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Method for preparing methyl phenyl dichlorosilane

A technology of methylphenyldichlorosilane and dimethyldisilane, which is applied in the field of preparation of methylphenyldichlorosilane, can solve the problems of low yield and difficult PhCl, etc., achieve less side reactions and easy industrialization , easy separation effect

Active Publication Date: 2012-07-18
唐山偶联硅业有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For the disilane cracking method, the applicant's research results found that even under the action of Pd (0), Ru and other tertiary amines, tertiary phosphines, quaternary ammonium halides, quaternary phosphine halides, PhCl is almost difficult to react with MeCl 2 SiSiClMe 2 and MeCl 2 SiSiCl 2 Cleavage reaction of two disilanes of Me, MePhSiCl in the product 2 very low yield

Method used

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  • Method for preparing methyl phenyl dichlorosilane

Examples

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Effect test

Embodiment 1

[0026] In a 500 ml three-necked flask equipped with a reflux condenser and a thermometer, add 50 mL of Me 2 ClSiSiCl 2 Me, 100mL bromobenzene, 0.25g Pd(PPh 3 ) 4 , 100mL [Emim]Br+AlCl 3 For ionic liquids, slowly heat up to 150°C, turn on magnetic stirring and reflux for 20 hours to remove MeSiHCl 2 , after the reaction to the product (mainly MePhSiCl 2 and dibromobenzene) to condense, solid-liquid separation to remove solid impurities, to obtain MePhSiCl 2 liquid mixture. The resulting liquid phase mixture is then analyzed by gas chromatography-mass spectrometry (GC-MS), and calculated, the conversion rate of raw material disilane is 71%, and the product MePhSiCl 2 The yield was 54%.

Embodiment 2

[0028] In a 500 ml three-necked flask equipped with a reflux condenser and a thermometer, add 50 mL of Me 2 ClSiSiCl 2 Me, 100mL bromobenzene, 0.25g Pd(PPh 3 ) 4 , 100mL [Bmim]Cl+AlCl 3 For ionic liquids, slowly heat up to 150°C, turn on magnetic stirring and reflux for 20 hours to remove MeSiHCl 2 , after the reaction to the product (mainly MePhSiCl 2 and dibromobenzene) to condense, solid-liquid separation to remove solid impurities, to obtain MePhSiCl 2 liquid mixture. Then the obtained liquid phase mixture is analyzed by GC-MS, and calculated, the conversion rate of raw material disilane is 77%, and the product MePhSiCl 2 The yield is 60%.

Embodiment 3

[0030] In a 500 ml three-necked flask equipped with a reflux condenser and a thermometer, add 50 mL of Me 2 ClSiSiCl 2 Me, 100mL bromobenzene, 0.25g Pd(PPh 3 ) 4 , 100mL [Bmim]PF 6 For ionic liquids, heat up slowly to 120°C, turn on magnetic stirring and reflux for 20 hours to remove MeSiHCl 2 , after the reaction to the product (mainly MePhSiCl 2 and dibromobenzene) to condense, solid-liquid separation to remove solid impurities, to obtain MePhSiCl 2 liquid mixture. Then the obtained liquid phase mixture is analyzed by GC-MS, calculated, the raw material disilane conversion rate is 83%, and the product MePhSiCl 2 The yield was 73%.

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Abstract

The invention discloses a method for preparing methyl phenyl dichlorosilane. The method comprises the following steps of: performing reflux reaction on 1,1,2,2-tetrachloro-1,2-dimethyldisilane and bromobenzene serving as main raw materials at the temperature of between 90 and 200 DEG C for 8 to 24 hours in the presence of a zerovalent palladium metal complex / ionic liquid serving as a catalyst, condensing a product, and performing solid-liquid separation to obtain the methyl phenyl dichlorosilane (MePhSiCl2). By the preparation method, the conversion rate of the raw materials is high, a volatile solvent is not used, and the yield of the target product, namely the MePhSiCl2 is high. The method for preparing the MePhSiCl2 is simple and practicable, easy to industrialize, low in equipment investment cost, safely and stably operated and good in industrial application prospect, and has the characteristics that the reaction is simple, the method is easy to operate, the product is easily separated from a byproduct, and the like.

Description

technical field [0001] The invention belongs to the field of fine chemical synthesis research, in particular to a kind of methylphenyl dichlorosilane (MePhSiCl 2 ) preparation method. Background technique [0002] Organosilicon materials are mainly a kind of polymer compound with Si-O bond as the main chain and organic groups as side chains on Si atoms. It has excellent performance and unique functions, and is widely used in military industry, aerospace, medical treatment, and chemical industry. and other fields. Organochlorosilanes are the most important raw materials for the preparation of organosilicon polymer materials and other functional silanes. Therefore, the production status of organochlorosilane largely determines the development level of a country's organosilicon industry. Among the more than 20 kinds of organosilicon monomers currently used in the production of polysiloxanes, methylchlorosilane is used in the largest amount, accounting for more than 90 wt% of...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 谭军陈洁刘辉皮永蕊韦晓燕
Owner 唐山偶联硅业有限公司
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