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

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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 phenylt

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

Examples

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Example Embodiment

[0027] Example 1: In a 2000mL three-necked flask equipped with a stirring and constant pressure dropping funnel, 1000g of MePhSiCl with a purity of 74.3% was added 2 The crude product is placed in a low temperature bath at 0°C, and then a mixture of 219g N-methylimidazole and 250g acetonitrile is added dropwise through a constant pressure dropping funnel. A white precipitate will soon be formed. As the reaction progresses , The white precipitation gradually increased. After the addition was completed, the reaction was stirred at room temperature for 0.5h. Then filtered to remove the white precipitate, the filtrate obtained was fractionated under atmospheric pressure through a distillation column (size 700×24mm, glass spring packing), the top temperature of the tower was 81~82℃ to obtain acetonitrile (yield 95.8%), the top temperature of the tower was 202 MePhSiCl is obtained between ~204℃ 2 The purity is 96.4%, and the yield is 85.3%.

Example Embodiment

[0028] Example 2: In a 2000 mL three-necked flask equipped with a stirring and constant pressure dropping funnel, 1000 g of MePhSiCl with a purity of 85.8% was added 2 The crude product is placed in a low temperature bath at –10°C, and then a mixture of 133g N-methylimidazole and 150g toluene is added dropwise through a constant pressure dropping funnel. A white precipitate will soon be formed. As the reaction progresses As it progresses, the white precipitate gradually increases. After the addition was completed, the reaction was stirred at room temperature for 2h. Then the supernatant was obtained by centrifugation and decantation, and then fractionated under normal pressure through a distillation column (size 700×24mm, glass spring packing). The top temperature of the tower was between 109 and 111°C to obtain toluene (96.5% yield). MePhSiCl is obtained when the top temperature is between 202~204℃ 2 The purity is 98.2%, and the yield is 90.6%.

Example Embodiment

[0029] Example 3: In a 2000 mL three-necked flask equipped with a stirring and constant pressure dropping funnel, 1000 g of MePhSiCl with a purity of 92.3% was added 2 The crude product is placed in a low temperature bath at –30°C, and then a mixture of 83g N-methylimidazole and 100g toluene is added dropwise through a constant pressure dropping funnel. A white precipitate will soon be formed. As the reaction progresses As it progresses, the white precipitate gradually increases. After the addition was completed, the reaction was stirred at room temperature for 2h. Then filter to remove the white precipitate, and the filtrate obtained is fractionated under normal pressure through a distillation column (size 700×24mm, glass spring packing). The top temperature is between 109~111℃ to obtain toluene (yield 95.4%), and the top temperature is 202 MePhSiCl is obtained between ~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 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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