Project Nebula

BASIC ENGINEERING

CONCEPT NOTES FOR

APG

Document Number
P90-AP98-01-001

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1.0 INTRODUCTION
Introduction:

Galsoft APG, a natural non - ionic surfactant synthesis can be completed with natural and
renewable sources and the compounds are biodegradable , is used in kitchen detergent, body
washing products, cosmetics, plastic and petroleum industry , textile, printing and dyeing, paper
making and other industrial / commercial uses.
• Cosmetics and Toiletries: Hair shampoo, Hair Cleansing, Body Wash, Body Scrub, Shower
Gel, Hand Cleansing, Foundation, Anti-ageing, Beauty Care, Baby Care, etc.

• Face Wash: Face washing foam, Face washing cream, Face washing liquid, Make-up
remover, etc.

• Soap and Other: Facial soap, Liquid Soap, Facial Cleanser, Skin Cleansing, Toothpaste, Bath
soap, Emulsifiers and Dispersing agents, etc.

Aim:

To create the facility to manufacture 600 TPA of Galsoft APG as a product under Project Nebula
at G-59 site in Tarapur.

Background:

• The Pilot batch is conducted at W-67 with a batch size of 90 kg and a batch cycle of 64
hours.

Process

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SOP of Process

1. Clean and wash the reactor by steam and dry the reactor.
2. Ensure the reactor is clean by visual testing
3. Apply Steam Jet Ejector vacuum and ensure vacuum in the reactor should be around 10
mm Hg
4. Charge the lauryl alcohol (107 kg) using vacuum
5. Start pump circulation and heat the mass to 40-50°C at 5-7 mm Hg to remove moisture.
6. Break the lumps of dextrose and charge dextrose slowly as free flowing powder (33 kg)
from manhole. Ensure circulation is ON.
7. Stir the reaction mass for ½ h at 50-60°C and at 5-7 mm Hg vacuum to remove the moisture
from the reaction mass
8. Check moisture content of reaction mass. It should be less than 0.1%.
9. After ensuring moisture content is within specifications, charge APG catalyst (151 g) at 60°C
under vacuum from top nozzle and increase the temperature up to 110°C - 112°C under 2-3
mm Hg vacuum.
10. Maintain temperature of reaction mass at 110°C-112oC for 6-6.5 h under 2-3 MM Hg
vacuum.
11. Conduct bottom top mixing 2 times after each 15 min and later after 1h, 2h & 3h to avoid
settling of catalyst & dextrose.
12. After 5-5.5 h, check the conversion of Dextrose by DNSA method as explained below
13. After passing smear test (after 6-6.5h), check % glucose in the reaction mass by DNS
method.
14. After concluding that glucose content is within the lower limit, cool the reaction mass to
around 70°C & add 40 g of caustic lye (48%)
15. Continue the mixing for total ½ h and check pH in 10% IPA: Water 60:40 solution. It should
be around 7-7.5.
16. Increase temperature of reaction mass to 120°C. Parallely, make jacketed cartridge filter
(10 μm) ready by heating it to 120-125°C using steam.
17. Cut off the circulation line and open by pass line to start filtration using nitrogen pressure
to the reactor.
18. Drain the circulation line material and add it to the reactor
19. Initially use lower nitrogen pressure of around 0.5 kg/cm2 for pressure filtration. When rate
of filtration slows down, increase the N2 pressure in the reactor in steps of 0.5 kg/cm2 up to
3kg/cm2.
20. As rate of filtration slows down even at 3kg/cm2, open the filter, clean and wash it and
restart filtration.
21. Collect the filtrate in top open 200kg HDPE drum
22. After completing filtration, drain material in line and wash reactor & cartridge filter.
23. After filtration of entire material, through peristaltic pump it is sent to SPDU Unit. SPDU
unit has steam jacketed body.
24. LA get condensed in internal condenser of SPDU, uncondensed will go to external LA
condenser.
25.Condensed will be collected in a receiver and sent back for next batch.

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26. MAAG pump for continuous displacement of bottoms from Vacuum to atmospheric
pressure.
27. Steam jacketed lines for downstream flow of molten APG at residue side.
28. Set up for continuous dilution of the material received from bottom (displaced by MAAG
pump).
29. At pilot scale dilution is a batch process, where measured amount of water is already kept
at 50-60 degree and continuous addition of APG through MAAG takes place.
29. Steam Pressure in the jacket of MAAG pump to be above 6-6.5 kg/cm2 to avoid choking
of APG inside the pump
30. For Bleaching, Adjust the pH of the mass to 10.0-10.5 using 48% caustic lye and then
increase the temperature gradually to 60-65⁰C.
31. Now, add required quantity of peroxide in 5 parts over a period of 2-3 hours.
(Note: Don’t add peroxide in one time).
32. Check pH of mass at 10 minutes regular interval (or continuously with online pH meter)
and maintain it to 10.0-10.5 during bleaching process.
33. Check free peroxide after 4-5 hours of bleaching process and if it is nil then add further
200-500 ppm peroxide.
34. Continue the reaction till there is no drop in peroxide observed (color of < 0.5 Gardner is
the internal specification (at pH=3-4) and < 2.5 Gardner at 11 pH).
35. Finally, allow the mass to cool to room temperature and then adjust and maintain the pH
in range of 11.5-12.0 using required quantity of 48% caustic lye for additional 4-5 hours (for
killing residual peroxide).
36. Kill the free peroxide carefully with the stoichiometric quantity of Sodium sulfite.
37. Adjust the final mass as per specification and then analyze it for free fatty alcohol, viscosity,
degree of polymerization etc.
38. Add 200 ppm sodium sulfite as a stabilizer in reaction mass.
39. Take the final adjusted mass for packing in HDPE drums of 200 Liter.

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Reaction Involved:
• Reaction will be carried out in at 115 degrees and in the presence of APG catalyst.

Raw material and Finished goods:

• Dextrose Anhydrous
• Lauryl Alcohol
• Myristyl Alcohol
• Capric Alcohol
• Capryl Alcohol
• Sodium Sulphite
• Magnesium Oxide
• Hydrogen Peroxide-50%
• Sodium Hydroxide
• Catalyst APG
• Product APG

Handling and Specifications of RM and FG:

1. Lauryl Myristal Alcohol

a. Lauryl Alcohol is procured in XX kg YYYY Drums/ISO.- This is mentioned separately
below in table.
b. The registered suppliers for Lauryl Alcohol to Galaxy are XX and YY and domestic
supply from VVF- This is mentioned separately below in table.
c. The specification for Lauryl Alcohol are;

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2. Dextrose Anhydrous
a. Procurement of Dextrose Anhydrous is put in separate table. And is to be stored at
25 to 35 ⁰C.
b. To be kept at dry place because it is susceptible to moisture
c. The specification for Dextrose Anhydrous are;

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3. Catalyst APG
a. Store the container tightly closed in a dry and well-ventilated place.
b. Packing MOC is PPFRP and Glass Lined.

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4. Caustic Lye (48% solution)
a. Keep container tightly closed. Keep container in a cool, well-ventilated area.
b. Suitable MOC for Caustic lye solution is SS304/PPFRP.
c. The registered suppliers for Caustic Lye to Galaxy are Gujrat Alkalies Chemicals
Ltd. and Ideal Chemicals Pvt. Ltd.

5. Hydrogen Peroxide (50% solution)

a. Hydrogen Peroxide (50% solution) is stored in narrow mouth 50 Kg carboys.

1. Magnesium Oxide (50% solution)

a. Magnesium Oxide is stored in narrow mouth XX bags.

1. Sodium Sulfite

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a. Sodium Sulphite is stored in narrow mouth25 Kg HDPE bags.

Sourcing and Packing Details;

Material Vendors Mfg. site of Packaging Packaging MOC
Vendor Type
Anhydrous Dextrose Universal Starch Karnataka 25kg HDPE HDPE
Chem Bags
Lauryl Alcohol Many Southeast Asia Flexi HDPE

Magnesium Oxide

Sodium GACL Gujarat Tankers SS

Hydroxide/Caustic DCM Shrirama Gujarat
Soda Lye Meghmani Gujarat
Reliance Gujarat
Sodium Sulphite Aditya Birla Thailand 25kg HDPE HDPE
Bags

Hydrogen Peroxide GACL Gujarat 50 L Carbouys HDPE

National Peroxide Kalyan, MH
Limited

HCL AARSHA Taloja, MH HDPE Drums HDPE

• Q and S Components

• Q components;

A. Reaction Step;
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1. Moisture recovery- Before reaction it is required to remove the moisture otherwise
it will form polydextrose.
2. Temperature of the reaction should be kept in between 112 to 115 ⁰C. The
reaction will take more time below 112 Degree C (Due to reduced rate of reaction).
And above it will change the degree of polymerization.
2. Vacuum to be kept below 0.5 torr during the reaction, otherwise the rate of
recovery of water will be more which will cause higher BCT.
3. Quality of Dextrose- Should as per specs may hamper overall reaction, such BCT
and colour bodies formation.
4. Quality of LA (C12-14 composition)- composition should be as per our
specifications otherwise product may have different properties such as viscosity and
foaming property and DP.
5. Mixing of Dextrose and LA should be efficient as it is a heterogeneous reaction.
Otherwise the BCT will get increase.
6. Catalyst effect- More catalyst forms more side reactions and lower lading of
catalyst increase BCT also impact on DP of product.

B. Filtration Step;
1. Temperature of Filtration- Filtration to be carried out at 120 degree, below that
temperature it will have an impact on degree of polymerization. Ultimately it will
change the final characteristic of Product (i.e. Product Viscosity and Degree of
polymerization).

C. Separation Step- LA and RX-APG

1. Inlet feed temperature of SPDU- Feed temperature of reaction mass should be
150 degree otherwise it will have an impact on working parameters of SPDU.
Ultimately the separation will be impacted.
2. In SPDU- 155 degree to be maintained, higher temperature will increase the color
of the material and lower will effect on separation.
3. Feeding rate of reaction mass to SPDU- The SPDU is designed for 100 kg/hr,
any change in feeding rate will effect on its working parameter.
4. Maag Pump inlet and outlet lines to be properly Steam jacketed otherwise APG
got choke in between (BP of APG =130 degree), will directly impact on SPDU
working which is in continuous mode.

D. Dilution Step;
1. Temperature in Dilution- Dilution to be carried out at 60 degrees else the mixing
of INP-APG and water will take more time.
2. Dilution to be carried out at low RPM- Higher RPM contributes to foaming.
(Experiments have been conducted at 10 RPM, similarly some value to be set at
commercial scale.

E. Bleaching Step;
1.

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• S Components;

1. Hydrogen Peroxide-
• Storage - Avoid contamination - Contamination could cause decomposition and
generation of oxygen which may result in high pressure and possible container rupture.
• Empty drums should be triple rinsed with water before discarding.
• Isolate post spill area. Keep people away from and upwind of spill/leak. Eliminate all
sources of ignition and remove combustible materials.

• Handling – Avoid contact with skin, eyes and clothing. Wear personal protective
equipment (Safety Goggle, Safety shoes, Mask, Gloves and safety helmet).

2. Sodium Sulphite-
• Handling – Avoid contact with skin, eyes and clothing. Wear personal protective
equipment (Safety Goggle, Safety shoes, Gloves and safety helmet).
3. Magnesium Oxide-
• Handling - Wash hands thoroughly after handling. Minimize dust generation and
accumulation. Avoid contact with eyes, skin, and clothing. Use with adequate
ventilation. Avoid breathing dust and fume.
• Wear personal protective equipment (Safety Goggle, Safety shoes, Mask, Gloves
and safety helmet).
4. Caustic Lye-
• Handling – Use Gloves, Mask, Goggle, Helmet and shoes. Face-shield, Corrosion-proof
suit.

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2.0 PHILOSOPHY
Process:

• Common Assembly till SPDU;

1. There will be 1 Reactor of 5 KL for reaction and 1 vessel of 5 KL for holdup.
2. Reactor have a limpet with steam and cooling water as a utility.
3. One Spiral Condenser unit will be there along with receiver for water recovery.
4. Oil Ring vacuum pump with booster followed by water ring vacuum pump will be there
for applying vacuum <0.5mmHG during the reaction.
5. APG Catalyst will be charged by double valve system with catalyst charging unit.
6. Dextrose will be charged manually/Solid charging system with silo arrangement (To be
discussed with sourcing team whether we will get Dextrose in Jumbo or not and will be
finalized later based on area available).
7. A lump breaker to be installed to break lumps of dextrose after solid charging system.
8. NaOH will be charged as same as catalyst charging unit.
9. Centrifugal Pump will be used for transferring the material from Reactor to SPDU feed
vessel.
10. Cartridge filter with provision of steam Jacketing to be put for removing the unreacted
dextrose from the reaction mass.
11. The entire line will be heat traced and insulated along with pump.
12. Hold up vessel has also provided with agitator for gentle rotation inside the vessel.
13. The capacity of holdup vessel is kept for 1 batch only, as its color gets degraded when
kept at high temperature for too long (more than 24 hrs).
14. A circulation Heat exchanger is provided to cool down the reaction mass from 120 to
60 degrees.
15. Metering pump will be kept after Hold-up vessel to feed precisely into the SPDU.
16. A preheater (Shell and Tube type) is there to preheat the material from 60 to 150 to
feed into the SPDU.
17. SPDU will have one condensing unit for LA and its two receivers. The residue i.e. APG
will go directly for dilution through Gear pump (Maag Pump).
18. Utility needed for condenser is cooling water. The collected LA of a batch will be kept
in the receiver and will be used in next consecutive batch.
19. LA receiver is designed in such a way to hold LA of two batches.
20. The entire line from SPDU feed to MAAG pump inlet of residue is steam jacketed with
insulation. Steam at pressure of 6 to 6.5 kg will be kept in the jacket to keep the APG
in molten state.
21. MAAG pump will have a seal pot with glycerin inside in it kept at pressure of 3-4 kg/cm2.
22. SPDU will be a continuous operation.
23. For the operations ahead we have evaluated few options below and based on
discussion selected one from them.

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• Feasible Options Evaluated

• Option 1 – With Two Dilution vessel

1. MAAG Pump outlet will directly go to a dilution vessel with high shear mixer arrangement.
2. There will be two vessel kept for dilution of equal capacity, one is used for first 24 hours
and other will be used for next day 24 hrs.
3. The amount of material coming out of SPDU in a Day- 40 kg/hr feed rate means in a day
960 kg of water at 80-90 C is kept in Vessel.
4. First vessel material will be sent to Bleaching vessel. Gear pump after dilution to bleaching.
5. Once the first vessel has run for 24 hrs, the SPDU feed will be shifted to 2 nd vessel using
three way valve. And there the process of dilution started .
6. MgO, NaOH and sodium Sulphite will be charged from manhole directly into the bleachng
vessel while H2O2 will be charged using Diaphragm pump directly through carbouys.
7. As there is heavy foam generates during the reaction, foam breaker type agitator to be
installed.
8. The final stabilized process in sent to Storage tank in Tankfarm for ageing.

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Advantages;
1. Very simple option in all, which will ease the operations.
2. In any case the APG does not mix properly with water due to spec change or any
abnormality, this option provides us the flexibility of time of digestion.
Disadvatages;
1. More number of bays are occupying in this option as compared to 2nd and 3rd option.
2. More equipment leads to more piping leads to high initial investment.
3. Inlet pipelines leads to more bends, high chances of dead zones could form, which can
cause solidification of material in longer duration.
4. More residence time at higher temperature leads to color variation.

Option-2- A shear mixer in place of dilution vessel with two Bleaching vessel.

1. MAAG Pump outlet will directly go to an inline High shear mixer with two feed stream
lines, one is hot water (80-90 C) and one is Inp- APG.
2. Inline shear mixer will also be jacketed and insulated.
3. There will be two vessel kept for bleaching of equal capacity, one is used for 24 hours
and other will be used for next day.
4. The amount of material coming out of SPDU in a Day- 40 kg/hr feed rate means 40
kg/hr feed rate of water is to be provided using a flowmeter.
5. MgO, NaOH and sodium Sulphite will be charged from manhole directly into the
bleachng vessel while H2O2 will be charged using Diaphragm pump directly through
carbouys.
6. As there is heavy foam generates during the dilution and bleaching, foam breaker type
agitator to be installed in bleaching vessel.
7. The final stabilized process in sent to Storage tank in Tankfarm for ageing.

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Advantages;
1. This option will require 1 bay lesser than option 1.
2. Scaleup will be easier.
Disadvantages
1. There will not be any flexibility of mixing of material if in any case the mixing will not be
proper due to spec change in SPDU.
2. This option needs proper jacketing of shear mixer as well, else solidification of product may
happen. Also Flooding of SPDU can happen.
3. Check the pressure zones- cavity formation- foam generation- check with vendor.
4. Initial investment of this option will be high as compared to 1 and 3.
5. Operational control is more in comparison to both the options.

Option-3- A dilution vessel with a Bleaching vessel.

1. MAAG Pump outlet will directly go to a dilution vessel with high shear mixer
arrangement.
2. Dilution vessel is of bigger size which can accommodate 40 hrs of batch inside it. Once
the 24hrs batch is done. The material upto 60% level will be transferred to bleaching
vessel.
3. The amount of material coming out of SPDU in a Day- 40 kg/hr feed rate means 40
kg/hr feed rate of water is to be provided using a flowmeter.

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4. Dilution vessel material will be sent to Bleaching vessel using Screw/rotary vane/Gear
pump after dilution to bleaching.
5. MgO, NaOH and sodium Sulphite will be charged from manhole directly into the
bleachng vessel while H2O2 will be charged using Diaphragm pump directly through
carbouys.
6. As there is heavy foam generates during the reaction, foam breaker type agitator to be
installed.
7. The final stabilized process in sent to Storage tank in Tankfarm for ageing.

Advantages
1. There will be only 1 dilution vessel, so saving 1 bay in comparison to option 1.
2. Less initial investment compare to all options.
Disadvantages
1. Mixing of entire mass should be uniform otherwise, solids will be stuck in the strainer of
pump from dilution to bleaching.
2. If due to any specification variation occurs during SPDU which is causing bleach to take
more time. This time flexibility is not there in dilution step due to only 1 dilution vessel. Else
we have to stop the SPDU.

Option 4- Slow stirring dilution vessel with continuous system and Bleaching will be at high
temperature.

1. MAAG Pump outlet will directly go to a dilution vessel with low RPM mixer arrangement.
2. Dilution vessel is of bigger size which can accommodate 40 hrs of batch inside it. Once
the 24hrs batch is done. The material upto 60% level will be transferred to bleaching
vessel.
3. The amount of material coming out of SPDU in a Day- 40 kg/hr feed rate means 40
kg/hr feed rate of water is to be provided using a flowmeter.
4. But rather doing the same we will reduce the flowrate of water by 4 kg’s and mix 36

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5. kg/hr of water with 40 kg/hr of APG.
6. Due to this type of system, there will be a buffer time of 1 hr in which if APG do not get
mix then also the concentration will not go below 50%.
7. Whatever value of concentration above 50% will be adjusted in bleaching phase.
8. There will be 1 more vessel of 200 litres with the provision of strainer will be kept in
between dilution and bleaching vessel to remove the lumps of any solid APG if it comes.
This will allow only clear liquid to go into the bleaching vessel.
9. The entire mass will be sent through Nitrogen.
10. In bleaching vessel, all the additions will be done and the batch will be completed in 24
hrs. at 50-60 degree temperature and additional 2 hrs will be required for foam settling
at 90 degree.
11. In bleaching, MgO, NaOH and Sodium Sulphite will be charged from manhole directly
into the bleaching vessel while H2O2 will be charged using Diaphragm pump directly
through carbouys.
12. The entire mass will be sent to storage vessel, packing will be done from storage vessel
kept in tank.
13. 8 hours (1 shift) will be required for packing.

Advantages
1. System will be easier in operation and easier in understanding.
2. Less initial investment.

Disadvantages
1.

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Option 5- Slow stirring in Dilution vessel with continuous system and 2 Bleaching vessel will be
at high temperature.

1. In this process the entire process of dilution is same as above till it is sent to bleaching
vessel.
2. The entire mass will be sent from Dilution vessel to bleaching vessel through Nitrogen.
3. In this option there will be two bleaching vessel, which enable us to keep the capacity
of bleaching for 48 hrs.
4. In this option the same vessel will be used for bleaching (means addition of MgO,
NaOH, H2O2 and sodium sulphite), Foam adjustment through heating and packing.
5. In bleaching vessel, all the additions will be done and the batch will be completed in 24
hrs at 50-60 degree temperature and additional 2 hrs will be required for foam settling
at 90 degree. And packing will be done in 8 hrs. So total 34 hrs of batch cycle.
Advantages
1. System will be easier in operation and easier in understanding.
2. Good buffer in bleaching process.
Disadvantages
1. Three bays will be engaged, so less space for future.

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Conclusion; To be discussed and decided.

Process Parameters
Process - Steps Intermediate Data Value
Name
1. Reaction RxAPG Density
RxAPG Viscosity @
a. Operational Operational temperature( at 112 oC )
temperature = < 400 cP
b. RT RT = Solid
c. Min and Max
(Range)

RxAPG pH 6.5-7.5 ( after pH adjustment by

caustic lye), during reaction it yet to
be checked.
RxAPG N2 Pressure 3 kg/cm2 (This pressure is during
filtration of Rx-APG)
2. Distillation Ref-APG Density -
Ref-APG Viscosity @
a. Operational Sr. Temperature Viscosity
temperature
b. RT No. (°C) (cP)
c. Min and Max 1 170 450
(Range)
2 160 630
3 150 850
4 140 2550

Below 130 oC it became solid.

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Ref-APG pH 5-5.4
3. Dilution INP-APG Density 1.07-1.09 g/cm3( 25 oC)
INP-APG Viscosity @ At 25 oC
a. Operational Min = 1000 cP (Note: Considering
temperature C0810 APG)
b. RT Max=25000 cP (Note: Considering of
c. Min and Max Plantcare analysis giving you
(Range) maximum viscosity).
INP-APG pH 4.5-5 (10-10.5 after pH
adjust)
N2 Pressure -
4. Bleaching Final APG Density 1.07-1.09 g/cm3( 25 oC)
Viscosity @
a. Operational At 25 oC
temperature Min = 1000 cP
b. RT Max=25000 cP
c. Min and Max
(Range)
pH During bleaching( 10-10.5) after
bleaching ( 11.5-12.5)
Temperature Range 85-90 oC
Pressure Water vapour pressure at 90 oC
N2 Pressure Need clarification

Tanfarm Philosphy;

1. Lauryl Alcohol will be kept in a 35 KL tank in tank farm.

2. Tank has MOC of SS304 and half of the tank is heat traced.
3. There will be two centrifugal pumps 1 for loading and 1 for unloading.

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4. There will be a strainer in-between ISO tanker and unloading pump. And a bucket filter in-
between tank and transfer pump of X microns.
5. There will be a provision of heat tracing in unloading and loading lines for keeping the
temperature 35 C.

Packing

• Packing is done manually using flexible SS316L stiff hose

• Packing is done in 200 kg HDPE Drums.
• Before Packing, Empty Drums are cleaned by cotton and by vacuum (water ring) to ensure
absence of external matter.
• If received Drums are odor and dust free then use them directly otherwise rinse them
with the material.

Utility:

1. Steam is required for Reaction vessel, Preheater of SPDU, SPDU, Dilution and bleaching
vessel.
2. Cooling water will be required in water condenser, condenser of SPDU and LA condenser.
3. Oil ring with booster (0.1 torr) and Water ring vacuum pump (50 torr) will be required for
Reaction vessel and SPDU respectively.
4. Nitrogen is required for purging and blanketing.
5. Soft water is required for Dilution and bleaching.
6. Chilling water for vacuum trap.

Effluent;

1. These effluents needs to be treated in ETP, following are the values;

Total Suspended Solids mg/l

Total Dissolved
Solids mg/l
COD mg/l
BOD mg/l
Oil & Grease mg/l
Chloride mg/l
Sulphate mg/l
pH

Mechanical:

• Reactor 1- Reaction Vessel

a. MOC- SS316 construction, with baffles and SS304 external limpet provision.
b. Ends- Vertical, cylindrical with tori spherical top and bottom dish.
c. Design- Vacuum and 250 oC temperature

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d. Equipped with SS316, agitator with double mechanical seal
e. Inlet and circulation nozzles with dip pipe
f. The reactor will have nozzle provision as below;
• Nitrogen purging- Dip Pipe
• Nitrogen blanketing
• Vapor line
• Circulation nozzle
• Sight glass
• light glass
• Pressure safety valve
• Pressure/vacuum indicator
• Bottom outlet
• Lauryl Alcohol inlet
• Catalyst Charging vessel inlet
• RTD
• Manhole- Dextrose Inlet
• Agitator
• Limpet inlet- Steam in
• Limpet outlet- Steam outlet
• Spare nozzles as on need
• Holding Vessel
a. MOC- SS316 construction, with baffles and SS304 external limpet provision.
b. Ends- Vertical, cylindrical with tori spherical top and bottom dish.
c. Design- Vacuum and 250 oC temperature
d. Equipped with SS316, agitator with mechanical seal
e. Inlet and circulation nozzles with dip pipe
f. The reactor will have nozzle provision as below;
• Nitrogen purging
• Nitrogen blanketing
• Vapour line
• Circulation line
• Sight glass
• light glass
• Pressure safety valve
• Pressure/vacuum indicator
• Bottom outlet
• Lauryl Alcohol inlet
• Catalyst Charging vessel inlet
• RTD
• Manhole
• Agitator
• Limpet inlet- Steam in
• Limpet outlet- Condensate out

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• Spare nozzles- To be closed by looking at CP batches.
1. Agitator
• MOC- SS316
• The agitator must able to make uniform mixing of LA and Dextrose.
• The agitator type will be discussed and decided later and will have double back to
back mechanical seal.
• Seal pot will have Glycerin and will be kept pressurized by nitrogen 2-3 kg/cm2.
• The motor will be flameproof, Protection class- IP55 and Efficiency class –IE3.
2. Centrifugal pump
• MOC- SS316 construction, double mechanical seal
• This pump is used in circulation, filtration and transferring the reaction mass to
holding vessel
• Strainers will be place in suction of pump.
• The motor will be flameproof, Protection class- IP55 and Efficiency class –IE3.
3. Cartridge Filter
4. SPDU
5. Maag Pump
6. Dilution Vessel and agitator
7. Bleaching Vessel and agitator

8. Piping material;
• All Process pipelines will be in SS316 construction.
• All SS pipes will be in ERW construction and fittings will be seamless.
• All the utility (steam, Chilled water and cooling water) will be in MS.
• Pipes up to 2” will be of Sch 40, 3”-6” will be of Sch 10 and above will be of Sch 5.
• Valve, Nut bolt will be of same or superior make compared to pipes
• NRVs of pipe equivalent MOC will be installed at pump discharge to avoid reverse
flow
• Maintenance platform and space at all required position
• Lifting beam for ease of maintenance.

Civil:
• This will be covered in one single concept notes of entire plant.

Electrical:
• The system will be considered under flameproof area.
• The motors used will be of IE3 class for all the running equipment.
• It will have proper lighting arrangement for proper illumination in night.
• All running equipment’s will have local emergency start stop button with protection.
• All the equipment and structure will have double earthing.
• Further more details will be included in concept notes of electrical.

Instrumentation:

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• Mass flow meters to be provided in the line of Lauryl Alcohol coming from Tank farm.
• Level Transmitter will be provided to the Reactor, LA Receiver, Dilution vessel, Bleaching
Vessel.
• Level switch to be provided to LA Receiver.
• Pressure gauges will be provided at Reactor, Receivers, Dilution and Bleaching Vessel,
cooling water inlet and outlet, chilling water inlet and outlet, steam inlet and in vacuum line.
• Temperature gauges will be provided at cooling water outlet, chilled water outlet and steam
inlet.
• RTD will be provided to the Reactor, Dilution and Bleaching vessel and it will have local
display.

Warehouse and Storage:

• Inventory to be maintained for Raw material; in which Lauryl Alcohol to be stored in storage
tanks in tank farm area and Dextrose comes in 25Kg bags.

Actual
Raw Material TPM Storage
Lauryl Alcohol 17 35

• All imported raw material will have inventory of minimum 15 days.

• All domestic raw materials within 500 km will have inventory of 7 days and above 500 km
distance will have inventory of 15 days.
• All consumables and IP materials will have inventory of 15 days
• All finished goods will have inventory of 15 days.
• Empty drums will be scraped or will be reutilized for effluent storage or any other purpose.
• Pigeons required for RM and Finished Good are yet to be finalized. This is to be discussed
with Sourcing once.

Safety:

1. The plant should be covered with FH system for handling the emergency.
2. Wherever required the required type fire extinguishers will be in place with clear
identification and easy to access.
3. Safety posters and MSDS to be displayed in all working areas.
4. Internal HAZOP study will be conducted for all process
5. Plant is having safety showers at appropriate locations, easy to access and with effluent
properly routed to effluent pit.
6. Walking and operational areas will be clearly marked with yellow strips.
7. Earthing to individual equipment.
8. Flange guards to be provided in flange joints location.

Laboratory Facilities:
• The laboratory setup is required for performing various analyses for RM and FG.

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• The various lab equipments required for APG process are;
o Polarimeter
o Gas chromatography
o Inductively coupled plasma mass spectrometry
o Karl fischer
o Refractometer
o UV
o pH meter
o NMR
o Brrokefield Viscometer

Material/Intermediate Test Method Instrument Required

Anhydrous Dextrose 1. Moisture content 1. Moisture by 1.Karl fisher

2. Appearance and odour using Karl 2.Polari meter
of solution (black fisher.
particles) 2. Clarity test
3. Specific rotation 3. Polarimetry
Lauryl Alcohol 1. Carbon chain 1. Gas 1. Gas chromatography
composition by GC chromatography
2. Determination 2. Wet analysis
of Carbonyl value
Magnesium Oxide 1. Metal analysis 1. ICPMS ICPMS ( we have in
2. Black partials in water 2. Wet analysis M-3 )
Sodium Hydroxide Wet analysis
Purity by acid-base titration

Sodium Sulphite 1. Determine Assay of Wet analysis

Sodium Sulphite
2. Determination of
Sodium bisulphite in
sodium sulphite
3. Determination of Free
alkalinity in sodium
sulphite
Hydrogen Peroxide

Rx-APG 1. DNSA method 1. UV-Visible

1. Unreacted Dextrose 2. Colour - By Spectrophotometer.
analysis using Lovibond 2. Lovibond
2. Colour 3. Viscosity – 3. Gas
3. Viscosity Brookfield chromatography
4. LA and APG Viscometer 4. Brookfield
composition 4. By extraction Viscometer.
5. pH method using 5. pH meter.
Gas

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chromatographic
method
5. pH of 10 %
solution
Intermediate-APG 1.Viscosity of intermediate 1. Brookfield 1. Brookfield
2.Colour of intermediate. Viscometer Viscometer
3.Metal analysis 2.Lovibond colorimeter. 2.Lovibond
4.% Alcohol contents 3.Metal analysis ( we colorimeter.
5.% Solids can send to another 3.ICPMS
6.% unreacted Dextrose location such as M-3 ) 4. Gas
7.Degree of polymerization 4. Gas chromatography
8.pH chromatography for % 5. Oven
alcohol estimation by 6. UV-Visible
extraction method. spectrophotometer.
5. Oven drying method 7. NMR
6. Unreacted Dextrose – 8. pH meter.
DNSA method by UV-
Visible
spectrophotometer.
7.. For degree of
polymerization – NMR
method (we can tie up
external lab for NMR)
8. pH of 10 % solution
Ref-APG 1.Viscosity 1. Brookfield 1. Brookfield
2.Colour Viscometer Viscometer
3.Metal analysis 2.Lovibond 2.Lovibond
4.% Alcohol contents 3.Metal analysis ( we 3.ICPMS
5.% Solids can send to another 4. Gas
6.% unreacted Dextrose location such as M-3 ) chromatography
7.Degree of polymerization 4. Gas 5. Oven
8. pH chromatography for % 6. UV-Visible
alcohol estimation by spectrophotometer.
extraction method. 7. NMR
5. Oven drying method 8. pH meter.
6. Unreacted Dextrose –
DNSA method by UV-
Visible
spectrophotometer.
7. For degree of
polymerization – NMR
method (we can tie up
external lab for NMR)
8. pH of 10 % solution

D/M water Hardness Wet analysis

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Statutory Aspects:

Others:

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3.0 SIZING

1.1 Tentative equipment list and details

Description Tag No. Dimensions Capacity Location Remarks

Reactor 1 5 KL 2nd floor
Agitator 1
Water Condenser 5 KL 2nd floor
Water Receiver
ORVP+Booster---1
WRVP
Circulation Pump
Jacketed Cartridge filter
Holdup Vessel---2
SPDU feed HE
SPDU Feed Pump----
SPDU
LA Receiver-1
LA Condenser
LA transfer Pump-1
LA Receiver-2
MAAG Pump
LA transfer Pump-2
Dilution Vessel

Bleaching Vessel
Dilution to bleaching transfer
pump.
Bleaching to Tank-
farm/Packing pump.
H2O2 Diaphragm Pump

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4.0 NEW CONCEPTS

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5.0 LAYOUT

• Plant layout will be covered in Plant Concept notes.

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6.0 ANNEXURE

6.1 Trials conducted for Bleaching, Dilution and Filtration

1. Dilution batch conducted at low RPM.

Process Followed-
1. Added 100 gms of material in 100ml of water.
2. Heated at 60 degree.
3. Kept at 12 RPM in a round bottom, get completely mixed in 3 hrs.
4. This experiment is conducted twice, and it was fully successful. The entire APG got
mixed in water without any formation of foam.
5. Shown in the attached Picture.

Image1: Dilution batch at low RPM

2. Bleaching is conducted in Centrifuge at lab scale at TTC.

Process Followed-
1. Once the foamy material gets formed after addition of H2O2 into APG.
2. This foamy APG is kept in tubular centrifuge with a G-Force of 10000.
3. Rotated for 5 mins, APG got separated from foam.
4. A slight layer of foam was found above the APG.

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Image 1: Tubular Centrifuge

Image 2: Foam and APG got separated.

3. Bleaching trial was conducted at Ultrasonication

Process Followed-
1. Kept Ultrasonic rod inside the foamy form of APG for Half an hour.
2. Also tried on water bath sonication.
3. But did not found any variation of foam before and after the experiment.
4. Found this process is not suitable to reduce or remove the foam.

4. Bleaching trial conducted in presence of vacuum.

Process Followed-
1. Experiment is conducted in a round bottom flask in a lab.
2. Measured amount of H2O2 is added in controlled manner in reaction mass.
3. Slight vacuum is applied during the reaction.
4. The expectation was to remove the O2 as its gets formed in the reaction.

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5. But the entire batch was coming up and as we release the vacuum batch goes down, no
reduction of foam was observed.
6. Found this process is not suitable to reduce or remove the foam.

5. All the addition of chemicals are done at 50 to 60 degrees and then

adjusted at 90 degrees.
Process Followed-
1. It is observation of separation of foam on the top and material at the bottom.
2. After keeping the RBF for 2 hours at 90°C, it was observed that all the foam broke and
clear liquid was obtained. 3 batches were conducted to establish the results.

Image 1.: Foam & material separation at >

80°C

Image 2.: Clear material at 90°C for 2h

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6. Filtration Trial;
1. Trial conducted with Filter having.
2. Ajinkya please put the details.

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