Synthesis of photo-cured fluorosilicone polymer and preparation method of photo-cured fluorosilicone polymer coating

A fluorosilicon polymer, light curing technology, used in coatings, polyurea/polyurethane coatings, epoxy resin coatings, etc.

Active Publication Date: 2014-07-23
江苏矽时代材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the defects and technical deficiencies in the existing preparation of photocurable fluorine-containing polysiloxane, and to provide a photocurable photocurable polysiloxane with simple synthesis, excellent performance, less pollution, energy saving, stable storage and practical value. Cured fluorosilicone polymer and preparation method of coating thereof

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] 1. Synthesis of dimethyl-methylhydrogen siloxane copolymer:

[0076] S1. According to parts by mass, 100 parts of D 4 , 2 copies of MM and 50 copies of D 4 H was added in the reaction kettle, slowly added 7 parts by mass of concentrated sulfuric acid at room temperature, after the reaction was balanced for 6 hours, the layers were statically separated, and the acidic water layer was removed;

[0077] S2. Na for oil layer 2 CO 3 Neutralize for 30 minutes;

[0078] S3. Collect the target product Me after filtration 3 SiO(Me 2 SiO) n (MeHSiO) m SiMe 3 , and the yield reached 97.4% (parts by mass).

[0079] The determination showed that the target product Me 3 SiO(Me 2 SiO) n (MeHSiO) m SiMe 3 The hydrogen content (mass fraction) is 0.38%~0.45%, and the product viscosity is 18mm 2 / s

[0080] 2. Synthesize light-cured fluorosilicone rubber raw rubber, the steps are as follows:

[0081] S1. Under the protection of nitrogen, slowly drop 46.1g of 0.1mol perflu...

Embodiment 2

[0093] 1. Synthesis of polymethylhydrogen siloxane:

[0094] S1. According to parts by mass, 100 parts of D 4 , 3 copies of MM and 30 copies of D 4 H was added to the reaction kettle, and 5 parts by mass of concentrated sulfuric acid was slowly added at room temperature. After the reaction was balanced for 6 hours, the layers were statically separated, and the acidic water layer was removed;

[0095] S2. Na for oil layer 2 CO 3 Neutralize for 30 minutes;

[0096] S3. Collect the target product Me after filtration 3 SiO(Me 2 SiO) n (MeHSiO) m SiMe 3 , and the yield reached 94.3% (parts by mass).

[0097] The determination showed that the target product Me 3 SiO(Me 2 SiO) n (MeHSiO) m SiMe 3 The hydrogen content (mass fraction) is 0.24%~0.31%, and the product viscosity is 30mm 2 / s

[0098] 2. Synthesis of photocurable fluorosilicone polymer, the steps are as follows:

[0099] S1. Under nitrogen protection, slowly drop 34.6g of 0.1mol perfluorohexylethylene and 50...

Embodiment 3

[0111] 1. Synthesis of polymethylhydrogen siloxane:

[0112] S1. According to parts by mass, 100 parts of D 4 , 0.5 MM and 60 D 4 H was added in the reaction kettle, and 4 parts by mass of concentrated sulfuric acid was slowly added at room temperature. After the reaction was balanced for 6 hours, the layers were statically separated, and the acidic water layer was removed;

[0113] S2. Na for oil layer 2 CO 3 Neutralize for 30 minutes;

[0114] S3. Collect the target product Me after filtration 3 SiO(Me 2 SiO) n (MeHSiO) m SiMe 3 , and the yield reached 92.7% (parts by mass).

[0115] The determination showed that the target product Me 3 SiO(Me 2 SiO) n (MeHSiO) m SiMe 3 The hydrogen content (mass fraction) is 0.5%~0.6%, and the product viscosity is 112mm 2 / s

[0116] 2. Synthesis of photocurable fluorosilicone polymer, the steps are as follows:

[0117] S1. Under nitrogen protection, slowly add 43.2g, 0.1mol trifluorooctyl methacrylate and 50ppm chloroplati...

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Abstract

The invention discloses a preparation method of a photo-cured fluorosilicone polymer. The photo-cured fluorosilicone polymer is a fluorosilicone polymer with light sensitivity, which is prepared by respective hydrosilylation of hydrogen-containing polysiloxane with fluorine-containing olefins and an olefin bifunctional reactive diluent. The photo-cured fluorosilicone polymer is used for preparing a photo-cured fluorosilicone composite coating. The structural formula of the photo-cured fluorosilicone polymer is shown in a formula (I) in the specification, wherein Rf is a fluorine-containing group, R is an alkylene-containing light sensitive group, x is 10-100, y is 10-30, z is 5-20, x accounts for 60-80% of the total quantity, and y+z accounts for 20-40% of the total quantity. The fluorine-containing group and the light-cured active group are introduced to side chains of the polysiloxane through hydrosilylation. Compared with a polycondensation method, the preparation method is relatively simple and has relatively high yield. After the synthesized light sensitive fluorosilicone polymer is fully mixed with a reactive diluent, a plasticizer, stuffing, a photoinitiator and the like, the fluorosilicone coating is formed by curing in ultraviolet light; the fluorosilicone coating has excellent performances such as high-temperature resistance, hydrophobicity and oleophobicity, antifouling property and weather resistance and can be applied to the fields of high and new technologies such as electronics and electrics, chemical engineering, automobiles and the like.

Description

technical field [0001] The invention belongs to the field of photocurable silicone. More specifically, it relates to a photocurable fluorine-containing polysiloxane and a preparation method thereof. Background technique [0002] In recent years, many UV-curable silicone polymers have been developed one after another. The side groups (or end groups) of the polysiloxane molecular chain are replaced by groups that can be crosslinked under the action of light curing agents such as acrylic acid and polyurethane acrylic acid. , under the action of visible light or ultraviolet light, it can be vulcanized at room temperature and can be applied in the fields of coatings, leather (fiber) coating agents, sealants, etc., and has received widespread attention because of its simple operation, high efficiency and environmental protection, and excellent performance. [0003] Organosilicon polymer coatings have excellent properties such as high and low temperature resistance, weather resist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/385C08G77/12C08G77/06C09D183/08C09D175/14C09D163/10C09D133/04C09D7/12
Inventor 张创
Owner 江苏矽时代材料科技有限公司
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