ITSAPT seminar, Guimaraes, November 2005 Use and determination of beta- cyclodextrin on textile substrates Bojana Vončina University of Maribor, Textile Department, Smetanova 17, 2000 Maribor, Slovenia

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: Surface modification) Application methods (Surface modification): Exhausting method Pad-batch method PrintingWashing Preparation of polymers In fibre spinning Surface modification Encaptulation

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  -cyclodextrin on cotton using polycarboxylic acid Grafting of  -cyclodextrin on cotton using polycarboxylic acid

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)

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 g/l β-CD, 6 g/l BTCA, 3 g/l SHPI

ITSAPT seminar, Guimaraes, November g/l β-CD, 6 g/l BTCA, 3 g/l SHPI

ITSAPT seminar, Guimaraes, November g/l β-CD, 6 g/l BTCA, 6 g/l SHPI

ITSAPT seminar, Guimaraes, November 2005 Quantitative determination of linked  -CD Gravimetrical method evaluation of  -CD fixed onto the textile materials by UV/Vis spectroscopy using alkaline solution of phenolphthalein. The objective of the present study has been to develop semi-quantitative method for the evaluation of  -CD fixed onto the textile materials by UV/Vis spectroscopy using alkaline solution of phenolphthalein.

ITSAPT seminar, Guimaraes, November 2005 amountC D (mL) pHABS (550 nm) A F -A DF AA brez11,350,96240, , ,350,74000, ,7400 0, ,380,63410, ,6341 0, ,360,45760, ,4576 0, ,360,37290, ,3729 0, ,350,34820, ,3482 0,6142

ITSAPT seminar, Guimaraes, November 2005 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

ITSAPT seminar, Guimaraes, November 2005 Mechanism of grafting with policarboxylic acids

ITSAPT seminar, Guimaraes, November 2005 Conclusions We successfully grafted  -cyclodextrin onto cellulose substrate by using crosslinking reagent BTCA. We successfully grafted  -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  -cyclodextrin bonded onto the textile material.