Process for preparing allyltriethoxysilicane

Abstract

The present invention provides a preparation method of allyl triethoxysilane. The material comprise : tetrahydrofuran accounting for effective dimension 20-40% of reaction container, 0.7-1mol magnesium, 0.9-1.3mol chloropropene and 0.7-1mol triethoxyhydrosilicon. adding 8-10% mixture of tetrahydrofuran, magnesium, chloropropene and triethoxyhydrosilicon in reaction container, adding the other chloropropene and triethoxyhydrosilicon mixture in dripping funnel, stirring, heating for inspiring reaction, controlling reaction temperature at 60-70 degree, opening dripping funnel when reaction being stable, dropping chloropropene and triethoxyhydrosilicon mixture in reaction kettle, then heating the reaction kettle to keep it at microboiling state 3-4 hours, reducing the temperature, removing solid salt from the solution, Distilling filtrate, and collecting distillate of 160-165 degree i.e. allyl triethoxysilane. The synthesis reaction can accomplish in one step and yield can amount to 50%.

Description

(1) Technical field [0001] The present invention relates to a method for preparing organic compounds, in particular to a method for preparing allyltriethoxysilane. (2) Background technology [0002] Allyltriethoxysilane is one of many organosilane coupling agents, it is widely used, suitable for unsaturated polyester, acrylic resin, also used for vulcanized rubber modifier, glass fiber treatment agent, high density poly Ethylene crosslinking agent, etc. Allyl trioxysilane itself has a unique performance, which can be used for the bonding of fluororubber, fluorosilicone rubber and other hard materials such as metal. The special performance of this product cannot be replaced by other materials, and it solves the application problem that fluororubber and fluorosilicone rubber with excellent performance are difficult to bond. [0003] But there is no synthesis research and application report of this kind of silane coupling agent in China at present. It is known from the liter...

AI Technical Summary

Problems solved by technology

[0003] But there is no synthetic research and application report of this kind of silane coupling agent in China at present.

It is known from the literature that scientists in the former Soviet Union used the Grignard reagent method in the laboratory research. The reaction is a two-step method. First, the Grignard reagent is synthesized from allyl chloride and metal magnesium in a specific solvent. The separated Grignard reagent is combined with Ethyl orthosilicate carries out molecular group exchange to obtain allyl triethoxysilane, and the product yield is 30%. American scientists adopt a thermal shrinkage method, and the raw materials used in the thermal shrinkage method are chloropropene, trichlorosilane, and ethanol. The reaction principle is that chloropropene and trichlorosilane react at high temperature (above 600°C) to form allyl trichlorosilane, which is then esterified with ethanol to form allyl triethoxy Silane, because the two-step reaction has hydrogen chloride gas to generate, it will pollute the environment, and then the thermal condensation reaction temperature is higher, and the C=C double bond of the synthetic raw material chloropropene is very easy to break at high temperature, so the synthetic yield of this method Very low, product yield is only 10-20%

Moreover, the thermal condensation reaction generates a large amount of hydrogen chloride gas, which will pollute the environment and corrode the production equipment.