Method for preparing phenyl iso-propenyloxysilane

A technology of phenylisopropenyloxysilane and phenyltrichlorosilane, which is applied in the field of preparation of phenylisopropenoxysilane, can solve the problems of research or production inconvenience, poor selectivity, and many by-products, and achieve the price of raw materials Inexpensive, easy to obtain raw materials, and high product purity

Active Publication Date: 2010-04-28
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following problems: the steps are long, the selectivity is poor, and there are many by-products, which brings a lot of inconvenience to research or production

Method used

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  • Method for preparing phenyl iso-propenyloxysilane
  • Method for preparing phenyl iso-propenyloxysilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a three-necked flask containing 500g of cyclohexane and 580g (10 moles of acetone), 8g of catalyst sodium carbonate was added under stirring, and 212g (1.0 moles) of phenyltrichlorosilane was added dropwise at 60°C for 3 hours. , keep warm for 5 hours. It was cooled and filtered to obtain 1152.5 g of filtrate. The composition of the filtrate was analyzed by a gas chromatograph (GC-2014, available from Shimadzu Corporation), and it was found that the filtrate was a mixture of 43.36% by weight of cyclohexane and 22% by weight of phenyltriisopropenyloxysilane.

[0020] The filtrate obtained as above was subjected to vacuum distillation, and 257 g of 150-170°C / 2-5kPa fraction was collected, and measured by gas chromatograph (GC-2014, purchased from Shimadzu Company), phenyltriisopropenyloxysilane in the fraction was The purity is 99.0145% by weight. The yield of phenyltriisopropenyloxysilane product was 92.03%.

Embodiment 2

[0022] In a three-necked flask containing 500 g of diethyl carbonate and 348 g of acetone (6 moles), 15 g of catalyst calcium carbonate was added under stirring, and 212 g of phenyltrichlorosilane (1.0 moles) was added dropwise at 120° C. The addition time was 3 hours, keep warm for 7 hours. It was cooled and filtered to obtain 938 g of filtrate. The composition of the filtrate was analyzed by a gas chromatograph (GC-2014, available from Shimadzu Corporation), and it was found that the filtrate was a mixture of 42.66% by weight of diethyl carbonate and 25.2% by weight of phenyltriisopropenyloxysilane.

[0023] The filtrate obtained as above is subjected to vacuum distillation, and 232 g of 150-170°C / 2-5kPa fractions are collected and measured with a gas chromatograph (GC-2014, purchased from Shimadzu Company), phenyltriisopropenyloxysilane in the fractions The purity is 98.7532% by weight. The yield of phenyltriisopropenyloxysilane product was 82.86%.

Embodiment 3

[0025] In a three-necked flask containing 500g of a mixed solvent of dimethyl carbonate and acetonitrile and 174g (3 moles) of acetone, 10g of catalyst potassium carbonate was added under stirring, and 212g (1.0 moles) of phenyltrichlorosilane was added dropwise at 60°C, The dropwise addition time was 3 hours, and the temperature was kept for 5 hours. It was cooled and filtered to obtain 765 g of filtrate. The composition of the filtrate was analyzed with a gas chromatograph (GC-2014, available from Shimadzu Corporation), and it was found that the filtrate was a mixture of 42.0% by weight of diethyl carbonate and 36.2% by weight of phenyltriisopropenyloxysilane.

[0026] The filtrate obtained as above is subjected to vacuum distillation, and 267 g of 150-170°C / 2-5kPa fractions are collected, and measured by gas chromatograph (GC-2014, purchased from Shimadzu Company), phenyltriisopropenyloxysilane in the fractions The purity is 99.2384% by weight. The yield of phenyltriisopr...

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Abstract

The invention discloses a method for preparing phenyl iso-propenyloxysilane, which has the advantages of simple synthesis process, cheap and easily available raw materials, and high yield. The raw materials phenyl trichlorosilane and acetone are reacted at a temperature of between 40 and 120 DEG C in a solvent in the presence of an alkali metal carbonate catalyst to generate a reaction product containing the phenyl iso-propenyloxysilane; and a high purity product is obtained after rectification under vacuum. The method is suitable for mass production of the phenyl iso-propenyloxysilane.

Description

technical field [0001] The invention relates to a preparation method of phenylisopropenyloxysilane. Background technique [0002] Phenylisopropenyloxysilane is mainly used in room temperature vulcanized silicone rubber, which can effectively improve its low temperature resistance and improve its flame retardancy. Phenylisopropenyloxysilane has the following structural formula: [0003] [0004] The phenyltrichlorosilane is a compound having the following structural formula: [0005] [0006] In the above structural formula, R is chlorine. [0007] In the existing synthesis research of phenylisopropenyloxysilane, a method that has been reported is to take phenyltrichlorosilane and chloropropanol as raw materials, and under negative pressure, react with triethylamine as an acid scavenger Generation of phenyltriisopropenyloxysilane. This method has the following problems: long steps, poor selectivity, and many by-products, thus bringing a lot of inconvenience to resea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 沈锦良张先林杨志勇李伟锋张丽亚
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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