Hydroxy group and epoxide group co-terminated linear polysiloxane preparation technology

A polysiloxane, preparation technology, applied in the direction of textiles, papermaking, fiber treatment, etc., can solve the problems of breaking emulsion sticky roll, non-hydrophilic, epoxy-based silicone oil semi-hydrophilic, etc., to speed up water absorption, improve Soft and slippery properties of fabrics, the effect of improving hydrophilicity and smoothness

Inactive Publication Date: 2019-06-18
TANGSHAN SANYOU SILICON IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation process of linear polysiloxane co-terminated with hydroxyl and epoxy groups, which solves the problems of yellowing, non-hydrophilic and emulsion-breaking sticky rolls of epoxy-terminated silicone oil in the traditional process, and also solves the problem of Patented (201810007597.0) the problem of semi-hydrophilic epoxy silicone oil

Method used

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  • Hydroxy group and epoxide group co-terminated linear polysiloxane preparation technology

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add DMC into the reaction kettle and raise the temperature to 80-85°C, add tetramethylammonium hydroxide solid catalyst under the protection of nitrogen, catalyze the polymerization for 10 minutes, the viscosity of the material in the kettle is 300000cs; raise the temperature to 110°C, add a certain amount under the protection of nitrogen The amount of water added is 0.03% of the DMC mass for the first degradation, the equilibrium reaction is 1h, and the viscosity drops to 80000cs; then add 1,3-bis(3-glycidylpropyl)-1,1,3,3- Tetramethyldisiloxane was degraded for the second time, the addition amount was 1.8% of the DMC mass, the equilibrium reaction was 4h, the viscosity dropped to 1800cs; the temperature was raised to 140°C to decompose the catalyst, and the gas discharged from the exhaust port of the reactor was detected to be neutral Finally, turn on the vacuum pump, the vacuum degree is -0.095-0.01MPa to remove low-boiling volatile substances, and obtain a linear pol...

Embodiment 2

[0023] Add DMC into the reaction kettle and raise the temperature to 80-85°C, add tetramethylammonium hydroxide solid catalyst under the protection of nitrogen, catalyze the polymerization for 30 minutes, the viscosity of the material in the kettle is 380000cs; raise the temperature to 110°C, add a certain amount under the protection of nitrogen The amount of water added is 0.15% of the DMC mass for the first degradation, the equilibrium reaction is 1h, and the viscosity drops to 40000cs; then add 1,3-bis(3-glycidylpropyl)-1,1,3,3- Tetramethyldisiloxane was degraded for the second time, the addition amount was 2.5% of the mass of DMC, the equilibrium reaction was 4h, and the viscosity dropped to 970cs; the temperature was raised to 140°C to decompose the catalyst, and the gas discharged from the exhaust port of the reactor was detected to be neutral Finally, turn on the vacuum pump, and the vacuum degree is -0.095-0.01MPa to remove low-boiling volatile substances, and obtain a ...

Embodiment 3

[0025] Add DMC into the reaction kettle and raise the temperature to 80-85°C, add tetramethylammonium hydroxide alkali gel catalyst under the protection of nitrogen, catalyze the polymerization for 10 minutes, and the viscosity of the material in the kettle is 350000cs; raise the temperature to 110°C, add some The amount of water added is 0.03% of the DMC mass for the first degradation, the equilibrium reaction is 1h, and the viscosity drops to 91000cs; then add 1,3-bis(3-glycidylpropyl)-1,1,3,3 -Tetramethyldisiloxane is degraded for the second time, the addition amount is 1.8% of the DMC mass, the equilibrium reaction is 4h, and the viscosity drops to 1560cs; the temperature is raised to 140°C to decompose the catalyst, and the gas discharged from the exhaust port of the reactor is detected to be medium After curing, turn on the vacuum pump with a vacuum degree of -0.095-0.01MPa to remove low-boiling volatile substances, and obtain a linear polysiloxane product co-terminated w...

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Abstract

The invention belongs to the field of fine chemistry, and relates to hydroxy group and epoxide group co-terminated linear polysiloxane preparation technology. The hydroxy group and epoxide group co-terminated linear polysiloxane preparation technology comprises followingsteps: DMC is introduced into a polymerization reaction vessel for heating to 80 to 85 DEG C; at nitrogen gas protection, a catalyst is added for ring-opening polymerization reaction; polymerization reaction is carried out until the viscosity reaches 200000 to 400000cs, and water is introduced into the reaction vessel for end capping degradation, wherein the mass amount of added water accounts for 0.03 to 0.5% of DMC; 1,3-bis(3-glycidoxypropyl)-1,1,3,3-tetramethyldisiloxane is introduced into the reaction vessel for epoxy end capping degradation; after end capping degradation, heating is carried out for catalyst degradation, vacuum removing of low boiling point volatile substances is carried out so as to obtain the hydroxy group and epoxide group co-terminated linear polysiloxane product.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, is mainly used in fabric finishing, and relates to a preparation process of linear polysiloxane co-terminated by hydroxyl and epoxy groups. Background technique [0002] With the wide application of fabric finishing agents, some problems have also been exposed, such as: the yellowing of traditional fabric finishing agents during use, the three major shortcomings of non-hydrophilicity and demulsification sticking to rollers. After analysis, these problems In terms of the preparation process of the main epoxy-terminated silicone oil, there are currently two main synthetic routes in China: 1. Grafting of terminal hydrogen-containing silicone oil and allyl glycidyl ether; 2. Grafting of terminal hydrogen-containing silicone oil and allyl glycidyl ether; These two methods are all prepared by hydrosilylation method, and the above-mentioned problems often occur during use. In order to solve the ab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/06C08G77/04D06M15/65
Inventor 陈春江孙长江刘彬赵磊赵洁曹鹤李献起刘秋艳曲雪丽任海涛周健张鹏硕严锦河王红娜王健江华郑颖郭文涛胡质云李双玲倪志远胡志国
Owner TANGSHAN SANYOU SILICON IND
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