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Synthetic method for di-tert-butoxydiacetoxysilane

A technology of di-tert-butoxydiacetoxysilane and tetraacetoxysilane, which is applied in the field of synthesis of organosilicic acidic crosslinking agents, can solve problems such as difficulty in achieving large-scale production, and reduce production costs and reduce production costs , Reduce the effect of impurity interference

Pending Publication Date: 2018-06-26
湖北环宇化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is also difficult to achieve large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0016] Put 600 kilograms of glacial acetic acid and 340 kilograms of silicon tetrachloride into the reaction kettle at room temperature, and stir for ten minutes. The temperature was raised in the water bath, and the temperature was controlled for 3 hours to slowly increase the internal temperature of the reactor from 35°C to 60°C. Nitrogen gas was continuously fed in, and the reaction was kept at 60°C for 1 hour. It was detected that almost no HCL gas was emitted. Distill excess glacial acetic acid under reduced pressure until the pH value of the material is 5-6. At this moment, a large amount of crystallization of material was separated out, and 100 kilograms of glacial acetic acid was added to make it dissolve and clarify, weighing 618.3 kilograms. The content of tetraacetoxysilane in the sampling kilogram C analysis material is 78.86%, which is 487.6 kilograms of tetraacetoxysilane. Control the temperature at 17~20°C, add tert-butanol dropwise with measured molar mass, an...

example 2

[0018] The reaction device is the same as before. Add 300 kg of glacial acetic acid at room temperature, reclaim 300 kg of glacial acetic acid and 340 kg of silicon tetrachloride, and stir for ten minutes. The temperature was raised in the water bath, and the temperature was controlled for 3 hours to slowly increase the internal temperature of the reactor from 35°C to 60°C. Nitrogen gas was continuously fed in, and the reaction was kept at 60°C for 1 hour. It was detected that almost no HCL gas was emitted. Distill excess glacial acetic acid under reduced pressure until the pH value of the material is 5-6. Now material becomes turbid or a large amount of crystallization is separated out, add 150 kilograms of glacial acetic acid to make it dissolve clarification, weigh 667.4 kilograms. The tetraacetoxysilane content in the sampling kilogram C analysis material is 72.85%, which is 486.2 kilograms of tetraacetoxysilane. Control the temperature at 17~20°C, add dropwise tert-buta...

example 3

[0020] 400 kilograms of glacial acetic acid, 800 kilograms of reclaimed glacial acetic acid and 680 kilograms of silicon tetrachloride were dropped into the reactor, and stirred for ten minutes. The temperature was raised in the water bath, and the temperature was controlled for 4 hours to slowly increase the internal temperature of the reactor from 35°C to 60°C. Nitrogen gas was continuously introduced, and the reaction was kept at 60°C for 1.5 hours. It was detected that almost no HCL gas was emitted. Distill excess glacial acetic acid under reduced pressure until the pH value of the material is 5-6. This moment, a large amount of material crystallized out, added 300 kilograms of glacial acetic acid to make it dissolve and clarified, weighing 1352.8 kilograms. The content of tetraacetoxysilane in the sampling kilogram C analysis material is 72.75%, which is 984.2 kilograms of tetraacetoxysilane. Control the temperature at 17~20°C, add dropwise tert-butanol with measured mol...

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Abstract

The invention relates to a synthetic method for di-tert-butoxydiacetoxysilane, belonging to the field of chemical synthesis. According to the invention, the method comprises the following steps: subjecting silicon tetrachloride and glacial acetic acid to mixing, heating and acylation successively to produce silicon tetraacetate; then adding a fixed amount of tert-butyl alcohol at a low temperaturedrop by drop with excess glacial acetic acid as a solvent, and carrying out an esterification reaction; and carrying out vacuum distillation so as to obtain the finished di-tert-butoxydiacetoxysilane, and subjecting by-produced glacial acetic acid to indiscriminate application in next batches. The synthetic method of the invention is reasonable in process, easy to operate, stable in product quality, greatly reduced in production cost and suitable for industrial scale production.

Description

technical field [0001] The invention relates to a method for synthesizing an organosilicon acidic crosslinking agent, which belongs to the field of chemical synthesis. Background technique [0002] The crosslinking agent is the core component of one-component room temperature vulcanizing silicone rubber, which can transform the linear base polymer into a three-dimensional network structure and form an elastomer. At present, the deacetate silicone rubber still occupies an important market share, and its crosslinking agent is mainly methyltriacetoxysilane. Methyltriacetoxysilane is solid at room temperature and is insoluble in polysiloxane, so it is often combined with ethyltriacetoxysilane, propyltriacetoxysilane, vinyltriacetoxysilane, diacetoxysilane, The use of tert-butoxydiacetoxysilane, etc., can improve the performance of silicone rubber, especially the addition of di-tert-butoxydiacetoxysilane can significantly improve the tensile strength, elongation at break, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
CPCC07F7/1896
Inventor 袁发强杨红艳黄国辉刘春香
Owner 湖北环宇化工有限公司