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Full Papers: Product Design in Food Industry Using The Example of Emulsification
Full Papers: Product Design in Food Industry Using The Example of Emulsification
Designing a product according to the consumers' needs is one of the key targets in food industry. Having once defined the target
product properties, it is of imperative importance to know which microstructure of the product is required (property function)
and how the target microstructure can then be determined by process parameters (process function). Many food products are
emulsions, either during production and/or in the moment of distribution and consumption. This review intends to depict the
design of emulsions according to target needs. Even if we concentrate on typical food emulsions as an example, the concept can
be widely applied, since emulsification in other branches of industry is governed by the same principles.
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process functions in food industry usually is the target of emulsifiers (in food industry these are most often proteins) are
process engineers and food technologists. Process functions used. Depending on the molecular structure of an emulsifier,
enable engineers to choose the best type of machine, to different adsorption mechanisms are found, both depicted in
optimize process parameters, and to scale up the process. Fig. 1. Besides stabilizing an emulsion, the emulsifier often
influences product properties, such as its viscosity. This will be
shown in chapter 5.
Thickeners are high-molecular weight molecules that are
3 Emulsion and Emulsification Basics
solved in the continuous phase, thus enhancing its viscosity.
They stabilize emulsions by slowing down droplet mobility.
3.1 Emulsions
Flocculation, sedimentation or creaming, and coalescence are
either slowed down or inhibited at all. Typical thickeners used
Emulsions are part of the product range in the chemical or
in food industry are (modified) starches and proteins. Since
petrol industry as well as in the pharmaceutical, cosmetic and
they increase continuous phase viscosity, they do not only
food industries. In food industry, typical emulsion products are
stabilize the emulsion, but also change its properties (see
milk, butter, mayonnaise, spreads, sauces, and dressings.
chapter 5).
An emulsion is a disperse system of at least two immiscible
liquids, e.g. water and oil (see Fig. 1). One of these phases is
finely dispersed and forms droplets in the other one.
3.2 Emulsion Properties
Depending on the droplet phase, oil-in-water- (o/w-) type
and water-in-oil- (w/o-) type emulsions exist. In rare cases, the
Important emulsion quality properties are the physical and
droplet phase itself is an emulsion. This review will concen-
microbiological stability, rheological properties (as consis-
trate on the simple emulsion type, consisting of two liquids,
tency, viscosity, texture, spread-ability), sensorial qualities
only.
(such as color, taste, and mouth-feel), as well as the
w o o w distribution of active ingredients, their dissolution rate and
bioavailability. They are influenced on the one hand by the
formula (type and concentration of main phases and
additives). On the other hand, the droplets' size distribution
has a big impact on the properties of an emulsion. Often, the
oil-in-water (o/w) water-in-oil (w/o) formula of an emulsion is already given (by recipe and/or
legislation). Thus, the droplet size distribution might be the
emulsifier: small molecular high molecular only possibility for engineers to influence the product quality.
weight: surfactants weight, e.g. protein Most often, the main process goal therefore is to produce a
hydrophilic lipophilic
required droplet size distribution for a given recipe.
surfactant only protein only protein and surfactant
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rotor-stator-machines, e.g. colloid mill high-pressure homogenizers In emulsification by means of ultrasonic waves (waves of
frequency > 18 kHz), droplets are disrupted in zones of locally
high turbulence caused by sound-induced cavitation. A
batchwise operation of a small scale is well known for
laboratory applications whenever fine droplets are required
in low viscous systems [5]. New publications now demonstrate
the possibility to produce finely dispersed emulsions by means
of ultrasonic waves continuously, as well [13,14]. Continuous
ultrasonic waves microporous membranes
applications require a flow chamber of special design into
which the ultrasound waves are introduced. Due to the limited
power of sound inducers, there are technical limits for very
high tonnages (e.g. > 1000 L/hr).
Droplet disintegration usually is done by tensions acting on
droplet interfaces via the continuous phase. In order to
produce the required flow pattern in the continuous phase,
Figure 2. Emulsification machines (mechanical emulsification).
high energy has to be applied. Only a negligible part of the
long residence time and, thus, emulsification time is required, energy (< 1 %) is used for droplet disintegration, while most of
often resulting in broad droplet size distributions. Small mean the energy is transferred into heat. It is therefore more
droplet diameters (as e.g. < 1 lm) can rarely be produced in efficient to produce droplets of the required size directly by a
stirred vessels. If processes are driven at higher temperatures droplet-forming process. This could be realized, e.g., by
(e.g., to lower viscosities or to melt ingredients), undesired pressing the future droplet phase through pores of small
byproducts may be formed. diameter and dispersing the droplets into the continuous
In order to solve these problems, the disruption zone has to phase. Industrially, this can be realized by using microporous
be small and well defined, and the power density should be membranes [15,16]. In membrane emulsification, the process
increased. This is realized in continuously working rotor- starts at a disperse-phase content of zero. During the process,
stator machines, such as colloid mills, or toothed-disk the disperse-phase content is then enhanced to the required
dispersing machines. In a colloid mill, the rotating part is a value by pressing more disperse phase through the membrane
truncated cone, most often toothed. It rotates within a stator, pores. This is realized by recirculation of the emulsion.
also toothed. In toothed-disk dispersing machines, rotor and Recirculation, in turn, decreases energy efficiency. Alterna-
stator consist of one or several disks having pins or teeth of tively, preemulsions may be pressed through the membrane
different design. Rotor-stator-machines are relatively easy to pores [17], and phase inversion during membrane emulsifica-
handle and of low cost. They can be operated at throughputs tion may be induced [18]. Thus, high quantities of emulsions
from about 50 L/hr to several tons per hour. Droplet (several tons per m2 of membrane surface and hour) having a
disruption is mainly due to turbulent flow within the high disperse-phase content (e.g. 50±80 %) may be produced
dispersing zone between rotor and stator [6]. by a single pass through the membrane. Membrane emulsi-
High-pressure homogenizers have been traditionally used in fication is reported to produce small droplets (< 3 lm) at a very
milk industry. These machines are operated continuously at narrow droplet size distribution and low energy input [15,17].
throughputs from 1 to several 1000 L/hr. They consist Investment and manufacturing costs are less than for high-
essentially of a high-pressure pump, and a homogenizing pressure homogenizing [16]. By microchanneling [19], emul-
nozzle. The high-pressure pump creates the energy, which is sions of extremely narrow droplet size distributions may be
then used by the nozzle to disintegrate the droplet phase. The produced. However, this process being under development is
design of the homogenizing nozzle influences the flow pattern far from industrialization until now.
of the emulsion in the nozzle and hence the results of droplet
disruption [7]. Recent developments in high-pressure homo-
genizing concentrate therefore on nozzle design. Examples of 4 Emulsion Property Functions
new homogenizing nozzles are opposing jets (Microfluidizer
[8]), jet disperser [9], and a simple orifice valve [10]. Droplet As already stated, property functions for emulsion products
disruption in high-pressure homogenizers predominantly is highly depend on product recipe. Thus, they have to be
due to inertial forces in turbulent flow and shear forces in determined anew for each product recipe. Therefore, we will
laminar elongational flow [7]; cavitation may also be found restrict ourselves to one example. In Fig. 3, the viscosity of a
[11,12]. salad-cream type emulsion (60 % of vegetable oil in water) is
The trend in emulsification is to produce emulsions of very depicted as a function of the type and concentration of the
fine droplets (< 1 lm) and narrow size distributions at low emulsifier, as well as the mean droplet size.
energy input. Continuous emulsification using ultrasonic The addition of a high-molecular weight emulsifier (such as
waves, microporous membranes, and microchannel systems Lacprodan-60, a spray-dried whey protein, mainly consisting
are to be mentioned in this context. of b-lactoglobulin) increases the product viscosity consider-
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60 % vegetable oil in water before being able to optimize the process, and to scale it up.
0.8 c Lac = 60 g/l Process functions, however, should be independent of the
c = 0 g/l
Tween 80
1,2 g/l
equipment or process parameters.
0.6
3,5 g/l In order to evaluate the effectivity of droplet disruption, the
7,5 g/l volumetric specific energy Ev was proposed by Karbstein [6]
0.4 15 g/l
as an independent parameter to describe continuous emulsi-
35 g/l
0.2
fication processes for all machine types and process param-
c = 0 g/l
c
Lac
= 150 g/l eters1).
Tween 80
0.0
E P V tres
0 1 2 3 4 5 Stang, 1998
EV Dph P (1)
mean droplet diameter x3,2 / µm _
V V
Figure 3. Example of a property function for a food emulsion: Viscosity g of the Herein, the power density is defined as
emulsion as a function of its mean droplet size x3,2 (Sauter diameter) and the
emulsifier type and concentration, respectively [10]. P
Pv (2)
V
ably compared to a low-molecular weight surfactant (e.g.
Tween 80, a sorbitane fatty acid). For a given recipe, however, Herein, E is the energy applied by the machine, V the
viscosity decreases with increasing mean droplet diameter. volume of the emulsion, P the power applied by the machine,
This effect is even more marked for the high-molecular-weight V_ the volume flow rate of the emulsion, Dph the homogenizing
emulsifier. pressure (in case a high-pressure homogenizer is used), Pv the
The parameter droplet size' thus offers a good possibility to mean volume power density of the machine, and tres the mean
influence rheological and sensorial quality parameters, such as residence time of the emulsion within the dispersing zone of
viscosity, creaminess or mouth-feel, even if the recipe is the machine.
already given by raw material or legislative restrictions. Using The specific energy summarizes the influences of machine
the property function (as in Fig. 3), the mean droplet size may and process parameters into the energy produced by these
be determined that is responsible for a target viscosity. This processes and applied to a certain volume of emulsion. Thus,
mean droplet size characterizes the microstructure, that now only one diagram per recipe/formula is required (see Fig. 4b),
has to be realized by an emulsification process. The necessary giving one curve per formula [6]. In a double logarithmic
equipment has to be chosen and the process to be designed. diagram, this curve is a straight line.
The specific energy also depicts the influences of power
density and residence time on the disruption process. The
5 Process Functions in Emulsification influence of the residence time is always found in continuous
emulsification processes of short residence times (tres << 1 s)
5.1 Independent Parameter for Describing Emulsification [20]. Similar dependencies are also found in wet grinding
Processes processes of solids [e.g. 21].
In batch processes, however, the residence time of the
Emulsification results are usually given as a mean droplet product in the emulsification machine is in the order of
diameter in dependency of a chosen machine type, and one minutes. Here, both, the power density Pv [5], and the
or more selected process parameters (such as rotor speed), residence time tres influence the mean droplet size. Since the
and/or machine parameters (e.g. dispersing zone design). dependencies on power density and residence time follow
These diagrams are then given for a selected recipe/formula different mathematical functions, they cannot be summarized
(e.g. Fig. 4a). Even if only one product formula has to be in the energy density, as for continuous emulsification
processes. Only for very long residence times tres ! ¥, no
30 % rape seed oil in water, emulsifier: LEO-10 influence of the residence time on the final emulsification
toothed discs dispersing machine
result is found.
5 10
1 r/s
36 mm (a) (b)
4 2 r/s
36 mm 5.2 Theory of Droplet Disruption
x3,2 / µm
x3,2 / µm
3 1 r/s
48 mm 1
2 r/s
rotor
2 48 mm speed Droplets are disrupted, if they are deformed over a period of
1 number or
diameter of r/s-discs
time tdef that is longer than a critical deformation time tdef,cr,
0 0.1 and, if the deformation (described by the Weber number, We)
0 4.000 12.000 20.000 106 107 108 exceeds a critical value, the critical Weber number Wecr [5]:
rotor speed n / min-1 spec. energy Ev / (J/m3)
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0:3
We > Wecr and tdef > tdef,cr (3) xµtres (11)
2=5
xmax|Oh®0µrc 1=5 c3=5 PV (9) x µ PV
0:25 ::: 0:4
f
tres gd 0 ::: 0:75
(14)
For highly viscous droplet phases: In most industrial processes, f(tres) can be described by an
exponential function as t±a. However, a saturation function
1=4
xmax|Oh®¥µ rc 1=2 gd3=4 PV (10) better describes the reality, such as:
Experiments depict that the droplet phase viscosity is btres
negligible for gd < 10 mPa s [6,25]. f
tres k e
xt (15)
res !1
In continuous emulsification processes, residence time is in
the order of milliseconds to tenths of a second. Thus, an Herein, k and b are constants, and xtres ®¥ is the equilibrium
additional dependency on residence time tres is found [20]: mean droplet diameter which is found for tres®¥.
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5.3 Process Functions for Droplet Disruption sonic emulsification) results in droplet sizes comparable to
those of effective high-pressure homogenizers.
Using the specific energy for continuous processes as well as However, if ultrasonic waves are applied to an emulsion
the power density for batch processes, process functions can continuously, there are some restrictions. Up to now, it is
be defined for emulsification (Eqs. (12) to (15)). For each almost impossible to avoid bimodal droplet size distributions,
formula, the proportional constants as well as the exact even if the specific energy is increased (Fig. 6). Droplets of the
exponents can then be determined using this diagram. The second peak are the remaining premix droplets. In a product to
required specific energy for a target mean droplet diameter be industrialized, these droplets will cause instabilities due to
may be determined by the resulting equation. Process sedimentation. Avoiding this instability problem requires
parameters, such as homogenizing pressure, or power input either recirculation of the emulsion or a design improvement
for a given throughput, can then be calculated. of the flow chamber [30]. Since cavitation causes droplet
Fig. 5 gives mean droplet diameters for emulsions of 30 % of disruption and high viscosities decrease cavitation, ultrasonic
rapeseed oil in water as a function of specific energy. The emulsification is restricted to products of low viscosity.
emulsions were stabilized using a very fast adsorbing In comparison to droplet disrupting machines, membrane
surfactant (a lauryl alcohol, LEO-10), that allows to have a emulsification is very efficient, if small droplets (x < 3 lm)
low re-coalescence rate. Thus, disruption governs the process have to be produced [15] (Fig. 5). However, the higher the
of emulsification. For food applications, this emulsifier would disperse phase content, the more specific energy has to be
have to be replaced by another small-molecular weight applied, since recirculation of the emulsion is required to
emulsifier, which is permitted for food by law, e.g. Tween 20. concentrate the dispersed phase. If a pre-emulsion is pressed
Using continuous rotor-stator machines or a high-pressure through the membrane pores instead of the droplet phase, no
homogenizer with a standard flat nozzle results in relatively recirculation is required [17]. This does not decrease the
large mean droplet diameters. If smaller droplet diameters are required energy input in total but simplifies the process for
required, machines have to be used that induce other flow industrialization. Emulsification by membranes results in very
patterns as well, e.g., laminar elongational flow or cavitation. steep droplet size distributions if the membrane surface is not
In commercial emulsification machines, this is realized in wetting the future continuous phase (small wetting angle). For
high-pressure homogenizers with, for example, the opposing example, in order to produce oil droplets, the membrane
jet nozzle, such as Microfluidizer, or the simple orifice valve, surface material has to be hydrophilic [16,31].
or by sound-induced cavitation (ultrasonic emulsification). In An improved effectivity in droplet disruption simplifies and
the simple orifice valve, for example, droplets are deformed cheapens emulsification processes. Producing a mean droplet
mainly by laminar elongational flow, destabilized, and thus diameter of, e.g., 1 lm by high-pressure homogenizing
easy to disrupt by the following turbulent flow conditions requires a homogenizing pressure of 35 bars only if the simple
[7,29]. This nozzle design is very efficient in droplet disruption, orifice nozzle is used for this recipe. However, about 2000 bars
especially if highly viscous phases have to be finely dispersed would have to be applied using the standard homogenizing
[10]. Similar results are found for the jet disperser [9,10]. nozzle. Using membranes instead of a high-pressure homo-
Emulsification mainly due to cavitation (continuous ultra- genizer would decrease the required specific energy by
an additional factor of 3±300 (Fig. 5). This is of interest
from both manufacturing costs and product quality point of
view (especially, if stress-sensitive products have to be
HPH: membrane em.
r/s-systems flat nozzle ϕ=1% produced).
ultrasonic em. orifice valve, ϕ = 50 %
opposing jet
10
mean droplet diameter x 3,2 / µm
2
10 % water in
vegetable oil
1.5 premix
EV / 107 J/m3
1 ϕ = 1 → 50 %
0.9
1 3.6
7.0
10
0.5 Behrend, 2001
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5.4 Theory of Droplet Recoalescence probability. At a constant specific energy, the coalescence rate
therefore is higher than in rotor-stator machines.
In emulsification, droplets are disrupted. However, they If the recoalescence rate is high, the emulsification result in
rarely exist for long due to recoalescence. This takes place total is changed [6,32]. The mean droplet diameter achievable
within milliseconds after disruption and is found in practically at a given specific energy increases. Using Eqs. (12) to (15),
every emulsification process [32,33]. This is due to the fact that that means, both the proportionality factor and the exponent
new droplets are not sufficiently stabilized directly after their of Ev and Pv increase. The negative slope of the line in the
disruption (either by adsorbing emulsifier molecules or by diagram x3,2 = f(Ev) decreases. For high recoalescence rates,
hydrodynamic effects). Emulsification processes are thus even an increase in mean droplet diameter is found for
governed by both droplet disruption and recoalescence of increasing specific energy (see chapter 6.5).
droplets [6]. Only if the droplet stabilization is very fast and if
the droplet concentration is very low, recoalescence rates are
low enough for droplet disruption to govern the emulsification 5.5 Process Functions for Droplet Disruption and
process. Recoalescence
The effect of recoalescence is well described in the literature
[summarized in 32]. A short insight will be given here, only. If a certain recipe requires an emulsion of a high content of
The number of droplet collisions (collision frequency c) disperse phase or slow stabilization characteristics (as is often
depends on several parameters and may be calculated for found in food industry), recoalescence of newly formed
turbulent flow according to [34]: droplets determines the emulsification result (characterized
by the mean droplet diameter).
c = K ´ u ´ x2 ´ n2 (16) Fig. 7 gives an example of a typical food emulsion
(mayonnaise type: 80 % oil in water, emulsifier: egg yolk).
with In this emulsion, the coalescence rate is high. A production in
p rotor-stator machines results indeed in droplet diameters
K 2 p=15 (17) larger than expected (compare to the results of a fast
adsorbing emulsifier, as e.g. LEO-10, in Fig. 7). However, if
p a high-pressure homogenizer is used, no emulsion can be
u e=md x (18) formed at all. The coalescence rate is so high that the disperse
and continuous phase separate within minutes after produc-
Herein, K is the collision coefficient, u the droplet velocity, x tion. In production, this phenomenon is called ªover-
the droplet diameter, n the number of droplets per volume processingº.
emulsion, e the mass-specific power density, and md the In conclusion, rotor-stator machines are recommended at
kinematic viscosity of the droplet phase. The coalescence higher coalescence probability [36]. Only at very low
probability of colliding droplets usually is smaller than 1. An coalescence rates, high-pressure homogenizers or ultrasonic
easy experimental method based on image analysis allows to devices are to be chosen. In this case only, one can profit from
determine the coalescence probability pcoal and the coales- the advantage of high disruption effectivity [37,38]. Using a
cence rate X for different emulsion formulas [32]: stabilization zone may help in preventing recoalescence
during the production of food emulsions of high coalescence
X = pcoal c (19) rates (high oil fraction and slowly stabilizing emulsifiers)
[10,39].
Coalescence is found whenever droplets are disrupted. In
case of very low disperse-phase contents (< 1±3 %), the
100
recoalescence rate in emulsification processes is low [35]. In RSM HPH - egg yolk
mean droplet diameter x3,2 / µm
industrial emulsification processes, the disperse-phase con- egg yolk --> emulsions break
tent is always higher. Thus, disruption and recoalescence are
RSM
found. In rotor-stator machines, droplets are disrupted at LEO-10 HPH:
relatively low power densities (Pv » 1 ... 109 W/m3) and long tv = 0.001 - 0.01 s
10
residence times (tres » 0.1 ... 1 s). The number of disrupted
droplets is relatively low, and time is given to stabilization.
Thus, the coalescence probability is relatively low. In high-
pressure homogenizers or in continuously working ultrasonic HPH
RSM:
devices, however, the power density is higher (Pv » 108 ... LEO-10
tv = 0.1 - 10 s
1012 W/m3), whereas the mean residence time is shorter
1
10 4 105 10 6 10 7 10 8
(tres » 0.001 ... 0.01 s). Many small droplets are formed in a time spec. energy Ev / (J/m3)
being too short for stabilization. In addition, the forces in Figure 7. Process function for emulsification at different coalescence rates
droplet collision are higher, leading to a higher coalescence (RSM: rotor-stator machine, HPH: high-pressure homogenizer).
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Knowing the property functions, the process has to be energy of 6 to 7 ´ 106 J/m3 results in the target mean droplet
designed based on the process functions. Since the production diameter of 4 lm. The required value of specific energy may be
quantities are low, a batch process is chosen. During realized by several combinations of process parameters, as
emulsification the product has to be heated above its melting rotor speed, gap width or tooth design. For scale-up, the
point. The product is of high viscosity during production, thus process function in Fig. 9b can also be used.
rotor-stator machines are able to realize the required high
specific energy for the target droplet diameter (xmax » 3 lm ).
As low-cost machines are a must for a product of low tonnage 6.4 Property and Process Functions for a Drink
and low price, a rotor-stator machine even is recommended.
The batch process allows heating and cooling to be combined A drink, of low viscosity, low fat content and high stability
with the emulsification process. The process functions are requires an o/w-emulsion type with a fat fraction below < 10 %.
given in Eqs. (14) and (15). A pilot plant trial has to be A fast stabilizing emulsifier, such as Tween 20, has to be used.
performed in order to determine the exponents of power A narrow droplet size distribution and a mean droplet
density, the residence time function, as well as the proportion- diameter < 1 lm ensure a high stability for this system. High
ality constant for this special recipe. Scale-up will then be done tonnages per year are best achieved by a continuous process.
using the same process functions for the rotor-stator machine Since a small mean droplet diameter is required and the
(see chapter 5.6). disperse-phase content (and thus the coalescence rate) is low,
a high pressure homogenizer is recommended. Using the
simple orifice plate as homogenizing nozzle keeps investment
6.3 Property and Process Functions for a Dressing costs and energy consumption low. The process function is
given in Eq. (13) (Eq. (12), respectively for other homogeniz-
The dressing should have a medium viscosity at a medium ing nozzles). As for the other products, a pilot-plant-scale trial
fat content and high stability. This requires an o/w-emulsion will give the proportionality constant and the exponents.
type with a fat fraction of 50±60 %. As emulsifier, Lacprodan- Having thus determined the required specific energy the
60 has been chosen. A mean droplet diameter below 5 lm homogenizing pressure is easily calculated. For scale-up, this
ensures a high stability in this viscosity range. Higher tonnages pressure has to be kept constant. In order to simplify the scale-
per year may be achieved in a semi-continuous process. up, the number of orifices should be multiplied without
changing geometry.
60 % vegetable oil in water, emulsifier: Lacprodan-60
mean droplet diameter x3,2 / µm
1.0 100
7 Summary
viscosity η / Pa s at 100 s-1
(a) (b)
0.8
Product design, in general, involves first the definition of the
0.6
10 toothed required product quality. On the basis of the quality
colloid mill
0.4 parameters as well as special marketing and production
ηe → x3,2 features, the product recipe can be defined. Knowing the
0.2
x3,2 → Ev
aspired quality and the predefined recipe, the property
0.0
0 1 2 3 4 5
1
105 106 107 function has to be measured. Thus, the required product
mean droplet diameter x3,2 / µm spec. energy Ev / (J/m3) microstructure will be defined. In the case of emulsions, the
Figure 9. Product design for a dressing based on the property function (left-hand
microstructure is characterized by the size of the droplets and
side) and the process function (right-hand side). the structure built up by the droplets and high-molecular
additives. Process functions are then determined using the
In Fig. 9 the determination of the property function for the specific energy for continuous processes or the power density
viscosity (a), as well as the process function for this process (b) and the residence time for batch processes, respectively. In a
is depicted. At an oil content of 60 %, the target viscosity limited number of pilot-plant trials, the exponents and the
of » 500 mPa s at 100 s±1 of this pseudoplastic emulsion is proportionality factor of the process functions have to be
achieved at a mean droplet size of » 4 lm. The viscosity of the determined. Using these functions, emulsification processes
emulsion is high enough to work with a rotor-stator system are easily designed, optimized and scaled up. The determina-
(such as a toothed colloid mill). This machine may be easily tion of process functions in emulsification was depicted in
used in a semi-continuous process. The process function detail. Product design was finally shown for three food
(Fig. 9b) has been determined in a pilot-plant trial. A specific emulsions of different properties.
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