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Synthesis process of dicyclopentyl dichlorosilane

A technology of dicyclopentyldichlorosilane and dicyclopentyldimethoxysilane, which is applied in the field of dicyclopentyldichlorosilane synthesis technology, can solve complex process, increase investment cost, production cost and operating cost , It is difficult to ensure job safety, environment, hygiene requirements and other issues, to achieve the effect of simple process, low equipment requirements and mild conditions

Active Publication Date: 2019-02-22
大连鼎燕医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This makes the process relatively complicated, which will inevitably increase investment costs, production costs and operating costs
[0011] 3. Using highly toxic dichlorosilane as raw material under high pressure, the requirements for airtightness of equipment are more stringent, and it is difficult to guarantee the safety, environment and hygiene requirements of the post

Method used

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  • Synthesis process of dicyclopentyl dichlorosilane
  • Synthesis process of dicyclopentyl dichlorosilane

Examples

Experimental program
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Effect test

Embodiment 1

[0024] In a 1L four-neck round-bottomed flask equipped with a stirrer, thermometer, gas bubbler and vent, first replace the air with nitrogen. Add 500g (2.2mol) dicyclopentyldimethoxysilane into the flask, start stirring, cool the reaction flask to 20-25°C with an ice-water bath, and slowly pass in dried HCl gas through a bubbler, (actually pass The molar ratio is 2.2 times that of dicyclopentyldimethoxysilane). The aeration time is 10h and the aeration time is 1h, the aeration speed is 0.48mol / h, after the reaction is completed, stop the agitation, let it stand for stratification, remove the upper layer of methanol, and collect the distillate at 105-110°C under reduced pressure at 4-5mmHg absolute pressure. Obtained 452.5 g of dicyclopentyldichlorosilane (ESI-MS: m / z=237[M+H] + ), a purity of 98.2%, and a yield of 85.4%.

Embodiment 2

[0026] In a 1L four-neck round-bottomed flask equipped with a stirrer, thermometer, gas bubbler and vent, first replace the air with nitrogen. Add 500g (2.2mol) dicyclopentyldimethoxysilane into the flask, start stirring, cool the reaction flask to 20-25°C with an ice-water bath, and slowly pass in dried HCl gas through a bubbler, (actually pass The molar ratio is 2.2 times that of dicyclopentyldimethoxysilane). The aeration time is 10h and the aeration time is 1h, the aeration speed is 0.48mol / h, after the reaction is completed, stop the agitation, let it stand for stratification, remove the upper layer of methanol, and collect the distillate at 105-110°C under reduced pressure at 4-5mmHg absolute pressure. Obtained 434.6 g of dicyclopentyldichlorosilane (ESI-MS: m / z=237[M+H] + ), a purity of 98.0%, and a yield of 81.9%.

[0027] Taking the dicyclopentyl dichlorosilane done in Example 2 as a raw material to synthesize dicyclopentyl diethylaminosilane:

[0028] In a 2L four...

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Abstract

The invention discloses a synthetic process of dicyclopentyldichlorosilane. According to the synthetic process, dicyclopentyldichlorosilane is synthesized from dimethoxydimethylsilane and dry hydrogen chloride gas. The synthetic process has the advantages that the conversion rate is high, and the selectivity is good; the condition is mild, and the process is simple; high temperature and high pressure are not required, and the facility request is low; no expensive catalyst is used, and the raw material cost is low; highly toxic chlorosilane is not produced, and the operation is relatively safe. Therefore, the synthetic process has superiority.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a synthesis process of dicyclopentyl dichlorosilane. Background technique [0002] Dicyclopentyldichlorosilane is an important intermediate for the synthesis of special organosiloxanes and silane coupling agents, and the cost of its preparation process is directly related to the process economy, which has attracted widespread attention in related fields at home and abroad. [0003] So far, although there are many synthesis literatures of the title compound [1] [2] [3], the synthesis process used is the same, and the difference is only in some details. The process uses cyclopentene and dichlorosilane as raw materials, and is prepared by addition reaction at 100-140°C (about 1.2MPa pressure) under the catalysis of Pt catalyst. The reaction equation is: [0004] [0005] 【1】Zhang Weidong. A synthesis method of dicyclopentyldichlorosilane: China, CN201210346632.4[P].20...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
CPCC07F7/123
Inventor 南海军孙立芹吕永智蔡鲁伯范莉莉程家良吴冬辉
Owner 大连鼎燕医药化工有限公司
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