Reactor Application • Reactor Application • Reactor Application • Reactor Application

Sizing of Temperature Control Units

for Reactor Applications
 Reactor Application

Precise temperature control has a significant influence on performance and quality in

chemical process engineering. The Unistat range of temperature control systems ensure
accurate temperatures and stable process conditions in research laboratories, pilot
plants and kilo labs worldwide.
 Reactor Applications

Sizing of

Temperature Control Units

for Reactor Applications
Authors: Daniel Huber, Kenneth J. Mackenzie, Dr. Patrick M. Delaney

Precise temperature control has a significant influence on performance and quality in chemical
process engineering. The Unistat range of temperature control systems ensure accurate temperatures
and stable process conditions in research laboratories, pilot plants and kilo labs worldwide.
The Unistat principle has been diversified into a wide range of different system designs to be able to
provide accurate temperature control on these different scales. Calculating the best Unistat for your
chemical process is the subject of these works.

Introduction Energy Balance of a Reactor System

When it comes to chemical reactions in processes, the When performing a chemical transformation A+BC,
right temperature is a crucial factor. Therefore, chem- we have to look at the energy balance of the system.
ical processes need an appropriate and reliable heat- Addition of reagents A and B may require the addition
ing/cooling system. For process engineers it is essential
to find the best possible compromise between yield,
quality, productivity and safety.
Over the years and with the support of process engi-
neers from the chemical and pharmaceutical industry,
the Unistat range has been developed and refined.
This collaboration has ensured that Unistats remain at
the forefront of technology, making them suitable for
controlling the temperature of chemical and bioreac-
tors, autoclaves, reaction blocks & calorimeters in mini,
pilot and distillation plants.
As a result of their thermodynamic characteristics, Un-
istats offer cutting-edge performance regardless of the
application and excelling even under heavily changing
system conditions. To demonstrate the performance
of the Unistat range over 200 case studies have been
carried out. They show the Unistats unique ability to
adapt to process requirements, offering precise stabil-
ity and control: To understand this we first need to un-
derstand the energy balance of a reactor system.

Fig. 1: Syrris Orb Pilot 50 L Scale-up Chemical Reactor

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 Reactor Applications

or removal of heat energy during the chemical process
to ensure a safe and reproducible delivery of compo-
nent C. The requirements for this depend on whether
the reaction is exothermic (heat energy is released to
the surroundings) or endothermic (heat energy is ab-
sorbed from the surroundings).
Energy balance here is defined as the sum of the heat
output or input of the system as equal to zero. To
maintain this balance do we therefore: A apply energy
(heat) to promote the chemical reaction (Endothermic)
to occur. Or B removes energy (cool) to perform the
chemical reaction (Exothermic) in a safe and controlled
manner , to prevent side reactions and increase reac-
tion yield. Too much heat can lead to incorrect chirality
or remove functional groups.

Endothermic Reaction
Activation
Energy
Potential Energy

Products
Released
Energy

Reactants

Reaction Progress

Fig. 2: Shown here is a 20l reactor connected to a Grande Fleur, heating the reaction media to +80 °C.

Exothermic Reaction
Activation
Energy
Potential Energy

Reactants
Released
Energy

Products

Reaction Progress

Fig. 3: Shown here is a 50l reactor connected to an Unistat 510w, cooling the reaction media to -40 °C.

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 Reactor Applications
All reactions require molecules A+B to come together
with sufficient potential energy to transform to product
C. An endothermic reaction requires heat to achieve re-
action initiation, for example heating of a reaction solu-
tion to reflux (see Fig. 2). The potential energy profile )
of an endothermic reaction indicates the activation en-
ergy required to generate product is greater than the
energy released by product formation. Therefore a net
heat gain is required.
In general, exothermic reactions are cooled, often to
sub ambient temperatures and in particular -50 to -78
°C. Shown here is a 50l reactor connected to a Unistat
510w, where we are cooling the reaction media to -40
°C.
Of note in both images above the Huber unit in both
thermal imaging photos show they are thermally inert
and are delivering the required heating/cooling to the
relevant application .
To understand your chemical process, reaction calo-
rimetry has become an invaluable tool for determin-
ing reaction kinetics and optimising known reactions
(dosing profiles, process temperatures etc.), while the
most important feature is the determination of pro-
cess safety, especially when scaling up the process for
production.
Generally, reaction calorimetry data should be availa-
ble before moving the development of a chemical pro-
cess to a larger scale (Kilo/Pilot plant scale). The data
obtained will provide the thermal and kinetic profile of
the reaction, on which the design of the larger scale
experiment and thus, production processes should be
built upon to run the process under safe conditions
Fig. 4: Shown here is a 80l glass lined stainless steel reactor
connected to an Unistat 912w, cooling down to -90 °C.
In standard process development scenarios, the reac-
tion calorimetry analyses take place during identifying
synthetic routes, and afterward during optimization of
the route selected. Reaction calorimetry will be usually
accompanied by thermal screening (determining the
thermal stability of the components/products), to es-
tablish most efficient and safe process.
However, the temperature control of the chemical pro-
cess is only part of the energy balance required. The
thermal properties of the equipment used to carry out
the experiment must be factored in to achieve preci-
sion temperature control.
In the Fig. 4 and 5 we can see heat loss and gains from
the reactor systems to the local environment. On the
Fig. 4 we have a glass lined stainless steel reactor which
has a smaller heat loss to the environment than the
reactor in Fig. 5, a jacketed glass reactor. In addition
to this we can see the reactor stand frame work in the
RHS side image is being cooled via air flow.
We have to look at all materials involved, not only in the
chemical process, but the application and the different
materials involved in the whole system set-up. Each dif-
ferent component will absorb and emit the heat that is
applied at different rates (heat capacity) and be pres-
ent in different masses.
Fig. 5: Shown here is a 50l jacketed glass reactor connected
to an Unistat 510w, cooling the reaction media to -40 °C.
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 Reactor Applications

Required Cooling and Heating Capacity for Key componets that influence temperature
Reactor Systems control across all scales
Using our knowledge from above we can calculate the Information required for sizing:
heating/cooling power required for different size re-
• Reactor (Glass, GLS, SS)
actors. However, before we perform a sizing calcula-
tion for the power requirements for the process being • Impeller (Glass, SS, PTFE)
scaled we need to access the application as a global • Baffles, Samplers etc.
function. By this we have to take into account all mate-
rials that shall be in contact with the heat transfer fluid • Reactor Volume
and the reaction medium. • Reactor Jacket Capacity
This calculation must include the supply lines running • HTF feed and return lines
from the temperature control unit to the application (Weight and capacity)
and their return feed also.

Sizing
For a process where the temperature input, tempera- Mass of System
ture output and flowrates of the heat transfer fluid are  (kg*cp) System
not known we can calculate cooling and heating capac- = the sum of materials (weight by heat capacity)
ity using the following equation.
Reactor weight (including lid), Impellers, Baffles, Tem-
Kilowatts required for heating or cooling perature Probe, HTF hoses/pipes
{[Mass of Materials x Heat Capacity] x Temp. Difference
start to end}/ required time frame Mass of Thermal Fluid
Q =[(kg*cp) System + (kg*cp) Thermal Fluid +  (kg*cp) Thermal Fluid
(kg*cp) Reaction Media] dT/t = the sum of HTF (weight by heat capacity)
If we look at a reactor system and TCU we can break Reactor Jacket, Hoses, Fill Volume of Huber Unit (Esti-
the Mass of Materials component of equation down mated based on unit end temp]
further to 3 components for the mass of materials.

Mass of Reaction Media

 (kg*cp) Reaction Media
= the sum of bulk materials (weight by heat capacity)
Reactor Contents Based on the Bulk Reaction Medium
(Assume reactor is at full capacity)

Fig. 6.1: Mass of System

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 Reactor Applications

Fig. 6.2: Mass of Thermal Fluid Fig. 6.3: Mass of Reaction Media

Q = [ (kg*cp) System + (kg*cp) Thermal Fluid + (kg*cp) Reaction Media] dT/t

Legend:
Q = Power required in kW
[of note a negative value in-
dicates cooling]
kg = kilogram
cp = specific heat capacity
dT = Delta (difference) in
temperature
t = time in seconds

Fig. 6: Components of the Equation

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 Reactor Applications

Worked Example:
Customer would like to cool a 50 l reactor containing
toluene from 120 °C to -30 °C in a time frame of 2.5 h. Fig. 7: Key data required for calculation

Material Weight Specific Heat Apacity m.Cp

Glass 60 kg 0.91 kJ/kgK 54.6

Stainless Steel 10 kg 0.5 kJ/kgK 5
HTF (M60) 25 kg 1.655 kJ/kgK 41.4
Reactor Contents (Toluene) 50 kg 1.612 kJ/kgK 80.6

Calculation
Delta T -150 k
Q =[(kg*cp)Material + (kg*cp)HTF + (kg*cp)Vessel Cont]dT/t
t 9000 s
Q =[59.6 + 41.4 + 80.6 kJ /k]( -150 k) / 9000 s
Q =[181.6 kJ /k] (-150 k) / 9000 s
Q =[181.6 kJ] (-150) / 9000 s
Please Note:
Q = -27,240 kJ / 9000 s
A negative value indicate cooling
Q = -3.0266 kJ/s
power required a positive value
1 kJ/s = 1kW is heating power.
Q = -3.02 kW

Therefore, based on our calculation the custom- From a search of the Huber case studies we can see
er would require 3 kW of cooling power at -30 °C to from the following example in Fig. 8 that in real-world
achieve the desired cool down time. From this calcula- testing we achieved a similar cool down ramp in 2h.
tion we would propose a Unistat 510w system.
Fig. 8: Casestudy
When scaling up a pro-
cess there are some key Jacket temperature
factors in addition to Process temperature
your process calorimetry. Setpoint

Performing a reaction on
benchtop scale we can
The jacket temperature ramps
observe some key data. quickly to -42°C to pull the
process temperature quickly
1. Reactor Volume to to its new setpoint
Jacket Capacity ratio
2. Watts per liter in rela-
tion to HTF in system
3. Flow rate of HTF in Process temperature
system reaches exactly the
new setpoint
By ensuring these values
are accessed in addition
to the process calorim-
etry one can ensure the
scale up of a process is
keeping to the true pa-
rameters of the bench
scale process.

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 Reactor Applications

Required Cooling Capacity

Reactor Condensers
When perfoming applications where heat is applied or
generated there is often the need to condense solvent
vapour by means of reflux or distillation.
If we are applying heat to the application, the cooling
power required should not be greater than this unless
the application is exothermic at elevated temperatures.
Taking in to account heat loss to the local enviroment
due to airflow ove the application. We can assume a
drop in temperature during the phase transistions
from liquid to gas during evapoursation and from gas
to liquid duting condendsation.
As a result if we look at a Unistat 510w on a 50l reac-
tor. We can apply a maximum of 6 kW of heat to the
application to achieve a reflux. If we then assume loss
of energy to atmosphere we are at 4 kW of heat in the
gas phase followed by 2 kW during condesnation from
gas to liquid phases in the condensor. Therefore, on a
50l reactor utilising a 6 kW heater pack at a minimum a
2 kW chiller would be fitted to the condenser.
Please note that certain reactor manufacturers will rate
the cooling power of their condensers based on the
effective cooloing on the internal surface area.

Fig. 9: Required Cooling Capacity Reactor Condensers

Condenser Cooling
∆ kW ≈ 1/3 X

Liquid Phase

Application Heat Gas Phase

X kW from TCU
kW ≈ 2/3 X

Heat applied should not Liquid

exceed maximum available
from TCU.
If application is exothermic,
calorimetry data should
be consulted to calculate
condenser cooling power.

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 Reactor Applications

Closed vs Open System

When it comes to the discussion of should we consider
an open bath circulator versus a hydraulically sealed
circulator there are a few factors to consider. If you
have calculated thermal loadings you may find you
could opt for either but the application should dictate
your requirements.
If we look at two styles of application elevated temper-
atures and subzero temperatures.

Fig. 10: CC-308B on a 1l Radleys Reactor Ready (Open)

Apparatus Size

Reactor Radleys 1L Jacketed

Hoses 2 x 1M

Jacket Fluid M20.190/235.20 (3 litres)

Reactor Content P20.275.50 (0.75 litres)

Agitation Speed 500 rpm

Unit Pump Speed 3500 rpm

PT100 Material PTFE

Delta T- Process + Internal 60 °C

PID TAC Fast, small overshoot

Jacket temperature
Process temperature
Setpoint

Start Temp End Temp Time

Internal 17 °C 195 °C 24 min

Process 11 °C 190 °C 47 min

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 Reactor Applications

Elevated Temperature
Open bath systems typically have a lower watts per liter
ratio due to their larger fill volume, they have a larger
heat loss via the lid aperture.
At elevated temperature HTFs can fume to the atmos-
phere as low boiling components boil out of the fluid.
This can lead to the application area being coated in a
thin layer of HTF.
Closed systems typically have a higher watts per lire
ratio, they are highly insulated against heat loss to at-
mosphere.
At elevated temperatures the expansion of fluid is di-
rected in to a thermally inert expansion tank resulting
in no fuming.

Fig. 11: Chili on a 1l Radleys Reactor Ready (Closed)

Apparatus Size

Reactor Radleys 1L Jacketed

Hoses 2 x 1M

Jacket Fluid M20.190/235.20 (8 litres)

Reactor Content P20.275.50 (0.75 litres)

Agitation Speed 500 rpm

Unit Pump Speed 3500 rpm

PT100 Material PTFE

Delta T- Process + Internal 60 °C

PID TAC Fast, small overshoot

Jacket temperature
Process temperature
Setpoint

Start Temp End Temp Time

Internal 12 °C 195 °C 15 min

Process 16 °C 190 °C 35 min

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 Reactor Applications
Subzero Temperature
When we look at comparing open bath to closed sys-
tem for subzero temperature a key point is the absorp-
tion of heat and of water into thermal fluid via the large
surface area in the bath.
Same as before the low watts per liter and level of sys-
tem insulation can have an effect on rate of cooling.
Fig. 12: Casestudy Ministat 240
with 2 L Radleys jacketed reactor
Performance
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Inspired by temperature
Whilst in both scenarios both open and closed systems
will achieve the desired temperature. One then has to
look at efficiencies of the application and turnaround of
the process. Of course budgets have to be consulted.
However, a long term view based on HTF fluid lifespan,
time taken to perform experiment and productivity
have to be taken into account.
Casestudy 1227: Ministat 240
This case study demonstrates the ability of Ministat 240
with displacement insert to cycle the process temper-
ature in a range from +100 °C to -20 °C, the closeness
of the temperature control and the minimum process
temperature achievable in the process mass.
Performance: Cooling down and heating up in a range
from +100 °C to -20 °C. The Ministat 240 needs ap-
proximately 85 minutes to cool down the reactor from
+100 °C to -20 °C and approximately 35 minutes to
heat it up from -20 °C to +100 °C.
Tmin: The Ministat 240 cools the reactor down to the
minimum achievable process temperature of -25 °C.
Apparatus Size
Reactor Radleys 2L Jacketed
Hoses M16x1; 2 x 1 m
Jacket Fluid M40.165.10
Reactor Content M20.195.20 (1 litres)
Stirrer Speed 200 rpm
Control Process
Lowest achievable temperature Tmin:
Jacket temperature
Process temperature
Setpoint
 Reactor Applications

Casestudy 1221: Petite Fleur

Fig. 13: Casestudy Petite
This case study demonstrates the closeness of the
Fleur with 2 L Radleys
temperature control and the minimum process tem-
jacketed reactor
perature achievable in the process mass.
Performance: This graphic shows the Petite Fleur
cooling the process in a 2-litre glass jacketed reactor
from 100 °C to -20 °C in a time of approximately 80
minutes, hitting and controlling at -20 °C with no over-
shoot. Heating back to 100 °C from -20 °C takes only
26 minutes with the same tight control at the target
temperature.
Tmin: This graphic shows that the process tempera-
ture asymptotes at -27 °C.

Apparatus Size

Reactor Radleys 2L Jacketed

Hoses M16x1; 2 x 1 m

Jacket Fluid M90.055.03

Reactor Content M40.165.10 (1 litres)

Stirrer Speed 200 rpm

Control Process

Performance Lowest achievable temperature Tmin:

Jacket temperature
Process temperature
Setpoint

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 Reactor Applications

Thermal Fluid
(HTF = Heat Transfer Fluid) When selecting a HTF you should
Huber heat transfer fluids have the best thermody- consider the following:
namic and environmentally friendly characteristics. The
choice of the correct fluid is decisive for efficient heat 1. Application material of construction in
transfer. The working temperature range is gene-rally particular seals and gaskets.
the most important criterion for choosing a particular 2. Are you operating an open bath or
fluid. The use of the correct heat transfer fluid guar- hydraulically closed system?
antees reliable and safe operation, optimum tempera-
ture control and a long life. 3. Your pumping capacity.

The majority of heat transfer fluids on the market in- 4. Have you got suitable expansion room
cluding those supplied by Huber are polymer-based in your system to accommodate thermal
fluids as they have excellent specific heat capacities. As expansion of heat transfer fluid.
part of their design, their liner thermal expansion coef- 5. What is your planned operating
ficient is measured. What this means temperature range?
is that when heat is applied the
polymers unfold and can swell 6. What is the viscosity of the fluid over
resulting in a net increase in the your operating temperature range?
volume of fluid in the system. 7. What is the density of the fluid over your
The expansion of the thermal flu- operating temperature range?
ids can be calculated using the
equation formula below.

Formula: Example calculation:

ß x ∆T x V0 What volume change is to be expected with 10 Liter
∆V =
Daverage M20.195/235.20 heated from -20 °C to +100 °C?

∆V = Change of volume
1,025 V0 = 10 liters
ß = Thermal expansion coefficient
t0 = -20°C
1,000 =
∆T Working temperature difference
t1 = +100°C
(Difference t1 final temperature
0,975
- t0 starting temperature) ∆T = t1 – t0 = +100°C - (-20°C) = 120 K

0

V0,950 = Filling volume ß = 10-5/K = 0,00101
D0,925
average
= Average density Daverage = 0,935 g/cm³

0,900
1,025
Change of volume:
0,875
1,000
Average density M20.195/235.20 = 0,935 g/cm³ 0,00101 g/ml/K x 120 K x 10 Liter
0,850
0,975 = 1,296 Liter
0,935 g/cm3
0,825
0,950

0,800
0,925 Result: The volume will expand by approx. 1,3 liters.

0,775
0,900
Tipp: Use an expansion tank to drain vessel jackets
0,750
0,875 into if they have swappable benchtop reactors.
-60 -40 -20 0 20 40 60 80 100 120 140 160 180 200 220 240 °C
0,850

0,825

0,800
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Inspired by temperature

0,775
 Reactor Applications

In addition to measuring of the liner thermal expansion Another factor that can affect temperature control is
coefficient the specific heat capacity of the thermal flu- the viscosity of a thermal fluid. As with most liquids at a
ids is also measured across a range of temperatures. certain temperature you achieve a pour point. Howev-
Meaning we can fully understand the characteristics of er, building up to this we seen an exponential increase
the fluid. in viscosity.
Ensuring you choose the correct thermal fluid for your
application is key to optimized delivery of temperature Case 1: 1:1 Glycol Water in Jacket | SilOil M80 in Vessel
control to your application. t -18 °C in 310 min
Case 2: SilOil M80 in Jacket | SilOil M80 in Vessel
A common choice is a 50:50 mix of glycol water in
t -18 °C in 150 min
benchtop systems. What we can see in Fig. 14 is the
fact that by using a polymer-based heat transfer flu-
id with an improved specific heat capacity we can hit Start Temp End Temp Time
our tMin of 18 °C in over half the time of that with glycol
water. Often customers believe they will make a small Case 1: 100 °C -18 °C 310 min
Glycol Water
cost saving by not using an appropriate HTF. However,
choice of the correct fluid will see productivity signifi- Case 2: 100 °C -18 °C 150 min
SilOil M80
cantly improved and processes speed up from day one.

Fig. 14: Casestudy CC-K6 controlling a 1-liter Labtex reactor

Setpoint
Jacket Temp Glycol Water as HTF
Process Process Temp Glycol lWater as HTF
Jacket SilOil M80 as HTF
Process SilOil M80 as HTF

100

Viscosity 90

[mm2/s] 80

70

60

50

Fig. 15: Viscosity data of Huber HTF 40

M40 oil at varoius temperatures. 30

20

At -40 °C the HTF has a 10

viscosity of 50 mm2/s. 0
-60 -40 -20 0 20 40 60 80 100 120 140 160 180 200 220 240 °C

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 Reactor Applications

This is observed in the following graph where we uti-
lized a Unistat 905 to demonstrate the effect of the
increase in viscosity of thermal fluid and temperature
control. We can see that cooling down to -40 °C is a
steady ramp down. However, at -40 °C the viscosity of
the thermal fluid increases and affects the stability of
the tI curve. This is evident in the temperature of the
evaporator and the return sensor tR also which are be-
fore and after tI in the fluid loop.

Fig. 16: Unistat 905 cooling down to -40 °C

System Pressure
To apply a pressure across a reactor jacket, one would
When it comes to glass reactor applications the ide-
have to shut the reactor jacket outlet with a valve and
al scenario for efficient temperature control is a high
create a dead head pressure across the reactor. A vast
flow, low pressure supply of HTF to the application.
majority of glass reactor manufacturers now fit pres-
However, a lot of concern is generated around system
sure relief devices to prevent this scenario from occur-
pressures. Under German DIN 12876 the maximum
ring.
pump pressure is measured as a dead head pressure
i.e. 0 l/min flow rate. Whereas a standard jacketed reactor will cause a pres-
sure drop due to the HTF entering a large void from a
Pumpenkennlinien
small aperture.

Unistat 510, 510w Many manufacturers promote the high-pressure rates

Unistat 515w that are achievable in their systems but the laws of
Unistat 520w, 525, 525w physics tell us that high pressure is actually detrimental
Unistat 527w, 530w
to flow rates and thermal transfer as shown in system
Unistat 540w
curves in Fig. 18.
bar
Pressure/ /bar
Druck

Increasing
pressure does
not increase
Catalouge data
flow
Pressure (bar)

Pressure (bar)

max pressure

Catalouge data
max flow

Förderstrom
Flow ratel/min
l/min Flow rate (l/min) Flow rate (l/min)

Messung erfolgte nach DIN 12876 mit Wasser bei 20° C

Fig. 17: Example pump curves according to Fig. 18: Example pump curves according to DIN 12876
DIN 12876 with water at 20 °C with water at 20 °C

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Inspired by temperature
 Reactor Applications
To negate the initial startup pressure or a dead head
pressure being applied we can also look at the use of
three options a variable pressure control pump and
automated or manual bypasses.
VPC was developed to protect glass reactors from
damage caused by high fluid pressure. VPC also com-
pensates for changes in viscosity as heat transfer fluid
is heated and cooled. Unistat for typical laboratory ap-
plications have a variable speed pump with soft-start,
and using a pressure sensor can control their maxi-
mum fluid pressure.
This is done by utilizing the pump speed (flowrate) to
pressure correlation. Therefore, by reducing pump
speed the observed pressure will be reduced. In the
Huber systems with a variable speed pump you can
control via either RPM or Pressure mode.
Bypass
Fig. 19: Bypass
VPC Bypass Pressure sensor Rupture disc (provided
(optional) by the responsible body)
Fig. 20: VPC Bypass
Unistat with larger capacities (LHS) can control the
pressure using a pressure sensor and a stepless au-
tomated bypass. Minimal pressure and maximum flow
encourage optimal heat transfer. The VPC allows ena-
bles the best operation while remaining within the de-
fined pressure limits of the application. Placement of
a pressure sensor adjacent to the application and not
TCU will ensure an optimal flow rate of HTF through the
application.
Where a manual bypass is selected to proportion of
the flow to reduce the pressure it should be placed at
the application to ensure efficient temperature control
occurs at the application.
In addition to controlling pressure if we introduce a
mass flow meter we can control on flow to ensure your
desired flow rate is achieved.
If quick disconnects are used on glass applications it is
advised to have a pressure relief device fitted between
the quick disconnect and the application. If HTF is
locked into the glass application jacket a slight raise in
room temperature may lead to an increase in hydraulic
pressure due to thermal expansion of the fluid and net
result in a shattered glass application. Please liaise with
the manufacturer of your glass for their guidelines on
pressure.
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 Reactor Applications

Huber-Unit

Com.G@te
VPC
Pilot ONE

LEVEL
POKO/ALARM
AIF REG-E-PROG
ECS STAND-BY

RS232/RS485
SERIAL
Volume VPC Unipump Pilot
flow Bypass ONE
meter
Temperature cont-
rol with Pilot ONE
CAN Switch Com.G@te Fig. 21: Functional diagram –
flow volume measurement/regulation

PT 100 – object. This charge can be suddenly discharged (such

Resistance Temperature Detector (RTD)
A temperature sensor which contains as a resistor (typ-
ically 100 or 1000 Ohms). The resistance changes with
temperature; this can then be correlated to provide a
temperature reading.
Sensors used in the chemical industry typically fall in to
the following material categories: Stainless steel, Has-
telloy, PTFE or FEP encapsulated.
A Pt100 probes is a resistance thermometer but have
a different coefficient of temperature. Depending on
the platinum used, Pt100 probes have a resistance of
0,385 Ohm/°C. For Pt100 probes, the measuring de-
vice compensates the inherent resistance of the con-
necting cable.
An issue that can arise with RTD is the discharge of stat-
ic electricity depending on the material of construction.
Static electricity is the buildup of electrical charge on an
1 mA measuring signal (Pt100)
Electrostacs +/-
as when a lightning bolt flashes through the sky) or it
can cause two objects to be attracted to one another.
Socks fresh out of the dryer that cling together are a
good example of this attraction in action. Specifically,
static cling is an attraction between two objects with
opposite electrical charges, one positive and one neg-
ative.
If we look at a glass reactor system the potential for a
static discharge is greater when we use a PTFE Pt100 in
the application. To understand this, we need to under-
stand the materials present.
We have two forms of fluid flow in the application.
1. HTF flow from the TCU around the jacket of the re-
actor. This can lead to the glass becoming positivly
charged
2. Reaction media being agitated by the overhead
motor, this media is in contact with the PTFE Pt100
and becoming negatively charged (worsened by
use of buffer solutions)
This is essential a modern-day equivalent to Kelvin Wa-
ter Dropper experiment.
Some of the dependency factors when using glass ap-
paratus and thermofluids are:

Thermofluid • the flow speed

• the electric conductivity of the thermofluid
• the viscosity of the thermofluid
Thermofluid If a static bleed point is not place either from the Pt100
or via the jacket connection of the reactor these is po-
tential for static discharge to occur. The majority of the
occasions this will travel along the Pt100 to the TCU.

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 Reactor Applications

Case Studies These case studies are performed with a medium load-
ed in the reactor. However, we do not mimic exo- or
At Huber we believe that the application is king, whilst
endothermic scenarios.
we manufacture a vast array of liquid based tempera-
ture control units. Whilst calculations give a ball park huber-online.com/casestudies
figure for cooling and heating this is in an ideal world
We have used the data gathered over the years to as-
scenario. To aid the selection of units Huber in collabo-
semble a quick guide for achievable process tempera-
ration with some of our global partners we have run a
tures versus size of reactor.
selection of case studies on glass reactors.

Reactor Achievable Sub Zero Process Tempertures

Size -10 °C -20 °C -30 °C -40 °C -50 °C -60 °C -70 °C -80 °C

0,5 Liter K6 M230 M240/PF Tango CC505/U705 CC805 U815 U905

1 Liter M125/K6 M240/PF Tango U405 CC508 U705 U815 U825/U905

2 Liter M125/K6 M230/240 CC505/PF U425 U705 U815 U825 U905

5 Liter M125 M230/PF M240/GF CC510 U705 U705 U825 U912w

M240 / GF/
10 Liter M240 U405 U430 U510w U620w U825 U912w
CC505

20 Liter M240 Tango U430 U510w U515w U830 U815w U912w

50 Liter Tango U410 U430 U510w U520w U905w U905w U925w

100 Liter U405 U430 U510w U540w U620w U912w U912w U930w

250 Liter U510w U530w U540w U615w U925w U930w U950w U950w

Model abbreviation: M = Ministat, U = Unistat, PF = Petite Fleur, GF = Grande Fleur

Please Note: Data in this table is based on selection of units that fit trends observed in Huber Performed Case
Studies. The data generated from case studies are highlighted in bold. Please note these are guidelines and
can differ depending on local enviroment and reactor contents.

19
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 Reactor Applications
Environmental Considerations
Natural refrigerants are the future. No matter what
needs to be temperature controlled or cooled in the
laboratory: from distillation apparatus through the
analyzer to the research reactor, natural refrigerants
contribute to a positive environmental balance. There
are no limitations in terms of performance and the
safety concerns are unfounded as can be seen in the
common domestic use of these gases as well as the
Conclusions  
When it comes to selection of temperature control
units for your reactor application, the key factor is de-
livery of cooling and heating power in an efficient and
effective manner. By carefully assessing your applica-
tion as a whole and not just the reaction media you can
calculate the effective cooling/heating power required
to deliver your process.
At Huber we have built our knowledge and technology
around the temperature control of chemical applica-
tion by working hand in hand with scientists.
Reliable temperature control of a chemical process is
critical to success and also dependent on an effective
thermal transfer. With traditional “open bath” thermo-
stats limitations occur: The flash point of thermal fluids
at high temperatures is causing a relatively narrow safe
operating temperature range. Degradation of thermal
fluid, due to evaporation, water absorption and oxi-
dation, dramatically reduces the thermal conductivity
of the fluid. The large volume of fluid required to fill a
bath, limits the performance and the dynamics of heat-
20
Inspired by temperature
historical record. When choosing a temperature con-
trol unit, users should keep in mind that the unit will
be in use for many years. During this time, the refriger-
ant has a significant impact on energy consumption. A
choice of refrigerant based on sustainability eliminates
the need for subsequent, costly retrofits and protects
against additional investment due to new regulations
and laws.
ing and cooling. The Unistat principle (Fig. 22), unlike
conventional technology, uses no internal bath. Instead
a low internal volume in conjunction with an expansion
vessel is used to compensate for volume change in-
duced by heating and cooling. This principle reduces
the mass of fluid and as a result dramatically increas-
es the rate of temperature change, achieving cooling
rates of several hundred degrees per hour. Pressure &
Flow High heating and cooling capacities are worthless
if pressure from the pump is too high. Key to good heat
transfer is the pump performance. In order to achieve
optimal circulation, high flow rates with low pump pres-
sure are required. This allows heating and cooling en-
ergy to be transported very effectively by the Unistat so
fast ramp rates are possible (Fig. 24).
Many manufacturers promote the high pressure rates
that are achievable in their systems, but the laws of
physics tell us that high pressure is actually detrimen-
tal to flow rates and thermal transfer. Pressure reduces
flow which causes restricted heat transfer - this has a
Figure 22:
The Unistat
Principle
 Reactor Applications

Selectivity Reaction Speed

Optimum Temperature

Figure 23: Temperature control of a chemical reaction has

Temperature a significant influence on selectivity and reaction rate. The
Interval optimum is often in a narrow temperature interval.

Temperature

dramatic effect on performance. Most glass reactors Author Information 

have a maximum pressure of 0.5 bar - anything above
will compromise the reactor. Pressure creates heat, Daniel Huber started his career at Huber in 1982
therefore, the heat losses associated with high pres- with an apprenticeship which he
sure have a greater impact when trying to achieve low finished as a technician for refrig-
temperatures. For a comparison of thermal dynamics eration technology. With a post-
it is essential to take into account the cooling power graduate degree in business ad-
density [W / l]. Cooling power density is particularly im- ministration from the University of
portant for applications with a continuously changing Offenburg he was appointed CEO being in charge
reaction mass. Precise temperature control and pro- of sales and marketing. His activities focused on
cess stability are crucial factors in obtaining the desired developing global sales and service channels,
temperature result. The better the heat transfer the founding daughter companies in strategically
quicker the temperature change. When endothermic important markets and generally managing the
or exothermic reactions occur, the Unistats impres- company. With the formation of HUBER AG, Dan-
sive ability to react to the process, quick temperature iel became the chairman and runs the operations
changes and an integrated process safety feature, al- together with his brosis.
lows the reaction to be kept under tight control with-
out over or undershoot, resulting in higher purity levels
(Fig. 23). Kenneth J. Mackenzie practical technical back-
ground is supported with an HNC
in Electronic Engineering and an
MBA. Starting with Huber as a dis-
Temperature °C tributor in the UK, he joined Huber
directly in 1999 as an Internation-
al Sales Manager gaining 20-years of application
experience from around the world across many
industries.

Dr. Patrick M. Delaney is the managing director

Setpoint temperature
Jacket temperature
Process Temperature
Time (min)
Figure 24: Regulation of an exothermic reaction in a
reactor is fast and reliable and destruction of the reactor
contents is avoided.
of Huber in UK and Ireland since
2017. Following his honours De-
gress in Applied Chemistry and
PHD in Organic Sysnthesis, he then
went on to work for a CRO working
on scales from medicinal chemistry (mg) to pro-
cess chemistry (kg). Upon leaving the laboratory
he went in to the reactor design and supply field,
making him the ideal contact person for selecting
the right equipment for optimum thermal trans-
fer of your chemical process.

21
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 Peter Huber Kältemaschinenbau AG
Werner-von-Siemens-Straße 1
77656 Offenburg, Germany
www.huber-online.com

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