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234 Deffense Eur. J. Lipid Sci. Technol.

2000, 234–236

Dry fractionation technology 2 Principle of the dry fractionation or the


in 2000 crystallisation from the melt
In this process, the fat is melted and heated to eliminate
Etienne Deffense any crystal memory. The molten fat is cooled down under
controlled agitation and cooling conditions to produce
Crystallisation & Degumming Sprl, Charleroi, Belgium crystals nuclei formed by the higher melting triglycerides.
Then, nuclei will grow to form crystals of the desired size.
When the crystallisation has progressed far enough, the
slurry is separated. In other words, the crystals or the sol-
1 Introduction id fraction, called stearin, is separated from the mother
liquor which is called olein.
Dry fractionation of oils and fats is the separation of high-
melting triglycerides from low-melting triglycerides by Apparently, it looks simple, but in practice, this physical
crystallisation from the melt. Apart from blending, it is the process is complicated by the fact that the formation of
cheapest process in oils and fats processing. It is a pure nuclei depends on the foreign particles, the agitation, the
physical process compared to other chemical modifica- temperature, the triglycerides composition and the type of
tion processes such as hydrogenation and interesterifica- pre-treatment followed by the fat. Crystals growth is de-
tion which modify triglycerides. termined by the number of nuclei present, the degree of
super-saturation of the molten fat.
Dry fractionation has probably been used for the first time If the quality of the olein mainly depends on the tempera-
in 1872, when Mège Mouriès produced the first margarine ture of the separation, the quality of the stearin and the
made of oleomargarine or tallow olein. Being considered yield of both fractions will depend on the following factors:
for many years as a tedious, expensive and bulky
process, the technology has been particularly driven by  The design of the crystalliser, i.e. the engineering:
the substantial growth in the volume of palm oil that is be-  the cooling exchange surface
ing fractionated for production of palm olein. In 1960 palm  the type of cooling system
oil, indeed, represented 4.7% of 15 oils and fats in total  the type of agitation
world consumption and it is expected to rise to 20% by
2005 or about 20 millions tons, equalling soybean oil. Only batch crystallising systems consisting of a certain
Nowadays, dry fractionation is gaining importance in oil number of tanks are applicable; the attempts to produce
and fat processing in view of current trends favouring continuous crystallising systems have failed so far. Each
the most “natural” or “green” approach: no additives, no tank is either a concentric crystalliser or a crystalliser
chemicals are used and it generates no effluent and loss equipped with either vertical cooling coils, helical cooling
of oil. Today dry fractionation is applied to many kinds of coils or vertical cooling plates or even with a bundle of
fats: palm oil, anhydrous milk fat, tallow, fish oil, lard, pipes used at the same time for agitation and cooling.
cottonseed oil, sunflower seed oil, palm kernel oil, tallow
butter fats, special fats and partially or hardened oils: The geometry of the cooling system, affecting notably the
soybean oil, rapeseed oil and fish oil. total cooling exchange surface of the crystalliser and the
type of agitation are the predominant factors. The trend is
going to increase as much as possible the ratio cooling
The most important applications are: palm olein used ex-
surface in sqm per ton of oil treated while keeping the
tensively as frying oil, palm super olein as salad oil and
slurry in suspension and agitation.
frying oil, the palm-mid fraction as component of cocoa
butter equivalent (CBE), palm kernel stearin as cocoa  The crystallisation cooling conditions:
butter substitute (CBS), anhydrous milk fat fractions for  cooling rate
bakery and confectionery products, spreadable butter, tal-  extent of supercooling
low olein for frying oil and spreads and finally hardened  agitation rate
oils for cocoa butter replacer (CBR).  crystallisation time

Each specific crystalliser is treated independently accord-


ing to agitation, heating and cooling parameters required
Correspondence: Etienne Deffense, Crystallisation & Degum-
ming Sprl, Terre l’Oreye 21, 6032 Charleroi, Belgium.
for each specific feedstock. Nowadays, most plants are
Phone: + 32 71 434624, Fax: + 32 71 477912; controlled by plc programme or by electronic device. The
e-mail: e.deffense@crystallisation.be oil is cooled either according to a linear cooling pro-
Eur. J. Lipid Sci. Technol. 2000, 234–236 Fractionation of fats – a dossier 235

gramme or to a multi-step cooling profile or also to a with a membrane filter press operating at 6 bar squeezing
differential temperature profile between the oil and the pressure. It means that the SE rises from 0.3–0.4 to
cooling water circulating through the cooling system. 0.5–0.6.
Presently, a good crystallisation can be successfully ob-
tained with RBD palm oil in 8 h. 3 New trends in separation
 The separation type:
Recently, a new type of separator has been developed by
 vacuum filter
Westfalia Separator. It consists of separating the crystals
 membrane filter press
by centrifuge without additives but playing on the differ-
 centrifuge
ence of specific gravity between the two fractions. This
When looking at the different processes proposed in the centrifuge requires small hard crystals.
market, they can be grouped into either fast or slow
Another type of centrifuge, a filter centrifuge or a worm-
processes: people promoting the fast process favour the
screen centrifuge has been investigated. It is a conical
membrane filter press, since for them the separation is
sieve centrifuge fitted with a tightly fitting, co-rotating
the most important aspect. On the other hand, those in
worm. The crystal slurry is fed through a co-axial tube to
favour of the slow process regard crystallisation as the
the narrow end of the cone and moves by the centrifugal
most important step. To them the separation process is
force over the screen in the direction of the wide end of
not the only tool for attaining a high efficient separation.
the cone. During this movement, the liquid olein passes
Stearins obtained by crystallisation from melted fat, al- through the screen whereas the stearin particles are re-
ways contain some portion of the olein resulting from the tained by the screen. Sieve and worm rotate at slightly dif-
formation of mixed crystals but also due to the difficulty in ferent speeds. Consequently, any crystals sticking to the
the separation of the olein from the stearin. The retention screen are regularly scraped off by the worm. At the same
of the olein either absorbed onto the surface of the crys- time, the worm prevents crystals from moving too fast and
tals or in the spaces between agglomerated crystals is thus provides them with a certain residence time. In addi-
called „entrainment“. It depends to some extent upon the tion, the worm may also cause the crystals to rotate and
process conditions used, but mainly on the type of sepa- thus expose new surfaces to the screen so that these sur-
ration. The reduction of entrainment has therefore been a faces are also provided with an opportunity to shed their
major objective of developmental work in edible oil frac- liquid oil.
tionation during this last decade and is still under devel-
opment. Although solvent and to a lesser extent deter- The SE of the filter centrifuge is much better than that ob-
gents have the advantage of high selectivity, both of them tained with a vacuum filter and is even slightly better than
have been banished for cost reason. that obtained with a membrane filter press using a stan-
dard squeezing pressure of 5 bar. This process has been
Consequently, the trend in fractionation has been to opti- used for production of CBE and CBR and is under devel-
mise the separation efficiency (SE) in the dry fractionation opment for other fats.
process, defined as the solid crystallised phase fraction in
the cake stearin measured by NMR. Both centrifuges have the advantage to offer an enclosed
system, continuous and hygienic separation.
The introduction in 1983 of the membrane filter press
greatly improved the separation efficiency of the dry
fractionation process. Its principle is similar to that of 4 Other trends in dry fractionation
a plate and frame filter except that the filter feed pressure
 Multi-step fractionation as a tool for production of
is kept at rather low value, 1.0 to 1.5 bar. Each chamber
super or special fractions.
is equipped with filter cloths and with one or two
membranes made of flexible material (rubber or poly-  Induced nucleation: The multi-stage fractionation looks
propylene). After filling, the membrane is slowly applied quite simple but in practice, the re-fractionation of olein
by means of a gas or a liquid, compressed air being most is complicated because it requires a long cycle time. A
common; some retained olein will be squeezed out, leav- recent study has therefore aimed at showing that with
ing a hard stearin cake. Depending on the type of feed- induced nucleation, the crystallisation rate can be
stock, the squeezing pressure may range from 5 bar for much faster and more selective and thus leads to a
soft products like fish oil to 5–15 bar for palm oil and much reduced cycle time. This can be cut by at least
anhydrous milk fat and to 25–30 bar for speciality fats 50% for super olein production.
(CBE, CBR and CBS). For anhydrous milk fat, for exam-
ple, the percentage of liquid in the stearin cake drops from For example, in standard conditions, a super olein of IV
60–70% obtained with a vacuum filter to around 40–45% 64–65 is produced industrially in around 60 h; the yield
236 Denet et al. Eur. J. Lipid Sci. Technol. 2000, 236–240

ranges between 50 and 55%. The same olein crystallised 2 Definition


in a well-designed crystalliser, well controlled and with
seeding, leads to a super olein in less than one day with Chromatography is a technique allowing the fractionation
an excellent yield (60%) and cloud point. of chemical products based on two main principles, an
equilibrium between a fluid phase (liquid, gaseous or su-
percritical) in which the products are soluble and a solid
5 Trends for the future adsorbent which has a delay effect [1].
May we imagine a continuous crystallisation combined to Various implementations of this technique exist when
a continuous separation. varying the mobile phase (physical state, composition),
the adsorbent nature (mineral oxides carbons, organic
Other alternative processes may take place to replace the
polymers), the interactions between the two phases
multi-step fractionation processes requiring a lot of time
(adsorption, partition, ion exchange, exclusion ...), the im-
and storage tanks handling.
plementation of the solid (fixed bed chromatography,
countercurrent moving bed, simulated moving bed) and
the goal of the separation (scale, price, toxicity ...).

In the case of fats separation, the desorbents the more of-


ten used are silica or silica bound to organic chain (polar
or not), and the interactions between stationary phase
and solute are adsorption or partition. Concerning the im-
plementation of the solid and the mobile phase, all the dif-
ferent possibilities can be used and will be detailed after.

Industrial chromatographic Whatever the products are, a precise study must be done
separation of fats for each case.

Félicie Denet, Willi Hauck, Roger Marc Nicoud 3 Batch chromatography:


NOVASEP, Vandoeuvre lès Nancy, France technical evolutions
The simplest implementation is per HPLC (high-perfor-
mance liquid chromatography) which enables easy han-
1 Introduction dling of the mobile phase, large range of solvent and thus,
a large range of application [2].
For a long time, chromatography was considered as an
excellent analytical technique, and purification performed It is a discontinuous process: for separation of the mixture
with this separation was limited to the laboratory scale. a precise quantity is injected at the inlet of the column,
Important technical evolutions have transformed chro- products are separated inside the column depending on
matography in a purification technique for the develop- their interaction with the mobile and the stationary phase;
ment scale and more and more for the industrial scale. at the outlet of the columns, the signal given by a detector
These progresses come from different fields, technical allows to orientate the different fractions in different lines.
improvement of batch chromatography (classic HPLC or
supercritical fluid chromatography), development of new The first main evolution is between an analytical tech-
processes (simulated moving bed), development of mod- nique to a preparative one. To jump this gap, it was first
elling tools allowing a better understanding and control of necessary to have large column diameter with high effi-
the processes. ciency.

These three orientations will be detailed and some exam- Good performance has been obtained by changing the
ples of the application of these techniques for fats purifi- column design and using the dynamic axial compressed
cation will be presented. technology [3]. Now, columns of more than 800 mm diam-
eter are available and give efficiencies equivalent to those
obtained on analytical columns (Fig. 1). These high effi-
Correspondence: Félicie Denet, NOVASEP, 15 rue du bois de ciencies allow to increase the productivity, taking into ac-
la Champelle, Parc Technologique de Brabois, BP50, 54502
Vandoeuvre lès Nancy.
count mobile and stationary phase consumption, and so
Phone: +33 383 447250, Fax: +33 383 447249; reduce the cost of the process. The main drawback of this
e-mail: novasep@novasep.com technique is the toxicity of the solvents and the high dilu-

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