Expt. No.

1
ISOLATION OF CELLULOSE MICRO FIBRIL FROM RAMIE FIBER BY ALKALINE
TRAETMENT METHOD USING SODIUM CHLORITE:
Step 1:
9.39 g of Ramie fiber is dissolved in 10% KOH solution (300 ml) and stirred for 14 hours.
Step 2:
50 ml 3% H2O2 is added to the above solution and stirring continues at temperature 45OC for
14 hours.
Step 3:
The solution with 10% KOH and 3% H2O2 was filtered and washed with distilled water.
Step 4:
The fibers are then mixed with 1% NaClO2 solution prepared by mixing 3g NaClO2 in 300 ml
water.
Step 5:
10% acetic acid solution is prepared and the mixed fiber with NaClO2 solution is adjusted at
pH 5 by the 10% acetic acid and the solution is stirred for I hour at 70OC and the solution is filtered
and washed with water.

Step 6:
The fibers are again mixed with 10% KOH and stirred for 14 hours. Then the mixture was
washed with distilled water till pH become neutral.

Step 7:
The fibers are now treated with 1% (wt) HCl (200 ml) solution at 80 OC for 2 hours and then
washed with distilled water to get neutral pH.
The residue was kept to dry.

Expt. No.2

Date: 13-12-2011

Ring opening polymerization of - caprolactone on ramie fiber with variation of different

concentration of [Al(OTf3)] at 1000C.
Materials:
Ramie fiber= 0.1 gm ;
[Benzyle Alcohol]=1.2X 10-1mol/L= 0.02ml
Toluene=10ml ; Time=6hrs ; Tempr.=1000C
Serial no.

[Al(OTf3)] (M)

N1
N2
N3
N4
N5

4.2 x 10-4
6.3 x 10-4
8.4 x 10-4
1.05 x 10-3
1.26 x 10-3

Weight of grafted
polymer
0.095
0.095
0.5761
0.1532
0.3671

% grafting

Kinetic analysis:
[Al(OTf3)] (molar)
4.2 x 10-4
6.3 x 10-4
8.4 x 10-4
1.05 x 10-3
1.26 x 10-3

Monomer conversion
8.38
8.38
50.84
13.52
32.40

60
50

% conversion

40
30
20
10
0
0

[Al(OTf3)] (molar)

Monomer
conversion
8.38
8.38
50.84
13.52
32.40

Expt. No.3

Date: 16-12-2011

Ring opening polymerization of - caprolactone on ramie fiber with variation of different

concentration of [Al(OTf3)] at 1100C.
Materials:
Ramie fiber= 0.1 gm
- caprolactone = 1.1 ml.
[Benzyle Alcohol]=1.2X 10-1mol/L= 0.02ml
Toluene=10 ml; Time=6 hrs; Temperature=1000C, N2 gas is passed.
Serial no.

[Al(OTf)3] (molar)

N1
N2
N3
N4
N5

4.2 x 10-4
6.3 x 10-4
8.4 x 10-4
1.05 x 10-3
1.26 x 10-3

Weight of grafted
polymer
0.0935
0.0917
0.0930
0.0896
0.0960

7.95
8.09
8.21
8.25
8.47

Kinetic analysis:
Serial No.

Monomer
conversion

[Al(OTf3)] (molar)
4.2 x 10-4
6.3 x 10-4
8.4 x 10-4
1.05 x 10-3
1.26 x 10-3

1
2
3
4
5

7.95
8.09
8.21
8.25
8.47

% conversion
8.5

% conversion

8.4
8.3
8.2
8.1
8
7.9
0.00021 0.00042 0.00063 0.00084 0.00105 0.00126 0.00147
[Al(OTf3)] (molar)

Monomer
conversion

% grafting

Expt. No.:4

Date: 23-12-2011

Atom transfer radical polymerization (ATRP) of Glycidylmrthylacrylate (GMA) on cellulose-gpCL to obtain cellulose-g-pCL-g-PGMA by varying the concentration of GMA at 1000C.
Materials:
Cell-g-pCL
CuCl2 = 0.093 gm
[PM-DETA]=1.1X10-2 mol/L = 0.02 ml
[EBIB]= 21.8X10-2 mol/L=0.32ml
DMF=10 ml
Temperature =1000C, N2 Gas is passed.

Sl.no.

Cell-g-pCl(g)

[GMA](M)

1
2
3
4
5

0.1072
0.1010
0.0886
0.1026
0.0849

0.25
0.50
0.75
1.00
1.50

Weight of
grafted
polymer
0.1055
0.1266
0.0970
0.2801
0.2720

% grafting

8.63
12.1
17.6
18.70
29.88

Kinetic analysis:
[GMA](M)

Monomer conversion

0.25
0.50
0.75
1.00
1.50

8.63
12.1
17.6
18.7
29.88

%monomer conversion

35
30
25
20
15
10
5
0
0

0.5

[GMA] (M)

1.5

Monomer
conversion

Expt. No.:5

Date: 03-01-2012

Atom transfer radical polymerization (ATRP) of Glycidylmrthylacrylate (GMA) on cellulose-gpCL to obtain cellulose-g-pCL-g-PGMA by varying the concentration of GMA at 1100C.
Materials:
Cellulose-g-pCL,
CuCl2 = 0.093 gm
[PM-DETA]=1.1X10-2 mol/L = 0.02 ml
[EBIB]= 21.8X10-2 mol/L=0.32ml
Ascorbic acid = 8.8 mg
DMF=10 ml
Tempr. =1100C, N2 Gas is passed.
Sl no.

Cell-g-pCl(g)

[GMA](M)

Weight of grafted
polymer

N1
N2
N3
N4
N5

0.0880
0.0862
0.0864
0.0880
0.0936

0.25
0.50
0.75
1.00
1.50

0.1145
0.0940
0.2791
0.1000
0.0952

% grafting

7.64
8.36
12.42
13.95
26.96

Kinetic analysis:
[GMA](M)

Monomer conversion (%)

0.25
0.50
0.75
1.00
1.50

7.64
8.36
12.42
13.95
26.96

polymerization (%)

30

% polymerization

25
20
15
10
5
0
0

0.5

1
[GMA][M]

Monomer
conversion

1.5

Expt No. 6:
Date: 03/02/2012
Ring opening polymerization of - caprolactone on ramie fiber with variation of different
concentration of [Al(OTf)3] at 1100C.
Ramie fiber= 0.1 gm;
- caprolactone = 1.1 ml.
[Octyle Alcohol] = 0.02ml
DMF=10 ml; Time=6 hrs; Temperature=1100C, N2 Gas is passed.

Serial no.

[Al(OTf)3] (molar)

N1
N2
N3
N4
N5

4.2 x 10-4
6.3 x 10-4
8.4 x 10-4
1.05 x 10-3
1.26 x 10-3

Weight of grafted
polymer
0.0911
0.0987
0.0983
0.1034
0.1077

8.04
8.71
8.67
9.13
9.50

Kinetic analysis:
Serial No.

% conversion

10

Monomer
conversion

[Al(OTf)3] (molar)
4.2 x 10-4
6.3 x 10-4
8.4 x 10-4
1.05 x 10-3
1.26 x 10-3

1
2
3
4
5

8.04
8.71
8.67
9.13
9.50

% conversion

9.5
9
8.5
8
7.5
0.00021

0.00042

0.00063

0.00084

[Al(OTf)3] (molar)

Monomer
conversion

% grafting

0.00105

0.00126

Expt No. 7:
Date: 23/02/2012
Atom transfer radical polymerization (ATRP) of Glycidylmrthylacrylate (GMA) on
cellulose-g-pCL to obtain cellulose-g-pCL-g-PGMA by varying the concentration of initiator EBIB at
1100C.
Materials:
Cellulose-g-pCL,
CuCl2 = 0.093 gm
[PM-DETA]=1.1X10-2 mol/L = 0.02 ml
[GMA] = 1M = 1.05 ml
Ascorbic acid = 8.8 mg
DMF=10 ml,
Temperature =1100C, Time: 6 hrs, N2 Gas is passed.
Sl. no.

Cell-g-pCL(g)

[EBIB](M)

Weight of grafted
polymer

N1
N2
N3
N4
N5

0.0878
0.0883
0.0879
0.0916
0.0900

0.0135
0.0270
0.0405
0.0675
0.0810

0.0955
0.0826
0.0891
0.0954
0.1083

% grafting

6.50
7.35
7.93
8.49
9.64

Kinetic analysis:
Serial
No.
1
2
3
4
5

[EBIB](M)

Monomer
conversion (%)

0.0135
0.0270
0.0405
0.0675
0.0810

6.50
7.35
7.93
8.49
9.64

Monomer conversion (%)

10
9.5

% conversion

9
8.5
8
7.5
7
6.5
6
0.01

0.03

0.05

[EBIB](M)

Monomer
conversion (%)

0.07

Expt No. 8:

Date: 29/02/2012
Ring opening polymerization of - caprolactone on ramie fiber with variation of different
concentration of [Al(OTf)3] at 1000C.
Materials:
Ramie fiber= 0.1 gm;
-caprolactone = 1.1 ml.
[Octyle Alcohol] = 0.02ml
DMF=10 ml; Time=6 hrs; Temperature=1000C
N2 Gas is passed.
Weight of grafted
Monomer
Serial no.
[Al(OTf)3] (molar)
% grafting
polymer(g)
conversion (%)
N1
4.2 x 10-4
0.089
7.85
-4
N2
6.3 x 10
0.092
8.13
-4
N3
8.4 x 10
0.096
8.47
-3
N4
1.05 x 10
0.099
8.73
-3
N5
1.26 x 10
0.097
8.58
Kinetic analysis:
Serial
No.
1
2
3
4
5

8.9

[Al(OTf3)] (molar)

Monomer
conversion (%)

4.2 x 10-4
6.3 x 10-4
8.4 x 10-4
1.05 x 10-3
1.26 x 10-3

7.85
8.13
8.47
8.73
8.58

conversion (%)

%conversion

8.7
8.5
8.3
8.1
7.9
7.7
7.5
0.00021 0.00042 0.00063 0.00084 0.00105 0.00126

[Al(OTf3)] (molar)

Expt No. 9:
Date: 15/03/2012
Atom transfer radical polymerization (ATRP) of Glycidylmrthylacrylate (GMA) on
cellulose-g-pCL to obtain cellulose-g-pCL-g-PGMA by varying the concentration of initiator EBIB at
1000C.
Materials:
Cellulose-g-pCL,
CuCl2 = 0.093 gm
[PM-DETA]=1.1X10-2 mol/L = 0.02 ml
[GMA] = 1M = 1.05 ml
Ascorbic acid = 8.8 mg
DMF=10 ml,
Temperature =1100C, Time: 6 hrs, N2 Gas is passed.
Sl. no.

Cell-g-pCL(g)

[EBIB](M)

N1
N2
N3
N4
N5

0.0844
0.0867
0.0898
0.0910
0.0870

0.0135
0.0270
0.0405
0.0675
0.0810

Weight of grafted
polymer

% grafting

9.5
11.35
14.93
20.49
25.64

Kinetic analysis:
Serial
No.
1
2
3
4
5

Monomer
conversion (%)

[EBIB](M)

Monomer
conversion (%)

0.0135
0.0270
0.0405
0.0675
0.0810

9.5
11.35
14.93
20.49
25.64