Fluorine-containing modified polysiloxane as well as preparation method and application thereof

A polysiloxane and modification technology, which is applied in the field of fluorine-containing modified polysiloxane and its preparation, can solve the problem of difficulty in controlling the viscosity, fluorine content and content of other groups of fluorosilicone oil, and the reaction is not easy to control, Solve the problem of low yield of silicone oil, and achieve the effects of easy control of the reaction, good yield and quality, and a wide range of applications

Active Publication Date: 2021-04-09
SHANDONG DONGYUE POLYMER MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many kinds of fluorosilicone oil products of different brands at home and abroad, but they are nothing more than hydrolysis and condensation reactions of trifluoropropyl dichlorosilane. When chlorosilane is directly added to water, the reaction is violent and the reaction is not easy to control. The viscosity and content of the prepared fluorosilicone oil The content of fluorine and other groups is not easy to control, the yield of the synthesized silicone oil is not high, and the quality varies.

Method used

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  • Fluorine-containing modified polysiloxane as well as preparation method and application thereof
  • Fluorine-containing modified polysiloxane as well as preparation method and application thereof
  • Fluorine-containing modified polysiloxane as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Dissolve 328g (0.5mol) of fluorine-containing dichlorosilane and 64.5g (0.5mol) of dimethyldichlorosilane in 200ml of trifluorotrichloroethane, add dropwise to 500ml of deionized water and hydrolyze at 60°C for 1.5h , followed by neutralization, filtration, drying, removal of solvent at 50mmHg, 50°C to obtain 294g (CH 3 )(R f )-SiO 2 / 2 :(CH 3 ) 2 SiO 2 / 2 =1:1 fluorinated hydrolyzed copolymer.

[0028] (2) Then add 12.48g (3.63×10 -2 mol) tetravinylcyclotetrasiloxane, 33g (0.1089mol) octamethylcyclotetrasiloxane, 0.236g (1.452×10 -3 ) hexamethyldisiloxane, followed by adding catalyst 0.5part perfluorosulfonic acid resin and reacting at 90°C for 8 hours. After the reaction was completed, the sulfonic acid resin was filtered off, decolorized, and 327g product was obtained by devolatilization at 140°C / 5mmHg for 25min. Viscosity 587mm 2 / s, the product has the following molecular formula:

[0029] (Me 3 SiO 1 / 2 ) 1.85 (HOME 2 SiO 1 / 2 ) 0.15 (CH 3 R f SiO...

Embodiment 2

[0031] (1) Dissolve 328g (0.5mol) of fluorine-containing dichlorosilane and 64.5g (0.5mol) of dimethyldichlorosilane in 200ml of trifluorotrichloroethane, add dropwise to 500ml of deionized water and hydrolyze at 60°C for 1.5h , followed by neutralization, filtration, drying, removal of solvent at 50mmHg, 50°C to obtain 292g (CH 3 )(R f )-SiO 2 / 2 :(CH 3 ) 2 SiO 2 / 2 =1:1 fluorinated hydrolyzed copolymer.

[0032] (2) Then add 12.40g (3.61×10 -2 mol) tetravinylcyclotetrasiloxane, 32g (0.1081mol) octamethylcyclotetrasiloxane, 0.268g (1.442×10 -3 ) divinyltetramethyldisiloxane, then add catalyst 0.5part perfluorosulfonic acid resin and react at 90°C for 8 hours, after the reaction is completed, filter out the sulfonic acid resin, decolorize, and devolatilize at 140°C / 5mmHg for 25min to obtain Product, viscosity 585mm 2 / s, the product has the following molecular formula:

[0033] (Me 2 ViSiO 1 / 2 ) 1.87 (HOME2 SiO 1 / 2 ) 0.13 (CH 3 R f SiO) 305 (Me 2 SiO) 593 (MeV...

Embodiment 3

[0035] (1) Dissolve 32.8g (0.05mol) of fluorine-containing dichlorosilane and 6.45g (0.05mol) of dimethyldichlorosilane in 20ml of trifluorotrichloroethane, add dropwise to 50ml of deionized water and hydrolyze at 60°C for 1.5 h, followed by neutralization, filtration, drying, removal of solvent at 50mmHg, 50°C to obtain 29.5g (CH 3 )(R f )-SiO 2 / 2 :(CH 3 ) 2 SiO 2 / 2 =1:1 fluorinated hydrolyzed copolymer.

[0036] (2) Then add 1.31g (5.47×10 -3 mol) Tetramethylcyclotetrasiloxane, 0.17g (1.093×10 -3 ) hexamethyldisiloxane, then add catalyst 0.5part perfluorosulfonic acid resin, react at 120°C for 4h, filter out the sulfonic acid resin after the reaction, decolorize, and devolatilize at 140°C / 5mmHg for 20min to obtain the product, Viscosity 125mm 2 / s, the product has the following molecular formula:

[0037] (Me 3 SiO 1 / 2 ) 1.95 (HOME 2 SiO 1 / 2 ) 0.05 (CH 3 R f SiO) 42 (Me 2 SiO) 41 (MeHSiO) 20 .

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Abstract

The invention belongs to the technical field of organic silicon, and particularly relates to fluorine-containing modified polysiloxane as well as a preparation method and application thereof. The method comprises the following steps: preparing a co-hydrolysate from dichlorosilane and fluorine-containing methyl dichlorosilane according to a molar ratio of (1-3): 1; supplementing a catalyst, an end-capping reagent and siloxane containing other functional groups, and conducting reacting for 2-12 h at a temperature of 60-140 DEG C; and after the reaction is finished, conducting evaporating under reduced pressure to remove unreacted substances so as to obtain the fluorine-containing modified polysiloxane. According to the method, viscosity, a fluorine content and the content of other groups can be well controlled, and silicone oil has high yield and quality. The fluorine-containing polysiloxane has good application prospects in the fields of lubricants, mold lubricants, release agents, hard coating antifouling and the like.

Description

technical field [0001] The invention belongs to the technical field of organosilicon, and in particular relates to a fluorine-containing modified polysiloxane, a preparation method and application thereof. Background technique [0002] Polysiloxane is a kind of polymer with repeated Si-O bonds as the main chain and organic groups directly connected to silicon atoms. It has the characteristics of both organic polymers and inorganic polymers. There are many varieties of organosilicon compounds with excellent performance, and they have become one of the fastest-growing varieties of new chemical materials. Among them, fluorine-containing modified silicone oil, because the introduction of fluorine segment not only has the basic characteristics of methyl silicone oil, but also has excellent oil resistance, chemical stability, solvent resistance, chemical resistance, etc., many properties are better than dimethyl silicone oil , Widely used as lubricant, paint additive, release age...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/24C08G77/20C08G77/12C08G77/06C08G77/26C09D183/08C09D5/16C10M155/02C10N30/02
CPCC08G77/24C08G77/20C08G77/12C08G77/06C08G77/26C09D183/08C09D5/1675C10M155/02C10M2229/041C10M2229/042
Inventor 史大阔顾廷海刘健冯威张永明
Owner SHANDONG DONGYUE POLYMER MATERIAL
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