Method for purifying dichloromethyl phenylsilane by chemical coordination effect

A technology of methylphenyldichlorosilane and phenyltrichlorosilane, which is applied in the field of purification of methylphenyldichlorosilane, can solve the problems of large by-products, strict requirements on the stability of distillation aids, etc., and achieves low reaction loss , The effect of fast reaction speed and mild reaction conditions

Inactive Publication Date: 2010-09-29
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the domestic production of methylphenyldichlorosilane mainly adopts the thermal condensation method. This method has the advantages of simple equipment flow, easy access to raw materials, stable process, and safe operation. While methylphenyldichlorosilane, a large amount of phenyltrichlorosilane (PhSiCl 3 )
According to this principle, the boiling point of the distillation aid must be higher than that of MePhSiCl 2 boiling point, and the stability of the selected distillation aid is demanding, which also limits the method in MePhSiCl 2 with PhSiCl 3 applications in separation

Method used

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  • Method for purifying dichloromethyl phenylsilane by chemical coordination effect
  • Method for purifying dichloromethyl phenylsilane by chemical coordination effect

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1: in the 2000mL three-neck flask that stirring and constant pressure dropping funnel are housed, add 1000g purity and be 74.3% MePhSiCl 2Put the crude product in a low-temperature bath at 0°C, and then add a mixture of 219g N-methylimidazole and 250g acetonitrile dropwise through a constant-pressure dropping funnel, and soon a white precipitate will form. , the white precipitate gradually increased. After the dropwise addition, the reaction was stirred at room temperature for 0.5 h. Then filter to remove the white precipitate, and the obtained filtrate is subjected to fractional distillation at normal pressure through a distillation column (specification 700×24mm, glass spring packing). MePhSiCl is obtained between ~204°C 2 , the purity is 96.4%, and the yield is 85.3%.

Embodiment 2

[0028] Embodiment 2: in the 2000mL three-neck flask that stirring and constant pressure dropping funnel are housed, add 1000g purity and be 85.8% MePhSiCl 2 Put the crude product in a low-temperature bath at -10°C, and then add a mixture of 133g N-methylimidazole and 150g toluene dropwise through a constant-pressure dropping funnel, and soon a white precipitate will form. Carried out, the white precipitate gradually increased. After the dropwise addition, the reaction was stirred at room temperature for 2 h. Then centrifuge and decant to obtain the supernatant, and then through the distillation column (specification 700×24mm, glass spring packing) fractional distillation at normal pressure, the temperature at the top of the column is between 109 and 111°C to obtain toluene (yield is 96.5%), the column The top temperature is between 202 and 204°C to obtain MePhSiCl 2 , the purity was 98.2%, and the yield was 90.6%.

Embodiment 3

[0029] Embodiment 3: in the 2000mL three-neck flask that stirring and constant pressure dropping funnel are housed, add 1000g purity and be 92.3% MePhSiCl 2 Put the crude product in a low-temperature bath at -30°C, and then add a mixture of 83g N-methylimidazole and 100g toluene dropwise through a constant-pressure dropping funnel, and soon a white precipitate will form. Carried out, the white precipitate gradually increased. After the dropwise addition, the reaction was stirred at room temperature for 2 h. Then filter to remove the white precipitate, and the obtained filtrate is subjected to fractional distillation at atmospheric pressure through a distillation column (specification 700×24mm, glass spring packing). MePhSiCl is obtained between ~204°C 2 , the purity is 99.7%, and the yield is 93.5%.

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Abstract

The invention relates to a method for purifying dichloromethyl phenylsilane by chemical coordination effect, which aims at solving the technical problems to realize the effects that the MePhSiCl2 in a raw material mixture can be effectively purified, and the purity and the yield are higher. The purifying method of the invention comprises the following steps: slowing adding coordination agents or the solution of the coordination agents into the dichloromethyl phenylsilane / phenyl trichlorosilane mixture during the stirring; and stirring the materials after the material adding so that the reaction is sufficient, or carrying out distilling purification after the sediment is removed to obtain the dichloromethyl phenylsilane, or directly carrying out distilling purification without removing the sediment to obtain the dichloromethyl phenylsilane. The valent weight ratio of the coordination agents to the phenyl trichlorosilane is 100 to 300 percent. The coordination agents are selected from imidazole, pyrrole, paradiazine, quinoline, isoquinolin, imidazole derivatives and pyridine derivatives.

Description

[0001] technical field [0002] The invention relates to the field of organic chemistry, in particular to a method for purifying methylphenyldichlorosilane by chemical coordination. Background technique [0003] Methylphenyldichlorosilane (MePhSiCl 2 ) as a raw material for special silicone monomers, has special application value in the production of high-grade silicone products such as high-temperature resistant silicone rubber and special silicone oil. MePhSiCl 2 The purity of its follow-up products, especially the production and performance of methylphenyl silicone rubber, has an important impact, usually requiring MePhSiCl 2 The purity must reach more than 99%. [0004] At present, the domestic production of methylphenyldichlorosilane mainly adopts the thermal condensation method. This method has the advantages of simple equipment flow, easy access to raw materials, stable process, and safe operation. While methylphenyldichlorosilane, a large amount of phenyltrichlor...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 来国桥胡应乾邬继荣张国栋蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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