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Preparation of siloxane modified polyurethane hydrolysate

A technology of siloxane modification and silane modification, which is applied in the direction of animal fiber, textiles, papermaking, fiber treatment, etc. It can solve the problems of non-compliance with clean production requirements, high baking temperature, hard hand feeling, etc., and achieve improved baking Effect of high temperature, improvement of washing resistance and anti-felting performance

Inactive Publication Date: 2011-04-27
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Currently, there are two most commonly used anti-felting methods in the industry: one is the traditional chlorinated wool anti-felting process, which releases adsorbed organic halides (AOX) during the process, which is not suitable for cleaning. Production requirements
The second is the use of non-chlorine polymer methods, including oxidation (non-chlorine oxidants, biological enzymes or plasma, etc.) The problem
The sol prepared by organically modified metal alkoxide can be transformed into a transparent porous oxide with a network structure under certain conditions after solvent volatilization or heat treatment, so as to achieve a good anti-felting effect. It is a kind of A new type of wool anti-felting process, but there are defects such as high baking temperature, yellowing of the fabric and easy damage

Method used

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  • Preparation of siloxane modified polyurethane hydrolysate
  • Preparation of siloxane modified polyurethane hydrolysate
  • Preparation of siloxane modified polyurethane hydrolysate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] At room temperature, add 60 grams of polyethylene glycol (the average number-average molecular mass is 1000) and 4 grams of dimethylol propionic acid into a four-necked bottle, raise the temperature to 120 ° C, and vacuumize for 2 hours under a pressure of 650 mmHg be down to room temperature, calculate the quality of isophorone diisocyanate that needs to be dropped into by a certain molar ratio (-NCO:-OH=2: 1), and add dropwise in the four-necked bottle, under nitrogen protection, heat up to 80° C., add 0.02 g of dibutyltin laurate, continue the reaction for 1 hour, lower the reaction temperature to room temperature, and obtain a prepolymer.

[0028] The ethanol of 20.7 grams is joined in the prepolymer, according to the content of the isocyanate group in the prepolymer measured (measured by the di-n-butylamine-hydrochloric acid titration method), according to a certain molar ratio -NCO:-NH 2 =1:1, after calculating the required mass of γ-aminopropyltriethoxysilane to ...

Embodiment 2

[0031] At room temperature, add 30 grams of polycaprolactone diol (the average number-average molecular weight is 3000) and 4 grams of trimethylolpropane into a four-necked bottle, raise the temperature to 120° C., and vacuumize for 2 hours under a pressure of 600 mmHg. hour; the system was down to room temperature, and the mass of hexamethylene diisocyanate calculated by the molar ratio (-NCO:-OH=1.5:1) was 13.86 grams, which was added dropwise in a four-necked bottle, and under the protection of nitrogen, the temperature was raised to 70° C., add 0.03 g of stannous octoate, continue the reaction for 2 hours, and lower the reaction temperature to room temperature to obtain a prepolymer.

[0032] 10 grams of acetone is added in the prepolymer, dilute, according to the content of the isocyanate group in the prepolymer measured (measured by the di-n-butylamine-hydrochloric acid titration method), according to a certain molar ratio -NCO:-NH 2 =1:2, after calculating the required ...

Embodiment 3

[0035] (1) Anti-felting finish

[0036] Four samples of undyed but boiled 100% wool gabardine, (211g / m 2), wherein three samples are dipped and rolled twice in the hydrolyzate in the above-mentioned embodiment 1, and the liquid carrying rate is 70-90%. Machine, Taiwan Labor Tex Co.LTD) in 80 ° C for 3 minutes, 110 ° C, 130 ° C, 150 ° C for 3 minutes each, and naturally dry, while the other sample was not treated. The pictures of the untreated sample and the sample baked at 130°C for 3 minutes are attached figure 1 And attached figure 2 .

[0037] (2) Anti-felting effect test

[0038] After washing the four samples with reference to the Woolmark TM 31 test standard and method, using a standard washing machine (Wascator FQM71 CLS, EIECTROLUx, program 3*5A wash cycles), the change of felt shrinkage was tested.

[0039] (3) Evaluation of the physical properties of the fabric after finishing

[0040] Four samples were tested for physical properties, including breaking streng...

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Abstract

The invention relates to a preparation method of hydrolysate of siloxane-modified polyurethane, which includes the following steps: (1) polyether glycol, polyester diol or polyether-tribasic alcohol and a crosslinking agent are vacuumized, unwatered and cooled to 10 DEG C, diisocyanate of the an aromatic series or aliphatic series is dropped in the mixed system, nitrogen is pumped to cause the temperature to rise to 30 to 100 DEG C, a catalyst is added and the reaction is carried out for 0.5 to 2 hours, thus achieving polyurethane prepolymer; (2) an organic solvent and amino silane are added and reacted in the temperature of minus 10 to 70 DEG C for 0.5 to 2 hours and then a product of a precursor of the silylated polyurethane is obtained; and (3) the organic solvent and deionized water are mixed and stirred for 0.5 to 2 hours, the precursor of the silylated polyurethane is dropped, and acid is added to adjust the pH to 5 to 7 and then the stirring is carried out for 0.5 to 7 hours and then the hydrolysate of siloxane-modified polyurethane is achieved. The hydrolysate of siloxane-modified polyurethane comprises a plurality of active groups, thereby improving the washability and shrink proofing of wool textiles.

Description

technical field [0001] The invention belongs to the field of polyurethane hydrolyzate preparation, in particular to a preparation method of siloxane-modified polyurethane hydrolyzate. Background technique [0002] With the continuous improvement of people's consumption level and the acceleration of the pace of daily work, it has become an important topic in the field of textile research in the world to solve the problem of felting shrinkage in the process of washing wool fabrics as soon as possible, so as to make them machine-washable and anti-felting. . [0003] Currently, there are two most commonly used anti-felting methods in the industry: one is the traditional chlorinated wool anti-felting process, which releases adsorbed organic halides (AOX) during the process, which is not suitable for cleaning. Production requirements. The second is the use of non-chlorine polymer methods, including oxidation (non-chlorine oxidants, biological enzymes or plasma, etc.) The proble...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/458D06M15/653D06M101/12
Inventor 阎克路杨世玉胡毅谭剑
Owner DONGHUA UNIV
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