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Method of making branched polysilane copolymers

A technology for branched polysilane and copolymers, which is applied in the field of preparation of branched polysilane copolymers, and can solve problems such as difficulties, complicated polysilane chemical methods, and difficult preparation methods

Inactive Publication Date: 2008-04-09
DOW CORNING CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Reproducing the preparation of polysilanes remains difficult and challenging due to the complexity and difficulty of developing the chemistry to prepare polysilanes

Method used

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  • Method of making branched polysilane copolymers
  • Method of making branched polysilane copolymers
  • Method of making branched polysilane copolymers

Examples

Experimental program
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Embodiment 1

Embodiment 1-synthetic branched polysilane copolymer

Preparation of phenyl-methyl, diphenyl, methyl terpolymers

[0030] Toluene (4025 g) and sodium metal (163 g) were charged in a 6 liter cylindrical glass reaction vessel and then the toluene was refluxed through the jacket using a circulating bath. A slightly positive nitrogen atmosphere was maintained throughout the procedure. The molten sodium was then dispersed using an impeller with double pitched blades and the jacket temperature was maintained at 110°C. A mixture containing phenylmethyldichlorosilane (365 g), diphenyldichlorosilane (127 g) and methyltrichlorosilane (89.3 g) was then introduced over 60 minutes by means of a dropper just above the upper impeller to the reaction vessel, resulting in an exotherm to 113°C. After maintaining the reaction temperature for 16 hours, the contents were cooled to 40°C, after which methanol (455 g) was slowly added to oxidize the residual sodium. This slurry is then centrifuged...

Embodiment 2

Embodiment 2-synthetic branched polysilane copolymer

Preparation of phenyl-methyl, diphenyl, methyl terpolymers

[0031] Toluene (4025 g) and metallic sodium (163 g) were charged in a 6 liter cylindrical glass reaction vessel, and then the toluene was refluxed through the jacket using a circulating bath. A slightly positive nitrogen atmosphere was maintained throughout the procedure. The molten sodium was then dispersed using an impeller with double pitched blades and the jacket temperature was maintained at 110°C. Then, over 60 minutes, by means of a dropper positioned just above the upper impeller, a solution containing phenylmethyldichlorosilane (445 g), diphenyldichlorosilane (68.7 g) and methyltrichlorosilane (69.3 g) was introduced. The mixture was transferred to the reaction vessel, resulting in an exotherm to 113°C. After maintaining the reaction temperature for 2 hours, the contents were cooled to 40°C, after which methanol (453 g) was slowly added to oxidize the r...

Embodiment 3

Embodiment 3-synthetic branched chain polysilane copolymer

Preparation of phenyl-methyl, diphenyl, methyl terpolymers

[0032] Toluene (4308 g) and metallic sodium (121 g) were charged in a 6-liter cylindrical glass reaction vessel, and then the toluene was refluxed through the jacket using a circulating bath. A slightly positive nitrogen atmosphere was maintained throughout the procedure. The molten sodium was then dispersed using an impeller with double pitched blades and the jacket temperature was maintained at 110°C. A mixture containing phenylmethyldichlorosilane (295 g), diphenyldichlorosilane (102 g) and methyltrichlorosilane (50.9 g) was then introduced over 120 minutes by means of a dropper just above the upper impeller to the reaction vessel, resulting in an exotherm to 112°C. After maintaining the reaction temperature for 2 hours, the contents were cooled to 40°C, after which methanol (338 g) was slowly added to oxidize the residual sodium. This slurry was then ...

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Abstract

Branched polysilane copolymers are prepared via a Wurtz-type coupling reaction by reacting a mixture of two different dihalosilanes and a single trihalosilane with an alkali metal coupling agent in an organic liquid medium. The branched polysilane copolymers are recovered from the reaction mixture. Capped branched polysilane copolymers are prepared via the same Wurtz-type coupling reaction with addition of a capping agent to the reaction mixture. The capping agent is a monohalosilane, monoalkoxysilane, dialkoxysilane, or trialkoxysilane. The branched polysilane copolymers and the capped branched polysilane copolymers are soluble in organic liquid medium.

Description

[0001] Cross References to Related Applications [0001] This application claims priority to US Provisional Application No. 60 / 675635, filed April 28, 2005. field of invention [0002] The present invention relates to a process for the preparation of branched polysilane copolymers, particularly the Wurtz-type coupling reaction of two different dihalosilanes and a single trihalosilane. The method of the present invention is improved in that it produces branched polysilane copolymers as opposed to branched polysilane homopolymers. The branched polysilane copolymer is soluble in an organic liquid medium. Background of the invention [0003] The earliest synthetic procedures for the preparation of polysilanes used Wurtz-type reductive coupling reactions of dichlorosilanes. For example, by (i) dehydrocoupling of monosubstituted silanes using transition metal catalysts, (ii) ring-opening polymerization of cyclosiloxanes, (iii) anionic polymerization of masked silanes, and (iv) w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C08L83/16
CPCC08G77/60C08G77/42C08L83/16C08G77/48
Inventor T·海因R·金B·T·源H·H·里斯M·A·史密斯H·X·沃
Owner DOW CORNING CORP