Analysis and modelling of a batch cooling process for cosmetics

Pr Olsson
Department of Chemical Engineering, Lund Institute of Technology, January 2005
Abstract
This MSc thesis was performed in cooperation with Tetra Pak Stainless Equipment in Jakarta, Indonesia. The task
was to analyse and model the cooling for batchwise production of cosmetics in agitated vessels. Most cosmetics are
oil in water emulsions, which make rheological properties such as the viscosity very important. Experiments were
performed in a pilot equipment. The first tests were performed with water then a water solution with 0.5% Carbopol
was used to simulate the rheological behaviour of a high viscosity emulsion. The varied parameters were the agitator
speed and the cooling water flow. The results show a great importance of a close clearance agitator when a high
viscosity product is processed and also importance of a turbulent flow in the jacket. The cooling was modelled in
MATLAB and a graphical user-friendly interface was developed into a cooling simulator to make future simulations
easier. To fit the simulations with the results from the experiments the constant before, C, and the exponent on, a,
Reynolds number in the Nusselt relation for the inner heat transfer coefficient were varied. No obvious relation was
found between these variables and the geometry of the vessel.
energy consumption or reduce the cost of the
equipment.

Introduction
Emulsions are normally produced batch wise in
vessels with batch sizes up to 20,000 kg. The tanks
usually have agitator systems that consist of more
than one type of agitator. For products with high
viscosity close clearance agitators are used, for
example scrapers, to improve the agitation. For the
emulsification step a high-shear rotor/stator mixer, a
so-called homogenizer, can be used. The tank is
equipped with a jacket for heating and cooling of the
product.

Theoretical background
Heat transfer
Dimensionless numbers are essential for heat transfer
calculations. The following dimensionless numbers
are used in this article:
Reynolds number

Re =

A typical process includes the following steps: fill the

batch vessel with hot water, add premixed and
preheated water-soluble ingredients, add surfactants
and structure builders and heat to 70-90C. Waxes are
melted and mixed in a separate vessel and added
through the homogenizer. After the emulsification the
product is cooled in the vessel under gentle agitation.
The product is often sensitive in this phase and loss of
structure, separation or crystallisation can occur.

dh v

(1)

where dh is the hydraulic diameter, v the velocity of

fluid, the density of fluid and the dynamic
viscosity of the fluid.
For agitation Reynolds number is defined as:
Re' =

For the conventional technology the cooling stands

for about 60% of the time consumption. It is desirable
to reduce the batch time and especially the time for
cooling, because of the sensitivity of the product
during this phase.

D2 N

(2)

where D is the diameter of the agitator and N the

agitator speed in rev/s.
Nusselt number

The aim of this thesis is to analyse and model the

batch process, especially the cooling step, for
cosmetics production. Through a better understanding
it might be possible to reduce the batch time, reduce

Nu =

h dv
k

(3)

where h is a local heat transfer coefficient, dv the

diameter of the vessel and k the thermal conductivity
of the fluid.

Q = M v Cpv

(9)

dt

where Mv is the mass of the liquid in the vessel and T

the temperature of the liquid in the vessel.

Prandtl number
Pr =

Cp
k

Combining these three equations give following

ordinary differential equation:

(4)

where Cp is the specific heat capacity of the fluid.

m j Cp j
dT
=
T T j , in + (T j , in T ) e Y
dt M v Cp v

The heat transfer in a vessel can be represented by the

overall heat transfer coefficient, U. For a wall with a
thickness dxw and a thermal conductivity kw the
overall heat transfer coefficient, U, can be calculated
as:

1
1
1 dx w
1
1
= +
+
+
+
U hi ff i
kw
ff j h j

= K

(6)

= ks N

k s = 35 n n / (1n )

(7)

(13)

Other correlations have also been developed for

anchor agitators, for example Rieger and Novk [4]
who presented following relationship:

where mj is the mass flow rate in the jacket, Tj,out and

Tj,in the temperature in to and out from the jacket,
respectively. The heat transmission through the wall:

Q = U A Tlm

(12)

where ks is the Otto-Metzner constant and N the

agitator speed (rev/s). Investigations with proximity
agitators have disclosed ks being dependent on the
power law index, n. Sestk, Zitn and Houska [3]
expressed following correlation for anchor agitators:

Three energy balances can describe the heat

transferred in the vessel. First the heat absorbed by
the cooling water:

Q = m j Cp j (T j , out T j , in )

(11)

The following simple relation from Metzner and Otto

[2] can be used to calculate the shear rate arising from
the agitation:

For the outside heat transfer coefficient the constant C

and the exponent a depend on the type of jacket while
they for the inside heat transfer coefficient depend on
the agitator type and geometry of the vessel.

(10)

where is the shear stress (Pa), the shear rate (s-1), K

is called the consistency (Pa sn) and n the power-law
index (-).

0.14

= C Re a Pr 0.33

Rheology
The Power law model (11) was used to describe the
rheological behaviour of an emulsion.

(5)

The heat transfer coefficient at the inside and at the

outside of the vessel wall can be calculated with a
Nusselt relation, (6). [1]

Nu w

where Y = U A

m j Cp j

where ffi and ffj represents the fouling factors while hi

and hj represents the heat transfer coefficient at the
inner and the outer side of the vessel wall,
respectively.

dT

k s = n 2.21 / (n 1)

(14)
Finally, Beckner and Smith [5] suggested another
correlation:

(8)

k s = 31 (1 n )

where A is the total heat transfer area and Tlm the

logarithmic mean temperature difference. The last
balance is the heat emitted from the product:

(15)

A comparison between the different correlations as a

function of n is plotted in Figure 1. For the result of
Rieger and Novak ks is approaching infinity for
decreasing n. Beckner and Smiths result predict zero
ks values for n approaching unity. It seems that Sestk
& Zitn present the best correlation when products
with a wide range of power law indices are processed.

Table 1 Rheological measurement.

Temp (C)
20
40
60
80

Reologica StressTech
K (Pa sn)
n
19,191
0,294
18,425
0,2753
18,077
0,2565
17,325
0,2421

Model
A model was developed to fit the results from the
experiments. Results from previous investigations
were analysed to find the most suitable correlations.
For the modelling work MATLAB was used and the
model was integrated in a GUI, Graphical User
Interface, to make further simulations easier, see
Figure 2.

Figure 1 How ks depend on the power law index.

Different correlations are compared.
Materials and methods
Experiments were performed in a 30 L pilot
equipment. The batch vessel has a double agitator
system with a central impeller and a rotating anchor
with scrapers, and the jacket type is conventional. A
homogenizer is placed in the bottom of the vessel to
create the emulsion. The temperature in the vessel
was measured during the cooling from 80C and for
20-25 minutes. The first tests were performed with
water after which a water solution with 0.5%
Carbopol was used to simulate the rheological
behaviour of a high viscosity emulsion. The rpm of
the agitators and the cooling water flow were varied
in the tests.

Figure 2 The developed Graphical User Interface,

called VC 1.0.

To calculate the outside heat transfer coefficient the

Nusselt relation (6) was used with C = 0.023 and a =
0.8, which is true for a spirally baffled jacket. For the
inside heat transfer coefficient, C and a had to be
specified in the simulator.
Equation (10) is the ordinary differential equation that
was used in the model to calculate the temperature in
the vessel during the cooling.

A sample of the Carbopol solution was analysed with

two different rheometers to confirm the obtained
results, first a Bohlin VOR rheometer was used and
then a Reologica StressTech rheometer. The
measurements were carried out at 20C, 40C, 60C
and 80C to cover the temperature interval used in the
tests. The consistency, K, and the Power law index, n,
were obtained from the analysis. The results from the
two rheometers were similar and the values for the
Reologica StressTech rheometer are in Table 1.

Following assumptions were done in the model:

Perfect mixing in the vessel, i.e. the

temperature in the vessel homogenous. This
of course is not true when a product with
very high viscosity is processed.
There is a constant distance (pitch) between
the baffles in the jacket.
No leakages take place between the baffles
in the jacket. The baffles are only welded at
one side and a small gap at the other side
will give some leakage, which will decrease
the outside heat transfer coefficient a little.

The fouling at the inside and outside of the

vessel wall is neglected.

Emulsion tests
The first tests were performed with varied cooling
water flow and constant agitation in the vessel. The
result is presented in Figure 5.

Results
Water tests
There was as expected a decrease in the cooling time
when the cooling water flow was increased, see
Figure 3.

80
Flow
Flow
Flow
Flow

Temperature centre, T (C)

70

23.7 l/min
21.65 l/min
16.11 l/min
5.82 l/min

60

50

40

30

20

10
15
Cooling time (min)

20

25

Figure 5 The flow of cooling water was varied at

constant agitation. The scraper was running at 50
rpm and the impeller at 100 rpm.
Figure 3 Time for cooling from 80C to 20C at
different cooling water flow.

These results show that when cooling a product with

high viscosity the change in flow of cooling water
will make a very little difference in the cooling time,
as long as you have some turbulence in the jacket.
The overall heat transfer will then be limited by the
heat transfer coefficient at the inside of the vessel. To
increase the heat transfer coefficient on the inside of
the vessel wall good agitation is important. The
following tests were performed with varied agitation
at constant flow of cooling water. The result is plotted
in Figure 6.

The curve is flattening out and when the flow in the

jacket becomes fully turbulent, at about 30 l/min,
further increase in the cooling water flow will not
affect the cooling time. The explanation of this
optimal cooling water flow is that the inside heat
transfer coefficient will be more dominating when the
cooling water flow is turbulent.
The cooling time was decreased when the speed of
the agitators was increased, which can be seen in
Figure 4.

80
Scraper
Scraper
Scraper
Scraper
Scraper

Temperature centre, T (C)

70

80
Scraper 20 rpm, Impeller 40 rpm
Scraper 80 rpm, Impeller 152 rpm

Temperature centre, Tm (C)

70

60

50

20
20
80
80
50

rpm,
rpm,
rpm,
rpm,
rpm,

Impeller
Impeller
Impeller
Impeller
Impeller

40 rpm
152 rpm
40 rpm
152 rpm
100 rpm

60

50

40

30

40
20

10
15
Cooling time (min)

20

25

30

Figure 6 The agitation was varied at constant flow of

chilled water, 24 l/min.

20

10

8
10
12
Cooling Time (min)

14

16

18

20

An increase in the rpm of the anchor agitator gives a

decrease in the cooling time, as expected. But only a
very small change in the cooling time was obtained
when the rpm of the central impeller was changed and
the rpm of the anchor agitator held constant. This

Figure 4 The agitation was varied with constant flow

of cooling water, 22.5 l/min.

shows the great importance of a close clearance

agitator when a high viscosity product is processed.

Conclusions and future work

The model for batch cooling in a vessel is to a great
extent depending on the geometry of the vessel and
the types of agitators. The performed simulations are
not enough to find any relation between the constant,
C, the exponent, a, and the geometry of the vessel. It
is obvious that C not only depends on the geometry of
the vessel.

Simulations
Simulations were done with the same conditions as
for the experiments to evaluate the model used in the
program. The constant, C, and the exponent, a, were
varied to fit the results from the simulations and the
experiments. When C was varied a was held constant
and then on the contrary.

The presented model and developed interface can be

used to simulate a batch cooling process and match
the result with real experiments made on similar
equipment. It can be used for better understanding of
the cooling step, sensitivity analysis, determination of
the most important variables, etc.

Figure 7 shows the result from a water simulation.

The values used for the simulations are presented in
table 2.

The rheological properties of the product are of great

importance when modelling the processing of a NonNewtonian fluid. A rheometer is necessary to
determine the consistency, K, and the power law
index, n, when the Power law model is used for the
modelling work.
In the future more tests have to be done to validate
and improve the model. Tests on larger equipment are
necessary to see if the model is valid also when the
geometries are scaled up.
Figure 7 Simulation with anchor 20 rpm and impeller
40 rpm. The simulation coincides with the line for the
experiment.

References
[1]
Coulson J. M.; Richardson J. F.; with
Backhurst J. R. and Harker J. H. Chemical
Engineering vol. 1; Pergamon Press: Oxford,
1990, 4th edition.
[2]
Metzner A. B.; Otto R. E., Agitation of NonNewtonian fluids, A.I.Ch.E. Journal, 1957, 3,
3-10.
[3]
Sestak J.; Zitny R.; Houska M., AnchorAgitated Systems: Power Input Correlation for
Pseudoplastic and Thixotropic Fluids in
Equilibrium, A.I.Ch.E. Journal, 1986, 32(1),
155-158.
[4]
Rieger F.; Novk V., Power Consumption of
Agitators in Highly Viscous Non-Newtonian
Liquids, Trans. Inst. Chem. Eng., 1973, 51,
T105.
[5]
Beckner J. L.; Smith J. M., Anchor-Agitated
Systems: Power Input with Newtonian and
Pseudoplastic Fluids, Trans. Inst. Chem. Eng.,
1966, 44, T224.

Table 2 Values for water simulations.

Anchor rpm
20
80
80

C
0.21
0.13
0.21

a
0.667
0.667
0.63

To get a good fit between the simulations and

experiments the constant, C, and the exponent, a, had
to be reduced when the rpm of the anchor agitator
was increased.
The emulsion simulations gave higher values of C,
but just as for the water simulations there was a
decrease of C and a with increased rpm of the anchor
agitator. The values for the emulsion simulations are
presented in Table 3.
Table 3 Values for emulsion simulations.
Anchor rpm
20
50
80
50
80

C
1.15
0.80
0.65
1.15
1.15

a
0.667
0.667
0.667
0.58
0.54