IMPACT OF CRYSTALLIZATION OF HIGH MELTING WATER IN FAT

EMULSIONS ON DISPERSE MICROSTRUCTURE AND PLASTICITY

H. Spitzbarth, W. Hanselmann, E. Windhab
Laboratory of Food Process Engineering, ETH-Swiss Federal Institute of Technology,
Zurich, Switzerland (heiko.spitzbarth@ilw.agrl.ethz.ch)

Keywords: plasticity, crystallized-emulsions, Low-Temperature-Extrusion.

Crystallized high melting water in fat emulsions are most relevant for confectionary as
well as for margarine and baking industries. The structure is build of a crystallized
continuous fat blend consisting of about 60 % high melting fat, 25 % low melting fat or
oil, respectively, emulsifier and the dispersed phase (water) [1, 2]. The macroscopic
behavior like plasticity, flowability, stiffness, etc. of such emulsions depends on their
mesoscale structure like crystallized fat content and structure density and last but not
least on their microscale structure like crystal size distribution, crystal-crystal
interactions like Van-der-Waals forces or covalent primary bindings [3, 4].
The properties of the crystallized bulk are influenced by the structure which is directly
linked to the crystallization process as cooling temperature TS, residence time tR and
applied shear forces [5]. Cooling temperatures influence the crystallization rate and
the solid fat content (SFC) as well as the crystal size distribution. Fast cooling of the
melted fat blend increases the number of fat crystals and reduces the crystals size.
Furthermore the result of a high cooling rate is a fast increase of viscosity due to high
SFC. Residence time distribution influences the dynamic treatment during
crystallization. Long residence times are necessary to brake crystal-crystal interactions
to get a smooth, plastic structure. If the residence times are to long fat crystals will melt
again due to dissipated energy which is the same effect for high applied shear forces.
High melting water in fat emulsions with an extended amount of crystallized fat which
are conventionally crystallized by scraped surface heat exchangers (SSHE) and
softworked by pin mixing devices (Figure 1) show high yield values, grainy structure,
high stiffness, extended crystal-crystal interactions and less plasticity. In this process
setups the crystallizing mass is treated by high rotational speeds (400 rpm to 1000 rpm).

Figure 1. Setup of conventionally crystallization process of water in fat emulsion. (1) vessel with stirrer,
(2) feed pump, (3) SSHE 1, (4) SSHE 2, (5) pin mixer, (6) resting tube

This treatment causes high friction and as a consequence high energy dissipation, which
is a function of viscosity and shear to the power of two. The dissipated energy is
converted into heat, which leads to partly remelting of fat crystals [5]. This noncrystallized fat crystallizes after processing under static crystallization in the resting
tube and during storage which is the reason for connected, dense networked fat crystals.
Finally with this process it is not possible to crystallize high melting, high solid matter
contenting water in fat emulsions under high shear to get small singular crystals without
remelting of crystallized fat and therefore extended static crystallization.
To realize such crystallized high melting emulsions with optimal plasticity a new
process is investigated. This innovative process is called Low-Temperature-Extrusion
(LTE) in which crystallizing masses are simultaneously shear treated and cooled to low
temperatures of about -5 C to -15 C. Typically lower rotational speeds (15 rpm to
50 rpm) of extrusion screws are adjusted in comparison to conventional crystallization
process (500 rpm to 1000 rpm). The main optimization criteria for the low temperature
extrusion devices were according to Windhab et al. [6], (Figure 2):
1.
2.
3.
4.

Uniformity of local shear stresses acting in the screw channel flow

Maximum dispersion of structural elements (minimum sizes)
Good mixing without local re-melting
Maximum heat transfer coefficient

Figure 2. Scheme of Low Temperature Extrusion process and flow directions of crystallizing masses
during laminar shear treatment.

With this new process setup (Figure 3) the viscosity increase due to crystallization and
the laminar, low shear treatment to decrease the crystal-crystal interactions is in balance.

Figure 3. Setup of Low Temperature Extrusion process and flow directions of crystallizing masses during
laminar shear treatment. (1) vessel with stirrer, (2) feed pump, (3) SSHE, (4) LTE

The first freezing step is the initialization of crystallizing at low viscosities with high
shear (nSSHE = 500 rpm) in a cooled (Twall, SSHE = -5 C) SSHE. This leads to singular,
small fat crystals slurries, which are pumped into the LTE where the fat slurry is further
crystallized under low, laminar shear and further cooling (Twall, LTE = -37 C). Low shear
causes low friction, which results in low energy dissipation and no remelting of fat
crystals.
After this process all fat crystals are formed due to low outlet temperatures and well
dispersed in the remaining non crystallized oil emulsion due to shear treatment along
the whole process, without remelting.
The samples were analyzed at 20 C by small (rheometer: oscillatory measurements)
and large deformation (texture analyzer: compression and cone penetration) as well as
by static laser light scattering measurements to get information about the formed fat
crystal network, the macroscopic behaviour and the fat crystal size distribution.
Furthermore X-ray diffraction measurements were carried out in order to analyze fat
crystal polymorph structure.
The LTE process leads to smaller fat crystals compared to the conventional process
(Figure 4) which is important for a smooth and plastic structure. Furthermore the LTEprocessed masses are more monodisperse so there is a slow change of crystal sizes due
to Ostwald ripening and high SFCs at the outlet causes less crystallizing of remaining
non crystallized fat under static conditions during storage.

Figure 4. Comparison of fat crystal size distribution at different rotational speeds for the conventional
process with SSHE and the LTE-Process.

One of the consequence of finer dispersed and smaller fat crystals are lower yield values
and smoother structures for LTE processed masses which is important for further
processing (Figure 5). For example for stamping, rolling out or forming different
shapes. According to Haighton crystallized fat with yield stresses above 1000 g/cm2
show a hard and less spreadable structure [7]. LTE processed masses have always yield
stresses below 1000 g/cm2 and show no significant change in plastic properties during
storage in contrast to conventional produced crystallized masses which are brittle, not
spreadable and show significant change in hardness during storage.

Figure 5. Comparison of yield stresses at different rotational speeds for the conventional process with
SSHE and the LTE-Process.

References:
[1]
[2]
[3]

[4]

[5]

[6]
[7]

Van den Tempel, M.V., Mechanical properties of plastic-disperse systems at very

small deformations. Journal of Colloid Science, 1961, 16(3), 284-296
Haighton, A., Blending, chilling, and tempering of margarines and shortenings.
Journal of the American Oil Chemists' Society 1976, 53(6), 397-399
Laia, O.M. et al., Physical and textural properties of an experimental table
margarine prepared from lipase-catalysed transesterfied palm stearin: palm kernel
olein mixture during storage. Food Chemistry 2000, 71(2), 173-179
Miskandar, M. et al., Effect of scraped surface tube cooler temperatures on the
physical properties of palm oil margarine. Journal of the American Oil Chemists'
Society 2002, 79, 931-936
Wildmoser, J., Impact of low temperature extrusion processing on disperse
microstructure in ice cream systems. Diss, technische wissenschaften ETH Zrich,
no. 15455,Laboratory of Food Process Engineering, 2004
Windhab, E. J.; Bolliger, S.; Wildmoser, H. Extrusion: A novel technology for the
manufacture of ice cream. Bulletin of the IDF, 2002, 374, 4349
Haighton, A., The measurement of the hardness of margarine and fats with cone
penetrometers. Journal of the American Oil Chemists' Society 1959, 36, 345-348