Compartment reactor 1273

Naoto Ohmura Research Article

Takafumi Horie
Norihisa Kumagai Process Intensification of Emulsion
Tatsuyuki Esaki
Takaki Yamazaki Polymerization Using a Compartment Reactor
Department of Chemical Attempts were made to intensify continuous emulsion polymerization using a
Science and Engineering, compartment reactor consisting of three well-mixing compartments. The goal of
Graduate School of this intensification is to obtain a stable and monodisperse particle size as well as
Engineering, Kobe University, high monomer conversion, by controlling the mixing under continuous opera-
Kobe, Japan. tion. A two-bladed paddle impeller was used in the first compartment to intensify
the dispersibility and reactivity in the aqueous phase, while a rotating disk was
used in the third compartment to avoid excessive flocculation of the polymer par-
ticles. In the second compartment, a two-bladed turbine impeller or a rotating
disk was used. The compartment reactor successfully obtained much higher
monomer conversion and also more stable and monodisperse particles than a sin-
gle continuous stirred-tank reactor. The oscillations of the mean particle size were
greatly suppressed by spatially different mixing operations.

Keywords: Compartment reactor, Continuous emulsion polymerization, Function modules,

Process intensification
Received: January 14, 2012; revised: March 25, 2012; accepted: April 11, 2012
DOI: 10.1002/ceat.201200034

1 Introduction to control the processing history. On the other hand, an ideal

Process intensification brings technological innovations to
drastically enhance energy efficiency and process performance,
thus contributing toward a sustainable society. In the chemical
industry, reactors, which are at the heart of chemical processes,
have received more attention than any other unit operation in
the context of intensification. Various intensification methods
for chemical reactors have been proposed. Conversion from a
batch reactor to continuous processing is one of the promising
methods that can drastically reduce reactor size and reaction
time. Stonestreet and Harvey [1] numerically showed that the
intensification of a batch saponification process by conversion
to continuous processing in an oscillatory baffled reactor
(OBR) resulted in a 100-fold reduction in reactor size (from
50 to 0.5 m3) and the OBR achieved the batch product specifi-
cation in a residence time (12 min) one-tenth that of the batch
reactor (2 h).
As Real et al. [2] described, it is crucial for process intensifi-
cation to enhance momentum, mass and heat transfer rates
and to give every molecule the same processing experience. A
continuous stirred-tank reactor (CSTR) has a broad residence
time distribution (RTD). It is therefore difficult for the CSTR
– a relatively wide PSD, the multiplicity of steady states [21],
Correspondence: Dr. N. Ohmura (ohmura@kobe-u.ac.jp), Department
of Chemical Science and Engineering, Graduate School of Engineering,
Kobe University, 1-1 Rokko-dai, Nada-ku, Kobe 657-8501, Japan.
plug flow reactor (PFR) is preferable for process intensification
based on the conversion of a batch reactor to continuous pro-
cessing. The ideal PFR has no mixing or diffusion along the
flow path plus high local mixing intensity and, consequently,
has an extremely narrow RTD. In PFR, each element of fluid
experiences exactly the same processing history. This helps re-
duce byproducts and reactor size. Due to backmixing, a simple
tubular reactor is not able to attain an ideal plug flow state. It
is therefore a crucial technological task to determine how to
approximate an ideal plug flow state. CSTR in series [3–5],
spinning-disk reactors [6], OBR [1, 7], Taylor-Couette reactors
[8–13], continuous tube-CSTR reactors [14], pulsed sieve plate
columns [15, 16], and pulsed packed columns [17, 18] are ex-
amples of intensified PFR.
Emulsion polymerization, an important industrial process
able to combine high polymerization rates with high molecular
weight [19], contains the important steps of particle nuclea-
tion and particle growth. When a batch or semi-batch reactor
is used, particle nucleation is usually completed early in the
polymerization, so that particle nucleation and particle growth
are virtually consecutive-rate processes [20]. Consequently, the
batch and semi-batch processes normally result in a narrow
particle size distribution (PSD). In a continuous reactor, on
the other hand, particle nucleation and particle growth occur
simultaneously, causing various operational difficulties such as
and self-sustaining oscillations in monomer conversion
[22–25]. The oscillations in monomer conversion are due to
the mechanism of periodic particle generations proposed by

Chem. Eng. Technol. 2012, 35, No. 7, 1273–1280 © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.cet-journal.com
1274
Kiparissides et al. [26]. This suggested mechanism leads to the
periodic formation of discrete particle populations and, conse-
quently, to fluctuations in the polymerization rate, conversion,
particle size, and other properties, synchronously [27]. On the
other hand, one of the authors found that, even while constant
monomer conversion was maintained in a steady state, the
particle size of latex particles varied with a very large time scale
[28]. A similar oscillatory behavior in continuous mini-emul-
sion polymerization was observed by Aizpurua et al. [29]. Our
previous studies [28] suggested that a large time scale variation
of the particle size can occur even under steady-state monomer
conversion, through competitive interaction of particle growth
and flocculation processes. The mechanism of the oscillations
in particle size is as follows: Oligomers and primary particles
are continuously generated via homogeneous nucleation. Due
to the wide RTD of the particles in a single CSTR, the primary
particles quickly flocculate to large particles, under the condi-
tion of sub-critical micelle concentration (CMC). Conse-
quently, the mean particle size becomes large. After the num-
ber of large particles has decreased by washing out the
matured particles in the effluent stream, a lot of new small par-
ticles appear in the reactor. Consequently, the mean particle
size becomes small. We successfully reproduced these kinds of
oscillation by numerical simulations using a stochastic model
based on the above mechanism [30]. In order to overcome the
above-mentioned oscillations in particle size and to lead to
process intensification, Horie et al. [31] proposed the com-
partment reactor shown in Fig. 1, consisting of three well-mix-
ing compartments, to bring the mixing characteristics close to
those of a PFR and to divide the polymerization events. Their
preliminary results showed that the compartment reactor
could obtain high monomer conversion and a stable and nar-
row PSD as compared with a single CSTR.
The compartment reactor has the additional advantage that
each compartment can keep a different non-equilibrium stea-
dy state with respect to each other. This indicates that each
compartment can be conducted under independent opera-
tional conditions and a steady and stable process can be at-
tained by converting an unsteady operation into a steady one
a) empty reactor b) reactor with polymerization underway
Figure 1. Overview of a compartment reactor.
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N. Ohmura et al.
under spatially different conditions. In order to make full use
of this advantage, a crucial issue is how to obtain the optimum
conditions for each compartment to efficiently intensify the
performance of the whole reactor. This paper will discuss a
process intensification method of continuous emulsion poly-
merization using a compartment reactor conducted by spa-
tially different mixing operations.
2 Strategy of Intensification Based on a
Function Module Representation
The present work set the goal of obtaining a stable and mono-
disperse particle size of latex as well as high monomer conver-
sion, by controlling the mixing under continuous operation. A
setup of two to three CSTR in series is easier to scale up and
has a higher degree of freedom for the mixing operation than
the compartment reactor at the present stage. However, our fi-
nal target is to develop a novel intensified reactor through the
parts-to-the-whole coevolutional process under the restriction
or feedback from the whole to the parts. The restriction from
the whole plays an important role for the evolution and devel-
opment of a novel reactor. From the above point of view, the
compartment reactor is suitable for our research policy.
As shown in Fig. 2, according to the coagulative model for
particle nucleation originally proposed by Feeney et al. [32],
emulsion polymerization of vinyl acetate consists of the fol-
lowing events: (1) radical initiation, (2) growth of oligomeric
radicals, (3) entry of oligomeric radicals into micelles or exist-
ing polymer particles, (4) homogeneous nucleation of oligo-
meric radicals and formation of primary particles, (5) floccula-
tion of primary particles, (6) polymerization growth, and
(7) flocculation of primary particles onto matured particles.
With regard to the mixing operation, strong agitation en-
hances the dispersibility and reactivity to obtain a higher
monomer conversion, while it is difficult to control the PSD
due to excessive flocculation. When a single CSTR is used, all
the events mentioned above occur simultaneously in the tank
reactor. This means that the reactor has conflicting events as
regards the mixing operation. The authors there-
fore tried to spatially decouple the conflicting
events using a compartment reactor.
First, an emulsion polymerization reactor was
categorized into four function modules based on
the function module representation proposed by
Freund and Sundmacher [33] (Fig. 3). The first
function module, called Contacting (Co) in this
work, refers to a physical process, i.e., dispersion of
monomer, initiator and emulsifier in the aqueous
phase and efficient mutual contact by agitation.
The second function module, called Activating
(Ac), works by radical initiation. The third func-
tion module, called Chemical Reaction (CR), is re-
lated to the oligomeric reaction in the aqueous
phase, the entry of oligomeric radicals into mi-
celles or existing polymer particles, homogeneous
nucleation of oligomeric radicals, and the forma-
tion of primary particles. The fourth function
module, called Particle Growth (PG), has the role
Chem. Eng. Technol. 2012, 35, No. 7, 1273–1280
 Compartment reactor 1275

ler is used in the first compartment to intensify the

Adsorption Adsorption dispersibility and reactivity in the aqueous phase,
Captured on monomer on existing while a rotating disk is used in the third compart-
by Micelles droplets particles ment to avoid excessive flocculation of the polymer
particles. In the second compartment, it is neces-
+ = sary to balance competing goals regarding mixing:
Flocculation of strong agitation for the enhancement of oligomer
primary particles
growth in the aqueous phase and mild agitation
Ho
Homogenous
nucleation
nuc for the nucleation of primary particles. Thus, a
paddle impeller or a rotating disk was used in the
R MR + MnR +
+ second compartment.
M M M
Polymerization
growth
Hydrophilic Hydrophobic
3 Experimental
+ =
3.1 Compartment Reactor
Flocculation onto
mature particles The present work used the same compartment re-
Figure 2. Coagulative model for particle nucleation. actor as the previous one [31, 34], but with differ-
ent impellers. As shown in Fig. 1, the reactor was
divided into three well-mixing compartments. The
of particle growth of the polymers. The second to fourth func- reactor was set vertically, and the lower, middle and upper
tion modules refer to the above-mentioned polymerization compartment were named the first, second and third compart-
events. Strong agitation is suitable for the functions of the Co ment, respectively. The first and third compartments had vol-
and Ac modules to enhance the reactivity, while mild agitation umes of 67 mL and the second compartment had a volume of
is suitable for the PG module to avoid excessive flocculation. 66 mL. The total volume of the reactor was therefore 200 mL.
The rates of the Co and Ac modules are so fast that these can Each compartment was divided by a Teflon® plate. The plate
occur almost simultaneously. The functions of Co and Ac can had four equally spaced holes (2 mm in diameter) along the
therefore be considered in a lump as Co-Ac. Strictly speaking, circumference of a circle at 2 mm inside of the inner cylinder
it is impossible to completely separate between module 1 wall of the reactor, for feeding the reactants to the next com-
(Co-Ac) and module 2 (CR). At the present stage, the focus is partment. These compartments were separately installed with
on determining the main event in each compartment. The water jackets to keep the reaction temperature constant.
first, second and third compartments were assigned to the
Co-Ac, CR and PG function modules, respectively. This means
that the compartment reactor has a clear distinction between 3.2 Emulsion Polymerization with the Compartment
the roles of each of the compartments with regard to these Reactor
three function modules. The PG function module contains
flocculation of primary particles, polymerization growth and Fig. 4 presents a schematic of the experimental apparatus. The
flocculation of primary particles onto matured particles. recipe for continuous emulsion polymerization is shown in
Hence, flocculation is considered to be a key function to influ- Tab. 1. Before starting each experiment, dissolved oxygen in
ence the particle size distribution. A two-bladed paddle impel- the aqueous mixture of emulsifier and initiator was completely
expelled by feeding nitrogen gas for a
sufficient time. As shown in Fig. 4, ni-
Polymeriza
on reactor trogen gas was continuously fed into
func
on modules the reservoir of the aqueous mixture of
emulsifier and initiator during the ex-
periment. Furthermore, the compart-
ment reactor was completely filled with
the solution, without an air zone. It
can therefore be considered that there
are no effects of air/oxygen gas. This
reaction system is very sensitive to the
initial conditions. Hence, the startup
3rd procedure was rigorously fixed in all
1st compartment 2nd compartment
ntt compartment
experiments. Initially, the first reactor
was filled with an emulsified mix-
ture (A). The reaction was started by
Figure 3. Representation of the continuous emulsion polymerization process in terms of a adding the initiator solution (B) to
potential sequence of function modules. the reactor. Ammonium peroxodisul-

Chem. Eng. Technol. 2012, 35, No. 7, 1273–1280 © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.cet-journal.com
1276 N. Ohmura et al.

of the compartment. The two-bladed turbine impeller has a

Figure 4. Experimental apparatus: (1) monomer, (2) nitrogen
gas, (3) aqueous mixture of emulsifier and initiator, (4) pump,
(5) stirrer, (6) compartment reactor, (7) temperature-controlled
bath, and (8) sample collector.
diameter of 20 mm and a blade width of 10 mm, while the disk
has a diameter of 30 mm and a width of 1 mm. The impeller
configurations are shown in Fig. 5. The first compartment into
which monomer and aqueous solutions of initiator and emul-
sifier were fed was always equipped with a two-bladed turbine
impeller, to well disperse the monomer droplets and to avoid
phase separation between water and monomer, while the sec-
ond and third compartments were equipped with a two-bladed
turbine impeller or a disk. In comparison, Case 3, in which all
compartments were equipped with a two-bladed turbine im-
peller, was also performed. The rotational speed of the impel-
lers was fixed at 250 rpm.

3.4 Mixing Characteristics

fate (water-soluble initiator) (special grade; Wako Pure Chem-
ical Industries) and sodium dodecyl sulfate (emulsifier) (first Before conducting the emulsion polymerization experiments,
grade; Wako Pure Chemical Industries) were premixed in an- the mixing characteristics of the compartment reactor were in-
other stirred tank. The vinyl acetate monomer (special grade; vestigated by the step response method with an electric con-
Wako Pure Chemical Industries) (D) and the aqueous solution ductivity cell. An aqueous solution of NaCl was used as tracer.
of initiator and emulsifier (C) were fed separately and continu- The tracer response curve in every case showed good agree-
ously into the reactor at a constant feed rate (8:1 v/v) by a ment with three continuous stirred tanks in series. This indi-
peristaltic pump (MP-3N; Tokyo Rikakikai Co.). The mean cates that, from the macroscopic viewpoint, uniform mixing
residence time, s, was determined by dividing the total effec- could be attained in every compartment.
tive volume of the reactor (200 mL) by the total feed rate of
the two streams. The temperature of the water fed into the
water jacket of the reactor was kept at 58 ± 1.0 °C. From the as-
pect of industrial emulsion polymerization, a very low concen-
tration of the emulsifier is preferable. Hence, the emulsifier
concentration in the reactor and in the feed was set
initially at 0.0026 kg m–3, considerably lower than
the CMC of 0.008 kg m–3, to eliminate the effect of Table 1. Recipe of continuous emulsion polymerization.
reactions within monomer-swollen micelles. The
Reagents Quantity
mean residence time was adjusted to 24.7 min. The
feed and effluent flow rates were precisely con- (A) Initial content of reactor Distilled water 175 mL
trolled to keep them constant by the peristaltic Vinyl acetate monomer 22 g
pump. The effluent solution from the compart-
ment reactor was sampled at fixed time intervals. Sodium dodecyl sulfate 0.15 g
The duration of each sampling was no more than (B) Initiator solution Distilled water 3.0 mL
1 min. Polymerization in each solution was
stopped with hydroquinone (special grade; Wako Ammonium peroxodisulfate 0.25 g
Pure Chemical Industries). Monomer conversion (C) Initiator and emulsifier solution tank Distilled water 5.0 L
was determined by measuring the mass of the coa-
Ammonium peroxodisulfate 6.25 g
gulated latex particles after adding an aqueous
solution of aluminum(III) chloride hexahydrate Sodium dodecyl sulfate 3.75 g
(2.5 kg m–3) (special grade; Wako Pure Chemical (D) Monomer tank Vinyl acetate monomer 500 mL
Indstries), rinsing with distilled water, and drying.
The PSD was obtained using a laser diffraction
particle size analyzer (SALD-300V Model-2; Shi-
madzu) on a number basis for percentage.
Case 1 Case 2 Case 3

3rd 3rd 3rd

3.3 Configuration of the Impellers Configurations of
Disk Disk Turbine
2nd 2nd 2nd
impellers Turbine Disk Turbine
The impellers were fixed on a single stirring rod to
1st 1st 1st
rotate at the same rotation speed. Each compart- Turbine Turbine Turbine
ment had a two-bladed turbine impeller of stain-
less steel or a Teflon disk that was set in the middle Figure 5. Impeller configurations.

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 Compartment reactor 1277

4 Results and Discussion Case 1

4.1 Monomer Conversion

Fig. 6 shows the time-dependent monomer conversion

for each compartment. The reaction time is expressed
3rd Compartment
in a non-dimensional form obtained by dividing by
2ndCompartment
the mean residence time of the whole reactor. The
1st Compartment
samples were taken simultaneously from each com-
partment. In all cases, the conversion of each compart-
ment reached a steady state when t/s was larger than
3. Almost 100 % outlet conversion was reached for the
compartment reactor. Plots over 100 % were measure-
ment errors due to residual initiator and terminator.
This high conversion could not be achieved for a single
CSTR in our previous study [28]. The monomer con-
version obtained by a single CSTR (s = 30 min, Case 2
V = 196 mL) was about 70 %, under the same reaction
conditions. In an ideal single CSTR, the feed is homo-
geneously mixed instantly in the whole reactor. Hence,
a large amount of unreacted monomer is in the efflu-
ent. On the other hand, the effluent of unreacted 3rd Compartment
monomer was drastically reduced, owing to the sharp 2ndCompartment
residence time distribution of the feed. Consequently, 1st Compartment
the monomer conversion was much higher than in a
single CSTR.
Case 3 gives the highest conversion in every com-
partment, while Case 1 gives the lowest one, i.e. more
turbine impellers are used, and higher monomer con-
version is obtained in every compartment. This means
that strong agitation enhances the reactivity to obtain
higher monomer conversion, as expected, and the mix- Case 3
ing conditions in the downward compartments affect
the reactivity in the upward compartments. Moreover,
the conversions of the first and the second compart-
ment were about 2–5 % and 37–53 %, respectively. The 3rd Compartment
mean residence times in the first and second compart- 2ndCompartment
ment were 8.2 and 16.4 min, respectively. When a sin- 1st Compartment
gle CSTR was used, the polymerization reaction did
not occur under such a high mean residence time con-
dition. Furthermore, as compared with Cases 1 and 3,
although up to the second compartment the impeller
configuration was the same in both cases, Case 3 gives
a higher monomer conversion in the first and second
compartments compared to Case 1. This can be attrib-
uted to the infinitesimal backmixing through the holes
in the partition plate. It can therefore be considered
that the infinitesimal backmixing through the holes in Figure 6. Time-dependent monomer conversion.
the partition plate has a feedback effect on the poly-
merization reaction. for a long time and grew larger, leading to the coexistence of
small and large particles. Fig. 7 shows the variation of the mean
4.2 Mean Particle Size and Particle Size Distribution particle size with time, obtained in the second and third com-
partments. In Case 3, although the oscillations were relatively
Oscillatory behaviors of the mean particle size were observed suppressed after a certain time, they still remained to some de-
in continuous operation using a single CSTR [17]. The authors gree. On the other hand, in Cases 1 and 2, which used one or
consider these behaviors to be caused by the particle agglom- two rotating disks, the oscillations almost ceased after t/s = 8.
eration induced by the particle size difference. In the present In the second compartment, the time-dependent mean particle
work for the single CSTR conducted at s = 30 min, oscillation size in Case 2 was more stable than that in Case 1. This indi-
was observed since some of the particles stayed in the reactor cates that the compartment reactor with a rotating disk suc-

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1278
cessfully stabilized the particle size by mild agitation to avoid
excessive flocculation of the polymer particles. Each compart-
ment kept a different non-equilibrium steady state with respect
to each other. This implies that the variation of the reaction
state in a batch reactor is converted to a spatial variation in the
compartment reactor. This quenching effect allows the poly-
merization to progress stepwise, which in turn allows the as-
signment of a different function module to each compartment.
It was inferred that the mean residence time was long enough
to achieve high conversion, and short enough to prevent ag-
glomeration induced by the particle size difference. Compar-
ing Fig. 7a with Fig. 7b, no phase lag of the oscillations could
be observed between the two compartments. This indicates
that there is no time delay of the particle size oscillations be-
tween the compartments, owing to the infinitesimal backmix-
ing effect between the compartments.
Fig. 8 shows the PSD obtained from the effluent solution
out of the third compartment in Cases 1 and 3, after the mean
particle size had reached steady state. In both cases, relatively
monodisperse distributions were obtained. Every PSD at dif-
ferent sample times was almost the same, with a mean diame-
a) 2nd compartment
b) 3rd compartment
Figure 7. Time variation of the mean particle size obtained at the second
and third compartments.
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N. Ohmura et al.
ter of about 0.45–0.47 lm in Case 1. The results of the PSD are
not shown in Fig. 8 due to space limitations; however, the PSD
in Case 2 have the same features as in Case 1. On the other
hand, the PSD slightly changed with time and the mean diam-
eter also changed over a wider range in conjunction with the
PSD in Case 3. As for the coefficient of variation (CV) for the
PSD, the values of the CV in Cases 1 and 2 concentrated
around 30 %, while those values in Case 3 took a wider range,
from 26 to 41 %. These results also suggest that the mild mix-
ing due to the rotating disk prevents excessive flocculation of
the polymer particles and stabilizes the PSD. Our previous
work [18] had revealed that the PSD in each compartment was
almost the same. The monomer conversion was raised toward
the downward compartments, as mentioned in the previous
section. These results indicate that the number of particles in-
creases toward the downward compartments. The conclusion
can be drawn that the polymer particles grow quickly to
0.4–0.5 lm via flocculation of the primary particles onto ma-
tured particles without excessive flocculation, and that particle
nucleation is slow compared with particle growth via floccula-
tion.
4.3 Optimization of the Mixing Operating
Conditions
The present work did not achieve to optimize the mixing
operating conditions. The following strategy to optimize
the mixing conditions is considered in future works. In the
first compartment, monomer dispersion is the dominant
factor. Using a high-shear impeller such as a dispersion
blade can be suitable for monomer dispersion. In the sec-
ond compartment, we regard polymerization in the water
phase as the main event. In this case, micro-mixing due to
turbulent flow should be controlled by a turbine impeller.
On the other hand, lower shear flow is suitable for particle
growth without excessive flocculation in the third com-
partment. Hence, a low-shear impeller such as a hydrofoil
impeller, a steep pitch impeller or a rotating disk can be
used in the third compartment. The compartment reactor
has a strong restriction regarding to mixing operation, i.e.
all the impellers are rotated at the same rotational speed.
This means that not only the partial optimization of each
compartment has to be taken into consideration but also
the total optimization of the compartment reactor. This re-
striction is the key factor connecting with each compart-
ment and the whole reactor, and the aim is to develop a
novel intensified reactor through the parts-to-the-whole
coevolutional process under this restriction.
The other thing taken into consideration is a microscop-
ic feedback effect. A microscopic feedback system is not al-
ways necessary for process intensification. However, it can
be considered that quantum leaps in process and/or plant
efficiency are often accomplished by taking advantage of
nonlinear dynamics of systems. In these cases, the feedback
effect plays an important role for process intensification.
Honestly speaking, at the present stage, we do not have a
clear solution for how to deal with the function of the local
feedback or nonlinearity of the system in process design by
Chem. Eng. Technol. 2012, 35, No. 7, 1273–1280

Case 1
τ =9.71
τ =12.15
τ =15.39
Figure 8. PSD obtained from the effluent solution out of the third compartment in Cases 1 and 3 after the mean particle size had reached
steady state.
using the function module representation. Ordinary design
methodologies are predicated on the linear concept that addi-
tive properties are satisfied. Therefore, how to deal with the
function of the local feedback or nonlinearity of the system is
our future subject.
In future work, optimization of the reactor configuration by
intensifying each main event in each compartment will be at-
tempted. For example, as for the separation between Co-Ac
and CR, the effect of decreasing the mean residence time of the
first compartment by reducing the volume will be investigated.
5 Conclusion
This work tried to intensify continuous emulsion polymeriza-
tion using a compartment reactor consisting of three well-mix-
ing compartments. The goal of this intensification is to obtain
Chem. Eng. Technol. 2012, 35, No. 7, 1273–1280 © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Compartment reactor 1279
Case 3
τ =9.71
τ =12.15
τ =15.39
a stable and monodisperse particle size as well as high mono-
mer conversion by controlling the mixing under continuous
operation. An emulsion polymerization reactor was categor-
ized into four function modules, i.e., Contacting, Activating,
Chemical Reaction and Particle Growth, based on the function
module representation proposed by Freund and Sundmacher
[33]. Then, Contacting and Activating were treated together
and the first, second and third compartments were assigned as-
signed to the Contacting-Activating, Chemical Reaction and
Particle Growth function modules, respectively. A two-bladed
turbine impeller was used in the first compartment to intensify
the dispersibility and reactivity in the aqueous phase, while a
rotating disk was used in the third compartment to avoid ex-
cessive flocculation of the polymer particles. In the second
compartment, a two-bladed turbine impeller or a rotating disk
was used.
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1280
The compartment reactor successfully obtained much high-
er monomer conversion than a single CSTR, since the re-
stricted axial dispersion suppressed the effluent of unreacted
monomer. It was found that the mixing conditions in the
downward compartments affect the reactivity in the upward
compartments. For the same mean residence time, polymeriza-
tion occurred in the first and second compartments, though
not in any single CSTR. In addition, there was no time delay
for the transient response of each compartment. This indicates
that the infinitesimal backmixing through the holes in the par-
tition plate has a feedback effect on the polymerization reac-
tion. Furthermore, the compartment reactor successfully pro-
duced stable and monodisperse particles. The oscillations of
the mean particle size were greatly suppressed by different
mixing operations in each compartment. The mild mixing due
to the rotating disk avoids too much flocculation of the poly-
mer particles and effectively stabilizes the PSD.
Each compartment could keep a different nonequilibrium
steady state with respect to each other. This quenching effect is
important from the viewpoint of process intensification be-
cause the process design restricted by the variation of the reac-
tion state in a batch reactor can be converted to that restricted
by spatial variation. The present work therefore shows a possi-
ble process intensification method by converting a batch pro-
cess to a continuous one.
Acknowledgment
The authors wish to thank the technical division of the Insti-
tute of Scientific and Industrial Research of Osaka University
for its technical support. This research was partially supported
by the Ministry of Education, Science, Sports and Culture of
Japan, Grant-in-Aid for Scientific Research (A), 20246115, and
Grant-in-Aid for Challenging Exploratory Research, 23656492.
The authors have declared no conflict of interest.
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