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Method for preparing gamma-(2,3-epoxypropoxy)propyltriethoxysilicane

A technology of propyltriethoxysilane and glycidyl oxide, which is applied in the field of synthesis of fine chemicals, can solve the problems of complex catalyst preparation, complex reaction operation, and long reaction time, and achieve easy separation and purification, simple preparation, highly selective effect

Active Publication Date: 2008-02-13
湖北武大有机硅新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In foreign countries, the zero-valent Pt complex of divinyltetramethyldisiloxane is dissolved in N-dimethylsilane-N-methylacetamide and toluene solution as a catalyst to synthesize γ-(2,3-epoxy Propoxy)propyltriethoxysilane, its molar yield is 87%, prepared in argon, experienced sealing, pumping, ventilation, etc., the reaction operation is complicated, and the yield is not high
In addition, the platinum complex of polyγ-methylselenopropyl triethoxysilane is used as a catalyst, and the yield is only 78%; there is also Pt loaded on styrene-divinylbenzene copolymer or activated carbon as a catalyst. Catalyst, but the reaction time is long and the catalyst preparation is complicated

Method used

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  • Method for preparing gamma-(2,3-epoxypropoxy)propyltriethoxysilicane

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preparation example Construction

[0010] A. Preparation of efficient catalyst: with chloroplatinic acid (H 2 PtCl 6 ·6H 2 O) and isopropanol as raw materials, add acid-binding agent, stir and heat to 55-70°C, add complexing agent, stir and heat to 90-100°C for 2 hours, cool to 30-50°C to obtain high-efficiency catalyst . Chloroplatinic acid (H 2 PtCl 6 ·6H 2 O), isopropanol is the mass percent ratio of raw material, acid-binding agent and complexing agent is: 1.5~3: 20~30: 60~80: 3~6.

[0011] Described acid-binding agent is ethers, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol diethyl ether, 1,2-epoxyhexane, 1,2-cyclo Oxyoctane, 1,4-dioxane, butyl ether, anisole, phenetole, ethylene glycol phenyl ether, diethylene glycol dimethyl ether, diethylene glycol butyl ether, terephthalene, One of methyl tert-butyl ether, diethylene glycol butyl ether and allyl glycidyl ether;

[0012] The complexing agent is cyclooctadiene, triphenylphosphi...

Embodiment 1

[0017] Preparation of high-efficiency catalyst: add 0.2gH to a 20ml round flask with magnetic 2 PtCl 6 ·6H 2 O, 2.7g (3.5ml) isopropanol, 7g (7ml) glycidyl ether, stir and heat to 58°C with a magnetic stirrer, add 0.4g triphenylphosphine, stir and heat to 93°C for 2 hours, cool to 30~ High-efficiency catalysts can be obtained at 50°C.

Embodiment 2

[0019] Preparation of high-efficiency catalyst: add 0.2gH to a 20ml round flask with magnetic 2 PtCl 6 ·6H 2 O, 2.9g (3.7ml) isopropanol, 6.8g (6.2ml) ethylene glycol phenyl ether, stirred and heated to 60°C with a magnetic stirrer, added 0.6ml acetylacetone, stirred and heated to 96°C for 2 hours, cooled to High-efficiency catalysts can be obtained at 30-50°C.

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Abstract

The invention discloses a preparation method of gamma-(2,3-glycidoxy)propyltriethoxysilane. Glycidyl ether is used as reactant, absolute ethanol is used as solvent, high-efficiency catalyst is added, under heating and stirring, triethoxysilane is added dropwise at a certain temperature, after dropping, react at a certain temperature for a certain period of time, and then cool down. After distilling out the solvent ethanol under normal pressure, distill under reduced pressure to obtain the front fraction at a certain temperature, and obtain a colorless transparent liquid at a certain temperature as the product. In the present invention, the high-efficiency catalyst is prepared by using chloroplatinic acid (H2PtCl6·6H2O) and isopropanol as raw materials, adding an acid-binding agent and a complexing agent. The preparation method is simple, the selectivity is good, the efficiency is high, and the molar action number is 100,000 to 180,000. ; The synthetic reaction time is short, the operation is convenient, and the reaction yield is high; the molar yield reaches 90-93%, the product content reaches 99%, and the product quality is high.

Description

technical field [0001] The invention belongs to the synthesis of fine chemicals, and more specifically relates to a preparation method of gamma-(2,3-glycidoxy)propyltriethoxysilane. Background technique [0002] γ-(2,3-Glycidoxypropoxy)propyltriethoxysilane is a widely used silane coupling agent, widely used in epoxy resin, phenolic resin, polyurethane, melamine resin, chlorinated polyether, Polymer materials such as polyester, polycarbonate, polystyrene and nylon to improve their bonding performance; synthetic epoxy hydrocarbon-based silicone oil, widely used as fabric softening agent, organic resin modifier and polishing modifier; It can also be used as a tackifier for room temperature vulcanized silicone rubber to improve the bonding performance of silicone rubber to glass and aluminum alloy materials. [0003] There is no report on the preparation of this product in China. In foreign countries, the zero-valent Pt complex of divinyltetramethyldisiloxane is dissolved in ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 廖俊张治民刘巧云董鹏何运凡陈圣云程鹏飞杨金玉高胜波丁强张先亮
Owner 湖北武大有机硅新材料股份有限公司