A kind of preparation method of methyl tributylketoxime base silane

A technology of methyl tributyl ketone oxime and methyl trimethoxysilane, which is applied in the field of preparation of methyl tributyl ketone oxime silane, can solve the problems that the process cannot be carried out continuously, easy to produce filter residue, unsafe process, etc., and achieves Easy to separate and purify, increase product yield, optimize process effect

Active Publication Date: 2018-08-10
JINGZHOU JIANGHAN FINE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to: provide a simple process, non-toxic, environmentally friendly, suitable for large-scale production, to solve the problems that the existing process cannot be carried out continuously, the output is small, and the efficiency is low; The preparation method of methyl tributylketoxime base silane

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  • A kind of preparation method of methyl tributylketoxime base silane

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Experimental program
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Effect test

Embodiment 1

[0021] Put 340g of methyltrimethoxysilane, 1305g of butanone oxime and 3g of p-toluenesulfonic acid into a 2000ml three-necked reaction flask, turn on the magnetic stirring, control the magnetic stirring at 300 revolutions per minute, and adopt the temperature programming method for the reaction temperature, and the reaction temperature is controlled at 65°C-153°C, the reaction time is 6 hours, that is, the average temperature rises 14.7°C per hour. During the reaction, methanol is recovered while reacting, and a semi-finished product is obtained after the reaction. The semi-finished product recovers excess butanone oxime through vacuum distillation, washes and filters the methyl tributylketoxime silane product obtained at the bottom of the bottle, and finally obtains 737g of methyl tributylketoxime silane product, which has 10 colors. The rate reaches 97.9%, and the product content is 98.7%.

Embodiment 2

[0023] Put 340g of methyltrimethoxysilane, 1305g of butanone oxime and 2g of p-toluenesulfonic acid into a 2000ml three-necked reaction flask, turn on the magnetic stirring, control the magnetic stirring at 300 revolutions per minute, and adopt the temperature programming method for the reaction temperature, the reaction temperature is controlled at 65°C-135°C, the reaction time is 7 hours, that is, the average temperature rises by 10°C per hour. During the reaction, methanol is recovered while reacting, and a semi-finished product is obtained after the reaction. The semi-finished product recovers excess butanone oxime through vacuum distillation, washes and filters the methyl tributylketoxime silane product obtained at the bottom of the bottle, and finally obtains 730g of methyl tributylketoxime silane product, which has 10 colors. The rate reaches 97.0%, and the product content is 98.5%.

Embodiment 3

[0025] Put 340g of methyltrimethoxysilane, 1305g of butanone oxime and 3.4g of catalyst p-toluenesulfonic acid into a 2000ml three-necked reaction flask, turn on the magnetic stirring, control the magnetic stirring at 300 revolutions per minute, and adopt the temperature programming method for the reaction temperature. The temperature is controlled at 85°C-153°C, and the reaction time is 7 hours, that is, the average temperature increase is 9.7°C per hour. During the reaction, methanol is recovered while reacting, and a semi-finished product is obtained after the reaction. The semi-finished product recovers excess butanone oxime through vacuum distillation, washes and filters the methyl tributylketoxime silane product obtained at the bottom of the bottle, and finally obtains 740g of methyl tributylketoxime silane product, the product is 10 colors, and the product is collected The rate reaches 98.3%, and the product content is 99.0%.

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Abstract

The invention belongs to the technical field of fine chemistry and relates to a methyltris(methylethylketoxime)silane preparation method.Methyltrimethoxysilane, diacetylmonoxime and p-toluenesulfonic acid which serves as a catalyst react according to a certain proportion, excessive diacetylmonoxime in the reaction process serves as a solvent to make the reaction more thorough and easier, and methanol is recovered during reaction. After reaction is finished, the diacetylmonoxime which serves as the solvent is recovered by reduced pressure distillation, and the recovered diacetylmonoxime can be recycled.Products obtained by distillation are washed and filtered to obtain high-purity methyltris(methylethylketoxime)silane. The methyltris(methylethylketoxime)silane preparation method has the advantages that product yield is above 97%, product content is above 98%, materials can be recycled completely, no waste liquid is generated, and accordingly environment pollution is avoided.

Description

technical field [0001] The invention relates to a preparation method of methyl tributylketoxime silane, which belongs to the technical field of fine chemicals. Background technique [0002] Methyl tributyl ketoxime silane is mainly used as a curing agent for silica gel and an anti-skinning agent for alkyd resin coatings. The preparation method of existing methyl tributyl ketone oxime base silane is: 1, drop into butanone oxime and solvent in reactor, slowly add methyl trichlorosilane dropwise through high position tank; After dropping, continue to react for a period of time, stand still Stratification; the upper material is neutralized and the solvent is evaporated to obtain the product, and the lower material is recovered butanone oxime. 2. Put methyltrichlorosilane, butanone oxime, ammonia, and 120# solvent gasoline into the reaction kettle; filter after reacting for a period of time, and the filtrate is crude methyl tributylketoxime silane, and the filter residue is ammo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/10
CPCC07F7/0892
Inventor 刘宇王灿陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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