WI3H02

EXTERNAL INTERNAL
(REFERENCE) EP2 / EP3
PREPARED BY :- ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE :- REVISION DATE : 15.07.04 REVISION NO. :3
REVISION :- EFFECTIVE DATE : 15.07.04 PAGE : 1 of 9
COPY NO. :

Production manual for

453550 i/MCT 60 X

Raw material/100kg Raw

material/11055kg
452593 60:40 Caprylic-Capric acid V (A) 122.10 kg 13500 ± 500 kg
or
452580 60 :40 Caprylic-Capric acid V
450485 Glycerol 19.9 kg 2200 ± 50 kg
453615 Activated Carbon 0.9 kg 100 kg

Chemical added during filteration

452771 Filter aid (A) 0.41 kg 45.3 kg
or
450346 Filter Aid

Chemical added for neutralisation (if needed)

450430 Sodium Hydroxide 50%

Sec. yield
453699 i/return C8/C10, MCT 60 21.6 kg 2388 kg

Inventory of 60 :40 Caprylic-Capric acid V in receiver for auto reflux 900 kg

1.0 REACTION

1.1 If a mixture of i/return C8 / C10, MCT 60 and fresh 60 :40 Caprylic-Capric acid V is
used, the acid value (AV) of the mixture should be checked and the amount of
glycerol required should be re-calculated as below :

Glycerol (kg) = AV X 2200

*
 WI3H02

EXTERNAL INTERNAL
(REFERENCE) EP2 / EP3
PREPARED BY :- ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE :- REVISION DATE : 15.07.04 REVISION NO. :3
REVISION :- EFFECTIVE DATE : 15.07.04 PAGE : 1 of 9
COPY NO. :

Note : * AV of fresh 60:40 Caprylic Capric Acid V (A) from QC Analysis result
 WI3H02

EXTERNAL INTERNAL
(REFERENCE)
PREPARED BY :- ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE :- REVISION DATE : 15.07.04 REVISION NO. :3
REVISION :- EFFECTIVE DATE : 15.07.04 PAGE : 2 of 9
COPY NO. :

1.2 Raw materials are charged into the reactor. The reactor is heated rapidly to 225 oC
±10oC through top and bottom coils and circulated through the product heater.

1.3 Reactor is maintained under slight nitrogen blanketing to 0.0 barg.

1.4 When temperature reaches 160 oC ± 10oC, vacuum is pulled through the first stage
until 900 ± 50 mbar. The top column temperature is set to ‘MAN’ mode and valve is
100% opened to receiver for auto reflux.

1.5 Heating is maintained until reactor temperature reaches 225 oC ±10oC.

1.6 Vacuum is increased gradually until 300 mbar to drive the reaction to completion.
Auto reflux should be in operation.

1.7 When temperature is about 225°C, sample is taken to check for the acid value.

1.8 When the acid value is stagnant or the drop in acid value is slowing down, the
reaction water in receiver is drained out. The auto reflux material is collected and
used for the next batch. Sufficient amount of return C8/C10 is left in the receiver for
the next batch.

1.9 Stripping is started by applying full vacuum to the reactor with 30 – 40 Nm3/h of
Nitrogen sparging to strip off the excess reactant. Short path is opened. Reactor
temperature is maintained at 220 oC ± 10oC .

1.10 After about 4 – 6 hrs of stripping and the Acid Value (AV) is below 1, product is
cooled under full vacuum. When product temperature after cooler is 130 oC ± 10oC
pressure is equalised with N2 to 0.0 bar. Product is then transferred to bleacher. In
bleacher product is then further cooled down to 100 oC before filtration.
 WI3H02

EXTERNAL INTERNAL
(REFERENCE)
PREPARED BY :- ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE :- REVISION DATE : 06.08.03 REVISION NO. :2
REVISION :- EFFECTIVE DATE : 06.08.03 PAGE : 4 of 9
COPY NO. :

2.0 FILTRATION PROCEDURE

2.1 Filter aid is added in bleacher and product is recycled through Niagara Filter back to
bleacher until most of the carbon has been trapped in the filter.

2.2 Product is then transferred to Tank 34 before feeding to the Deglycerination plant for
deodorisation process.

3.0 Neutralisation (Alkaline washing) Procedure

(Procedure is applied if the acid value hangs or does not drop even after deodorisation)

3.1 Final AV in the bleacher is checked.

3.2 The amount of Sodium Hydroxide 50% solution (NaOH) for neutralisation is
calculated as follows :-

m NaOH,50% (kg) = AV x Product Qty. (kg) x 2.2

1402.5

3.3 For direct neutralisation, the calculated amount of NaOH, 50% is added directly into
bleacher through the pot. For alkaline washing, the calculated amount of NaOH, 50%
is dissolved in 1 mt. of water. The NaOH solution is then sprayed to the top of
bleacher with agitator running at low speed for 1/2 hour.

3.4 After 1/2 hour, the agitator is stopped. Product is let to settle for 1 hour. After 1 hour,
the water phase and soap layer is decanted out from bottom of bleacher and pumped
to sump pit. Sample is taken to check for AV. If AV is > 0.05, the alkaline
washing is repeated or else drying is continued.

3.5 If the AV is < 0.05, product is dried by heating to 110 oC ± 10oC under full vacuum
for about 1 hour. After 1 hour, R104-12 is purged with nitrogen to 0.0 barg and
cooled down to 70oC± 10oC . Sample is taken to check for the AV.

3.6 Product is then transferred to the nominated intermediate tank. Sample is taken for
full analysis.
 WI3H02

EXTERNAL INTERNAL
(REFERENCE)
PREPARED BY :- ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE :- REVISION DATE : 06.08.03 REVISION NO. :1
REVISION :- EFFECTIVE DATE : 06.08.03 PAGE : 5 of 9
COPY NO. :

4.0 STRIPPING/DEODORIZATION

4.1 From the intermediate tank (T34) product is fed to the deglycerination column to
remove the excess fatty acid. The parameter for the column are set as below : -

Description Set point Unit

0
Preheater E302 set temperature 180 -200 C
(TC31201)

0
E303 condensor temperature 40 ± 10 C
(TC31305)

Feed column 1.0 - 2.5 m3/hr

Dry steam to column (steam supply) 50 - 80 kg/hr

4.2 The product from receiver V303 is recycled back to column. Sample is sent to check
for acid valve (AV). If AV ≤ 0.05, product is diverted to an intermediate tank.
 WI3H02

EXTERNAL INTERNAL
(REFERENCE)
PREPARED BY :- ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE :- REVISION DATE : 06.08.03 REVISION NO. :1
REVISION :- EFFECTIVE DATE : 06.08.03 PAGE : 6 of 9
COPY NO. :

PRODUCTION DESCRIPTION FOR FINISHING PLANT

Product name Process name

Refer table below ESTER PLANT DRUMMING STATION

Item number Product characteristic Packaging Unit

Refer table below LIQUID DRUM 190 KG

Product no. Intermediate product Product no. End product

453550 i/MCT 60 X 453495 MCT 60 X
453550 i/MCT 60 X 455833 MCT 60 X-CO

Drumming Procedure

1. If the product conform to the specifications, the intermediate product in the intermediate tank
is transferred into the Ester Plant drumming / loading tank.

2. Product from this tank is circulated through GAF filter (using 1 micron filter bag - double
length) and 0.2 micron cartridge filters before going to the drumming machine. Sample is
taken to check for the AV, moisture and filtration. If all the analysis are within the
specification, product is drummed otherwise, Site Manager / Process Controller is informed
for the next course of action.

3. Before drumming, the empty drum is vacuumed and checked externally and internally for the
cleanliness and any contaminant. Rejected drums should be separated and not to be used.

4. After complete drumming, samples are sent to QC for analysis.

 WI3H02

EXTERNAL INTERNAL
(REFERENCE)
PREPARED BY : - ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE : - REVISION DATE : 06.08.03 REVISION NO. :1
REVISION : - EFFECTIVE DATE : 06.08.03 PAGE : 7 of 9
COPY NO. :

PRODUCT DESCRIPTION FOR FINISHING PLANT

Product name Process name

MCT 60 XA/D ESTER PLANT DRUMMING STATION

Item number Product characteristic Packaging Unit

454931 LIQUID DRUM 190 KG

Intermediate product : Quantity (kg)

453550 i/MCT 60 X 100

454902 Mixed Natural Tocopherol 0.003

Drumming Procedure

1. If the product conform to the specifications, the intermediate product in the intermediate tank
is transferred into the Ester Plant drumming / loading tank .

2. Product from this tank is circulated through GAF filter (using 1 micron filter bag - double
length) and 0.2 micron cartridge filters before going to the drumming machine. Sample is
taken to check for the AV, moisture and filtration. If all the analysis are within the
specification, product is drummed otherwise, Site Manager / Process Controller is informed
for the next course of action.

3. Before drumming, the empty drum is vacuumed and checked externally and internally for the
cleanliness and contaminant. Rejected drums should be separated and not to be used.
 WI3H02

EXTERNAL INTERNAL
(REFERENCE)
PREPARED BY : - ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE : - REVISION DATE : 06.08.03 REVISION NO. :1
REVISION : - EFFECTIVE DATE : 06.08.03 PAGE : 8 of 9
COPY NO. :

4. After drumming, sample are sent to QC for analysis.

 WI3H02

EXTERNAL INTERNAL
(REFERENCE)
PREPARED BY : - ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE : - REVISION DATE : 06.08.03 REVISION NO. :1
REVISION : - EFFECTIVE DATE : 06.08.03 PAGE : 9 of 9
COPY NO. :

PRODUCTION DESCRIPTION FOR FINISHING PLANT

Product name Process name

MCT 60 X/J ESTER PLANT DRUMMING STATION

Item number Product characteristic Packaging Unit

433518 LIQUID 20L T/H Steel Blue Drum 18 KG

Intermediate product :

453550 i/MCT 60 X

Drumming Procedure

1. If the product conform to the specifications, the intermediate product in the intermediate tank
is transferred into the Ester Plant drumming / loading tank .

2. Product from this tank is circulated through GAF filter (using 1 micron filter bag - double
length) and 0.2 micron cartridge filters before going to the drumming machine. Sample is
taken to check for the AV, moisture and filtration. If all the analysis are within the
specification, product is drummed otherwise, Site Manager / Process Controller is informed
for the next course of action.

3. Before drumming, the empty drum is vacuumed and checked externally and internally for the
cleanliness and contaminant. Rejected drums should be separated and not to be used.

4. After drumming, sample are sent to QC for analysis

 WI3H02

EXTERNAL INTERNAL
(REFERENCE)
PREPARED BY : - ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE : - REVISION DATE : 06.08.03 REVISION NO. :1
REVISION : - EFFECTIVE DATE : 06.08.03 PAGE : 10 of 9
COPY NO. :

PRODUCT DESCRIPTION FOR FINISHING PLANT

Product name Process name

MCT 60 X/C ESTER PLANT DRUMMING STATION

Item number Product characteristic Packaging Unit

455529 LIQUID 1000L IBC-EX Steel Pallet 950 KG

Intermediate product :

453550 i/MCT 60 X

Drumming Procedure

1. If the product conform to the specifications, the intermediate product in the intermediate tank
is transferred into the Ester Plant drumming / loading tank .

2. Product from this tank is circulated through GAF filter (using 1 micron filter bag - double
length) and 0.2 micron cartridge filters before going to the drumming machine. Sample is
taken to check for the AV, moisture and filtration. If all the analysis are within the
specification, product is drummed otherwise, Site Manager / Process Controller is informed
for the next course of action.

3. Before drumming, the empty drum is vacuumed and checked externally and internally for the
cleanliness and contaminant. Rejected drums should be separated and not to be used.

4. After drumming, sample are sent to QC for analysis

 WI3H02

EXTERNAL INTERNAL
(REFERENCE)
PREPARED BY : - ISSUE DATE : 28.08.02 ISSUE NO. :3
DATE : - REVISION DATE : 06.08.03 REVISION NO. :1
REVISION : - EFFECTIVE DATE : 06.08.03 PAGE : 11 of 9
COPY NO. :

PRODUCT DESCRIPTION FOR FINISHING PLANT

Product name Process name

Refer table below ESTER PLANT DRUMMING STATION

Item number Product characteristic Packaging Unit

Refer table below LIQUID ISOTANKER ~ 20000 KG

Product no. Intermediate product Product no. End product

453550 i/MCT 60 X 453505 MCT 60 X/T
453550 i/MCT 60 X 455846 MCT 60 X/T-CO

Loading Procedure

1. If the product conform to the specifications, the intermediate product in the intermediate tank
is transferred into the Ester Plant drumming / loading tank .

2. Product from this tank is circulated through GAF filter (using 1 micron filter bag - double
length) and 0.2 micron cartridge filters. Sample is taken to check for the AV, moisture and
filtration. If all the analysis are within the specification, loading is started otherwise, Site
Manager / Process Controller is informed for the next course of action.

3. After loading, samples are sent to QC for analysis.

Refer to WI3P106 - Work Instruction for Loading into Roadtanker and Isotanker.