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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 strict stability requirements of distillation aids and large by-products, and achieve fast reaction speed , low reaction loss and high reaction selectivity

Inactive Publication Date: 2012-10-10
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] 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

Examples

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Embodiment 1

[0026] Example 1: In a 2000 mL three-necked flask equipped with stirring and a constant pressure dropping funnel, 1000 g of MePhSiCl with a purity of 74.3% was added 2The crude product was placed in a low-temperature bath at 0°C, and then the mixed solution of 219 g N-methylimidazole and 250 g of acetonitrile was added dropwise through a constant pressure dropping funnel, and a white precipitate was formed soon. As the reaction progressed, 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 × 24 mm, glass spring packing). MePhSiCl can be obtained between 202~204℃ 2 , the purity is 96.4%, and the yield is 85.3%.

Embodiment 2

[0027] Example 2: In a 2000 mL three-neck flask equipped with stirring and a constant pressure dropping funnel, add 1000 g of MePhSiCl with a purity of 85.8% 2 The crude product was placed in a low-temperature bath at -10°C, and then a mixture of 133 g N-methylimidazole and 150 g toluene was added dropwise through a constant-pressure dropping funnel, and a white precipitate was formed soon, followed by As the reaction progressed, the white precipitate gradually increased. After the addition was complete, the reaction was stirred at room temperature for 2 h. Then the supernatant was obtained by centrifugation and decantation, and then fractionated at normal pressure through a distillation column (specification 700 × 24 mm, glass spring packing). The temperature at the top of the tower is between 202 and 204°C to obtain MePhSiCl 2 , the purity was 98.2%, and the yield was 90.6%.

Embodiment 3

[0028] Embodiment 3: In the 2000 mL three-necked flask that is equipped with stirring and constant pressure dropping funnel, add 1000 g of MePhSiCl with a purity of 92.3% 2 The crude product was placed in a low-temperature bath at -30°C, and then a mixture of 83 g N-methylimidazole and 100 g toluene was added dropwise through a constant pressure dropping funnel, and a white precipitate was formed soon, followed by As the reaction progressed, the white precipitate gradually increased. After the addition was complete, 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 × 24 mm, glass spring packing). MePhSiCl can be obtained between 202~204℃ 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 thesediment 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

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for purifying methylphenyldichlorosilane by chemical coordination. Background technique [0002] 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%. [0003] 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 (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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