Process for preparing full-fluorine group end capping siloxane oligomer for hard surface finish and uses thereof

A technology of siloxane oligomer and perfluoroalkyl peroxide, applied in the production field of siloxane oligomer, can solve the problems of low yield and the like, achieve low temperature, low requirements on equipment material, and low reaction rate. short time effect

Inactive Publication Date: 2009-01-14
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

but lower yield

Method used

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  • Process for preparing full-fluorine group end capping siloxane oligomer for hard surface finish and uses thereof
  • Process for preparing full-fluorine group end capping siloxane oligomer for hard surface finish and uses thereof
  • Process for preparing full-fluorine group end capping siloxane oligomer for hard surface finish and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 0.0107 mol of vinyltriethoxysilane and 200 ml of perfluorobutyl ethyl ether to a 250 ml three-necked bottle, slowly add 0.0107 mol of perfluorodioctyl peroxide dropwise at 40°C under nitrogen Tetrafluoropropyl methyl ether solution, iodometric method to track the reaction of peroxide. After 5 hours, perfluorodioctyl peroxide disappeared, and the reaction ended. Perfluorobutyl ethyl ether was distilled off to obtain a perfluorooctyl-terminated triethoxysilane oligomer. Gas chromatography showed a conversion of vinyltriethoxysilane of 74%.

Embodiment 2

[0027] Add 0.0214 mol of vinyltriethoxysilane and 200 ml of tetrafluoropropyl methyl ether to a 250 ml three-necked bottle, slowly add 0.0107 mol of perfluorodioctyl peroxide dropwise at 50°C under nitrogen Tetrafluoropropyl methyl ether solution, iodometric method to track the reaction of peroxide. After 5 hours, perfluorodioctyl peroxide disappeared, and the reaction ended. Tetrafluoropropyl methyl ether was distilled off to obtain a perfluorooctyl-terminated triethoxysilane oligomer. Gas chromatography showed a conversion of vinyltriethoxysilane of 74%.

Embodiment 3

[0029] Into a 250ml three-neck flask, add 0.043mol of vinyltripropoxysilane and 200ml of tetrafluoropropyl difluoromethyl ether, and slowly add 0.0107mol of perfluoroperoxide at 60°C under argon. Dioctyl tetrafluoropropyl difluoromethyl ether solution, iodometric method to follow the reaction of peroxide. After 6 hours, perfluorodioctyl peroxide disappeared, and the reaction ended. Tetrafluoropropyl difluoromethyl ether was distilled off to obtain a perfluorooctyl-terminated tripropoxysilane oligomer. Gas chromatography showed that the conversion of vinyltripropoxysilane was 71%.

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Abstract

The invention relates to a synthesizing method of poly fluoro-alkyl silanes used to finish the hard surface, in particular to a production method of siloxane oligomer of the blocking of a perfluoro group used to finish the hard surface. The procedures are as follows: perfluoroalkyl group peroxide and siloxane that contains unsaturated double bond are added into the container; a fluorine containing compound which does not consume the oxygen barrier layer is used as a solvent; in the inert atmosphere, radical addition reaction is generated under minus 10 to 70 DEG C, and the reaction time is 5 to 6 hours; then the redundant perfluoroalkyl group peroxide is steamed away, and the needed product is obtained; and the molar ratio is 1: 1 to 1: 20 of the perfluoroalkyl group peroxide to the siloxane that contains unsaturated double bond. With the synthesizing method, the prepared siloxane oligomer of the blocking of the perfluoro group has perfect selectivity and conversion rate and stable performance, and thus can be used to finish the hard surface. The process of the synthesizing method is simple, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing polyfluorosilane for hard surface finishing, in particular to a method for producing perfluorogroup-terminated siloxane oligomers for hard surface finishing. Background technique [0002] Fluorosilicone is the product of organosiloxane modified by fluoroaliphatic compounds, also known as fluorosilicone finishing agent, which is another type of water and oil repellent with good effect after many functional silicone finishing agents. It is a type of surface finishing additive with the comprehensive properties of fluorine and silicon materials. Surface finishes can generally be divided into soft surface finishes and hard surface finishes. Fluorosilicone hard surface finishing agent is to introduce fluorine-containing groups on the main chain of silicone oligomers through the reaction of fluorine-containing silicon functional group monomers or other methods to form a water-repellent and oil-repellent nano...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 杨勇王珲王真陈秉堄
Owner TONGJI UNIV
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