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A kind of preparation method of methyl vinyl bis (n-ethyl acetamido) silane

A technology of methylvinyldichlorosilane and ethylacetamido is applied in the field of preparation of methylvinyldisilane, can solve the problems of few synthesis methods, low product yield, hydrogen chloride side reaction, etc., and achieves high yield , the process is simple, the effect of mild conditions

Active Publication Date: 2022-04-29
湖北新蓝天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

However, there are very few synthetic methods of methylvinylbis(N-ethylacetamido)silane reported at present, and the prior art uses N-ethylacetamide and methylvinyldichlorosilane as raw materials to produce methylvinyl In the method of two (N-ethyl acetamido) silane, the hydrogen chloride that reaction generates can cause the generation of side reaction, makes product productive rate lower

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  • A kind of preparation method of methyl vinyl bis (n-ethyl acetamido) silane

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Effect test

Embodiment 1

[0016] 174 g of N-ethylacetamide, 2 g of pyrrole, 82.95 g of pyridine, 106.05 g of triethylamine, 100 g of toluene, 100 g of dioxane into a 1000 ml four-mouth flask, the thermometer, condensing tube, mechanical stirring device and constant pressure drip funnel were inserted in the four-mouth flask, and the flask was placed in a smart thermostatic electric heating sleeve; 141 g methyl vinyl dichlorosilane was added to the constant pressure drip funnel to open the stirring and heating device When the temperature in the flask rises to 70 degrees Celsius, the methyl vinyl dichlorosilane is added dropwise, and the drop-add temperature is maintained at 70-80 degrees Celsius, and the drop-dosing time is 2 hours; after the drop-added, the temperature is heated to 90 °C, and the heat is kept for 3 hours; it is cooled to room temperature, filtered to obtain crude products, and then distilled and purified, resulting in a content of 97% of the product 217 grams, with a yield of 89.7%.

Embodiment 2

[0018]174 g of N-ethylacetamide, 2 g of pyrrole, 80.975 g of pyridine, 108.575 g of triethylamine, 100 g of toluene, 100 g of dioxane into a 1000 ml four-mouth flask, inserted a thermometer, condensate tube, mechanical stirring device and constant pressure drip funnel in the four-mouth flask, and placed the flask in an intelligent thermostatic electric heating sleeve; 141 g methyl vinyl dichlorosilane was added to a constant pressure drip funnel to open the stirring and heating device When the temperature in the flask rises to 70 degrees Celsius, the methyl vinyl dichlorosilane is added dropwise, and the drop-add temperature is 70-80 degrees Celsius, and the drip addition time is 2 hours; after the drop-added, the temperature rises to 90 °C, and the heat is kept for 3 hours; cooled to room temperature, filtered to obtain crude products, and then distilled and purified, 216 grams of the product with a content of 97% are obtained, and the yield is 89.3%.

Embodiment 3

[0020] 174 g of N-ethylacetamide, 2 g of pyrrole, 84.925 g of pyridine, 103.525 g of triethylamine, 100 g of toluene, 100 g of dioxane into a 1000 ml four-mouth flask, inserted a thermometer, condensing tube, mechanical stirring device and constant pressure drip funnel in the four-mouth flask, and placed the flask in an intelligent thermostatic electric heating sleeve; 141 g methyl vinyl dichlorochlorosilane was added to a constant pressure drip funnel to open the stirring and heating device When the temperature in the flask rises to 70 degrees Celsius, the methyl vinyl dichlorosilane is added dropwise, and the drop-add temperature is 70-80 degrees Celsius, and the drop-dosing time is 2 hours; after the drop-added, the temperature is heated to 90 °C, and the heat is kept for 3 hours; cooled to room temperature, filtered to obtain crude products, and then distilled and purified, 211 grams of the product with a content of 97%, and the yield is 87.2%.

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Abstract

The invention discloses a method for preparing methylvinylbis(N-ethylacetamido)silane. In the method, the catalyst pyrrole and N-ethylacetamide, formaldehyde, and the molar ratio are 2:1:2.05-2.15 Add vinyl dichlorosilane and acid-binding agent into the organic solvent to obtain solution A; then slowly add methyl vinyl dichlorosilane to solution A at 70-80°C under stirring conditions, and wait until methyl vinyl dichlorosilane After adding silane, keep the reaction solution at 85-95° C. for 2-4 hours, cool the reaction solution to room temperature, filter it, and rectify the filtrate to obtain methylvinylbis(N-ethylacetamido)silane. The invention has mild reaction conditions, simple operation and high yield, and is beneficial to industrial production.

Description

Technical field [0001] The present invention belongs to the field of silicones, specifically relates to a method for preparing methyl vinyl bis (N- ethylacetamin) silane. Background [0002] Methyl vinyl bis(N-ethylacetamin) silane as a chain spreader, it can make the silicone sealing material in the crosslinking at the same time so that its molecular chain linear lengthening, crosslinking point reduction, network topology changes, by changing the density and distribution of the crosslinking point, can achieve modulus and other mechanical properties of the regulation, the preparation of deamide sealing material has a lower modulus and a high elongation of break. However, at present, it has been reported that the synthesis method of methyl vinyl bis(N-ethylacetamin) silane is very small, and the prior art uses N- ethylacetamide and methyl vinyl dichlorosilane as raw materials to produce methyl vinyl bis (N-ethylaceta) silane, the reaction of hydrogen chloride will lead to the occ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/10
CPCC07F7/10
Inventor 肖俊平陈发德王璟赵颖陈隽
Owner 湖北新蓝天新材料股份有限公司