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Alkyl cyclohexyl dialkoxy silane prepared by sodium condensation method

A technology of cyclohexyldialkoxysilane and sodium condensation method, which is applied in the field of synthesis of alkylcyclohexyldialkoxysilane by sodium condensation method, can solve the problems of useless production, expensive organic lithium, poor stability, etc., and achieve reduction The effect of production cost, shortened reaction cycle, and accelerated reaction speed

Inactive Publication Date: 2007-11-28
盐城市华业医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] This method has a faster start-up speed and a higher yield, but organolithium is expensive and has poor stability, so it is rarely used for synthesis at present. No more reports for production

Method used

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  • Alkyl cyclohexyl dialkoxy silane prepared by sodium condensation method
  • Alkyl cyclohexyl dialkoxy silane prepared by sodium condensation method
  • Alkyl cyclohexyl dialkoxy silane prepared by sodium condensation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1: Add 30g of toluene into a three-necked flask, then add 11.5g of metallic sodium, heat and stir, break the sodium into sodium sand above 100°C, then slowly drop in 30g of chlorocyclohexane and 68g of methyl Chlorodimethoxysilane [CH 3 SiCl(OCH 3 ) 2 ] and 20g of n-heptane mixed solution, the reaction temperature is controlled at 100 ~ 104 ℃. The mixed solution was dropped within 35 minutes, kept warm for 0.5 hours, and the product was evaporated under reduced pressure. According to gas chromatography analysis, the yield of methylcyclohexyldimethoxysilane was 51.9% (mass fraction).

Embodiment 2

[0044] Example 2: Add 40 g of toluene and 6 g of sodium metal into a three-necked flask, raise the temperature to 100 ° C, and break the sodium metal into sodium sand under stirring, and mix 15 g of chlorocyclohexane and CH at 106 ° C 3 SiCl(OCH 3 ) 2 34g of the mixed solution was slowly dripped into the three-necked flask, and the dripping was completed within 40min, kept at reflux temperature for 1.5h, and then the product was evaporated under reduced pressure, and analyzed by gas chromatography to obtain methylcyclohexyldimethoxysilane. Rate 49.9%.

Embodiment 3

[0045] Embodiment three: 23.5g (content 98%) sodium metal and 100g CH 3 Si(OCH 3 ) 3 Add it to a three-necked flask, heat and stir, break metal sodium into sodium sand, keep it above 100°C, drop 59g of chlorocyclohexane and 84g of methylchlorodimethoxysilane at the same time, within about 1h After dripping all the raw materials, keep the temperature at 102-106°C for 2 hours, distill the crude product under reduced pressure, the remaining residue is off-white, a total of 58g, the crude product is analyzed by gas chromatography, and the yield of methylcyclohexyldimethoxysilane is 61 % (mass fraction).

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Abstract

The present invention relates to sodium condensation process for synthesizing alkyl cyclohexyl diphenyl alkoxyl silane. After metal sodium is dissolved in solvent through heating and stirring inside a reactor, halogenated cyclohexane and RaXbSi(OR' )c, where, R is CH3, R' is CH3- or C2H5-, X is Cl or Br, a is 0 or 1, b is 1, 2 or 3, c is 1, 2 or 3, and a+b+c=4, in certain proportion are dropped into the system to produce sodium condensation reaction. Through maintaining for some time, filtering or vacuum distillation to obtain coarse product, and decompression fractionation, the product is obtained. The process has facile materials, simple operation, short reaction period, high safety and high yield.

Description

Technical field [0001] The present invention relates to the synthesis of alkylcyclohexyldialkoxysilane by sodium condensation method. Background technique [0002] The cocatalyst-electron donor used in the production of polypropylene generally uses diphenyldimethoxysilane or methylphenyldimethoxysilane, but because it contains phenyl groups, it has certain toxicity, which limits the use of polypropylene. Application and promotion of products in food and hygiene fields, methylcyclohexyldimethoxysilane Because it is non-toxic and highly efficient, it can prolong the active life of the catalyst, has greater operating flexibility, can greatly improve the isotacticity of polypropylene, and has better resin processing performance. Therefore, it has been used as a cocatalyst in large-scale continuous polypropylene production, and its application has been continuously expanded, and it will eventually replace diphenyldimethoxysilane and the like. [0003] The preparation method of...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 张银华王一璐
Owner 盐城市华业医药化工有限公司
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