PSE Group Project – WS 2019/20

Continuous Production of High Quality Bis-Tertiary-Butylamino-Silane

in a Modular and Automated Plant

Group: 1

Report: 5

Examiners: Prof. Dr.-Ing. Sebastian Engell

Prof. Dr.-Ing. Andrzej Górak

Supervisors: M.Sc. Pourya Azadi

M.Sc. Anwesh Reddy Gottu Mukkula

Group members

Surname Name
Alagu Anusha Roshini
Anggara Aditya Rio
Ayala Jonathan León
Bonakdar Zahra
Galvis Cordoba Maria Paola
Garduno Farias Rodrigo
Mani Sakthi Gokul Siddarth
Palandagam Acharige Dilshan Mihiranga
Panindra Rohit J
Sharifov Ibrahim
Theeda Uma Jaya Ravali
Vora Paras
Submission date: 19.12.2019
Table of contents

1. Introduction ..................................................................................................... 1

2. Heat integration using tick-off heuristic ........................................................... 2

3. Control structures and interlocks .................................................................... 3

Feed vessel section ........................................................................................ 3

Reaction Section ............................................................................................ 3

Control structures..................................................................................... 3

Interlocks ................................................................................................. 4

Filtration Section ............................................................................................. 5

Rotary drum control structures ................................................................. 5

Rotary drum interlocks ............................................................................. 6

Membrane filtration control structures ...................................................... 6

Separation section .......................................................................................... 7

Control structures..................................................................................... 7

Interlocks ................................................................................................. 8

4. Plant start-up .................................................................................................. 9

Reaction section start-up procedure ............................................................... 9

Filtration section start-up procedure ............................................................. 10

Separation section start-up procedure.......................................................... 10

5. Plant Shutdown ............................................................................................ 12

Reaction section shutdown procedure.......................................................... 12

Filtration section shutdown procedure .......................................................... 12

Separation section shutdown procedure ...................................................... 13

6. Emergency shutdown procedure .................................................................. 14

7. Process safety .............................................................................................. 15

8. Conclusions .................................................................................................. 16

Appendix 1................................................................................................................. 17

Appendix 2................................................................................................................. 21

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Appendix 3................................................................................................................. 22

Appendix 4................................................................................................................. 23

Appendix 5................................................................................................................. 24

Appendix 6................................................................................................................. 25

Appendix 7................................................................................................................. 26

Appendix 8................................................................................................................. 29

Appendix 9................................................................................................................. 32

Appendix 10............................................................................................................... 35

Appendix 11............................................................................................................... 38

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List of figures

Figure 1. Process flow diagram (PFD) ......................................................................... 17

Figure 2. Grid diagram of stream data. ........................................................................ 18
Figure 3. Match between streams (1). ......................................................................... 19
Figure 4. Match between streams (2). ......................................................................... 19
Figure 5. Optimal grid network..................................................................................... 20
Figure 6. Control structure of the reaction section ....................................................... 21
Figure 7. Interlocks of the reaction section .................................................................. 22
Figure 8. Control structures for rotary drum ................................................................. 23
Figure 9. Membrane filtration control structure ............................................................ 24
Figure 10. Membrane filtration interlock structure........................................................ 24
Figure 11. Control structures for distillation columns. .................................................. 25
Figure 12. Atmospheric column pressure control using flooded condenser. ............... 26
Figure 13. Pressure control loops ................................................................................ 26
Figure 14. Columns interlocks connections. ................................................................ 27
Figure 15. Start-up procedure for R-101. ..................................................................... 29
Figure 16. Start-up procedure for F-201. ..................................................................... 30
Figure 17. Start-up procedure for C-302. ..................................................................... 31
Figure 18. Shutdown procedure for R-101................................................................... 32
Figure 19. Shutdown procedure for F-201. .................................................................. 33
Figure 20. Shutdown procedure for C-302................................................................... 34

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List of tables

Table 1: Process stream data ...................................................................................... 18

Table 2. Position of shut-off valves once alarm is initiated .......................................... 24
Table 3. Distillation columns alarms and trips.............................................................. 28
Table 4. Emergency shutdown .................................................................................... 35
Table 5. An overview of chemical compounds hazard identification ............................ 38
Table 6. Possible utility failures, affected equipment and possible solutions ............... 38
Table 7. Possible overpressure occurrences ............................................................... 39
Table 8. A brief overview of fire safety of BTBAS plant ............................................... 39

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Abbreviations
BTBAS Bis(t-tbutylamino)silane
C Cold stream
CP Heat capacity
CSTR Continuous stirred tank reactor
CV Control valve
CWR Cold water return
CWS Cold water supply
DCS Dichlorsilane
ESD Emergency shut down
H Hot stream
HV On/off valve
RPM Revolutions per minute
SCBA Self-contained breathing apparatus
TBA Tert-Butylamine
TTBAS Tri(t-butylamino)silane
VLR Venturi loop reactor

Greek letters
φ Degree of submergence

Chemical compounds formulas

CO2 Carbon dioxide
N2 Nitrogen

Nomenclature
ΔToptmin Optimum minimum approach temperature difference
Pmax Pressure maximum
Tmax Temperature maximum

Instrumentation nomenclature
First letter Additional letter Following letter/symbol
A / / Alarm
C / / Controller
D Density Difference /
F Flow ratio /
H Manual control High
I / / Indicator
L Level Low
P Pressure / /
Q Quality / /
S Speed / Switch
T Temperature /
+ / / High
- / / Low
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List of Authors

1. Introduction
2. Heat integration using tick-off heuristic Rohit J Panindra
3. Control structures and interlocks
Feed vessel section Gokul Siddharth
Reaction Section
Control structures Ibrahim Sharifov
Interlocks Rodrigo Garduño Farías
Filtration Section
Rotary drum control structures Zahra Bonakdar
Rotary drum interlocks Zahra Bonakdar
Membrane filtration control structures Gokul Siddharth
Separation Section
Control structures Jonathan León Ayala
Pressure control Maria P Galvis Cordoba
Interlocks Maria P Galvis Cordoba
4. Plant start-up
Reactor section start-up procedure Uma Jaya Ravali Theeda
Filtration section start-up procedure Aditya Rio Anggara
Separation section start-up procedure Paras Vora
5. Plant Shutdown
Reactor section shutdown procedure Uma Jaya Ravali Theeda
Filtration section shutdown procedure Aditya Rio Anggara
Separation section shutdown procedure Paras Vora
6. Emergency shutdown procedure Anusha Roshini Alagu
7. Process safety Dilshan Mihiranga
8. Conclusions

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1. Introduction

Bis-(tert-butylamino)silane (BTBAS) is used in the semiconductor processing industry as

a precursor for the fabrication of silicon nitride wafers. The aim of this project is to design
a plant to produce 35 tons of BTBAS in 8000 hours per annum with at least 98 wt.% purity
for application in silicon chip manufacturing. The designed plant must be continuous and
automated. The plant should be modular, in the aspect of being able to cope with ± 30%
fluctuation of the nominal production demand. The plant is assumed to be built inside a
chemical complex where basic utilities and waste stream treatment is available.

Based on the chosen reaction pathway (aminolysis of silane in excess of amine), the raw
materials used are tert-butylamine (TBA) and dichlorosilane (DCS). TBA is also used as
the solvent for the production of BTBAS. Tert-butylamine hydrochloride (TBA.HCl) is the
salt obtained as by-product and tri-(tert-butylamino)silane (TTBAS) is the side product.
TBA is a colorless liquid classified as category 2 flammable liquid, which has an ammonia-
like odor, is soluble in water, and is highly toxic if inhaled or swallowed [1]. DCS is a
colorless gas under normal conditions and hydrolyzes to form hydrochloric acid and
siloxanes [2]. TBA.HCl is insoluble in the reaction mixture and TTBAS is the least volatile
component.

In order to achieve the required specifications, the following equipment have been chosen
in the course of process development. Venturi loop reactor was selected for the mass
transfer-limited reaction of TBA and DCS. Rotary drum and membrane filters were chosen
for separation of TBA.HCl from the reaction mixture. Finally, for the purification of the salt-
free liquid mixture, two distillation columns are used. In the previous report, the design of
the reactor was validated and its performance was analyzed by means of modelling and
simulation. Process automation for alternate switching of membrane filters was done to
realize continuous operation. The sizing of all vessels and distillation columns was carried
out. Piping system and pumps were designed and pinch analysis was performed for
minimization of utility requirements.

In this report, heat integration would be described to determine the optimal number of
heat exchangers. The control structures for reaction, filtration and separation sections
would be presented. Furthermore, start-up and shutdown procedures as well for the
above, would be listed. The emergency procedure and safety aspects of the processes
are also dealt with in this report.

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2. Heat integration using tick-off heuristic

In the biweekly report 4 (section 5.2), it was found that the pinch point was located at
171°C. The resulting minimum heating and cooling utility requirements were 1.3 kW and
7.35 kW respectively. A heat integration technique called tick-off heuristic is applied here
to maximize heat recovery [3].

The process streams (Table 1, Appendix 1) were divided at pinch temperature as shown
in Figure 2 (Appendix 1). For a hot (H) and cold (C) stream to be matched, the heat
capacity (CP) of a hot stream must be less than or equal to that of cold stream above
the pinch [4]. Below the pinch, CP of hot stream must be greater than or equal to CP of
cold stream for a match [4]. However, the aforementioned CP rules can be relaxed for
process streams away from the pinch [4]. Stream splitting was not required above the
pinch as there was only one cold stream [3]. As number of hot streams were higher than
that of cold streams below the pinch, no stream splitting was required there [3]. The
streams H4 and C1 were matched below the pinch ensuring optimum minimum approach
min
temperature difference of 10°C (ΔTopt , biweekly report 4: section 5.2) as depicted by
Figure 3 (Appendix 1). Consequently, heat load of 0.17 kW of stream H4 is completely
transferred to stream C1, which requires 0.24 kW. The remainder of 0.07 kW for stream
C1 could be provided by the stream H3, which possesses 0.43 kW. Hence, streams H3
and C1 were matched (Figure 4, Appendix 1) and the cooling utility requirement of H3
reduced to 0.36 kW. Thus, the requirement of heating utility for stream C1 was eliminated
as a result of heat integration with process streams H4 and H3 (Figure 4, Appendix 1).
Similarly, the cooling utility requirement for stream H4 was eliminated (Figure 4,
min
Appendix 1) by heat integration with stream C1.The violation of ΔTopt prevented
matching other process hot and cold streams on either side of the pinch. Hence, cooling
utilities were provided for streams H1, H2 and H3. Similarly, heating utilities were provided
for streams C2 and C3.

In PFD (Figure 1, Appendix 1), the stream S1 (C1) could be used for its preheating up
to 71% of the required value and complete cooling of stream S2 (H4). Further preheating
of stream S1 is achieved by condensation of stream S2 up to 16% (H3). Remaining
condensation of stream S2 is realized by cooling utility. The savings in heating and
cooling utility requirements were 16% and 3% respectively (biweekly report 4: Section
5.2). The required optimal number of heat exchangers is seven (Figure 5, Appendix 1).

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3. Control structures and interlocks

Feed vessel section

DCS from the cylinders in battery limit is fed to the pressure vessel V-103 before
injecting into the reactor. This is done to avoid flow fluctuations during replacement of
DCS cylinders when it gets emptied. Pressure is maintained at 1.3 bar using a control
valve CV-103 on the upstream of the pressure vessel and the flow to the reactor is
controlled using a flow control valve CV-104 on the outlet line, which goes to the reactor.
In Figure 6 , control structure of the DCS pressure vessel V-103 is also shown. Fresh
TBA from the battery limit is stored in the vessel V-101, which also acts as a recycle
drum collecting unreacted TBA from the downstream. Level of vessel V-101 is controlled
by adjusting the inlet fresh TBA flow rate using control valve CV-101. TBA flow rate to
the reactor is controlled by the control valve CV-102 on the outlet line of V-101. Figure
6, Appendix 2 depicts the control structure of vessel V-101. As shown in Figure 7,
Appendix 3, for level control, a high-level alarm LA+ is initiated at 90%, which actuates
shutoff valve HV-101 to close, and it is followed by a tripping LA ++ at 95%. Low-level
alarm LA- is initiated 50% which shutoff valve HV-102 to close followed by tripping LA--
is initialed at 45%.

Reaction Section

Control structures

Control structures are important for reactor system in order to ensure 2 main objectives,
namely desired reaction conditions and production quality at steady state in automated
mode. To achieve those targets, individual control loops (general control structure is
shown in Figure 6, Appendix 2) has been chosen.

Desired production rate of BTBAS can be achieve giving set point for DCS as DCS is
the limiting reactant in the system and nearly 100% conversion of DCS is achievable.
Since amount of TBA supplied is related to the DCS flowrate due to TBA being provided
in determined amount of excess, ratio control has been used to regulate flowrate of TBA.
In general, excess reactant control in multiphase reactors reduces the dependence on
concentration control. [5]

Considering CSTR-type behaviour of VLR holding vessel, volume of the reactor is also
important factor in terms of residence time. The residence is also extremely important
as in two phase system transport from the gas phase to liquid phase in longer residence

3
times is also significant issue. Considering constant area for the vessel, volume is
related to height of the column, which can be regulated based on flowrate values of
reactants. Level change in control is provided by altering the speed of the pump P-101
at the outlet of reactor.

In the VLR reactor system, recycle flowrate serve two main purposes. First of all, the
amount of flowrate is mainly fixed such that it will allow enough suction of gas through
the nozzle. Therefore, for each set value of DCS gas flowrate, recycle flowrate can be
adjusted and fixed. Second point is regarding the temperature control; however, it has
been previously shown that flowrate will always be high enough that amount of heat duty
can be removed from the system by altering cooling water flowrate in the heat
exchanger. Cascade control for temperature has been chosen, where temperature
transmitter, measuring reactor temperature, is sending signal to flow controller that in
turn manipulates the position of CV-106 valve to keep the temperature at desired value.

Finally, the reaction pressure is defined to be 2 bar. Although amount of DCS

unconverted will be less as conversion is nearly 100%, there will be still some amount
of DCS accumulating in the system which in turn increase pressure over time. This will
be regulated using to CV-105 valve, directing excess amount of gas back to DCS
pressure vessel V-102.

Interlocks

An interlock circuit should be designed to act on devices (e.g. on/off valves) in order to
deal with an emergency situation. These emergency situations or states are established
by an alarm system. Figure 7, Appendix 3 shows the interlock system for the reactor
which is explained as follows:

 Low liquid level interlock

If the lower level limit alarm for the holdup vessel of the reactor gets activated, a trip will
start which will close the valve HV-109 and at the same time will shut down the pump
P-101 which then will prevent the vessel from getting drained further.

 High liquid level interlock

When the holdup vessel of the reactor gets overfilled, the diffusor would get covered
which could lead to a mechanical failure which would directly affect the operation of the
venture loop reactor, therefore if the higher level limit alarm for the holdup vessel of the
reactor gets activated, a trip will start which will close the valve HV-104 and the valve

4
HV-102 at the same time which then will prevent the vessel from filling any further,
avoiding the diffusor to get affected.

 High temperature interlock

The main control of the temperature in normal operation will be carried out by the loop
heat exchanger but in case of cooling failure, a cooling jacket around the reactor will be
available to account for emergency situations. If the higher temperature limit alarm of
the reactor gets activated, a trip will start which will close the valve HV-104 which then
will stop the heat generation due to the reaction. Then the valves HV-108 and HV-106
will also open in order to quickly decrease the temperature of the reactor and the inlet
liquid temperature, respectively.

 High pressure interlock

If the higher-pressure limit alarm for the reactor gets activated, a trip will start which will
open the valve HV-105 which then will relieve the reactor pressure.

Filtration Section

Rotary drum control structures

Rotary drum filter has many variables that can be controlled or manipulated. According
to the procedure that is followed in order to design and derive the size of this unit
operation, pressure and degree of submergence of the drum are set at a desired value
and the cake moisture is meant to be as least as possible for least BTBAS and TBA
waste. For this purpose, the controller structures are implemented. A buffer tank after
the reactor is placed which collects the product stream from the reactor. In order to keep
the degree of submergence of the drum at 30, a level controller is implemented which
controls the inlet flowrate to the rotary drum through the control valve CV-201. The
amount of fresh TBA for rinsing purpose differs based on the capacity of the plant (∓30%
of the nominal capacity). This value can be controlled through the valve CV-202.
Moreover, rotary speed depends on the capacity as well and by indicating the inlet flow
rate of the rotary drum, its speed will be controlled and kept at a proper value resulting
in least cake moisture. The pressure within the rotary drum filter should be controlled
and set as 20 kPa as the operation condition. This is done by a vacuum pump and in
order to avoid evaporation of TBA under vacuum condition, inert stream (N2) is applied
through CV-207 for V-201 and through CV-208 for V-202. Outlet flowrates of the vessels

5
are regulated by the LICs regarding different capacities. Control loop structures for
rotary drum filter are shown in Figure 8, Appendix 4.

Rotary drum interlocks

There will be an alarm for low level indication LA- in vessel V-201 which leads to turning
off the pump P-201 and closing the valve HV-204. Same case is applied for the vessel
containing TBA. If the level indicator shows low level in the vessel V-202 pump P-202
should turn off and the valve HV-202 will be closed. High level scenarios are not
considered for these two vessels as interlocks, since the inflows to the rotary are already
regulated through CV-201 and CV-202 and if any problem in the reactor happens
leading to high flow rates, that case will already lead to alarm for high level HL + in V-
102. When there is high level alarm in V-102 the valve HV-110 will be closed. In case of
low level alarm in V-102 the valve HV-201 will be closed leading to shut off the rotary
drum motor and turning pumps off.

Membrane filtration control structures

In membrane filtration, the increasing pressure drop due to filter clogging eventually
retards the permeate flow. Constant permeate flow is desired which is accomplished by
using a flow meter on the permeate line and using that signal to control the feed flow.
This can be achieved by having a control valve after the pump and making it open to
maintain the permeate flow or increasing the RPM of the feed pump [6]. The control
structure of the membrane filtration is shown in Figure 9, Appendix 5. Flow meter
transmits the signal to the control valve CV-205, which opens to increase the flow. When
the transmembrane pressure reaches 4 bar or when the control valve CV-205 is fully
opened (maximum flowrate) to achieve required permeate flow, three way valve CV-206
diverts the flow from the current membrane system to the other stand-by membrane
system. A high differential pressure alarm DPIA+/DPIB+ at 4.5 bar is initiated in order to
avoid membrane degradation. The alarm, can be possibly triggered due to the failure of
three way valve CV-206, activates the shutoff valves. The location and valve position of
shutoff valves once the alarm is initiated are shown in Figure 9 and Figure 10 (Appendix
5) respectively. Diversion of flow by three way valve to the stand-by membrane system
enables the backwashing procedure on the clogged membrane.

6
 Separation section

Control structures

In the process investigated in this project, two distillation columns are used. The first
column (C-301) removes TBA, while the second column (C-302) purifies BTBAS from
side products. In this section, control structures are presented for the foregoing
distillation columns. In distillation processes the feed rate and feed composition must be
considered as disturbances. Heat input from the reboiler, external reflux, distillate, and
bottom product rates are manipulated variables [7]. Two of those manipulated variables
are used to meet mass balance. Therefore, there are two degrees of freedom that
usually are used to control composition. When starting the design of controls, it is
convenient to first layout all material balance controls [8]. Material balance is met
following the method described in [9], which determines the manipulated variable to
control level hold-up. Distillate and bottom rates were assigned to control levels, which
were cascaded to flow controllers as inner loops. One reason to use cascade loops is
to isolate slow control loops from nonlinearities in the final control element [10]. Another
relevant aspect is feed enthalpy changes because it might cause significant
disturbances in the product composition [11]. Therefore a preheater is located before
column C-301, a temperature control loop cascaded with a flow loop is used to control
feed enthalpy. The quality of the final product is proposed to be controlled using a quality
measurement, the main reason is that there is no clear relation between temperature
and concentration that can be used. Hence, taking advantage of the difference of
densities of TBA and BTBAS (0.696 g/ml and 0.816g/ml respectively at ambient
temperature) and the accuracy of density meters available in the market, up to ±0.00025
g/ml [12], quality control is located in the reflux ratio drum. Following thermodynamic
and hydrodynamic principles, the quality of the top of the column is controlled using the
reflux rate [8], usually, cascaded with a flow controller [10]. On the other hand, at the
column base, the temperature of the column is controlled via the heat provided by the
heater. In order to avoid high perturbances in the feed conditions of both columns buffer
tanks are used. Each tank requires level control. Buffer tank for C-301 requires a
cascade control system of level and flow controller being the secondary loop because
upstream pressure might vary significantly due to the previous unit which is a membrane
process [7]. For the buffer tank of the second column, only one valve is enough to control
the level because the upstream pressure is higher than the column C-302.

7
  Pressure control

Pressure control in a distillation column is important for the separation performance as

it directly influences the vapor-liquid equilibrium. In order to effectively control the
pressure of the atmospheric column C-301, the vapor space within it must be regulated.
As expressed in [13], this should be done by manipulating a major source or sink of
vapors, such as the rate of condensation or the rate of vaporization. In case the later
was to be chosen, the degrees of freedom to control the column bottoms would be
reduced; and as explained above, the provided heat by the coil H-303 (rate of
vaporization) is used to control the temperature in the lower section of the column. Thus,
the rate of condensation is chosen as the variable to regulate the column pressure. On
increasing pressure, the condensation rate must be increased either by providing a
larger heat transfer area or a higher temperature difference. For the first alternative, a
flooded condenser is needed and the most common control arrangements are shown in
Figure 12, Appendix 7. In the second alternative, a higher coolant flowrate translates
into a decrease of its return temperature maintaining the temperature difference higher
along the heat exchanger. Since a faster response is expected with the second option
and it works properly for low cooling media flowrates [13], the cooling water supply
flowrate is chosen as the manipulated variable to control the pressure of column C-301
(Figure 13, Appendix 7). In case of the vacuum column C-302, the pressure is
maintained by the flowrate of non-condensable compounds passing through the vacuum
pump P-303. As the TBA is assumed to be the non-condensable compound and its
flowrate coming from C-301 is low, it is not recommended to use this as the manipulated
variable. Instead, as proposed in [13], an external flow of inert gas can be introduced at
the gas outlet of the condenser H-304 before the vacuum system. By manipulating said
flowrate, a more accurate and reliable pressure control is achieved (Figure 13, Appendix
7).

Interlocks

As explained in [14], interlocks are a protective response initiated on the detection of a

process hazard, which should be physically separated from the process control
structures. In case of distillation columns the most relevant indicators of a malfunction
are tanks/drums level, column top pressure, column pressure drop, and column sump
level and temperature. A list of the proposed alarms and their corresponding trips is
given in Table 3, Appendix 7. The interlock connections are shown in Figure 14,
Appendix 7.

8
4. Plant start-up

In this section, the start-up procedure of all the equipment has been discussed. Start-up
procedure has to be followed for safe starting of the plant and to bring the plant to steady
operating condition. This procedure has to be followed for the first start-up
(commissioning of the plant) and after every maintenance shutdown. This procedure is
referred to as cold start-up. The following check list must be complied with before the
start-up:

1. Pre-start up safety review has been done and all the clearance for start-up from
all department has been received.
2. All utilities such as cooling water, instrument air, power, inert blanking, etc. are
available.
3. No interlocks or alarms are active.
4. Inerting procedure for all equipment has been carried out.

Reaction section start-up procedure

Reactor start-up shall be performed to bring it to full production scale after construction
and commissioning. The following sequence of start-up procedure shall be followed
(refer to Figure 6, Appendix 2 and Figure 15, Appendix 8):

1. HV-106 should be opened to ensure continuous coolant flow.

2. HV-101 should be opened to fill V-101 up to half volume with fresh feed TBA.
3. HV-103 should be opened to vent out any nitrogen from R-101 while filling TBA
HV-102 shall be opened until the pressure is 1 bar.
4. Afterwards HV-102, HV-111 and H-103 should be closed.
5. The liquid level in R-101 shall be decreased to 80% in level by flowing fluid to V-
102. For this, HV-109 and HV-110 need to be opened and P-101 shall be started.
6. Before introducing DCS into the reactor, the recycle flow needs to be achieved.
Hence, HV-110 shall be closed and HV-107 shall be opened.
7. After having established a steady recycle flow, TBA will be cooled until 8 °C.
8. HV-111 should be opened to pressurize R-101 to 2 bar.
9. HV-102, HV-104, HV-110 should be opened to feed in reactants for the reactor
to begin.
10. The reactor shall be kept in operation until a steady state and product
concentrations are achieved.

9
 11. HV-101 should be kept open to achieve continuous start-up, but when recycle
TBA from C-101 is received, this should be closed.

Filtration section start-up procedure

The following procedure should be performed out to ensure safe start-up of filtration unit
(refer to Figure 8 in Appendix 4, Figure 9 - Figure 10 in Appendix 5 and Figure 16 in
Appendix 8):

1. As rotary vacuum drum filter operates at 20 kPa, vacuum condition is reached by

activating vacuum pump P-203.
2. Once minimum level of V-102 is reached (indicated by LISL_V_102), bottom valve of
V-102 (HV-201) is opened.
3. Feeding is conducted by regulating CV-201 until the degree of submergence (𝜑) of
F-201 reaches 30°.
4. As 𝜑 is fulfilled, the speed of drum rotation (0.56 rpm) is set and screw conveyor is
activated.
5. HV-203, CV-203, HV-204, CV-205, P-201 should be switched on once minimum level
of V-201 is reached.
6. HV-202, P-202 and CV-204 should be switched on once minimum level of V-202 is
reached.
7. By opening CV-206, filtrate is subsequently pumped to membrane (F-203A/B)

Separation section start-up procedure

Distillation column C-301 is operated at atmospheric pressure and column C-302 is

operated under vacuum (55 mmHg). The start-up procedure for both columns is similar.
The difference between the two columns is that C-301 does not have the vacuum system
and C-302 does not have a preheater. The following start-up procedure of C-302 for
safe starting up (refer to Figure 11 in Appendix 6 and Figure 17 in Appendix 8):

1. Vacuum pump P-303 should be switched on. The operating pressure of the
column should be below of 55 mmHg.
2. Cooling water supply to condenser H304 and the product sub cooler H-306
should be started by opening the valves HV-313 and HV-314. The temperature
of condenser should be ensured below the dew point of the distillate.
3. Feed to C-302 should be started by opening valve HV-306.

10
4. The re-boiler H-305 should be switched on once the liquid sump has enough
liquid hold up.
5. The column should be operated under total reflux till the sufficient till sufficient
liquid hold up is achieved in the reflux drum V-302.
6. Pump P-302A/B should be switched on to transfer distillate to storage tank.
7. Pump P-305A/B should be switched on to transfer bottoms to storage tank.
8. The product composition should be monitored to ensure the steady state is
reached.

11
5. Plant Shutdown

The purpose of plant shutdown is to create complete overhaul of all plant activities, for
instance to perform required maintenance, repairs or equipment replacements.
Furthermore, all equipment has operational and warranty requirement for service and
inspection.

Reaction section shutdown procedure

The following procedure for the reactor shall be followed when it needs to be shut down
for maintenance or emergency purposes (refer to Figure 6, Appendix 2 and Figure 18 in
Appendix 9):

1. Feed to the reactor system needs to be shut off first. Hence, HV-104, HV-102
and HV-111 should be closed.
2. Depressurization of R-101 should be continuously performed, as a result, HV-105
should be opened.
3. Contents of R-101 should be removed by shutting off HV-107 and opening
HV-109 and HV-110. The pump P-101 should remain on to transfer the contents
to V-102.
4. When R-101 is empty, the pump should be switched off and HV-109 and HV-110
should be closed.
5. Finally, the coolant shall be turned off by shutting off HV-106.

Filtration section shutdown procedure

The following procedure should be performed out to guarantee safe start-up of filtration
unit (refer to Figure 8 in Appendix 4, Figure 9 - Figure 10 in Appendix 5 and Figure 19
in Appendix 9):

1. HV-201 and CV-201 are closed to discontinue any incoming flow filtration.
2. The operation of pump P-201 and P-202 should be switched off.
3. The following valves are to be switched after switching off the pump (HV-203,
CV-203, HV-204, CV-205, HV-202, CV-204).
4. As no inlet flow is introduced, degree of submergence (𝜑) of F-201 will decrease due
to steady vacuum filtration.

12
5. Once minimum 𝜑 is satisfied, 2 minutes will be allocated for final drum rotation prior
to complete shutdown. During the allocated time, 1 full rotation of 0.56 rpm ensures
liquid filtration and cake scrapping.
6. Vacuum pump P-203 is switched off while keeping the rotation for 2 minutes to ensure
cake discharge out of the screw conveyor.
7. Finally, screw conveyor inside the rotary drum filter unit should be deactivated.

Separation section shutdown procedure

The shutdown procedure for both distillation column are similar. The following procedure
needs to be followed for safe shutdown of C-302 (refer to Figure 11 in Appendix 6 and
Figure 20 in Appendix 9):

1. The feed to the column should be stopped by closing HV-306.

2. The re-boiler H-305 should be switched off.
3. The contents of column and reflux drum should be transferred to the storage
tanks by switching on pumps P-302A/B and P-305A/B.
4. Pumps P-302A/B and P-305A/B should be switched off, once all the contents of
column are transferred.
5. Vacuum pump P-303 should be switched off.
6. Cooling water supply to H-304 and H-306 should be stopped by closing the
valves HV-313 and HV-314.
7. The column C-302 should be isolated closing the valves HV-301 and HV310.
8. Inerting procedure should be started.

13
6. Emergency shutdown procedure

Emergency shut down (ESD) is a method for stopping process operations, using a
detailed process situation analysis for temporary isolation or complete shutdown of the
entire process plant to reduce the possibility of an unwanted and dangerous event
quickly [15]. The purpose of the ESD system is to protect personnel, be able to protect
facilities, and prevent environmental impacts from process activities [15]. In the reactor
(R-101), if there is no incoming of the reactant(s) (DCS and/or TBA), this will lead to a
serpentine failure [15]. In this situation, all units should be shut down along with all the
associated valves. The reactor unit should be quarantined, if the recycle TBA does not
flow into reactor, by initiating an immediate shut down. Chilled water flow should be
increased in R-101 when there is a rise in the temperature than the desired. When the
flow of the streams are blocked, causing pressure build up, a relief or depressurizing
valve is used to mitigate the situation [15]. The relief valves are also used for pumps to
depressurize, if required [15]. ESD needs to be executed if the pumps malfunction by
shutting down all the units and closing all the valves of the individual units. In the heat
exchanger (H-101, H-302/303/304/306), if the temperature builds up, then the cooling
utilities (cooling water and chilled water respectively) flow should be increased.

In rotary drum filter (F-201), in case of failure of the vacuum pump to maintain pressure
increases from 20 kPa to atmospheric pressure 100 kPa (1 bar), the drum cannot hold
the cake. Hence the cake falls down to the trough. No significant pressure gradient
between inlet and outlet in membrane screens (F-302A/B) leads to crude BTBAS liquid
carries unfiltered salt (particle size < 1 µm) to the distillation unit. These situations in the
filtration units can be solved by using an auxiliary filter of same standards by channeling
the contents to this auxiliary filter yet running the process. Buffer tanks present in the
plant at several positions could have an increase in the level of the liquid which could
be drained by transferring the excess liquid to the auxiliary buffer tank. Distillation
columns (C-301 and C-302) are also subject to a lot of potential failure situations. It is
noted that an increase in pressure of distillation column, may occur due to excessive
heat input. To avoid any damage to the quality of product, the reboiler operation should
be halted and feed to the column should be shut immediately.

All the other potential failure situations in the entire plant along with the actions required
are tabulated in Table 4, Appendix 10.

14
7. Process safety

The emphasis on process safety at the design stage of the BTBAS plant provided the
opportunity for achieving maximum inherent safety at the lowest cost. As a result,
appropriate design features were selected to achieve avoidance and mitigation of
accidents such as, the release of flammable or toxic materials that could lead to a fire,
explosion and environmental damage. The proposed design features add multiple layers
of protection to the process starting with the basic design, and include control systems,
alarms and interlocks (Section 3), safety shutdown system (Section 6), protective
systems and emergency response plans [16].

Process safety in the basic design starts from the safe handling of the materials by
understanding their physical and chemical properties. An overview of the hazard
identification of the reactants and main products are given in Table 5, Appendix 11. Due
to the violent reactivity of BTBAS with water, it would be essentially ensured that water
would not enter the system as an impurity with TBA or as moisture by leakage. The
designed plant has relatively low pressures and temperatures (Pmax ≈ 0.7 MPa at E-101
liquid inlet and Tmax ≈ 171 °C at H-305), leading to the simpler design and less demand
for the mechanical strength of equipment construction. The efforts made in process
intensification of the reactor (choosing VLR) and the distillation columns (structured
packing internals) led to the minimization of inventory which in turn reduced the potential
quantity of hazardous materials that could be released. in the event of plant utility failure,
suitable features would be added to the utility system as summarized in Table 6,
Appendix 11 to prevent the equipment and the operation from being affected.

Protective systems against accidental release of materials by equipment overpressure

or vacuum would be provided in three layers starting from, ensuring the high integrity of
equipment and piping, depressurizing and finally the pressure relief systems [17].
Occurrences that would require overpressure protection in the BTBAS plant are
summarized in Table 7, Appendix 11. Considering the properties of the chemical
compounds and the scale of the plant, vapor and liquid effluent generated from
emergency conditions or shutdowns, would be directed to a closed drain header
blowdown system until further treatment. Fire protection system for the plant consists of
gas and smoke detection, alarm systems, active and passive protection, response and
fire control. Basis for the fire response system is summarized in Table 8, Appendix 11.

15
8. Conclusions

Heat integration using tick-off heuristic was carried out and the optimal number of heat
exchangers required was found to be seven with savings in utility requirements. The
control structures for the feed vessel and reactor involved control of pressure and inlet
fresh TBA flow rate respectively. In the reactor section, ratio control was also used to
regulate the flow rate of TBA. Cascade control was chosen for temperature control and
the pressure in the reactor was controlled by manipulating the flow of excess DCS to
the pressure vessel. Interlocks were used in the reactor for emergency cases such as
low and high liquid levels in holdup vessel, high temperature and pressure. Interlocks
were also provided for feed vessel in the event of high flow rate of TBA.

In the filtration section, control structures were implemented to obtain desired cake
moisture and degree of submergence of the rotary drum. For this purpose, a level
controller was used to control the inlet flow rate to rotary drum. Additionally, alarms and
interlocks were used in the event of high flow rates to the rotary drum. The permeate
flow in the membrane filter was controlled by maintaining the inlet flowrate. A high
differential pressure alarm was placed to avoid membrane degradation.

In the distillation section, cascaded control loops were used to maintain quality at top of
the column through external reflux rate. Control loops were also implemented to
maintain the temperature and level in the column. Additionally, the enthalpy at the inlet
of the columns was controlled. The pressure of the first column was controlled through
condensation rate by manipulating the cooling water flow rate. The pressure of the
C-302 was controlled by manipulating the inert flow rate through vacuum pump.
Interlocks were also provided for the distillation columns in the event of malfunctions.

The start-up and shutdown procedures were listed for reaction, filtration and distillation
sections. The logic instructions were implemented as sequential function chart in
Codesys. The emergency shutdown procedures in the event of failures with respect to
each section was listed. Process safety was discussed to ensure multiple layers of
protection for inherent safe operation of the plant.

In the upcoming stages of the project, cost analysis would be carried out to determine
the economics of the plant. Piping and instrumentation diagram incorporating all the
control loops discussed in this report would be developed. The plant layout and location
would also be finalized.

16
Rohit J Panindra

Appendix 1
V-102
V-103 R-101 V-101 P -101 H-101 V-304 H -301 C-301 V-301 C-302 H-304 V-302 P -303
Reactor outlet E-101 H -302 E-301
DCS Buffer tank Venturi Loop TBA Collection Reactor Loop Reactor LoopFiltration outlet Crude Liquid TBA Distillation TBA Reflux BTBAS Vacuum BTBAS BTBAS Reflux BTBAS Vacuum
buffer tank Reactor Ejector TBA Condenser BTBAS Ejector
Reactor Drum Pump Heater buffer tank Preheater Column Drum Distillation Condenser Drum Pump
Tower

V -103

DCS
V-101
H-302
E- 101
P -303A/B

H-101 V -304 V-301

C-301

R-101
H-301
P-301 A/B
S3 H-304
P -101 A/B S1

P -203 A/B V-302

TB A 9

V-305 C-302
P-001 A/B H-303
V-102

F-201 P -302A/B
V -202
B TB A S
S2
H-306

V- 201
F-202 A
H-305
P-202 A/B

Sid e Pr o d.

F-202 B
P-201 A/B
P-305
TBA.HCl

P -203 V-202 P -202 H -303 P -301 V-305 P -305 H -305 P -302 H-306 V-303 P-304
F-201 V-201 P-201 M-201 F-203 A/B F-202
Rotary filter TBA Liquid TBA Liquid TBA Column TBA Column Atmospheric Side Product BTBAS Column BTBAS Column BTBAS Product BTBAS/TBA TBA Recycle
Crude Liquid Crude Liquid Crude Liquid TBA-Salt Membrane Crude Liquid
Vacuum Collector Pump Reboiler Reflux Pump column outlet Pump Reboiler Reflux Pump Cooler Scrubber Pump
Fliter I Collector Pump Mixer Filters Fliter II
Pump buffer tank
Rev 19/12

Figure 1. Process flow diagram (PFD)

17
 Rohit J Panindra

Table 1: Process stream data

Specific Heat
Inlet Outlet Latent Flow Heat
Equipment heat Capacity,
Stream temperature temperature heat rate load
ID capacity CP
T [°C] t [°C] [kJ/kg] [kg/h] [kW]
[kJ/kgK] [kW/K]
H-101 H1 35 7 2.12 - 317.78 0.187 5.23
H-301 C1 30 47 2.45 - 20.90 0.014 0.24
H-302 H2 44 44 2.62 388.00 16.37 - 1.76
H-303 C2 161 161 2.10 242.60 16.38 - 1.10
H-304 H3 86 86 2.10 242.60 6.36 - 0.43
H-305 C3 184 184 2.09 206.80 3.30 - 0.19
H-306 H4 86 20 2.10 - 4.45 0.003 0.17

Figure 2. Grid diagram of stream data.

18
Rohit J Panindra

Figure 3. Match between streams (1).

Figure 4. Match between streams (2).

19
Rohit J Panindra

Figure 5. Optimal grid network.

20
Ibrahim Sharifov

Appendix 2

Figure 6. Control structure of the reaction section

21
Rodrigo Garduño Farías

Appendix 3

Figure 7. Interlocks of the reaction section

22
Zahra Bonakdar

Appendix 4

Figure 8. Control structures for rotary drum

23
Gokul Siddharth

Appendix 5

Table 2. Position of shut-off valves once alarm is initiated

Alarm Valves and Position

HV205 HV206 HV207
DPIA+ close close open
DPIB+ open open close

Figure 9. Membrane filtration control structure

Figure 10. Membrane filtration interlock structure

24
Jonathan León Ayala

Appendix 6

PC+

from F-202A/B
CWR CWS
CV-302 HV-312
H-302
LI+-
PD+
QC LC+

V-304 V-301
to knockout
C-301 FC
HV-304 drum
Condensate

FC
M P-301A/B
H-301 FC

HV-301
to V-101
HV-305
TC
P-306A/B

TC PI TC+
P-303A/B

LC+-
to flare
Steam E HV-307
HV-315
CV-301
H-303

to knockout
HV-302
drum N2 CV-307
HV-303
PC+

CV-305
FC

CWR CWS
H-304 HV-313

PD+
QC LC+
CWS
V-305
V-302
to knockout
C-302 FC
HV-308 drum
HV-314
LC+-

P-302A/B CV-310

FC TC

HV-306 BTBAS
HV-309
H-306

PI TC+ CWR

LC+-
E
H-305

to knockout
drum
HV-311

FC

Side Pr od.
HV-310 CV-311

P-305A/B

Figure 11. Control structures for distillation columns.

25
Maria P. Galvis Cordoba

Appendix 7

a) b)
Figure 12. Atmospheric column pressure control using flooded condenser.
a) Control valve at the condensate line between the condenser and reflux drum. b) Skin-tight reflux
drum. [13]

P-303A/B

to flare
HV-307

N2 CV-307
PC+

PC+

CWR CWS
CWR CWS H-304
CV-302
H-302

V-302
to flare
V-301 C-302 HV-308

C-301 to flare
HV-304 CWS
CV-308

CV-303 P-302A/B CV-310

P-301A/B
BTBAS
HV-309 CV-309
H-306
to V-101
HV-305 CV-304 CWR

a) b)
Figure 13. Pressure control loops
a) atmospheric column C-301. b) vacuum column C-302
*Additional controllers omitted for simplicity, for complete control logic see Figure 11

26
 Maria P. Galvis Cordoba

PA+

to P-201A/B

CWR CWS
from F-202A/B I
H-302 CV-302 HV-312
PDA+ I
LA- LA+
V-301 I
LA+
V-304
I to knockout
C-301 M drum
HV-304
LA-
I Condensate
CV-303
P-301A/B
M
H-301
to HV -315
HV-301 to V-101
P-306A/B CV-301 I HV-305 CV-304
PI
Steam TA+

HV-315 LA + P-303A/B
E
I LA- to flare
H-303 HV-307
to knockout
drum
HV-303 I

N2 CV-307
PA+
HV-302

CV-305 I

PDA+ CWR CWS

H-304 HV-313
LA+
V-305
LA- LA+
V-302 I

CWS
I
LA - C-302 to knockout
M
HV-308 drum
HV-314
I
CV-308
P-302A/B CV-310

BTBAS
HV-306 CV-306
HV-309 CV-309 H-306

PI
TA+
I
CWR
LA+
E
I LA- H-305

to knockout
drum
HV-311 I

HV-310

CV-311

Side Prod .

P-305A/B

Figure 14. Columns interlocks connections.

*Process controllers omitted for simplicity, for control structures see Figure 11

27
Maria P. Galvis Cordoba

Table 3. Distillation columns alarms and trips.

Equipment Alarm/trip Remarks/actions
Buffer tank LA+ High liquid level. Turn off pump P-201.
V-304 LA- Low liquid level. Turn off pump P-306.
Reflux drum LA+ High liquid level. Open HV-304, allow for temporal
V-301 drainage.
LA- Low liquid level. Turn off pump P-301 and coil H-303.
Atmospheric PA+ High pressure. Shut off coil H-303.
column PDA+ High pressure drop. Shut off coil H-303. Flooding
C-301 indicator.
LA+ High liquid level. Open HV-303, allow for temporal
drainage.
LA- Low liquid level. Shut off coil H-303, close HV-302.
TA+ High temperature. Shut off coil H-303. Turn off HV-315.
Buffer tank LA+ High liquid level. Turn off HV-302.
V-305 LA- Low liquid level. Turn off HV-306.
Reflux drum LA+ High liquid level. Open HV-308, allow for temporal
V-302 drainage.
LA- Low liquid level. Turn off pump P-302 and coil H-305.
Vacuum PA+ High pressure. Shut off coil H-305.
column PDA+ High pressure drop. Shut off coil H-305. Flooding
C-302 indicator.
LA+ High liquid level. Open HV-311, allow for temporal
drainage.
LA- Low liquid level. Shut off coil H-305, close HV-310.
TA+ High temperature. Shut off coil H-305.
* If alarm continues, proceed to emergency shutdown of columns (see Section 6).

28
Uma Jaya Ravali Theeda

Appendix 8

Figure 15. Start-up procedure for R-101.

29
Aditya Rio Anggara

Figure 16. Start-up procedure for F-201.

30
Paras Vora

Figure 17. Start-up procedure for C-302.

31
Uma Jaya Ravali Theeda

Appendix 9

Figure 18. Shutdown procedure for R-101.

32
Aditya Rio Anggara

Figure 19. Shutdown procedure for F-201.

33
Paras Vora

Figure 20. Shutdown procedure for C-302.

34
Anusha Roshini Alagu

Appendix 10

Table 4. Emergency shutdown

Emergency Consequences Required action

Serpentine failure No reactant(s) to reactor All units are shutdown

Blockage in the flow of Pressure build up Relief valve is used

streams
(reactants/contents from
pumps and other units)

Temperature control Extreme temperature rise Increase chilled water flow

failure in reactor R-101

Recycle loop failure No flow of recycled TBA Immediate shut down and
isolation of this unit

Level control failure in Increase in level Initiate shut down

reactor R-101
Decrease in level Increase reactants flow

Level control failure in Increase in level Usage of auxiliary buffer

buffer tank tank to achieve desired
level

Temperature control Increase cooling water

failure in heat exchanger flow
Temperature increase
H-101

H-302/303/304/306 Increase chilled water flow

H-301 Temperature decrease Increase hot water flow

Cooling utilities (chilled Temperature increase 1.Close the flow of hot

and cooling water) failure streams and initiate
normal shutdown

2.Isolation of the unit

35
Anusha Roshini Alagu

Hot water failure Temperature decrease 1.Close the flow of cold

streams and initiate
normal shut down

2.Isolation of unit

Failure of the vacuum Pressure increases, drum Usage of auxiliary rotary

pump in rotary drum filter cannot hold the cake drum filter unit
(F-201)

Pressure control failure in No significant pressure Usage of auxiliary

membrane screens gradient between inlet membrane screen filter
(F-302A/B) and outlet this leads to unit
crude BTBAS liquid
carries unfiltered salt to
the distillation unit

Double failure in rotary Malfunction of the unit and Immediate shut down and
drum filter (F-201) wastage of products isolation of the unit

Double failure in Malfunction of the unit and Immediate shut down and
membrane screens wastage of products isolation of the unit
(F-302A/B)

Level control in columns Liquid level increase and Immediate shut down of
C-301 and C-302 excessive static head the required unit

Temperature control Internal heating coil leak Immediate shut down of

failure of the coils in the or rupture the required unit
columns C-301 and C-302

Pressure control failure in High vapor pressure leads Immediate shut down of
columns C-301 and C-302 to excessive heat input the required unit

Temperature control Heating and thermal Immediate shut down of

failure in the columns expansion of liquid the required unit
C-301 and C-302

36
Anusha Roshini Alagu

Condenser failure in Uncontrolled Immediate shut down of

columns C-301 and C-302 condensation/absorption the required unit
of vapor phase component

Blockage of packing/trays Leading to excessive 1.Immediate shut down of

in the columns C-301 and pressure drop in column the required unit
C-302
2.Isolation and cleaning of
the required unit

Temperature control Fire when exposing Immediate shut down of

failure in the columns packing internals with the required unit
flammable material during
C-301 and C-302 maintenance

Corrosion of internals in Heat transfer surface leak Immediate shut down of

the columns C-301 and or rupture and possible the required unit
overpressure of the low-
C-302 pressure side

Instrument air failure Valve malfunction 1.All valves must reach fail
safe position

2.Normal shut down is

executed

Power failure in preheater Function is stopped Immediate shut down

Steam failure in preheater Function is stopped Immediate shut down

Power failure Pumps are stopped 1.Close all valves around

equipment and all utilities
to heat exchanger

2.Reactor and other units

are depressurized

* Created based on [15] [18] [19] [20] [21] [22] [23] [24] [25] [26]

37
Dilshan Mihiranga

Appendix 11

Table 5. An overview of chemical compounds hazard identification

Hazard TBA [27] DCS [28] BTBAS [29] TBA.HCl [30]

Flammability Highly Extremely Flammable N/A

flammable liquid flammable gas liquid and vapor
Reaction with water N/A N/A Violently reacts N/A
with water
Releases
flammable
gases which
may ignite
spontaneously
Acute oral toxicity Harmful if N/A Toxic if Harmful if
swallowed swallowed swallowed
Acute inhalation toxicity Toxic if inhaled Fatal if inhaled N/A N/A

Skin corrosion/ irritation Causes severe Causes severe Causes severe N/A
skin burns skin burns skin burns
Eye damage Causes severe Causes severe Causes severe N/A
eye damage eye damage eye damage
Target organ toxicity May cause May cause N/A N/A
single exposure - respiratory respiratory
respiratory irritation irritation
Target organ toxicity May cause N/A N/A N/A
repeated exposure - damage to
kidney, liver organs

Table 6. Possible utility failures, affected equipment and possible solutions

Utility failure Equipment affected [31] Possible solutions [17]

Electricity Pumps and compressors Emergency power supply

Heaters Uninterruptible power supply
Instrument air
Vacuum pumps Refrigeration
units Instrumentation
Motor operated valves
Cooling water Condensers Emergency power supply
Coolers for process fluids Uninterruptible power supply
Alternative pumping
arrangements
Corrosion inhibitors
Instrument air Transmitters and controllers Air or nitrogen cylinders as
Process-regulating valves compatible back up fluids
Alarm and shutdown systems
Pumps
Inert gas Seals Nitrogen cylinders as backup
Purge of equipment

38
Dilshan Mihiranga

Table 7. Possible overpressure occurrences

Failure condition Liquid or Vapor-relief amount

Closed outlets Total incoming vapor plus that generated therein

relieving conditions
Cooling-water failure to condenser Total vapor to condenser at relieving conditions

Column top reflux failure Total incoming vapor plus that generated therein at
relieving conditions less vapor condensed by side
stream reflux
Overfilling Maximum liquid pump-in rate

Failure of automatic controls Case-by-case basis

Abnormal process heat or vapor input -

Hydraulic expansion -

Exterior fire -

Heat transfer equipment failure -

Power failure Based on effect of power failure

Relief valve sized considering the worst-case scenario
Maintenance -

* Created based on [31]

Table 8. A brief overview of fire safety of BTBAS plant

TBA [27] DCS [28] BTBAS [29] TBA.HCl [30]

Fire Water spray Fine water spray or CO2 Water spray

extinguisher CO2 fog Dry chemical CO2
media Dry chemical Dry chemical powder Dry powder
powder powder Do not use: Water
Alcohol resistant Foam and alcohol
foam Do not use: CO2 resistant foam
Do not use: Solid Stop leak if safe
water stream Do not extinguish if
leaking
Isolate fire and let it
burn out
PPE for fire SCBA SCBA SCBA SCBA
fighters Full protective gear Gas tight Face shield
chemically Butyl rubber
protective clothing equipment
(Type 1) EN 943-2 Full protective gear
Specific fire Heat may cause Heat may cause Heat may cause N/A
hazards the containers to the containers to violent rupture of
explode explode packages
Vapors may travel Flash back
to source of ignition possible over
and flash back considerable
distance

39
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