reactor ph optimization - validation report

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FPG Oleochemical Category: FPG – Utility Plant Subcategory: Glycerin Acidulation pH Optimization- Validation Report Originator: Faudzi Abd Rahman Date Approved: 15/2/2008 Owning Area: Refined Glycerin Technical Standard #: U001/08 OBJECTIVE: The objective of this Experimental Order is to increase Dowtherm Header Process Control Strategy . This will also reduce the amount of salt generation in crude glycerin. This is a concurrence type validation. CONCLUSION: From the EO, it is concluded that the acidulation pH can be increased up to 3 in order to produce refined glycerin that is able to meet the specification as per GCAS #95897935. At acidulation pH higher than 3, there is possibility that Fatty Acid & Ester in refined glycerin is not able to meet the specification of 0.3% Max. FINDINGS & OBSERVATIONS: Based on the observation during the whole period of EO from July 23 2007 until December 6 2007, few observations were made as below: At acidulation pH of 3 there is reduction in HCL index and NaOH consumption. At the same time NaCl content in crude Glycerin reduce to around 2.8%. No issue observed on crude glycerin and refined glycerin quality. At acidulation pH of 3.5 and 4.0, there is quality issue on high Fatty Acid & Ester carry over in RG distillate at Glycerin Still. FA&E content was higher than the maximum limit of 0.35. Quality summary of Glycerin Still distillate when acidulation pH at 3.5 and 4.0 as per attachment:

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Reactor PH Optimization - Validation Report

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Page 1: Reactor PH Optimization - Validation Report

FPG Oleochemicals

Category:FPG – Utility Plant

Subcategory:Glycerin Acidulation pH Optimization-Validation Report

Originator:Faudzi Abd Rahman

Date Approved:

15/2/2008

Owning Area:Refined Glycerin

Technical Standard #:U001/08

OBJECTIVE:

The objective of this Experimental Order is to increase Dowtherm Header Process Control Strategy . This will also reduce the amount of salt generation in crude glycerin. This is a concurrence type validation.

CONCLUSION:

From the EO, it is concluded that the acidulation pH can be increased up to 3 in order to produce refined glycerin that is able to meet the specification as per GCAS #95897935. At acidulation pH higher than 3, there is possibility that Fatty Acid & Ester in refined glycerin is not able to meet the specification of 0.3% Max.

FINDINGS & OBSERVATIONS:

Based on the observation during the whole period of EO from July 23 2007 until December 6 2007, few observations were made as below:

At acidulation pH of 3 there is reduction in HCL index and NaOH consumption. At the same time NaCl content in crude Glycerin reduce to around 2.8%. No issue observed on crude glycerin and refined glycerin quality.

At acidulation pH of 3.5 and 4.0, there is quality issue on high Fatty Acid & Ester carry over in RG distillate at Glycerin Still. FA&E content was higher than the maximum limit of 0.35. Quality summary of Glycerin Still distillate when acidulation pH at 3.5 and 4.0 as per attachment:

Therefore the acidulation pH can only be increased up to 3. The crude glycerin and refined glycerin quality summary during the EO period is attached below:

RECOMMENDATION:

Page 2: Reactor PH Optimization - Validation Report

Therefore it is recommended that that acidulation pH to be controlled between 0.5 and 3.0.Other operating parameters for Crude Glycerin recovery system is as per table 1.

Table 1

Location Critical Parameters Range Target

Glycerin Reactor Acidulation Feed Temperature

80 max < 80

pH into reactor 0.5 – 3.0 2.5Acidulation Interface

Level40-80 75

pH of Neutralized Glycerin

5.0 – 7.0 5.3

Glycerin Evaporation

Feed Tank Level 110 - 410 405

Evaporator Pot Level 40 - 60 50Evaporator Pressure 70 70

Pot Temperature 98 - 103 100Crude Glycerin pH 5 - 7 6

Glycerin Hotwell Hotwell pH 6 - 10 7Hotwell level 40 - 60 50

ATTACHMENT:

SIGNATURES:

By signing below, we indicate that the Validation Report is sufficient to revise the Process Control Strategy (Glycerin / Utilities) FPG-II-022.

Page 3: Reactor PH Optimization - Validation Report

Role Name Signature Date

OriginatorMohd Faudzi Abd Rahman

Mohd Faudzi Abd Rahman

14/1/2008

Validation System Owner

Mohd Fairuz Azli B Sulong

10/2/2008

Operation Manager

Azahari Bin Din 13/2/2008

QA ManagerHasni B Hj

Ahmad15/2/2008