Beta cyclodextrin in Wrinkle Recovery Finishing

Bojana Vončina University of Maribor, Textile Department, Smetanova 17, 2000 Maribor, Slovenia Use and determination of beta cyclodextrin on textile substrates... Applications of β cycl

Bojana Vončina

University of Maribor, Textile Department, Smetanova 17,

2000 Maribor, Slovenia

Use and determination of beta cyclodextrin on textile substrates

Structure and dimensions of

cyclodextrins

Conical structure of β cyclodextrin

Host–guest complex of β cyclodextrin and

toluene

Applications of β cyclodextrin in textile:

Application methods (Surface modification):

 Exhausting method

 Pad-batch method

 Printing

Washing

Preparation of polymers

In fibre spinning

Surface modification

Encaptulation

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)

Grafting of β -cyclodextrin on cotton using

polycarboxylic acid

O

C O

C H

COOH

C H COOH

C O

O

• Mercerised cotton, immersed in treated baths

• Fixation at 170 º C, 3 minutes

Concentration

of β-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)

β-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/β-CD treated textile materials

 Phenol red forms a yellow coloured complex with β-CD,

so Phenol red changes colour from red to yellow when

β-CD is present at the textile substrate

These qualitative methods can be use for white textile

materials only

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

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

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

Quantitative determination of linked β -CD

 Gravimetrical method

 The objective of the present study has been to develop semi-quantitative method for the evaluation of β-CD fixed onto the textile materials by UV/Vis spectroscopy using alkaline solution of phenolphthalein

D (mL)

pH ABS

(550 nm)

A F -A DF ∆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

C

C H C

COOH O

O

O Cell

O CD

C

C

C H C

COO Na

O

O Cell

O CD

alkaline treatment

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

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

1567,17 1639,31 1724,80

80 82 84 86 88 90 92 94 96 98 99,9

%T

1711,45 1561,83 1414,88

Mechanism of grafting with policarboxylic acids

C

C

C H C

COOH

C

C

C H C

C

O O O O O O

C

O

COOH

COOH

O

+ CD-OH

 We successfully grafted β -cyclodextrin onto cellulose substrate by using crosslinking reagent 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 β -cyclodextrin bonded onto the textile material.