SOLID-LIQUID CONTINOUS STIRRED TANK REACTOR (SL-CSTR)

RIBEIRO, F.
FREIRE, F. G.; MORAES, R.; LEMOS, F.; RAMOA

Abstract

Its presented a laboratory viable well mixed continuous reactor geometry able to oper-
ate with fine divided solids without recurring to a sintered filter.
g
It was found that for a solid with diameters until 1m, 3.7 cm 3 density can be efficiently
mixed with water and the overflowing outflow contains less than 1% of the inner con-
centration of solids.
The main objective of this device is to be applied to the study of heterogenous catalytic
liquid reactions where the constance reactor liquid volume and the amount of catalyst
inside the reactor is of paramount importance for chemical kinetic studies.

keywords: laboratory solid-liquid CSTR, heterogeneous CSTR, solid-liquid separation,

multifunction reactors.

Introduction

Human needs are taking reaction engineering to new paradigms. Ficher Tropsch, Biomass
to liquid, vegetable oils hydrogention/transalkylation and much more synthetic fuel pro-
duction and other low temperature chemical commodities are requiring SL-CSTR or
even gas-liquid-solid three-phasic continuos thank reactors.
Studying solid-liquid reactions in the laboratory can be easily done in continuos fixed
bed tubular or slurry reactors . However, when these reactions need to be done in con-
tinuos mixed reactors (SL-CSTR), solid-liquid separation can be a problem. Usually,
the solid-liquid separation is guaranteed by a filter at the outlet.
When the solid to be studied has little particles ( m diameter) clogging can occur
making it difficult to control the liquid level and there is always the doubt if the segre-
gated catalyst powder is contributing or not to the reaction.
There are several industrial systems solving this problem with more or less success. The
importance in this systems to retain the maximum solids inside the reactor as possible
are of environmental and/or economical importance. The environmental importance
is related with the usual heavy metal content of catalysts and with their disposal and
Date: 26-05-2009.
1
2 RIBEIRO, F.
FREIRE, F. G.; MORAES, R.; LEMOS, F.; RAMOA

manipulation when they accumulate in the distillation columns and in all the other
equipment after the reactor or when they escape to the purges, effluents and/or are
burned in final environmental treatments and go, for instance, to chimneys.
One of the possible geometries industrially used for SL-CSTR is the two bodies reactor
described as reactor/decanter system (Figure - 1). This system is known to be highly
efficient for retaining the fine catalyst particles, however, usually a further separation
unity is necessary after the decanter to diminish the environmental problems already
described. One of the problems of this system is the necessity of having a recycling
hight concentrated solids current from the decanter to the reactor. This flow is difficult
to control and have clogging problems, besides the energy consuming pumping system.

Figure 1. Two bodies reactor, reactor/decanter system.

Our motivation was to implement this kind of reactor at a laboratory scale to achieve
an easy to use design for chemical kinetics and mechanistic studies.

Methods

The geometrical and operating conditions where chosen to simulate a industrial sys-
tem, namely retention time in the order of 1.5 hr, particle size and density and solid
concentration in the order of 50 g/L.

3.1. Reactor Geometries

All studied reactors have a common geometry (Figure - 2), changing only the curvature
and position of the bulkhead for liquid level control and decanter plates (Figure - 3). In
Table 1, we can find the reactor dimensions and the differences between them.
The geometrical differences between the reactors gave origin to different volume distri-
bution, between the reactor and decanter, see Table 2.
 SOLID-LIQUID CONTINOUS STIRRED TANK REACTOR (SL-CSTR) 3

Figure 2. Reactor/decanter geometrie.

Figure 3. Reactor/decanter geometries system.

3.2. Materials
All reactors were built in P erspex
R
.
A laboratory magnetic stirrer with spin speed control was used. The magnetic stir bar
was 3.8 x 0.8 cm. All tests were performed at atmospheric pressure and ambient
g
temperature. Taped water was used as liquid phase (density considered as 1 cm 3 ). A
industrial hydrogenation catalyst was used as solid phase. The solids have a mean stokes
diameter of 10m, a minimum of 1m and a maximum of 100m. The wet particles
g
have a mean specific density of =3.7 cm 3 . The water inlet flow was imposed and
controlled with a metering pump ().

3.3. Operation Mode

The tests begins putting a determined amount of catalyst and a magnetic stirrer in the
reactor and the water inlet opened afterwords. All tests toke 1 hr after the firsts drops
ml
run out from the reactor. The flow was varied between 2.5, 3.0 and 3.5 min , stirrer speed
from 500 to 900 rpm in 100 rpm steps and with solid mass 5 g, 10 g and 15g. As the
three reactors have different volumes, the initial solid concentrations is a bit different in
each reactor (see Table 3).
4 RIBEIRO, F.
FREIRE, F. G.; MORAES, R.; LEMOS, F.; RAMOA

Table 1. Reactors dimensions

Reactor
dimension A B C
(cm)
a 13.0
b 7.0
c 0.6 1.4 1.4
d 14.1
e 5.6 5.3 1.0
f 0.4 1.6 0.6
g 7.6 7.0 7.1
h 8.6 8.5 8.4
i 1.4 0.9 0.8
j 1.7 2.1 1.8
i+j 3.1 3.0 2.6
bulkhead curve curve curve
decanter plate curve curve flat

Table 2. Reactor-decanter volumes distribution

section volume (cm3 ) A B C

reactor 271 239 234
decanter 49 41 46
total 320 280 280

Table 3. Volume, initial concentrations and porositys for each reactor.

Reactor A B&C
Volume (cm ) 3 320 280
Initial mass (g) [S]* (g/L)  (%) [S]* (g/L)  (%)
5 15.6 99.58 17.9 99.52
10 31.3 99.16 35.7 99.03
15 46.9 98.73 53.6 98.55
* [S] - reactor initial solid concentration

At the end of each test, the reactor inlet suspension was filtered, dried and weighted.
The calculated efficiencies () were calculated as in equation (1).

(initial catalyst mass) (f inal catalyst mass)

(1) (%) = [1 ] 100%
(initial catalyst mass)
 SOLID-LIQUID CONTINOUS STIRRED TANK REACTOR (SL-CSTR) 5

The initial porositys () were calculated as in equation (2).

initial catalyst mass
reactor volume
(2) (%) = 100%
reactor volume

and the initial solid concentration [S] in g/L ais in equation (3).
initial catalyst mass (g)
(3) [S](g/L) =
reactor volume (L)

Retention time in the settling section (not stirred), can be calculated (equation 4)
for the different reactors and operating conditions. In Table 4, are presented the these
times.
reactor volume
(4) = (min)
f low

Table 4. Retention time for each reactor function of the flow.

Flow (min)
(cm3 /min) A B C
2.5 19.6 16.4 18.4
3.0 16.3 13.7 15.3
3.5 14.0 11.7 13.1

Results

It was found that for all geometries, the most important influencing condition on ef-
ficiency was the concentration of solids in reactor. In Figure 4, its represented as
function of [S] for all reactors at different stirrer speeds and for higher flow (lowers ).
Other influencing effect is . In Figure 5, its represented as function of (indepen-
dently of the reactor where was obtained) for three stirrer speeds (rpm).
6 RIBEIRO, F.
FREIRE, F. G.; MORAES, R.; LEMOS, F.; RAMOA

Figure 4. [S] and stirrer speed influence on

Figure 5. and stirrer speed influence on