Deepak Nitrite Limited

Division APL, Roha.

SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

Responsibility :
Plant in Charge (for overall control).
Shift - in -Charges (for implementation).
Use PPEs Helmet,handgloves,Goggals,safety shoes,Belts,Gas mask (whichever
required)
Use appropriate PPEs While handling of chemicals & gases.
In process material Spec define in SOP are for guidelines &corrective action only Material
rejection criteria is not applicable for the deviations.
A)

Batch Nitration:

Records maintained in APDR 31 for Cumene , APDR33 for M-Xylene .& ARDR 33 A for
p-Xylene

Measurement of R.M.
Sulfuric acid Measurement.
1.Check the initial level of outdoor storage tank of Sulfuric acid.
2.Ensure that the measuring tank (MT)of sulfuric acid is empty.
3.Check the bottom valve of sulfuric acid measuring tank and close it , if it is open.
4.Open suction and discharge valve of sulfuric acid storage tank pump and receive sulfuric
acid into the measuring tank, till overflow start overflow nozzle at 2400 kg provided for
measured qty.
5.as soon as the overflow is observed , Switch off the pump and close both valve at
suction and discharge.
Nitric acid Measurement.
1.Check the initial level of outdoor storage tank of Nitric acid.
2.Ensure that the measuring tank (MT)of Nitric acid is empty.
3.Check the bottom valve of Nitric acid measuring tank and close it , if it is open.
4.Open suction and discharge valve of Nitric acid storage tank pump and receive Nitric
acid into the measuring tank, till overflow start till overflow start overflow nozzle at 1580 kg
provided for measured qty

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Page 1 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

5.As soon as the overflow is observed , Switch off the pump and close both valve at
suction and discharge.

Stage I : Preparation of Mixed acid.

1 Confirm that that the mixed acid preparation vessel is empty.
2.Close the bottom valve of Mixed acid preparation vessel.
3.Receive sulfuric acid from measuring tank.
4.Check outage if required
5.Then start the stirrer and apply cooling through the jacket by opening inlet and
outlet valves.
6.Ensure that the scrubber system is alkaline i.e. pH is more than 87.Ensure the cooling tower / chilling pumps is ON and cooling inlet, outlet and
vessel vent valves are open.
8.Start Nitric addition and maintain the temp. As per specified in log sheet.
9.As soon as the nitric acid addition is completed stir the mass for half an hour.
10. Withdraw the sample by sample point and send to laboratory for
analysis.Range of Sp. Gr. Is specified in log sheet.
11.Open the suction and discharge valve of mixed acid transferring pump.
12.Ensure mixed acid storage tank bottom valve is close and vent to scrubber is
open.
13.Ensure mixed acid is totally transferred from vessel and received in required
mixed acid storage tank.
Cumene / M-Xylene/Para Xylene Measurement.
1.Check the initial level of outdoor storage tank of Cumene / m-Xylene/p-Xylene.
2.Ensure that the measuring tank (MT)of Cumene/M-Xylene/p-Xylene is empty.
3.Check the bottom valve of Cumene/m-Xylene/p-Xylene measuring tank and close it , if it
is open.
4.Open suction and discharge valve of Cumene/m-Xylene /p-xylenestorage tank pump and
receive Cumene /m-Xylene/p-Xylene into the measuring tank, till overflow start till overflow
start overflow nozzle is provided at 1950 kg (Cumene) 1820 kg (m-Xylene)provided 1018
kg ParaXylene measured qty
5.As soon as the overflow is observed, Switch off the pump and close both valve at suction
and discharge

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Page 2 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

Stage II: Nitration.

1 Ensure that required Nitrator is empty and bottom valve, Manhole are closed and
vent to scrubber is open.
2 Ensure that chilling plant and supply and discharge valve are open
3 Receive Cumene/m-Xylene/p-xylene and start stirring.
4 For para xylene start addition at 15-17 dec c & after the one hrs maintain the
temp 10-15 deg C.
5 Start mixed acid addition in specified temp range between 0 to 8 deg C.for
cumene & m-xylene
6 After completion of totally mixed acid addition Close the mixed acid addition
valves.
7 Stir the reaction mass for 2 hr.(+,- 1 hr). Check the % of Para xylene.
8 Separate out the spent acid by high speed centrifuge in spent acid storage tank
and Nitromass in washing vessel.
Stage III: Washing.
For Cumene & m-Xylene Nitromass.
1 Ensure the bottom valve of washing vessel is closed and Receive two Nitrator
batches in washing vessel for washing.
2Stir well and send sample to Q.C.Lab.
3 First wash - Add equal qty. Of water and stir of 30 to 60 min.
4 Settle the mass for 30 to 60 min.
5 Separate out the water layer in washing water tank.
6 Second wash - Add equal qty. Of water and stir of 30 to 60 min.
7 Settle the mass for 30 to 60 min.
8 Separate out the water layer in washing water tank.
9 For Neutralization Charge 10-12 5 soda ash solution to bring the pH 7.25 to 9.5.and
stir it well.
10 Settle the mass for 30 to 60 min.

11
12
13
14
15

Separate out the water layer in washing water tank.

Plain wash - Add equal qty. Of water and stirr of 30 to 60 min.
Settle the mass for 30 to 60 min.
Separate out the water layer in washing water tank.
Check Initial Dip and Transferred the Nitromass in Storage tank.

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Page 3 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

16 Take final Dip and measure the Qty of batch.

Washing process for p-xylene Nitromass.

1 Ensure the bottom valve of washing vessel is closed and Receive Two Nitrator
batches in washing vessel for washing.
2 Stir well and send sample to Q.C.Lab.
3 Give water wash of 2 KL , stir for 30 min settle it for 30-60 min.
4 Check acidity
5 Calculate sodiumn bisulphite for % of tolualdeyde
Batch QTY*% of aldehyde=Net aldehyde
Convert quantity in to mole (Net aldehyde/120 mole wt of tolualdehyde)
Multiply it by 104 Mole wt of sodium bisulphite.
Multiply it by 6 for (1:6) ratio = sodium bisuphite qty
6 Prepaire 10% sol of Sodium bisulphite qty
7 Add sol into organic mass in washing vessal
8 Stirr for 3 hrs.settle for 30-60 min .
9 Check sample for % of aldehyde It should be less than 0.5 %
If aldehyde more than 0.5% then calculate as per above calculation and add extra
qty & stirr for 1-2 hrs & check the sample
10 Settle for 30-45 min &Separate the aqueous layer
11 Add 2500 2800 lit water for plain wash Settle 30-60 min and separate water
12 Add 4-5% ammonia solution and 2500-2800 L water
13 check sample for pH 6.5 to 8, Settle for 30-60 min And separate the aqueous
layer
14 Add 2500-2800 lit water for plain wash, Settle for 30-60 min And separate the
aqueous layer
15 Separate organic mass & transfer it to storage tank

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Page 4 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

B)

08

CONTINUOUS NITRATION

Records maintained in (APDR 32 for Cumene / M-Xylene.) (O-Xylene APDR-32A)

Standard Operating Procedure for Continuous Nitration plant.

Measurement of R.M.
Sulfuric acid Measurement.
1.Check the Initial level of sulfuric acid (B-6) storage tank on DCS system.
2.Open suction and Discharge valve of sulfuric acid storage pump.
Nitric acid Measurement.
1.Check the Initial level of Nitric (B-7) storage tank on DCS system.
2.Open suction and Discharge valve of Nitric acid storage pump.
Spent acid Measurement.
1.Check the Initial level of Spent acid (B-8) storage tank on DCS system.
2.Open suction and Discharge valve of Spent acid storage pump.
M-Xylene Measurement.
1.Check the Initial level of M-Xylene (B-502 A) storage tank on DCS system.
2.Open suction and Discharge valve of sulfuric acid storage pump.
Stage I Preparation of Spent acid. Whenever process requirement.
1. Ensure that the R1, R2, R3, f1 and R7, F5 all are empty.
2. Check the Bottom valve of R1, R2, R3, R7 are closed and interphase valve F1
and F5 separator is open.
3. Before starting spent acid preparation start cooling tower or chilling plant for
temp. Maintaining.
4. Start agitator of R1 for spent acid preparation.
5. Prepare spent acid by using sulfuric acid & water. The flow rate is given below
6. Sulfuric acid = 930 kg/hr
7. Water = 360 kg/hr
8. Check analysis of spent acid,reports contain
9. Sulfuric acid=70-72% & sp.grvity =1.65

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Page 5 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

10. If analysis of spent acid is ok then fill the nitrater with spent acid
R1,R2,R3,F1&also B8 level % is 40%
11. Ensure that the reactor R4,R5,R6 &F2,F3,F4 is empty
12. Ensure that bottom valve of R4, F2, R5, F3, R6, F4 is closed. Insure that
interphase valve is closed.then fill the whole washing section with water up to
interphage level.when spent acid preparation completed in nitration, then fill the
water in washing section. Now plant is ready for nitration start up.
Stage II NITRATION Process Start up
Start blower & scrubber
1. Start agitator of R1&R2.
2. Ensure that all raw material line up should be ok.

STARTING OF NITRATION
1. Press the nitration start push button provided on mimic panel
2. This will start the by pass timer ON
3. Timer will initially by pass the high \low flow trip during the start up.
4. Provision for setting this time should be available on DCS alarm\trip set page.
5. This timer will start all the nitration related pumps & control valves.
6. If the feed back of pump & flow are ok. Then nitration will start smoothly.

RATES & PRAMETERS FOR NITRATION.

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Page 6 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

Capacity wise Flow rates.

For N-Xylene
Raw material
Sulphuric Acid (98%)
Nitric Acid (98%)
Meta Xylene
Spent Acid

80
310
354
600
1200

85
330
376
637
1250

% age
90
350
398
675
1300

95
370
420
712
1350

100
390
443
750
1400

Note: (i) If the Dinitro / M-Xylene contents are higher than 2% , change the flow
rates as per
the results of analysis.
(ii)The temperature range of R1 & R2 chilled water is 30-45C and if the
temperature
goes above 45C then plant will be tripped.
(iii)The temp range of R1&R2 with Cooling tower is 30-50C and if the
temperature
goes above 50C then plant will be tripped.

For N-Cumene
Raw material
Sulphuric Acid (98%)
Nitric Acid (98%)
Cumene
Spent Acid

Reviewed by:
Plant in charge:

80
280
320
500
1100

85
298
340
531
1150

% age
90
315
360
562
1200

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Page 7 of 12

95
332
380
593
1300

100
350
400
625
1300

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

Note: (i) If the di-nitro contents/Cumene are higher than 2%, change the flow rates
as per
the results of analysis.
(ii)The temperature range of R1 & R2 chilled water is 25-35C and if the
temperature goes above 35C then plant will be tripped
. CONTINUOUS NITRATION
Measurement of R.M. For o-Xylene nitration
Check all interlockings before start the process
Sulfuric acid Measurement.
1.Check the Initial level of sulfuric acid (B-6) storage tank on DCS system.
2.Open suction and Discharge valve of sulfuric acid storage pump.
Nitric acid Measurement.
1.Check the Initial level of Nitric (B-7) storage tank on DCS system.
2.Open suction and Discharge valve of Nitric acid storage pump.
Spent acid Measurement.
1.Check the Initial level of Spent acid (B-8) storage tank on DCS system.
2.Open suction and Discharge valve of Spent acid storage pump.
O-Xylene Measurement.
1.Check the Initial level of O-Xylene (B-502 A) storage tank on DCS system.
2.Open suction and Discharge valve of sulfuric acid storage pump.
Stage I Preparation of Spent acid. Whenever process requirement.
1 Ensure that the R1, R2, F1 are empty.
2 Check the Bottom valve of R1, R2,are closed and inter phasevalve F1
separator is open.to highspeed separator
3 Before starting spent acid preparation start chilling plant for temp. Maintaining.
Write hourly Temp & pressure of chilling water supply line.

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Page 8 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

4
5
6
7
8

Start agitator of R1 for spent acid preparation.

Prepare spent acid by using sulfuric acid & water. The flow rate is given below
Sulfuric acid = 930 kg/hr
Water = 276 kg/hr
Once spent acid come out from R-1 Check sample for analysis of spent acid,
Sulfuric acid should be 72-75% check 2-3 Samples during the Spent acid
preparation. Fill it thr R1,R2,F1,Sep thr B-8.( while S.Acid. Preparation isolate
the separator by applying link.)
9 Prepare Spent acid up to 20 % level of B-8.
10 Ensure that the reactor R4,R5,R6 &F2,F3,F4 are empty
11 Ensure that bottom valve of R4, F2, R5, F3, R6, F4 is closed. Insure that
interphase valve is closed.then fill the whole washing section with water up to
interphage level.when spent acid preparation completed in nitration, then fill the
water in washing section. Now plant is ready for nitration start up.
Stage II NITRATION Process Start up
Start blower & scrubber
3. Start agitator of R1&R2, &Separator (F3).
4. Ensure that F1 Inter phase (SA) line valve to separetor,Organic

valve to B-1122 &S acid valve to B-8 are open

5. Ensure that all raw material line up should be ok.
6. Monitor the F1 Temp .should be 24 + 5 deg C
7. Ensure the chilling supply &outlet is open
STARTING OF NITRATION
7. Press the nitration start push button provided on mimic panel
8. This will start the by pass timer ON
9. Timer will initially by pass the high \low flow trip during the start up.
10. Provision for setting this time should be available on DCS alarm\trip set page.
11. This timer will start all the nitration related pumps & control valves.
12. If the feed back of pump & flow are ok. Then nitration will start smoothly.
13. Check nitromass level in B-8 in each shift and recover it .
14. Monitor B-8 temp (20-35 deg C)

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Page 9 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

Capacity wise Flow rates.

RATES & PRAMETERS FOR NITRATION.
Raw material
Sulphuric Acid (98%)
Nitric Acid (98%)
Ortho Xylene
Spent Acid

In kgs
185
211
300
1300

215
246
350
1550

230
263
375
1600

245
281
400
1660

260
299
425
1700

I) Unreacted O-Xylene in R-2 3% min & 7 % Max. & Dinitro range in R2 1.0%
ii)The temperature range of R1 (20-23 degC)& R2 -23C Max on chilling plant and
if the temperature goes above 24C then plant will be tripped

Stage III Washing and Neutralization (R4,F2,R5,F3,R6,F4) for -Nitroxylene

1. Continuous washing process By MIDC water.
2. R-4 Fresh water wash to remove acidity. (Water flow -1000 kgs /hrs + 200
kgs/hrs.)
3. Check the level of B1122 nitromass continuously and take it for washing
4. F2 separation of acidic water.
Neutralization
1. R5-Neutralize the mass (Water flow 350 kgs /hrs +100 kg, 10% Amonia
Solution 110 kgs/hrs + 50 kgs /Hrs.)
2. F3 separation of acidic wash
3. R6-Plain water wash. (Water flow -700kgs /hrs + 50 kgs/hrs.) To get till clear
separation in F4 add drop wise spent acid range of PH (1 min.-8 Max) if
required
4. F4-Separation of plain water wash and N-Xylene to B-14.
Maintain pH of Niro mass6.5 to 8) at k2 bottom.
Stage IV Distillation (K-2)
Continuous distillation by feeding Nitro mass from B-14 to separate out m-Xylene
from top and product from Bottom .Unreacted o-Xylene ( below 0.2 %) and pH
(Range 6.5 7.5) of product.
1. O-Xylene collected from top to be collected in o-Xylene charging tank to R1.
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Page 10 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

08

2. Bottom product to be collect in storage tank and transferred to Distillation

columns .
Parameters for K-2distillation.
Vacuum ( Range-700 mm/hg +,-25 mm/hg). Bottom temp (Range 170 + 5 0 C)
Top Temp ( Range- 85 + 15 0 C)
Nitration

Stage III Washing and Neutralization (R4,F2,R5,F3,R6,F4) for Meta Nitro

Xylene
5. Continuous washing process By MIDC water.
6. R-4 Fresh water wash to remove acidity. (Water flow -750 kgs /hrs + 50
kgs/hrs.)
7. F2 separation of acidic water.
Neutralization
5. R5-Neutralize the mass by 10% soda solution. (Water flow 325 kgs /hrs +50
kg, Soda Solution 200 kgs/hrs + 50 kgs /Hrs.)
6. F3 separation of acidic wash
7. R6-Plain water wash. (Water flow -600 kgs /hrs + 50 kgs/hrs.) To get till clear
separation in f4 add drop wise spent acid range of PH (1 min.-7.5 Max)
8. F4-Separation of plain water wash and N-Xylene to B-14.
Maintain pH of N-Xylene (Range 6.5 to 7.5) at k2 bottom.
Stage IV Distillation (K-2) for ortho Xylene NMass
Continuous distillation by feeding Nitro mass from B-14 to separate out m-Xylene
from top and product from Bottom .Unreacted m-Xylene ( below 0.2 %) and pH
(Range 6.5 7.5) of product.
3. M-Xylene collected from top to be collected in M-Xylene charging tank to R1.
4. Bottom product to be collect in storage tank and transferred to Distillation
columns .
5. If Imp Before O-Xylene ( N-Nonane ) above 45% the stop the recycling & drain
the material in drums.
Parameters for K-2distillation. For Meta Xylene
Vacuum ( Range-650 mm/hg +,-25 mm/hg). Bottom temp (Range 170 + 5 0 C)
Top Temp ( Range- 85 + 15 0 C)
Sample points of Continuous Nitration plant

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Page 11 of 12

Deepak Nitrite Limited

Division APL, Roha.
SOP & Safe Operating procedure of Batch &

Reference Clause Nos. 7.5.1

Continuous Nitration plant.

Department : Production

Document No. :

APD302

Issue No. :

Effective date :

15.05.10

S.R.
1

08

Frequency of use
If required
Daily in each shift
If required
If required
If required

Purpose
GC & Spent Analysis
GC & Spent Analysis
GC & Spent Analysis
Acidity
N-Cresols

if required

GC

Daily in each shift

Whenever solution
preparation

GC,PH,N-Cresols
Strength of solution

Sample point location

R-1
R-2
R-3
F-1
Washing
R-5
Distillation
K-2 Columns
Top collection line or
tank
Bottom product line
Soda/ammoni Manhole
a solution
preparation
B-501A
Bottom drain valve.

6
7

B-502A
B-502B

Bottom drain valve.

Bottom drain valve.

While change Over Decontamination

While change Over Decontamination

8
9
10
11

B-8
B-14
B-1014
B-11/12

Bottom drain valve.

Bottom drain valve.
Bottom drain valve.
Outlet or bottom valve

While change Over

While change Over
While change Over
While change Over

2
3

Steps
Nitration

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While change Over Decontamination

Decontamination
Decontamination
Decontamination
Decontamination

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Page 12 of 12