Feature Report
Engineering Practice
Sensing Change
In Batch Reactors
A new method for controlling temperature
and monitoring processes can improve
the economic performance of batch reactors
Robert Ashe David Littlejohn, Alison Nordon,
Ashe Morris Ltd. and Pamela Allan, University of Strathclyde
T
he batch reactor is the workhorse
of the fine chemical and phar-
maceutical industries. Within it,
many different unit operations
are performed such as chemical reac-
tions, bioreactions, crystallization, dis-
tillation and dissolution. Despite their
significance to the industry, batch
reactors have been controlled by the
same underlying method for the past
50 years. This article discusses a rela-
tively straightforward design change,
constant flux control, which delivers
compelling benefits to both tempera-
ture control and process monitoring.
These two aspects of batch reac-
tor control, temperature control and
process monitoring, are particularly
important to manufacturing econom-
ics. Good temperature control is gen-
erally desirable and particularly so
where product change is influenced
by temperature (for example, crys-
tallization, polymerization, chemical
reactions and temperature sensitive
materials). Conventional batch reac-
tors tend to respond slowly to heat
load changes. They also suffer from
a variety of localized temperature
deviations even when the bulk tem-
perature appears satisfactory.
Product quality, yield and produc-
tivity can be optimized by employing
ideal process methods. In many cases,
however, the ideal process method is
linked to factors that can vary from
batch to batch. The only way to employ
ideal process methods under these
conditions is to link process control de-
cisions (such as addition rate, reaction
56 Chemical Engineering www.che.com March 2008
time and cooling rates) to realtime
process analytical data. Although opti-
cal analytical instruments can be used
for this purpose, they can present the
user with significant problems (for ex-
ample, cost, flexibility, reliability, foul-
ing, calibration, ease of use, and area
classification) when employed in the
manufacturing environment.
New designs of the jacket for batch
reactors, such as a variable-geometry
heat-transfer surface, allow the user
to regulate both jacket area and jacket
temperature in realtime. This not only
addresses long-standing temperature-
control problems but also enables very
sensitive heat-balance measurements
to be made. This latter capability pro-
vides a simple and versatile process
analytical technology (PAT) tool.
Temperature control
One of the most intractable problems
of scale up is that of temperature con-
trol. Good temperature control in a
batch reactor needs to take account
of two factors. First, the temperature
controller needs to be able to hold the
bulk product temperature at the de-
sired value and respond to changes in
the heating or cooling load in a timely
manner. Second, the wall temperature
in the reactor needs to be maintained
at levels that do not adversely affect
the product.
A typical heating and cooling sys-
tem for a conventional batch reac-
tor is shown in Figure 1. The reactor
body is surrounded by an outer jacket
through which heat transfer fluid is
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Figure 1. A conventional batch reactor
is surrounded by an outer jacket through
which heat transfer fluid is circulated
circulated. On larger vessels, multiple
injection points are used to improve
distribution of the heat transfer fluid
within the jacket.
The cooling or heating power of the
reactor is controlled by regulating the
jacket temperature. This is achieved
by injecting fresh hot or cold heat-
transfer fluid into the circulation loop
as required (an alternative arrange-
ment uses external heat exchangers
to raise or lower the heat transfer
fluid temperature).
There are two common designs of re-
actor jacket (Figure 2). The most famil-
iar is the one-piece jacket, which forms
an outer chamber around the vessel.
Heat transfer fluid is injected tangen-
tially into the jacket at velocities in
excess of 10 m/s. This promotes mixing
and dispersion of heat transfer fluid
within the jacket. The other common
arrangement is the “half coil” jacket.
The half coil jacket is fabricated as a
series of pipes cut longitudinally and
welded around the outside of the ves-
sel. Heat transfer fluid travels in a plug
flow manner through the channels.
Apart from size, one of the most ob-
vious differences between small and
large reactors is relative heat-trans-
fer area. A typical 5,000-L reactor, for
example, has 30 cm2 of heat transfer
surface per liter of product. By con-
trast, a 1-L lab reactor has more than
1,000 cm2/L. Thus, for the same ther-
mal duty, the wall temperature of the
5,000-L reactor has to be 30 times hot-
ter (or colder) than a 1-L vessel.
Operating reactor jackets at extreme


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Figure 2. Two kinds of conventional batch reactors are the single
jacket (left) and the half coil jacket (right) vessels
temperatures can damage the product.
The problem is further compounded
by the fact that jacket temperature is
a poor guide to the internal wall tem-
perature. The graph in Figure 3 shows
the relationship between vessel wall
temperature and the process-side film
coefficient under conditions where the
jacket temperature and product tem-
perature remain constant.
The process-side film coefficient is
a measure of how easily heat can be
transmitted between the product and
the vessel wall. Factors that contrib-
ute to low film coefficients include
high product viscosities, low thermal
conductivity and poor agitation. In
many operations, the film coefficient
can change significantly during the
process cycle with the result that a
safe jacket temperature at one stage
can cause surface burning or freez-
ing at another. To protect the prod-
uct from extreme wall temperatures,
plant operators have to set jacket
temperature limits. However, setting
these to cope with low film coefficients
at one part of the process means that
the heat transfer capacity has to be
restricted for the whole process cycle.
This leads to unnecessarily long cycle
times. A better solution is to monitor
the wall temperature directly and use
this to adjust the jacket temperature
as necessary. Such measurements,
however, are not practical in tradi-
tional batch reactors.
Restricting jacket temperature pro-
vides a measure of protection for the
product. It does not eliminate hot or
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The severity and frequency of
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Figure 4. A constant-flux control reactor is
efficient, proportional-integral- made up of multiple, small heat-transfer chan-
derivative (PID) control set- nels rather than the one or two large heating-
tings and prevailing conditions and-cooling elements traditionally employed
of the heat transfer fluid. This
problem is an inherent weakness of fluid. The split jacket concept, how-
using jacket temperature as the pri- ever, has the drawback that processes
mary control parameter. often have changing liquid levels. To
One other cause of hot (or cold) spots cope with this, the split point for the
is the “dry wall” effect. Any heated (or lower jacket has to be set at a low
cooled) wall surface inside the ves- level. This severely limits the heat
sel, that is not covered by process transfer capacity.
fluid, will get significantly hotter (or Sluggish temperature control is a
colder as applicable) than the process problem associated with large batch
temperature. Product which splashes reactors and is responsible for slow
onto this surface is exposed to more and erratic temperature control of
extreme heating or cooling conditions. the product. This can be particularly
The traditional solution to this prob- undesirable for processes like crystal-
lem is to use a split jacket. This is a lization where the required cooling
heating and cooling jacket with upper load can change rapidly at nucleation.
and lower sections. By switching off With conventional batch reactors, the
the upper section of jacket, the user turnover rate of heat transfer fluid
can restrict the heat transfer surface in the jacket tends to fall as the ves-
to a zone which is covered by process sel size increases. The turnover rate
Chemical Engineering www.che.com March 2008 57
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Figure 6. Butyl acetate concentration (from off-line GC data) and en-
thalpy data at 30, 40 and 50°C are plotted against time for standard reac-
Figure 5. The above chart profiles the tempera- tions carried out in the 10-L constant-flux reactor. Mean data from the
ture curves for an esterifiction reaction (at 40°C) standard reaction are plotted from five repeat reactions (at 40°C) with error
carried out in the 10-L constant flux reactor and in bars representing ± the standard deviation of the results from five repeat
a 5-L conventional reactor, plotted against time standard reactions. The start of the butanol addition was at zero seconds

in a conventional 5,000-L reactor
jacket, for example, is about 50 times
slower than that of a 1-L reactor. This
is the primary cause for temperature
control problems on large systems.
Historically, users of batch reactors
have employed software solutions to
compensate for slow jacket-turnover
rates. This, however, means imposing
more extreme temperature shifts in
the heat transfer fluid entering the
jacket. Although this can deliver mod-
est improvements to response speed,
it does so with the expense of creating
more severe hot or cold spots within
the jacket.
The problems of controlling temper-
ature in batch reactors are related to
hardware design, and for this reason
they need a hardware solution. One
solution is a reactor with a constant
(heat) flux control system as shown in
Figure 4.
The constant flux jacket. This con-
figuration is made up of multiple,
small heat-transfer channels rather
than one or two large heating and
cooling elements. Each heat transfer
channel is a pipe, which is clamped or
welded around the external surface of
the vessel (or in some cases these may
be internal coils) and is connected to
a multi-port piston valve. A control-
ler regulates the valve position and
as it does so, heat transfer elements
open and close in a cascade fashion. A
second control loop regulates the tem-
perature of the heat transfer fluid. By
varying the number of coils in service,
the control system is effectively regu-
lating heat transfer area. This means
58 Chemical Engineering www.che.com March 2008
that it can alter heating or cooling
power without changing the jacket
heat flux (hence constant flux).
The constant flux jacket has sig-
nificant advantages over conventional
jackets. Transient hot or cold spots as-
sociated with heat load changes can
be eliminated, since the heating or
cooling power can be altered without
changing the jacket temperature. The
jacket also functions like a split jacket,
which can be set at any height to suit
the process level. This can even vary
as the process level changes.
The turnover rate of the heat trans-
fer fluid in the constant flux jacket
is very high. A 5,000-L constant flux
reactor, for example, has a jacket
turnover rate that is equivalent to, or
better than, a conventional 1-L labora-
tory reactor. This means that temper-
ature-control dynamics are virtually
unaffected by scale.
The control characteristics of the
constant flux jacket have been com-
pared with conventional reactors in
both simulation studies and live tests.
In both cases, the control capabilities
of the constant flux jacket have been
found to be significantly faster and
more stable than conventional ves-
sels. Figure 5 profiles a reaction be-
tween butanol and acetic anhydride
using 1,1,3,3-tetramethylguanidine
as the catalyst. The experiment was
repeated in a conventional 5-L reac-
tor and a 10-L reactor with a constant
flux jacket.
When the reaction was performed in
a conventional 5-L reactor (grey line)
the initial temperature dip is caused
by the cooling effect of the butanol ad-
dition (which is added at room tem-
perature). As the reaction starts, the
process temperature suffers a signifi-
cant overshoot followed by a small but
prolonged undershoot. The blue line
shows the same experiment performed
in a 10-L constant flux controlled reac-
tor. Even though this vessel is larger,
the overshoot and undershoot effects
are virtually eliminated to give near
perfect temperature control.
Process monitoring
The function of reactor jackets is to
add or remove heat. Where this heat
can be measured, however, it can also
serve as a valuable PAT tool. Unfor-
tunately, erratic temperature shifts
associated with temperature control
in conventional reactor jackets make
such measurements unreliable and
difficult to perform. Constant flux
jackets, by contrast, have essentially
constant jacket temperatures, and
thus, the heat can be measured by a
simple heat-balance technique.
Figure 6 shows the results of a heat
balance measurement performed
during a chemical reaction. In this
experiment, the change in enthalpy
was monitored during the formation
of butyl acetate. The reaction was
repeated at three different tempera-
tures and the enthalpy trends show
good correlation with changes in the
concentration of butyl acetate deter-
mined by gas chromatography.
Heat balance measurement is an ef-
fective way of sensing change in batch
reactors. As a PAT tool, it is multi pur-
pose, simple to use, non-intrusive and
requires very little calibration. Heat
balance measurement can be used for
monitoring process change, internal
wall temperatures and heat transfer
coefficients. The same set of instru-
ments and calibration settings are
used whether monitoring chemical
reactions, crystallization or biopro-
cesses. The practical uses for heat bal-
ance measurement include end-point
detection, addition control, crystalli-
zation control and control of bioreac-
tors. In heating or cooling duties (for
example, evaporation, distillation,
heat up and cool down) the wall tem-
peratures in the vessel can be moni-
tored from the temperature and heat
balance data. This allows the user to
regulate the jacket temperature ac-
cording to the observed internal-wall
temperature. This means faster heat-
ing and cooling without exposing the
product to damage from excessively
hot or cold wall temperatures.
Authors
Robert Ashe (Ashe Morris
Ltd., The Heath Business
& Technical Park, Runcor,
Cheshire, WA7 4QX, U.K.;
Phone: + 44 (0) 1928 51 54
54; Email: robert.ashe@ash-
emorris.com) is a chemical
engineer and has worked in
the batch process industries
for 30 years. For most of this
time he has been closely in-
volved with the design and
operation of batch process equipment. In 1990
he started working on the idea of variable-area
heat transfer surfaces for batch vessels. In 2000
he co-founded a company with David Morris and
together they built and tested a variable area
batch reactor. Variable area reactors have now
been successfully developed for use in lab, pilot
scale and manufacturing systems. He is continu-
ing to develop uses for this technology as a pro-
cess analytical tool.
David Littlejohn (Depart-
ment of Pure and Applied
Chemistry, University of
Strathclyde, Glasgow, Scot-
land, G1 1XL, U.K.; Phone:
+44 (0)141 548 2067 Fax:
+44 (0)141 548 4212; Email:
d.littlejohn@strath.ac.uk) re-
ceived his B.S. and Ph.D. in
chemistry from the University
of Strathclyde. After a period
working at ICI, he returned
to Strathclyde in 1981 and has been Professor
of Analytical Chemistry at the University since
1988. He is currently head of the Department
of Pure and Applied Chemistry. His activities in
the development and application of inline, online
and non-invasive methods of process monitoring
cover a range of techniques and data analysis
methods, including NMR, NIR, MIR, and Raman
spectrometries, acoustic techniques and mass
spectrometry. David is a founding member of
the Centre for Process Analytics and Control
Technology (CPACT), a multi-disciplinary indus-
try-university collaboration devoted to research,
technology translation and training in realtime
monitoring, process optimization and control.
Conclusions
Constant flux control affects the me-
chanical design of the external cooling
jacket and temperature control valve.
With this design, temperature control
is not only faster and more stable, but
the problem of hot and cold spots in
the jacket is also eliminated. The sta-
bility of the jacket temperature makes
accurate and sensitive heat-balance
measurement possible. This provides
a non-intrusive tool for monitoring
most of the common unit operations
carried out in batch reactors. Further-
more, as the constant flux technology
is independent of reactor size, the ben-
efits can be realized at development,
pilot and manufacturing scales.  ■
Edited by Matthew Phelan
Acknowledgements
The authors acknowledge the contri-
butions from Katy Basford, Martin de
Cecco and Maryann Ehly with respect
to some information used in Figure 6.
Alison Nordon (Department
of Pure and Applied Chemis-
try, University of Strathclyde,
Glasgow, Scotland, G1 1XL,
U.K.; Phone: +44 (0)141 548
3044; Fax: +44 (0)141 548 4212;
Email: alison.nordon@strath.
ac.uk) is a lecturer and Royal
Society University Research
Fellow in the Department of
Pure and Applied Chemistry
at the University of Strath-
clyde. Alison obtained a B.S. (Hons) in Chemistry
and a Ph.D. in solid-state NMR spectroscopy from
the University of Durham. She then moved to
the Department of Pure and Applied Chemistry
at the University of Strathclyde where she held
research fellow and senior research fellow posts
with the CPACT. In 2004, she was awarded a
Royal Society University Research Fellowship
to work on the development of non-invasive ac-
tive acoustic techniques for process monitoring
and control. Alison’s current research interests
are the development of non-invasive and in situ
spectroscopic measurements (NMR, optical tech-
niques and acoustics) for process monitoring and
control, chemometrics and signal processing.
Pamela Allan (Department
of Pure and Applied Chemis-
try, University of Strathclyde,
Glasgow, Scotland, G1 1XL,
U.K.; Email: pamela.allan@
strath.ac.uk) received her un-
dergraduate M.S. in ‘Forensic
and Analytical Chemistry’ at
the University of Strathclyde
in Glasgow. She has held a
studentship from CPACT to
carry out research with Pro-
fessor Littlejohn at Strathclyde since October
2004, and is now finalizing her Ph.D. thesis.
Allan is an affiliate member of the Royal Soci-
ety of Chemistry and a member of the Society of
Chemical Industry.
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