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Method for preparing fluorine-containing acrylate copolymer textile finishing agent

A fabric finishing agent, acrylate technology, applied in fiber treatment, textiles and papermaking, etc., can solve the problems of the decline of water and oil repellency of copolymers, the increase of surface energy, the decrease of receding dynamic contact angle, etc., to achieve excellent water and oil repellency. performance effect

Active Publication Date: 2011-04-06
江苏梅兰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the reduction of the length of the perfluoroalkyl chain, the receding dynamic contact angle decreases and the surface energy increases, which reduces the water and oil repellency of the obtained copolymer.

Method used

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  • Method for preparing fluorine-containing acrylate copolymer textile finishing agent
  • Method for preparing fluorine-containing acrylate copolymer textile finishing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Preparation of perfluorobutyryloxyethyl acrylate

[0033] 13.19 g (0.114 mol) of hydroxyethyl acrylate, 9.57 g of pyridine, 65.95 g of dichloromethane and 0.013 g of phenothiazine were added to the flask with condenser. After cooling and keeping the temperature in the flask at 5°C, 22.15 g (0.095 mol) of perfluorobutyryl chloride was added dropwise. After the dropwise addition, it was stirred for another 30 minutes, then heated to 30° C. and stirred and refluxed for 2 hours. Then the mother liquor is poured into ice water, washed with ice water until the organic phase is neutral to obtain the crude product (a fluorine-containing acrylate dichloromethane solution containing a small amount of pyridine), which is subjected to vacuum distillation to obtain 25.62g perfluorobutyl acrylate Acyloxyethyl ester CF 3 CF 2 CF 2 COOCH 2 CH 2 OOCCH=CH 2 , yield 86.4%.

Embodiment 2

[0035] Preparation of perfluorocaproyloxyethyl methacrylate

[0036] Add 16.42g (0.126mol) of hydroxyethyl methacrylate, 15.38g of triethylamine, 42.84g of diethyl ether and 0.016g of phenothiazine into a flask with a condenser. Cool and keep the temperature in the flask at 0°C, and start dropping 35.64 g (0.107 mol) of perfluorohexanoyl chloride. After the dropwise addition, stir again for 1 h, raise the temperature to 40° C. and stir and reflux for 3 h. Then the mother liquor was poured into ice water, washed with ice water until the organic phase was neutral, and the crude product was obtained. After vacuum distillation, 35.58 g of perfluorocaproyloxyethyl methacrylate CF was obtained. 3 (CF 2 ) 4 COOCH 2 CH 2 OOCC (CH 3 )=CH 2 , yield 84.6%.

Embodiment 3

[0038] Preparation of 2-trifluoromethyl-3-oxa-octafluorohexanoyloxyethyl acrylate

[0039] 16.18g (0.139mol) hydroxyethyl acrylate, 19.14g N, N-dimethylaniline and 0.016g phenothiazine dissolved in 66.33g methylene chloride were added in the flask with condenser, cooled and kept at a temperature of At -15°C, 39.11 g (0.118 mol) of 2-trifluoromethyl-3-oxa-octafluorohexanoyl fluoride was added dropwise. After the dropwise addition, stir again for 1 h, raise the temperature to 35° C. and stir and reflux for 7 h. Then the mother liquor was poured into ice water, washed with water until the organic phase was neutral, and the crude product was obtained, which was then rectified under reduced pressure to obtain 44.79g of acrylic acid 2-trifluoromethyl-3-oxa-octafluorohexanoyloxy Ethyl CF 3 CF 2 CF 2 OCF (CF 3 ) COOCH 2 CH 2 OOCCH=CH 2 , yield 88.7%.

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Abstract

The invention belongs to the technical field of fabric finishing agents, and particularly relates to a method for preparing a fluorine-containing acrylate copolymer textile finishing agent, which is characterized by sequentially comprising the following steps of: 1, preparing fluorine-containing acrylate: slowly dripping a perfluor alkyl acyl compound by using (methyl) acrylic hydroxy alkyl ester as a raw material and phenothiazine as a polymerization inhibitor in the presence of a catalyst; and 2, preparing a fluorine-containing acrylate copolymer: pre-emulsifying polymer monomer by adding an emulsifying agent, and dripping an initiator into pre-emulsion for polymerizing the emulsion under the protection of nitrogen. The fluorine-containing acrylate copolymer emulsion is used as a waterproof oil resistant finishing agent for fabrics; and the finished fabrics present excellent waterproof oil resistance property. Carbon atoms of long-chain perfluor alkyl in the fluorine-containing acrylate monomer prepared by the method are not less than 8, and hidden dangers of damaging the environment and harming human health by the long-chain perfluor alkyl waterproof oil resistant fabric finishing agent do not exist.

Description

technical field [0001] The invention belongs to the technical field of fabric finishing agents, and relates to a waterproof and oil-repellent fabric finishing agent and a preparation method thereof, in particular to a preparation method of a waterproof and oil-repellent fluorine-containing acrylate copolymer. Background technique [0002] At present, with the development of textiles at home and abroad and the needs of people's lives, people are increasingly calling for the development of new and efficient fabric finishing agents. [0003] Organic fluorine fabric finishing agent has excellent hydrophobic and oleophobic properties, and at the same time, due to the large electronegativity and small diameter of its F atom, it can shield the C-F bond. It shows high stability in various environments. In addition, because of its low concentration and high effect, the treated fabric maintains a good hand feeling, excellent air permeability and moisture permeability. Compared with ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/24C08F220/18C08F2/30C08F2/28D06M15/277
Inventor 刘红阳徐荣归钱厚琴
Owner 江苏梅兰化工有限公司
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