Beta cyclodextrin in Wrinkle Recovery Finishing
18
ITSAPT seminar, Guimaraes, November 2005 Bojana Vončina Bojana Vončina University of Maribor, Textile Department, University of Maribor, Textile Department, Smetanova 17, 2000 Maribor, Slovenia Smetanova 17, 2000 Maribor, Slovenia nd determination of beta cyclodextrin on textile su
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Transcript of Beta cyclodextrin in Wrinkle Recovery Finishing
ITSAPT seminar, Guimaraes, November 2005
Bojana Vončina Bojana Vončina University of Maribor, Textile Department, Smetanova 17, University of Maribor, Textile Department, Smetanova 17,
2000 Maribor, Slovenia2000 Maribor, Slovenia
Use and determination of beta cyclodextrin on textile substrates
ITSAPT seminar, Guimaraes, November 2005
Structure and dimensions of cyclodextrins
ITSAPT seminar, Guimaraes, November 2005
Conical structure of cyclodextrin
ITSAPT seminar, Guimaraes, November 2005
Host–guest complex of cyclodextrin and toluene
ITSAPT seminar, Guimaraes, November 2005
Applications of cyclodextrin in textile:
Application methods (Surface modification)Surface modification): Exhausting method Pad-batch method Printing
WashingWashing
Preparation of polymersPreparation of polymers
In fibre spinningIn fibre spinning Surface modificationSurface modification
EncaptulationEncaptulation
ITSAPT seminar, Guimaraes, November 2005
Polycarboxylic acids like 1,2,3,4 butanetetracarboxlic acid (BTCA) are well known nonformaldehyde crosslinking reagents. BTCA has four carboxylic acid groups, which can react with hydroxyl groups of cellulose and form stable ester bonds Esterification can occur with heat alone or it can be accelerated by the presence of salts of weak acids, such as sodium hypophosphite (SHPI). Physical properties of cotton fabrics treated with BTCA were comparable with those obtained for cotton treated with the most effective N-methylol reagents such as N, N’-dimethyloldihydroxy-ethylene-urea (DMDHEU)
ITSAPT seminar, Guimaraes, November 2005
Grafting of -cyclodextrin -cyclodextrin on cotton using on cotton using polycarboxylic acidpolycarboxylic acid
OC
O
CH
COOH
CH
COOH
C
O
O
ITSAPT seminar, Guimaraes, November 2005
• Mercerised cotton, immersed in treated baths • Wet pick up 100%• Predried at 110 º C, 10 minutes• Fixation at 170 º C, 3 minutes• Washed in cold water and at 60 º C 30 minutes
Concentration of -CD in
finished bath (g/l)
Concentration of BTCA in
finished bath (g/l)
Concentration of SHPI in
finished bath (g/l)
Curing
temperature
(º C)
20 6 3 170
20 6 6 170
30 6 3 170
3030 66 66 170170
3030 66 66 200200
ITSAPT seminar, Guimaraes, November 2005
-cyclodextrin molecules linked to textile substrate can be
determined qualitatively by Phenolphthalein and Phenol
red.
Alkaline solution of Phenolphthalein changes colour from carmine red for untreated textile substrate to colourless for BTCA/-CD treated textile materials.
Phenol red forms a yellow coloured complex with -CD, so Phenol red changes colour from red to yellow when -CD is present at the textile substrate.
These qualitative methods can be use for white textile
materials only.
ITSAPT seminar, Guimaraes, November 2005
20 g/l β-CD, 6 g/l BTCA, 3 g/l SHPI
c(CD)
pH
0 (g/l) 20 (g/l) washed in cold water
washed at 60º C
3
c(CD)
pH
0 (g/l) 20 (g/l) washed in cold water
washed at 60º C
12
ITSAPT seminar, Guimaraes, November 2005
30 g/l β-CD, 6 g/l BTCA, 3 g/l SHPI
c(CD)
pH
0 (g/l) 30 (g/l) washed in cold water
washed at 60º C
3
c(CD)
pH
0 (g/l) 30 (g/l) washed in cold water
washed at 60º C
12
ITSAPT seminar, Guimaraes, November 2005
30 g/l β-CD, 6 g/l BTCA, 6 g/l SHPI
c(CD)
pH
0 (g/l) 30 (g/l) washed in cold water
washed at 60º C
3
c(CD)
pH
0 (g/l) 30 (g/l) washed in cold water
washed at 60º C
12
ITSAPT seminar, Guimaraes, November 2005
Quantitative determination of linked -CD
Gravimetrical method
The objective of the present study has been to develop semi-quantitative method for the evaluation of evaluation of -CD -CD fixed onto the textile materials by UV/Vis spectroscopy fixed onto the textile materials by UV/Vis spectroscopy using alkaline solution of phenolphthaleinusing alkaline solution of phenolphthalein..
ITSAPT seminar, Guimaraes, November 2005
amountCD (mL)
pH ABS(550 nm)
AF-ADF A
brez 11,35 0,9624 0,9624-0,9624
0
1 11,35 0,7400 0,9624-0,7400
0,2224
2 11,38 0,6341 0,9624-0,6341
0,3283
3 11,36 0,4576 0,9624-0,4576
0,5048
4 11,36 0,3729 0,9624-0,3729
0,5895
5 11,35 0,3482 0,9624-0,3482
0,6142
ITSAPT seminar, Guimaraes, November 2005
CH2 C
CH COOH
CH
CH2 C
COOH
O
O
O Cell
O CD
CH2 C
CH COO Na
CH
CH2 C
COO Na
O
O
O Cell
O CD
alkalinetreatment
- +
- +
Conversion of carboxylic acid groups to carboxylate anions
After-treatment of BTCA/CD finished cotton fabrics with alkaline solution separate ester carbonyl band from
carboxylic acid band
ITSAPT seminar, Guimaraes, November 2005
ATR FT-IR spectroscopy of nanoencaptulated cotton
2000,0 1950 1900 1850 1800 1750 1700 1650 1600 1550 1500 1450 1400 1350 1300 1250 1200 1150,0
84,1
85
86
87
88
89
90
91
92
93
94
95
96
97
98
99,0
cm-1
%T
1567,171639,31
1724,80
4000,0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600,0
73,0
74
76
78
80
82
84
86
88
90
92
94
96
98
99,9
cm-1
%T
1711,45
1561,83
1414,88
ITSAPT seminar, Guimaraes, November 2005
Mechanism of grafting with policarboxylic acids
CH2 COOH
CH COOH
CH
CH2 COOH
COOH
CH2 C
CH C
CH
CH2 C
C
O
O
OO
O
O
C
O
Cell O CH2CH
COOH
COOH
O
-H2O + Cell-OH+ CD-OH
CH CH2 C CDO
ITSAPT seminar, Guimaraes, November 2005
Conclusions
We successfully grafted We successfully grafted -cyclodextrin-cyclodextrin onto onto cellulose substrate by using crosslinking reagent cellulose substrate by using crosslinking reagent BTCA.BTCA.
In our research the rapid and simple spectroscopic method for determination of micro-amount of cyclodextrin in solution was adopted to determine the amount of -cyclodextrin bonded onto the textile material..
