Batch Reactor Control: APACT 2007

Ashe Morris
Batch Reactor Control
APACT 2007
3rd May 2007 Robert Ashe
Ashe Morris Ltd
© Ashe Morris Ltd 2006 (16:00 to 16:30)

Agenda
• Process control
• Constant flux temperature control
• Temperature control
• Process control with analytical data
© Ashe Morris Ltd 2006

Batch reactor control
Improving batch reactor control
Improved method Improved equipment
Temperature
Increased use of feed
control
back control
Continuous improvement Improved heating/cooling system

of process method
Process analytics

Constant flux temperature control
Conventional
Conventional control
control Coflux®® control
Coflux control
T TC
T TC
tj
Patented
Q = U.A.(T-tj) Q = U.A.(T-tj)
Jacket temperature controlled Jacket area controlled

Why use ‘area’ control

T TC
1. Better temperature control
2. Enables sensitive heat monitoring
3. More energy efficient
Patented

Lab
Industrial

Temperature control
Temperature control

Temperature control
A flat temperature line does not

imply good temperature control
T
The temperature sensor only
reveals the product
temperature at one point

Temperature control
Good temperature control
1. Understand the heat flux conditions

2. Good bulk temperature control
3. Uniform jacket temperature
4. No heating or cooling on dry walls

Heat flux
Fixed area/volume ratio = 0.1 m2/litre

300C
290C
TC T
t
Lab system
(25 W/l process heat)
-250C

Heat flux
Fixed area/volume ratio = 0.003 m2/litre

400C
00C
TC T
t
Production system
(25 W/l process heat)
5000 litres
-250C

Heat flux
By limiting the heat transfer area,

the heat flux conditions of large
reactors can be simulated
0.003 m2/litre
0.003 m2/litre
00C
400C
00C 400C
Coflux jacket with reduced
area (25 W/l process heat)

Bulk temperature control
T TC
The quality of bulk temperature control is

primarily determined by the time it takes to
adjust the jacket temperature
tj

A conventional batch reactor jacket takes between 100 and 1000
seconds to alter the jacket temperature
Simulation on 4,000 litre reactor

334.0
Temperature [K]
T TC 333.5
333.0
332.5
332.0
331.5
tj 331.0
330.5
330.0
0 1,000 2,000 3,000 4,000 5,000 6,000
Time [s]
Information by permission of Imperial College
Faster response is achieved by injecting fluid in to the jacket at an extreme

temperature. This however increases the tendency for overshoot.
A Coflux jacket takes less than 10 seconds to adjust the jacket
temperature.
Simulation on 4,000 litre reactor

334.0
Temperature [K]
333.5
T TC 333.0
332.5
332.0
331.5
331.0
330.5
330.0
0 1,000 2,000 3,000 4,000 5,000 6,000
Time [s]
Information by permission of Imperial College
This eliminates sluggish temperature control, overshoot and control hunting.

Uniformity of jacket temperature
Conventional jacket
T TC
The utilities on a typical industrial
heating/cooling system use:
Hot at 1700C
Mid at 200C
Cold at -250C
tj
Transient hot/cold spots can exist which may be 1000C different to

the process temperature (there are no instruments to alert the plant
operator to this).

Uniformity of jacket temperature
T TC
The jacket temperature is constant. A

sudden increasing in cooling/heating load
is responded to by a rapid change in heat
transfer area. This eliminates jacket
hot/cold spots.

Dry wall effects
Dry wall effect No dry wall effect
T TC

Process monitoring
Process monitoring

Heat monitoring
Heat monitoring represents a versatile PAT tool
Total process change

Enthalpy
Power
Rate of process change
Chemical reactions
Polymerisation
Crystallisation
Dissolution
Evaporation/condensation
Fermentation
Mammalian cell growth

Heat measurement
Heat measurement in conventional

reactor jackets is difficult and unreliable.
Variations in jacket temperature obscure
the heat signal
TC T
This is due to large enthalpy variations in

the heating cooling jacket (jacket heat
noise can be 3 orders of magnitude bigger
than the process heat signal)

Heat measurement
By keeping the jacket temperature

constant and varying the heat transfer
area, very sensitive heat measurements
can
T TC
Simple to use (switch on the cooling system).

Calibration free (other than commissioning)
tin Non intrusive
tout Unaffected by process conditions
m
Robust (2 temperature probes and a flow meter)
q = m.Cp(tin – tout)

Hydrolysis of acetic anhydride
80 60000
50 ml
70
6.75 ml
50000 12.5 ml
60 25 ml
40000
50
Enthalpy (kJ)
Enthalpy (kJ)
40
25 ml 30000 50 ml
30 20000
12.5 ml
20
10000
Measured
6.75 ml
10 Theory
0
0
0 1000 2000 3000 4000 5000 6000 0 1000 2000 3000 4000 5000 6000
-10 -10000
Time (s)
Time (s)
1 litre LARA Coflux unit.

Reproduced by permission of Pfizer

1. Heat measurement
Crystallisation
Crystallisation control

1. Heat measurement
Crystallisation
Poor Crystallisation control affects

yield, quality and process cycle time
• Slow filtration (fines blind the filter)

• Loss of yield (fines pass through the filter)
• Low product quality (uneven particle size)
• Long drying times

Crystallisation monitoring
Ice Experiment
Rate of crystallisation Mass of crystals

Heat transfer co
efficient
Te
mp
e ra
tur
e
50 150 250 350 450 550 650 750
Reproduced by permission of Syrris Technologies Ltd

Ideal crystallisation control
Moving set point relies on a

Rate of temperature change of pre-defined recipe (e.g.
process is used as a proxy for cooling curve)
the true process variable
PV
SP
T
Controller
tj

Ideal crystallisation control
True set point is a function
of surface area (of crystals)
SP
True process variable
is rate of crystallisation
PV
?
T
Controller
tj

PV Controller
SP
40000 6
35000 5
30000 Precipitate (kg) 4 T TC

Enthalpy (J)
25000 3
20000 2
15000 1
10000 0
5000 -1
0 -2
-50 50 150 250 350 450 550 650
-5000 -3
Time (s) A
Enthalpy is a more reliable parameter for

determining set point

1. Heat measurement
Controller
SP
PV
450 6
400 5
350 Rate T TC
4
300
(kg/s)
Power (W)
3
250
2
200
1
150
0
100
-1
50
0 -2
-50
-50
50 150 250 350 450 550 650 750
-3 A
Time (s)
Crystallisation heat is the true process variable

1. Heat measurement
Changing viscosity
Ice formation
110 6
5
100
HT Coefficient (100 = initial)
90 3
2
80
1
70 0
HT Coeff
-1
60
Temperature -2
T TC
50 -3
-50 50 150 250 350 450 550 650 750
Time (s)

Coflux® reactors
robert.ashe@ashemorris.com

Batch Reactor Control: APACT 2007

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Ashe Morris

Batch Reactor Control

Ashe Morris Ltd

© Ashe Morris Ltd 2006 (16:00 to 16:30)

• Constant flux temperature control

• Process control with analytical data

© Ashe Morris Ltd 2006

Improving batch reactor control

Improved method Improved equipment

Continuous improvement Improved heating/cooling system

© Ashe Morris Ltd 2006

Jacket temperature controlled Jacket area controlled

© Ashe Morris Ltd 2006

Why use ‘area’ control

1. Better temperature control

2. Enables sensitive heat monitoring

3. More energy efficient

© Ashe Morris Ltd 2006

© Ashe Morris Ltd 2006

© Ashe Morris Ltd 2006

A flat temperature line does not

© Ashe Morris Ltd 2006

Good temperature control

1. Understand the heat flux conditions

© Ashe Morris Ltd 2006

Fixed area/volume ratio = 0.1 m2/litre

© Ashe Morris Ltd 2006

Fixed area/volume ratio = 0.003 m2/litre

© Ashe Morris Ltd 2006

By limiting the heat transfer area,

© Ashe Morris Ltd 2006

Bulk temperature control

The quality of bulk temperature control is

© Ashe Morris Ltd 2006

Simulation on 4,000 litre reactor

Faster response is achieved by injecting fluid in to the jacket at an extreme

Simulation on 4,000 litre reactor

This eliminates sluggish temperature control, overshoot and control hunting.

© Ashe Morris Ltd 2006

Transient hot/cold spots can exist which may be 1000C different to

© Ashe Morris Ltd 2006

The jacket temperature is constant. A

© Ashe Morris Ltd 2006

Dry wall effect No dry wall effect

© Ashe Morris Ltd 2006

© Ashe Morris Ltd 2006

Heat monitoring represents a versatile PAT tool

Total process change

Rate of process change

© Ashe Morris Ltd 2006

Heat measurement in conventional

This is due to large enthalpy variations in

© Ashe Morris Ltd 2006

By keeping the jacket temperature

Simple to use (switch on the cooling system).

© Ashe Morris Ltd 2006

1 litre LARA Coflux unit.

© Ashe Morris Ltd 2006

© Ashe Morris Ltd 2006

Poor Crystallisation control affects

• Slow filtration (fines blind the filter)

© Ashe Morris Ltd 2006

Rate of crystallisation Mass of crystals