Project Nebula

BASIC ENGINEERING

CONCEPT NOTES FOR

GALHUESHIELD HCS

Document Number
P90-TG59-01-003

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1.0 INTRODUCTION
Introduction:
Hair coloring is a growing global trend and most colors that are applied to hair are highly
susceptible to fading due to UV light.
The best hair conditioner is combined with the best UV absorber to create the magic in
the form of a multi-functional hair and hair-color protector. Galhueshield HCS is highly
substantive to hair surface (zeta potential > + 45 mv). Its surface active nature (1% aqueous
dispersion 35Mn/m) helps in wetting the surface. Molecular weight above 500 Daltons (601g/m)
makes it dermatologically safe as far as skin penetration is concerned.
Hair Tresses treated Galhueshield HCS shampoo was not damaged and showed good
hair manageability both in wet & dry combing even after 48 hours of UV exposure.
Galhueshield HCS is a powerful UV absorbing moiety. It prevents damage to hair due to di
sulphite cleaving by harmful UV radiations.
Galhueshield HCS shows minimum hair color loss after 10 cycles of rinsing and UV
exposure as compared to the other available hair color protectors and market benchmark
conditioner.
Galhueshield HCS shows exceptional affinity for the hair. Due to its cationic nature it gets
adsorbed on the hair surface and smoothens disrupted cuticle hence improving sensorial
properties of hair.

Application:
Galhueshield HCS has wide range of applications due to its cationic nature such as
o Protects and retains applied hair color and imparts sensorial properties
o Unique dry and wet sensory
o Superior conditioning during wet and dry combing
o Formulator-friendly
o Exceptional affinity for hair
o Decent anti-dandruff activity
o Improves rheology of rinse-off formulations
o Aligns disrupted cuticles improving manageability of hair
o Reduces tangles after application
o Imparts viscosity boosting effect
o Efficient care for tangled and frizzy hair

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Aim:
 To create facility to manufacture 50 TPA of Galhueshield HCS at G-59 Tarapur.

Background:
Currently Galhueshield HCS is manufactured at W-67 and it is stored at N46 warehouse facility .
Existing process details at W67:
Synthesis of Galhueshield HCS is in four steps.
 Step-1 Chlorination reaction (synthesis of RB-650)

a. Raw materials PMCA 1 mole (solid) & Catalyst D (0.25 % of acid) are charged
through manhole without stirring.
b. TC is charged from MS drum to charging receiver by using vacuum.
c. Thionyl chloride (1.05 mole) is added by maintaining 700-750 torr vacuum through
water jet ejector, Reaction is endothermic, during TC addition temperature is
dropped from room temperature to 0°C.
d. After complete TC addition reaction mass is heated up to 30°C & agitation is
started.
e. Reaction mass is digested for first 4 hours at 35 to 40°C and 2 hours at 60-65°C
under 700-750 torr using water jet ejector.
f. Then again digested for 2 hours at 78°C to 80°C under 0.1 to 0.5 torr using steam
jet ejector for vacuum.
g. Crude Base 650 is taken for distillation under 0.1 to 0.5 torr using steam ejector at
150-165°C.
h. Distilled RB650 mass is unloaded in carboy. & stored at room temperature.

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 Step-2 Amidification reaction (Synthesis of RB-700)

a. In this step MDC (25-27% on solid) & DMAPA are charged using AOD pump
(SS316) from drum.
b. Reaction mass is cooled to below 15°C.
c. MDC (50 %) is added in carbouy having Distilled RB650 mass 50 %, & prepared
1:1 MDC in RB 650 mixture. This mixture is prepared before 4 hours.
d. This mixture is charged in PP charging vessel by using vacuum.
e. Addition of solution of Base 650 & MDC (1:1 w/w) is started with maintaining temp
below 15°C.
f. After addition, stop cooling & digest reaction mass for 4 hours up to it attains room
temperature.
g. DM water (30% on solid) is used to extract RB-700 product from MDC layer.
Needs washing twice (70% & 30 % of total water) by DM water followed by
separation of the MDC and aqueous layer.
h. MDC is recovered from Aqueous layers in reactor by heating at 40-45 °C for 2
hours & 1 hours at 40-45°C under 0.5 torr. (We insure that whether all MDC is
recovered or not. If excess MDC (in PPM) from reaction is not recovered, then
Problem occurs in centrifuge for Separation. That’s why we do MDC recovery
under vacuum. If we increase temperature instead of applying vacuum, then
product gets decomposed & another unknown byproduct might get formed.
i. Caustic lye is added for getting pH 12-13 by maintaining temperature from 20°C to
25°C.After that cool reaction mass below 15°C & stir for 1 hour.
j. Mass is filtered by a Centrifuge & then cake is charged in reactor followed by 1:1
washing (to remove alkalinity) using water which is then followed by separation
using centrifuge.
k. RB700 cake is stored in 25-30 kg HDPE bag at room temperature.

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 Step-3 Chlorination Reaction (Synthesis of Behenyl Chloride).

a. Behenyl alcohol pellets (1mole) from bag & catalyst –D (0.5% on alcohol) from
HDPE drum are charged through manhole.
b. Reaction mass is heated up to 65 ̊ C with stirring under N2 blanketing (0.2 kg/cm2.)
c. After melting Behenyl alcohol ,730-750 torr Vacuum is applied by using water jet
ejector.

d. TC (1.05 mole) is charged from MS drum to charging receiver by using vacuum.

e. TC is added by maintaining temp 60-65 °C under 730-750 torr.

f. After completion of addition reaction mass is digested for 6 hours.
g. Sample is collected from reactor bottom valve, if Behenyl alcohol content is below-
1% then reaction mass is heated to 80 °C & apply full vacuum of water jet ejector
50-60 torr.
h. Traces of HCl & SO2, SOCl2 are removed at 80 ° C under full vacuum (0.1 torr) by
using steam jet ejector.
i. Reaction mass is cooled to room temperature & vacuum is break using nitrogen.
j. After completion of reaction Soda ash & water (1 :0.5 w/w) are added to remove
HCl & SO2.
k. Agitation done for 1 hour at 45 -50 °C and then kept for proper separation of two
layer.

l. Organic & aqueous layer gets separated and reaction mass is again charged for
second wash.
m. Applied plain water wash (1:0.5 w/w) to remove alkalinity. After that Agitation done
for 1 hour at 45-50 °C and then kept for proper separation of two layer.
n. Crude Behenyl chloride is unloaded in HDPE drum.
o. Crude Behenyl chloride is charged in SSR for distillation.

p. Vacuum is applied 0.1 to 0.3 torr using steam jet ejector.

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q. Reaction mass heating is started using thermic fluid. (1st set point for thermic fluid
is 150°C) up to 130-150°C moisture is removed.
r. After removing of moisture reaction mass is heated up to 215-220°C by using
thermic fluid as a utility.
s. After distillation reactor bottom mass is drained in SS bucket.
t. Distilled Behenyl chloride is unloaded in to HDPE carbouy.

 Step-4 Quaternization Reaction. (synthesis of Galhueshield HCS)

a. Behenyl chloride (1.01mole), DM water (on 30 % solid) & Galhueshield HCS (3%)
are charged through manhole.
b. Then N2 purging is started.
c. By keeping N2 purging RB 700 (1 mole) (solid) is charged through manhole.
d. Applied N2 pressure 0.2 kg/cm2 & the reaction mass is heated up to 120-125°C by
using steam.
e. At this temperature reactor pressure is observed 3 kg/cm2.
f. Reaction mass is digested for 12 hours.
g. After digestion reaction mass sample is collected from bottom valve of reactor.
Amine % is checked if it is not less than 1% then continue the digestion for 2
hours.
h. After achieving required result reaction mass is cooled to 70°C.
i. Reaction mass is unloaded in 50 kg HDPE carbouy. (Through nylon filter 5
micron) & stored to room temperature.

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Process block Diagram:
Step 1): Synthesis of p-Methoxycinnamoyl Chloride i.e. RB-650 (Chlorination )

HCl & SO2

gas to
scrubber RB -650


Reaction of p- Traces of
 gas removal
Methoxy
cinnamic acid at about Vacuum
 Digestion at
and Thionyl 55-60°C for 80°C under distillation of
chloride below 4hrs full vacuum crude RB-650 Bottoms
RT for 2 hrs

 Step 2): Synthesis of p-Methoxycinnamidopropyldimethylamine i.e. RB-700

(Amidification)

 Reaction of Two times

MDC recovery
 RB-650 and water
from aqueous
DMAPA in Digestion for washing to
layer at 40°C
 MDC below 4 hrs. at RT the MDC
under vacuum
15°C layer


Addition of
Filtration and 1:1 water Filtration Caustic lye in
RB -700 packing washing below 15°C aqueous layer
at 20-25°C

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Step- 3): Synthesis of Behenyl Chloride (Chlorination)

HCl & SO2 Behenyl

gas Water
Chloride

Reaction of Traces of
Behenyl gas removal soda ash &
alcohol and at about plane water Vacuum
Thionyl 80°C under washing at distillation
chloride at 55- full vacuum RT
60°C Residue

Step 4): Synthesis of Galhueshield HCS (Quaternization)

Reaction of RB-
700 and Packing and
Cooling to cooling to Storage at
Behenyl chloride
70°C 15°C RT
in water at
140°C under 1 Galhues
Kg N2 pressure hield

Q components for the process:

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 Step 1. Synthesis of RB-650
1. PMCA free from moisture within limit (below 0.5%).
o If moisture content is high in PMCA then yield & purity of product is reduced.
2. Reactor should be free from Moisture.
o If moisture is present in rector, then yield & purity of product is reduced.
3. Distillation done at temp 150-165°C.
a. If temp is increased above 165°C, then product degradation occurs.
4. 0.1 to 0.5 torr vacuum is required for RB 650 distillation.
a. To reduce batch cycle time & to get all recovery of product.
 Step 2. Synthesis of RB-700
1. Reactor should be free from Moisture.
o If moisture is present in rector, then yield & purity of product is reduced.
2. Addition of RB-650 and MDC mixture should be done slowly by maintaining temp
below 15°C.
o If addition is performed above 15°C, then Acid Chloride hydrolysis may occur.
Product color & yield may damage. (Required color is white),
3. Complete recovery of MDC should be carried out
o If total MDC from reaction is not recovered, then Problem occurs in centrifuge
for Separation.
4. Distilled RB-650 stored & transferring should be done at temperature above 50°C.
o Melting point of RB-650 is 49-50°C.
Step 3. Synthesis of Behenyl Chloride
1. Reactor should be free from Moisture.
o If moisture is present in reactor, then yield & purity of product is reduced.
2. Heating of Behenyl Alcohol done under N2 Blanketing.
o To avoid contact with air. If Behenyl alcohol comes in contact with air, then
damage color.
3. Distillation done at bottom temp 218-230°C under 0.1 to 0.3 mm Hg vacuum.
o If temp is increased above 231°C, then product degradation occurs.
4. In distillation top collection done in only one cut.
o Carbon chain distribution may vary.

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Step 4. Quaternization reaction
1. Reaction carried out under 0.2 to 1 kg/cm2 N2 pressure.
o In atmospheric condition Reaction will not go forward
o In atmospheric condition yield, color & purity of product is reduced.
2. Product drain /Unload under N2 pressure & at 70°C.
o In below 70°C temp / Room temperature Viscosity of product will increase
that’s why our packing time also increase.

S components for the process:

 Step 1. Synthesis of RB-650
1. Addition of TC should be done slowly
o If TC addition rate is increased, rate of generation of HCl & SO2 will increase
drastically which can pressurize the vessel
2. Thionyl chloride needs to be handled carefully.
o It is highly corrosive and irritant. use proper PPE.
3. HCl Scrubber system is required during entire chlorination reaction.
o To scrub out HCl, SO2 & unreacted SOCl2 gas from reaction
4. RB 650 bottom is drained at high temperature (@ 140 oC), nearby area should be
free from solvent, use proper PPE.
 Step 2. Synthesis of RB-700
1. MDC need to be stored/handled carefully.
o MDC is irritating to the skin, eyes, and respiratory
2. DMAPA need to be stored / handled carefully.
o It has strong amonical Odour & therefore caution: not to inhale.
 Step 3. Synthesis of Behenyl Chloride
1. Addition of TC done slowly by maintaining temp 55-60°C.
o If TC addition rate is increased, rate of generation of HCl, SO2 & SOCl2 will
increase drastically which can pressurize the vessel
2. BC bottom is drained at high temperature (@ 210-220 oC), nearby area should be
free from solvent, use proper PPE.
 Step 4. Quaternization reaction
1. Provide reactor safety valve & RD for emergency case.
3. Reaction is carryout in 3 kg/cm2 pressure.
2. Proper arrangement required to unload/drain the product from reactor.

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4. Product unloading done at 70°C.
Raw material, Intermediates and Finished goods:

 The raw material required for Galhueshield manufacturing are:

Sr.No. Raw Material Physical form

01 p-Methoxy Cinnamic Acid Solid powder

02 Thionyl chloride Liquid

03 Cat D Liquid
04 MDC Liquid
05 DMAPA Liquid
06 Caustic Soda Lye Liquid
07 Behenyl Alcohol White Pellets

 Intermediate products:
Sr.No. Intermediate products Physical form
01 RB 650 Solid
02 RB 700 Solid
03 Behenyl Chloride Colorless Liquid above 41°C

 finished goods:
Sr.No Finished Product Physical form
01 Galhueshield At 70 °C Liquid
At RT-Solid

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Handling and Specifications of RM, intermediates and FG:
1. Behenyl alcohol
o It is procured in 50 kg HDPE bag.
o This material to be stored at ambient conditions.
o The registered suppliers for Behenyl alcohol is VVF India. ltd Taloja.
o The specification required;

Sr. Impurities /
Specifications Limit Impact
No. Deviation
1 Appearance at 25°C White Pastilles
2 Colour 20 max.
3 Acid Value, mg of KOH /gm 0.1 max.
Saponification Value mg of
4 0.5 max.
KOH /gm
Iodine value (Wij's) gms of
5 1.0 max.
I2 /100 gm
Hydroxyl value mg of
6 170-180
KOH/gm
7 Moisture % by wt 0.1 max.
8 Solidification range (°C) 62-67
Carbon chain distribution
C16 Alcohol 0.5 max.
C18 Alcohol 4 to 8
9
C20 Alcohol 15 to 20
C22 Alcohol 72 to 80
C24 Alcohol 1.5 Max
10 Hydrocarbons, % by GLC 1.0 max.

2. Thionyl Chloride
o It is procured in 300 kg GI drum.
o This material to be stored at ambient conditions.
o The registered suppliers for TC to Galaxy are Lanxess india pvt.ltd Gujarat. &
Gwalior chemical India ltd. Gujrat.
o The specification required;

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Sr.
Specifications Limit Impurities/Deviation Impact
No.

1 Nature / appearance Liquid

Colorless to pale
2 Odour
yellow liquid

3 Colour on APHA , max 150

4 Purity % , min. 99.8

3. Catalyst D
o It is procured in 50 kg HDPE carbouy.
o This material to be stored at ambient conditions.
o The registered suppliers for catalyst D to Galaxy are – AMI chemicals, Tarapur.
o The specification required;
4. Caustic Soda Lye
o This material to be stored in M-3 plant 30 KL storage tank at ambient conditions.
o From M3 we transfer it in 50 kg HDPE drum/ carbouy.
o The registered suppliers are Reliance industries Gujrat; Ideal chemicals, &
Sheryal chem India pvt ltd.
o The specification required;

Sr. Impurities /
Specifications Limit Impact
No. Deviation

1 Nature / Appearance Clear Liquid

2 Colour Colorless

3 Assay % by mass , min. 47

4 Iron as Fe ppm , max 10

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5. p- Methoxy Cinnamic Acid

o It is available in HDPE bag.
o This material to be stored at ambient conditions.
o The registered job work company for PMCA is Alba organic, Tarapur MIDC.
o The specification required;
Sr. Specifications Limit Impurities/Deviation Impact
No.
1 Appearance Light yellow powder
2 Moisture content (%) 0.5
3 Assay by titration (%) 99.46

6. Methyl di chloride (MDC)

o It is procured in 250 kg HDPE drum.
o This material to be stored at ambient conditions.
o The registered suppliers for MDC is Remi chem Industries, Mulund Mumbai.
o The specification required;

Sr. Impurities /
Specifications Limit Impact
No. Deviation
1 Nature Clear Liquid
2 Colour Colorless
3 Clarity clear
Moisture content , % by wt.
4 0.2
Max
5 Purity % (by GC) 98

7. Di Methyl Amino Propyl Amine (DMAPA)

o It is generally imported from Belgium, Germany and is available in 165 kg MS
drum.
o This material to be stored at ambient conditions.
o The registered suppliers are B.A.S.F, Germany; Taminco BVC , Belgium & Alkyl
amine chemical, India.
o The specification required;

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Sr. Impurities /
Specifications Limit Impact
No. Deviation
1 Nature Clear Liquid
2 Colour Colorless to pale yellow

3 Colour on APHA , Max. 20

4 Clarity clear

5 Assay % , by GC , Min. 99

6 Amine value , Min 1080

7 Equivalent Mass. Max 103.8

Moisture content , % by
8 0.3
wt. Max

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Intermediate:
1. p- Methoxy Cinnamoyl Chloride (RB 650)
o We store it in 30 kg HDPE drum
o This material to be stored at ambient conditions.
o The specification required;
Sr Impurities /
Specifications Limit Impact
No. Deviation
1 Appearance/ Nature solid crystal
2 Odor Characteristic
3 Color amber
4 Assay % , by mass , min 98

2. RB-700
o We store it in 25 kg HDPE bag.
o This material to be stored at ambient conditions.
o The specification required;
Sr
Specifications Limit Impurities/Deviation Impact
No.
1 Appearance/ Nature solid cake
2 Odor Characteristic
3 Color white
4 Assay % , by mass , min 89-90

3. Behenyl Chloride
o We store it in 25 kg HDPE drum.
o This material to be stored at ambient conditions.
o The specification required;
Sr
Specifications Limit Impurities/Deviation Impact
No.
Yellow to reddish
1 Appearance/ Nature
semi solid
2 Odor Characteristic
3 % Behenyl alcohol (by GC) 1 max

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4 Purity % , by GC , min 99
Finished Goods
1. Galhueshield HCS
o It is packed in 50 kg HDPE drum /carbouy
o This material to be stored at ambient conditions.
o we sale it to Tri-k industries & Pure play skin science india pvt ltd.
o The specification requirement for Galhueshield are;

Specifications Limit / Result Impurities/Deviation Impact

Pearly off-white
paste. Clear high
Appearance/ Nature
viscous pale yellow
liquid above 55⁰C
Odor Characteristic
Color Pearly off-white
Color on Lovibond (5¼“ cell, Y+R),
(50% solution in 1 : 1 IPA-Water 11.8
above 55 °C)
pH Value (1% aqueous dispersion) 6.7
E1% 1 cm, @ λ max 306 nm in Et
120.3
OH
Solids Content, % by mass 29.57

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2.0 PHILOSOPHY
Existing Facility at W67:
Existing Batch cycle time distribution for synthesis of Galhueshield BCT at W-67 is as follows:
1. Synthesis of RB 650
Description Time (min)
Ref. batch #12 ; 21.09.18
Product RB 650 105
Charging of PMCA & catalyst D 40
Addition of TC 155
heating Hot water circulation/ steam 45
Digestion 360
Heating up to 165°C 180
Distillation 1150
unloading 30
TOTAL 1960
Time for 106 kg RB650 32.7 Hrs.

2. Synthesis of RB 700
Description Time (min)
Ref. batch #04 ; 03.09.18
Charging of MDC & DAMAPA 60
Addition of RB-650 (dissolved in MDC) 540
Digestion 240
Addition of DM water(1st wash) 30
Settling & separation 60
Charging of MDC layer 30
Addition of DM water(2nd wash) 20
Settling & separation 60
Charging of Aq.layer 30
Heating & MDC recovery 540
Cooling up to RT 30
Addition of Caustic lye 30
cooling below 15 ̊C & maintaining 60
Filtration 420
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Water wash (remove free Alkalinity) 60

Filtration & Packing 420
TOTAL 2630
Time for 170 Kg RB 700 43.8 hrs.

3. Synthesis of Behenyl Chloride

a. Behenyl chloride reaction
Description Time (min)
Ref. batch #02 ; 23.05.2016
Charging of Behenyl alcohol 60
Charging of Catalyst -D 30
Heating (in N2 blanketing) 120
Addition of TC 420
Digestion 520
Cooling up to RT 120
Washing twice 1.soda ash & plane wash 470
TOTAL 1740
Time for 106 Kg Crude Behenyl Chloride 29 hrs.

b. Behenyl chloride Distillation

Description Time (min)
Ref. batch #01 ; 10.05.2016
Charging of crude Behenyl chloride 30
Heating 240
Distillation 600
TOTAL 870
Time for 174 Kg Crude Behenyl Chloride 14.5 hrs

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4. Synthesis of Galhueshield

Description Time (min)

Ref. batch #01 ; 13.05.2016
Charging of Behenyl chloride, DM water,
90
RB700 ,Galhueshield HCS
Apply N2 & Heating 150
Digestion 960
Cooling up to 70 ̊C 120
Packing 120
TOTAL 1440
Time for 1250 kg Galhueshield 24 hrs.

Time required to Synthesis of 1250 kg Galhueshield

Description Time (hrs.)

Synthesis of RB 650 (1 batch) 32.7
Synthesis of RB 700 (1 batch) 43.8
Synthesis of crude Behenyl Chloride Reaction (2 batch) 58
Synthesis of Behenyl Chloride Distillation (1 batch) 14.5
Synthesis of Galhueshield (1 batch) 24
Total Time for 1250 kg Galhueshield 173 hrs.

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Existing equipment details:
Equipmen Vacuum
Phase Capacity Agitator
t System
Anchor
Reaction GLR-2 160 Lit 1. Oil Ring
Step- blade
1 Vacuum Pump:
Anchor
Distillation GLR-2 160 Lit 350 m3/h
blade
Vacuum-0.1 torr
Anchor
reaction GLR-1 1000 Lit 2. Booster
blade
pump -1200
Step- MDC
SSR-1 1000 Lit Intermig m3/h. Vacuum-
2 recovery
0.1 torr
25 lit wet
Filtration Centrifuge NA 3. Steam Jet
cake
Ejector: 1800
Anchor
Step- Reaction GLR-2 160 Lit m3/h 3 stage
blade
3 steam jet and 1
Distillation SSR-4 200 Lit PBT
stage water jet.
Step- Vacuum-0.1 torr
Reaction SSR-1 1000 Lit Intermig
4

 Packing:
o Packing is done manually using flexible PVC stiff hose
o It is done through nylon filter (Size: 5 micron).
o Packing is done in 50 kg HDPE drums / Carbouy & sent to N46 warehouse.

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 Storage
o Galhueshield stored in N 46 warehouse and store at room temperature.
o Each pallet of Sunbeat drums is plastic wrapped whole together and kept in
rack.
o During dispatch the outer wrapping is removed and wrapped again and
dispatched.
RM / Units
Packin Capacit Packin
Material Intermediat per Storage Area
g Unit y (KG) g MOC
e / FG pallet
N-46
PMCA RM bag 25 HDPE 26
warehouse
Thionyl N-46
RM Drum 300 MS/GI 4
chloride warehouse
Carbou 9 or N-46
Catalyst D RM 50 HDPE
y 18 warehouse
N-46
MDC RM Drum 220 HDPE 4
warehouse
M-3
DMAPA RM Drum 165 MS/GI 4
warehouse
Caustic Carbou 9 or M-3
RM 50 HDPE
Soda Lye y 18 warehouse
Behenyl N46
RM bag 25 HDPE 26
alcohol warehouse
Intermediat carbou 9 or
RB 650 30 HDPE W-67
e y 18
Intermediat
RB 700 bag 25 HDPE 26 W-67
e
Behenyl Intermediat carbou
25 HDPE 26 W-67
chloride e y
Galhueshiel Carbou 9 or N-46
FG 50 HDPE
d HCS y 18 warehouse

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Feasible options evaluated:

Reactor used for SunBeat

Reactor used for Galhueshield

Option-1
 There will be 3 Nos. reactors in which both Sunbeat & Galhueshield production will be
done.
 In this option we conduct RB 700 reaction, RB-650 Reaction, BC reaction in 2 KL GLR.
 RB 650 & BC distillation is conduct in 1 KL HR.
 MDC recovery, Sunbeat & Galhueshield reaction carried out in 2 KL SSR.
 The reactor size & MOC is –
Reactor
Process Cap. Required Utility Reactor Remarks
(KL)
RB-650 Reaction
RB-700 Reaction Steam, cooling,
2 GLR Scrubber system required
Behenyl Chloride chilling ,N2
Reaction

RB-650 Distillation
Behenyl Chloride 1 thermic fluid,N2 Hastelloy ORVP + booster required
Distillation

1.Steam jet ejector / ORVP

MDC Recovery + booster required
2.filtration system
Steam, Cooling,
RB-900 Reaction 2 SSR filtration system
chilling, N2
Sunbeat Reaction Sparkler filter
Galhueshield
Reaction

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Advantages-
1. In this option we will cover all production quantity of Sunbeat & galhueshield given by
commercial team
2. The desired amount of product will be generated in 15 days.
3. Investment for of one reactor & its accessories will be saved in this option as we will go
for three reactors instead of four.
4. We will occupy 1 less bay compared with option 2
Disadvantages-
1. Man hours increases as number of batches in respective reactors will increase.
2. Required extra receivers to store RB-650 intermediate material.
3. Low flexibility for other acid chloride batches for R&D
Option-2
 There will be 4 Nos. reactors used for both Sunbeat & Galhueshield production.

 In this option we conduct RB 700 reaction, SunBeat reaction in 3.5 KL GLR

 MDC recovery, & Galhueshield reaction carried out in 3 KL SSR.
 We conduct RB-650 & Behenyl chloride reaction in 1 KL GLR
 Distillation of RB650 & Behenyl chloride conduct in 0.7 KL Hastelloy.
 Reactor Size & MOC is-
Reactor
Cap. Required
Process Reactor Remarks
Utility
(KL)
RB-650 Reaction Steam / Hot
Behenyl Chloride 1 Water, GLR Scrubber system required
Reaction cooling ,N2

RB-650
Distillation Thermic
0.7 Hastelloy ORVP + booster required
Behenyl Chloride fluid,N2
Distillation

RB-700 Reaction chilling ,cool

3.5 ing ,steam, GLR Sparkler filter
Sunbeat Reaction N2

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1.Steam jet ejector / ORVP +

MDC Recovery booster required
Steam, 2.filtration system
3 Cooling, SSR
RB-900 Reaction chilling, N2 filtration system
Galhueshield
Reaction

Advantages-
1. In this option we will cover all production quantity of Sunbeat & galhueshield given by
commercial team
2. The desired amount of product will be generated in 9 days only.
3. Flexibility of conducting different batches is more in this option as we have four reactors
to accommodate same.
4. We need to take only 4 batches of RB 700 to reach our goal. In synthesis of RB-700 we
need to conduct reaction, MDC recovery, MDC distillation). So due to less batches man-
hour is reduced.
5. Relatively more Operational ease due to separate GLR as process RB650 & RB-700
reaction) are being complicated.
6. Due to two GLR present there will be less interdependency of Sunbeat and Galhueshield
batches on each other.
7. More flexibility in this option as SunBeat & Galhueshield batches will be conducted in
different reactor.
8. As there are Maximum days available to take other batches or in future if demand get
raise the same set up will be used for other same type of reaction
9. The total production quantity at maximum capacity is more in option 2 as compared with
option 1.(approx..40 TPA).
Disadvantages-
1. As we install one more reactor the investment, maintenance cost will increase.
2. We will occupy 1 extra bay compared with option 2


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 Reactor Occupancy per month-
RB - 650 Reaction A MDC Recovery & Distillation F
RB - 650 Distillation B RB-900 Reaction G
Behenyl chloride reaction C Sunbeat Reaction H
Behenyl chloride distillation D Galhueshield Reaction I
RB-700 Reaction E Changeover

 Option-1

Reactor 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15

GLR:2 KL A A E E E E E E E C

HR: 1 KL B B D

SSR:2 KL G F F F F F F F H H H I I I

 Option-2

Reactor 1 2 3 4 5 6 7 8 9

GLR:1 KL A A A A C C
HR: 0.7 KL B B B B D D
SSR:3 KL G F F F F I I
GLR:3.5 KL E E E E H H

Conclusion-
1. Option 2 is more flexible and suitable for operational point of view as we are considering
one more reactor than other option.
2. The intermediate (RB-650) that is formed in our process will not require any extra
receiver in option 2 than other options.
3. In option 2 no. of batches of RB-700, MDC recovery, MDC distillation are less compare
with option 1 which are complex in operation.
4. Less interdependency of production of Sunbeat and Galhueshield on each other

So we are going for option 2 for Product Sunbeat and Galhueshield

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Process Flow Diagram-
Step-1. Synthesis of RB 650

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Step-2 Synthesis of RB-700

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Step-3 Behenyl Chloride

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Step-4 Galhueshield

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Process Details for New Proposal:
 Step-1 Chlorination reaction (synthesis of RB-650)
a. The Raw materials PMCA (1 mole (solid)) & Catalyst D (0.25 % of acid) will be
charged through manhole without stirring.
b. TC (1.05 mole) will be charged through an additional SS316 charging vessel. It
will be charged by gravity.
c. During charging of TC vacuum 700-750 torr will be maintained by scrubber
ejector. For scrubber we consider water jet ejector. (Reaction is endothermic,
during TC addition temperature will drop from room temperature to 0°C.)
d. Here we considered a catch pot above reactor to avoid carryover of FFA.
e. After complete TC addition reaction mass will be heated up to 30°C using steam
as a utility & mixing (agitation) will be started.

f. Reaction mass will be kept for digestion for first 4 hours at 60°C & under 700-750
torr.

g. After getting free PMCA ≤ 2%, it will be kept for second digestion for 2 hours at
78°C to 80°C under 0.1 torr vacuum. Here we will use steam jet ejector for
vacuum.

h. Crude RB 650 will be charged in Hastelloy reactor for distillation.

i. Vacuum 0.1 to 0.5 torr will be applied using steam ejector / (ORVP + Booster).

j. The reaction mass will be heated up to temperature150-165°C using thermic fluid

as a utility. (same reactor is used for both BC & RB650 distillation, in BC
distillation we required 230 °C temperature so we use thermic fluid as a utility)

k. Distilled RB-650 will be collected in receiver which will be having electric heat
tracing for maintaining distillate in liquid form (>50°C)

l. Distilled RB 650 mass will be transferred to another receiver having that 50%
MDC solution at below 15°C. to prepare 1:1 MDC & RB 650 mixture.
 Step-2 Amidification reaction (Synthesis of RB-700)

a. In this step MDC (25-27% on solid) & DMAPA (1.04 mole) will be charged from
drum / carbouy by using AOD pump. (for fresh MDC) Distilled MDC will be
charged from receiver.
b. Reaction mass will be cooled to below 15°C using chilled water.

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c. Addition of solution of Base 650 & MDC (1:1 w/w) will be started through receiver
by gravity with maintaining temp below 15°C.
d. After complete addition, chilling water will be stopped.
e. Reaction mass will be kept for digestion for 4 hours till it attains room temperature.
f. After that soft water (70% on total required water) will be added through water
meter to extract product from MDC layer.
g. Agitation will be done for 30 min and then will be kept for proper separation of two
layer.
h. Lower MDC layer and top aqueous layer will be separated by density difference.
(Aqueous layer contains product). Bottom MDC layer is transferred to GLR for
second water wash.
i. Before transferring reaction mass to SSR pH will be checked & Reaction mass will
be neutralized.
j. Soft Water (30% of total water) will be added through water meter.
k. Agitation will be done for 30 min and will be kept for proper separation of two
layer.
l. Both layer will be collected separately. Aqueous layer will be charged in reactor
SSR and will be heated the reactor using steam, MDC recovery will get started.
m. MDC will be recovered from Aqueous layers in reactor by heating at 40°C under
full vacuum for 3 hours. Here we will use steam ejector / ORVP + Booster for
create vacuum.

m. After completion of MDC recovery, Caustic lye will be added for getting pH 12-13
(since RB700 in final form is alkaline) by maintaining temperature from 20°C to
25°C.

n. After that reaction mass will be cooled below 15°C using chilled water & will be
kept under stirring for 1 hour.
o. Reaction Mass then will be filtered by a Centrifuge to separate the cake.
p. Again cake will be charged in reactor followed by 1:1 washing using DM water.
(To remove alkalinity & improve quality of product)
q. Then Reaction Mass will be filtered by a Centrifuge to separate the cake. & cake
is stored in bag at room temperature.

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Step-3. Synthesis of Behenyl Chloride (Chlorination)
a. Raw material Behenyl alcohol pellets (1mole) from bag & catalyst –D (0.5% on
alcohol) from HDPE drum will be charged through manhole.
b. Reaction mass will be heated up to 65 ̊ C with stirring under N2 blanketing (0.2
kg/cm2.)
c. After melting Behenyl alcohol ,730-750 torr Vacuum will be applied from scrubber
system.
d. TC (1.05 mole) will be charged through an additional charging vessel. It will be
charged through gravity with glass tube rotameter.
e. During charging of TC vacuum 730-750 torr will be maintained through scrubber
ejector
f. TC will be added by maintain temp 60-65 °C under 730-750 torr.
g. After completion of addition reaction mass will be digested for 6 hours.
h. Sample will be collected from reactor bottom valve if Behenyl alcohol will be
below-1% then reaction mass will be heated to 80 °C & apply full vacuum through
scrubber steam jet ejector.
i. Traces of HCl & SO2, SOCl2 will be removed at 80 ° C under full vacuum (0.1 torr)
by using steam jet ejector.
j. Reaction mass will be cooled to room temperature & vacuum will be break using
nitrogen.
k. After completion of reaction Soda ash & water (1 :0.5 w/w) will be added to
remove HCl & SO2.

l. Agitation done for 1 hour at 45 -50 °C and then it will be kept for proper separation
of two layer.
m. Organic & aqueous layer will be separated. And reaction mass will be charged for
second wash.
n. Plain water wash (1:0.5 w/w) will be applied to remove alkalinity. After that
Agitation done for 1 hour at 45-50 °C and then keep for proper separation of two
layer.
o. Crude Behenyl chloride will be unloaded in HDPE drum.
p. Crude Behenyl chloride will be charged in Hastelloy reactor for distillation.

q. Vacuum will be applied 0.1 to 0.3 torr using steam jet ejector.
r. Reaction mass heating will be started using thermic fluid. (1st moisture will be
removed from reaction mass at 150°C.

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s. After removing of moisture reaction mass will be heated up to 215-220°C by using
thermic fluid as a utility.
t. After distillation reactor bottom mass will be cooled to 110°C & drained in MS
drum.
u. Distilled Behenyl chloride will be stored in receiver.

 Step-4. Quaternization Reaction. (synthesis of Galhueshield HCS)

a. Behenyl chloride (1.01mole) will be charged from Behenyl chloride receiver.
b. DM water (on 30 % solid) will be charged from DM water tank through water
meter.
c. Galhueshield HCS (3%) will be charged through manhole.
d. Then N2 purging will be started.
e. By keeping N2 purging RB 700 (1 mole) (solid) will be charged through manhole.
f. N2 pressure 1 kg/cm2 will be applied & the reaction mass will be heated up to
140°C by using steam.
g. At this temperature reaction will be carried out at 3 kg/cm2.
h. Reaction mass will be digested for 10 hours.
i. After digestion reaction mass sample will be collected from bottom valve of
reactor. Amine % will be check if it is not less than 1% then continue digestion for
2 hours.
j. After achieving result reaction mass will be cooled to 70°C.
k. Reaction mass will be unload in 50 kg HDPE carbouy. & stored to room
temperature.
 Breakup of BCT consideration for design

1. Synthesis of RB 650
a. Reaction.
Description Time (min)
Charging of PMCA 120
Addition of TC 180
heating 60 ̊C 60
Digestion 360
Transfer of Crude RB-650 30
750

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b. Distillation
Description Time (min)
Charging of Crude RB-650 30
Heating 180
Distillation 1200
Unloading 30
1440

2. Synthesis of RB 700
a. Reaction
Description Time (min)
Charging of MDC 45
Charging of DMAPA 45
Addition of RB-650 (dissolved in MDC) 540
Digestion 240
Addition of DM water(1st wash) 60
Settling & separation 60
Charging of MDC layer 45
Addition of DM water(2nd wash) 45
Settling & separation 90
TOTAL 1170
b. MDC Recovery
Description Time (min)
Charging of Aq.layer 45
Heating & MDC recovery 240
Cooling up to RT 60
Addition of Caustic lye 60
maintaining 60
cooling below 15 ̊C 45
Filtration Centrifuge 600
Water wash (remove free Alkalinity) 60
Filtration Centrifuge 600
TOTAL 1770

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3. Synthesis of Behenyl Chloride

a. Reaction
Description Time (min)
Charging of Behenyl alcohol 120
Charging of Catalyst -D 30
Heating (in N2 blanketing) 90
Addition of TC 402
Digestion 480
Cooling up to RT 60
Washing 480
TOTAL 1662

b. Distillation
Description Time (min)
Charging of crude Behenyl chloride 45
Heating 180
Distillation 1095
TOTAL 1320

4. Synthesis of Galhueshield HCS

Description Time (min)
Charging of RB-700 45
Charging of Behenyl Chloride 45
Charging of DM water 30
Charging of Galhueshield HCS 30
Apply N2 30
Heating 120
Digestion 720
Cooling up to 70 ̊C 90
unload material 120
TOTAL 1230

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Utility:

Process Reactor Utilities to be used

Synthesis of RB 650 Reaction Reactor-1 Steam / Hot Water, cooling ,N2

Synthesis of RB 650 Distillation Reactor-2 thermic fluid,N2

Synthesis of RB 700 Reactor-3 chilling ,N2

MDC Recovery & distillation Reactor-4 Steam, Cooling, N2

synthesis of crude Behenyl N2, chilling ,cooling, steam, steam jet
Reactor-1
Chloride ejector
Distillation of Behenyl Chloride Reactor-2 N2,Thermic fluid, Steam jet ejector

synthesis of Galhueshield HCS Reactor-4 N2,cooling,steam

Effluent:
Analysis
Kg/MT
of Proposed
Process step Effluent stream of
Effluent Treatment
product
streams
HCL solution (30 %) 65
Synthesis of RB-
SBS solution (30%) 189
650
Distillation bottom 8 incineration
Extraction of water & 6-7 %
415
Synthesis of RB- centrifuge water NaCl
700 2-5 %
RB 700 washing 13
NaCl
HCL solution (30 %) 61
Behenyl Chloride SBS solution (30%) 178
Distillation bottom 8 incineration

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Mechanical:
A. Reactor-1
 The requirement for RB-650, BC reaction reactor are;
a. Size – 1 KL
b. Design – Full vacuum to 6 bar and 160°C, Jacket design for 6 bar
c. MOC – MS GLR
d. Agitator- Suitable agitator will be designed after getting viscosity data of reaction
mass. (Radial mixing, Medium shear, Homogeneous mixing & solid-liquid
mixing.)
 The reactor will have nozzle provision as below;
1. Nitrogen blanketing
2. Vapor line
3. Sight glass
4. light glass
5. PSV
6. Pressure indicator
7. Bottom outlet
8. RM inlet 1
9. RM inlet 2
10. Thermowell -1
11. Manhole
12. Agitator
13. Jacket inlet
14. Jacket outlet
15. Spare nozzle as on need
B. Reactor-2
 The requirement for RB-650, BC distillation reactor are;
a. Size – 0.7 KL
b. Design – Full vacuum to 6 bar and 280°C, Limpet design for 12 bar
c. MOC – Hastelloy
Agitator- Suitable agitator will be designed after getting viscosity data of reaction
mass.
(Solid liquid reaction, homogeneous mixing, effective in low bottom clearance with liquid
submergence)
 The reactor will have nozzle provision as below;
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1. Nitrogen blanketing
2. Vapor line
3. Sight glass
4. light glass
5. PSV
6. Pressure indicator
7. Bottom outlet
8. RM inlet 1
9. Thermowell -1
(as product is costly & process temperature parameter is critical we need to
have more accurate temperature. Also here thermic fluid is used as a utility
the temperature of reaction mass might fluctuate)
10. Thermowell -2
11. Manhole
12. Agitator
13. Limpet inlet
14. Limpet outlet
15. Spare nozzle as on need.
C. Reactor-3
 The requirement for MDC recovery, RB900 & Galhueshield reactor are;
a. Size – 3 KL
b. Design – Full vacuum to 6 bar and 280°C, Limpet design for 12 bar
c. MOC – SS316 L
d. Agitator- Suitable agitator will be designed after getting viscosity data of reaction
mass. (Solid liquid reaction, homogeneous mixing, effective in low bottom
clearance with liquid submergence)
 The reactor will have nozzle provision as below;
1. Nitrogen blanketing
2. Vapor line
3. Sight glass
4. light glass
5. PSV
6. Pressure indicator
7. Bottom outlet
8. RM inlet 1
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9. RM inlet 2
10. Thermowell -1
11. Manhole
12. Agitator
13. Limpet inlet
14. Limpet outlet
15. Spare nozzle as on need.
D. Reactor-4
 The requirement for RB 700& Sunbeat reaction reactor are;
a. Size – 3.5 KL
b. Design – Full vacuum to 6 bar and 160°C, Jacket design for 6 bar
c. MOC – MS GLR
Agitator- retreat curve impeller. Suitable agitator will be designed after getting
viscosity data of reaction mass.
(Radial mixing, Medium shear, Homogeneous mixing & solid-liquid mixing .)
 The reactor will have nozzle provision as below;
1. Nitrogen blanketing
2. Vapor line
3. Sight glass
4. light glass
5. PSV
6. Pressure indicator
7. Bottom outlet
8. RM inlet 1
9. RM inlet 2
10. Thermowell -1
11. Manhole
12. Agitator
13. Jacket inlet
14. Jacket outlet
15. Spare nozzle as on need

Civil:
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 Details will be covered in concept notes of 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 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:
 DCS Monitoring will be required to generate alarm wherever required.
 Pressure gauges will be provided to the reactors, cooling water inlet and outlet, thermic
fluid inlet and outlet, vacuum line, on receiver.
 RTD/Temperature gauges will be provided at cooling water inlet and outlet, thermic fluid
inlet and outlet.
 RTD/Temperature transmitter will be provided for both reactors, and it will have local
display.

Laboratory Facilities:

 The laboratory setup is required for performing various analyses for RM, FG and IP.
 These quality checks of lab will be conducted at plant laboratory
 The lab equipment’s required for Sunbeat process are;
o HPLC
o Titration setup
o Gas chromatography
o Lovibond color comparator
o UV Spectrophotometer
o RI spectrophotometer
o Karl Fischer
o pH meter
o Oven

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o Electric burner
o Muffle furnace
o Hydrometer / Pycnometer
o Melting point apparatus

Sr No Material Test Method

Purity Iodimetric titration
1 Thionyl chloride
Colour standard comparison
Colour Lovibond color
Assay GC
2 DMAPA
Amine value Acid base titration
Moisture content Karl fischer
Purity Iodimetric titration
3 SMBS pH PH meter
Iron content UV spectrophotometer

Caustic Soda Assay Acid base titration

4
Lye Iron content UV spectrophotometer
Colour Lovibond color
Acid value Acid base titration
Saponification Value Acid base titration
Iodine value Iodometric titration
5 Behenyl alcohol Acid base titration ( acetic
Hydroxyl value
anhydride & pyridine )
Moisture content LOD method (oven)
Carbon chain
HPLC
determination
Moisture content LOD method (oven)
6 Cinnamic Acid
Assay Acid base titration

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Warehouse and Storage:
 All imported raw material will have inventory of minimum 15 days.
 All consumables 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 in-process material storage

Safety:
 The reactor will have pressure safety valves.
 Pressure safety vale at Hytherm inlet will be provided.
 N2 blanketing line will have PRV.
 The plant is covered with FH system for handling the emergency.
 Wherever required the required type fire extinguishers will be in place with clear
identification and easy to access.
 Safety posters and MSDS to be displayed in all working areas.
 Internal HAZOP study will be conducted for all process
 Plant is having safety showers at appropriate locations, easy to access and with effluent
properly routed to effluent pit.
 Walking and operational areas will be clearly marked with yellow strips.
 Earthing to individual equipment.
 Flange guards to be provided in flange joints location

Statutory Aspects:
 It will be covered in separate concept notes.

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3.0 SIZING
 Tentative list of equipment is as follows:

Capacit Dimension
Description MOC
y s (m)
Reactor 1 for crude RB-650,BC
reaction Glass lined 1 KL
Piping for reactor-1 MS-PTFE
Reactor 2 for RB-650 distillation,
BC distillation Hastelloy 0.7 KL

Piping of reactor -2 Hastelloy

TC receiver PP/glass lined 0.3 KL
steam jet ejector / ORVP +
Booster for RB 650 distillation
Condenser to reactor – 2
Receiver for Reactor-2 Hastelloy/glass lined 0.5 KL
Receiver for RB-650 & MDC
mixture Hastelloy/glass lined 1 KL
Reactor-3 RB-700 Reaction Glass lined 3.5KL
MDC receiver SS316 2 KL
Epichlorohydrin receiver SS316 0.5 KL
Filtration system- centrifuge for
RB-700
Reactor 4 for MDC recovery,
MDC distillation, Galhueshield
HCS SS316/SS316 L 3KL
Sparkler filter system SS316/SS316L

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4.0 NEW CONCEPTS
1. Theme 1:
 Addition of RB 650 dissolved in MDC through a charging vessel.
 Existing procedure:
1. Currently at W-67, RB 650 is unload in carbouy. Mixture of RB650 & MDC is
prepared in carbouy then it is charged in small charging pot
2. Addition of dissolved RB 650 in MDC is done by maintaining temp below 15°C, so
controlled addition is required.
 Thought process:
1. We have considered an additional receiver for preparing mixture of RB-650 & MDC
which is also used as charging vessel.
2. RB650 & MDC mixture is charged by gravity through closed glass tube rotameter. It
is to be provided for safety point of view and ease in charging of RB 650 dissolved
in MDC.
 Benefits:
1. Controlled addition makes ease in operation.
2. This will avoid manual contact which makes the operation condition safer.
2. Theme 2:
 Distillation of RB 650 in Hastelloy or Titanium. (Innovation team is checking the
compatibility)
 Existing procedure:
1. Currently at W-67, RB 650 distillation done in GLR. For distillation we required
temperature 165°C. GLR jacket is designed for 6 kg/cm2 (g) steam pressure. We
require 8-9 kg/cm2 (g) steam pressure to achieving the distillation temperature
during final stages.
 Thought process:
1. We have considered Hastelloy reactor for distillation with heating media thermic
fluid.
 Benefits:
1. Batch cycle time is reduced & the recovery of distilled product also increased.
2. Required temperature can be easily achieved.
3. It can also be used for Distillation of Behenyl chloride.

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3. Theme 3:
 Addition of DM water from DM water storage tank through water meter.
 Existing procedure:
1. Currently at W-67, manual addition is taking place.
2. Addition of DM water is done after weighing of water quantity. Due to this manual
procedure BCT is unnecessarily increased.
 Thought process:
1. DM water is charged from DM water storage tank by gravity through water meter. It
is ease in charging operation.
 Benefits:
1. Addition through water meter makes ease in operation.
2. BCT is reduced.

a. LAYOUT

 It will be covered in concept notes of plant.

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6.0 ANNEXURE
Document No. of MSDS

Material Document No.

Behenyl Chloride 0118090PBEPMT004

Caustic Soda Lye 0118090PBEPMT005

Con.HCl 0118090PBEPMT006

MDC 0118090PBEPMT007

DMAPA 0118090PBEPMT008

NaOH pellets 0118090PBEPMT013

p-Methoxy Cinnamic Acid 0118090PBEPMT014

Thionyl chloride 0118090PBEPMT017

Abbreviation
1. PMCA - para Methoxy Cinnamic acid
2. TC - Thionyl Chloride
3. BC - Behenyl chloride
4. ORVP – Oil Ring vacuum pump
5. RB - Refined Base
6. MDC - Dichloromethane
7. DMAPA - 3-Dimethylaminopropylamine
8. BCT – Batch Cycle Time
9. RT- Room temperature
10. LOD - Loss on Drying

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