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Method for preparing cyclic polysilane compound

A technology of cyclic polysilane and manufacturing method, which is applied in the direction of silicon organic compounds, etc., and can solve problems such as complicated operation

Active Publication Date: 2020-09-25
KUREHA KAGAKU KOGYO KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In the technique like Patent Document 2, there is a problem of complicated operation including purification operation for removing the solvent (xylene) from the synthesized polydimethylsilane
In addition, in the technique like Patent Document 3, the alkali metal is deactivated by adding a deactivation solution containing alcohol and water, so in order to further obtain dodecamethylcyclohexasilane from the obtained polysilane compound, it is necessary to use The purification operation to remove alcohol and water still has the problem of complicated operation

Method used

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  • Method for preparing cyclic polysilane compound
  • Method for preparing cyclic polysilane compound
  • Method for preparing cyclic polysilane compound

Examples

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preparation example Construction

[0042] The temperature for preparing the liquid mixture of the silane monomer compound and the solvent is not particularly limited, but mixing and stirring are preferably performed at 0° C. to room temperature.

[0043] The silane monomer compound is preferably added batchwise, more preferably dropwise. This reduces the local increase in the concentration of the silane monomer compound, thereby suppressing the generation of a chain polysilane compound. Therefore, in the first step, the ratio of the reaction to generate the cyclic polysilane compound without passing through the chain polysilane compound increases, and the final yield of the cyclic polysilane compound after the second step increases.

[0044] When adding the silane monomer compound to the mixed solution of the sodium dispersion and the solvent, the temperature of the mixed solution is preferably -10°C or higher, more preferably -5°C or higher, and is preferably lower than the reflux temperature, more preferably ...

Embodiment 1

[0093] In a 200 mL four-necked flask, 30 mL of tetrahydrofuran and 11.07 g of a sodium dispersion ("25% by weight sodium dispersion") were charged and stirred to prepare a mixed liquid. 3.22 g of dichlorodimethylsilane was dissolved in 25 mL of tetrahydrofuran to prepare a silane monomer compound solution. The above mixed solution was cooled and kept at 0°C, and the above silane monomer compound solution was added dropwise over 5 hours while stirring, and after the dropwise addition was completed, stirred at room temperature for 3 hours, and then allowed to react overnight (first step). Next, 0.83 g of naphthalene was added thereto at room temperature, followed by heating to reflux with stirring for 4 hours (second step). Heating was stopped and the reaction liquid was analyzed. As a result, formation of dodecamethylcyclohexasilane as a cyclic polysilane compound was confirmed, and the yield was 87.3%.

Embodiment 2

[0095] Dodecamethylcyclohexasilane was synthesized in the same manner as in Example 1 except that the addition amount of the sodium dispersion liquid was 8.86 g. Its yield was 83.4%.

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Abstract

Provided is a method for preparing a cyclic polysilane compound from a silane monomer compound in one pot. This method for preparing a cyclic polysilane compound includes: a first step in which a silane monomer compound is added to and reacted with a mixture of a sodium dispersion and a solvent; and a second step in which an aromatic hydrocarbon is added to a reaction solution obtained in the first step, and the resultant mixture is heated and refluxed.

Description

technical field [0001] The invention relates to a method for producing a cyclic polysilane compound. Background technique [0002] Silicon carbide fiber is a fiber excellent in heat resistance and oxidation resistance even in a high-temperature atmosphere of several hundred degrees. Utilizing this characteristic, its application in the fields of atomic energy and aerospace is expected. [0003] The silicon carbide fiber is obtained by spinning, infusible, and firing a silicone polymer compound such as polycarbosilane as a precursor. In order to obtain super heat-resistant silicon carbide fibers, it is necessary to suppress the introduction of oxygen atoms into the fiber-forming polymer compound. Therefore, a super heat-resistant silicon carbide fiber is produced by using a silicone polymer compound with a low oxygen content and not introducing oxygen when it is not melted. Cyclic polysilane compounds such as dodecamethylcyclohexasilane can obtain polycarbosilane with an o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21C08G77/60
CPCC08G77/60C07F7/21
Inventor 内藤良太远宫拓
Owner KUREHA KAGAKU KOGYO KK
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