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DOI: 10.4172/2155-9589.1000140

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ISSN: 2155-9589

Mini Review Article

Research OpenAccess
Open Access

Nano-Filtration and Ultra-Filtration Ceramic Membranes for Food

Processing: A Mini Review
Daniele Mancinelli and Cynthia Hallé*
Department of Hydraulic and Environmental Engineering, Norwegian University of Science and Technology, S.P. Andersens vei 5, Trondheim, Norway

Abstract
This mini-review investigates the application of nano- and ultra-filtration ceramic membranes in the field of
food processing. This type of application appeared recently and the number of food processing sectors that can be
interested with these techniques is likely to increase. In addition, food production represents a novel niche for ceramic
membranes. Selected publications reviewed the application of ceramic membranes in the field of drinking water,
dietary fats, carbohydrates, proteins and fermentation broths production. Research shows that ceramic membranes
are a promising alternative to more traditional methods, although there are some challenges to overcome in order
to become competitive, such as the control and reduction of membrane fouling, and a deeper understanding of the
relationships at the molecular level between the solutes and the membrane surface.

Keywords: Ceramic membrane; Food process; Nanofiltration; with 50% of the total publications found being released during the
Ultrafiltration last three years. During the period from 2012 to 2014, 21 papers were
published, thus 27% of the total publications were submitted during
Introduction the last three years while the initial paper appeared during the first half
The development of inorganic membranes started with vycor type of the 1985’s (i.e. 30 years earlier).
glass membranes initially studied around the 1940’s. The first period
that proceeded the current generation of inorganic membranes was Publications Ceramic Membrane for UF/NF
related to the separation of uranium isotopes by gaseous diffusion Cumulative Pub. NF Food Cumulative Pub. UF/NF Cumulative Pub. UF/NF Food
processes. The challenge was to employ membrane materials who
can sustain aggressive environment and offer reliable performances. 90
78
Following such developmental work, two companies in the 1973, 80
Ceraver and Euroceral, started to produce ceramic oxide based
70
supports used to supply the Nuclear Fission Industry of suitable 57
propeller. The nature of the membranes still operating in Eurodif plant 60

(France) remains classified [1]. The second period consists on the 50 45

development of microfiltration (MF) and ultrafiltration (UF) inorganic 40 34
membranes as a consequence of the knowledge accumulated by the 25
30
companies producing gaseous diffusion plants [1]. In the 1960’s, Carre 19
16
(a subsidiary of DuPont) developed the concept of liquid filtration 20
11 13
on dynamic zirconium hydroxide supported on stainless steel. In 10
1 3 5 4 6
6 6
2 2 12
the 1970’s, Union Carbide developed ceramic oxide layers coated on 0
carbon supports [1]. The first commercial cross-flow filtration system
equipment with inorganic membrane was manufactured by SFEC in
the 1978. The concept of multichannel support was introduced in the Figure 1: a) (blue line) the curve indicates the total amount of publications
1980’s from Ceraver [1] and could be considered the starting point found up to the indicated period concerning UF and NF via ceramic membrane.
on the development of the new generation of ceramic membranes b) (orange line) the curve indicates the total amount of publications found
up to the indicated period concerning UF and NF via ceramic membrane
(CM) which began to operate at lower porosity scales: UF first and employed in food processes; c) (violet line) the curve indicates the total
nanofiltration (NF) more recently. amount of publications found up to the indicated period concerning NF via
ceramic membrane employed in food processes.
This mini-review includes articles and papers published within the
period from 1945 to 2014 that address the topic of UF and NF with CM.
A total of 78 publications were selected, using Web of Science was used
as search engine, for the study of which 25 were further investigated *Corresponding author: Cynthia Hallé, Department of Hydraulic and
Environmental Engineering, Norwegian University of Science and Technology,
because of their direct application to food production processing. Trondheim, Norway, Tel: +4745029086; E-mail: [email protected]
As shown in Figure 1, the first publication was published in 1985 Received  November 02, 2015; Accepted November 30, 2015; Published
indicating that CM is an emerging technology. The steady increase December 08, 2015
of yearly publications indicates that interest in UF and NF ceramic Citation: Mancinelli D, Hallé C (2015) Nano-Filtration and Ultra-Filtration Ceramic
membranes is growing rapidly. The first food processing applications in Membranes for Food Processing: A Mini Review. J Membra Sci Technol 5: 140.
the field of UF and NF with CM were published during the 1997-1999 doi:10.4172/2155-9589.1000140
period. According to Figure 1, the most recent development in the food Copyright: © 2015 Mancinelli D, et al. This is an open-access article distributed
processing industry is the use of NF-CM at the beginning of the 2000’s under the terms of the Creative Commons Attribution License, which permits
unrestricted use, distribution, and reproduction in any medium, provided the
[2], but it is growing at an even higher rate than the total publications original author and source are credited.

J Membra Sci Technol

ISSN:2155-9589 JMST an open access journal Volume 5 • Issue 2 • 1000140
Citation: Mancinelli D, Hallé C (2015) Nano-Filtration and Ultra-Filtration Ceramic Membranes for Food Processing: A Mini Review. J Membra Sci
Technol 5: 140. doi:10.4172/2155-9589.1000140

Page 2 of 13

The review begins by looking at the basic principles of filtration of turbulent flow of retentate on the membrane surface: cross-flow
followed by a section on ceramic membrane development and challenges configuration. RF represents the membrane fouling which the
in their applications. Several applications of CM in the field of drinking resistance is created by the progressive accumulation of particles on
water, dietary fats, carbohydrates, proteins and fermentation broths the membrane surface and within the pores of the membrane causing a
production are discussed. The wide scope of this review indicates the decrease of permeates flux.
high potential of CM in the food industry. Finally, the review includes
recommendation for future works that must be addressed in order to Ceramic membranes development
make improvement in ceramic membrane processes. Filtration technologies based on inorganic membranes are a
relatively new field that is receiving increasing interest from the industry.
Fundamental of Membrane Filtration The CM represents a very important class of inorganic membranes [1].
Separation mechanisms The main type of ceramics currently in use for the manufacturing of
filtration membranes consists of refractory oxides: alumina, zirconia
The flux through an ideal semipermeable membrane can be or titania [3]. Nevertheless, a number of other ceramic materials such
described by the following equation: as cordierite, mullite, silicon nitride, silica and borosilicate glasses were
J = Qp / A (1) indicated as suitable materials for inorganic membrane production [4].
One of the advantages of the application of CM over the polymeric
J indicates the flux through a membrane; calculated as volume of counterparts is the capacity to withstand harsh operating conditions
liquid permeating per m2 of membrane surface area in an hour time in terms of pH, temperature, pressure and chemical stability [5-7]. CM
period (L/hm2). Qp indicates the permeate flow rate (in liter per hour), can be operated with liquid or gaseous media. They are manufactured
and A indicates the membrane surface area (m2). within a wide range of superficial porosity and they can be employed
In the case of MF and UF, the osmotic pressure of the permeate and in MF (macropores above 0.1 µm in diameter), UF (mesopores ranging
retentate can be neglected while for nanofiltration (NF) and reverse from 0.1 µm to 10 nm of diameter) and NF (nanopores below 10 nm
osmosis (RO) this value increase to a point it becomes the dominant of diameter) [8]. Porous CM is becoming widely applied in MF and
resistance force. UF. Recently, they entered the NF domain and their applications are
increasing.
According the Hagen-Poiseuille law, the flux through an ideal
membrane of an incompressible liquid can be expressed as: Ceramic membranes can be produced with different geometries:
flat, tubular, multichannel or monolithic geometry. Du Pont have
J =
ε dp2 PT / 32 ∆x µ (2) proposed alumina hollow fibers in the microfiltration range [1]. An
ε indicates the porosity of the membrane, dp is the channel interesting application of a MF ceramic membrane with stamped
diameter, PT is the applied transmembrane pressure, Δx is the length geometric design was successfully tested for a food production process
of the channel, µ is the viscosity of the permeate. If a specific membrane [9].
was tested it can be assumed that for such membrane ε, dp, and Δx are Initially the CM were of tubular shape with a low volume to surface
constants and they can be included in a constant that can be defined as ratio but their design has constantly evolved toward multichannel
permeability coefficient A (A = ε dp / 32 Δx). Therfore the equation (2) cylindrical geometries [1]. The tubular shaped channels developed into
can be rewritten as: flower shaped multichannel further optimizing the surface to volume
J = A PT / µ (3) ratio and ultimately they reached a monolithic structured design with
very high density of cells and thin walls. This development led to
The equation (3) shows the relationship existing between J, PT, and considerably larger hydraulic sections and high filtrating surface per
µ. As the pressure increases J increases. As temperature increases the element. All these ceramic membrane elements are currently available
viscosity of the fluid is reduced and the permeate J increases. If A/µ is on the market.
defined as the reverse of membrane resistance (1/RM), equation (3) can
be transformed into: All the publications examined in this mini-review concern CM used
in a cross-flow configuration. The liquid feed circulates tangentially to
J = PT / RM (4) the surface of the membrane while the permeated liquid goes through
During the actual filtration operation, RM may become a minor the membrane perpendicularly to the feed flow direction. The filtration
resistance factor if compared to other forms of membrane resistance. driving force is generally the transmembrane pressure applied from the
In order to obtain a more representative calculation of the flux retentate side.
concentration polarization (RG) and fouling (RF) should be considered Challenges
(equation 5):
Typically, the flow through the membrane decreases during
=J PT / ( RM + RF + RG ) (5) the operation with fluids [8], one of the major causes of such loss of
RG is the resistance caused by the concentration polarization, productivity is the fouling phenomenon. The membrane fouling
which becomes particularly significant in case of UF, NF and RO. was defined by Koros et al. [10] as the “process resulting in the loss
Concentration polarization is caused by the accumulation of solutes at of performance of a membrane due to deposition of suspended or
the surface of the membrane. When the flux and diffusion coefficient dissolved substances on its external surface, or within its pores”. This
are in the same order of magnitude the solutes tend to accumulate on phenomenon is complex [11] and not yet adequately described by
the membrane surface creating a secondary filtration layer that cause a current proposed models [12]. It influences the lifespan of a membrane,
significant increase in resistance. increases energy demand, maintenance and cleaning costs [13,14].

This type of phenomenon can be attenuated via the creation We can identify four general types of fouling:

J Membra Sci Technol

ISSN:2155-9589 JMST an open access journal Volume 5 • Issue 2 • 1000140
Citation: Mancinelli D, Hallé C (2015) Nano-Filtration and Ultra-Filtration Ceramic Membranes for Food Processing: A Mini Review. J Membra Sci
Technol 5: 140. doi:10.4172/2155-9589.1000140

Page 3 of 13

Organic fouling [15-17]: is generated by the deposition or prior NF process steps [36,37] or reverse osmosis [38].
adsorption of dissolved organic materials [18]. Some of the organic
Flocculation and adsorption methods [39].
materials typically involved in such processes can have a biological
origin such as proteins or polysaccharides [19]. The hydrophobic Oxidating agents such as H2O2 or UV which showed potential for
fraction of natural organic material (NOM) present in water was found certain type of pesticides and hydrogen sulfide removal, mitigation of
to be one of the major factors causing permeate flux reduction when flux decline, and improvement in membrane cleanability [40].
processing water [20].
The cleaning procedures of the membranes play a very significant
Colloidal fouling [21]: is generated from the accumulation role in the overall process performances and must be optimized based
of particles and colloidal matter. The materials involved in such not only the surface composition but also depending of the type of feed
phenomenon can be organic colloids such as aggregated NOM and processed [41]. Chemical cleaning exploits chemical reactions [42]
proteins [22,23], or inorganic colloids such as colloidal silica, clay such as hydrolysis, solubilization, saponification, dispersion, chelation
minerals, metal oxides (Fe, Al and Mg), suspended matter, precipitated (example using EDTA [43]), enzymatic hydrolysis [44] or variation of
salts and organic colloids [21]. pH [45].
Scaling: Typical of NF or RO where the polarization concentration Cleaning techniques based on physical methods such as back-
of scarcely soluble salty molecules causes their precipitation on the pulsation and backflush [46,47], gas bubbling [48], ultrasounds [49,50]
membrane surface due to oversaturation of such compounds [24]. or the application of electric fields [51,52], can be combined with the
Examples of this type of salts could be calcium and barium sulfates, chemical cleaning methods in an attempt to prolong the lifespan of
calcium carbonate and silica scales [25,26]. the membranes and reverse at least partially the fouling phenomenon.
The determination of the cleaning requirements and frequency is of
Biofouling: It is generated by the growth of microorganisms with
critical importance for an efficient and robust filtration process. There
accumulation of extracellular materials on the membrane surface [27-
is evidence that cleaning at an early fouling stage is preferable to when
31]. Generally, more than one specific type of fouling is involved. For
the fouling layer is more compacted [53]. Normally the cleaning
example, the presence of organic fouling will enhance the biofouling
procedures are applied when the flux decline is higher than 10-30%
through accumulation of nutrients that bacteria can utilize to grow and
[12]. In some cases NF can be used with very rare cleaning steps when
proliferate [32,33].
subcritical fluxes are used [54], this is caused by the fact the smaller
Generally, more than one specific type of fouling is involved. For pore size of the NF membranes are less subjected to pore plugging than
example, the presence of organic fouling will enhance the biofouling UF and MF membranes [12].
through accumulation of nutrients that bacteria can utilize to grow and
proliferate [32]. Food application of UF and NF Ceramic Membranes
When the range of the membrane pore size reaches that of the The use of membrane technologies in the food industry gives
NF scale two phenomena become of particular interest for the overall advantages such as food safety [55], ease of cleaning and sterilization,
filtration performances: concentration polarization and osmotic and environmental friendliness [56]. They allow for a simplification of
pressure. The concentration polarization is generated from the retention the process flow sheets avoiding steps that are more complex or cause
of solutes on the membrane surface that causes the creation of a layer of chemical stress for the products [57]. They can contribute to the
where such molecules are much more concentrated if compared to the production of high quality foods and the creation of novel fractions that
bulk solution. Such increase in concentration can contribute to scaling, can be used for new type of dietary supplements allowing this industrial
gel layer formation and other fouling types with drastic reduction of sector to satisfy more easily the evolving consumer demand coming
the process performances [34]. The concentration polarization also from the markets [58]. This review considers as a food ingredient the
produces an increase of osmotic pressure at the membrane retentate drinkable water which is not only a fundamental component of many
surface side which creates a pressure force opposing the applied types of food products such as beverages but it is also a fundamental
transmembrane pressure (TMP) thus reducing the flow of the permeate. component of most of the processing steps necessary to arrive to the
Both phenomena can be reduced via the application of a cross-flow, final products.
which constantly reduces both the concentration polarization and the Drinking water
osmotic pressure generated.
Drinking water is a fundamental component of many food
The production costs of CM are still higher than the polymeric products, especially beverages and a critical component of most of
membranes (PM) and usually result in higher investment costs. food production processes. Many factors are contributing to the
However, the investment costs can be balanced by a reduction of constant increase in demand for drinking water such as population
operation costs due to several factors such as reduced need for growth, personal use increase, increasing presence of pollution
pretreatments of the products before the UF or NF steps [3], longer and contamination in the environment (especially concerning in
membrane lifespan, more efficient cleaning to limit the fouling [35] developing countries such as India, China, and the African continent)
and better sanitizing conditions [5]. [59], and reduced availability due to global warming effects such as
The fouling control and mitigation strategies must be optimized desertification or glaciers melting.
depending on the mechanisms and factors contributing to the specific The first publication testing CM operating in the UF range
case taken into consideration. They often consist on pretreatment was released during the year 1997 [60]. The tests compared the
methods or cleaning procedures. performance of two UF ceramic membranes to filter the raw waters
Examples of pretreatments methods can include: of the Muskan Lake (in Sweden) which contains high color content
of mostly humic substances (up to 100 mg Pt/l) as well as odor and
pressure-driven methods such as pretreatment with MC or UF taste problems particularly during the algae blooming period. The two

J Membra Sci Technol

ISSN:2155-9589 JMST an open access journal Volume 5 • Issue 2 • 1000140
Citation: Mancinelli D, Hallé C (2015) Nano-Filtration and Ultra-Filtration Ceramic Membranes for Food Processing: A Mini Review. J Membra Sci
Technol 5: 140. doi:10.4172/2155-9589.1000140

Page 4 of 13

CM were produced by SCT (France) and were coated with an active

layer of zirconia oxide with 50 nm and 100 nm pore size respectively.
The equipment was operated in cross-flow set up producing a permeate
flow of 600 L/h m2Bar and stable conditions with a 50 nm pore size
membrane up to a volume reduction factor of 20. The water produced
with the use of the UF membranes contained between 3 and 12 mg/l of
total organic carbon and a color ranging between 8 and 45 mg Pt/l. The
PM, which could operate on the NF range, contained a significantly
reduced amount of humic substances probably due to their lower
molecular weight cut off (MWCO) with less than 1 mg/l of total
organic carbon (TOC) and 1 mg Pt/l or less of color. This fact leads Figure 3: Mean value of flux with different membranes at 6 bar [1].
the researcher to conclude that the UF ceramic membranes were not a
suitable option this application. Figure 2 shows the results obtained in The tests were performed at 6 bars. These new membranes were
terms of flux with ceramic membranes. It would have been interesting tested and compared with unmodified TiO2 ceramic membranes as
to test and compare how CM with MWCO in the range of the NF would a pretreatment for the traditional reverse osmosis (RO) processes.
have performed in comparison with a PM of comparable MWCO. The goal was to increase the process efficiency and reduce the energy
requirements. Figure 3 shows a comparison between the fluxes (J) of
More recently, a highly integrated hybrid process was tested for the
some of the membrane tested.
treatment of micro-polluted raw water in order to produce drinking
water [59]. The superior physical and chemical stability of the CM is The unmodified ceramic membrane achieved a total dissolved
compared with PM. CM is integrated into one unit of the coagulation, solids rejection of about 5%, while the Pt-impregnated and the Ag-
ozonation, and filtration [59], replacing conventional sedimentation impregnated membranes had respectively a 22% and 29% total
and sand filtration processes. This configuration allows for a significant dissolved solids rejection. The rejection considering only the salt
reduction of the treatment time and footprint of the plant. This technique content of the seawater was respectively 17% and 24%. Their rejection
was able to achieve high performance with less land occupation and was not significant with monovalent ions such as Na+ but it was much
lower costs compared with the conventional processes. The results greater with divalent cations. The Ca+2 was rejected with about 60%
of the tests were encouraging with >99% reduction of turbidity from efficiency from both modifications while in the case of Mg+2 the two
the raw water, and an excellent rejection performance of the CM. The membranes expressed significantly different rejection values with 80%
filtration module was provided from Meidensha Corporation (Tokyo, rejection for the Pt-impregnated membrane and 65% rejection with the
Japan) with 60-70 nm average pore size. Ag-impregnated membrane. The reduction of biofouling appeared to
be satisfactory due also to the fact that especially Ag+ has antibiotic and
NF polymeric membranes were initially developed as an ultra-
bacteriostatic properties [64].
low pressure tool for the removal of hazardous organic contaminants
present in water, color or as water softeners [61-63]. Dietary fats
The Centro de Estudios Académicos sobre Contaminación CM can be employed in the oil industry with potential gains in
Ambiental (CEACA), Santiago de Querétaro, published the first NF terms of both productivity as well as reduction of production steps.
application to seawater and brackish water desalinization [64] that They can be applied directly to crude oils or to their miscella in
used CM. The test used seawater taken from three locations: Playa combination with organic solvents.
Blanca, San Jose del Cabo and Holbox. Analysis showed that the three
samples had very similar parameters. They used modified ceramic NF In 2002, Alicieo et al. [65] investigated the use of a UF ceramic
membranes coated with TiO2 that were impregnated with reduced membranes with pore size of 10 nm directly on the crude soybean oil
Ag or Pt metals. The membranes were tubular mono channel with a with the aim of purifying it from some undesirable components such
contact surface of 0.0047 m2 and a MWCO of approximately 5 kDa. as phospholipids, free fatty acids, pigments, sterols, carbohydrates,
proteins and their degradation products. One advantage offered from
the application of the CM if compared to the PM is their thermal
stability, which allows for the use of higher temperatures during the
process reducing considerably the viscosity of the oil. In this case,
a high level of rejection was achieved for most of the mentioned
components [65]. They achieved a rejection of 54, 45% for the free
fatty acids, 97.91% for soaps, 99.14% for the phospholipids, and 42%
reduction in color. The filtration conditions were 6 Bar pressure at
50°C in cross-flow configuration, a value of 4, 16 Kg/m2h was achieved.
More details on the flux compared with time of the process are shown
in Figure 4. During the study, the ceramic membrane was compared
with a polysulphone hollow fiber membrane provided from AIG
Technology Corporation (MWCO of 100 kDa). The results showed a
higher rejection for the undesired contaminants to be removed from
the soya oil in the case of the ceramic membrane but a lower flow rate
when compared to the polysulphone hollow fibers. It is reasonable to
Figure 2: Flux vs volume reduction factor for the SCT ceramic membranes. attribute such differences in performances mostly to the pore size of
Avera pressure 0.1 MPa [1].
the two membranes.

J Membra Sci Technol

ISSN:2155-9589 JMST an open access journal Volume 5 • Issue 2 • 1000140
Citation: Mancinelli D, Hallé C (2015) Nano-Filtration and Ultra-Filtration Ceramic Membranes for Food Processing: A Mini Review. J Membra Sci
Technol 5: 140. doi:10.4172/2155-9589.1000140

Page 5 of 13

alumina layer. This could be an interesting advantage if compared with

most PM, which tend to become unstable in the presence of organic
solvents or swell up sensibly and decrease their permeability. The test
showed promising performances in terms of flux and process stability
but the rejection was around 20% of the initial values to decrease to
lower values as the concentration of the triglycerides increased. The
reason of the significantly low yield obtained was the use of a too large
pore size membrane. It would have been interesting to have a test of
this technique utilizing a NF ceramic membrane type.
The solubilization of crude oil into organic solvent could be
used to remove phospholipids (degumming), and other undesired
compounds from a crude oil. In a paper from 2008 [69], a miscella
of corn oil solved into hexane was ultrafiltrated with an alumina
multichannel ceramic membrane with an average pore size of 50 nm
at a temperature of 40°C. The miscella contained between 25% and
35% w/w of crude oil. Such concentrations of organic solvent were not
sufficient to reduce drastically the formation of heavy micelles, which
Figure 4: Permeate flux at 50⁰C with ceramic membrane [1]. did not permeate through the membrane. Surprisingly the tangential
velocity had a greater influence on the permeate flux than the TMP. A
higher percentage of crude oil into the miscella favored the retention
More recently, a similar process was tested in order to degum and of phospholipids (PL) while negatively influenced the permeate flux.
remove waxes from sunflower oil [66]. A ZrO2 activated layer ceramic In a test 35% w/w of crude corn oil was ultrafiltrated with a tangential
membrane on α-Al2O3 with pore size of 100 and 20 nm were tested. As velocity of 2,4 m/s, 40°C and 1.5 Bar TMP, achieving a 93.5% w/w
predicted, the filtration with the lower pore size membrane gave better rejection of the phospholipid content and a flux of 65,8 Kg/m2 h which
results in terms of rejection with 97% rejection of the phospholipids according to the comments was considered a promising result.
at 2 bar pressure. The crude oil presented a high viscosity due to the
The CM could offer a substantial reduction of energy consumption
presence of various particles and a relatively high level of waxes.
if combined with supercritical fluid extraction. It could offer the
According to the authors [66] a multi UF step was necessary with larger
possibility of recovering the liquid CO2 separating it from the substrate
porosity size as a pretreatment in order to increase the productivity of
being extracted without the decompression and recompression phase
the technique so that this method could offer advantages in terms of
which plays a significant role in the total energy requirements of this
economy and environmental friendliness of the process.
technology. It appears that several research groups have recently
The CM could also be applied to recover the product contained in started to test the feasibility of this technique. A paper published some
an organic solvent extract, substituting at least in part the evaporation preliminary results produced with a supercritical fluid extraction set
processes necessary to remove the solvent from the non-volatiles, which up where the liquid CO2 was combined with different components
is a stressful and energy consuming process. With improvement of the typically present in these type of applications, including oils composed
product quality and reduction of the energy consumption of the overall by triglycerides [70]. The ceramic NF membrane consisted of a layer of
process, In 1999 a publication described an experiment concerning TiO2 deposited on a ceramic support. The MWCO of the membrane
soybean oil extracted with hexane [67]. The goal was to test the in the tested conditions was estimated to be at 800 Da, with an average
possibility of recovering part of the solvent via UF, reducing the energy pore size of 0.9 nm. In one experiment, a trimyristin oil, with a
costs of its recycling through evaporation. This allows for a reduction molecular weight (MW) of 723 Da, was nanofiltrated in the presence
of the total energy consumption for the process as well as a reduced
stress imposed on the substrate during its production, improving the
final product’s characteristics [68]. The extract was directly collected
from the solvent extractor without refining. It typically contained near
33 wt% of soybean oil, 0.6 wt% of phospholipids and less than 0.1 wt%
of free fatty acids. The experiment performed at room temperature
employed a porous alumina anodisc of 47 mm in diameter. The pore
diameter of the top layer was 20 nm with a thickness of about 1 µm.
The permeate flow was recycled back to the 5 L reservoir, which was
sufficient to keep a constant concentration in the recycled retentate.
During the first 2 hours, the flux changed rapidly. Therefore, separation
data were acquired after 2 hours of permeation when a clean membrane
was used. Figure 5 shows the recorded parameters obtained during the
tests.
When pure hexane was used, there was no readable transmembrane
pressure even at the maximum feed rate of the pump (about 40 ml/
min). This is a clear sign that the filtration via CM of non-polar
solvents is strongly dependent on the liquid viscosity and there was
no noticeable structural modification at the level of the pore size of the Figure 5: Permeation with various transmembrane pressures [1].

J Membra Sci Technol

ISSN:2155-9589 JMST an open access journal Volume 5 • Issue 2 • 1000140
Citation: Mancinelli D, Hallé C (2015) Nano-Filtration and Ultra-Filtration Ceramic Membranes for Food Processing: A Mini Review. J Membra Sci
Technol 5: 140. doi:10.4172/2155-9589.1000140

Page 6 of 13

of hexane as a co-solvent at a pressure of 150 Bar and a temperature of

333 K achieving a rejection of 98%. The permeate flux decreased only of
about 20% and recovered nearly completely within a few minutes after
the injection of the substrate was stopped [70]. In another interesting
test, oil was nanofiltrated. The triglyceride oil contained about 25 wt%
of each of the following components: tricaprin (MW 554 Da), trilaurin
(MW 639 Da), trimyristin (MW 723 Da) and tripalmitin (MW 807
Da). The membrane exhibited a selective permeability. The smaller
molecules (in particular tricaprin) showed a greater permeability,
producing a permeate fraction highly enriched of tricaprin which
doubled in concentration from the initial values if compared with the
feed composition as illustrated in Figure 6. This type of selectivity could
play an important role in the production of high quality oils enriched
with high molecular weight triglycerides, highly unsaturated with
reduced content of low MW triglycerides, free fatty acids and other
contaminants that would not require a winterization process.
Figure 7: Time evolution of permeate flux in the first step: experimental (◊) and
In conclusion these initial tests illustrate how important are the
calculated (-) values [1].
specific interactions between the membrane surface and the substrates
which can be adsorbed on it or flow through the nano-pores with
different velocities. The pressure of 150 bar used in the set up appears
to be on the lower end of the standard extractions performed in the
food industry which are typically around 200-400 bar or even higher
in case of co-solvent extractions [71]. It can however be regarded as a
promising sign that this direction could lead to energy efficiency gains
in this type of processes.
Sugar and carbohydrates
The sugar industry is emerging as another field where CM could
innovate, increasing efficiencies, waste products recovery and help to Figure 8: Calibration with (a) water and (b) cumulated permeate from the first
develop novel food supplements. step of 1 kDa ceramic membrane [1].

Two publications showing the use of UF and NF ceramic membranes

for the purification of oligosaccharides recovered from caprine milk
that could be used for the production of infant milk formulas [72,73] of the module was 50 kDa. More than 98% of the lactose and the
were recently published. It is well documented that the goat milk has oligosaccharides were eluted after 4 diavolumes, while 94% of the
a very similar carbohydrate profile to the human milk [74]. They help original protein content was retained together with 76% of the calcium
protecting infants from pathogens [75] as well as helping the correct which was probably linked to the large casein micelles. The flow during
development of the bifidogenic flora typical of breastfed children [76]. the UF decreased probably due to fouling as shown in Figure 7.
The tests employed a double step filtration via CM. The second step was performed with a ceramic membrane of the
The objective of the first step was to retain the protein fraction, same dimensions but smaller pore size and a MWCO of 1 kDa. The aim
separating it from the oligosaccharides and lactose fraction that were of this step was to concentrate the oligosaccharides in the retentate and
able to permeate. The membrane employed an INSIDE CéRAMTM reduce the concentration of lactose and salts that permeated through
module (TAMI Industries, Lyon, France) made of ZrO2-TiO2, 25 cm the membrane. The flux through the membrane with pure water and
long, three channels and a membrane area of 94 cm2. The MWCO with the permeate coming from the first step demonstrated to be
correlated with the pressure as shown in Figure 8.
In order to avoid an excessive compaction of the fouling layer,
the transmembrane pressure was selected at 150 kPa. After the 10 h of
continuous operation the flux of the permeate decreased from nearly 30
to about 20 l/m2 h, then stabilized as illustrated in Figure 9, suggesting
that the fouling did not affect the sieving properties of the membrane
for the lactose and calcium.
The permeation of the calcium and lactose was good, after 3
diavolumes 94% of the lactose was eluted. During the second filtration
step 82% of the initial oligomers were recovered while most of the
lactose and calcium were removed as shown in Figure 10.
During the same year another paper was published describing a
ceramic membrane set up used for the separation of non-sucrose
Figure 6: Comparison of triglyceride mixture composition between
feed and permeate; membrane sample 5, 125 bar feed pressure, compounds from syrup as a part of the sugar-beet processing [77].
ΔP = 15 bar, temperature 323 K [1]. White sugar has to satisfy rigorous demands for quality, particularly

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Page 7 of 13

30% greater change compared to NSM-mode configuration. At the end

of the process, the difference was significantly greater when it reached a
65% improvement compared to the NSM-mode process.
Some years later another publication concerning this type of set
up obtained very similar results, this type of static mixer technology
was used with a 20 nm pore diameter ceramic membrane composed by
a layer of zirconium oxide deposited on an aluminum oxide support
[78]. A purity elimination of 80% on average compared to the feed was
achieved. The static mixer appeared to have a significant impact on the
permeate flux through the membrane at 80°C only when the cross-flow
was below 150 L/h. At higher transmembrane pressure, the effect was
less marked as illustrated from Figure 11.
The production and purification of xylo-oligosaccharides (XO)
is a very expensive and complex process comprised of several steps
Figure 9: Time dependent evolution of permeate flux in the second step: [79], which often include HPLC purification technology, in order to
experimental (◊) and calculated (-) [1].
reach a sufficient level of purity. The range of 75 – 95% purity is of
critical importance for their use as food additives, pharmaceuticals, and
nutraceuticals [80]. The possibility of employing ceramic membranes
in the NF range was investigated from a paper, which tested the use of a
monolithic module Kerasep Nano (from Novasep) with 1 kDa MWCO
[79].
Rise husk was obtained from a local factory (Procesadora Gallega
de Alimentos, Lalin, Pontevedra, Spain), air-dried, homogenized and
analyzed for its content. The dry material was mixed with a ratio of
1:8 w/w with water in a Parr reactor. Applying the standard heating
temperature profile, the maximum xylooligomer concentration was
reached exploiting its auto-hydrolytic activity [81]. The liquors were
recovered by filtration and further processed after being analyzed for
their content.
The liquors were initially filtrated with a 0.45 µm membrane
in order to remove particulate material. Then tested with three
Figure 10: Evolution of the normalized retentate concentration for
oligosaccharides (●), protein (■), lactose (□), and calcium [1]. modules of ceramic membrane coated with TiO2/ZrO2: Membralox
Ti-70 1000 with 1 kDa MWCO (Pall), Membralox Ti-70 5000 with
those concerning its color. The non-sucrose compounds with intense 5000 kDa MWCO (Pall), and Kerasep Nano with 1 kDa MWCO
color tend to be incorporated into the sucrose crystals during the (Novasep). All experiments were carried out at room temperature.
purification process, especially if the purity of the beet is poor. Some of The initial composition of the liquors was about 2.55 wt% of non-
the advantages of the application of a UF step in the proper conditions volatile compounds of which about 42.47% were composed of xylo-
and the use of a membrane with adequate characteristics are high oligosaccharides. During the tests, several PM were tested as well. The
purity and low color of the ultrafiltrated syrups, absence of starch and first observation was that the CM had up to three fold higher flow rates
acid substances, and drastic reduction of environmental pollution. It (J) even when compared with PM that had higher MWCO ranges (at
was also observed a faster crystallization if compared to conventionally least declared from the producer). Figure 12 shows the results of three
purified syrups. The cross-flow filtration system was connected to tests performed with two PM (a and b) and a ceramic membrane.
a tubular ceramic membrane whose pore diameter was 5 nm. The
membrane consisted of a titanium oxide layer coated on alumina The permeate flux obtained with the test of the Kerasep Nano
support. The membrane was single channel, 250 mm long, with 6.8 monolithic module increased in a linear proportion up to 10 bar . The J
mm inner diameter. The useful membrane surface was 4.62 × 10-3 m2.
The effect of the turbulence promotion on the filtration performances
was investigated by the use of a static mixer. The tests were performed
with a temperature of 70°C and 80°C but the results reported on the
publication concerned only the 80°C tests.
The conclusions were that the static mixer contributed to an
increase of the fluxes in most of the ultrafiltration phases. The highest
flux achieved in the presence of the static mixer (SM-mode) at the
beginning of the operations was approximately 35% greater than
the flux in non-static-mixer mode (NSM-mode). The difference was
even greater at the end of the process, when it reached a 45% increase
compared to the NSM-mode UF.
In terms of color changes, the static mixer achieved a maximum of Figure 11: Flux as a function of tangential flow rate at 80°C [1].

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Page 8 of 13

gives a summary of the results of the tests performed at 8 bar pressure;

the values included in the highlights are regarding the mentioned
membranes.
The best performances in terms of flow and fractionation effect
were obtained from Kerasep Nano and ESP04 (its surface was
chemically modified via addition of metal salts to the polymeric matrix
which changes the surface negatively and this can attenuate its fouling
tendency). Kerasep Nano at 8 bar pressure was able to express higher
fluxes about the double of the ESP04 and a better purification effect
because able to reject with comparable efficacy the oligosaccharides but
retaining less efficiently of the monosaccharides.
Proteins
The possibility of employing membrane technologies in the
recovery of proteins discharged from several industrial processes into
the environment is very attractive for such industries because it opens
to the possibility of increasing the range of products that can be offered
and reduces waste treatment costs.
The first publication about the use of CM for this type of food
processes was found in 2003 [2]. The test was about the possibility
of recovering fish proteins contained in the wastewaters of Chilean
Figure 12: Time dependence of the permeate flux obtained with the (a)
ESP04, (b) PU608 and (c) Kerasep Nano NF membranes, operating at fishmeal industries.
selected transmembrane pressures (○ – 2 bar; ■– 4 bar; ♦ – 6 bar; □ – 8 bar;
The tests employed a Kerasep Nano01A (made in Orelis from
“filled triangle” – 10 bar; ● – 12 bar; Δ – 14 bar) during the processing of raw
autohydrolysis liquors. Feed velocity, 2 m/s for the UF membranes and 3 m/s Rhodia) based on TiO2 deposited on a Al3O2 – TiO2 support. The
for the NF membrane, 26 ± 4°C), [1]. tubular membrane had 19 channels of 2,5 mm, 856 mm length, with
a total area of 0,1277 m2 and a MWCO of 1 kDa. The pilot plan used
for the tests was assembled by Rhodia. A sample of 30 L was collected
from the wastewaters generated from a fish meal factory located in
Talcahuano, Chile. It was filtrated through a battery Omnifilter MF
cartridge of pore sizes 80, 20 and 5 µm, then stored in a refrigerator at
4°C. It was observed that this filtration was not sufficient to produce a
clear permeate liquid and it was recommended the use of a smaller pore
size Omnifilter MF cartridge for future tests. The NF operations were
carried out with a pressure ranging from 3 to 5 bar with a cross-flow
velocity ranging from 2 to 4 m/s (at 5 bar pressure the flow velocity of
4 m/s was not reached for pump flow limitations). The permeate was
circulated back into the feed tank in order to minimize concentration
changes in the retentate. The permeate flux, J, was measured at the
beginning of each experiment and after 15 minutes of operation. After
a first testing phase the pressure of 4 bar and cross-flow of 4 m/s were
chosen as optimal experimental conditions for the NF tests.
The membrane flux rapidly decreased to 21% of the pure water
values of J (Jw), probably due to a strong adsorption of the proteins on
the membrane surface and/or formation of a dynamic membrane layer
on top of the ceramic layer. As the VRF increased, a smooth decrease
Figure 13: Effect of pressure on the permeate flux obtained during membrane to 16% of Jw was observed. After a complete washing procedure with
processing of raw autohydrolysis liquors (feed flow velocity, 2-3 m/s; basic and acid washing solutions, the J of the membrane was recovered
temperature, 26 ± 4°C). ● – PCI AFC30; “filled triangle” – osmonics DL2540;
Δ – PCI ESP04; ♦ PCI PU608; ■ – Kerasep Nano; ○ – Pall membralox 1 kDa;
to its initial values (Jw). The Figure 14 illustrates the behavior of the
□ – Pall membralox 5 kDa [1]. protein rejection in relation to the volume reduction factor (VRF) and
the observed flows. It had an initial value of 69% and increased to 82%
when a value of 5 in the VRF was reached. Fouling was detected and
was constant and presented no reversible fouling during the utilization the flux could not be recovered back to the initial values until proper
when the TMP was lower than 8 bar as it can be seeing in Figure 12c. The chemical washing was applied.
results showed that the transmembrane flux limit for this membrane
was 40 L m-2 h-1 (around 8 bars), higher pressures produced fouling The extent of the fouling and its limitation in a continued operation
and gradual loss of performances. In Figure 13 a comparison between set-up needed to be further investigated.
tested membranes polymeric and ceramic types can be observed. Most Very recently a new application for ceramic membrane was tested
of the membranes that demonstrate high initial J values appear to suffer and published concerning protein recovery from shrimp shells [82]
also from a higher reversible fouling when the TMP increases. Table 1

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Page 9 of 13

Membrane J (L/m2 h) at 8 bar R R Fouling

oligcmccharides (%) monosaccharides (%) (% MVP)
Nanomax 95° xr.100 xr.100

AFC30 6.1 99.7 80 33

DL2540 8 99.4 76 20
Kerasep 40 93 5 40
Nano  

Membralox T1-70 1000n 34 78 7 60

ESPO4 21 93 10 65
Mcmbralox 47 70 4 63
TI -70 500 (rPU608) 15.7 84 5 75
Fouling was measured by percent reduction in pure water flux.

a Data at 6 bar.

b Data at 20 bar.

Table 1: Comparison of membrane performance (flux, fouling and rejection) during the processing of the raw autohydrolysis liquor. The tests were performed at 8 bar.
Fouling results are reported as pure water flux drop (PWF), [1].

larger protein molecules accumulating on the surface of the UF

membrane created a secondary filter layer that increased the rejection
from the initial 30% to over 90%. If this hypothesis was confirmed it
would be interesting to test the use of a NF ceramic membrane that
could reject directly the majority of the proteins and maybe reduce
the formation of the secondary filter layer with flow and performances
benefits.
Fermentation broth products
The possibility of combing emerging technologies such as NF with
Figure 14: NF of microfiltrated fish meal effluent (membrane Kerasep
other techniques can offer opportunities concerning the production of
NanoN01A, T=23°C, pH 6,3). R is the rejection for the protein fraction expensive but important ingredients for the food industry. For example
expressed in % w/w compared to the starting material [1]. in the production of fermentation products such as lactic acid or
succinic acid, the production of lactic acid via fermentation is complex
and requires many purification steps [84]. Duke et al., [85], proposed a
which compose 18-42% of the shell wastes produced from the industrial
simplification of the process for the enrichment of lactic acid. Two type
processing of crustaceans and could be recovered during the process of
of CM were prepared. One was a γ-alumina ceramic membrane with
production of chitin [83].
average pore size of about 4 nm, the other was composed by a support
Shrimp shells from a seafood restaurant from the species P. of γ-alumina coated with silica with a pore size of about 0.3 nm. The
longirostris were washed under running water in order to remove separation was performed in a pervaporation set up where the liquid
soluble organics, adherent proteins and other impurities. Then contacted with the membrane was converted into vapor under vacuum
they were boiled in water for about 1 h in order to remove their soft as it penetrated through the membrane. The tests were performed at
tissues. The obtained shells were dried in an oven at 160°C for 2 h and 25⁰C; a downstream vacuum pump induced the vapor phase, which
finally crushed into a fine powder. Finally, the dried shells powder permeated through the membrane. In order to simulate an actual
was mixed with an alkaline solution of sodium hydroxide in order fermentation medium a starting solution was prepared containing 15
to extract the removable protein fraction from the shells and create wt% of lactic acid (LA) and 0,1 wt% of glucose.
the protein-water solution to concentrate via UF [82]. The protein
The results of the tests showed that the γ-alumina ceramic
concentration experiments were carried out using 130 S UF pilot unit
membrane had a lower value of rejection if compared to the coated
(Gamma filtration company, France) equipped with a Membralox-
version with silica. The Figure 16a shows that the rejection of the
Ceraver module. This module was a multi-channel ceramic membrane
γ-alumina ceramic membrane reduced as the concentration increased.
composed of ultrafine porous ZrO2 with 50 nm pore size coated on a
Figure 16b shows that when the coated silica membrane was used the
porous alumina support (15 µm). Total filtration area was 0,2 m2. Every
rejection values improved as the concentration increased.
test used 5 L volume of shell-proteins water which was concentrated
to 2,1 L over a period of 50 minutes. The rejection coefficient of the The flux was more than one order of magnitude higher with the
filtration increased from the initial value of 32% to over 90% after about γ-alumina ceramic membrane though it decreased much faster than
30 minutes as illustrated from Figure 15a. The flow decreased to about the silica-coated membrane. The scientists working on these tests
64 L m-2 h-1 from an initial value of 160 L m-2 h-1 as illustrated in Figure produced their own theoretical models about the working mechanisms
15b. of two membranes, which might differ under some points of view;
Figure 17 illustrates the proposed mechanisms.
A possible explanation for the flux reduction before stabilization
after about 25 minutes from the beginning of the experiment is that The conclusion was that these initial studies were promising but

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Figure 15: a) Rejection coefficient % at U = 6 m/s, P = 3 bar; b) Jvat U= 6 m/s, P = 3 bar [1].

Figure 16: a) Pervaporation test performed with γ-alumina ceramic membrane at 25°C. Startup concentration of 15 wt% LA and 0.1 wt% glucose [1];
b) Pervaporation test performed with silica coated ceramic membrane at 25°C. Startup concentration of 15 wt% LA and 0.1 wt% glucose [1].

a) b)

Figure 17: a) Mechanism of surface interaction and diffusion of water and LA within the pores of γ-alumina at the beginning of the permeation (left)
and after steady state (right). b) Mechanism of surface interaction and diffusion of water and LA within the pores of the molecular sieve silica at the
beginning (left) and after steady state (right). [1].

more tests were needed in order to improve the overall performances electrostatic interaction or molecular sieving effect. NF using CM
of the process. might have a useful application in this sector. The separation and
concentration of succinic acid from a multicomponent aqueous
Another very important fermentation product is the succinic
solution was explored in terms of simple enrichment via NF with CM
acid, which can be produced from microbial bioconversion of the
[86]. The tests were performed with a tubular ceramic mono-channel
glycerol. There is growing interest in this type of technologies because
membrane coated with TiO2 provided from TAMI Industries (France),
the amount of waste glycerol produced from biodiesel conversion is
with a MWCO of 450 Da and an effective surface of 0.0125 m2. All the
increasing in recent years [86].
experiments were carried out at room temperature and at a TMP in the
The succinic acid has important applications in the food, range of 0.5-1.5 MPa. The composition of the solutions used for the NF
pharmaceutical and chemical industries (production of bioplastics). experiments is shown in Table 2.
It has gained a growing interest as a renewable building block
After the completion of a NF test the permeability of the membrane
for chemical products such as 1, 4-butane-diol, tetrahydrofuran,
to water was tested, verifying the presence of irreversible fouling on
polybutylene succinate (PBS) and other chemical compounds [87].
its surface. The permeability reduction was completely removed after
One of the challenges to overcome during its production is the
the washing procedure suggested from the producer. The results of the
isolation of the compound from other fermentation molecules. In case
tests performed with the different solutions are illustrated in Figure 18.
of separation of weak dicarboxylic acids such as the succinic acid, it is
important to consider that also factors like pH play an important role The pH and the presence of other components in the solution
in their separation efficiency. The capacity of the membrane to reject appears to produce an effect on the performances concerning both the
these compounds and the mechanisms by which such compounds permeate flux as well as the retention performances. An increase of
are rejected are strongly influenced from the mentioned parameters: the applied pressure produced generally a reduction in the retention

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Solution number pH Components of solution

a)   1% Succ
1 <28
b)   3% Succ
a)   1% Succ + 0.1% Cit
2 <28
b)   3% Succ + 0.3% Cit
3 <2.8 a) 1% Succ + 0.1% Ac
a)   1% Succ + 0.1% Cit ÷ 0.1% Ac
4 <28
b)   3% Succ + 0.3% Cit + 0.3% Ac
a)   1% Na2Succ
5 > 10
b)   3% Na2Succ
a)   1% Na2Succ + 0.1% Na3Cit
6 >10
b)    3% Na2Succ + 0.3% Na3Cit
7 >10 a) 1% Na2Succ + 0.1% NaAc
a)    1% Na2Succ + 0.1% Na3Cit + 0.1% NaAc
8 > 10
b)    3% Na2Succ + 0.3% Na3Cit + 0.3% NaAc
Table 2: Characterization of the solutions used for the NF tests [1].

Figure 18:a) Permeate flux NF of acid solutions after 20 minutes permeation; b) Permeate flux NF of salt solutions after 20 minutes permeation; c)
Retention of acid solution components after 20 minutes of permeation; d) Retention of salt solution components after 20 minutes permeation [1].

of succinic acid during the NF of the acid solutions (except in the case its applications are gradually increasing. Nevertheless, a lot of work
of the NF of the solution 4a), while in the salt solution the retention and development are still necessary to allow this type of application to
of the succinic salt didn’t follow a clear trend. The best retention compete with more mature technologies. Particular effort is needed on
percentage was obtained from the NF of the solution 8a at a pressure understanding and reducing the membrane-fouling issues in order to
of 0.4 MPa. It appears clear that the difference in retention between allow gains in productivity and process robustness. A limited number
the acid and the salt solutions does not depend on the sieving effect of of scientific papers are available on industrial applications of UF or
the membrane itself but from a polar repulsion between the membrane NF ceramic membranes in combination with solvent extraction or
surface (negatively charged) and the negatively charged molecules of any type of solvent treatment in the food processing industry. Some of
the Na2-succinate salt. Another possibility to consider, might be, that them routinely employ solvent extraction and might be interested to
the Na2-succinate salts molecules organized with Na-Ac and Na-citrate investigate this technology for possible integration into their processes
salts to form larger agglomerates that were retained more efficiently. in order to reduce their environmental impact, gain in energy efficiency,
product quality, and produce novel products.
Conclusions
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Citation: Mancinelli D, Hallé C (2015) Nano-Filtration and Ultra-Filtration Ceramic Membranes for Food Processing: A Mini Review. J Membra Sci
Technol 5: 140. doi:10.4172/2155-9589.1000140

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Development of Pressurized Extraction Processes for Oil Recovery from Wild

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