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Preparation method of 1,3-diphenyl-1,1,3,3-tetramethyl disiloxane

A disiloxane and double-head technology, which is applied to chemical instruments and methods, silicon organic compounds, compounds of group 4/14 elements of the periodic table, etc., can solve the problems of cumbersome synthesis process, and achieve simple operation, enhanced Large market application and high-value utilization, the effect of gentle and controllable process

Active Publication Date: 2017-04-19
JIUJIANG UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Dong et al. (J. Chem. Eng. Data 2016, 61, 1485−1495) synthesized phenyldimethylethoxysilane with dimethyldiethoxysilane and chlorobenzene by the Wurtz method, and then synthesized 1, 3-phenyl-1,1,3,3-tetramethyldisiloxane, the synthesis process of this method is relatively cumbersome

Method used

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  • Preparation method of 1,3-diphenyl-1,1,3,3-tetramethyl disiloxane

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Embodiment 1

[0024] The dimethyldiethoxy high boiler is rectified to obtain 1,3-diethoxy-1,1,3,3-tetramethyldisiloxane fraction. N 2 Under protection, 23g of sodium was added to 115g of toluene, stirred and heated to 100°C to prepare sodium sand, and then 112.5 g of chlorobenzene was added to react for 4 h. At 60°C, 111.2 g of 1,3-diethoxy-1,1,3,3-tetramethyldisiloxane solution was added and reacted for 3 hours. Stop the reaction, cool and filter, and rectify the filtrate to 1,3-diphenyl-1,1,3,3-tetramethyldisiloxane.

Embodiment 2

[0026] The dimethyldiethoxy high boiler is rectified to obtain 1,3-diethoxy-1,1,3,3-tetramethyldisiloxane fraction. Under the protection of argon, add 23g of sodium to 115g of toluene, stir to prepare sodium sand, then add 137g of bromobutane, and react for 1.5 h. At 30°C, 55.6 g of 1,3-diethoxy-1,1,3,3-tetramethyldisiloxane solution was added and reacted for 2 hours. Stop the reaction, cool and filter, and rectify the filtrate to obtain 1,3-dibutyl-1,1,3,3-tetramethyldisiloxane.

Embodiment 3

[0028] The dimethyldiethoxy high boiler is rectified to obtain 1,3-diethoxy-1,1,3,3-tetramethyldisiloxane fraction. N 2 Under protection, 23g of sodium was added to 115g of toluene, stirred and heated to 100°C to prepare sodium sand, and then 76.5 g of allyl chloride was added to react for 1.5 h. At 10°C, 67.3 g of 1,3-diethoxy-1,1,3,3-tetramethyldisiloxane solution was added and reacted for 3 hours. Stop the reaction, cool and filter, and rectify the filtrate to obtain 1,3-diallyl-1,1,3,3-tetramethyldisiloxane.

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Abstract

The invention discloses a preparation method of 1,3-diphenyl-1,1,3,3-tetramethyl disiloxane. The preparation method is characterized in that the Wurtz method or Grignard method is adopted, and 1,3-diphenyl-1,1,3,3-tetramethyl disiloxane is synthesized through disiloxane rectified from an organosilicon high-boiling component and a halogenated compound. According to the preparation method, market application and high-value utilization of the organosilicon high-boiling component are expanded, and a raw material basis can be further provided for preparation of organosilicon materials with special functions.

Description

technical field [0001] The invention specifically relates to a method for preparing disiloxane double-heads from organosilicon high boilers, and belongs to the technical field of synthesis of organosilicon monomers. Background technique [0002] Silicone high boiler is a mixed liquid with pungent odor and strong corrosiveness produced by-product in the production process of silicone monomer. Its components are very complicated, its market application is limited, and its industrial added value is very low. At present, how to improve the industrial added value and market application of high boiling substances is an urgent problem to be solved in the silicone industry. At present, the treatment methods of organic silicon high boiling substances are mainly used to prepare products such as silicone oil, waterproofing agent, silicone resin and methyl monomer. From the perspective of industrial value and market application, these treatment methods cannot greatly improve the high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08C07F7/10
CPCC07F7/0838C07F7/0878C07F7/10
Inventor 谭景林陈浩
Owner JIUJIANG UNIVERSITY
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