Preparation method of bis (N-methylbenzamide) ethoxymethylsilane

A technology of ethoxymethylsilane and methylbenzamide is applied in the field of preparation of diethoxymethylsilane, can solve the problems of difficult separation and purification, high production energy consumption, low production energy consumption and the like, and achieves atomic The effect of high utilization rate, low production energy consumption and three wastes

Pending Publication Date: 2021-12-07
ZHEJIANG QUZHOU GUIBAO CHEM
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Problems solved by technology

[0008] The present invention aims to overcome the shortcomings of the existing bis(N-methylbenzamide)ethoxymethylsilane preparation method with many by-products, low yield, difficult separation and purification, and high production energy consumption, and provides a by-product The preparation method of a kind of bis(N-methylbenzamide) ethoxymethylsilane with low production rate, high yield, easy separation and purification, and low production energy consumption

Method used

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  • Preparation method of bis (N-methylbenzamide) ethoxymethylsilane
  • Preparation method of bis (N-methylbenzamide) ethoxymethylsilane

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preparation example Construction

[0026] A kind of preparation method of two (N-methylbenzamide) ethoxymethylsilane, reaction equation is as figure 1 shown, including the following steps:

[0027] A. Add N-methylbenzamide solution with 2~2.3 times the molar weight of methyl dichlorosilane into the glass-lined kettle, heat to 60~120℃, and feed 2~2.4 times the molar weight of methyl dichlorosilane Double the ammonia gas circulation, drop methyl dichlorosilane to react, react for 1~3h, and get the intermediate product bis(N-methylbenzamide) methylhydrogensilane;

[0028] B. Control the temperature in the kettle to 40~80°C, close the ammonia gas circulation, empty the tail gas, add a nickel chloride catalyst to the intermediate product system of step A, add ethanol in an equimolar amount to methyl dichlorosilane to continue the reaction, and keep Keep the pressure in the kettle constant, continue to react for 3~5h, filter the reaction solution, and vacuum distill the filtrate to separate the solvent to obtain bis...

Embodiment 1

[0030] A. Add 1000kg of N-methylbenzamide into a 3000L glass-lined kettle, add 1000L of toluene, replace the nitrogen, stir and heat to 60°C, feed 120kg of ammonia gas at a rate of 12.2kg / hr, and start the ammonia gas cycle Machine circulation, drip methyl dichlorosilane 380kg reaction with the speed of 40kg / h, dropwise complete reaction 3h, obtain intermediate product bis(N-methylbenzamide) methylhydrogensilane;

[0031] B. Control the temperature in the kettle to 50°C, turn off the ammonia gas circulation, empty the tail gas, add 100g of nickel chloride catalyst to the intermediate product system of step A, add 153kg of ethanol dropwise to continue the reaction, keep the constant pressure in the kettle, continue the reaction for 5h and then filter Reaction solution, filter residue is exported, and filtrate vacuum distillation is separated petroleum ether, obtains two (N-methylbenzamide) ethoxymethylsilanes of 1130kg, by figure 2 It can be seen that the integral ratio of pro...

Embodiment 2

[0033] A. Add 1000kg of N-methylbenzamide into a 3000L glass-lined kettle, add 1000L of 120# petroleum ether, replace nitrogen, stir and heat to 120°C, feed 120kg of ammonia gas at a speed of 12.2kg / hr, and start Ammonia circulator circulates, drips 380 kg of methyl dichlorosilane at a rate of 40 kg / h for reaction, and reacts for 1 hour after the dropwise addition to obtain the intermediate product bis(N-methylbenzamide) methylhydrogen silane;

[0034] B. Control the temperature in the kettle to 80°C, turn off the ammonia gas circulation, empty the tail gas, add 100g of nickel chloride catalyst to the intermediate product system of step A, add 153kg of ethanol dropwise to continue the reaction, keep the constant pressure in the kettle, continue the reaction for 3 hours and then filter The reaction solution and the filter residue were transported outside, and the filtrate was vacuum distilled to separate petroleum ether to obtain 1135 kg of bis(N-methylbenzamide)ethoxymethylsila...

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Abstract

The invention relates to the technical field of silane cross-linking agents, and provides a preparation method of bis (N-methylbenzamide) ethoxymethylsilane in order to overcome the defects that an existing preparation method of bis (N-methylbenzamide) ethoxymethylsilane is large in byproduct number, low in yield, not prone to separation and purification and high in production energy consumption. Methyl dichlorosilane is used as an initial raw material, bis (N-methyl benzamide) ethyoxyl methylsilane is obtained through a one-pot reaction with N-methyl benzamide and ethyl alcohol, the obtained bis (N-methyl benzamide) ethyoxyl methylsilane is high in purity and yield, easy to separate and purify and low in production energy consumption, the obtained ammonium salt can be recycled, few three wastes are generated, and the atom utilization rate is high.

Description

technical field [0001] The invention relates to the technical field of silane crosslinking agents, in particular to a preparation method of bis(N-methylbenzamide)ethoxymethylsilane. Background technique [0002] Room temperature vulcanized silicone rubber is a high-tech material. The most notable feature of this rubber is that it can be cured without heating at room temperature, and it is extremely convenient to use. Therefore, as soon as it came out, it quickly became an important part of the entire silicone product, and has been widely used in construction, decoration, automobile, electronics, solar energy and other industries, and its new uses are constantly being developed. There are several systems for RTV silicone rubber. The common ones are deketoxime type system with ketoximosilane as crosslinking agent, deacidification type system with acyloxysilane as crosslinking agent, dealcoholization type system with alkoxysilane as crosslinking agent, and Isopropenyloxysilan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10
CPCC07F7/10Y02P20/584
Inventor 王伟李冲合徐建清陈嘉华金涵
Owner ZHEJIANG QUZHOU GUIBAO CHEM
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