Lab report of Wuhan Textile University

1. Basic information

Name Gender Male

Nationality

Student number

Speciality

2. Basic informations

Name Gender

Bangladeshi
Nationality

Student number

Speciality

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 Experiment name Preparation of Polyurethane acrylate Binder for Pigment Printing
1 Synthesis of three polymers.
2 Design the recipes for polymerization.
Experiment contents
3 Design the conditions for synthesis of polymer.
4 Evaluate the synthesis process.
1 Synthesis of hard and soft polymer.
Concentration of the polymeric materials should be 30%, 35% and
2
Experiment 40%.
purposes Solid content of polymers should be ≤ 30%, ≤ 35% and ≤ 40%
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respectively.
4 Conversion rate of polymer should be about 90%.
Recipe design & dosage
Here in below we are giving a clear indication of the name of monomers and auxiliaries that we
employed and their dosage, proportion in recipe.
Recipe 1: (For Preparation of Soft Polymer)
 Hard Monomer

 A.N 25 gms

 S.T. 10 gms
 Soft Monomer

 EA 25 gms

 B.A. 18 gms

 PU 17 gms
 Functional Monomer

 A.A. 03 gm

 H.E.A 02gm
Total Monomers = 100 gms
 Initiators / Catalyst (0.5% of total monomer)

 A.P.S. .57gm
 Surfactants (4% of total monomer)

 SDS (2.5%) 3 gms

 K-12 (1.5%) 2gm

 Required Water (70% of total materials)

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 = {(100 + 0.57 + 3 + 2) / 0.4} ml ‒ 100 ml.

= (263.925 ‒ 100) ml. = 163.925 ml ≈ 164ml

Recipe 2: (For Preparation of Hard Polymer)

 Hard Monomer
 M.A. 26 gms

 S.T. 12 gms
 Soft Monomer
 EA 24 gms

 BA 17 gms

 PU 16gms
 Functional Monomer
 A.A. 03 gm

 H.E.A 02gm
Total Monomers = 100 gms
 Initiators / Catalyst (0.5% of total monomer)
 A.P.S. 0.57gm
 Surfactants (4% of total monomer)
 SDS (2.5%) 3 gms

 K-12 (1.5%) 2gm

Required Water (70% of total materials
 Required Water (70% of total materials)

= {(100 + 0.57 + 3 + 2) / 0.4} ml ‒ 100 ml.

= (263.925 ‒ 100) ml. = 163.925 ml ≈ 164ml

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 Reaction conditions design
Now we are giving the flow chart of the experiment. Furthermore, the experiment conditions
should be listed in detail too.
Recipe 1:
Step I → Emulsify the monomer with surfactants at room temperature. Take OP-10 and K-12,
then add 20% of total water and put all the monomer one by one at 5 minutes of time interval.
Then run about 30 minutes at RT with continuous stirring.
Step II → Make the solution of Initiators. Add 0.25 gms of Ammonia per sulphate in 20 ml of
water.
Step III → Take 1/6 parts pre-emulsion in a 3 neck bottle; add remaining 80% of total water, then
raises the temp. With continuous stirring. At temp 75 oc, add 1/3 parts of initiators in the pre-
emulsion solutions and run about 20 minutes. Continue the process till for observing the blue
beam in mixtures solutions.
Step IV → When blue beam observed then remaining 5/6 parts of pre-emulsion and 2/3 parts of
initiators put into the reactor simultaneously one by one in 90 minutes of time intervals at 80 oc
temp.
Step V → Increase the temp from 80oc to 85oc and keep it about 30 minutes. Stirring speed should
be slower. Run the process till for observing sweet smell. (Note: If sweet smell not found or strong
smell observed then add 10% extra initiators to the mixtures. Need to run another 20 min. at
85oc.).
Step VI → When sweet smell is observed, lower the temperature at 40 oc.Nuetralize the solutions
by adding ammonia water (20%) to the solutions mixtures until PH=7 is not achieved.
Step VII → Lower the temperature of the solution to room temperature and collect all the
segments and residue by filtration. Wash the entire residue and dry it at 105o c for 90 minutes.
Recipe 2:
Step I → Emulsify the monomer with surfactants at room temperature. Take OP-10 and K-12,
then add 20% of total water and put all the monomer one by one at 5 minutes of time interval.
Then run about 30 minutes at RT with continuous stirring.
Step II → Make the solution of Initiators. Add 0.25 gms of Ammonia per sulphate in 20 ml of
water.
Step III → Take 1/6 parts pre-emulsion in a 3 neck bottle; add remaining 80% of total water, then
raises the temp with continuous stirring. At temp 75 oc, add 1/3 parts of catalyst in the pre-
emulsion solutions and run about 20 minutes. Continue the process till for observing the blue
beam in mixtures solutions.

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Step IV → When blue beam observed then remaining 5/6 parts of pre-emulsion and 2/3 parts of
initiators put into the reactor simultaneously one by one in 90 minutes of time intervals at 80oc.
Step V → Increase the temp from 80oc to 85oc and keep it about 30 minutes. Stirring speed should
be slower. Run the process till for observing sweet smell. (Note: If sweet smell is not found or
strong smell observed then add 10% extra initiators to the mixtures. Need to run another 30 min at
85oc.).
Step VI → When sweet smell is observed, lower the temperature at 50 oc.Nuetralize the solutions
by adding ammonium water (20%) to the solutions mixtures until PH=7 is not achieved.
Step VII→ Lower the temperature of the solution at room temperature and collect all the segments
and residue by filtration. Wash the entire residue and dry it at 105o c for 90 minutes.

Experimentation track record Recipe 1

Operation Phenomena Attentions
Treated in room temp. And dosing
Step I None.
carefully all monomers.
Make solution of initiator with 20
Step II None.
ml. water.
Add 80% water and then add 1/6
Observed blue beam after parts emulsifier & 1/3 parts
Step III
25 min. Initiator (APS) drop by drop then
raise the temp. at 75oc temp.
Raise the temp. 80oc and add the
After evenly dosing we
rest quantity of emulsifier and
Step IV observed that the blue beam
initiator same ratio one by one
going to light.
evenly and stirring slowly.
Raise the temp. 85oc and stir
At the beginning feel strong slowly about 30 min. and continue
Step V smell and lastly feel sweet till feel sweet smell. If the smell is
smell. strong we should add initiator
again in same temp. for 20 min.
Step VI Neutralize in PH=7 Reduce the temp. 40oc and
neutralize by 20% ammonia water
(NH3).

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 Experimentation track record Recipe 2
Treated in room temp. And dosing
Step I None.
carefully all monomers.
Make solution of initiator with 20
Step II None.
ml. water.
Add 80% water and then add 1/6
Observed blue beam after parts emulsifier & 1/3 parts
Step III
25 min. Initiator (APS) drop by drop then
raise the temp. at 75oc temp.
Raise the temp. 80oc and add the
After evenly dosing we
rest quantity of emulsifier and
Step IV observed that the blue beam
initiator same ratio one by one
going to light.
evenly and stirring slowly.
Raise the temp. 85oc and stir
In the beginning feel strong slowly about 30 min. and continue
Step V smell and lastly feel sweet till feel sweet smell. If the smell is
smell. strong we should add initiator
again in same temp. for 20 min.
Reduce the temp. 40oc and
Step VI Neutralize in PH=7 neutralize by 20% ammonia water
(NH3).

Testing results
Please see the list related testing results in table:
For Recipe 1:
A. Gel Ratio = (Dry weight of Total residue / Total weight of monomer)×100
= (0.28 / 100)×100
= 0.28%

B. Solid Content = (G1/G0)×100 Where, G1 → Constant dry weight of

= {(1.96-0.70)/5.50}×100 the sample,(1.96-0.70)= 1.26 gm
= 0.229×100 Empty paper weight is = 0.70 gm

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 = 22.90 % Paper wt. + Dry sample wt. = 1.96gm
G0 → Sample weight, 5.50 gm
C. Conversion ratio:
{(G1-G0W) / (G0M×Solid content)}×100
Where, W = (APS + Emulsifier) / (APS + Emulsifier +Monomers)
= (0.57+5.00) / (0.57+5.00+100)
= 5.57/105.57=0.052
M = Monomers / (APS + Emulsifier + Monomers)
= 100/(0.57+5+100)
= 100/105.57
= 0.95
G1 = 1.26 gm, G0=5.50 gm and Solid content=0.229
Therefore, Conversion ratio = [{1.26-(5.50×0.052)}/{(5.50×0.95) ×0.229}]×100
= [.974/1.196] ×100
= 0.82×100
= 82%

D. Emulsion stability test:

 Dilution stability: The emulsion was diluted to a solid content of 3%, then the emulsion
was poured into 30ml tubes after dilution, the liquid column height of 20cm, is placed 72h,
measuring the volume of supernatant and precipitate upper portion.
Result: No change found in the emulsion.
 Acid and Alkali stability: In two test tubes were charged emulsion 5g sample tested, the
two tubes were then added drop wise 1ml (1mol / L) hydrochloric acid and 1ml (1mol / L)
solution of KOH. After shaking, the PH test and observe the emulsion is stable. Then the
two tubes placed at room temperature for 24h, and then observe the stability of the
emulsion.
Result: No change found, Emulsion is resistant to both acid and alkali.
 Electrolyte resistance stability: Added 16ml polymer emulsion sample into the test tube,
then add 4ml of 0.5% CaCl2 solution, shake and let stand 48h, the emulsion changes
observed.
Result: No change found, Emulsion is resistant to electrolyte.

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For Recipe 2:
A. Gel Ratio = (Dry weight of Total residue/ Total weight of monomer)×100
= (0.29/100)×100
= 0.29 %
B. Solid Content = (G1/G0)×100 Where, G1 → Constant dry weight of
= {(2.09-0.75)/5.50}×100 the sample,(2.09-0.75)= 1.34 gm
= 0.244×100 Empty paper weight is = 0.75 gm
= 24.4% Paper wt. + Dry sample wt. =2.09 gm
G0 → Sample weight, 5.50 gm
C. Conversion ratio:
{(G1-G0W)/(G0M×Solid content)}×100
Where, W = (Aps + Emulsifier) / (Aps + Emulsifier + Monomers)
= (0.57+5.00) / (0.57+5.00+100)
= 5.57/105.57=0.052
M = Monomers / (APS + Emulsifier + Monomers)
= 100/(0.57+5+100)
= 100/105.57
= 0.95
G1 = 1.34 gm, G0=5.50 gm and Solid content=0.244

Therefore, Conversion ratio = [{1.34-(5.50×0.052)}/{(5.50×0.95) ×0.244}]×100

= [1.054/1.283] ×100
= 0.83×100
= 83 %

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 D. Emulsion stability test:
Same result found as emulsion-1.

Table 1.1: Testing results

Polymer Gel Ratio Solid content Conversion Ratio Remarks

Recipe-1 (30%) 0.28% 22.90% 82%
Recipe-2 (30%) 0.29% 24.4% 83%

Table 1.2: Stability Test results

Polymer Dilution Acid Stability Alkali Stability Electrolyte resistance

Stability Stability
Recipe-1 (30%) Stable Stable Stable Resistant
Recipe-2 (30%) Stable Stable Stable Resistant

Experiment gist
Through this experiment we have to understand the emulsion polymerization technique by using
soft, hard and functional monomers. Also our realization is that, emulsion polymerization is a type
of radical polymerization that usually starts with an emulsion incorporating water, monomer, and
surfactant. With increasing proportion of monomers in the formulation, lower conversion was
observed which could be due to the lower reactivity of monomers for radical polymerization in the
presence of these others monomers. More study for the utilization of monomers in polymer
synthesis is needed which, on successful optimization, would give a cost-effective alternative to
various commercial areas. In the area of testing result we have found that, gel ratio and solid
content percentage of soft polymer is less than the hard polymer but on the other hand conversion
ratio percentage is more on hard polymer than the soft polymer. Also the dilution, acid, alkali and
electrolyte resistance stability for both polymers are stable. In our experiment we are sometimes

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unable to put the monomers one after another simultaneously and also sometimes it was difficult
to control the temperature in different stages. Our advise is, to get the better result on gel ratio,
solid content and conversion ration we must be aware of the required temperature on every stage.
Also we must put monomer one by one to the reactor instead of putting monomers quickly & must
be aware of the stirring speed which should not be more, less comparing with the standard.

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