205 ton 500.592048 kg ( )

( )

( ) )

( )

( ) )

Where : A is Lignin B is Oxygen C is Vanillin D is Vanillin Acid Product

34

Preliminary Design of Vanillin Production Plant From Black Liquor

Rate Law :

The product from CS-101 is pumped using P-106 through HE-103 to Ultrafiltration membrane UF-101. The filtrate then pumped to spray dryer SD-101 (80oC). In SD-101 the liquid vanillin is powdered with hot air after passing the HE-102 at 120oC. Vanillin powder then is brought to packing building to be packaged. The cake from UF-101 is pumped to waste storage.

35

Preliminary Design of Vanillin Production Plant From Black Liquor

CHAPTER 3 MASS AND ENERGY BALANCE 3.1 3.1.1 Mass Balance Overall Mass Balance Overall mass balance in this system is explained in table 3.1 below :
Table. 3.1 Mass Balance in Entire Process

OVERALL FEED Black Liquor CO2 Water H2SO4 NaOH O2 N2 Waste Lean liquor Liquid acid Alkali sulfat Filtrate cake Hot air PRODUCT Vanillin TOTAL

Input (ton) 111.17 1.10 14.54 0.88 6.67 0.16 0.16 1.02 135.70

Output (ton) 0 0 22.98 0 0 0 0.16 68.92 25.48 5.29 10.14 2.22 0.50 135.70

While the composition of the black liquor and its content found in Figure 3.2
Table. 3.2 Black Liquor Composition

Black Liquor Composition Lignin (4.5%) Water (8%) Lean liquor (87,5%)

Total mass (ton) 5 8.89 97.27

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Preliminary Design of Vanillin Production Plant From Black Liquor

3.1.2

Mass Balance Process Units Primary Process Description and Mass Balance in Every Process Units are explained in the table below :
Table. 3.3 Mass Balance in Storage

STORAGE Lignin Alkali Water Lean liquor TOTAL

Input 1 (ton) 10.01 8.89 92.27 111.17

Output 2 (ton) 10.01 8.89 92.27 111.17

Table. 3.4 Mass Balance in Acidification Process

ACIDIFICATION I Lignin Alkali Water Lean Liquor CO2 Liquid Acid TOTAL

Input 2 (ton) 10.01 8.89 92.27 0 0 111.17

Input 3 (ton) 0 0 0 1.10 0 1.10

Output 4 (ton) 10.01 8.44 92.27 0 1.55 112.27 112.27

112.27

Table. 3.5 Mass Balance in Filtration Process

FILTRATION I Lignin Alkali Water Lean Liquor Liquid Acid lean liquor solid TOTAL

Input 4 Input 5 (ton) (ton) 10.01 0 8.44 11.12 92.27 0 1.55 0 0 0 112.27 11.12 123.38

Output 6 Output 7 (ton) (ton) 10.01 0 0 19.56 0 68.92 0 1.55 23.35 0 33.35 90.03 123.38

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table. 3.6 Mass Balance in Acidification Process

ACIDIFICATION II Lignin Alkali Lean liquor solid H2SO4 Lignin Alkali Sulfat Liquid acid TOTAL

Input6 (ton) 10.01 23.35 0 0 0 0 33.35 34.23

Input 8 (ton) 0 0.88 0 0 0 0.88

Output 9 (ton) 0 0 0 5 5.29 23.93 34.23 34.23

Table. 3.7 Mass Balance in Filtration Process

FILTRATON II Lignin Alkali sulfat Liquid acid Water TOTAL

Input 9 (ton) 5 5.29 23.93 0 34.23

Input 10 (ton) 0 0 3.42 3.42 37.65

Output 11 Output 12 (ton) (ton) 5 0 0 5.29 0 23.93 0 3.42 5.00 32.65 37.65

Table. 3.8 Mass Balance in Blending Process

BLENDING Lignin NaOH Lignin slurry TOTAL

Input 11 Input 13 (ton) (ton) 5 0 0 6.67 0 0 11.67

Output 14 (ton) 0 0 11.67 11.67

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table. 3.9 Mass Balance in Storage Lignin slurry

STORAGE Lignin NaOH Lignin slurry TOTAL

Input 13 Input 14 (ton) (ton) 5 0 0 6.67 0 0 11.67

Output 15 (ton) 0 0 11.67 11.67

Table. 3.10 Mass Balance in Oxidation Process

REACTOR OXIDATION Lignin slurry N2 O2 Alkali Ligin Slurry Water Vanillin Others TOTAL

Input 15 (ton) 11.67 0 0 0 0 0 0 11.67

Input 16 (ton) 0 0.16 0.16 0 0 0 0 0.33

Output 18 (ton) 0 0 0 5.36 1.20 0.50 4.78 11.84

Output 19 (ton) 0 0.16 0 0 0

0 0

0.16 12.00

12.00

Table. 3.11 Mass Balance in Ultrafiltration Process

ULTRAFILTRATION Vanillin Alkali Lignin Slurry water Others Filtrate Cake TOTAL

Input 18 (ton) 0.50 5.36 1.20 4.78 0 11.84 11.84

Output 20 Output 21 (ton) (ton) 0.50 0 0 0 1.20 0 0 0 0 10.14 1.70 10.14 11.84

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table. 3.12 Mass Balance in Drying Process

DRYING Vanillin water Hot Air Vanillin Powder TOTAL

Input 20 (ton) 0.50 1.20 0 0 1.70 2.72

Input 26 (ton) 0 0 1.02 0 1.02

Output 28 (ton) 0 0 2.22 0 2.22

Output 29 (ton) 0 0 0 0.50 0.50 2.72

3.2

Energy Balance
Table. 3.3.1 Mass Balance in Storage

STORAGE Lignin Alkali Water Lean liquor TOTAL

Input 1 (ton) 10.01 8.89 92.27 111.17

Output 2(ton) 10.01 8.89 92.27 111.17

Energy In (Joule) 0 0 0 0

Energy Out (Joule) 0 0 0 0

Table. 3.3.2 Mass Balance in Acidification Process

ACIDIFICATION I Lignin Alkali Water Lean Liquor CO2 Liquid Acid

Input 2 (ton) 10.01 8.89 92.27 0 0 111.17

Input 3 (ton) 0 0 0 1.10 0 1.10

Output 4 (ton) 10.01 8.44 92.27 0 1.55 112.27 112.27

Energy In (Joule) 0.00 141.31 0.00 27.64

Energy Out (Joule) 0.00 134.15 0.00

34.79

TOTAL

112.27

168.94

168.94

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table. 3.3.3 Mass Balance in Filtration Process

Input 4 FILTRATION I (ton) Lignin Alkali Water Lean Liquor Liquid Acid lean liquor solid TOTAL TOTAL 10.01 8.44 92.27 1.55 0 112.27 123.38

Input 5 (ton) 0 11.12 0 0 0 11.12

Output 6 (ton) 10.01 0 0 0 23.35 33.35

Output 7 (ton)

Energy In (Joule) 0 0 0 0 0 0

Energy Out (Joule) 0 0 0 0 0 0

0 19.56 68.92 1.55 0 90.03 123.38

Table. 3.3.4 Mass Balance in Acidification Process

ACIDIFICATION II Lignin Alkali Lean liquor solid H2SO4 Lignin Alkali Sulfat Liquid acid TOTAL TOTAL

Input6 (ton) 10.01 23.35 0 0 0 0 33.35 34.23

Input 8 (ton) 0

Output 9 (ton) 0 0

Energy In (Joule) 49689.61 138.50

Energy Out (Joule) 24844.81 24494.23 489.08

0.88 0 0 0 0.88

0 5 5.29 23.93 34.23 34.23

49828.12 49828.12

49828.12 49828.12

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table. 3.3.5 Mass Balance in Filtration Process

FILTRATON II Lignin Alkali sulfat Liquid acid Water

Input 9 (ton) 5 5.29 23.93 0 34.23

Input 10 (ton)

Output 11 (ton) 5

Output 12 (ton) 0 5.29 23.93 3.42 32.65

Energy In (Joule) 0 0 0 0 0

Energy Out (Joule) 0 0 0 0 0

0 0 3.42 3.42 37.65

0 0 0 5.00 37.65

TOTAL

Table. 3.3.6 Mass Balance in Blending Process

BLENDING Lignin NaOH Lignin slurry TOTAL

Input 11 (ton) 5 0 0 11.67

Input 13 (ton) 0 6.67 0

Output 14 (ton) 0 0 11.67 11.67

Energy In (Joule) 0 0

Energy Out (Joule)

0 0

Table. 3.3.7 Mass Balance in Storage Lignin Slurry

STORAGE Lignin NaOH Lignin slurry TOTAL

Input 11 (ton) 5 0 0 11.67

Input 13 (ton) 0 6.67 0

Output 14 (ton) 0 0 11.67 11.67

Energy In (Joule) 0 0

Energy Out (Joule)

0 0

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table. 3.3.8 Mass Balance in Oxidation Process

REACTOR OXIDATION Lignin slurry N2 O2 Alkali Ligin Slurry Water Vanillin Others Total TOTAL

Input 15 (ton) 11.67 0 0 0 0 0 0 11.67 12

Input 16 (ton) 0 0.16 0.16 0 0 0 0 0.33

Output 18 (ton) 0 0 0 5.36 1.20 0.50 4.78 11.84 12

Output 19 (ton) 0 0.16 0 0

Energy In (Joule) 57971.22 0 0 0.00

Energy Out (Joule) 0 0 0 0

0 0 0.16 57971.22 57971.22

0 0 2811317971.22 2811317971.22

Q masuk tambahan : 2811260000 J

Table. 3.3.9 Mass Balance in Ultrafiltration Process

ULTRAFILTRATION Input 18 (ton) Vanillin Water Alkali Lignin Slurry Others Filtrate Cake 0.50 5.36 1.20 4.78 0 11.84 TOTAL 11.84 Output 20 (ton) 0.50 0 1.20 0 0 1.70 11.84 Output 21 (ton) 0 0 0 0 10.14 10.14

Energy In (Joule) 0 0 0 0 0 0

Energy Out (Joule) 0 0 0 0 0 0

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table. 3.3.10 Mass Balance in Drying Process

DRYING

Input 20 (ton) 0.50 1.20 0 0

Input 26 (ton) 0 0 1.02 0

Output 28 (ton) 0 0 2.22 0

Output 29 (ton) 0 0 0 0.50

Energy In (Joule) 142800

Energy Out (Joule) 4445.67

Vanillin Hot Air Water Vanillin Powder

286850.67 0.00 0.00

1.70 TOTAL 2.72

1.02

2.22 2.72

0.50

142800

291296.34

Q masuk tambahan dari steam : 148496.34 J So, Total of the heat steam that we need is = 2811408496.34 = 2811.41 MJ

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Preliminary Design of Vanillin Production Plant From Black Liquor

CHAPTER 4 UTILITIES 4.1 Water Utility Water availability system in this vanillin plant is really needed to support the whole plant production. The water utility in this plant is needed as processes water, water for equipment washing, domestic water availability and fire extinguishing water. The water source design based on the water collection, processing system efficiency and economical factor. The explanation about this water utility consist as follows : 4.1.1 Water Utility Classification

4.1.1.1 Process Water Process water that used in this plant is used to solute NaOH that will enter oxidation reactor and for washer in filtration. In the whole process for this plant, water is not too needed because water component in the main raw material (black liquor) is 26% and the most of others materials is liquid solution. The water process needs in this plant reach 123,40 m3 per day. The details about the needs of water describes as follows :
Table 4.1 Total Process Water Needs in Plant

Unit Filtration 1 Filtration 2 Blending Total

Water (kg) 11120 3420 730 15270

4.1.1.2 Domestic Water This water is used to fulfill water needs for staff and other employers. Domestic water include toilet facilities, drinking water, water for watering gardens and many more. Assuming the total domestic water everyone is 100 litre/day. So, total water for domestic water if there is 100 persons in this plant is 10.000 litre/day.

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Preliminary Design of Vanillin Production Plant From Black Liquor

4.1.1.3 Fire Extinguishing Water Fire Extinguishing Water is used to extinguish fire if one day there is fire. This water is reserved to be used anytime. The firefighting water used was water with
the low specs, but has under gone treatment first. The amount of water required for fire is assumed to10,000 kg/day.

4.1.1.4 Total Water Requirements

Total water requirements needed for this plant per day covers the water needed for process water, cooling water, water heater, boiler feed water, domestic water and fire water. Total water requirement is shown in the table 5.1 below: Table 4.2 Total Water Needs in Plant

Using water Processing Water Domestic water Fire Extinguishing Water Total

Total (Kg/day) 15270 10000 1000 26270

4.1.1.5 Water Sources

Water supply to the plant will be taken from PT. Riau Andalan industrial area. PT Riau Andalan independently manage all water providers to the needs of industries that exist within the industry. Water supplied by PT Riau Andalan is considered clean enough and qualify for use as water for industrial plants. So in the factory there is no clean water management facilities further.

4.2

Electric Utility
As the plant in general, to run the equipment contained in the plant Vanillin,

energy required is not small. Equipment that requires a supply of energy, among others:

Pump Agitator Mixing Tank

Electricity need for vanillin production in this vanillin plant can be seen in the following table.

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table 4.3 Total Electricity Needs in Plant

Item No. V-101 V-102 V-103 P-101 P-102 P-103 P-104 P-105 P-106 P-107 P-108 P-109 P-110 P-111 C-101 C-102 C-103 C-104

Process unit Agitator CO2 precipitation tank Agitator H2SO4 precipitation tank Agitator lignin slurry tank Black liquor pump Black liquor pump CO2 precipitation pump Slurry pump Slurry pump Slurry pump Slurry pump Water pump H2SO4 precipitation pump Water pump NaOH pump Alkali lignin cake conveyor Black liquor solid conveyor Lignin solid conveyor Vanillin conveyor TOTAL

Kwh/ day 36.32 1.58 0.09 19.31 258.99 56.18 2.89 0.53 3.86 0.18 14.19 0.28 10.38 1.78 7.44 7.44 5.95 5.95 433.34

Kwh/year 10897 474.83 26.68 5792.45 77696.04 16854.27 865.74 157.70 1157.32 53.46 258.08 84.69 3113.53 533.65 2232 2232 1785 1785 125999.44

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Preliminary Design of Vanillin Production Plant From Black Liquor

Electricity need at vanillin plant is AC (accuired current) power type. Total electricity needs for processes of this plant is equal to 433.34 kWh/day. While the need support for lighting and other assumed 30% of the total energy is 130 kWh/day. So the total electricity need of vanillin plant is 125999.44 kWh/year. Electrical power is largely used for two purposes primary. The first necessity is requiring electrical power needs the production process. The second purpose is to use electrical power production support facilities. Electricity used for support facilities for the needs of lighting and air-conditioning (AC) in the office, laboratories, workshops, as well as the control room, air supply (tap and clean), water supply (and the net), and the sewage treatment plant. 4.3 Steam Utility In this vanillin plant, steam utility is needed for heating the reactor through

the jacket. Reaction temperature needed in that process is 170oC. Based on calculation, it is obtained that heat needed for reactor is 253.01 MJ per day. It is assumed that steam needed is provided from diesel as fuels. Assuming that efficiency from boiler is 40%. So, the diesel as fuels to produce steam in this vanillin plant is :

m = 303 litre per day

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Preliminary Design of Vanillin Production Plant From Black Liquor

BAB 5 SIZING 5.1 Vessel 5.1.1 Black Liquor Storage Tank (S-101)

STORAGE TANK

Identification:

Item Item no. No. required

Black Liquor Storage Tank S-101 3

Function: Operation: Material handled: Composition (%): Black Liquor Design data

Storage black liquor to keep it from microorganism and algae Discrete Black Liquor

100 Capacity (kg) Feed quantity (m3/h) Operating temperature (K) Operating pressure (psi) Storage Tank Specification Type Material of construction Diameter (m) Height (m) Thickness of shell (cm) Thickness of Roof (cm) Flat-bottomed cylindrical vessel Stainless steel 316 7.16 9.55 2.97 2.97 333500 326.57 333 14.70

Controls:

S-101 for controlling Black liquor solution

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.1.2

Acidification Tank (V-101) MIXER TANK

Identification:

Item Item no. No. required

Mixer Tank V-101 5

Function: Operation:

To precipitation black liquor with CO2 Discrete

Material handled: Black Liquor slurry Composition (%): Black Liquor Slurry Design data Capacity (kg) Feed quantity (m3/h) Operating temperature (K) Residence time (h) Operating pressure (psi) Mixer Tank Specification Type Material of construction Diameter(m) Height (m) Thickness of shell (cm) Thickness of roof (cm) Impeller Design Type Diameter (m) Agitator space from based (m) Blade width (m) Impeller speed (rpm) Power (kWh) Controls: Flow turbine with 4 blades 1.16 0.55 0.15 60 0.81 V-101 for precipitation black liquor slurry Flat-bottom cylindrical vessel Stainless steel 316 2.90 3.87 2.12 2.12 22230 21.773 333 1 14.7 100

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.1.3

Acidification Tank (V-102) MIXER TANK

Identification:

Item Item no. No. required

Mixer Tank V-102 (A) 1

Function: Operation:

Acidification process of black liquor slurry Discrete

Material handled: Black Liquor slurry Composition (%): Black Liquor Slurry Design data Capacity (kg) Feed quantity (m3/h) Operating temperature (K) Residence time (h) Operating pressure (psi) Mixer Tank Specification Type Material of construction Diameter(m) Height (m) Thickness of shell (cm) Thickness of roof (cm) Impeller Design Type Diameter (m) Agitator space from based (m) Blade width (m) Impeller speed (rpm) Power (kWh) Controls: Flow turbine with 4 blades 0.92 0.43 0.12 60 0.23 V-102 for precipitation black liquor slurry Flat-bottom cylindrical vessel Stainless steel 316 2.30 3.06 2.06 2.06 20540 21.58 333 0.5 14.7 100

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Preliminary Design of Vanillin Production Plant From Black Liquor

MIXER TANK

Identification:

Item Item no. No. required

Mixer Tank V-102 (B) 1

Function: Operation:

Acidification process of black liquor slurry Discrete

Material handled: Black Liquor slurry Composition (%): Black Liquor Slurry Design data Capacity (kg) Feed quantity (m3/h) Operating temperature (K) Residence time (h) Operating pressure (psi) Mixer Tank Specification Type Material of construction Diameter(m) Height (m) Thickness of shell (cm) Thickness of roof (cm) Impeller Design Type Diameter (m) Agitator space from based (m) Blade width (m) Impeller speed (rpm) Power (kWh) Controls: Flow turbine with 4 blades 0.80 0.38 0.10 60 0.12 V-102 for precipitation black liquor slurry Flat-bottom cylindrical vessel Stainless steel 316 2.01 2.68 2.02 2.02 13690 14.38 333 0.5 14.7 100

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.1.4

Blending Tank (V-103)

MIXER TANK Identification: Item Item no. No. required Function: Operation: Mixer Tank V-103 1

To make lignin slurry Discrete

Material handled: Lignin slurry Composition (%): Lignin Slurry Design data Capacity (kg) Feed quantity (m3/h) Operating temperature (K) Residence time (h) Operating pressure (psi) Mixer Tank Specification Type Material of construction Diameter(m) Height (m) Thickness of shell (cm) Thickness of roof (cm) Impeller Design Type Diameter (m) Agitator space from based (m) Blade width (m) Impeller speed (rpm) Power (kWh) Controls: V-103 for make lignin slurry Flow turbine with 4 blades 1.81 0.86 0.23 60 8.8 Flat-bottom cylindrical vessel Plate steels SA-283 grade C 4.53 6.04 0.70 0.70 100

150075 6.89 333 0.167 13.24

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.1.5

Lignin Slurry Storage (S-102)

STORAGE TANK

Identification:

Item Item no. No. required

Lignin Slurry Storage Tank S-102 1

Function: Operation:

Storage lignin slurry before enter to bubble column reactor Discrete

Material handled: Black Liquor Composition (%): Lignin Slurry Design data 100 Capacity (kg) Feed quantity (m3/h) Operating temperature (K) Operating pressure (psi) Storage Tank Specification Type Material of construction Diameter (m) Height (m) Thickness of shell (cm) Thickness of Roof (cm) Controls: Flat-bottomed cylindrical vessel Stainless steel 316 1.93 2.58 2.10 2.10 11670 6.43 333 14.70

S-102 for controlling lignin slurry

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.1.6

Waste Storage (S-103)

STORAGE TANK

Identification:

Item Item no. No. required

Waste Storage Tank S-103 2

Function: Operation:

Waste storage from the process Discrete

Material handled: Waste from process Composition (%): Waste Design data 100 Capacity (kg) Feed quantity (m3/h) Operating temperature (K) Operating pressure (psi) Storage Tank Specification Type Material of construction Diameter (m) Height (m) Thickness of shell (cm) Thickness of Roof (cm) Controls: Flat-bottomed cylindrical vessel Carbon steel 7.07 9.43 3.63 3.63 597670 13.11 333 14.70

S-103 for controlling waste from process

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.1.7

H2SO4 Storage (S-104) STORAGE TANK

Identification:

Item Item no. No. required

H2SO4 Storage Tank S-104 1

Function: Operation:

Storage H2SO4 to keep it before enter to process Discrete

Material handled: H2SO4 Composition (%): H2SO4 Design data 100 Capacity (kg) Feed quantity (m3/h) Operating temperature (K) Operating pressure (psi) Storage Tank Specification Type Material of construction Diameter (m) Height (m) Thickness of shell (cm) Thickness of Roof (cm) Controls: Flat-bottomed cylindrical vessel Stainless steel 316 3.07 4.09 2.40 2.40 47273.63 25.69 333 14.70

S-103 for controlling H2SO4 from process

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.1.8

NaOH Storage (S-105) STORAGE TANK

Identification:

Item Item no. No. required

NaOH Storage Tank S-105 1

Function: Operation:

Storage NaOH to keep it before enter to process Discrete

Material handled: NaOH Composition (%): NaOH Design data 100 Capacity (kg) Feed quantity (m3/h) Operating temperature (K) Operating pressure (psi) Storage Tank Specification Type Material of construction Diameter (m) Height (m) Thickness of shell (cm) Thickness of Roof (cm) Controls: Flat-bottomed cylindrical vessel Stainless steel 316 5.75 7.67 2.70 2.70 360180 169.10 333 14.70

S-105 for controlling NaOH

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.2 Filtration 5.2.1 Plate and Frame Filter (PF-101)

Lignin Alkali Press Filter Identification: Item Item no. No. required Function: Operation: Material handled: Design data: Lignin Press Filter PF-101 4

To get lignin alkali solid and lean liquor solid, separate it from lean liquor, liquid acid, and water. batch Lignin slurry Operating temperature (K) Operating pressure (Pa) Type Material of construction Effective filtration Area (m2) Filtration area with safety factor 20% (m2) Filter chamber size (m) Number of chambers L (m) W (m) H (m) Weight empty (ton) Total press filter required (item) Total plates required 303 7 x 105 Vertical Plate Airblow (VPA) Stainless steel 316 345

414 2.03 x 2.03 50 15.6 4.25 4.58 80 4 200

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.2.2

Plate and Frame Filter (PF-102)

Lignin Press Filter

Identification:

Item Item no. No. required

Lignin Press Filter PF-102 1

Function: Operation: Material handled: Design data:

To get solid lignin and separate it from alkali suphate, liquid acid, and water. batch Lignin slurry Operating temperature (K) Operating pressure (Pa) Type Material of construction Effective filtration Area (m2) Filtration area with safety factor 20% (m2) Filter chamber size (m) Number of chambers L (m) W (m) H (m) Weight empty (ton) Total press filter required (item) Total plates required 303 7 x 105 Vertical Plate Airblow (VPA) Stainless steel 316 40.06

48.08 1.5 x 1.5 24 8.5 3.8 3.16 27.5 1 21

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.3 Pump 5.3.1 Black Liquor Pump (P-101) Function : Pumping black liquor to acidification tank I Type Number of Unit No. 1 2 3 : Centrifugal pump : 1 unit

Specification Scope Service condition Operating condition Capacity (ton/h) Suction pressure (Pa) Power (kWh) 66.77 100,000 0.32 Double end-Vertical screw pump Continuous process

Liquid Properties Liquid to be handled Viscosity (cp) Black liqour 5.091

Temperature of liquid at inlet 60 (C) 5 Material Stainles steel

5.3.2 Black Liquor Acidification pump (P-102) Function : Pumping black liquor slurry from acidification tank to press filter I Type Number of Unit No. 1 2 3 : Centrifugal pump : 2 unit

Specification Scope Service condition Operating condition Centrifugal pump Continuous process

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Preliminary Design of Vanillin Production Plant From Black Liquor

Capacity (ton/h) Suction pressure (Pa) Power (kWh) 4 Liquid Properties Liquid to be handled Viscosity (cp)

33.38 105,000 2.36

Black liqour 1.70

Temperature of liquid at inlet 60 (C) 5 Material Stainles steel

5.3.3 Lignin Acidification Pump (P-103) Function : Pumping sludge from acidification tank to filter press II Type Number of Unit No. 1 2 3 : Piston pump : 1 unit

Specification Scope Service condition Operating condition Capacity (ton/h) Suction pressure (Pa) Power (kWh) 61.68 105,000 2.56 Screw pump Batch process

Liquid Properties Liquid to be handled Viscosity (cp) Black liqour 1.3169

Temperature of liquid at inlet 60

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Preliminary Design of Vanillin Production Plant From Black Liquor

(C) 5 Material Stainles steel

5.3.4 Lignin Solution Pump (P-104) Function : Pumping lignin slurry (lignin+water) from mixing tank to storage Type Number of Unit No. 1 2 3 : Screw Pump : 1 unit

Specification Scope Service condition Operating condition Capacity (ton/h) Suction pressure (Pa) Power (kWh) 35.15 105,000 0.07 Screw pump Batch process

Liquid Properties Liquid to be handled Viscosity (cp) Lignin Solution 2.0801

Temperature of liquid at inlet 60 (C) 5 Material Stainles steel

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.3.5 Lignin Solution Pump (P-105) Function : Pumping lignin slurry (lignin+water) from storage to BCR Type Number of Unit No. 1 2 3 : Screw Pump : 1 unit

Specification Scope Service condition Operating condition Capacity (ton/h) Suction pressure (Pa) Power (kWh) 49.21 105,000 0.12 Screw pump Batch process

Liquid Properties Liquid to be handled Viscosity (cp) Lignin Solution 2.0801

Temperature of liquid at inlet 60 (C) 5 Material Stainles steel

5.3.6 Vanillin Slurry Pump (P-106) Function : Pumping Vanilin solution from BCR to Ultrafikasi Type Number of Unit No. 1 2 3 : Screw pump : 1 unit

Specification Scope Service condition Operating condition Capacity (ton/h) 4.87 Screw pump Continous process

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Preliminary Design of Vanillin Production Plant From Black Liquor

Suction pressure (Pa) Power (kWh) 4 Liquid Properties Liquid to be handled Viscosity (cp)

200,000 0.32

Vanillin Solution 5.13

Temperature of liquid at inlet 60 (C) 5 Material Stainles steel

5.3.7 Vanillin Solution Pump (P-107) Function : Pumping Vanillin Solution to Spray Dryer Type Number of Unit No. 1 2 3 : Screw pump : 1 unit

Specification Scope Service condition Operating condition Capacity (ton/h) Suction pressure (Pa) Power (kWh) 0.85 105,000 0.03 Screw pump Continous process

Liquid Properties Liquid to be handled Viscosity (cp) Vanillin Slurry 1.65

Temperature of liquid at inlet 60 (C) 5 Material Stainles steel

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.3.8 Water Pump (P-109) Function : Pumping water from the reservoir to filtration Plate and Press I Type Number of Unit No. 1 2 3 : Piston Pump : 2 unit

Specification Scope Service condition Operating condition Capacity (ton/h) Suction pressure (Pa) Power (kWh) 3.34 105,000 0.26 Piston Pump Batch process

Liquid Properties Liquid to be handled Viscosity (cp) Water 1.65

Temperature of liquid at inlet 60 (C) 5 Material Carbon steel

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.4 Conveyor

Conveyor I and II Function Type Material Operating Condition :To transfer filtrate from filtrasi to acidification II. : horizontal belt conveyor : Stainless steel : - Temperature (T) = 300 C - Pressure (P) = 1 atm
Conveyor I and II Rate of material Looseness factor Conveyor Capacity Spesifikasi Width of Belt Area Normal Belt Speed Maximum Belt Speed Power 6.67 ton/10 min 52.23 ton/h 54 ton/h 18.00 0.02 76.00 107.00 2.50 inch m2 m/min m/min hp 40.18 ton/h

0.46 m 1.27 1.78 1.86 7.44 2,232.00 m/s m/s kW kWh/day kWh/year

Number of Conveyor

2 pieces

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Preliminary Design of Vanillin Production Plant From Black Liquor

Conveyor III Function Type Material : Transfer of Cake of Filtration to mixer tank. : horizontal conveyor belt : Stainless steel

Operating conditions : Temperature (T) = 300C Pressure (P) = 1 atm

5.5 Bubble Column Reactor Equipment Code Operation Mode Operation Temperature Pressure Volume Retention Time 170 10 C Bar
o

CS-101 Batch

25.52 m3 2 hours Dimension Height 4.48 M Diameter 2.69 M Thickness 6,44 mM Multiple Ring Sparger Diameter 3 mM Number of Holes 15 Material Stainless Steel 316

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.6 Ultrafiltration
Vanillin Solution Ultrafilter Identification: Item Item no. No. required Function: Operation: Material handled: Design data: Vanillin solution ultrafilter UF-101 6

Separate vanillin solution from lignin alkali solution after oxidation Continuous Lignin alkali and other by product Operating temperature (oK) Operating pressure (Psi) Type 353 30 Hollow fiber membrane Polyvinylidenefluoride Material of construction PVDF (for filter membrane) Effective filtration Area (m2) Filtration area with safety factor (m2) Available filter area (m2) Number of fiber in each module L (m) W (m) D (m) Membrane cut-off rating (kDa) Total equipment required (item) 130 10000 2.36 0.34 0.23 1 6

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.7 Spray Dryer

SPRAY DRYER

Identification:

Item Item no. No. required

Spray Dryer SD-101 2 (1 active, 1 stand by)

Function: Operation: Material handled: Composition (%): Vanillin solution Design Data:

Make vanillin powder from vanillin solution Batch Vanillin Solution

100 Type Material of construction Atomizer Volume (m3) Height cylindrical (m) Column Diameter (m) Thickness (m) Volume Cone (m3) Cone Angle (o) Max Temp Operating (oC) Max Press Operating (psi) Power (hp) Closed spray dryer Stainless steel Centrifugal Disc (Vane) 5.52 1.47 2.45 0.0025 4.05 20.57 180 600 116

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Preliminary Design of Vanillin Production Plant From Black Liquor

5.8 Heat Exchanger 5.8.1 Heat Exchanger HE-101

Tipe Jenis Heat transfer area, m2 Heat transfer coefficient, W/m2 0C Agen pemanas Laju alir pemanas, kg/hari Jumlah tube Shell Side Material Densitas, kg/m3 Cp, Temperature in, C Temperature out, C
0 0

Shell and Tube Countercurrent Floating Head 273.50 900 Superheated steam 190oC 32000 218 Tube Side SS304 1060 2.08 60 170

SS 304 0.521 2.09 190 190

5.8.2 Heat Exchanger HE-102

Tipe Jenis Heat transfer area, m
2

Shell and Tube Countercurrent Floating Head 202 900 Superheated steam 190oC 32000 161 Shell Side Tube Side SS304 1.02 1.00 25 120

Heat transfer coefficient, W/m2 0C Agen pemanas Laju alir pemanas, kg/hari Jumlah tube

Material Densitas, kg/m3 Cp, Temperature in, 0C Temperature out, 0C

SS 304 0.521 2.09 190 190

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Preliminary Design of Vanillin Production Plant From Black Liquor

CHAPTER 6 PROCESS CONTROL 6.1 Process Control Instrumentation Process control system is absolutely necessary in a factory to control all

the variables such as temperature, pressure, level, and more so the process runs. Some process control objective to be achieved are as follows: a) Avoiding dangerous circumstances that may occur in the operation (safety) b) Maintaining the quality of the resulting product c) Keeping the equipment is working in a range of operating conditions d) Keeping operations and various byproducts produced run in accordance with environmental standards e) Monitor and diagnose the operation F) Keeping operations running optimally so keep the plant gains At this plant a variety of variables controlled by using a variety of instruments that are available at the P & ID. Here is an explanation of the control system in the main equipment. 6.2 Process Control on Raw Material Storage Tank Black liquor storage tank is connected to the acidification vessel. Yield

products from this vessel will greatly depend on the composition of the input to the output reactor or storage tank. Flow rate control system of storage tanks needed for the flow rate from the storage tank maintained. The control system used to control the flow rate is bypass control system. The process of controlling the flow rate of the tank using orifice meter as a sensor to measure the flow rate output before entering the control valve. Flow rate measurements made of the difference in pressure at P1 and P2. The output of the orifice meter is then analyzed by the controller based on set point. Then the controller controls the flow rate of the control valve (open when the flow rate is too small and close when the flow rate is too large) to adjust the flow rate to set point.

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Preliminary Design of Vanillin Production Plant From Black Liquor

6.3

Process Control on Heat Exchanger Process control in the heat exchanger also has a similar system of controls

for each heat exchanger. Controlled variable is the temperature of the main product output heat exchanger. The parameters are controlled steam flow rate or cooling water into the heat exchanger. Temperature is one of the important variables to be controlled. Heat exchangers are the main components that require temperature control. Heat exchanger serves to exchange heat between the main product with steam / cooling water. Controlling the temperature of the product is required to be maintained in accordance with the main design. The control system used for temperature control are feed back control system. Process control using a thermocouple as a temperature sensor on the output of main products in heat exchangers. The output of the thermocouple is then analyzed by the controller based on set point. Then the controller controls the flow rate of the flow control valve on the pipe steam / cooling water before it enters the heat exchanger. Control valve controlling the flow rate of steam / cooling water to adjust the flow rate of steam / cooling water with a temperature set point to achieve the appropriate design. 6.4 Process Control on Reboiler Process control more towards the boiler temperature control in steam

output. Boiler using diesel fuel to vaporize water into steam. Controlled variable is the temperature of the steam output of the boiler. The parameters were controlled flow rate of diesel fuel and water into the boiler. And also controlling the pressure in boiler so it can result the high steam pressure needed. 6.5 Process Control on Black Liquor Treatment Vessel Process control in black liquor treatment vessel is a control process that

involves more than one variable that needs to be controlled. Variables that are controlled from the oxidation reactor is the flow rate, height, composition, and pressure. Height The height is a variable that must be maintained during the lignin separation from black liquor. The height of the fluid is maintained in order

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Preliminary Design of Vanillin Production Plant From Black Liquor

not higher than the feed inlet and not too low. Sensors are deployed using a floating sensor surface fluid in the vessel. The parameters are controlled liquid flow rate at the outlet. Pressure The pressure in the black liquor treatment vessel is kept equal to or slightly above atmospheric pressure. Excessive pressure can affect the quality of the product and can also be dangerous when the reactor exploded due to excess pressure. To prevent excess pressure of the reactor is equipped with a relief valve to release the pressure in the reactor. Controlled variable is the pressure inside the reactor. When the pressure exceeds the set point, then the relief valve on the reactor will open thereby releasing the pressure in the vessel. Composition The composition is a variable that can affect the production yield of the reactor. The process of composition control over the direction of the control fluid homogeneity in the vessel. Controlled variable is the composition of the sample in the vessel. The parameters are speed controlled agitator. Sensor compositions using gas liquid chromatography (GLC). When the results of the GLC analysis are deviations from the set point, the parameters changed by the addition of agitation speed of stirring. 6.6 Process Control on Acidification Vessel and Lignin Solution Vessel Process control in acidification and liginin solution vessel is a control

process that involves more than one variable that needs to be controlled. Variables that are controlled from the oxidation reactor is the flow rate, height, composition, and pressure. Height The height is a variable that must be maintained during the lignin separation from black liquor. The height of the fluid is maintained in order not higher than the feed inlet and not too low. Sensors are deployed using a floating sensor surface fluid in the vessel. The parameters are controlled liquid flow rate at the outlet.

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Preliminary Design of Vanillin Production Plant From Black Liquor

Pressure The pressure in the acidification vessel is kept equal to or slightly above atmospheric pressure. Excessive pressure can affect the quality of the product and can also be dangerous when the vessel exploded due to excess pressure. To prevent excess pressure of the vessel is equipped with a relief valve to release the pressure in the vessel. Controlled variable is the pressure inside the reactor. When the pressure exceeds the set point, then the relief valve on the reactor will open thereby releasing the pressure in the vessel.

Composition The composition is a variable that can affect the production yield of the reactor. The process of composition control over the direction of the control fluid homogeneity in the reactor. Controlled variable is the composition of the sample in the reactor. The parameters are speed controlled agitator. Sensor compositions using gas liquid chromatography (GLC). When the results of the GLC analysis are deviations from the set point, the parameters changed by the addition of agitation speed of stirring.

6.7

Process Control on Oxidation Reactor Process control in the manufacture of vanillin making oxidation reactor is

a control process that involves more than one variable that needs to be controlled. Variables that are controlled from the oxidation reactor is the input flow rate, height, composition, pressure and temperature. Flow rate The flow rate input is an important variable to be controlled in a reactor. The flow rate input into the reactor can affect the composition in the reactor that will also affect the yield of the reactor. In addition flow rate can also affect the height of the liquid in the reactor. Sensors are used to measure the flow rate is orificemeter. Flow rate is then controlled by the controller input based on set point. Control the flow rate by the flow control valve (FCV).

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Preliminary Design of Vanillin Production Plant From Black Liquor

Height The height is one important variable but often forgotten in BCR tank. Sensor height is needed in order to know whether the height of the fluid is sufficiently safe for the agitator to operate. The parameters that are controlled from the control height is input flow rate into the reactor. Height sensors are used to using sensors floating in the fluid surface. The height of the fluid in the reactor is controlled by the controller based on set point. Control the flow rate by the flow control valve (FCV) on the same input stream as the flow rate control input.

Composition The composition is a variable that can affect the production yield of the reactor. The process of composition control over the direction of the control fluid homogeneity in the reactor. Controlled variable is the composition of the sample in the reactor. The parameter control is speed of gas O2 through component in BCR. Sensor compositions using gas-liquid chromatography (GLC). When the results of the GLC analysis are deviations from the set point, the parameters changed by the addition of flow rate O2 from gas sparger to BCR.

Pressure Pressure is an important variable in the reactor. The pressure in the reactor was kept at pressure of 10 bar above atmospheric pressure, but do not be too excessive. It is intended that the oxidation of lignin into vanillin could happen. Pressure changes can occur due to the continuous input reactor and the reaction in the reactor. Excessive pressure can affect the quality of the product and can also be dangerous when the reactor exploded because excess pressure. To prevent excess pressure of the reactor is equipped with a relief valve to release the pressure in the reactor. Controlled variable is the pressure inside the reactor. When the pressure exceeds the set point, then the relief valve on the reactor will open thereby releasing the pressure in the reactor.

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Preliminary Design of Vanillin Production Plant From Black Liquor

Temperature Temperature is the most variable can change in the reactor. The process of oxidation reaction produces heat which can change the temperature in the reactor. The reaction in the reactor must be on guard at 170 C for the reaction to occur and produce vanillin. To keep the temperature inside the reactor is used jackets. The temperature sensor used is a thermocouple. Controlled variable is the temperature in the reactor.

6.8

Process Control on Spray Dryer Process control in the spray drayer is a control process that involves more

than one variable that needs to be controlled. Variables that are controlled from the spray dryer is the input flow rate, composition, and pressure. Flow rate The flow rate input is an important variable to be controlled in a spray dryer. The flow rate input can affect timing and composition amount. Sensors are used to measure the flow rate is orificemeter. Flow rate is then controlled by the controller input based on set point. Control the flow rate by the flow control valve (FCV). Composition The composition is a variable that can affect the vanillin powder production of spray dryer. The process of composition control is over the direction of the contain of vanillin. Controlled variable is the composition of the sample in the spray dryer. The parameters controlled is rate of evaporation. Sensor compositions using gas-solid chromatography (GSC). When the results of the GSC analysis are deviations from the set point, the parameters changed by the addition of rate of hot air into spray dryer. Pressure Pressure is an important variable in the reactor. The pressure in spray dryer was kept at atmospheric pressure or above atmospheric pressure, but do not be too excessive. Pressure changes can occur due to the continuous input to spray dryer. Excessive pressure can affect the quality of the product and can also be dangerous when the spray dryer exploded because excess pressure. To prevent excess pressure of the spray dryerr is equipped

76

Preliminary Design of Vanillin Production Plant From Black Liquor

with a relief valve to release the pressure in the reactor. Controlled variable is the pressure inside. When the pressure exceeds the set point, then the relief valve will open thereby releasing the pressure in the spray dryer.

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Preliminary Design of Vanillin Production Plant From Black Liquor

S-101 BL Storage

P-102 BL Pump

V-101 BL Solid Treatment Vessel

F-101 CO2 Fan

P-103 Slurry Pump

PF-101 Plate & Frame Filter

FT 106 FIC 106

P-105 Water Pump

Water
P-108

Lean Liquor

FT 101

FIC 101

LT 101 FIC 102 AT 101

AC 101

PT 101

PIC 101

V-19 LT 102 FT 104 FIC 104

Black Liquor
P-101 S-101 P-102

FT 102

P-14

V-101

P-103

PF-101

To V-102

FT 103

FIC 103

CO2

VANILLIN PLANT FROM LIGNIN PIPING AND INSTRUMENTATION DIAGRAM Drawn By : Checked By Revised By : Drawing No : Notes : Group 6 Date : Date : Without Scale A4

Figure 6.1 Piping and Instrumentation Diagram - 1

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Preliminary Design of Vanillin Production Plant From Black Liquor

V-102 Acidification Vessel

P-105 H2SO4 Pump

P-106 H2SO4 Pump

P-107 Lignin Slurry Pump

PF-102 Plate & Frame Filter

P-108 Water Pump

V-103 Lignin Solution Vessel

P-109 Lignin Solution Pump

FT 107

FIC 107

Water
P-106

Alkali sulfat

AC 102 AT 102

PT 102

PIC 102

From PF-101

V-23 LT 103 FT 105 FIC 105

TO V-104
P-4 V-5

V-102
FT 105 FIC 105

P-107

PF-102
AT 103

AC 103

PT 103

PIC 103

FC 109

V-22 LT 104 FT 109

H2SO4
P-109

V-103

P-104

FT 108

FIC 108

NaoH
P-111 Drawn By : Checked By Revised By : Drawing No : Notes : VANILLIN PLANT FROM LIGNIN PIPING AND INSTRUMENTATION DIAGRAM Group 6 Date : Date : Without Scale A4

Figure 6.2 Piping and Instrumentation Diagram - 2

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Preliminary Design of Vanillin Production Plant From Black Liquor

H-101 Heat Exchanger

C-101 O2 and N2 Compressor

CS-101 Oxidation Reactor

F-102 Air Blower

H-102 Heat Exchanger

P-112 Water Pump

H-103 Heat Exchanger

B-101 Steam Reboiler

FT 110a FIC 110a

N2
PT 104 PIC 104 AC 104

AC 104 AT 104

PT 106

PIC 106 P-30

LT 106

FT 110

FIC 110

AT 104 TT 101

LT 105

P-33

From P-109

H-101

P-105 V-104
FT 110 FIC 110

To UF-101
TIC 101

H-102

O2 & N2
FT 114

FIC 104

P-106 CS-101

Steam
FT 114 FIC 114 TIC 103

To SD-101 Air
H-103

F-102
TIC 102 TT 103

PIC 105 FT 115 FIC 115

PT 105

TT 102

O2 & N2
B-101 P-112 Drawn By : Checked By

VANILLIN PLANT FROM LIGNIN PIPING AND INSTRUMENTATION DIAGRAM Group 6 Date : Date : Without Scale Notes : A4

Revised By : Drawing No :

Figure 6.3 Piping and Instrumentation Diagram - 3

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Preliminary Design of Vanillin Production Plant From Black Liquor

UF-101 Membrane Ultrafiltration

P-111 Filtrate Pump

SD-101 Spray Dryer

Others

PT 111

FIC 111

From H-102

FT 112

FIC 112

P-111
TT 104 FIC 113 AC 105

PT 107

PIC 107

FT 113

TIC 103

Air From H-103

AT 105

FT 114

FIC 114

Powder Vanillin

VANILLIN PLANT FROM LIGNIN PIPING AND INSTRUMENTATION DIAGRAM Drawn By : Checked By Revised By : Drawing No : Notes : Group 6 Date : Date : Without Scale A4

Figure 6.4 Piping and Instrumentation Diagram - 4

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Preliminary Design of Vanillin Production Plant From Black Liquor

CHAPTER 7 PLANT LAYOUT AND PIPING DESIGN

Vanillin plant is subsidiary of Riau Andalan Pulp & Paper. The location of our plant is beside RAPP, in Langgam, Pelalawan Regency, Riau. Our Plant Must near with RAPP because black liquor as vanillin plant raw material sourced from RAPP byproduct. RAPP total land area in langgam is 10,100 Ha with the following boundaries area. North : PT Mitra Unggul Pusaka (rubber) East : PT Mitra Unggul Pusaka (rubber)

South : PT Siak Raya Timber West : Rubber plantations

Vanillin Plant

Riau Andalan Pulp & Paper (Sumber Black Liquor)

Figure 7.1. Location of vanillin plant building

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Preliminary Design of Vanillin Production Plant From Black Liquor

Our vanillin plant is divided into several areas. The first area is the main area of the factory, which is the production area adjacent to a black liqour storage tank. Additionally, there are utility area at the back of the factory. For the purposes of administration and personnel, there is a 3-storey office and other facilities such as clinics, mosque, cafeteria, and athletic fields. For the power source, there is an electric generator room adjacent to the living room maintanance tools and fire safety. Vanillin plant construction is based on safety considerations, ease of distribution of raw materials, utilities, land availability, ease of marketing and transportation of goods. Vanillin plant layout and process equipment layout can be seen in the following figure.

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Preliminary Design of Vanillin Production Plant From Black Liquor

155 m
wastewater Storage CHEMICAL ENGINEERING DEPARTMENT ENGINEERING FACULTY UNIVERSITAS INDONESIA

Black Liquor Storage

65 m

INFORMATION Room or Area: - Black Liquor storage tank - Raw material storage - Control Room - Production Process Area - laboratorium - Utility Area - Security Post - Meeting point - Fire Safety - Maintenance Room - Electric Generator Room - Vehicle Parking Area - Main Office
OWNER PROJECT GROUP 6 PLANT DESIGN 2012 Truck Parking Area

Process Production Area

70 m

Utility room

Security post

Raw Material Storage

Laboratorium

Control Room

Product Storage

Truck Parking Area

SKALA 1:5
Fire Station Project MASTER PLANT OF VANILLIN PLANT

30 m

125 m
Main Road
Pedistrian road Parking Area Pedistrian road clinic Mosque

Main Road

Pedistrian road

PICTURE Electric generator room Sport Field DESIGN LAYOUT OF VANILLIN PLANT

50 m
Meeting Point

Pedistrian road

PICTURE NO:
NO. Page

Main Office

canteen

Maintenance room

PL 001/2012

Total Page

Figure 7.2. Design Layout of Vanillin Plant

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Preliminary Design of Vanillin Production Plant From Black Liquor

160 m
65 m

2.9 m 7.16 m 2.5 m

8.7 m 2.36 m

CHEMICAL ENGINEERING DEPARTMENT ENGINEERING FACULTY UNIVERSITAS INDONESIA INFORMATION

2.83 m 4m 15 m 2.5 m 8m

2m 1.5 m

70 m

1.35 m

2.34 m

1m 1.86 m 8.5 m 30 m

Utility room 15 m

4.25 m

3.8 m

Equipment: - Raw material storage tank - Acidification Vessel 1 - Plate & Frame Filtration - Belt Conveyor - Elevator - Acidification Vessel 2 - Solution lignin Vessel - Heat Exchanger - Ultrafiltration - Spray Drying - Wastewater tank - Air tank - Compressor
OWNER PROJECT GROUP 6 PLANT DESIGN 2012

Raw Material Storage

15 m

15.6 m

10 m

Laboratorium

Control Room

10 m

Product Storage

125 m

15 m

15 m

15 m

15 m

15 m

10 m

SKALA 1:5
Project MASTER PLANT OF VANILLIN PLANT

PICTURE DESIGN LAYOUT OF VANILLIN PLANT EQUIPMENT PROCESS

PICTURE NO:
NO. Page

PL 002/2012
Black Liquor Storage Acidification vessel 1 Elevator, acidification vessel 2, plate&frame filtration Vessel, storage, Heat exchanger, reactor, ultrafiltation, spray drying wastewater Storage

Total Page

Plate & Frame filtration

Figure 7.3. Design Layout of Vanillin Plant Equipment Process

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Preliminary Design of Vanillin Production Plant From Black Liquor

CHAPTER 8 HEALTH, SAFETY, AND ENVIRONMENT MANAGEMENT Health, Safety, and Environment Program (HSE) is a standard for industries in Indonesia in order to protect workers' rights. Safety and good health can improve safety and morale for employees or labor in general. A sense of safety and employee morale which is great significance for the improvement of labor productivity is the key to the success of a company or factory. In order to implement the good HSE program, in the factory applied some policies regarding work place safety and health. The purpose of the HSE policy implementation include : 1. Set a target of increasing annual health and safety and make sure everything is fulfilled by conducting regular audits 2. Prevent personal injury and health risks for all people who are in the factory 3. Develop, design, build, set up, operate and maintain the process, plant, equipment, including disposal in accordance with company guidelines and regulations on occupational safety and health, and document process control methods are classified as hazardous 4. Provide and maintain a safe system of work and prepare all necessary plans to tackle any kind of disturbance or damage 5. Ensure that all employees at the location of the company to realize responsibility for occupational safety and health 6. Ensures staff provide guidance on occupational safety, health and environmental issues receive adequate training 7. Involve all employees in the implementation of policies and procedures using advice and training to facilitate the emergence of a sense of involvement and responsibility 8. Ensuring and summarizes all the experience of occupational safety and health hazards that are relevant and disseminate the conclusions for the business as a whole 9. Reviewing periodically and health policy in line with central policy

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Preliminary Design of Vanillin Production Plant From Black Liquor

8. 1

Health Aspects Health factor is one of the main supporters milling operations. With good

health in the factory, all the factors supporting plant performance, especially the employees will be more productive at work. To prevent disruption of the environmental health aspects of plant it is necessary to consider what are the factors that could potentially endanger the health aspects in plant environments. Danger to the health aspects can be avoided by analyzing the potential hazards affecting the environmental health aspects of the plant. 8. 2 Safety Aspects Safety is a very important factor in a factory. Analysis of the factors of

potential harm occurred in this plant needs to be done so that we get the data and considerations necessary for handling. Hazard Analysis is an analysis of the composition of the dangers of a place that has the potential dangers. Identify Adverse events leading to a hazard material Mechanism analysis of opportunities possible unexpected events The estimated magnitude of the dangers that may arise. Hazard analysis can be divided into two, namely: 1. HIRA (Hazard Identification and Risk Assessment) 2. HAZOP (Hazard and Operability Study) 8.2.1 Hazard Identification and Risk Assessment (HIRA) HIRA is the identification of risks to an activity. Hazard Identification and

Risk Assessment (Hazard Identification and Risk Assessment), analysis carried out in daily activities and in the factory. In determining HIRA, there are several steps that must be done. The stages are as follows: Sorting activities to be carried out into smaller sub-activities and specific Identify potential hazards for each sub-activity Determination of the risks that might occur (hazard effects and the possibilities) Determining how to prevent and control the risk of harm Conclusion potential hazards and risks involved for each activity Conclusion to overall job Risk = Hazard x Exchange Rate Possible Dangers
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Preliminary Design of Vanillin Production Plant From Black Liquor

o Harmful effects are still composed of HIGH, MEDIUM and LOW o The possible dangers consist of HIGH, MEDIUM and LOW

Table 8.1 Parameter in Counting Dangers Possibilities

PARAMETER

HIGH Each time the work was done Almost every time the work is done Without experience, never done before work

MEDIUM Once in 10-100

LOW

Frequency of harm Frequency of adverse danger

One time during the job done Once in 100 or more

Once in 10-100

Ability level executive jobs

Less experienced

Experienced, have good ability and often do the work

Table 8.2 Parameter in Counting Danger Effects

PARAMETER

HIGH Death, disability, body dysfunction, severe injuries

MEDIUM Medium wounds, the body can still work

LOW

Human Resources

minor injuries

Asset

Damage to the equipment, production halted

The damage causes decreased production levels

Little damage, does not affect the production of protection tool Tools available with sufficient protection, installation of insulated More than 30 minutes

Protection Tool

No protective devices are in an environment with the presence of a flammable substance Less than 1 minute

Minimal protection device

Evacuation time availability

Between 1-30 minutes

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Preliminary Design of Vanillin Production Plant From Black Liquor

Table 8.5 Hazard Identification and Risk Assessment (HIRA)

Types of Activities Potential Danger Danger Possible Rate Risks Rate Effects Pre-Operational Stage Final Risks

Dangers

Prevention and Management

Falling from Height

Permanent Injuries Death

Work on construction activities in accordance with SOP and using PPE safety belt Work on construction activities in accordance with SOP and using PPE safety helmet Work on construction activities in accordance with SOP and using PPE safety shoes

Plant Building

Objects falling from height

Moderate to severe injuries

Tripped up by construction equipment scattered Falling or pinched tool Installation Tool Hit or tripped work equipment

Mild to moderate injuries Death and organ dysfunction Nonpermanent injuries

Using PPE and safety belt

Checking the condition of the tool to be used to start a job

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Preliminary Design of Vanillin Production Plant From Black Liquor

Electric shock Electrical installation

Death, permanent injury Death and organ dysfunction

Using rubber boots, gloves and other tools that are insulators

Fall at the time of installation of the high

Using PPE and safety belt

Plant Operation Stage

Exposure to chemicals
Charging of raw materials in tanks

Irritation and minor injuries

Wearing PPE such as gloves and masks when filling the tank of raw materials Wearing PPE such as gloves and masks when filling the tank of raw materials

Slip away due to chemicals

Permanent injuries and death

The operation of the process

Electric shock at the pump

Permanent injuries and death

Perform regular checks and maintenance of the pump according to SOP

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Preliminary Design of Vanillin Production Plant From Black Liquor

Exposure to heat flow and heat exchange equipment boiler Exposure to chemicals in a leaky pipe

Injuries caused by the heat of the skin Irritation and injury by heat on the skin. Nonpermanent minor injuries Irritation and minor injuries

Workers doing the work in accordance with SOP

Perform regular checks on the piping system and start planning a better pipeline Workers work carefully and in accordance with SOP Carry out work in accordance with the SOP and training employees periodically

Bumped by pipelines & reactors

Exposure to chemicals directly Storage of raw materials / product

Contamination in the end product storage

Decline in value and product quality

Implementation and maintenance work as per SOP tank periodically

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Preliminary Design of Vanillin Production Plant From Black Liquor

Factory Maintenance Stages

Stumble and fall

Nonpermanent injuries to permanent Nonpermanent injuries to permanent Irritation and minor injuries

Maintenance jobs done mentati applicable SOPs

Pinched or scratched appliance Exposure to chemicals

Using PPE and safety belt Obey SOP jobs Maintenance jobs done mentati applicable SOPs

Maintenance Process

Electric shock on job-related electrical installation

Permanent injuries to farm

Perform maintenance and replacement electrical equipment periodically and perform maintenance work on a regular basis

Treatment Plant Facilities

Falling from a height

Permanent injuries to death

Perform maintenance work in accordance with the procedures and PPE safety belt

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Preliminary Design of Vanillin Production Plant From Black Liquor

Electric shock

Permanent injuries to death

Perform maintenance and replacement electrical equipment periodically and perform maintenance work on a regular basis

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Preliminary Design of Vanillin Production Plant From Black Liquor

8.2.3 Hazard Operability Study (HAZOP) of Vanillin Plant Operation Unit Equipment Code

Parameter

Deviation

Causes Blocking of raw material supplies and not suitable with the equipment capacity Raw material capacity more than machine capacity

Effects

Prevention

Control

Less S-101 S-102 S-103 S-104 S-105 V-101 V-102 V-103

Vessel doesn't work efficiently

Ensure that raw material capacity must suitable with equipment capacity Installing controller such as valve at the input of reactor to adjust raw material capacity which entering the equipments Flow control (FC)

Flow rate

Vessel

More

Vessel will be damaged easily

Less Agitator Velocity More P-101 P-102 P-103 P-104 P-105

Power resources is low Agitator velocity isn't appropriate

Reaction doesn't work Giving extra power such perfectly and as electrical power too long Making bubble Determine agitator in the agitating velocity value (rpm); process Controlling regularly Pump heat and damaged easily

Flow control (FC)

Pump

Flow rate

No

Blocking in pump

Pump cleaning and controlling regularly

Flow control (FC)

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Preliminary Design of Vanillin Production Plant From Black Liquor

P-106 P-107 P-108 P-109 P-110 P-111

Less

Blocking or leaking in pump Overload stirring performance Blocking or leaking in HE Input flow rate increase Steam supply will decrease

Low supply Pump damaged easily Supply will be clogged HE will be damaged easily Temperature process will increase too long Encrement of temperature will be excessed Temperature process will increase too long Encrement of temperature will be excess Supply will be

Pump cleaning and controlling regularly, installing valve and flow indicator Controlling regularly

More

Less Flow rate More H-101 Less Heat Exchanger Temperature More

Controlling regularly Controlling regularly and installing valve in HE input Increasing steam to HE Temperature control (TC) Decreasing steam to HE Flow control (FC)

Steam supply will increase

Less H-102 Temperature More HE-103 Flow rate Less

Steam supply will decrease Steam supply will increase Blocking or

Increasing steam to HE Temperature control (TC) Decreasing steam to HE Controlling regularly Flow
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Preliminary Design of Vanillin Production Plant From Black Liquor

leaking in HE More Input flow rate increase Chilling water supply increase

Temperature

Less

clogged HE will be damaged easily The temperature reduction will be excess Temperature reduction process will too long Heating will be blocked Damaged equipment Reactor doesn't work efficiently

control (FC) Controlling regularly and installing valve in HE input Decreasing water supply to HE Temperature control (TC) Increasing water supply to HE Lean liquor flow rate setting Installing pressure valve

More

Chilling water supply is less Blocking or leaking in Boiler The result of combustion increase Raw material input is blocked and unsuitable with equipment capacity Raw material capacity more than machine capacity

Less Boiler B-101 Flow rate More

Flow control (FC)

Less Bubble column reactor

Ensure that raw material capacity must suitable with equipment capacity Installing controller such as valve at the input of reactor to adjust raw material capacity which entering the equipments Flow control (FC)

CS-101

Flow rate More reactor damaged easily and liquid spilled

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Preliminary Design of Vanillin Production Plant From Black Liquor

Less Blower F-101 Flow rate More

Low power supply Overload stirring performance Blocking or leaking in pump Overload stirring performance in pump

Acidification process doesn't Giving extra power such work as electrical power effectively Blower/fan damaged Controlling regularly easily Supply will be decreased Filtration process will take time too long Materials which will be streamed from one place to another would pile on operations Supply products are expected to be the product will be too big Controlling pump and flow regularly; Installing flow rate controller Controlling pump and flow regularly; Installing flow rate controller

Flow control (FC)

Less Plate and Frame Filtration PF-101 PF-102 Flow rate More

Flow rate Control

Less Conveyor CON-101 CON-102 CON-103 CON-104 Belt Speed

Low driving force

Provide additional power in the form of electric power

Flow Control (FC)

More

Incorrectness set point

Determining the value of a new set point and controlled on a regular basis

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Preliminary Design of Vanillin Production Plant From Black Liquor

Less Temperature of the Hot air More Spray Drying SD-101 Less Flow rate input

Hot air temperature which use to atomized is too small Hot air temperature which use to atomized is too big Input flow rate is too small Input flow rate is too large Blocking of material supplies and not suitable with the equipment capacity Raw material capacity more than machine capacity

vanillin still contain a water Vanillin may participate evaporate Decreases debit fluid Flooding, crystalization cannot maximum running Ultrafiltration doesn't work efficiently

Increase temperature of hot air Temperature Control (TC) Decrease flow rate and temperature steam Increasing the flow rate input Reducing the flow rate input Flow rate Control (LC)

More

Less

Ensure that material capacity must suitable with equipment capacity Installing controller such as valve at the input of ultrafiltration to adjust raw material capacity which entering the equipments Flow control (FC)

Ultrafiltration

UF-101

Flow rate

More

Ultrafiltration will be damaged easily

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Vanillin Production from Lignin

8. 3. Environmental Aspects An industrial process can have a negative impact on the environment if not handled

properly. The negative impact on the environment can affect the sustainability of production and the local environment. In this section, we discuss some of the environmental impacts that may result from the presence of the vanillin plant is that the manufacturing process produces substances called residual waste. Based on his form, the waste produced by the plant can be grouped into four types, namely: 8. 3. 1. Liquid Waste Wastewater produced by this plant are lean liquor that will be recycled by PT Riau Andalan Pulp and Paper and water which is reused for chilling water in heat exchanger. 8. 3. 2. Solid Waste No solid waste is removed from the production process of this vanillin plant. 8. 3. 3. Waste Gas Majority of the waste gas produced is CO2 emissions resulting from the generator. 8. 3. 4. Waste Sound (Noise) Possible noise pollution generated by tools such as pumps and motors drive stirrer. Noise can also be caused due to the damage to the mechanical system on the appliance. To reduce the noise level equipment necessary regular maintenance schedule has been determined. For workers who are diarea that generate noise should be equipped with ear protection (ear plugs). Meanwhile, for tools that can generate noise can be added by means of dampening noise. Noise standards set by the minister of health is 60-70 dB, while the minister of labor is a maximum of 85 dB for 8 hours. Expected kenisingan of indigo dye plant is not too large because the pump used is not too large, as well as other tools. 8. 4. Risk Management Risk Management aims to solve the problem even prevent accidents. A particular

effort is needed to reduce or eliminate potential risks. Risk is a condition where there is the possibility of an accident or occupational disease because of the presence of a hazard. The danger is of a material nature, administration of a tool, how to do a job or work

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environment that can lead to property damage, occupational disease, or the loss of human lives. To avoid the danger of necessary control components with potential risks such as human factors, equipment and materials, as well as the methods and sources of danger. Risk management system is a management process carried out with the intention of minimizing the risk or the extent possible to avoid the risk altogether. In a risk management system, which required the application of the hierarchy of control measures against the risk of a hazard, with the following steps: Elimination (eliminate the hazard) Substitution (use raw materials more secure) Engineering (redesign existing processes to make it more secure) Administrative control (changing methods or procedures work in a more secure) Personal protective equipment (using the appropriate protective equipment to isolate the body from harm) To meet risk management will require tools and backup facilities to prevent or overcome danger danger that occurs in plants. The tools and means necessary including body protective gear for employees, fire extinguishers, MSDS (Material Safety Data Sheet), and Account Head Point (local assembled) for all employees if fire occurs. 8.4.1. Personal Protection Equipment Equipment protection for employees is the main standard for a company to protect its employees from the threat of disruption to the aspects of safety and health at work. Based on the major needs in the field of personal protective equipment can be divided into:

a. General Personal protective equipment as a minimum requirement to enter the plant, ie safety helmet, googles, and safety shoes.

b. Special

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PPE is used in accordance with the needs of employees in the workplace each based on hazard and risk. For example: safety goggles, respirators, ear protection, gloves, earplugs, etc. Here are some of the personal protective equipment used in the factory: a. Protective equipment fall Fall protective equipment used in the petrochemical industry is the seat belt / safety belt is one of safety for the protection of workers in performing work activities in high places where workers are likely to fall. Things that need to be considered for fall protection equipment, namely: Safety belt used to be in high places over 4 ft, the rope should be tied firmly on building / sustaining a capable Defence weight Ensure seat belt component in a condition to be good To keep the belt remains in good condition, the equipment belt should be cleaned with hot water and soap, and stored away from the sun and ultaviolet very strong, also the chemical that causes the fibers to become brittle and weak belt Type of fall protection equipment consists of: Belts or harnesses are equipped components stitching, buckles, D-rings, cuts and abration The rope is made up of components rot, proper hook and knots, frayed strands or broker.

b. Respiratory protection The usefulness of this protection tool, especially in an emergency, eg labor should help others who suffer accidents / when must escape a sudden atmospheric air composition changes such that endanger his soul / when should perform repairs equipment in where very high levels of contaminants. Respirator or air purifying respirator which serves to clean the air that has been contaminated in the form of dust, gases, metal vapors, smoke and fog, and protect the work force has been a breath of danger, composed of chem respirator (steam and gas

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contaminants), mech filter respirators (dust, mist, vapor metallic, sour) and cartridge / canister respirator (mixed gas / vapor with solid particles equipped with a filter). Breathing apparatus (air supply respirator), which supplies clean air or oxygen to the wearer. Respirator is not equipped with a filter or cartridge, but supplies the user with compressed air / air cleaner / from an oxygen tank.

Figure 8.1. Respirator

c. Hand protection tool To protect from possible dangers that occur, it is expected that workers in work activities always wore gloves, which must be adjusted to the working conditions and in the absence of injured / contamination of the hands. Various kinds of gloves according to the types of hazards that must be prevented: Asbestos gloves, leather, PVC should be used when heat is caused by the heat generated in the factory work, eg welding gloves to be used must pass through the wrist Rubber gloves, made of synthetic material, vinyl as well as natural, to protect hands from chemicals caustic acids, alkalis and various types of other solvents Gloves canvas / leather, wear gloves of canvas or heavy cotton is typically used when the main danger is very high heat caused by friction Gloves with chrome leather or PVC material with special design, to reduce the hazard when in contact with sharp objects

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Figure 8.2. Gloves

d. The tool foot protector Safety shoes should protect workers against accidents caused by heavy items falling to the feet, protruding nails, liquid metal, and so on. The types of tools used: Protective Footwear, used in good condition should provide some protection against the impact of falling objects or punctures caused by sharp objects to be secure, end-coated steel in a protective layer of skin shoes worn feet will not slip or high heels at least 3 / 8 inch, 1-1/2 inch maximum.

Figure 8.3. Safety Shoes

e. Eye protection Use eye protection of workers flake delicate objects and spray chemicals that can enter and cause irritation to the eyes or even injure the eyes. This tool can also protect your

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eyes from impact workers against a hard object. For eye protection, personal protective equipment supplied googles or safety glasses for workers.

Figure 8.4. Goggles

f. Ear protective devices Ear protective devices commonly used in the area located the tools that may cause loud noises such as compressors, pumps, steam generators, conveyors and other tools that use motors for propulsion. For protection against ear every employee who deals with the tools required to use earplug process provided by the company.

Figure 8.5. Earplugs

g. Protective equipment head The tool used in the form of head protection safety helmet. This headwear is a protective device that is used to protect the head from impact by hard objects while working in the field.

h. The tool body armor

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Personal protective equipment such as protective clothing body safe. Clothing was named coverall which serves to avoid the possibility of a leak or spill liquid products in bulk, so it can protect the body and to avoid direct contact with the skin of workers. To clean up the spill using absorbent material must be non-combustible inorganic. In addition, protective clothing or clothing that workers should not be used that has a crease on the bottom of his pants. 8.4.2. Fire extinguisher Determining the type of fire extinguishers are provided to extinguish the fire and fire prevention and control efforts tailored to the classification of fire, state buildings and items that exist in the building. Classification of types of fires, as follows: Types of fire extinguishers, among others: a. Water type fire extinguishers, consists of two types: Soda Acid Water CO2 Fire extinguisher soda acid type is not used anymore because it is dangerous to humans. Water type fire extinguisher was used to extinguish the fire Class-A and has the following specifications: Red tube. Distance sprays to tubes 9 liters (12-15 kg) is 6 meters. When usage is 1-2 minutes depending on the size of the tube

b. Fire extinguisher types of dry dust, consisting of three types: BC-class Dry Dust Fire Class - B and C Class ABC dry dust Fire Class - A, B and C Dry Dust class D Fire Class - D fire extinguishers dry dust types have the following specifications: a. Light blue tube b. Consists of chemicals such as:

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o Sodium Bicarbonate (97%) o Magnesium Stearate (1.5%) o Magnesium Karbinat (1%) o Tricalcium phosphate (0.5%) c. Tube size 1-12 kg d. Distance 9 liters spray tube is 4-6 meters e. Long time usage depending on size, to the size of 14-16 kg is 15 seconds c. Types of fire extinguishers carbon dioxide (CO2) Extinguisher was used to extinguish the fire Class-B and C and has the following specifications: o black tube o distance 4.5-8 kg spray tube is 2 meters o spending time is 14 seconds o gas CO2 in liquid tube. o the level of development is 450:1

d. The type of fire extinguisher foam (foam), consists of three types: o Scum Chemistry o Self-Aspirating o Non-Aspirating AFFF The type of fire extinguisher foam or foam used to extinguish the fire classes A and B. Specifications of this type extinguishers are: o Creamy white colored tube o Distance sprays to tubes 9 liters (14-16kg) is 4-5 meters o The duration is 30 seconds spending o The level of development is 1:8

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8.4.3. MSDS (Material Safety Data Sheet) MSDS are data from material or plant material in the interests of health and safety. Any material or chemicals present in the plant must have a MSDS which serves as the basis for the use of (material handling). MSDS data serves to communicate and inform everyone working with these materials so that they can use the material properly and act appropriately if there is immediate danger. MSDS of some materials of this plant will be showed in appendix. 8.5. Quality Control in Vanillin Plant All the food people eat must be absolutely pure and clean. This is one of the most important principles of the food industry. One decisive criterion here is that products leave factory without any metal contaminations and other contaminants. Product manufacturers and service industries have realized that competition in a global market require a continual and committed effort towards the improvement of product and service quality. Quality control process consists of raw materials, process, product and service. Major factors in process that cause variability in quality of finished product are people, equipment and methods or technologies employed in the process. Use of proper statistical process control methods is vital for assurance of the product quality. Statistical quality control comprises the following procedure: Finished product is measured Value of quality characteristics is used to provide feedback on how process can be improved Sampling occurs for days or weeks Lot is either accepted or rejected based on information from sample This procedure provided slow feedback of information. Recognizing the importance of quality control of food products, Government of Indonesia has legalized the Act No. 7 of 1996 on food and our plant use it as regulation of quality control. The Food Act is intended as a legal basis for the regulations, development, and control on the production activities or process, the circulation, and trade of food. This Act also provides a reference for various legislative regulations related to food, both already in existence and to be established.

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CHAPTER 9 ECONOMIC ANALYSIS
This chapter gives the economic analysis of vanillin plant from lignin. The steps to analyze the plant economic is explained below.

9.1 Plant Cost Estimation

For total Capital Investment estimation of vanillin plant, we use Guthrie method with the following formula.

CTCI CTPI CWC CTBM Csite Cbuildings Coffsite facilities Ccontingency Ccontractor fee CWC
1. Total Bare Modul Cost (CTBM) Total bare module cost can be calculated using the costs of bare module (CBM) from each equipment manufacturer. Cost of bare module (CBM) for each equipment can be seen in table 9.1 while total bare module cost (CTBM) can be seen in table 6.2.

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Table 9.1. Recapitulation CBM value for each equipment Unit Year Cost Index Cost $ Amount Basis Year Basis 1 8,565.84 2007 525.4 2 1 1 1 1 1 2 1 1 1 3 5 1 1 1 1 1 1 2 4 1 1 1 1 2 1 1 1 8,401.91 8,485.19 7,836.77 8,168.08 7,076.06 6,955.41 7,092.47 7,005.95 7,234.38 7,814.68 2,646.54 885.85 586.39 1,892.34 996.13 93,131.21 21,853.70 10,708.90 112,472.97 215,362.25 56,454.18 21,700.00 21,700.00 19,000.00 70,834.40 32,269.54 17,032.24 49,066.96 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2004 2004 2004 2004 2004 2004 2004 2004 2004 2004 2004 2007 2007 2007 2000 2000 2000 2004 525.4 525.4 525.4 525.4 525.4 525.4 525.4 525.4 525.4 525.4 444.2 444.2 444.2 444.2 444.2 444.2 444.2 444.2 444.2 444.2 444.2 525.4 525.4 525.4 394.0 394.0 394.0 444.2

Code

Equipment

P-101 BLACK LIQUOR PUMP BLACK LIQUOR ACIDIFICATION P-102 PUMP P-103 LIGNIN ACIDIFICATION PUMP P-104 LIGNIN SOLUTION PUMP P-105 LIGNIN SOLUTION PUMP P-106 VANILLIN SOLUTION PUMP P-107 VANILLIN SLURRY PUMP P-108 WATER PUMP P-109 H2SO4 PUMP P-110 WATER PUMP P-111 NAOH PUMP S-101 BLACK LIQUOR STORAGE V-101 ACIDIFICATION VESSEL V-102 ACIDIFICATION VESSEL 2 (A) V-102 ACIDIFICATION VESSEL 2 (B) V-103 BLENDING VESSEL S-102 LIGNIN SLURRY STORAGE S-103 H2SO4 STORAGE S-104 NaOH STORAGE S-105 WASTE STORAGE PF-101 PLATE AND FRAME FILTRATION PF-102 PLATE AND FRAME FILTRATION E-101 HE E-102 HE E-103 HE UF-101 ULTRAFILTRATION SD-101 SPRAY DRYING B-101 BOILER CS-101 BUBBLE COLUMN REACTOR

Cost Index in 2013 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 587.88 615.40 615.40 615.40 615.40 615.40 615.40 587.88

Cost in 2013 ($) 9,584.48 18,802.11 9,494.24 8,768.70 9,139.42 7,917.54 7,782.54 15,871.81 7,839.09 8,094.69 8,743.99 10,507.74 5,861.90 776.06 2,504.44 1,318.34 123,255.24 28,922.45 14,172.78 297,706.49 1,140,091.49 74,714.73 25,417.17 25,417.17 22,254.66 221,276.60 50,402.72 26,603.14 64,938.06

Source sinnot,2009 sinnot,2009 sinnot,2009 sinnot,2009 sinnot,2009 sinnot,2009 sinnot,2009 sinnot,2009 sinnot,2009 sinnot,2009 sinnot,2009 sinnot,2004 sinnot,2004 sinnot,2004 sinnot,2009 sinnot,2012 sinnot,2009 sinnot,2012 matche,2007 sinnot,2004 sinnot,2004 sinnot,2004 Seider, 2003 Seider, 2003 Seider,2003 Seider, 2003 Seider, 2003 Seider, 2003 sinnot, 2004

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Table 9.2. Recapitulation CTBM value
Code Equipment FOB/unit ammount ($) 9,584.48 18,802.11 9,494.24 8,768.70 9,139.42 7,917.54 7,782.54 15,871.81 7,839.09 8,094.69 8,743.99 10,507.74 5,861.90 776.06 2,504.44 1,318.34 123,255.24 28,922.45 14,172.78 297,706.49 1,140,091.49 Total Module Factor 3.47 3.47 3.47 3.47 3.47 3.47 3.47 3.47 3.47 3.47 3.47 1.41 4.2 1.5 1.47 4.2 1.47 4.2 3.37 1.5 3.47 3.37 Bare Modul Cost ($) 33,258.15 65,243.33 32,945.02 30,427.41 31,713.78 27,473.87 27,005.41 55,075.17 27,201.64 28,088.57 30,341.66 14,815.92 24,619.97 1,164.08 3,681.52 5,537.01 181,185.20 121,474.31 47,762.27 446,559.73 3,956,117.46

P-101 P-102 P-103 P-104 P-105 P-106 P-107 P-108 P-109 P-110 P-111 S-101 V-101 V-102 V-102 V-103 S-102 S-103 S-104 S-105 PF-101 PF-102

BLACK LIQUOR PUMP BLACK LIQUOR ACIDIFICATION PUMP LIGNIN ACIDIFICATION PUMP LIGNIN SOLUTION PUMP LIGNIN SOLUTION PUMP VANILLIN SOLUTION PUMP VANILLIN SLURRY PUMP WATER PUMP H2SO4 PUMP WATER PUMP NAOH PUMP BLACK LIQUOR STORAGE ACIDIFICATION VESSEL ACIDIFICATION VESSEL 2 (A) ACIDIFICATION VESSEL 2 (B) BLENDING VESSEL LIGNIN SLURRY STORAGE H2SO4 STORAGE NaOH STORAGE WASTE STORAGE PLATE AND FRAME FILTRATION PLATE AND FRAME FILTRATION

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74,714.73 E-101 E-102 E-103 UF-101 SD-101 B-101 CS-101 HE HE HE ULTRAFILTRATION SPRAY DRYING BOILER BUBBLE COLUMN REACTOR Total Bare Modul Cost ($) 25,417.17 25,417.17 22,254.66 221,276.60 50,402.72 26,603.14 64,938.06 1.5 2.06 3.37 2.7 2.7 2.24 1.41 251,788.64 38,125.75 52,359.37 74,998.21 597,446.81 136,087.36 59,591.04 91,562.66 6,493,651.30

Csite cost calculation ( )

Cbuilding cost calculation ( )

Coffsite facilities cost calculation ( )

Ccontingency cost calculation

Ccontractor fee cost calculation

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CWC cost calculation

( )

Therefore total capital investment of vanillin plant can be found with following equation.

( )

( )

Table 9.3. Total Cost Investment

Component Total Bare Modul Cost (C TBM) ($) Site Development Cost (C site) ($) Building Cost (C building) ($) Offsite Facilities Cost (C offsite facilities) ($) Contingency ($) Contractor fee ($) Working Capital (C WC) ($) Total Cost Investment ($) Value in $ 6,493,651.30 1,298,730.26 1,298,730.26 15,000.00 974,047.70 194,809.54 2,182,403.43 14,306,866.92

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9.2 Annual Operating Costs Annual operating costs are divided into two types; fixed and variable cost, this cost

will be issued during the plant operating. Some of the assumptions used for calculate the operating costs are as follows: 1. Plant operating life is 20 years. 2. In 1 year, this plant operated for 300 days, 24 hours. 3. The production capacity is 100% since the plant operated. 4. Depreciation is 9%, inflation is 4%, and interest rate is 10% per year. Operating costs are calculated by performing the following details: 9.2.1 Raw Material Costs Raw material used in this plant consists of: 1. Black Liquor Costs Black liquor is result of the paper mill waste. Black liquor obtained from Riau Andalan Pulp and Paper mill without charge. It because PT. Riau Andalan Pulp and Paper is owner of this plant. Needs for a year Raw material cost Raw material cost per year : 200,100 tons/year : $ 0 /tons : 200,100 tons/year X $ 0 /tons = $ 0 /year 2. Carbon Dioxide Needs for a year Raw material cost Raw material cost per year : 1,500.30 m3/ year : $ 2.04 /m3 : 1,500.30 m3/ year X $ 2.04 /m3 = $ 3,055.53 /year 3. Sulfuric Acid Needs for a year Raw material cost Raw material cost per year : 2,362.50 tons/ year : $ 412.83 /tons : 2,362.50 tons/ year X $ 412.83 /tons = $ 975,315.48 /year 4. Sodium Hydroxide

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Needs for a year Raw material cost Raw material cost per year : 450 tons/ year : $ 1,767.78 /tons : 450 tons/ year X $ 1,767.78 /tons = $ 795,500.61 /year 5. Water Needs for a year Raw material cost Raw material cost per year : 333,166.50 tons/ year : $ 0.13 /tons : 333,166.50 tons/ year X $ 0.13 /tons = $ 44,604.48 /year 6. Air (O2 and N2) Needs for a year Raw material cost Raw material cost per year : 612 m3/ year : $ 3.16 /m3 : 612 m3/ year X $ 3.16 /m3 = $ 1,935.21 /year

Thus, the total direct material cost is $ 1,820,411.31 per year.

Table 9.4. Raw Material Cost per Year

Materials Amount Unit/batch Needs per year 333,166.50 1,500.30 45,022.50 450.00 612.00 Cost in 2012 ($) 0.12 1.90 385.14 1,649.20 2.95 Cost in 2015 ($) 0.13 2.04 412.83 1,767.78 3.16 Raw Material Cost Per Year ($) 44,604.48 3,055.53 975,315.48 795,500.61 1,935.21 1,820,411.31

Water CO2 H2SO4 NaOH

Air (O2 and N2)

370.19 1.67
50.03 0.50 0.68

ton m3 ton ton m3

Total Raw Material Cost Per Year

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9.2.2 Operating Labor Costs Table 9.5. Indirect Labor costs Cost per month ($) Cost per year ($) 60000 42000 24000 18000 10800 18000 10800 18000 10800 24000 18000 10800 18000 10800 18000 10800 36000 21600 21600 21600 21600 14400 Total cost per year ($) 60000 42000 24000 18000 21600 18000 21600 18000 21600 24000 18000 21600 18000 21600 18000 21600 36000 21600 21600 21600 21600 43200 553,200.00 110,640.00 663,840.00

Qualification Commissioner President Director

Amount

1 5000 1 3500 FINANCIAL Financial Director 1 2000 Marketing Department Manager 1 1500 Marketing Department Staff 2 900 Financial Department Manager 1 1500 Financial Department Staff 2 900 Budgetary Department Manager 1 1500 Budgetary Department Staff 2 900 HUMAN RESOURCES Human Resources Director 1 2000 Public Relation Manager 1 1500 Public Relation Staff 2 900 Personnel Manager 1 1500 Personnel Staff 2 900 Education & Training Manager 1 1500 Education & Training Staff 2 900 OPERATIONAL Operational Director 1 3000 Engineering Manager 1 1800 Processing Manager 1 1800 HSE Manager 1 1800 Research & Development Manager 1 1800 Research & Development Staff 3 1200 Fixed Cost of Indirect Labour Variable Cost of Indirect Labour = 20% TIL Total Indirect Labour

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Table 9.6. Direct Labor costs Cost per month ($) Cost per year ($) Total cost per year ($) 900,000.00 43200 43200 43200 43200 172,800.00 34,560.00 207,360.00 871,200.00

Qualification Supervisor Engineering Staff Processing Staff HSE Staff R&D Staff

Amount

2 1500 450,000.00 3 1200 14400 3 1200 14400 3 1200 14400 3 1200 14400 Fixed Cost of Direct Labour Variable Cost of Direct Labour = 20% TDL Total Direct Labour Total Operating Labour (OL)

9.2.3 Utilities Costs The table below explain the detail of the utilities cost needed per year.

Table 9.7. Total Utilities Cost per Year Utilities Electricity Domestic Water Fuel for Steam Amount Unit Needs per year 126129.44 3000.00 568161 Cost in 2012 ($) 0.08 0.12 1.10 Cost in 2015 ($) 0.09 0.13 1.18 Utilities Cost Per Year ($) 54432.38 401.64 669913.58 681131.08

126129.44 kwh/year 10.00 m3/day 210.43 L/batch

Total Utilities Cost Per Year

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9.2.4 Total Direct Costs Table 9.8. Total Direct Costs per Year Total Raw Material Costs Total Operating Labour (OL) Total Utilities Cost Maintanance Cost (10% Fc) Direct Supervisory (20% Operating Labour) Operating Supplies (1%Fc) Laboratory Charges TOTAL DIRECT COST
$ 1820411.31

$ 871200.00 $ 681131.08 $ 1212446.35 $ 174240.00 $ 121244.63 $ 87120.00 $ 4967793.37

9.2.5 Total Fixed Costs Table 9.9. Total Fixed Cost Fixed Cost Local Taxes Insurance Total Fixed Cost 9.2.6 Plant Overhead ( ) ( ) 3% Fc 1% Fc $ 363733.90 $ 121244.63 $ 484978.54

9.2.7 Total Manufacturing Cost Table 9.10. Total Manufacturing Cost Total direct cost $ 4967793.37

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Total Fixed Cost Plant Overhead Total Manufacturing Cost $ 484978.54 $ $ 6281542.17

9.2.8 Expenses Cost

Here, we can know value of TOC, with the estimating that total manufacturing cost is 85% Total Operating cost. So, the value of TOC is :

We can get the expenses cost.

The details of expenses cost is in table 6.11 Table 9.11. Total Expenses Cost EXPENSES COST EXPENSES COST = 15% TOC Administrative Cost = 15% OL Financial Interest = 5% Fc Distribution&Selling + R&D = EC (AC+FI) $ $ 130680.00 $ 606223.17 $ 371604.27

9.2.9 Total Operating Cost

So, total operating cost of this plant is

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9.3 Equity The total investment from this vanillin plant is $ 14306866.92 (according to the

preliminary equation). The initial capital came from the plant 60% equity and 40% of the bank loan.

Table 9.12. Source investment Source investment Self investment Bank Loan % 60% 40% value 8584120.15 5722746.77 Interest / year 5% 10%

Table 9.13. Bank Source Equity

Year 2014 2015 2016 2017 2018 2019 2020 Bank Loan 5722747 6295021 6924524 5539619 4154714 2769809 1384905 Interest 0 629502 692452 553962 415471 276981 138490 End Year Payment 0 0 2077357 1938867 1800376 1661886 1523395 Loan remaining 0 6924524 5539619 4154714 2769809 1384905 0

Table 9.14. Self Investment Source Equity

Year 2014 2015 2016 2017 2018 2019 2020 Investment Loan 8584120 9442532 9914659 7931727 5948795 3965864 1982932 Interest 0 472127 495733 396586 297440 198293 99147 End Year Payment 0 0 2478665 2379518 2280372 2181225 2082078 Loan Remaining 0 9914659 7931727 5948795 3965864 1982932 0

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9.4 Investment feasibility Analysis To determine a project feasible or not to do, it is necessary a feasibility analysis of

investment. Investment is called feasible if it gives more profit than the expected. Expected minimum profit are commonly known as the MARR, while profits are calculated on the investment feasibility analysis are known as the IRR. Some of the usual investment parameters analyzed are given below.

9.5.1 Cash Flow Cash flow can indicate fluctuations in income earned over the life of the plant through net income. The calculation is by subtracting the cash inflow with cash flow out. Calculations of cash inflow involving revenue after taxes cutting, depreciation, rest value of equipment called the after-tax cash flow (ATCF). Meanwhile, out cash flow can be an investment, cost, and loans. Calculations before and after tax cash flow is shown in Table 9.15 and is represented in the cash flow diagram in Figure 9.1

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After Tax Cash Flow

10000000.00

5000000.00

0.00 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22

-5000000.00

-10000000.00

-15000000.00 ATCF Total ATCF Bank ATCF Investor

Figure 9.1. Cash flow diagram

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Table 9.15 shows the calculation of cash flow that calculated from the initial construction plant. In early 2013, the construction of the plant is beganwhich an investment is for the purchase of the entire instrument. Figure 6.1 shows that the largest investment incurred in the first year. In 2013, the construction is still going on until the middle of 2014, so it is still a cash flow investment. In 2015, our factory started operation. 9.5.2 IRR To find out how IRR can be obtained from the cash flow in table 6.12 above, it can be calculated that the number of trial IRR values PW = 0,

Table 9.16 IRR Calculation

NPV PV Bank -5334763.94 -341252.11 -3605180.83 3268169.31 2952272.39 2666450.82 2407854.71 2173905.94 1962271.72 1770840.74 1597701.86 1441124.77 1299542.74 1171536.95 1055822.43 951235.31 856721.38 771325.68 694183.17 624510.20 561596.91 504800.24 PV Investor -7929399.12 -511878.16 -5457383.83 4992616.20 4551412.99 4148485.59 3780528.12 3444523.34 3137716.59 2857592.27 2601852.57 2368398.15 2155310.70 1960837.02 1783374.61 1621458.53 1473749.51 1339023.03 1216159.45 1104134.97 1002013.39 908938.61 PW -14592249.73 -853130.27 -8237587.18 6825122.96 5635018.13 4651632.90 3839150.13 3167951.53 2613544.42 2155674.62 1777593.30 1465450.68 1207794.80 995156.86 819708.42 674977.72 555615.10 457198.91 376074.98 309223.76 254150.51 208794.37

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Based on the trial was obtained IRR = 20.35%. Then, to know the NPV value as one component of determining the feasibility of the realization of the design, PW calculation with i = MARR = 10%, at which NPV = PW.

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9.5.3 Net Present Value (NPV) An investment is feasible to be implemented if the investment has a value of NPV> 0. This value indicates that the value for money of the plant profit not lower than the value of the money spent as an investment in the factory default. Therefore all of the above ATCF then be calculated present value rate of 10% MARR. Table 6.17 shows the calculation of our plant NPV. Table 9.17 NPV Calculation
Year

NPV PV bank PV Investor -7929399.12 -511878.16 -5457383.83 4992616.20 4551412.99 4148485.59 3780528.12 3444523.34 3137716.59 2857592.27 2601852.57 2368398.15 2155310.70 1960837.02 1783374.61 1621458.53 1473749.51 1339023.03

-1 -5334763.94 0 -341252.11 1 -3605180.83 2 3268169.31 3 2952272.39 4 2666450.82 5 2407854.71 6 2173905.94 7 1962271.72 8 1770840.74 9 1597701.86 10 1441124.77 11 1299542.74 12 1171536.95 13 1055822.43 14 951235.31 15 856721.38 16 771325.68

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17 694183.17 18 624510.20 19 561596.91 20 Total NPV NPV total 504800.24 5143803.48 908938.61 18242597.62 23386401.11 1002013.39 1104134.97 1216159.45

From the table above we can see that the value of the plant NPV is greater than zero. 9.5.4 Pay Back Period The payback period can be determined where the number of cumulative ATCF to year n is equal to zero. From table 6.15, payback period value is located between 3 and 4 years because in year 3 the value of cumulative ATCF is negative and in year 4 the value of cumulative ATCF is positive. Table 9.18 Pay Back Period Calculation Year Payback Bank Payback Self investment 3 4 PBP
-1272777.01 2631173.64 -1909165.51 3946760.46 -3181942.52 6577934.10

Payback overall

3.33

3.33

3.33

From the table above, we using the interpolation, we get the payback period is 3,74 years. This shows that the construction of the plant is feasible to be realized. 9.5.5Break Event Point (BEP) Break Event Point states where the total sales volume of income exactly equal to the total cost, so the company does not make a profit nor suffer a loss. Problems of Break event will appear in the company if it has a Variable Costs and Fixed Costs. A company with a certain production volume may suffer a loss

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Vanillin Production from Lignin

of income due to sales is only able to cover variable costs and can only cover a small portion fixed costs.
( ) ( ) ( )

Where the variable cost is the total of raw material price, labour price, and plant overhead. The data is gotten from table 6.15.

So, the BEP of this plant is 495,95 tonnes. 9.5.6 Sensitivity Analysis Sensitivity for product price Table 9.19. Sensitivity analysis for product price
Deviasi Price -0.20 -0.10 -0.05 0.00 0.05 0.10 0.20 IRR NPV (%) PBP (tahun) -5658627.61 12.30 4.71 8863886.75 16.58 3.86 16125143.93 18.51 3.57 23386401.11 20.35 3.33 30647658.29 22.11 3.13 37908915.46 23.80 2.96 52431429.82 27.00 2.69

14.40 16.20 17.10 18.00 18.90 19.80 21.60

From the table above, we can see that if the price become cheaper, the value of NPV, IRR and the payback period become lower. The payback period is sensitive with deviation -20% or the price of vanillin $ 14.40 because the NPV become a negative value although the PBP below 5 years and IRR still above 10% (below MARR).

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Vanillin Production from Lignin

Product Price Effect

60000000.00 50000000.00 40000000.00 NPV 30000000.00 20000000.00 10000000.00 -0.30 -0.20 0.00 -0.10 0.00 0.10 -10000000.00 PriceDeviation 0.20 0.30 Series1 Linear (Series1) y = 1E+08x + 2E+07 R = 1

Figure 9.2. Sensitivity analysis

for product price

Sensitivity for Raw material price Table 9.20. Sensitivity analysis for raw material cost effect
IRR Deviasi Raw Material Cost NPV (%) PBP (tahun) 0.00 1820411.31 23386401.11 20.35 3.33 0.05 1911431.87 21782327.30 19.94 3.38 0.10 2002452.44 20178253.37 19.51 3.44 0.20 2184493.57 16970105.67 18.66 3.57 0.50 2730616.96 7345662.59 16.03 4.02

From the table above, we can see that if the raw material cost become higher, the value of NPV and IRR become smaller while payback period lower. The payback period is sensitive with deviation 50% or raw material cost $ 2730616.96.

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Vanillin Production from Lignin

Operational Cost Effect

25000000.00 20000000.00 NPV 15000000.00 10000000.00 5000000.00 0.00 0.00 0.20 0.40 0.60 Cost Deviation Series1 Linear (Series1) y = -3E+07x + 2E+07 R = 1

Figure 9.3. Sensitivity analysis

for raw material cost effect

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Vanillin Production from Lignin

APPENDIX

1. Vessel 1.1 Black Liquor Storage Tank (S-101) Calculation Storage tank functioning as a repository of black liquor that will be used for the production of vanillin. To calculate the dimensions of the tank needs to know the total volume of the tank. The total volume of the tank is calculation of tank working volume and tank head space. In the design of storage tanks, assumptions using are: - Ratio of height to diameter of the tank is 4:3 - Tank working volume is 0.85 of the total volume of tank - residence time is 1 hour. Black liquor flow rate:

Tank working volume :

Diameter and height of the tank: ( ) ( )

Where; D is diameter of the tank and H is height of the tank. From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 9.55 m and 7.16 m.

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Vanillin Production from Lignin

Thickness of shell tank: x (CA n) P (psi) = Poperation (psi) + Pstatis + safety factor = 14.7 psi + 21.8 psi + 20 psi = 56.50 S = Allowable stress, for stainless steel 316 = 20000 psi E = Joint efficiency = 0.85 CA= Corrosion Allowance = 0.001 m/year n = equipment life = 20 years ( )

Roof thickness of the tank:

1.2 Acidification Tank (V-101) Calculation a. Tank Design Mixer tank functioning as a tank to mix black liquor slurry with H2SO4. To design mixer tank, the dimensions of the tank needs to know the total volume of the tank. The total volume of the tank is calculation of tank working volume and tank head space. In the design of storage tanks, the assumptions used are: - Ratio of height to diameter of the tank is 4:3 - Tank working volume is 0.85 of the total volume of tank - residence time is 1 hour. Black liquor flow rate:

Tank working volume :

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Vanillin Production from Lignin

Diameter and height of the tank: ( ) ( )

Where; D is diameter of the tank and H is height of the tank. From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 3.87 m and 2.90 m.

Thickness of shell tank: x (CA n) P (psi) = Poperation (psi) + Pstatis + safety factor = 14.7 psi + 4.78 psi + 20 psi = 39.48 S = Allowable stress, for stainless steel 316 = 20000 psi E = Joint efficiency = 0.85 CA= Corrosion Allowance = 0.001 m/year n = equipment life = 20 years ( )

Roof thickness of the tank:

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b. Impeller Design Calculated of impeller design are: Diameter (Da) = 0.4 x 2.90 m = 1.16 m Blade width (W) = 0.125 x 1.16 m = 0.15 m Agitator space from based (E) = 0.167 x 3.29 m = 0.55 m

1.3 Acidification Tank (V-102) Calculation a. Tank Design Mixer tank functioning as a tank to mix black liquor slurry with H2SO4. To design mixer tank, the dimensions of the tank needs to know the total volume of the tank. The total volume of the tank is calculation of tank working volume and tank head space. In the design of storage tanks, the assumptions used are: - Ratio of height to diameter of the tank is 4:3 - Tank working volume is 0.85 of the total volume of tank - residence time is 0.5 hour. Black liquor flow rate:

Tank working volume :

Diameter and height of the tank: ( ) ( )

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Vanillin Production from Lignin

Where; D is diameter of the tank and H is height of the tank. From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 3.06 m and 2.30 m.

Thickness of shell tank: x (CA n)

P (psi) = Poperation (psi) + Pstatis + safety factor = 14.7 psi + 7.05 psi + 20 psi = 41.75 S = Allowable stress, for stainless steel 316 = 20000 psi E = Joint efficiency = 0.85 CA= Corrosion Allowance = 0.001 m/year n = equipment life = 20 years ( )

Roof thickness of the tank:

b. Impeller Design Calculated of impeller design are: Diameter (Da) = 0.4 x 2.30 m = 0.92 m Blade width (W) = 0.125 x 0.92 m = 0.12 m Agitator space from based (E) = 0.167 x 2.60 m = 0.43 m 1.4 Blending Tank ( V-103) Calculation

133

Vanillin Production from Lignin

c. Tank Design Mixer tank functioning as a tank to mix black liquor slurry with H2SO4. To design mixer tank, the dimensions of the tank needs to know the total volume of the tank. The total volume of the tank is calculation of tank working volume and tank head space. In the design of storage tanks, the assumptions used are: - Ratio of height to diameter of the tank is 4:3 - Tank working volume is 0.85 of the total volume of tank - residence time is 10 minute. Black liquor flow rate:

Tank working volume :

Diameter and height of the tank: ( ) ( )

Where; D is diameter of the tank and H is height of the tank. From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 2.04 m and 1.54 m.

Thickness of shell tank: x (CA n)

P (psi) = Poperation (psi) + Pstatis + safety factor

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Vanillin Production from Lignin

= 14.7 psi + 4.49 psi + 20 psi = 39.19 S = Allowable stress, for stainless steel 316 = 20000 psi E = Joint efficiency = 0.85 CA= Corrosion Allowance = 0.001 m/year n = equipment life = 20 years ( )

Roof thickness of the tank:

c. Impeller Design Calculated of impeller design are: Diameter (Da) = 0.4 x 1.54 m = 0.61 m Blade width (W) = 0.125 x 0.61 m = 0.08 m Agitator space from based (E) = 0.167 x 1.74 m = 0.29 m

1.5 Lignin Slurry Storage (S-102) Calculation Storage tank functioning as a repository of alkali lignin slurry before enter to bubble column reactor. To calculate the dimensions of the tank needs to know the total volume of the tank. The total volume of the tank is calculation of tank working volume and tank head space. In the design of storage tanks, assumptions using are: - Ratio of height to diameter of the tank is 4:3 - Tank working volume is 0.85 of the total volume of tank - residence time is 1 hour. Black liquor flow rate:

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Vanillin Production from Lignin

Tank working volume :

Diameter and height of the tank: ( ) ( )

Where; D is diameter of the tank and H is height of the tank. From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 2.58 m and 1.93 m.

Thickness of shell tank: x (CA n) P (psi) = Poperation (psi) + Pstatis + safety factor = 14.7 psi + 5.65 psi + 20 psi = 40.35 S = Allowable stress, for stainless steel 316 = 20000 psi E = Joint efficiency = 0.85 CA= Corrosion Allowance = 0.001 m/year n = equipment life = 20 years ( )

Roof thickness of the tank:

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Vanillin Production from Lignin

1.6 Waste Storage (S-103) Calculation Storage tank functioning as a repository of waste from vanillin production process. To calculate the dimensions of the tank needs to know the total volume of the tank. The total volume of the tank is calculation of tank working volume and tank head space. In the design of storage tanks, assumptions using are: - Ratio of height to diameter of the tank is 4:3 - Tank working volume is 0.85 of the total volume of tank - residence time is 1 hour. Black liquor flow rate:

Tank working volume :

Diameter and height of the tank: ( ) ( )

Where; D is diameter of the tank and H is height of the tank. From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 9.43 m and 7.07 m.

Thickness of shell tank:

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Vanillin Production from Lignin

x (CA n) P (psi) = Poperation (psi) + Pstatis + safety factor = 14.7 psi + 21.6 psi + 20 psi = 56.34 S = Allowable stress, for stainless steel 316 = 20000 psi E = Joint efficiency = 0.85 CA= Corrosion Allowance = 0.001 m/year n = equipment life = 20 years ( )

Roof thickness of the tank:

1.7 H2SO4 Storage (S-104) Calculation Storage tank functioning as a repository of H2SO4 before used in vanillin production process. To calculate the dimensions of the tank needs to know the total volume of the tank. The total volume of the tank is calculation of tank working volume and tank head space. In the design of storage tanks, assumptions using are: - Ratio of height to diameter of the tank is 4:3 - Tank working volume is 0.85 of the total volume of tank - residence time is 1 hour. Black liquor flow rate:

Tank working volume :

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Vanillin Production from Lignin

Diameter and height of the tank: ( ) ( )

Where; D is diameter of the tank and H is height of the tank. From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 4.09 m and 3.07 m.

Thickness of shell tank: x (CA n) P (psi) = Poperation (psi) + Pstatis + safety factor = 14.7 psi + 9.09 psi + 20 psi = 43.79 psi S = Allowable stress, for stainless steel 316 = 20000 psi E = Joint efficiency = 0.85 CA= Corrosion Allowance = 0.001 m/year n = equipment life = 20 years ( )

Roof thickness of the tank:

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Vanillin Production from Lignin

1.8 NaOH Storage (S-105) Calculation Storage tank functioning as a repository of NaOH before used in vanillin production process. To calculate the dimensions of the tank needs to know the total volume of the tank. The total volume of the tank is calculation of tank working volume and tank head space. In the design of storage tanks, assumptions using are: - Ratio of height to diameter of the tank is 4:3 - Tank working volume is 0.85 of the total volume of tank - residence time is 1 hour. Black liquor flow rate:

Tank working volume :

Diameter and height of the tank: ( ) ( )

Where; D is diameter of the tank and H is height of the tank. From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 7.67 m and 5.75 m.

Thickness of shell tank: x (CA n) P (psi) = Poperation (psi) + Pstatis + safety factor

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Vanillin Production from Lignin

= 14.7 psi + 19.72 psi + 20 psi = 54.42 psi S = Allowable stress, for stainless steel 316 = 20000 psi E = Joint efficiency = 0.85 CA= Corrosion Allowance = 0.001 m/year n = equipment life = 20 years ( )

Roof thickness of the tank:

2. Plate and Frame Filter 2.1 Plate and Frame Filter (PF-101) Sizing Calculation : 1. Component mass and volume Component Lignin Alkali Water Lean Liquor Liquid Acid lean liquor solid Total Total Mass Filtrate Total Mass Cake 2. Filtrate density ( ( 3. Cake density ) ) input mass (ton) 2 3.91 18.45 0.31 0 24.68 output mass (ton) 2 3.91 13.78 0.31 4.67 24.68 18.01 6.67 Density (ton/m3) 1.3 1 1 1 1 13.35 input volume (m3)/ batch 1.54 3.91 18.45 0.31 0 24.22 Total VolumFiltrat output volum (m3)/ batch 1.54 3.91 13.78 0.31 4.67 24.22 18.01

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Vanillin Production from Lignin

( ( 4. Thickness of cake (L) Estimated thickness of cake is = 0.06 m 5. Estimated cake porosity Cake porosity ( ) of black liquor with pH 9 at 30C = 0.7 6. Dry solid per unit area ( ) ( ( kg/m2 ) ) ) )

7. Effective filtration area (A)

m2 8. Safety factor = 20% 9. Filtration area (A) ( )

10.In this design, we use press filter with the filter area 2 x 2 m (4 m2) and have 50 chambers. So, total press filter that we need for this process is:

And total minimum plate required is:

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Vanillin Production from Lignin

2.2 Plate and Frame Filter (PF-102) Sizing Calculation: 1. Component of lignin Slurry input mass (ton) 5 5.29 23.93 3.42 37.64 output mass (ton) 5 5.29 23.93 3.42 37.64 32.64 2.5 input output Density 3 volume (m )/ volum (m3)/ (ton/m3) batch batch 1.3 2.66 1 1 3.85 1.99 23.93 3.42 33.18 Volume filtrate 3.85 1.99 23.93 3.42 33.18 29.34

Component

Lignin alkali sulfate Liquid Acid water total total mass filtrate total mass cake

2. Filtrate density

3. Cake density

4. Thickness of cake (L) Estimated thickness of cake is = 0.06 m 5. Estimated cake porosity Cake porosity ( ) of black liquor with pH 3 at 30C = 0.33 6. Dry solid per unit area ( ) ( ( kg/m2 ) )

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Vanillin Production from Lignin

7. Effective filtration area (A)

m2 8. Safety factor = 20% 9. Filtration area (A) ( )

10.In this design, we use press filter with the filter area 1.5 x 1.5 m (2.25 m2) and have 24 chambers. So, total press filter that we need for this process is:

And total minimum plate required is:

Pump

3.1 Black Liquor Pump (P-101)&(P-102) Operation Condition : Psuction= 100,000 Pa Pdischarge= 105,000 Pa T = 600 C Mass Rate = 66.77 ton/h Density = 1818.2kg/m3 Liquid Viskosity = 5.09 cP

Pump design : ( ) ( ) (Timmerhaus, 2004)

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Vanillin Production from Lignin

From tabel A.3 buku Noel de Nevers (1991), we choose pipe with spesification: Nominal Measure: 6 inch Schedule number : 40 Inner Diameter (ID) : 6.065in Outer Diameter (OD) : 6.625 in Inside sectional area : 28.9 inch2 Velocity,

Reynold Number: (aliran turbulen)

To get the value of the friction factor, used 6:10 on the book charts Noel de Nevers (1991), in which the first note / D. To pipe the design of this plant, used types of commercial steel. From table 6.2 on the book Noel de Nevers (1991), is known for stainless steel pipes , value = 0,000046 m. So, value /D = 0.0029 From 6:10 charts Noel de Nevers book (1991), the value of the friction factor (f) = 0,0034

Assumption of friction loss in the pipe is relatively the same. Friction loss : Number of Velocity Tank outlet Tank inlet 0.5 1 Equivalent pipe diameter 25 50

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Vanillin Production from Lignin

Gate valve 4 elbow Total 0.3 9 10.8 15 450 540

Extra Length of Pipe:

Total Length

Pressure Drop

Pressure Drop = 4381.08 N/m2

Head

: 3.87 m

Pressure Differences : 5000 N/m2 Efficiency

Eff = 82.77%

From Energy Balance, So we can get, W : 43.08 J/kg

Power : 0.32 kWh/operation 3.2 Black Liquor Acidification Pump (P-102) Operation Condition : Psuction= 105,000 Pa
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Vanillin Production from Lignin

Pdischarge= 700,000 Pa T = 600 C Mass Rate = 33.38 ton/h Density = 1020kg/m3 Liquid Viskosity = 1.7 cP

Pump design : ( ) ( ) (Timmerhaus, 2004)

From tabel A.3 buku Noel de Nevers (1991), we choose pipe with spesification: Nominal Measure: 6 inch Schedule number : 40 Inner Diameter (ID) : 6.065in Outer Diameter (OD) : 6.625 in Inside sectional area : 28.9 inch2 Velocity,

Reynold Number: (Turbulen Stream)

To get the value of the friction factor, used 6:10 on the book charts Noel de Nevers (1991), in which the first note / D. To pipe the design of this plant, used types of commercial steel. From table 6.2 on the book Noel de Nevers (1991), is known for stainless steel pipes , value = 0,000046 m. So, value /D = 0.0029 From 6:10 charts Noel de Nevers book (1991), the value of the friction factor (f) = 0,0034

Assumption of friction loss in the pipe is relatively the same.

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Vanillin Production from Lignin

Friction loss :
Number of Velocity Tank outlet Tank inlet Gate valvle 4 elbow Total 0.5 1 0.3 6 7.8 Equivalent pipe diameter 25 50 15 300 390

Extra Length of Pipe:

Total Length

Pressure Drop

Pressure Drop = 1271.13 N/m2

Head

: 4.58 m

Pressure Differences : 595,000 N/m2 Efficiency

Eff = 82.49%

From Energy Balance, So we can get, W Power : 629.46 J/kg :2.35 kWh/operation

3.3 Lignin Acidification Pump (P-103) Operation Condition : Psuction= 105,000 Pa Pdischarge= 700,000 Pa T = 600 C

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Vanillin Production from Lignin

Mass Rate = 61.68 ton/h Density = 1774.71kg/m3 Liquid Viskosity = 1.32 cP

Pump design : ( ) ( ) (Timmerhaus, 2004)

From tabel A.3 buku Noel de Nevers (1991), we choose pipe with spesification: Nominal Measure: 6 inch Schedule number : 40 Inner Diameter (ID) : 6.065in Outer Diameter (OD) : 6.625 in Inside sectional area : 28.9 inch2 Velocity,

Reynold Number: (Turbulen Stream)

To get the value of the friction factor, used 6:10 on the book charts Noel de Nevers (1991), in which the first note / D. To pipe the design of this plant, used types of commercial steel. From table 6.2 on the book Noel de Nevers (1991), is known for stainless steel pipes , value = 0,000046 m. So, value /D = 0.0029 From 6:10 charts Noel de Nevers book (1991), the value of the friction factor (f) = 0,0034

Assumption of friction loss in the pipe is relatively the same. Friction loss :
Number of Velocity Equivalent pipe diameter

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Vanillin Production from Lignin

Tank outlet Tank inlet Gate valvle 4 elbow Total 0.5 1 0.3 9 10.8 25 50 15 450 540

Extra Length of Pipe:

Total Length

Pressure Drop

Pressure Drop = 3601.57 N/m2

Head

: 3.16 m

Pressure Differences : 595,000 N/m2 Efficiency

Eff = 81.98%

From Energy Balance, So we can get, W Power : 368.26 J/kg : 2.56 kWh/operation

3.4 Lignin Solution Pump (P-104) Operation Condition : Psuction= 105,000 Pa Pdischarge= 105,000 Pa T = 600 C Mass Rate = 35.15 ton/h Density = 1814.6kg/m3

150

Vanillin Production from Lignin

Liquid Viskosity = 2.08cP

Pump design : ( ) ( ) (Timmerhaus, 2004)

From tabel A.3 buku Noel de Nevers (1991), we choose pipe with spesification: Nominal Measure: 4inch Schedule number : 40 Inner Diameter (ID) : 4.026in Outer Diameter (OD) : 4.5 in Inside sectional area : 28.9 inch2 Velocity,

Reynold Number: (Turbulen Stream)

To get the value of the friction factor, used 6:10 on the book charts Noel de Nevers (1991), in which the first note / D. To pipe the design of this plant, used types of commercial steel. From table 6.2 on the book Noel de Nevers (1991), is known for stainless steel pipes , value = 0,000046 m. So, value /D = 0.0044 From 6:10 charts Noel de Nevers book (1991), the value of the friction factor (f) = 0,0035

Assumption of friction loss in the pipe is relatively the same. Friction loss :
Number of Velocity Tank outlet Tank inlet Gate valvle 0.5 1 0.3 Equivalent pipe diameter 25 50 15

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Vanillin Production from Lignin

4 elbow Total 3 4.8 150 240

Extra Length of Pipe:

Total Length

Pressure Drop

Pressure Drop = 3165.23 N/m2

Head

: 3.12 m

Pressure Differences : 0 N/m2 Efficiency

Eff = 79.83 %

From Energy Balance, So we can get, W Power : 32.32 J/kg : 0.06 kWh/operation

3.5 Lignin Solution Pump (P-105) Operation Condition : Psuction= 105,000 Pa Pdischarge= 105,000 Pa T = 600 C Mass Rate = 49.21 ton/h Density = 1814.6kg/m3 Liquid Viskosity = 2.08cP

152

Vanillin Production from Lignin

Pump design : ( ) ( ) (Timmerhaus, 2004)

From tabel A.3 buku Noel de Nevers (1991), we choose pipe with spesification: Nominal Measure: 6 inch Schedule number : 40 Inner Diameter (ID) : 6.625in Outer Diameter (OD) : 6.065 in Inside sectional area : 28.9 inch2 Velocity,

Reynold Number: (Turbulen Stream)

To get the value of the friction factor, used 6:10 on the book charts Noel de Nevers (1991), in which the first note / D. To pipe the design of this plant, used types of commercial steel. From table 6.2 on the book Noel de Nevers (1991), is known for stainless steel pipes , value = 0,000046 m. So, value /D = 0.0044 From 6:10 charts Noel de Nevers book (1991), the value of the friction factor (f) = 0,0035

Assumption of friction loss in the pipe is relatively the same. Friction loss :
Number of Velocity Tank outlet Tank inlet Gate valvle 4 elbow Total 0.5 1 0.3 3 4.8 Equivalent pipe diameter 25 50 15 150 240

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Vanillin Production from Lignin

Extra Length of Pipe:

Total Length

Pressure Drop

Pressure Drop = 1129.98 N/m2

Head

: 4.48 m

Pressure Differences : 0 N/m2 Efficiency

Eff = 81.32 %

From Energy Balance, So we can get, W Power : 44.53 J/kg : 0.12 kWh/operation

3.6 Vanillin Slurry Pump (P-106) Operation Condition : Psuction= 105,000 Pa Pdischarge= 200,000 Pa T = 600 C Mass Rate = 4.87 ton/h Density = 1609kg/m3 Liquid Viskosity = 5.13cP

Pump design :

154

Vanillin Production from Lignin

( ) ( ) (Timmerhaus, 2004)

From tabel A.3 buku Noel de Nevers (1991), we choose pipe with spesification: Nominal Measure: 1.5inch Schedule number : 40 Inner Diameter (ID) : 1.9in Outer Diameter (OD) : 1.61 in Inside sectional area : 2.04 inch2 Velocity,

Reynold Number: (Turbulen Stream)

To get the value of the friction factor, used 6:10 on the book charts Noel de Nevers (1991), in which the first note / D. To pipe the design of this plant, used types of commercial steel. From table 6.2 on the book Noel de Nevers (1991), is known for stainless steel pipes , value = 0,000046 m. So, value /D = 0.0011 From 6:10 charts Noel de Nevers book (1991), the value of the friction factor (f) = 0,0055

Assumption of friction loss in the pipe is relatively the same. Friction loss :
Number of Velocity Tank outlet Tank inlet Gate valvle 4 elbow Total 0.5 1 0.3 3 4.8 Equivalent pipe diameter 25 50 15 150 240

Extra Length of Pipe:

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Vanillin Production from Lignin

Total Length

Pressure Drop

Pressure Drop = 52,223 N/m2

Head

: 0.34 m

Pressure Differences : 95,000 N/m2 Efficiency

Eff = 79.73 %

From Energy Balance, So we can get, W Power : 94.83 J/kg : 0.32 kWh/operation

3.7 Vanillin Solution Pump (P-107) Operation Condition : Psuction= 105,000 Pa Pdischarge= 150,000 Pa T = 600 C Mass Rate = 0.85 ton/h Density = 1015.67kg/m3 Liquid Viskosity = 1.65cP

Pump design : ( ) ( ) (Timmerhaus, 2004)

156

Vanillin Production from Lignin

From tabel A.3 buku Noel de Nevers (1991), we choose pipe with spesification: Nominal Measure: 1.5 inch Schedule number : 40 Inner Diameter (ID) : 1.9in Outer Diameter (OD) : 1.61 in Inside sectional area : 2.04 inch2 Velocity,

Reynold Number: (Turbulen Stream)

To get the value of the friction factor, used 6:10 on the book charts Noel de Nevers (1991), in which the first note / D. To pipe the design of this plant, used types of commercial steel. From table 6.2 on the book Noel de Nevers (1991), is known for stainless steel pipes , value = 0,000046 m. So, value /D = 0.0011 From 6:10 charts Noel de Nevers book (1991), the value of the friction factor (f) = 0,0055

Assumption of friction loss in the pipe is relatively the same. Friction loss :
Number of Velocity Tank outlet Tank inlet Gate valvle 4 elbow Total 0.5 1 0.3 3 4.8 Equivalent pipe diameter 25 50 15 150 240

Extra Length of Pipe:

Total Length

157

Vanillin Production from Lignin

Pressure Drop

Pressure Drop = 52,223 N/m2

Head

: 0.34 m

Pressure Differences : 45,000 N/m2 Efficiency

Eff = 79.69 %

From Energy Balance, So we can get, W Power : 50.12 J/kg : 0.029 kWh/operation

3.8 Water Pump (P-108) Operation Condition : Psuction= 105,000 Pa Pdischarge= 700,000 Pa T = 600 C Mass Rate = 3.33 ton/h Density = 1000kg/m3 Liquid Viskosity = 0.89cP

Pump design : ( ) ( ) (Timmerhaus, 2004)

From tabel A.3 buku Noel de Nevers (1991), we choose pipe with spesification: Nominal Measure: 1.5 inch Schedule number : 40
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Inner Diameter (ID) : 1.9in Outer Diameter (OD) : 1.61 in Inside sectional area : 2.04 inch2 Velocity,

Reynold Number: (Turbulen Stream)

To get the value of the friction factor, used 6:10 on the book charts Noel de Nevers (1991), in which the first note / D. To pipe the design of this plant, used types of commercial steel. From table 6.2 on the book Noel de Nevers (1991), is known for stainless steel pipes , value = 0,000046 m. So, value /D = 0.0011 From 6:10 charts Noel de Nevers book (1991), the value of the friction factor (f) = 0,005

Assumption of friction loss in the pipe is relatively the same. Friction loss :
Number of Velocity Tank outlet Tank inlet Gate valvle 4 elbow Total 0.5 1 0.3 6 7.8 Equivalent pipe diameter 25 50 15 300 390

Extra Length of Pipe:

Total Length

Pressure Drop

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Pressure Drop = 91.87 N/m2

Head

: 4.58 m

Pressure Differences : 595,000 N/m2 Efficiency

Eff = 76.51 %

From Energy Balance, So we can get, W Power : 639.97 J/kg : 0.25 kWh/operation

Tank working volume :

Diameter and height of the reactor: ( ) ( )

Where; D is diameter of the tank and H is height of the tank.From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 1.89 m and 1.134 m.

Thick walls of the tank:

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P (psig) = P operation (psia) + Pstatis + safety factor = 159,7 psia + 14.7 psia + 25 psia = 199,4 psia = 184,7 psig S = Allowable stress, for Stainless Steel 316 = 74500 psig E = Joint efficiency = 0.8 (Walas, 1988) R = D/2 = 0,8465 m = 33,32 in Corrosive factor = 0.15 in

Bubble Column Reactor

Stoichiometry 1 Lignin Oxidation : 0.5 L + 1.56 O2 --> V + 114 X Initial (mol) Change (mol) Remaining (mol) 2350.242 10781.25 -1645.17 -7332.75 4700.483

Conversion

70%

705.0725 3448.496 4700.483

Stoichiometry 2 Vanilin Oxidation : V + O2 --> Product Initial (mol) Change (mol) Remaining (mol) 4700.483 3448.496 -3290.34 -3290.34 3290.338

1410.145 158.1582 3290.338 massa 500592.048 gram

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0.50059205 ton 500.592048 kg

Reactor Volume = 25.51 m3 Reactor functioning as a tank to mix and react lignin slurry with oxygen in alkaline condition. To design bubble column reactor, the dimensions of the reactor needs to know the total volume of the reactor. In the design of reactor, the assumptions used are: - Ratio of height to diameter of the bubble column reactor is 5:3 - residence time is 2 hour. Diameter and height of the reactor: ( )

( )

Where; D is diameter of the tank and H is height of the tank. From the results of calculation and rounding up to 0.1 m, height and diameter of the tank is obtained respectively 4.48 m and 2.69 m.

Thickness of shell tank: x (CA n)

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P (psi) = Poperation (psi) + Pstatis + safety factor = 145 psi + 6787 psi + 20 psi = 174.84 S = Allowable stress, for stainless steel 316 = 20000 psi E = Joint efficiency = 0.85 CA= Corrosion Allowance = 0.001 m/year n = equipment life = 20 years ( )

Roof thickness of the tank:

5 Ultrafiltrasi Sizing Calculation : Component mass and volume Component Input mass Output (ton) Density Input volume (m3)/ batch Vanillin Alkali Lignin Slurry Water 0.500 5.360 1.200 0.500 0.000 1.200 1.05 1.22 1 0.476 4.393 1.200 Output volume (m3)/ batch 0.476 0 1.200

mass (ton) (ton/m3)

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Others Filtrate Cake Total total mass filtrate 4.780 0.000 11.840 0.000 10.140 11.840 1.700 1 1.3 4.780 0 10.849 volum filtrat 0 7.800 9.476 1.676

Filtrate density ( ( 3. Cake density ( ( 4. Thickness of cake (L) Estimated thickness of cake is = 0.03 m 5. Estimated cake porosity Cake porosity ( ) of product = 0.2 6. Dry solid per unit area ( ) ( ( ) ) kg/m2 7. Effective filtration area (A) ) ) ) )

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m2 8. 9. Safety factor = 20% Filtration area (A) ( )

10.In this design, we use hollow fiber ultrafiltration with the filter area 190 m2 and have 10000 fibers per module. So, filter that we need for this process is:

6 Spray Dryer Surface moisture is removed in about 5 sec, and most drying is completed in less than 60 sec. Parallel flow of air and stock is most common. Atomizing nozzles have openings 0.012-0.15 in. and operate at pressures of 300-4000 psi. Atomizing spray wheels rotate at speeds to 20,000rpm with peripheral speeds of 250-600 ft/sec. With nozzles, the length to diameter ratio of the dryer is 4-5; with spray wheels, the ratio is 0.5-1.0. For the final design, the experts say, pilot tests in a unit of 2 m dia should be made.

Diameter of particle, T air inlet = 120oC T air oulet = 110oC T feed inlet = 80oC T feed outlet = 90oC

= 55,65 m

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Vanillin Production from Lignin

Design aspect include : Atomizer : its type & design, flow rate of the heated inlet air, settling velocity, solid & Gas operating velocity, chamber Diameter, residence time, design of Conical bottom.

Atomizer : Centrifugal disk atomization is particularly advantageous for atomizing suspensions and pastes that erode and plug nozzle. Type of Disk atomizer (Vane, Kesner, Pin) Ref. patent US20040139625. Diameter of the disk atomizer 5-45 cm. Rotational speed 33.000 rpm, peripheral speed 6000 m/min. Mean particle size 55 micron.

Feed Rate = 730 kg/hr = 24 lb/min Peripheral speed is got from Herring and Marshal chart (peripheral speed vs. mean particle diameter, with feed rate as parameter). On interpolation we get 473 ft/s (v =8952 m/min).

Disk Selection Disk selected = B-1, with diameter 0,59 ft. Vane height= 0,406 ft, vane length = 1 ft, number of vanes = 60. Rotational speed (N) = N = 473 * 60 = 15800 rpm So, power consumption of atomizer can be calcaulated below ( )

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Spray Chamber design

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Vanillin Production from Lignin

X1 = 0.015, X2 = 0.003 Y1 = 0.01317 (by psychometric chart at given DB & WB) humidity air HL1= 112.2 kJ/kg of dry solid, HL2= 121.68 kJ/kg of dry solid H1= 134.29 kJ/kg dry air Simultaneously solving mass balance and enthalpy balance eq (1) and (2) we get Y2= 0.0206 Evaporation rate of water = (0.015-0.003)*1500 kg/hr = 18 kg Assumed chamber efficiency is 70%, therefore net evaporation rate of water is 18/0.7 =25.71 kg water /hr. Moisture removed per kg of dry air = (0.0206-0.01317)=0.00743 kg water per kg of dry air. Gs = 25.71/0.00743 = 3460 kg/hr.

After this we must calculate humid volume

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Vanillin Production from Lignin

Humid volume inlet (Vin) = 0.283 m3/kg dry air Humid volume outlet (Vout) = 0.281 m3/ kg dry air Vavg = (Vin + Vout)/2 = 0.282 m3 / kg dry air Assume Dp = 100 micron And then we calculate operating velocity. The operating velocity in the case of non-dusting spray dryer is taken as two times the settling velocity of the drop.

Settling velocity didapatkan berdasarkan perhitungan adalah sebesar 0.25 m/s. Stokes law is applicable if Re < 2. So we must check the reynold number

So we can get operating velocity, va= 2vs = 2*0.25 = 0.5 m/s

Column Area:

= 3.1 m2

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Vanillin Production from Lignin

Column diameter : factor, Dc = 2.1 m. Residence time :

= 1,974 m, for safety, assuming 15 % safety

Time required to evaporate moisture from droplet :

p = 0.00969 sec, p < td, design is acceptable

Chamber is a cylindrical with a conical bottom Total volume of chamber (Vt) = Gs*Vav*td = 5.2 m3 Minimum height of cylindrical portion (hmin) = vs*p = 0.00068 m Recommended height of cylindrical portion (hcyl) = 0.6 *Dc = 1.47 m Volume Cone = Height of cone (hcone) = Cone angle : tan(a/2) = Dc/2hcone a = 20.57 degree Thickness of chamber : tmin = (Dc+100)/1000 = 0.11 inch = 3.1 m3 m

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7. Material Safety Data Sheet (MSDS) 1. Black Liquor Properties Molecular Weight (g/mol) Melting Point (0C) Boiling Point (0C) Form Odor pH Color Solubility Flammability Information Not available Not available Variable Slurry rotten egg odor Typical Range 10-12 Black liquid Soluble in cold and hot water Not flammable, will burn at very high temperatures Aluminum and acids. Contact with acids and oxidizing agents can result in release of potentially lethal concentrations of hydrogen sulfide (H2S) gas Corrosive with aluminum Causes eye and skin irritation and corrosion; respiratory airways irritation if ingested in large amounts : digestive tract irritation and corrosion, vomiting, diarrhea, and death (possible) Do not contact with eyes, skin, and clothing. Do not be inhaled Do not contact with the acid Keep away from acids and aluminum Gloves, respirator, eye protection, goggles and footwear Open ventilation and insulation use

Materials to avoid

Corrosivity Toxic effect

Handling

Storage Personal protective equipment Spill procedures

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Vanillin Production from Lignin

a shovel to dispose of spill 2. H2SO4 Properties Molecular Weight (g/mol) Melting Point (0C) Boiling Point (0C) Form Odor pH Color Solubility Flammability Materials to avoid Corrosivity 98 10.36 100 Liquid Odorless Typical Range 2-3 Transparent Soluble in cold and hot water Easy to flammable Organic material, metal, acids, and alkali Corrosive with aluminum, stainless steel (304,316), not corrosive with glass Causes eye irritation and burn if contact with skin. Do not contact with eyes, skin, and clothing. Keep in closed container, cool, and good ventilated Gloves, respirator, eye protection, goggles and footwear Spare with soil, sand, and not flammable material Information

Toxic effect Handling Storage Personal protective equipment Spill procedures

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Vanillin Production from Lignin

3. NaOH Properties Molecular Weight (g/mol) Melting Point (0C) Boiling Point (0C) Form Odor pH Color Solubility Flammability Materials to avoid Corrosivity Toxic effect Handling Storage Personal protective equipment Spill procedures 40 323 1388 Solid Odorless 13.5 (Basic) White Easily soluble in cold water Not flammable Aluminum Very caustic to aluminum and other metals in presence of moisture. Causes damage to the following organs: lungs Do not contact with eyes, skin, and clothing. Keep in closed container and cool Gloves, respirator, eye protection, goggles and footwear Insulation use a shovel to dispose of spill Information

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Vanillin Production from Lignin

REFERENCE A, m. Z., silva, e. B., & rodrigues, a. (2007). Recovery of vanillin from lignin/vanillin mixture by using tubular ceramic ultrafiltration membranes. Journal of membrane science , 221237. Arajo, j. D. (2008). Production of vanillin from lignin present in the kraft black liquor of the pulp and paper industry. Biological and chemical engineering . Arajo, j. D., grande, c. A., & rodrigues, a. E. (2010). Vanillin production from lignin oxidation in a batch reactor. Chemical engineering research and design , 10241032. Heradewi. (2007). Isolasi lignin dari lindi hitam proses pemasakan organosolv serat tandan kosong kelapa sawit (tkks). Bogor: institut pertanian bogor. Jo, j. D., grande, c. A., & rodrigues, a. E. (2009). Structured packed bubble column reactor for continuous production of vanillin from kraft lignin oxidation. Journal of catalysis today , s330-335. Peters, m. S., & timmerhaus, k. D. (1991). Plant design and economics for chemical engineers. New york: mcgraw-hill. Priefert, h., rabenhorst, j., & steinbchel, a. (2001). Biotechnological production of vanillin. Appl microbiol biotechnol , 56:296314. Silvaa, e. B., zabkovaa, m., arajoa, j., c.a. Catetob, c., & barreirob, m. (2009). An integrated process to produce vanillin and lignin-based polyurethanes from kraft lignin. Chemical engineering research and design , 12761292. Sinnott, R. K. (2005). Chemical Engineering Design, Vol. 6. ButterworthHeinemann: Elsevier. Tomani, p. (2009). The lignoboost process. Cellulose chemistry and technology .

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