system 300

FPG Oleochemicals

FPG CONTROLLED DOCUMENT

STANDARD OPERATING PROCEDURE (SOP)

Title:

SYSTEM 300

Document No. : FPG-III-962

Revision : 1

Expiry Date : Until Superseded

Page : 1 of 38

Owning Area : Operation

Created : Zairitah Johanis Johan, Mohamad Azman

Awang

Issue Date : 12-Sept-2011

SCOPE

System 300 – Crude Glycerine Making System.

APPROVAL

Signature Date Role

Originator:

____________________

Mohd Latifi Marop

___________________

Ester Associate

Approval:

___________________

Azizi Mohamad

___________________

MPO/Operation Manager

QA Approval:

____________________

Anh Lenuhoang

___________________

Site QA Manager

Note : Last approver forward to Standards Office.

REASON FOR ISSUE:

1. To combine SOP FPG-III-073, FPG-III-074, FPG-III-075, FPG-III-076, FPG-III-077, FPG-III-078,

FPG-III-079, FPG-III-080, FPG-III-081, FPG-III-083, FPG-III-202 into one SOP. This is due to all this

SOP are under System 300.


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1.0 Objective

To standardize the operating parameter and procedure for glycerine making process as to ensure

production of on spec product.

2.0 Scope

System 300- Crude glycerine making system.

3.0 Definition

None.

4.0 Reference

None.

5.0 Responsibilities

Ester Associates Engineer, Ester and Utility Associate Engineer.

6.0 Procedure

Follow to index.


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INDEX PAGE

1. System Description 4 - 5

2. Chemical Reaction 6

3. Flows 6

4. Equipment and Controls 7 - 9

5. Start Up 10 - 22

6. Normal Operations 23 - 28

7. Shutdown (Normal Shutdown & Emergency Shutdown.) 28 - 32

8. Operating Conditions 32

9. Troubleshooting 33 – 34

10. System Purging 35 - 36

11. Attachment 37 - 38


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1 SYSTEM DESCRIPTION

1.1 General:

1. Crude glycerine is produced as a by-product in the esterification process. Crude glycerine

produced in Ester Reactor/Settlers (T-102) is pumped to Dry Glycerine Tank (V-301) through two

heat exchangers:

i) Heavy Cut Ester/Dry Glycerine Interchanger (E-308 A/B)

ii) Dry Glycerine Pre-Heater (E-301)

These two heat exchangers are used to heat up crude glycerine to 123oC in order to vaporize

excess methanol from crude glycerine.

2. Dry glycerine from Dry Glycerine Tank (V-301) is fed into the Glycerine Column (T-301) through

two separate column inlet lines. One line is going through reboiler inlet, blended with hot

glycerine from the pot of the Glycerine Column. The other line is by passing the reboiler and

entering the Column in the middle of the packing for additional flexibility in minimizing foam

generation. Only one inlet line is use at a time.

3. Wet glycerine comes from wash water used in the Ester Wash Column (T-103).

Wet glycerine is fed into the glycerine column (T-301) through three separate column inlet lines.

i) One line is going through above the packing section of the column.

ii) The second line is going through the middle packing of the column.

iii) The other line is by passing the packing section and going through reboiler inlet blended with

hot glycerine from the pot of the glycerine column. Only one inlet line is use at a time.

This wet glycerine is interchanged with hot crude glycerine from the column prior before

introduced into the column. Anti-foam is also being introduced continuously into this line.

Methanol Dryer Feed tank (V-401) which is being introduced into wet glycerine line (if needed)

for additional flexibility in minimizing foam generation. Also to minimize glycerine carry over to

Methanol Dryer (T-401). Basically this wet glycerine acts as reflux to cool down the column

overheads temperature in order to minimize glycerine carry over to the Methanol Dryer (T-401).

Small amounts of glycerine carry over to the Methanol Dryer will cause significant foaming in the

Dryer, decreasing the tray efficiency.

4. The Glycerine Column removes extra methanol from Crude glycerine and recovers glycerine from

wash water prior to being sent for acidulation, neutralization, and evaporation processes.

1.2 Acidulation


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1. The Glycerine Acidulation system converts the soaps in the crude glycerine to fatty acids, and then

separates the fatty acids from the crude glycerine.

2. Crude glycerine from the Glycerine Column is fed along with HCI through an in-line mixer (M-

301) into the Glycerine Reactor/Settler Tank (S-302). The chemical reaction (refer to the

acidulation chemical reaction) converts the soaps into fatty acid, and as they settle down in the

Glycerine Reactor Settler (S-302), fatty acid will float to the top of the glycerine layer. This fatty

acid is skimmed continuously to the Acidulated Soapstock Surge Tank (S-306)

3. Acidulated crude glycerine from Glycerine Reactor/Setter (S-302) is fed to the Glycerine

Hydroclone (F-315) using Glycerine Hydroclone Feed Pump (P-315). The two phase mixture is

then separates into an organic phase containing predominately the fatty acis, and an aqueous

phase containing the water, the glycerine, and the residual HCL.The aqueous phase flows to the

Glycerine Neutralization feed Tank (S-315)

1.3 Neutralization

1. Excess 33% Hydrochloric Acid leaving with the glycerine out of Glycerine Neutralization Feed

Tank (S-315) is neutralized with 10% dilute caustic solution (NaOH). Leaving the Neutralization

Feed Tank (S-315), the acidulated glycerine is fed into neutralization in-line mixer (M-302)

together with dilute caustic solution and sent to the Glycerine Evaporator Feed Tank (V-305).

(Refer to the dilute caustic solution preparation description).

1.4 Evaporation

1. While settling in the Glycerine Evaporator Feed Tank (V-305), some fatty acid will float to the

top layer of the glycerine. This fatty acid is skimmed off to the Acidulated Soapstock Surge Tank

(S-306).

2. From the Glycerine Evaporator Feed Tank (V-305), semi-crude glycerine is fed into the Glycerine

Evaporator (V-306) by vacuum suction created by the Glycerine Evaporator ejector system.

3. The Glycerine Evaporator removes most of the water present in the crude glycerine.Dry glycerine

from the Glycerine Evaporator is cooled down from 100oC to 93oC using the Glycerine Product

Cooler (E-309) prior to being pumped to glycerine analysis/settling tank (S-1108).

1.5 Dilute Caustic Solution

1. The dilute caustic tank is a batch mix process; 50% caustic solution and water (ratio to the caustic)

is fed continuously into the Caustic Dilution Tank (S-303) until the tank is filled. An agitator (M-

303) in the tank ensures good mixing. The 50% caustic is supplied from the Caustic Storage Tank

(S-1104), and water is supplied from the process water tank which is steam condensate.


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2 CHEMICAL REACTION

2.1 Acidulation Chemical Reaction

In the Glycerine Column, sodium methoxide excess from the esterification process reacts with water to

form sodium hydroxide.

H2O + NaOCH3 NaOH + CH3OH

Water Sodium Sodium Methanol

Methoxide Hydroxide

Sodium hydroxide in turn reacts with carryover ester to produce soap.

Therefore, the crude glycerine out of the Glycerine Column will consist of some soap and sodium

hydroxide before being acidulated.

2.2 By acidulation process, soap is broken into fatty acid and salt.

R COONa + HCI RCOOH + NaCI

Soap Hydrochloric Fatty Salt

Acid Acid

2.3 By neutralization process, salt and water will be formed.

HCI + NaOH H2O + NaCI

Hydrochloric Sodium Water Salt

Acid Hydroxide

NaOH + RC O OCH3º RCOONa + CH3OH

Sodium Ester Soap Methanol

Hydroxide


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3 FLOWS

Refer to Piping and Instrumentation Diagram (P&ID) page number A1-311 to A1-317 and Process

Flow Diagram (PFD).

4 EQUIPMENT AND CONTROLS

4.1 Glycerine Flash System:

EQUIPMENT CONTROLLERS DESCRIPTION LOCATION

Dry Glycerine

Preheater (E-301)

TIC C001 Temperature

Controller to regulate

and control steam

flow

Temperature control

valve is located at

steam inlet line to the

preheater.

Dry Glycerine Tank

(V-301)

LIC C006 Dry Glycerine Tank

level controller

Dry Glycerine Feed

Pump (P-301)

FIC C010

SC C010

Glycerine Flow

Controller to regulate

glycerine flow from

V-301 to T-301

Pump speed control

Primary Element

(FIT C010) is at

pump discharge line.

4.2 Glycerine Column:


Glycerine

Interchanger

(E-302)

LV C024 Level control valve in

response to LIC C024

Interchanger inlet

line.

Glycerine Column

(T-301)

LIC C024

LIC C134

PIC C029

Level controller to

maintain column pot

level at setpoint.

Level controller to

maintain column pot

level at setpoint.

Pressure controller to

maintain overheads

pressure.

Primary element LG

C024 at column pot.

Pressure control

valve PV C029 is at

vapor outlet line to

Methanol Dryer

Glycerine Column

Reboiler (E-303)

TIC C023 Temperature controller to

maintain pot temperature.

Temperature valve

TV C023 is at the

steam inlet line to the

Reboiler.


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4.3 Glycerine Acidulation/Neutralization:


Acidulation Mixer

(M-301)

AIC C040

pH analysis

controller to respond

to the pH of

acidulated glycerine.

Primary element AE

C040 is at mixer

discharge line.

Glycerine

Reactor/Settler

(S-302)

LIC C043

TIC C044

Settler level

controller.

Temperature

controller for

acidulated glycerine

in settler.

Primary element

LGC043 is located

at the settler tank.

Level control valve

LVC220 is at

Acidulated

Glycerine pump (F-

315) discharge line.

Temperature control

valve TV C044 is

located at Glycerine

Bottoms Cooler (E-

306).

Glycerine

Neutralization Feed

Tank (S – 315)

LIC C222 Glycerine

Neutralization Feed

Tank level controller

Primary element LE

C222 is located at

the Neutralization

Feed Tank. Level

control valve, LV

C053 is located at

the acidulated

glycerine pump (P-

306A/B) discharge

line.

Neutralization Mixer

(M-302)

AIC C059 pH analysis

controller to respond

to the pH of

neutralizer glycerine.

Primary element AE

C-59 is at mixer

discharge line.

Acidulated Soapstock

Surge Tank (S-306)

LSH C106

LSL C106

Tank level controller Level control is

located at Soapstock

Surge Tank.


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4.4 Glycerine Evaporation V-306:


Glycerine Evaporator

(V-306)

LIC C080

FIC C081

Evaporator level

controller

Glycerine flow

controller by

Manipulating pump

speed controller SC

C081

Primary element LG

C080 at glycerine

evaporator pot.

Flow Element FE

C081 at discharge of

pump P311-Glycerine

product pump.


Reboiler

(E-307)

TIC C077

FIC C086

Reboiler temperature

controller.

Steam flow

controller.

Temperature primary

element TE C077 is at

glycerine inlet line to

reboiler.

Flow primary element

is at the reboiler steam

inlet line together with

flow control valve FV

C086.


Feed Tank

(S-305)

LIC C069

FIC C071

Feed tank level

controller.

Flow controller.

Flow valve FV C071 is

at the evaporator inlet

line.


Condensate Tank (S-

307)

LIC C079 Tank level controller. Flow control valve LV

C079 is located at

condensate pump,

P310 discharge line to

Ester Fat Trap or

Methanol

Concentrator.


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AICC 212 Hotwell pH

controller by

manipulating the

Glycerine Hotwell

Dilute Caustic pump

(P-308) Stroke

Controller SCC212

Primary element is at


condensate Tank (S-

307)

5 START UP

5.1 Dry Glycerine Tank V-301

5.1.1 Empty Startup:

1. Set Interface Level Controllers from Ester Reactor Settlers (T-102 B/C/D) at 20% in "Automatic".

The controllers are LIC A060, LIC A064 and LIC A073.

2. Open block valves on dry glycerine feed lines from the settlers.

3. Start the Ester Reactor Glycerine Pump (P-104).

Do not stand infront of the pump's seal.

Verify pump suction valving is open and NPSH is sufficient. Verify pump discharge is not dead

headed.

4. Open manual block valve from HCE distillate line to HCE/Glycerine Interchanger (E-308 A/B) if

the distillate is available.

5. On TDC, set Preheater Temperature Controller (TIC C001) at 121oC and set valve (TV C001) at

20% opening manually.

6. Open steam block valve to Preheater (E-301).

7. Raise Dry Glycerine Preheater temperature to 121oC slowly and set temperature controller (TIC

C001) in "Automatic".

8. On TDC, set Dry Glycerine Tank Level Controller (LIC C006) at 150 cm in “Automatic”.

9. Prepare for Glycerine Column startup when the level in Dry Glycerine Tank (V-301) is sufficient.

5.1.2 Normal Startup:

1. Recirculate Glycerine Column to its operating pot temperature slowly.

2. On TDC, set Dry Glycerine Tank Level Controller (LIC C006) at 150 cm in Automatic.


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3. Open block valves on dry glycerine feed lines from the settlers.

4. Start the Ester Reactor Glycerine Pump (P-104).

Ensure hand is dry.



headed.

5. Open manual block valve from HCE distillate line to HCE/Dry Glycerine Interchanger (E-308

A/B) if the distillate available.

5 START UP (cont)

5.1 Dry Glycerine Tank V-301 (cont)

5.1.2 Normal Startup: (cont)

6. On TDC, set Dry Glycerine Preheater Temperature Controller (TIC C001) at 121oC and 20%

opening in "Manual".

7. Open steam block valve to Dry Glycerine Preheater (E-301).

8. Raise Dry Glycerine Preheater temperature to 121oC slowly and set Temperature Controller (TIC

C001) in "Automatic".

9. If the tank level is already above setpoint (150 cm) during the startup, open bottom block valve to

Glycerine Column inlets and start Dry Glycerine Feed Pump (P-301) prior to step # 8. If not,

proceed in this order to preheat the glycerine.

Ensure hand is dry.



headed.

10. When flow is steady, set Glycerine Flow Controller (FIC C010) in "Cascade" mode to Tank Level

Controller Controller (LIC C006).

5.2 Glycerine Column T-301:


1. Set Methanol Dryer on "Recycle".

2. Open manual block valve on vapor line (overhead) to Methanol Dryer.

3. On TDC, set Overheads Pressure Controller (PIC C029) at 0.55 barg on TDC in "Automatic".

4. On TDC, set Reboiler Temperature Controller (TIC C023) at 140oC and set valve (TV C023) at

15% opening in "Manual".


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5. On TDC, set Glycerine Column Pot Level Controller (LIC C134) at 60 cm in "Automatic".

6. On TDC, set Glycerine Flow Controller (FIC C010) at desired rate in "Automatic".

7. Line up valves from Dry Glycerine Tank to Glycerine Column through Reboiler (E-303) to fill up

the pot.

8. Close block valve which bypass Glycerine Column Reboiler (E-303) from Dry Glycerine Tank to

Glycerine Column (T-301) middle packing..

9. Open block valve from Dry Glycerine Tank and start Dry Glycerine Feed Pump (P-301) to fill up

the pot.

5 START UP (cont)

5.2 Glycerine Column T-301: (cont)

5.2.1 Empty Startup: (cont)

Wear leather glove.



headed.

10. When there is enough level in pot, open Glycerine Column bottom block valve.

11. Close block valve on product line to Glycerine Interchanger E302(A/B/C/D/E) in order to

recirculate glycerine through Reboiler (E-303).

12. Start Glycerine Column Pump (P-304).



headed.

13. Open manual steam block valve to Glycerine Column Reboiler (E-303).

14. Recirculate the glycerine until the pot temperature and level are maintained. Raise the pot

temperature slowly.

Note :

If the pot temperature is raised to rapid, PSV C027 will lifted and realease to T-401. If the

pressure keep on increasing, PSE C026 will burst. This will also carry the glycerine to T-401. If

the pot temperature is raised too fast, it will blow the rupture disk or the pot level will trip, sending

glycerine to the Methanol Dryer (T-401).

15. Monitor the overheads temperature (TI C031) and pressure (PIC C029). When the overheads

temperature starts rising, open block valve on Ester Wash Column line to Interchanger

(E302(A/B/C/D/E) and to Glycerine Column.


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16. When pot temperature is about 140oC, set Reboiler Temperature Controller (TIC C023) in

"Automatic".

17. When feed flow is stable, set Glycerine Flow Controller (FIC C010) in "Cascade".

18. Check methanol concentration at pot of T-401 (0.10% max). Remove the ‘recycle’ mode if the

quality is within specification. Put back the controller at T-401 as in T-401 start up procedure.

19. Open block valve on product line to Glycerine Interchanger (E-302 A/B/C/D/E) and to Glycerine

Acidulation. If the pot level is too high during pot recirculation, let the product go, but be sure to

send wash water from T-103 + through Glycerine Interchanger (E-302 A/B/C/D/E) first.

20. Glycerine acidulation system should be ready when dry glycerine starts to flow through Glycerine

Acidulation Mixer (M-301).

5 START UP (cont)

5.2 Glycerine Column T-301 (Cont.)


1. Inform Ester Making area to set Methanol Dryer on "Recycle".

2. Open overheads vapor block valve to Methanol Dryer.

3. On TDC, set Overheads Pressure Controller (PIC C029) at 0.55 barg in "Automatic".

4. On TDC, set Reboiler Temperature Controller (TIC C023) in "Manual" at 20% opening with

setpoint at 140oC.

5. On TDC, set Glycerine Column Level Controller (LIC C134) at 60 cm in "Automatic".

6. Close block valve on product line from Glycerine Column to the Glycerine Interchanger (E-302

A/B/C/D/E).

7. Open block valve on product line from Glycerine Column to Glycerine Column Reboiler (E-303).

8. Start Glycerine Column Pump (P-304).



headed.

9. Open steam block valve to Glycerine Reboiler (E-303).

Wear leather glove and safety glasses.

10.Recirculate the glycerine in the pot until the pot temperature is maintained. Raise the pot

temperature slowly to 140oC.


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11. Watch the overheads temperature and pressure through TI C031 and PIC C029), respectively.

12. When the overheads temperature starts to rise, open block valve on Ester Wash Column Line to

Glycerine Interchanger (E-302 A/B/C/D/E). Make sure process water line block valve to wash

column is open.

13. While recirculating the glycerine column pot, prepare the startup procedures for Dry Glycerine

Tank (V-301). Refer to Dry Glycerine Tank (V-301) start up procedures.

14. Open bottom block valve on Dry Glycerine Tank to start the feed to Glycerine Column when it is

ready to do so.

15. Start Dry Glycerine Feed Pump (P-301).



headed.

16. Monitor pot temperature (TI C025) at 140oC and pot level (LIC C134) at 60 cm.

17. Open tempered water supply to Glycerine Column Cooler (E-306).

18. If pot temperature and level are maintained, open block valve on product line to Glycerine

Interchanger (E-302 A/B/C/D/E) and Glycerine Acidulation Reactor/Settler (S-302).

19. Prepare for Glycerine Acidulation Reactor/Settler (S-302) startup.

20. Check methanol concentration at pot T-401 (0.10% max). Remove the ‘recycle’ mode if the quality

is within specification. Put back the controller at T-401 as in T-401 starting procedure.

5.3 Glycerine Acidulation Reactor/Settler:


A. Pre-Startup:

1. Check the level in Hydrochloric Acid Storage Tank (S-1103).

2. Wash all pH probes with process water.

Use heavy duty rubber gloves and goggles.

Full body apron.

3. Check the Glycerine Column (T-301) level.

B. Startup Procedures:

1. On TDC, set Glycerine Bottom Cooler Temperature Controller (TIC C044) in "Automatic" at

79oC.

2. On TDC, set Acidulated pH Controller (AIC C040) in "Automatic" at pH 2.0.


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3. On TDC, set Glycerine Reactor Level Controller (LIC C043) in "Automatic" at 75%.

4. Open tempered water block valve to Glycerine Bottom Cooler (E-306).

5. When the glycerine flow is established, open Hydrochloric Acid Storage Tank (S-1103) block

valve. Make sure line to Acidulation Mixer (M-301) is clear.

Wear rubber gloves and goggles.

6. Start Acid Feed Pump (P-1103 A/B).

7. When the level in Glycerine Reactor is established, prepare for neutralization process startup.


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5 START UP (cont)

5.3 Glycerine Acidulation Reactor/Settler (Cont.)


1. Check level in Glycerine Column pot (T-301).

2. Check level in Glycerine Reactor/Settler (S-302).

3. If level in Glycerine Reactor/Settler (S-302) is below the interface level setpoint of 75%, proceed

with acidulation startup procedures.

4. If level in Glycerine Reactor/Settler (S-302) is above the interface level setpoint of 75%, proceed

with neutralization startup procedures.

5.4 Glycerine Neutralization:


A. Pre-Startup:

1. Check the level in Caustic Dilution Tank (S-303).

2. Check caustic dilution concentration 8-10%wt.

Use rubber glove and goggles.

3. Check the level in Glycerine Reactor Settler (S-302).

4. Ensure Glycerine Reactor Settler skimming valve is open.

5. Wash pH probe with water.

Use rubber gloves and goggles.

B. Startup Procedures:

1. On TDC, set Acidulated Glycerine Level Flow Controller (LIC C043) in "Manual" at 10% valve

opening.

2. On TDC, set neutralized pH controller (AIC C059) in "Automatic" at pH 5.1.

3. Open Glycerine Reactor/Settler (S-302) product block valve.

Use rubber gloves.

4. Start Acidulated Glycerine Pump (P-306 A/B).

Use rubber gloves.


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5. Open Caustic Dilution Tank (S-303) block valve.

Use rubber gloves.

6. Start Dilute Caustic Pump (P-307 A/B).

Use rubber gloves.

7. When the flow of Acidulated Glycerine and interface Level in Glycerine Reactor/Settler (S-302)

are established, set Acidulated Glycerine level controller (LIC C043) in automode.

5.5 Glycerine Evaporator:

5.5.1 Empty Startup

5.5.1.1 Pre-Startup Check

1. Check the level in Glycerine Evaporator Feed Tank (S-305) to make sure the glycerine level is

sufficient.

2. Open chilled water supply block valves to Glycerine Evaporator Ejector Intercondenser (E-310)

and open booling water supply block valve to Glycerine Evaporator Ejector Aftercondenser (E-

311).

3. Open cooling water block valve to the Glycerine Evaporator Condenser (spiral) (E-305).

4. Purge the product line to S-1106A/B.

Note: Proceed with System Startup if vacuum startup procedures are not to be conducted.

5. Open tempered water supply block valve to Glycerine product cooler (E-309)

5.5.1.2 Vacuum Startup

A. Startup Glycerine Evaporator Ejector System and Conduct No-Load Test.

1. Refer to Appendix A on starting and testing the ejector system.

B. Check Utilities Supply To Glycerine Evaporator.

1. Make sure cooling water block valve to the Glycerine Evaporator Condenser (spiral) (E-305) is

opened.

2. Make sure chilled water block valve to Glycerine Evaporator Ejector Intercondenser (E-310) is

opened.

3. Check to make sure that cooling water block valve to Glycerine Evaporator Ejector after

Condenser is opened.

Note: Refer to the Pre-Startup Check.


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5 START UP (cont)

5.5 Glycerine Evaporator (Cont.)

5.5.1 Empty Startup (Cont.)

5.5.1.2 Vacuum Startup (Cont.)

C. Conduct Leak Check On Evaporator Vapor Block Valve.

1. Open Glycerine Evaporator vapor block valve.

2. On TDC, monitor Glycerine Evaporator vacuum pressure through Overhead Pressure Controller

(PIC C078) to build up.

Note: It might take sometime for the vacuum to build up `and becomes steady.

3. When vacuum in Glycerine Evaporator is steady, close Glycerine Evaporator vapor block valve.

4. Monitor vacuum pressure change. If vacuum breaks drastically, there is some leak in the system.

Troubleshoot, if necessary.

5. If vacuum does not break drastically, stop steam supply to Glycerine Evaporator ejector starts from

first stage ejector (J-301A) followed by the second stage ejector (J-301B).

6. Monitor vacuum pressure change again. If vacuum breaks drastically, Glycerine Evaporator

vacuum vapor block valve is leaking, otherwise it is okay. Troubleshoot, if necessary.

D. Restart Glycerine Evaporator Ejector System.

1. Open steam block valves to the second stage ejector (J-301B) then to the first ejector (J-301A).


3. On TDC, monitor Glycerine Evaporator vacuum

E. Conduct Glycerine Evaporator Vacuum Drop Test.

1. When vacuum in Glycerine Evaporator is steady, close Glycerine Evaporator vapor block valve.

2. Monitor vacuum change. If vacuum breaks drastically, there is leak in the system. Troubleshoot,

if necessary.

3. Open Glycerine Evaporator bottom block valve. Monitor vacuum change. If the vacuum breaks,

there is leak in the system. Troubleshoot, if necessary.

4. Open suction valve of Glycerine Evaporator Pump (P-309). Monitor vacuum change.


5. Open discharge valve of Glycerine Evaporator Pump (P-309). Monitor vacuum change.



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6. Close suction and dishcarge valves of Glycerine Evaporator Pump (P-309).

7. When there is no drastic change in vacuum , the system is confirmed no vacuum leak

5 START UP (Cont)



5.5.1.3 System Startup

1. On TDC, set the Overhead Pressure Controller (PIC C078) in "Automatic" at 70 mm Hg.

2. Open the bypass block valve on Glycerine Evaporator vacuum bypass line.

Note: This valve is closed during the No-Load Test on the Ejector system.


Note: This valve is closed during the Vacuum Drop Test.

4. Open steam block valves to the Glycerine Evaporator steam ejectors. Open the steam block valve

to the second ejector (J-301B) first, then to the first ejector (J-301A).

Note: The steam ejectors are not working if the vacuum startup procedures are not carried out

prior to the System Startup.

5. On TDC, set Glycerine Evaporator Pot Level Controller (LIC C080) in "Automatic" at 50%.

6. On TDC, set glycerine Feed Flow controller FIC-C071 in ‘Auto’ 3000kg/hr - 5000 kg/hr to build

up level in glycerine Evaporator.

7. On TDC, set steam Flow Controller (FIC C086) in "Manual" at 20% valve opening. Introduce

steam only when pot in Glycerine Evaporator is established and pump P-309 is running.

8. On TDC, set Overheads Pressure Controller (PIC C078) in "Automatic" at 70 mm Hg.

9. On TDC, set Evaporator Product Flow Controller (FIC C081) in "Automatic" at desired rate.

10. Open block valves of glycerine feed from Glycerine Evaporator Feed Tank (S-305) to Glycerine

Evaporator (V-306).

11. Close Glycerine Evaporator product block valve to Glycerine Product Cooler (E-309).

12. When the level in Glycerine Evaporator pot level reaches 50%, open Glycerine Evaporator bottom

block valve.

13. Start Glycerine Evaporator Pump (P-309).

Give audible signal "All Clear" to warn people in the vicinity before start button is pushed.

Ensure guard in place before start the pump.



Revision :1


Page : 20 of 38


headed.

14. On TDC set Glycerine Feed Flow Controller FIC C071 in ‘cascade’ to glycerine evaporator feed

tank level controller LIC C069 set point at 405 cm.

5 STARTUP (Cont.)



5.5.1.3 System Startup (Cont.)

15. Open steam block valve to Glycerine Evaporator Reboiler (E-307).

16. Recycle the product through the Glycerine Evaporator Reboiler (E-307). Raise the pot temperature

slowly until it reaches 100oC and set Steam Flow Controller (FIC C086) in "Cascade" to Interface

Temperature Controller TICC 077..

17. When the moisture level in glycerine is within specification, open product block valve to Glycerine

Product Cooler (E-309).

18. Open valve to glycerine analysis/settling tank (S-1106A/B). Ensure valve line up to one tank at

one time. (Refer to SOG System 1100).

19. Start Glycerine Product Pump (P-311).





headed.

20. Set Glycerine Evaporator Product Flow Controller (FIC C081) in "Cascade" to Glycerine

Evaporator Pot Level Controller (LIC C080).

21. Open suction valve and discharg valve of Glycerine Hotwell Dilute Caustic Pump (P-308).

Use rubber gloves.

22. On TDC, set glycerine hotwell pH controller (AIC C212) in “Automode” at pH setpoint 7.5.

23. Start Glycerine Hotwell Dilute Caustic Pump (P-308) to neutralize condensate in the hotwell.

24. Set the Glycerine Evaporator Condensate Tank Level Controller (LIC C079) at on "Automatic" at

50%.

25. When the level reaches 50%, open the Glycerine Evaporator Condensate Tank (S-307) bottom

block valve.

26. Open block valve to Methanol Concentrator (T-403) unless methanol concentrator is down, then

divert to Ester Fat Trap.


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27. Start the Glycerine Evaporator Condensate Pump (P-310) and send the condensate to Ester Fat

Trap (T-403) or Methanol Concentrator.





headed.

5 START UP (cont)


5.5.2 Normal Startup

5.5.2.1 Pre-Startup Check

1. Check the level in Glycerine Evaporator Feed Tank (S-305) to make sure the glycerine level is

sufficient.

2. Open chilled water supply block valves to Glycerine Evaporator Ejector Intercondenser (E-310)

and cooling water supply block valves to Glycerine Evaporator Ejector Aftercondenser (E-311).

3. Open cooling water block valve to the Glycerine Evaporator Condenser (spiral) (E-305).

5.5.2.2 System Startup

1. On TDC, set the Overhead Pressure Controller (PIC C078) in "Automatic" at 70 mm Hg.

2. Open the bypass block valve on Glycerine Evaporator vacuum bypass line.


4. Open steam block valves to the Glycerine Evaporator steam ejectors. Open the steam block valve

to the second ejector (J-301B) first, then to the first ejector (J-301A).

5. On TDC, set Glycerine Evaporator Pot Level Controller (LIC C080) in "Automatic" at 50%.

6. On TDC, set Glycerine Feed Flow Controller (FIC C071) in "Automatic" at desired rate. Begin

with low rate.

7. Check the Evaporator pot level. If there is no level present, follow the empty startup procedures.

8. If the level is present, open bottom block valve and line up valves through the Reboiler circulating

line.

9. Start Glycerine Evaporator Pump (P-309) and recirculate the glycerine in the pot.

Do not stand infront of pump's seal.


headed.


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Page : 22 of 38

10. Open steam block valve to the Reboiler.

11. On TDC, set Steam Flow Controller (FIC C086) in "Manual" at 20% valve opening. Open valve

gradually to raise temperature slowly to 100oC (TIC C077)

12. On TDC set pot temperature (TIC C077) on "Automatic" at 100°C and change Steam Flow

Controller FICC 086 from "Manual" to "Cascade".

13. When the vacuum and pot temperature are maintained, test the moisture content in the evaporated

glycerine.

14. Open Glycerine Evaporator Feed Tank (S-305) block valve. Start feeding the Evaporator at desired

rate.

15. Open tempered water block valve throttle it to get temp within 95OC to 100

OC to the Glycerine

Product Cooler (E-309).

16. Open glycerine product block valve through the Glycerine Product Cooler (E-309) to the Glycerine

Analysis/Settling Tank (S-1106A/B).

17. Open block valve to Glycerine Analysis/Settling Tank (S- 1106A/B). Before starting P-311, ensure

valve line up to either S-1106 A or B is already open. (One tank at one time). (Refer to SOG

System 1100).

18. Start Glycerine Product Pump (P-311).



headed.

19. On TDC, set Glycerine Hotwell pH Controller (AIC C212) in “Automode” at pH setpoint 7.5.

20. Line-up suction and discharge valve of glycerine Hotwell Dilute Caustic Pump (P-308).

Use rubber gloves.


5.5.2 Normal Startup (Cont.)

5.5.2.2 System Startup (Cont.)

21. Start Glycerine Hotwell Dilute Caustic Pump (P-308).

22. Set the Glycerine Evaporator Condensate Tank Level Controller (LIC C079) on "Automatic" at

50%.

23. When the level reaches 50% and pH condensate in the hotwell is 7 to 8, open the Glycerine

Evaporator Condensate Tank (S-307) bottom block valve.


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24. Open block valve to Methanol Concentrator (T-403). (If methanol concentrator is down, then open

to Ester Fat Trap.)

25. Start the Glycerine Evaporator Condensate Pump (P-310) and send the condensate to Methanol

Concentrator (T-403).



headed

5 START UP (cont)

5.6 Caustic Dilution:

Caustic solution process is a batch mix process.

5.6.1 Startup:

1 On TDC, set Water Flow Controller (FFIC C056 ) in "Cascade" mode with Caustic Controller (FIC

C055)

2. Set the flow rates at desired setpoint to obtain caustic concentration of 8-10 wt %.

3. Open cooling water block valve to Caustic Dilution Water Cooler (E-304).

Wear glove.

Ensure the valve is clean of oil or any particle that is jutting out.

4. Open water block valves from process water supply line to the Caustic Dilution Tank (S-303).

Wear glove.


5. Open Caustic Storage Tank (S-1104) block valve to caustic Dilution Tank S-303.

Wear rubber glove.


6. Start the Caustic Delivery Pump (P-1102).

7. When tank level is established, start the Caustic Dilution Tank Mixer (M-303).

8. Obtain sample to adjust the concentration.

Wear eye protecting goggles and face shield when working around caustic.

Flush with water for at least 15 minutes if splashed into eye.

Wear rubber glove and apron. Wear protective clothing.

Use an approved neutralization solution if available.

9. When tank is full, the solenoid valves on both caustic and process water supply lines will close

automatically. The Caustic Delivery Pump (P-1102) will stop automatically.


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Page : 24 of 38

10. Proceed with Caustic Dilution Shutdown. ( Section 8 )

6 NORMAL OPERATION

6.1 Glycerine Column:

1. Always monitor pot temperature by controlling the reboiler temperature.

2. Monitor reboiler steam valve which can be out of control whenever pot level starts to change.

3. If pot level keeps fluctuating , possible reason can be foaming in the pot. Use the required

antifoaming to solve the foaming problem.

4. Keep overheads temperature TIC 031 at 102oC -113

o

C by controlling the amount of (Wash Column

Water Flow) introduced to the column overhead.

5. Check Dry Glycerine Preheater (E-301) temperature and Dry Glycerine Tank (V-301) temperature

set at 121oC-1250C.

6. Too high overheads vapor temperature will upset the Methanol Dryer performance.

7. Monitor the Glycerine Bottoms Cooler (E-306) performance in order to keep the glycerine

temperature at 79°C prior to being acidulated.

8. Check the Dry Glycerine Tank (V-301) level.

9. Monitor the overheads pressure at PIC C029 (0.55 barg) to avoid rupturing the rupture disc.

6.2 Glycerine Acidulation:

1. Always check Caustic Dilution Tank (S-303) level to ensure enough caustic supply.

2. Check for dilute caustic concentration to be within 8-10 wt. %.

3. Check HCL Storage Tank Level to ensure enough HCL supply.

4. Check the Glycerine Bottoms Cooler (E-306) performance. Make sure that the glycerine

temperature out of the Glycerine Bottoms Cooler (E-306) is at 79oC.Otherwise, too high

temperature will damage the pH probes and fiberglass Glycerine Reactor/ Settler (S-302) tank.

5. Watch for the Glycerine Reactor/Settler (S-302) level and temperature.

6. Control the amount of tempered water to the Glycerine Bottoms Cooler (E-306) to avoid the

glycerine from making up in the cooler.


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Page : 25 of 38

7. Always check for pH probes performance by verifying the reading with pH paper. Run the water

through pH probe lines, if the probes are found dirty. Make sure that both pH probes are calibrated

once per week by E & I.

8. The optimum acidulation pH is 2. If for any reason, pH 2 can not be reached, the maximum

allowable acidulation is 3.

9. The pH for the neutralization process is between 5 to 7 with the target of 5.2.

10. Failure to maintain the acidulation pH at max 3 can lead to a major upset in downstream process.

Unacidulated glycerine becomes jelly like material and creates line plugging problem. The

Glycerine Evaporator operation will go erratic as the unacidulated Glycerine will go up and plug

up the ejector system. If this situation occur, system need to be shutdown to fix the problem. It

also will cause product in storage to have high TFA.

11. Failure to maintain the neutralization pH between 5.0 to 6.0 can also lead to downstream

process upset. It will also pose a danger of the downstream equipment structural damage due to

the acidity condition. If he condition is too alkaline, vacuum will fluctuate indicating foaming in

Glycerine Evaporator and also MeOH Concentrator.

12. The fat is skimmed continuously from the Glycerine Reactor/Settler (S-302) to the Acidulated

Soap Stock Surge Tank (S-306). Refer to Skimming Procedure to Glycerine Acidulation

Reactor/Settler (S-302).

13. Prepare the dilute caustic batch, if necessary, to keep the dilute caustic supply available. Always

keep the mixer running as there is liquid over the agitator blades.

6.3 Glycerine Evaporator:

1. Check the level in the Glycerine Evaporator Feed Tank (S-305).

2. Skim the fat out of Glycerine Evaporator Feed Tank to the Acidulated Soap Stock Surge Tank (S-

306). Refer to Skimming Procedure for Glycerine Evaporator Feed Tank (S-305).

3. Maintain the evaporator pot temperature by controlling TIC C077 at 100oC.

4. Maintain the vacuum in the evaporator at 70 mm Hg vacuum.

5. Check the level in the Glycerine Evaporator Condensate Tank (S-307).

6. Obtain a sample from the Glycerine Evaporator Feed Tank and test for moisture if Glycerine

Evaporator having problem such as vacuum problem. (Refer to SOG System 300 –

Troubleshooting)

7. Obtain a sample from the Glycerine Evaporator line to Glycerine Analysis/Settling Tank and check

for glycerine concentration, moisture, ash content, etc. (refer to control sample plan).

8. Maintain the temperature of glycerine out of Glycerine Product Cooler (E-309) at 93oC.

9. Maintain the Glycerine Evaporator pot level by operating in CAS mode FIC C081 or adjust the

flow rate if necessary.


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Page : 26 of 38

6 NORMAL OPERATION (Cont)

6.3.a E 307 Glycerine Evaporator Reboiler -- Steam Blow Procedure

1. Stop feed from Evaporator Feed Tank to Glycerine Evaporator

2. Reduce Evaporator Pot level to 5%

3. Stop P-311, Glycerine Pump to Analysis Tank

4. Stop P-309, Glycerine Evaporator Pump

5. Close FV C086, steam control valve to E-307

6. Close 4" steam block valve upstream of FV C086

7. Close 3" block valve at the inlet of E-307

8. Close 6" block valve at the inlet of E-307

9. Connect 1/2" h/p steam hose to drain valve at inlet of E-307

10. Steam blow through this valve into E-307

11. Monitor vacuum and temperature of Evaporator

12. Stop steam blow after 15 minutes

13. Reopen 6" block valve at the inlet of E-307

14. Connect 4nos. 1/2" h/p hose to the following locations:

2 nos. at inlet to Reboiler E-307

1 nos. at PI C076 (outlet of Reboiler)

1 nos. at sample point of P-309 discharge

15. Run back P-309

16. Open all the valves (4 nos.) and drain glycerine into Soapstock Surge Tank through bucket

strainer.

17. Stop pump P-309 when it start to cavitate.

18. Pump filtered glycerine to Soapstock Tank S-1101


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Page : 27 of 38

19. Line up all the valves back to normal position and start back glycerine system

6.4 Caustic Dilution:

1. Caustic dilution process is a batch mix process. Proceed with startup and shutdown procedures

when supply in the tank is empty or full.

2. Always verify the concentration of the solution to be at 8-10 wt %.


6.5 Skimming Procedure:

6.5.1 Dry Glycerine Tank (V-301)

1. On TDC, set the Dry Glycerine Tank Level Controller (LIC C006) at sufficient level to perform the

ester skimming. The Dry Glycerine Feed Pump (P-301) speed will automatically slow down in

order to reach the set point. (Assuming under normal operation the level is below the skimming

level).

2. As the level reaches set point, open the highest draw off skimming block valve.

Wear glove.


3. Open the self-closing valve on the sample connection to check the ester present in the Dry

Glycerine Tank (V-301). If nothing flowing out, open the next draw off skimming block valve.

Wear glove.


4. Put water in a beaker and test for ester. If ester present it will float on top of the water otherwise if

it is glycerine it will mix with water.

Wear glove.


5. If ester present open the skimming block valve to the Glycerine Storage Tank (s-1102).

Wear glove.


6. Allow the skimmed ester flow to the Glycerine Storage Tank (S-1102) for a while before

performing another test for ester.

Wear glove.


7. If glycerine present stop skimming. Close the skimming block valve to the Glycerine Storage Tank

(S-1102) and close the draw off skimming block valve.


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Page : 28 of 38

Wear glove.



6.5 Skimming Procedure (Cont.)

6.5.2 Glycerine Acidulation Reactor/Settler (S-302)

1. Fatty acid skimmed from the Glycerine Reactor/Settler and Glycerine Evaporator Feed Tank is fed

into the Soap Stock Surge Tank.

2. As the level of Fatty Acid in the Soap Stock Surge Tank reaches a certain high level, the

Acidulated Soap Stock Transfer Pump (P-312) will start automatically and transfer the fatty acid to

the Soap Stock Storage Tank (S-1101 A/B).

3. As the level in the Soap Surge Tank reaches a certain low level, the pump will stop automatically.

6.5.3 Glycerine Evaporator Feed Tank (S-305)

1. On TDC, set the Glycerine Evaporator Feed Tank Level Controller (LIC C069) to sufficient level

to perform fatty acid skimming. This will automatically reduce the flow of glycerine to the

Glycerine Evaporator (V-306).

2. As the level reaches set point, open the highest draw off skimming block valves.

Wear glove.


3. Open the sample connection block valve to check the fatty acid present in the Glycerine Evaporator

Feed Tank (S-305). If nothing flowing out, open the next draw off skimming block valve.

Wear rubber glove.


4. Get an empty beaker and draw some sample in. Observe the color of the sample. Fatty acid is a

black soapy liquid whereas glycerine is a dark brown liquid.

Wear glove.


Wear the proper protection clothing anytime a sample is taken including eye protection.

Keep sample away from heat or open flame.


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Page : 29 of 38

5. Allow the skimmed fatty acid flow to the Soap Stock Surge Tank (S-306) for a while before

performing another test for fatty acid.

Wear glove.


Wear the proper protection clothing anytime a sample is taken including eye protection.

Keep sample away from heat or open flame.

6. If glycerine present stop skimming, close the skimming block valve to the Soap Stock Surge Tank

(S-306) and close the draw off skimming block valve.

Wear glove.


6. NORMAL OPERATION (Cont)

6.5 Skimming Procedure (Cont.)

6.5.4 Glycerine Storage Tank (S-1102)

1. Divert rework from Glycerine Storage Tank (S-1102) to Soapstock Surge Tank to avoid sludge or

black material from entering Glycerine Acidulation Reactor/Settler (C-302).

2. Get an empty beaker and draw some sample in. observe the color of the sample. Sludge or black

material are viscous whereas glycerine is a dark brown liquid.

Wear rubber glove.


Wear the proper protection clothing anytime a sample is taken including eye protection (goggles).

3. If glycerine present open block valve to Glycerine Acidulation Reactor/Settler (S-302) and stop

skimming. Close the skimming block valve to the Soapstock Surge Tank (S-306).

Wear glove.


7. NORMAL SHUTDOWN

7.1 Dry Glycerine Tank V-301

1. Close steam block valve to Preheater (E-3 01 ).

2. Close HCE distillate block valve to HCE/Dry Glycerine Interchanger (E-308).

3. Close manual block valves on dry glycerine feed lines.

4. Monitor Dry Glycerine Tank level.

5. Prepare for Glycerine Column shutdown.

Any particle that is jutting out.


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7.2 Glycerine Column T-301

1. Set Methanol Dryer on "Recycle".

2. Remove Dry Glycerine Tank Level Controller (LIC C006) from "Cascade" mode with

Glycerine Flow Controller (FIC CO 10) and set Glycerine Flow Controller (FIC CO 10) in

"Automatic" mode.

3. Let the Dry Glycerine Tank level drop to a reasonable level, approximately 40%, so that

another 10% of heated glycerine can be added to preheat the tank content during the startup.

7. NORMAL SHUTDOWN (Cont)

7.2 Glycerine Column T-301 (Cont)

4. Close steam block valve to Glycerine Column Reboiler (E-303).

5. Stop Dry Glycerine Feed Pump (P-301).

6. Close Dry Glycerine Tank (V-301) block valve.

7. Stop Glycerine Column Pump (P-304).

8. Close Glycerine Column (T-301) bottom block valve.

9. Purge the line with nitrogen:

i) Close block valve from Dry Glycerine Tank to Glycerine Column Reboiler (E-303) line so that

nitrogen will purge the dry glycerine inlet line to Glycerine Column located in between two

packings.

Wear leather gloves and goggles.

ii) Then, close block valve from Dry Glycerine Tank to the dry glycerine inlet line to Glycerine

Column and open the block valve for the line going through the Glycerine Column Reboiler

(E-303). This way, nitrogen will purge the reboiler recirculation line.

Close block valve when the line is clear and stop purging.

Wear leather gloves and goggles.

10. Purge the line to Glycerine Reactor/Settler thru Glycerine Interchanger with Nitrogen. Make sure

the acidulation pH probe is already isolated.

Wear leather glove and safety glasses.

11. Inform Ester Making area to prepare to shutdown the Ester Wash Column (T-103). Close water

block valve from Ester Wash Column to Glycerine Column.

12. If overheads vapor pressure is lower than its setpoint (0.55 barg), pressure control valve (PV C029)

is already in close position.

13. Secure the vapor line to Methanol Dryer by closing the manual block valve on vapor line to


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Page : 31 of 38

Methanol Dryer.

14. Remove Methanol Dryer from recycle, if necessary.

7.3 Glycerine Acidulation Reactor/Settler

1. Isolate acidulation pH probe (AE C040) prior to purging the line.

Use rubber gloves.

2. When the glycerine from Glycerine Column stops flowing to Acidulation Mixer (M-301), stop

the HCL acid feed pump (P-1103 A/B).

Use heavy duty rubber gloves.

3. Close block valve at HCL Storage Tank (S-1103).


4. Close acid line block valve to Acidulation Mixer (M-301).


5. Close glycerine line block valve to mixer when nitrogen purging from Glycerine Column clears the

line.

6. Clean up the pH probe (AE C040) with process water.


7. Let the pH probe (AE C040) immerse in water.

7.4 Glycerine Hydroclone

1. Stop Glycerine Hydroclone feed pump (P-315)

2. Close 3” block valve from Glycerine reactor/settler (S-302)

3. Porceed with Nitrogen blow from S-302 to Glycerine Neutralization feed Tank (S-315)

4. Put LIC C043 at manual 0% valve output.

5. Close suction valve of hydroclone feed pump.

6. Close 1” block valve inlet to glycerine hydroclone (F-315)

7. Then proceed with glycerine neutralization process shutdown procedure.

7.5 Glycerine Neutralization;


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Page : 32 of 38

1. Stop Dilute Caustic Pump (P-307 A/B). Refer to Caustic Dilution Normal Shutdown procedures.

2. Close Caustic Dilution Tank (S-303) block valve.


3. Stop Acidulated Glycerine Pumps (P-306 A/B).

4. Close glycerine Neutralization Feed Tank (S-315) outlet block valve.

5. Isolate the neutralization pH probe (AE C059).


6. Purge acidulated glycerine line with N2 from S-315 to Evaporator Feed Tank (S-305).

7. When acidulated glycerine line clears, stop purging.

8. Put LIC C222 in Manual 0% control valve output.

9. Wash the pH probe (AE C039) with process water.

Use rubber gloves.

10. Let the pH probe immerse in water.

7.6 Glycerine Evaporator V-306;

1. Close steam block valve to Glycerine Evaporator Reboiler (E-307).

2. Close manual block valve of glycerine feed from Glycerine Evaporator Feed Tank (S-305) to

Glycerine Evaporator (V-306).

3. Purge the line with N2·

4. Stop Glycerine Evaporator Pump (P-309).

5. Close bottom block valve of Glycerine Evaporator (V-306).

6. Stop Glycerine Product Pump (P-311).

7. Close block valve line to Crude Glycerine Surge Tank (S-1108).

8. Purge the product and recirculating lines with N2·

9. Purge line from Pump (P-311) to Crude Glycerine Surge Tank (S-1108) with N2.

10. Close steam block valve to ejector system. Close steam block valve to the first ejector (J-301A)

first and then to the second ejector (J-301B).

11. Close cooling water supply block valve to Glycerine Evaporator Condenser (Spiral) (E-305).


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Page : 33 of 38

12. Close chilled water supply block valves to ejector intercondenser (E-310) and cooling water supply

block valve to ejector aftercondenser (E-311).

13. Close tempered water supply block valve to Glycerine Product Cooler (E-309).

14. When the recirculating line is clear, close the recirculating line block valve. This will prevent the

glycerine from flowing back through the line.

15. Stop all N2 purging when lines are clear.

7. NORMAL SHUTDOWN (Cont)

7.7 Caustic Dilution

1. Close caustic block valve at Caustic Storage Tanks (S-1104).

Wear glove.


2. Purge the caustic line with nitrogen until the line is clear.

Ensure all the valve on that line is open to avoid over pressure.

3. Stop purging.

Wear glove.


4 Close water block valve from process water supply line.

Wear glove.


5. Close cooling water block valves to the Caustic Dilution Water Cooler (E-304).

Note: The agitator will keep running until the level reaches a certain low level where the agitator

will stop automatically.

Wear glove.

Ensure the valve is clean of oil or any particle that is jutting out

8 EMERGENCY SHUTDOWN

Initiate when: Fire in process area

Power failure

Evacuation Order


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A. Procedures:

1. Activate all fire valves on all tanks, Methanol Dryer and Sodium Methoxide Column.

2. On TDC, manually close all steam control valves to Reboiler and preheaters.

3. Disconnect the circuit breakers to stop all feed pumps.

4. On TDC, set controllers on "Manual" mode and output at zero.

9 OPERATING CONDITIONS

Refer to Basic Operating Guideline (BOG)

System 300.

10 TROUBLESHOOTING

A. Glycerine Acidulation and Neutralization:

PROBLEM POSSIBLE CAUSE ACTION/RESPONSE

Too low of pH from

Glycerine Acidulation

Mixer (M-301)

Dirty pH probe

Acid pump speed is too high.

1. Check the pH with pH

paper.

2. Clean up the probe with

water. Check probe for

crack.

3. Recalibrate the probe and

transmitter.

1. Check pump motor

transducer.

Too high of pH from

Glycerine Acidulation

Mixer (M-301).

Dirty pH probe.

Acid pump fails.

Acid storage empty.

1. Recheck the pH with pH

paper.

2. Clean up the probe. Check

phrobe for crack.

3. Recalibrate the probe and

transmitter.

1. Check the pump.

2. Check the acid storage

level.


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High glycerine

temperature out of

Bottoms Cooler

Fouling in heat exchanger.

Out of tempered water.

1. Hot water wash in

glycerine line or, if

possible, use acid wash.

1. Check tempered water

supply.

10 TROUBLESHOOTING (Cont.)

B. Glycerine Evaporator:



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Loosing Vacuum Air leaks.

High level in ejector condenser.

Low water flow to ejector into

and after condensers.

Low steam pressure to ejectors.

Too much condensate in steam

line.

Too much water sources in feed.

Too much water in the

neutralized glycerine.

1. Run pressure drop test on

Glycerine Evaporator to

check for leaks or any

means available.

1. Check valve line-up to

condensate tank.

1. Increase water flow. After

condenser might be fouling.

1. Increase steam pressure.

1. Check steam traps.

1. Check feed moisture

content.

1. Check caustic and acid

concentration.

2. Check process water line to

pH probe for leaking

valves.

Low pot temperature Fouling reboiler. 1. Check reboiler.

2. Check steam pressure.

Too low concentration Low pot temperature. 1. Raise pot temperature.

10 TROUBLESHOOTING (Cont.)

B. Glycerine Evaporator:


P-311 trip on high

amp upon starting

after shutdown

N2 pocket trapped in line

Dead headed

1. Check discharge pressure

2. Check line up at Glycerine

Analysis/Settling Tank

11 SYSTEM PURGING

1. The N2 line purge to glycerine line to reactor is still on while purging the reactor system. Open

bottom block valve and skimmer line block valve on Dry Glycerine Tank (V-301).


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Page : 37 of 38

2. Check oxygen content in Dry Glycerine Tank (V-301). If less than 1%, close bottom and ester

skimmer line block valves.

3. Stop N2 purging to glycerine line from Reactor to Dry Glycerine Tank (V-301).

4. Open N2 line to purge the glycerine line to Glycerine Column. Make sure all valves on that line

are opened.

5. Open glycerine column bottom block valve.

6. Open glycerine column overheads vapor block valve to MeOH Dryer.

7. Check oxygen content in the Glycerine Column. If less than 1%, close bottom block valve.

8. Close overheads vapor block valve.

9. Stop N2 purging through glycerine line to Glycerine Column.

10. Open N2 line to purge glycerine line from Glycerine Column to Glycerine Reactor (S-302).

11. Open N2 line to purge glycerine line from Glycerine Storage Tank (S-1102) to Glycerine Reactor

(S-302).

12. Open N2 line to purge HCL line from HCL Storage Tank (S-1103) to Glycerine Reactor (S-302).

13. Open Glycerine Reactor (S-302) bottom block valve.

14. Check oxygen content in Glycerine Reactor (S-302). If less than 1%, close Glycerine Reactor (S-

302) bottom block valve.

15. Stop all N2 purging to Glycerine Reactor (S-302).

16. Open N2 line to purge acidulated glycerine from Glycerine Reactor (S-302) to Glycerine

Evaporator Feed Tank (S-305).

17. Open Glycerine Evaporator Feed Tank (S-305) bottom block valve.

18. Open soap draw-out line block valves to soap stock surge tank.

19. Check oxygen content in Glycerine Evaporator Feed Tank (S-305). If less than 1%, close bottom

block valve on Glycerine Evaporator Feed Tank (S-305).

20. Close soap draw-out line block valves to soap stock surge tank.

21. Open N2 line to purge glycerine line from Glycerine Evaporator Feed Tank to Glycerine

Evaporator (V-306).

22. Open Glycerine Evaporator bottom block valve.

23. Open Glycerine Evaporator Condenser (E-305) block valve.

24. Check oxygen content in Glycerine Evaporator (V-306). If less than 1%, close Glycerine

Evaporator bottom block valve.


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25. Close Glycerine Evaporator Condenser (E-305) block valve.

26. Stop N2 purging to Glycerine Evaporator.

27. Open N2 line to purge Glycerine Evaporator bottom product line to glycerine analysis tank.

28. Close block valve of bottom product line to Glycerine Evaporator Reboiler (E-307).

29. Stop N2 purging when it's clear.

7.0 Attachment

7.1 Appendix A (System Purging)

7.0 Attachment

7.1 Appendix A (System Purging)


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Page : 39 of 38

No-Load Test on Ejector System

A. Line up valves on each ejector system to start no load test.

1. Close the vacuum vapor block valve separating the process stream and the ejector system.

2. Close the block valve on vacuum by pass line.

3. On TDC, set the Vacuum Pressure Controller on "Manual" and close the control valve completely.

4. Make sure the main steam supply valve on the main steam supply line to the ejector system is

closed.

5. Close the steam inlet valve to each ejector.

6. Make sure that the steam condensate valve on the condensate line (downstream of the steam

separator) is open.

7. Make sure water level in the Hot Well is enough.

B. Drain steam condensate from vacuum system.

1. Open bleeder valves on steam supply line to each ejector to drain out any steam condensate. Close

back the valve when draining is completed.

2. Open bleeder valves of each ejector steam chest to drain out any trapped condensate. Close back

the valves when draining is completed.

C. Start cooling water flow through the ejector condensers

1. Open the cooling water inlet valves to each ejector condensers to start water flow (if closed).

2. Make sure cooling water flow is established through the ejector condensers.

3. Check that high point vents are working.

D. Start steam supply to ejector system.

1. Open the main supply valve on the steam supply line to ejector system.

2. Slowly crack open the bleeder valves before the steam inlet to each ejector.

7.1 Appendix A (System Purging) (cont)

D. Start steam supply to ejector system. (cont)


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3. Close back the bleeder valves when steam is observed to come out of the bleeder. This will

confirm that the steam flow has been established, and also to bleed off any remaining condensate

in the steam line.

4. Open the steam inlet valves to the ejector system. Begin by opening the steam supply to the

second stage ejector and then to the first stage ejector.

E. Set the flow of the cooling water throughout the ejector condensers.

1. When steam flow through the ejector condensers has been established, throttle the cooling water

outlet valve of each of the condenser.

2. Check the temperature difference across each condenser. A temperature difference of 10-15oC is

an indication of good heat exchange.

3. Make adjustment to the throttled position of the outlet valve until the temperature difference (10-

15oC) is achieved.

F. Check the "No-Load Point" of the ejector system.

1. Check the ejector system pressure at the local pressure indicator is around 10 barg.

2. Place a pressure indicator at the pre-determined location of the ejector vacuum system and read the

ejector vacuum pressure.

3. Cross check the ejector system pressure by placing the pressure indicator at several pressure

indicator locations at the ejector system.

Note: This pressure is the "no-load pressure" of the ejector system.

4. Compare the pressure reading with the design specification of the system (or commissioning data).

This will give an indication of how the system performs versus the design specification.

G. Check the "Orifice-Point" of the ejector system.

1. Open the block valve at the restricted orifice (RO) to let air to be sucked into ejector system to be

established for few minutes.

2. Read the vacuum pressure at the local pressure indicator of the ejector system.

Note: This pressure is the "orifice-point pressure" of the ejector system.

3. Compare the pressure reading with the design specification of the system (or commissioning data).

This will give and indication of the condition of the ejector orifice (wear and tear).

system 300

Documents

crude glycerine

glycerine column t

hot glycerine

wet glycerine

sop fpg

dry glycerine tank v

dry glycerine preheater

scope system