32000 Stage-I & 32003 (New Route)
Std. Qty./
Time /
Temp
Step
No.
Procedure
1.
Ensure SS Reactor _____
2.
Charge DM Water Qty.:
____ Lt,
Charge NaOH Qty.: ____
Kg,
Charge Methanol Qty.:
_____ Lt at 25°C to 35°C.
DM Water:
2.5 Lt
NaOH:
0.3 Kg
Methanol:
0.7 Lt
Parallel Operation:
Dissolve TBAB Qty.: ____
Kg with DM Water Qty.:
_____ Lt
Charge above prepared
TBAB solution into the
reactor.
Chill the reaction mass to
10°C to 15°C and maintain
the reaction mass for 45 to
60 minutes.
TBAB:
0.01 Kg
DM Water:
0.05 Lt
3.
4.
5.
6.
7.
8.
9.
Parallel Operation:
Charge Cyclohexanone
Qty.: ____ Kg and charge
4-Methoxy phenyl
acetonitrile Qty.: ____ Lt
and Methanol Qty.: ____
Lt
Add slowly above prepared
solution into the reaction
mass at 10°C to 15°C.
After completion of
addition maintain the mass
for 3 hours at 10°C to 15°C
10°C to
15°C
45 to 60
min
4-Methoxy
phenyl
acetonitrile:
1.0 Kg
Cyclo
Hexanone:
0.9 Kg
Methanol:
0.8 Lt
Date
Time
From
Observation
To
Temp:
____ °C
Temp:
____ °C
10°C to
15°C
Temp:
____ °C
3 hrs
10°C to
15°C
Temp:
____ °C
Ensure Centrifuge _____
Filter the reaction mass in
centrifuge and top wash the
10.
wet cake with DM Water
Qty.: _____ Lt
DM Water:
0.5 Lt
11. Ensure SS Reactor _____
Charge DM Water Qty.:
____ Lt, charge Wet
12. Material Qty.: ____ Kg,
charge Methanol Qty.:
____ Lt
DM Water:
4.0 Lt
Methanol:
0.518 Lt
Wet
Material
Qty.:
____ Kg
Done
by
Checked
by
32000 Stage-I & 32003 (New Route)
Step
No.
Procedure
Adjust the mass pH to
13. NMT 6.0 using Acetic
Acid Qty.: ____ Lt
Std. Qty./
Time /
Temp
Acetic
Acid:
0.02 Lt
Date
Time
From
Observation
To
pH:
_____
14. Ensure Centrifuge _____.
Filter the reaction mass in
centrifuge and top wash the
15.
wet cake with Methanol
Qty.: _____ Lt
Unload the material and
16. proceed for 32003
Hydrogenation
Methanol:
0.2 Lt
Wet
Material
Qty.:
____ Kg
Done
by
Checked
by
32000 Stage-I & 32003 (New Route)
Std. Qty./
Time /
Temp
Time
Step
No.
Procedure
1.
Ensure SS Reactor: _____
Parallel Operation:
Charge Thinner Qty.: ____
Lt.
Charge 32000 Stage-I
(Dried Basis) Qty.: _____
Kg.
Charge TMAC Qty.:
______ Kg.
Cool the reaction mass to
10°C to 20°C and transfer
into SS reactor
(Hydrogenation Reactor)
Thinner:
3.5 Lt
32000
Stage-I:
1.0 Kg
TMAC:
0.04 Kg
10°C to
20°C
Temp:
____ °C
2.
Ensure SS Reactor: _____
Charge Thinner Washed
Raney Nickel Qty.: _____
Kg.
Charge Liq Ammonia Qty.:
____ Lt
Raney
Nickle:
0.4 Kg
(For fresh
batch)
(for top up
0.05 Kg)
Liq. NH3:
1.0 Kg
Temp:
____ °C
3.
Transfer mass to SS
Reactor at 10°C to 20°C.
10°C to
20°C
Temp:
____ °C
4.
Flush out Nitrogen &
Hydrogen.
5.
6.
Maintain the Hydrogen
pressure at 8 ± 1 Kg/cm2 at
18°C to 22°C for 3 hours,
then raise the temperature
of reaction mass 25°C to
30°C, maintain for 4 hours
8± 1 Kg/cm2 at 25°C to
30°C.
Check TLC/HPLC for
reaction completion. If not
complies maintain 8± 1
Kg/cm2 at 25°C to 30°C till
complies.
Date
From
Observation
To
Temp:
____ °C
8±1
Kg/cm2
3 hours
18°C to
22°C
Temp:
____ °C
4 hours
25°C to
30°C
8±1
Kg/cm2
25°C to
30°C
Temp:
____ °C
Complies/
Not
Complies
Done
by
Checked
by
32000 Stage-I & 32003 (New Route)
Step
No.
1.
Procedure
If TLC/HPLC complies,
settle the mass for 2
hours, proceed for
Nutsche Filtration.
After filtration completion
Charge Thinner Qty.:
______ Lt, stir for 20 min,
settle for 1 hour and filter
the mass through Nutsche
filter.
Ensure SS Reactor: _____
Distill out thinner mass
below 60°C under
vacuum completely, then
Charge Water Qty.: ____
Lt and distill out Water
completely under vacuum
at below 60°C.
Std. Qty./
Time / Temp
Date
Time
From
Observation
To
Temp:
____ °C
Thinner:
0.4 Lt X 2
times
Temp:
____ °C
Below 60°C
Water:
0.65 Lt
Temp:
____ °C
4.
Cool the mass to 25°C to
35°C, Charge DM Water
Qty.: ____ Lt.
Charge Formic Acid Qty.:
_____ Kg.
DM Water:
3.0 Lt
Formic Acid:
0.2625 Kg
Temp:
____ °C
5.
Wash the reaction mass
with 2* times MDC Qty.:
____ Lt at 25°C to 35°C.
Stir 10min settle 30min
separate MDC
MDC:
1.0 Lt X 2
times
Temp:
____ °C
2.
3.
6.
7.
Ensure GL Reactor
_______
Transfer the reaction mass
to GL reactor, Add
Formic acid Qty.: ____
Kg and Formaldehyde
Qty.: _____ Kg to
reaction mass.
Raise reaction mass
temperature 95°C to
100°C and maintain the
reaction mass 5±1 hour at
95°C to 100°C.and ensure
reaction completion with
TLC/HPLC
Formic acid
0.88 Kg
Formaldehyde
1.1 Kg
95°C to
100°C
Temp:
____ °C
Complies/
Not
Complies
Done
by
Checked
by
32000 Stage-I & 32003 (New Route)
Std. Qty./
Time /
Temp
Time
Step
No.
Procedure
8.
If complies, Transfer the
mass to SS reactor and cool
the reaction mass, Charge
n-Heptane Qty.: _____ Lt
at below 40°C and raise the
reaction mass temperature
to 50°C to 55°C.
n-Heptane:
3.25 Lt
Temp:
____ °C
9.
Parallel Operation:
Dissolve NaOH Qty.: ____
Kg in Water Qty.: ____ Lt.
Water:
0.5 Lt
NaOH:
0.625 Kg
Temp:
____ °C
Charge above prepared
NaOH solution and adjust
10. the mass pH to 10.5 to 11.5
at 50°C to 55°C.
50°C to
55°C
pH:
10.5 to 11.5
Temp:
____ °C
pH:
_____
Cool the reaction mass to
25°C to 35°C,
11. Chill the reaction mass to
0°C to 3°C and maintain 2
hours.
Date
From
Observation
To
25°C to
35°C
0°C to 3°C
Temp:
____ °C
2 hours
Ensure Centrifuge ____
Filter the reaction mass in
centrifuge and Top wash
12.
the wet cake with pre
chilled n-Heptane Qty.:
_____ Lt
n-Heptane:
0.4 Lt
Temp:
____ °C
Wet
Material
Qty.:
___ Kg
Ensure Tray Dryer: _____
Dry the wet material in
13. Tray dryer at 40°C to 45°C
for 4 to 8 hours till MC
reaches to NMT: 0.5 %
40°C to
45°C
MC:
NMT
0.5 %
MC:
____ %
Done
by
Checked
by