Crystallisation Technology
Crystallisation Technology
Crystallisation technology
Table of Contents
Executive Summary - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 3
Introduction to SPX Flow Technology - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 3
Vision and commitment- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 3
Customer focus - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 3
Introduction to crystallisation technology - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 4
Margarine production - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 4
The fat phase - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 4
Crystallisation of fat - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 5
Minor ingredients in the fat phase - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 6
The aqueous phase - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 6
Low fat spreads - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 7
Emulsion preparation - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 7
Crystallised fat products - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 7
Trans fatty acids - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 9
Quailty of margarine - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 9
2 Crystallisation technology_01_2011
Executive Summary Introduction to SPX Flow
Technology
Food companies today are like other manufacturing Vision and commitment
businesses not only focusing on the reliability and SPX's Flow Technology segment designs,
quality of the food processing equipment but also on manufactures and markets process engineering and
various services which the supplier of the processing automation solutions to the dairy, food, beverage,
equipment can deliver. Apart from the efficient marine, pharmaceutical and personal care industries
processing lines we deliver, we can be a partner through its global operations.
from the initial idea or project stage to the final
commissioning phase, not to forget the important We are committed to helping our customers all over
after-sales service. The SPX Flow Technology has the world to improve the performance and profitability
Gerstenberg Schröder installations in more than 110 of their manufacturing plant and processes. We
countries around the world. achieve this by offering a complete range of
products and solutions from engineered components
The objective of this paper is to describe the basics to complete process engineering and design of
in crystallisation technology and additionally explain complete process plants supported by world-leading
the interchangeability of fats and oils, including the applications and development expertise.
compounding and processing of margarine, spreads
and shortening. We continue to help our customers optimise the
performance and profitability of their plant throughout
its service life with support services tailored to their
individual needs via a finely meshed customer service
and spare parts network.
Customer focus
SPX Flow Technology develops, manufactures and
installs modern, high efficient and reliable processing
lines for the food industry. For the production of
crystallised fat products like margarine, butter,
spreads and shortenings we offer our Gerstenberg
Schröder solutions which also comprise process lines
for emulsified food products such as mayonnaise,
sauces and dressings.
Crystallisation technology_01_2011 3
Introduction to crystallisation technology
4 Crystallisation technology_01_2011
Puff pastry
However, certain technical limitations exist when
70 margarine combining one or more ingredients from the 3 groups.
60
50
Table The crystallisation habit, or polymorphism, of the used
margarine
40 fat can set limits on the proportion of the particular fat
Frying
30 used in the blend. In addition, the crystallisation rate
margarine
20
10 Soft table of the fat blend is of great importance in the regard
margarine
0 to the set up of the plant, in other words how much
10°C 20°C 30°C 40°C Low fat
margarine
resting or holding time in the equipment the emulsion
needs in order to be fully crystallised by the end of the
The ingredients used in the formulation of the fat processing line.
blend can be derived from any animal, vegetable or
marine oil source. The choice of fats will depend on Crystallisation of fats
legislation, economics, quality, functionality and
on marketing constraints. The latter can limit the Fats tend to crystallise in various forms having
interchangeability of fats if e.g. 100% vegetable- or different melting points. Each of these crystalline
as now when low trans fatty acid margarines are in forms with their respective melting point are called
market demand. In addition, the availability of fats can polymorphs and the phenomenon is called
be limited due to legislation, religious prohibitions, or polymorphism.
trade barriers. The triglycerides exhibit, with some exceptions, three
It is possible to divide ingredients into three main basic crystalline forms designated alpha (α), beta
categories: liquid oils, semisolid fats, and hard stocks. prime (β‘), and beta (β).
A suitable blend can be made by combining one or In general, transformations take place in the order:
more ingredients from each of the three groups. Later α -> β‘ -> β
some recipe examples of margarine, spreads and fat
products will be shown. The transformations are irreversible except by
melting and re-crystallisation. It is possible that the
Liquid oils are considered to be completely transformation from one polymorphic form to another
interchangeable as components of margarine takes place in the solid state without melting. This
and shortening blends due to the modern refining transformation will only take place in the direction of
processes. Fat modification processes, such as a more stable form, seeking the most compact crystal
fractionation, hydrogenation, and interesterification form and the lowest thermodynamic energy state
enable a high degree of interchangeablity among fats. possible.
The modification processes produce, individually or
in combination, the full range of fatty intermediates The different polymorphs can be coexisting in the fat.
used in the manufacture of all types of margarines These different forms show melting points depending
and these processes enable fats to become almost on the cooling and heating history of the fat. Due
completely interchangeable. to a so-called crystal memory, crystalline structure
is preserved even though the fat is melted. This
SEMISOLID structure will affect crystallisation directly, especially
LIQUID OILS HARD STOCKS when the rate of cooling is high. Polymorphic changes
FATS
Hydrogenated Hydrogenated in the margarine may lead to a grainy structure.
Unsaturated
vegetable oils, vegetable oils,
vegetable oils When cooling the melt, α crystals are generally
MP: 32-34°C MP> 40°C
formed, but this form is never stable in triglycerides
Hydrogenated
Palm olein marine oils, MP:
Interesterified and transformation to β‘ is a reality. In most cases, β‘
blends, MP>40°C crystals are relatively slowly transformed to the stable
32-34°C
Palm kernel Palm Beef tallow
β form. The time of transformation from one crystal
form to another depend on the composition of the
Coconut Lard Palm stearin
triglycerides and the presence of diglycerides in the
fat blend. However, some fats possess both β‘ and β
forms, others only either stable b‘ form with no further
A particular product specification can be met by a
transition or stable β form.
large number of alternative formulations. The producer
attains the flexibility, in times of shortage or high cost, The literature states that the degree to which fats
to interchange the best available and cheapest raw will exhibit either β or β‘ tendency depends on
materials in an ever-changing market situation. The hydrogenation and depend to a lesser extent on
consumers are hereby certain to buy a product with blending factors. Also the palmitic acid content of the
continuously the same quality and price. fat seems to be responsible for exhibiting a particular
Crystallisation technology_01_2011 5
crystal habit. Fat containing relatively low amount of by saturated monoglycerides. If a blend of mono- and
palmitic acid (C16:0), approximately 10%, seem to be diglycerides is used, it is important to remember that
β tending, where fats with at least twice the amount in it is only the monoglycerides that have the emulsifying
general are β‘. effect and the total amount added should therefore be
larger than if a distilled monoglyceride was used.
Not only the amount of palmitic acid seems to
determine the crystal habit, but also the distribution Soya lecithin can be used with the emulsifier to
in the glycerol molecule. For instance, lard and tallow improve the effects of the emulsifier. To achieve the
contain approximately 24% and 25% palmitic acid maximum effect of the emulsifier-lecithin system,
respectively, but lard is β tending due to the high the emulsifier is heated with the lecithin and liquid
concentration of palmitic acid in the sn-2 position of oil before the mixture is dissolved in the melted fat
the glycerol molecule whereas tallow is β‘ tending blend. Additionally, lecithin reduces spattering in
because of sn-1,3 positioning. frying margarine, and it prevents burning of sediment
compounds (lactose and casein) since lecithin
The table below shows crystal habits of selected fats.
incorporate these compounds. Lecithin is also a good
β' TENDING FATS β TENDING FATS antioxidant.
Butter oil/milk fat Canola Fat soluble flavour and colour, e.g. butter flavour
Coconut Cocoa butter and β-carotene respectively, are added to achieve a
Cotton seed Corn product that tastes and looks like butter. In addition,
Modified lard Lard
β-carotene has pro-vitamin A activity.
Palm Soyabean Antioxidants can be added in order to improve the
Tallow Sunflower shelf life of the product, since these substances
can delay the onset or slow the rate of oxidation.
Source: Wiedermann In margarine production the following antioxidants
Apart from a few types of shortening the β‘ crystals can be added to the water or fat phase according
are the most desirable. They are relatively small and to solubility: natural tocopherols, BHA (Butylated
can incorporate a larger amount of liquid oil in the hydroxyanisole), BHT (butylated hydroxytoluene),
crystal network. β‘ crystals result in a glossy surface Ascorbic acid, and Ascorbic palmitate.
and a smooth texture.
The aqueous phase
The transition from the α-form to the β‘-form takes
place in the crystallisation equipment. All fats tend to The water phase differs depending on the type of
crystallise in the β‘-form when crystallisation takes margarine, thus it has a certain influence on the
place in a SSHE plant. Fats that are not stable in the finished margarine. It consists mainly of water in which
β‘-form due to its triglyceride composition will during the minor ingredients such as salt, preservative, milk
storage transform into the β-form. The rate of this protein and conceivably sugar are dissolved. Water-
transition is increased by temperature fluctuations. soluble flavour and colour can also be added, but are
primarily used in low fat spreads.
Minor ingredients in the fat phase
Salt is added primarily to improve taste, but also
Apart from the fat blend, the fat phase consists of to prevent growth of microorganisms. In frying
minor ingredients such as emulsifier, lecithin, flavour, margarine, salt helps to prevent spattering. The
colour, and antioxidants. These minor ingredients are amount added varies from 0.2% to 2.5%.
dissolved in the fat phase before emulsification. Citric acid is used to lower pH which means it acts as
Emulsifiers are surface-active compounds and are a preservative but additionally concerning puff pastry
used to reduce the interfacial tension between the margarine, the low pH will help give the finished
water and the fat phase. The emulsifier stabilises pastry a better lift.
the liquid emulsion before crystallisation to secure Other preservatives often used in margarine are
a homogeneous product and to achieve a finely benzoates and sorbates. They are most active at pH
dispersed and stable water distribution in order to around 4.5 which makes the advantage of adding
improve the microbiological keeping properties in the them doubtful due to the fact that pH in most
margarine. Furthermore, addition of emulsifier ensures margarine emulsions is often close to neutral.
that the emulsion is heat stable during baking.
Milk proteins such as skim milk powder, whey powder,
The most commonly used emulsifiers in margarine are cream powder or sweet butter milk powder have
monoglycerides or mixtures of mono- and diglycerides. an O/W emulsifying effect, which means that
The best water binding effect in margarine is achieved these ingredients work against the margarine W/O
6 Crystallisation technology_01_2011
emulsifier system, and thus destabilises the margarine Low fat emulsions have been found to be sensitive
emulsion. However this enhances the flavour release to in-line pressure and cooling rate. If too extensive
and milk protein is added to the emulsion when chilling takes place early in the process, the shearing
producing table margarine and reduced calorie spreads forces might become too large and the emulsion
to influence the taste. Milk proteins give additionally might break. Therefore, low fat products should be
the desired browning effect in margarine used for frying. produced by high-liquid, low SFC profile blends to
minimise this problem.
In 80% margarine, preservatives are not necessary
as long as the product is properly crystallised and
packed. If the water droplets are finely distributed and Emulsion preparation
their size are between 1 to 5 microns, microorganisms
Initially, the emulsion is prepared. For low fat spreads
cannot growth.
as for other types of margarine, the various fats
There are a large variety of stabilisers or hydrocolloids of the specific blend are melted. Usually, the high
on the market. When the manufacturer chose the melting fats or fat blends are added first followed by
stabiliser, the water binding capacity and organoleptic the lower melting fats and the liquid oil. To complete
properties has to be considered. Typically alginate, the preparation of the fat phase, the emulsifier and
pectin, carrageenan, starch and mixtures are used. other oil-soluble minor ingredients are added to the
fat blend. When all the ingredients for the fat phase
Low fat spreads have been properly mixed, the water phase is added
and the emulsion is created under intensive but
During the last decades, low fat spreads have controlled mixing. It is important when producing
become very popular due to an increasing awareness low fat spreads that the aqueous phase and the oil
in the population concerning the degree of fat intake. have similar temperature and are combined slowly
when forming the emulsion. Additionally, it is very
Back in the late 60’s, the first margarines with a
important that the emulsion is proper agitated to
fat content reduced to approximately 40% were
ensure homogeneity. However, care should be taken
produced. Thus, these products contained only
not to incorporate air during emulsification. Prior to
50% of the normal fat content and consisted of
entering the crystallisation equipment, the emulsion
only fat, water, salt, emulsifier, flavour, vitamins and
is pasteurised either in a plate heat exchanger (PHE)
preservatives. These products showed poor melting
or in a low pressure SSHE, the Consistator®, or in a
and flavour release properties due to very tight water-
high pressure SSHE, the Nexus, the Kombinator or
in-oil emulsions. This tight emulsion was required in
the Perfector.
order to have the needed stability.
Depending on the composition of the emulsion and
In the early 80’s, 40% fat products containing very high
especially the aqueous phase, low fat emulsions can
amount of milk solids were marketed in the US. These
be more or less stable. Stable, viscous emulsions are
products exhibited, however, very poor microbiological
easy to crystallise. Relatively low cooling temperature
stability. Consequently, these products did not have
can be applied and the product can be produced like
the 4 to 6 months shelf life like other spreads and
normal table margarine.
were therefore withdrawn from the market. Today,
higher quality products containing lower fat, usually Leaving the last chilling section the product is ready
milk proteins and stabiliser systems are being for filling. The filling temperature is normally higher
produced with great success in many countries. for low fat products than the corresponding 80% fat
products since the emulsion is more viscous. If the
Some recipe suggestions for low fat spreads, i.e.
filling temperature is too low, the final product may
products containing 40% fat of the total emulsion, are
become crumbly with water leakage as it is packaged.
shown below.
Crystallisation technology_01_2011 7
SOFT PUFF is a 100% vegetable product. The ratio of RBD palm
FATS AND OILS TABLE oil to liquid oil can vary, and RBD palm oil can be
TABLE PASTRY
Palm stearin - - 62 parts
substituted by other semisolid fats, such as partially
hydrogenated vegetable oil.
Interesterified blend,
40 parts 20 parts 25 parts
MP 41/43°C When all the ingredients are mixed and properly
RBD palm oil 20 parts 20 parts 13 parts emulsified as previously described, the emulsion
Liquid oil 40 parts 60 parts - is transferred from the mixing tank to the buffer or
run tank. The emulsion is then pumped through the
Liquid oil: soybean oil, cottonseed oil, palm olein, canola (rapeseed)
oil, etc. crystallisation equipment, where sub cooling and later
crystallisation takes place. The Perfector plant shown
The recipe for puff pastry margarine is compounded on the flow diagram consists of 4 chilling tubes with 2
to be used at approximately 25°C. Puff pastry independent cooling systems and is mounted with 3
margarine has the features of exhibiting a very good intermediate crystallisers.
plasticity without being oily. The plasticity of the
finished margarine depends on the crystallisation
process, on the composition of the fat blend and on
the processing conditions. The puff pastry recipe
contains a relatively high amount of palm stearin,
since puff pastry margarine containing palm oil
exhibits excellent plasticity. However, in some areas
of the world, palm oil as a raw material for margarine
is not an option, and other raw materials have to be
used. By substituting palm stearin with another hard
stock which could be hydrogenated vegetable oil or
an interesterified hard stock, a suitable puff pastry
margarine fat blend could be made.
In regard to fat products not containing an aqueous
phase, recipe suggestions for shortening and
vanaspati will be described below.
8 Crystallisation technology_01_2011
to manufacture a high quality product with the desired the multiple scientific research published on the issue,
texture, no matter which raw materials are used. and the legislative initiatives, e.g. the ban of trans
fats in Denmark by 2004 and the FDA labelling rule
Trans fatty acids effective by January 2006. The majority of the larger
players in the fats and oils industry (e.g. ADM, Frito-
Traditionally, the margarine fat blend consists of Lay, McDonalds, Nestlé) have already shifted to low
partially hydrogenated vegetable oil in certain ratio trans products, however certain parts of the world are
to the liquid oil, as described earlier. In general, not yet focused on the problem.
hydrogenated fats crystallise relatively faster than
unhydrogenated fats and provide the finished Quality of margarine
margarine with the required characteristics. But
during the hydrogenation process various trans fatty
acids are formed and these isomers are nutritionally
undesirable. Scientific reseach indicates a correlation
between a certain intake of these isomers and the risk
of cardiovascular heart diseases.
The main direct sources of trans fatty acids in the
human diet is margarine and crystallised fat products.
Indirectly sources cover products such as baked
products, fried foods etc.
Partially hydrogenated oils may contain up to 55% In the case of food products, quality falls into two
trans fatty acids, depending on the source of oil, the groups: apparent and hidden quality. Apparent quality
refining and hydrogenation process. The higher degree is what the customer perceives and hidden quality
of unsaturation, the higher amount of trans fatty acids is values that cannot be judged sensoricly. Nutritive
will be present after the partial hydrogenation process value and no presence of dangerous microbiological
all other things being equal. or chemical contaminations are examples of hidden
Animal fat contains naturally up to 5% trans fatty quality values. The manufacturer has to guarantee
acids, which occur due to the fermentation processes these values which most often are specified by
done by microorganisms in the rumen of ruminants. legislation.
Deodorised oils may contain up to 3% trans fatty acid The hidden quality is a specific term compared to
due to the high temperature this process is performed apparent quality since it covers measurable values
under. and standardised analytical methods are available.
It is possible to produce non trans vegetable oil The apparent quality varies among the margarine
intermediates by the classical modification processes, manufacturers and there is not much literature
such as fractionation, hydrogenation and available dealing with this issue most likely because of
interesterification. These fats will still fall into the three competition. However, margarine can be evaluated
main groups of liquid, semisolid, and hard stock fats. according to its flavour, texture, mouthfeel and
The increase in the melting point done by neatness of packaging. In addition surface
hydrogenation process is due to bond changes, appearance, oil/water separation, grainy texture,
either due to an increase in saturation or change sticky mouthfeel, meltdown of the margarine and
in the configuration from cis to trans. However, flavour release has to be rated when the margarine is
certain potential disadvantages arise with trans free evaluated.
formulations. Blends consisting of low trans fats, The various types of margarine are evaluated in regard
i.e. cis blends, have shown a decrease in oxidative to their use.
stability when compared to similar blends containing
The spreadability of table, tub and low fat margarine
trans fatty acids. Additionally, since trans fatty acids
and spreads is a very important quality parameter. The
have a higher melting point than the corresponding
homogeneity, consistency, gloss, sandiness, loss of
cis fatty acids, the amount of saturated fatty acids in
water can hereby be determined.
the blend have to be increased in order to achieve
blends with the desired melting point. The stability of table margarine and spreads can be
described by the spreadability test. The test involves
The global trend of lowering the amount of trans fatty
speading of the sample with a knife on cardboard,
acids in food products continues at great speed and
and the following rating system where values from 5-1
the food industry worldwide is decreasing the use of
can be used. The value 5 describes a highly stable
partially hydrogenated fats. The driving force has been
and very smooth sample, the value 3 describes a
Crystallisation technology_01_2011 9
sample that separates when worked, 1 describes a they are being reduced in thickness during the folding
sample that separates during processing where e.g. and rolling procedure. To function as a barrier the fat
free water is visible. should not be absorbed by the dough layers, and it
must remain as a continuos fat film throughout the
When producing low and reduced fat spreads, the
rolling process.
eating properties should be similar to those of full
fat soft tub margarines in terms of mouth-feel and The main demands to puff pastry margarine are
flavour release. In addition, the products should be therefore plasticity and firmness, since soft and oily
spreadable directly from the refrigerator. margarines tend to be absorbed by the dough and
hard and brittle margarines are difficult to spread
Mouth-feel and flavour release can individually be
between the two dough layers during the rolling
rated as follows: fast, average and slow.
procedure. In both cases the baking performances
Margarine which apart from being used for speading may be affected negatively. Puff pastry margarine is
on bread additionally is used for cooking should by the professional baker evaluated by a subjective
further be evaluated for functionality. Frying margarine method called finger evaluation of plasticity, which
should be evaluated in regard to spattering and include a thumb test and a kneading test. The thumb
surface burning of the pan. In regard to industrial test is performed by pressing the thumb several times
margarine and shortening, the appearance is less in adjacent areas in a slice of margarine. This gives an
important, the functionalities being the significant indication if the margarine is firm and homogeneous
properties and consequently the evaluation should be without lumps.
concentrated on these matters.
The test of kneading is a method that determines
Cake and cream margarines are evaluated in the body of the margarine and is accomplished by
regard to the creaming performance. Margarine is working or moulding a piece of margarine. A slice
whipped with sugar according to a standardised is kneaded by hand for a couple of minutes. If the
procedure and by weighing a known volume the sample retains toughness it indicates that the sample
ability to incorporate air is then calculated. Flavour is will be able to withstand the rolling procedure. The
important for all types of margarines, but in the case bending test is another subjective method showing
of margarine and shortening used for baking, the whether a slice of margarine can be bent without
flavour has to exhibit certain heat stability in order not cracking. If the margarine can be bent, the margarine
to disappear completely during baking. In the case of is evaluated to be plastic.
puff pastry margarine, the best way to evaluate this
Good baking performance is not always in
product is by test baking. But several other objective
accordance with subjective evaluation, since the
and subjective methods are available.
margarine that was initially evaluated as being of poor
quality can perform very well in baking. However,
it can be difficult to persuade the baker to use the
margarine if the subjective evaluation does not meet
the standard of the specific baker. Consequently,
the evaluation of plasticity can be very important in
regard to the description of the quality. The baking
test is performed in order to evaluate the abilities of
the puff pastry margarine as a roll-in fat. The height
of the pastry and the uniformity of the lamination are
evaluated.
When producing puff pastry, a basic dough is It is very important in the case of evaluating margarine
rolled out and the roll-in margarine, the puff pastry to define the quality parameters, since these vary from
margarine, is placed on the dough in one flat piece country to country, sometimes even from region to
and following completely covered with the dough. region. Also, most of the above-mentioned evaluation
Several folding and rolling procedures follows in order principles are based on subjective procedures but
to produce multiple alternate dough/margarine layers. objective methods are available like the creaming
These layers result in products with flaky structure. performance test described. In addition, Texture
The flakiness depends on the formation of thin films Analyzer equipment, like the TA TXplus, can be used
of gluten which trap water vapor and carbon dioxide to objectively describe the plasticity, stickiness, and
from fermentation. These laminates can form a three- homogeneity of the margarine. Standard methods are
dimensional structure and for this not to occur, the used in the industry today but complementarily to the
laminates must be separated by continuous sheets 'old-fashioned' subjective evaluation principles.
of fat. Thus fat works as a barrier between the basic
dough layers and prevents them from joining while
10 Crystallisation technology_01_2011
SPX Flow Technology
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should not be relied upon unless confirmed in writing.