Case Study Batch Reaction Lesson 1

Thermal Safety Case Study- Lesson 1
This case study shows through an example of a batch

reaction how to systematically assess the thermal risk
related to runaway reactions.
It was prepared by R.Perrayon and P.Lerena based on
the knowledge of the Swiss Safety Institute (Basel,
Switzerland)
Lesson 1 is a step by step procedure to allow a
preliminary evaluation of both severity and probability
using simple experimental techniques (SCREENING).
Summary of lessons
What is risk?
Traditionally the risk is defined as the product of the
severity of a possible incident times its probability of
occurrence. Hence the risk assessment requires the
evaluation of both the severity and probability.
The following lessons are a guide to a systematic
evaluation of the risks of a chemical process.
Lesson 1 is a step by step procedure to allow a
preliminary evaluation of both severity and
probability using simple experimental techniques
(SCREENING).
Lesson 2 expands the study through the use of more
data if the conclusion of the previous SCREENING is
that the thermal risks of the process are high.
Lesson 3 summarizes the results obtained in the
previous lessons through the construction of a
COOLING FAILURE SCENARIO and the assessment
of its CRITICALITY.
Lesson 4 analyzes the operating conditions required
to mantain the process under thermal control as well
as the measures that should be taken to prevent an
incident from occuring.
Case study :
Batch reaction
Lesson 1
The following is a short description
of an actual manufacturing
procedure for the substitution of
para-chloro-nitrobenzene:
A quantity of 1-chloro-4-nitrobenzene is
charged in a reactor with ammonia
(27% by weight in water).
The autoclave is then heated in about 3
hours to 195C and maintained at this
temperature for 5 hours. The pressure
finally reaches 41-42 atms.
After this time, the reaction mass is
colled down to room temperature.
Cl NO
2
H
2
N
2 NH
3
NH
4
Cl NO
2
Reaction scheme
+
+
Process data
Charge
Compound Mass kmol Molar ratio
(kg)
1-Chloro-4-
nitro-benzene 423 2.7 1
Ammonia 27% 2024 32.1 12
(pure NH
3
)
Total 2447
Reactor data
Stage Reaction mass Approximate
(kg) volume (m
3
)
Initial 2447* 2.6
Final 2447* 2.6
*In a batch process, the initial and final
reaction mass are the same.
Lesson 1
The results of lesson 1
should be summarized in
risk analysis forms 1 and 2.
Using these forms fill in the
headings and the BATCH
SIZE section of form 1 for
the process data shown
opposite.
Case study : Batch reaction Thermal Data of Reaction
BASIC DATA FOR RISK ANALYSIS FORM 1
Product: Batch reaction Ident No:
Location: Case study Proc. dated:
Author of risk analysis: ( Your name ) Date: ( actual date )
DESCRIPTION OF SYNTHESIS REACTION (USE ONE SHEET PER STEP)
BATCH SIZE 2.7 kmol
at the start 2.6 m
3
2447 kg
at the end 2.6 m
3
2447 kg
Case study : Batch reaction Thermal Stability
BASIC DATA FOR RISK ANALYSIS FORM 0h
CHARACTERISTIC DATA OF DECOMPOSITION REACTIONS
(USE SEVERAL SHEETS IF NECESSARY)
Lesson 1
Use risk analysis forms 1 and 2 to summarize the results
DESCRIPTION OF SYNTHESIS REACTION (USE ONE SHEET PER STEP)
BATCH SIZE 2.7 kmol
at the start 2.6 m
3
2447 kg
at the end 2.6 m
3
2447 kg
BASIC DATA FOR RISK ANALYSIS FORM 0h
CHARACTERISTIC DATA OF DECOMPOSITION REACTIONS
(USE SEVERAL SHEETS IF NECESSARY)
Lesson 1
Case study :
Batch reaction
Lesson 1
Assessment of severity
Lesson 1
In order to obtain a preliminary
evaluation (SCREENING) of the
severity of the chemical process
under study, one should
determine the following data:
Heat of the desired
reaction
Heat of the
decomposition reaction
Specific heat capacity of
the reaction mixture
Lesson 1
In order to evaluate the heat of the desired
reaction and the heat of the decomposition
reaction two thermograms were supplied by
the thermal safety laboratory.
A linear temperature ramp from 23C to 450C
was used in both measurements (scan rate
4Cmin
-1
).
The overall potential thermogram shows an
endothermic signal (fusion of the product) and
two overlapping exothermic signals. The first
signal equals a potential of +30 kJkg
-1
and the
second ones a total potential of -750 kJkg
-1
.
A sample of the reaction mixture after
completing the desired reaction (final reaction
mixture thermogram) shows, excepted the
endotherm, only one peak of -500 kJkg
-1
. This
energy is in the same temperature range of the
second exothermic peak of the overall potential
thermogram.
Overall potential thermogram:
Quantitative differential thermal analysis of a
mixture of the starting materials.
Final reaction mixture thermogram:
Quantitative differential thermal analysis of the
final reaction mixture.
-0.6
-0.4
-0.2
0
0.2
0.4
0.6
0.8
1
1.2
0 100 200 300 400
-500 kJkg
-1
+30 kJkg
-1
Heat release rate (Wg
-1
)
scan rate: 4Cmin
-1
Temperature (C)
Heat release rate ( Wg
-1
)
-1
-0.5
0
0.5
1
1.5
2
50 100 150 200 250 300 350
-750 kJkg
-1
+30 kJkg
-1
Temperature (C) scan rate: 4Cmin
-1
Baselines
Answer this question:
According to the results of
experimental
measurements, what is the
heat of the desired
reaction?
(Units should be kJkg
-1
)
-0.6
-0.4
-0.2
0
0.2
0.4
0.6
0.8
1
1.2
0 100 200 300 400
-500 kJkg
-1
+30 kJkg
-1
-1
)
scan rate: 4Cmin
-1
Temperature (C)
-1
)
-1
-0.5
0
0.5
1
1.5
2
50 100 150 200 250 300 350
-750 kJkg
-1
+30 kJkg
-1
-1
Baselines
experimental
heat of the desired
reaction?
-1
)
Right answer:
The heat of the desired
reaction is
250 kJkg
-1
-0.6
-0.4
-0.2
0
0.2
0.4
0.6
0.8
1
1.2
0 100 200 300 400
-500 kJkg
-1
+30 kJkg
-1
-1
)
scan rate: 4Cmin
-1
Temperature (C)
-1
)
-1
-0.5
0
0.5
1
1.5
2
50 100 150 200 250 300 350
-750 kJkg
-1
+30 kJkg
-1
-1
Baselines
experimental
heat of the decomposition
reaction?
-1
)
-0.6
-0.4
-0.2
0
0.2
0.4
0.6
0.8
1
1.2
0 100 200 300 400
-500 kJkg
-1
+30 kJkg
-1
-1
)
scan rate: 4Cmin
-1
Temperature (C)
-1
)
-1
-0.5
0
0.5
1
1.5
2
50 100 150 200 250 300 350
-750 kJkg
-1
+30 kJkg
-1
-1
Baselines
experimental
heat of the decomposition
reaction?
-1
)
Right answer:
The heat of the
decomposition reaction is
500 kJkg
-1
-0.6
-0.4
-0.2
0
0.2
0.4
0.6
0.8
1
1.2
0 100 200 300 400
-500 kJkg
-1
+30 kJkg
-1
-1
)
scan rate: 4Cmin
-1
Temperature (C)
-1
)
-1
-0.5
0
0.5
1
1.5
2
50 100 150 200 250 300 350
-750 kJkg
-1
+30 kJkg
-1
-1
Baselines
Case study :
Batch reaction
Lesson 1
Lesson 1
In a preliminary evaluation
(SCREENING) of the severity of
the chemical process under study
the following data are already
known:
Heat of the desired reaction
QR = 250 kJkg
-1
Heat of the decomposition
reaction
QD = 500 kJkg
-1
These results are summarized in
the risk analysis forms 1 and 2.
POTENTIAL
Heat of reaction Specific heat capacity Adiabatic Temperature Rise
(Ratio Q
R
/ Cp)
Q
R
= 250 kJ/kg Cp = kJ/kg/K Tad = C
Highest theoretical attainable temperature in case adiabatic conditions occur: C
Total gas evolution: l/kg l/batch
Source of data:
Consequences of allowing adiabatic reaction (Check appropriate boxes)
Harmless temperature rise Boiling (Bp = C) Gas release
Critical temperature rise Decomposition Pressure build up
Other :
Lesson 1
POTENTIAL
(Ratio Q
R
/ Cp)
Q
R
= 250 kJ/kg Cp = kJ/kg/K Tad = C
Source of data:
Other :
Lesson 1
Severity:
Energy potential of relevant decomposition reactions: 500 kJ/kg
Specific heat capacity of reaction mass: kJ/kg/K
Adiabatic temperature rise: C
Boiling point of reaction mass (if relevant): C
Gas evolution: m
3
/batch
Known decomposition products:
Source of data:
Assessment of severity: Low Medium High
Lesson 1
Severity:
Specific heat capacity of reaction mass: kJ/kg/K
Adiabatic temperature rise: C
Gas evolution: m
3
/batch
Source of data:
Lesson 1
Lesson 1
(SCREENING) of the severity of
the chemical process under study
the following data are already
known:
QR = 250 kJkg
-1
reaction
QD = 500 kJkg
-1
The next step of lesson 1 is to
estimate the specific heat
capacity of the reaction
mixture.
Case study :
Batch reaction
Lesson 1
Example
Estimate of the specific heat capacity of a mixture
of 2000 kg of an organic compound in 2500 kg of
ammonia (27% by weight) in aqueous solution.
Table of data
Compound Cp M MCp
(kJkg
-1
K
-1
) (kg) (kJK
-1
)
Organic
compound 1.8 2000 3600
Ammonia
27% by wt. 3.9 2500 9750
Total 4500 13350
Cp Specific heat capacity of the reaction mixture
(kJkg
-1
K
-1
)
Mi Mass of a compound (kg)
Cpi Specific heat capacity of a compound
(kJkg
-1
K
-1
)
MR Total mass of the reaction mixture (kg)
Cp
MiCpi
MR
=
=
13350
4500
= 3.0 kJkg
-1
K
-1
Specific heat capacity calculation
Lesson 1
A rough estimate of the specific heat
capacity of the reaction mixture can be
obtained by addition of the heat capacities of
its components.
The table below shows approximate values
of specific heat capacities for different
compound classes. The example shows how
to calculate the specific heat capacity of a
mixture of 2000 kg of an organic compound
in 2500 kg of ammonia (27% by weight) in
aqueous solution.
Compound Specific heat capacity
(kJkg
-1
K
-1
)
Organic 1.8
Inorganic 1.0
Ammonia 27% 3.9
Water 4.2
Process data
Charge
(kg)
1-Chloro-4-
Ammonia 27% 2024 32.1 12
(pure NH
3
)
Total 2447
Remember the following approximate
values of specific heat capacities for
different compound classes:
(kJkg
-1
K
-1
)
Organic compounds 1.8
(fused or in solution)
Inorganic 1.0
Ammonia 27% 3.9
Water 4.2
According to process data
shown opposite, what is the
specific heat capacity of the
reaction mixture?
-1
K
-1
)
Process data
Charge
(kg)
1-Chloro-4-
Ammonia 27% 2024 32.1 12
(pure NH
3
)
Total 2447
Remember the following approximate
values of specific heat capacities for
different compound classes:
(kJkg
-1
K
-1
)
Organic compounds 1.8
(fused or in solution)
Inorganic 1.0
Ammonia 27% 3.9
Water 4.2
According to process data
shown opposite, what is the
specific heat capacity of the
reaction mixture?
-1
K
-1
)
Right answer:
The specific heat capacity
of the reaction mixture is
3.5 kJkg
-1
K
-1
Lesson 1
(SCREENING) of the severity of the
chemical process under study the
following data are already known:
QR = 250 kJkg
-1
reaction
QD = 500 kJkg
-1
Specific heat capacity of the
reaction mixture
Cp = 3.5 kJkg
-1
K
-1
These results are summarized
in risk analysis forms 1 and 2.
Remark
The following procedure is suggested for estimating the
specific heat capacity of the reaction mixture.
Table of data
Compound Cp M MCp
(kJkg
-1
K
-1
) (kg) (kJK
-1
)
1-Chloro-4- 1.8 423 761.4
nitro-benzene
Ammonia 27% 3.9 2024 7893.6
Total 2447 8655
Cp Specific heat capacity of the reaction
mixture (kJkg
-1
K
-1
)
Mi Mass of a compound (kg)
Cpi Specific heat capacity of a compound
(kJkg
-1
K
-1
)
MR Total mass of the reaction mixture (kg)
Cp
MiCpi
MR
=
=
8655
2447
= 3.5 kJkg
-1
K
-1
Specific heat capacity calculation
POTENTIAL
(Ratio Q
R
/ Cp)
Q
R
= 250 kJ/kg Cp = 3.5 kJ/kg/K Tad = C
Source of data:
Other :
Lesson 1
POTENTIAL
(Ratio Q
R
/ Cp)
Q
R
= 250 kJ/kg Cp = 3.5 kJ/kg/K Tad = C
Source of data:
Other :
Lesson 1
Lesson 1
In a preliminary evaluation (SCREENING) of
the severity of the chemical process under
study the following data are already known:
QR = 250 kJkg
-1
Heat of the decomposition reaction
QD = 500 kJkg
-1
Specific heat capacity of the reaction
mixture
Cp = 3.5 kJkg
-1
K
-1
The adiabatic temperature rise of the
decomposition reaction will be
determined in the next step of
lesson 1.
Lesson 1
The adiabatic temperature rise of a reaction is calculated by
dividing the heat of reaction by the specific heat capacity of
the reaction mixture.
Example
The adiabatic temperature rise of a high exothermic
decomposition reaction having a heat of reaction of
2000 kJkg
-1
in a reaction mixture with 2 kJkg
-1
K
-1
specific
heat capacity is:
Tad
=
QR
Cp
=
2000
2
=
1000 C
Tad adiabatic temperature rise (K or C)
QR heat of reaction (kJkg
-1
)
Cp specific heat capacity (kJkg
-1
K
-1
)
Remember
For the process under study, the following data are already
known:
QR = 250 kJkg
-1
QD = 500 kJkg
-1
Specific heat capacity of the reaction mixture
Cp = 3.5 kJkg
-1
K
-1
Lesson 1
Example
2000 kJkg
-1
-1
K
-1
specific
heat capacity is:
Tad
=
QR
Cp
=
2000
2
=
1000 C
-1
)
-1
K
-1
)
Remember
known:
QR = 250 kJkg
-1
QD = 500 kJkg
-1
Cp = 3.5 kJkg
-1
K
-1
What is the adiabatic
temperature rise of the
decomposition reaction?
(Units should be K)
Lesson 1
Example
2000 kJkg
-1
-1
K
-1
specific
heat capacity is:
Tad
=
QR
Cp
=
2000
2
=
1000 C
-1
)
-1
K
-1
)
Remember
known:
QR = 250 kJkg
-1
QD = 500 kJkg
-1
Cp = 3.5 kJkg
-1
K
-1
decomposition reaction?
(Units should be K)
Right answer:
The adiabatic temperature
rise of the decomposition
reaction is
143 K
Lesson 1
decomposition reaction is a direct measure
of the severity of a possible incident.
As a guideline, the following values can be
used
Severity Adiabatic temperature rise
HIGH Tad > 200 C
MEDIUM 50 C < Tad < 200 C
LOW Tad < 50 C
(1)
(1)
where the boiling point is not reached
Remember
In the previous step of lesson 1 the adiabatic
temperature rise due to the decomposition
reaction was calculated. Its value is 143 C.
What is the severity of a
potential incident?
(Type HIGH, MEDIUM or LOW)
Lesson 1
decomposition reaction is a direct measure
of the severity of a possible incident.
As a guideline, the following values can be
used
Severity Adiabatic temperature rise
HIGH Tad > 200 C
MEDIUM 50 C < Tad < 200 C
LOW Tad < 50 C
(1)
(1)
where the boiling point is not reached
Remember
In the previous step of lesson 1 the adiabatic
temperature rise due to the decomposition
reaction was calculated. Its value is 143 C.
What is the severity of a
potential incident?
(Type HIGH, MEDIUM or LOW)
Right answer:
The severity of a potential
incident is
MEDIUM
Lesson 1
The conclusion of the
initial steps of lesson 1
is that the severity of a
possible incident in the
process is MEDIUM.
Lesson 1
The severity of a possible
incident in the process is
MEDIUM due to the amount
of energy which can be
released by the
decomposition reaction. The
adiabatic temperature rise is
a direct measure of this
energy potential.
Data used for the
assessment of severity are
summarized in risk analysis
form 2.
Severity:
Specific heat capacity of reaction mass: 3.5 kJ/kg/K
Adiabatic temperature rise: 143 C
Gas evolution: m
3
/batch
Source of data:
Lesson 1
Severity:
Gas evolution: m
3
/batch
Source of data:
Lesson 1
Case study :
Batch reaction
Lesson 1
Rough estimate of
probability
Lesson 1
The conclusion of the initial
steps of lesson 1 is that the
severity of a possible
incident in the process is
MEDIUM.
The next step of lesson 1 is
to make a rough assessment
of the probability of
triggering the decomposition
reaction in the event of loss
of control of the desired
reaction.
Tad, R adiabatic temperature
rise of the desired
reaction(C).
Tmax, R maximum attainable
temperature if the
desired reaction occurs
under adiabatic
conditions (C).
Lesson 1
To give a rough estimate of the
probability of triggering the
decomposition reaction in the
event of loss of control of the
desired reaction, the following
data should be determined:
Lesson 1
Use the equation below to calculate the
adiabatic temperature rise of the desired
reaction.
The parameters which are already known are
given.
Tad, R
=
QR
Cp
rise of the desired
reaction (K or C)
QR heat of the desired
reaction ( 250 kJkg
-1
)
Cp specific heat capacity of
( 3.5 kJkg
-1
K
-1
)
Lesson 1
reaction.
given.
Tad, R
=
QR
Cp
rise of the desired
reaction (K or C)
reaction ( 250 kJkg
-1
)
( 3.5 kJkg
-1
K
-1
)
desired reaction?
(Units should be K)
Lesson 1
reaction.
given.
Tad, R
=
QR
Cp
rise of the desired
reaction (K or C)
reaction ( 250 kJkg
-1
)
( 3.5 kJkg
-1
K
-1
)
desired reaction?
(Units should be K)
Right answer:
The adiabatic temperature
rise of the desired reaction
is
71 K
Lesson 1
maximum attainable temperature if the
desired reaction occurs under adiabatic
conditions.
given.
temperature if the
under adiabatic
conditions (C)
Tp process temperature
(195C)
rise of the desired
reaction ( 71C)
Tmax, R = Tp + Tad, R
What is the maximum
attainable temperature if the
desired reaction runs under
adiabatic conditions?
(Units should be C)
Lesson 1
maximum attainable temperature if the
desired reaction occurs under adiabatic
conditions.
given.
temperature if the
under adiabatic
conditions (C)
Tp process temperature
(195C)
rise of the desired
reaction ( 71C)
Tmax, R = Tp + Tad, R
What is the maximum
attainable temperature if the
desired reaction runs under
adiabatic conditions?
(Units should be C)
Right answer:
The maximum attainable
temperature if the desired
reaction runs under
adiabatic conditions is
266C
Tad, R: adiabatic temperature rise
of the desired reaction(71C).
Tmax, R: maximum attainable
temperature if the desired
reaction occurs under adiabatic
conditions (266C).
Lesson 1
To give a rough estimate of the
event of loss of control of the
desired reaction, the following
data are already known:
These results should be
summarized in risk analysis
form 1.
Case study :
Batch reaction
Lesson 1
Rough estimate of
probability
POTENTIAL
(Ratio Q
R
/ Cp)
Q
R
= 250 kJ/kg Cp = 3.5 kJ/kg/K Tad = 71 C
Highest theoretical attainable temperature in case adiabatic conditions occur: 266C
Source of data:
Other :
Lesson 1
POTENTIAL
(Ratio Q
R
/ Cp)
Q
R
Source of data:
Other :
Lesson 1
Lesson 1
In the event of loss of thermal
control of the desired reaction,
the temperature will rise until
266C.
The next step in making a rough
estimate of the probability of
triggering the decomposition
reaction, is to determine if at this
temperature (266C) the
decomposition reaction is active
enough to produce an incident,
in a time too short to take
counter-measures.
Case study :
Batch reaction
Lesson 1
Rough estimate of
probability
Lesson 1
Taking account of
experimental conditions, one
can assume that if the trace
of the decomposition
reaction shows an
observable signal at 266C,
then at this temperature this
reaction is active enough to
produce an incident in a time
too short (minutes) to take
counter- measures.
Lesson 1
In the final reaction mixture thermogram,
the signal corresponding to the
decomposition reaction is detected at
235C.
Quantitative differential thermal analysis of final
reaction mixture.
Remark: This assumption depends
on the sensitivity of the measuring
instrument (10 Wkg
-1
) and the scan
rate (4Cmin
-1
).
-0.6
-0.4
-0.2
0
0.2
0.4
0.6
0.8
1
1.2
0 100 200 300 400
-500 kJkg
-1
+30 kJkg
-1
-1
)
scan rate: 4Cmin
-1
Temperature (C)
235C Tmax,R=266C
Lesson 1
A rough estimate indicates that at
the maximum temperature
attainable on loss of control of
the desired reaction (266C) , the
decomposition reaction will give
rise to an incident in a very short
time (minutes).
This means that in a preliminary
approximation (SCREENING), the
decomposition reaction is HIGH.
Lesson 1
Remark Remark
Morever, the overlapping signals
of the heat of the desired reaction
and the heat of the
final reaction mixture thermogram
gives a clear evidence that the
PROBABILITY of triggering the
decomposition reaction is HIGH.
Lesson 1
Pressure build up related to the Pressure build up related to the
process... process...
The pressure build up caused by
uncontrolled heat release of the desired
and decomposition reactions is an
important risk especially in industrial
synthesis reactions performed under
pressure.
To assure a safe design of the process
and the plant including the choice of an
appropriate pressure relief system, it is
indispensible to know the maximum
pressure that can be reached in the event
of a failure.
We will study it later in lesson3.
Case study :
Batch reaction
Lesson 1
Pressure build-up
Lesson 1
Maximum Temperature for Maximum Temperature for
Technical reasons (MTT)... Technical reasons (MTT)...
In order to complete the consequences of
loss of thermal control of the desired
reaction, we must consider if the
Maximum Temperature for Technical
reasons (MTT) could be reached in the
event of a failure.
The Maximum Temperature for Technical
reasons is the temperature at which the
pressure reaches the maximum
permissible value.
In the case under study, the reactor is
equipped with a safety valve. The safety
limit of this valve will be attained if the
temperature of the reactor attains 200C.
Lesson 1
Potential at the Maximum Potential at the Maximum
Temperature for Technical Temperature for Technical
reasons (MTT)... reasons (MTT)...
As the process temperature is 195C,
only 5C of the 71C adiabatic
temperature rise of the desired
reaction is needed to reach the
Maximum Temperature for Technical
reasons (MTT = 200C).
Consequently, the remaining energy
potential of the desired reaction will be
still high at this point.
Lesson 1
According to the results of a
preliminary evaluation of the thermal
risks of the process under study
(SCREENING), the consequences of a
loss of thermal control over the
synthesis reaction may lead to a
critical situation:
- the Maximum Temperature for
Technical reasons (MTT) will be
reached
- at this point, the potential of the
desired reaction is still high: there
exists a risk of pressure build up
- the decomposition reaction will be
triggered.
The results
obtained in
lesson 1
should be
summarized in
risk analysis
forms 1 and 2.
POTENTIAL
(Ratio Q
R
/ Cp)
Q
R
Source of data:
Harmless temperature rise Overpressure (MTT = 200C) Gas release
Other :
Lesson 1
Conclusions
POTENTIAL
(Ratio Q
R
/ Cp)
Q
R
Source of data:
Harmless temperature rise Overpressure (MTT = 200C) Gas release
Other :
Lesson 1
Conclusions
Severity:
Maximum Temperature for Technical reasons (MTT): 200 C
Gas evolution m
3
/batch
Source of data:
Lesson 1
Conclusions
Severity:
Maximum Temperature for Technical reasons (MTT): 200 C
Gas evolution m
3
/batch
Source of data:
Lesson 1
Conclusions

Case Study Batch Reaction Lesson 1

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Case Study Batch Reaction Lesson 1

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Thermal Safety Case Study- Lesson 1

This case study shows through an example of a batch

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