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Method for synthesizing polysilane containing two bonds

A synthesis method and technology of polysilane, applied in the field of polysilane synthesis, can solve the problems of inability to form polysilane containing double bonds, unfavorable large-scale production of polysilane, low retention rate of polysilane double bond, etc., shorten the preparation cycle, It is conducive to large-scale industrial application and reduces the effect of mechanical damage

Inactive Publication Date: 2009-07-08
SHANGHAI UNIV
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  • Abstract
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Problems solved by technology

[0005] In the above synthetic route, there are many problems: the Wurtz reduction coupling method is adopted in the technical route (1), the reaction conditions are more severe, and phenomena such as detonation are prone to occur
Due to the presence of alkali metals, the reaction is dangerous, which is not conducive to the large-scale production of polysilane. At the same time, because the double bond is difficult to withstand this severe reaction condition, the double bond retention rate of the synthesized polysilane is quite low.
The result of technical route (2) shows, directly carry out electrochemical reaction to vinyl dichlorosilane (methyl vinyl dichlorosilane or phenyl vinyl dichlorosilane), the vinyl group on the monomer is in electrochemical reaction process The reaction occurred in the polysilane obtained, the side group of the obtained polysilane is a saturated structure, and the polysilane containing double bonds cannot be formed

Method used

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  • Method for synthesizing polysilane containing two bonds
  • Method for synthesizing polysilane containing two bonds
  • Method for synthesizing polysilane containing two bonds

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Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: In an electrochemical reaction flask equipped with a ventilation tube, a stirrer and a thermometer, methyltrichlorosilane and allyl chloride in different molar ratios were respectively added. Then add about 130ml of tetrahydrofuran (add a small amount of sodium for dehydration and distill, take a fraction at 66°C) and lithium perchlorate (LiClO) with a concentration of 0.1mol / L 4 ) as the supporting electrolyte. Magnesium blocks are used as cathode and anode. After three times of vacuuming and nitrogen filling, start stirring and ultrasonic wave, and then turn on the electricity to start the reaction. When the reaction power reaches 1340mA*h, stop the electricity, add 200ml of toluene, and pass in a balloon of ammonia gas to neutralize the remaining Si-Cl bonds. After secondary pressure filtration and vacuum distillation, a light yellow liquid polysilane containing double bonds is obtained. The molar ratio of methyltrichlorosilane and allyl chloride used...

Embodiment 2

[0024] Embodiment two: prepare the infrared spectrogram of polysilane containing double bond by the addition ratio of methyltrichlorosilane and allyl chloride molar ratio 3 / 1, as figure 1 shown. Among them 2960, 2920cm -1 The peak corresponds to the polysilane CH 3 - Stretching vibration of upper saturated C-H; 1450, 1410cm -1 for Si-CH 3 Deformation vibration of middle C-H; 1260cm -1 for Si-CH 3 Middle CH 3 Deformation vibration; 1080cm -1 It is the characteristic absorption peak of the silicon-oxygen bond, which is caused by the inability to completely isolate oxygen during the experiment; 790, 690cm -1 for Si-CH 3 stretching vibration; 460cm -1 It is the characteristic absorption peak of silicon-silicon bond. This indicates that polysilanes containing double bonds have Si-CH 3 , saturated C-H, Si-Si and other structural groups. At the same time, polysilanes containing double bonds also have some special double bond absorption peaks: 1640cm -1 It is the stretchi...

Embodiment 3

[0025] Embodiment three: prepare the polysilane containing double bond by the addition ratio of methyltrichlorosilane and allyl chloride molar ratio 3 / 1 1 HNMR spectrum, such as figure 2 shown. Among them, the peaks with chemical shift δ at 0.09, 0.25, 0.5-0.6 and 0.85 belong to polysilane Si-CH 3 Structural unit, because Si-CH in polysilane containing double bond 3 The structure around the group is very complex, so in its 1 Si-CH in HNMR spectrum 3 The peak shape is broad and complex. The spectral peaks with chemical shift δ at 5.8, 5.1-5.2, and 3.8-3.9 are assigned to the H on the one, two, and three-position carbons of the allyl group, respectively. This further proves that the synthesized polysilane has an allyl structure.

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Abstract

The invention relates to a preparation method of double bond-containing polysilane. The method of the invention adopts an electrochemical synthesis method, uses a magnesium block as an anode and cathode, and polymerizes methyltrichlorosilane and allyl chloride in a tetrahydrofuran solution to synthesize polysilane with a double bond. The double bond-containing polysilane obtained by the method of the present invention has mild reaction conditions, is easy to control, is simple and safe to operate, and the obtained double bond-containing polysilane has a high quality retention rate and a relatively high ceramic yield, The ceramic production rate of the precursor can be improved well, the preparation cycle of C / C-SiC is shortened, and the mechanical damage caused to the composite material during the preparation process is reduced. It effectively solves the problems existing in the early research and is conducive to large-scale industrial application.

Description

technical field [0001] The invention relates to a method for synthesizing polysilane, in particular to a method for synthesizing polysilane containing double bonds. Background technique [0002] Polysilane is a new type of polymer whose main chain is completely composed of silicon atoms. This special structure makes its electrons widely delocalized along the main chain, thus endowing it with special electronic spectra, thermochromism, spectral hole burning, and photoelectricity. Many unique properties such as conductivity, electroluminescence, electrical conductivity and nonlinear optical properties make it have broad application prospects in photoresists, photoinitiators, waveguides, photoconductors and nonlinear optical materials. . In addition, as a ceramic precursor, polysilane is used as a ceramic precursor, and one of its uses is to prepare silicon carbide ceramic materials through high-temperature cracking. antioxidant properties. However, polysilanes, as ceramic p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60
Inventor 吴市陈来张峰君范雪骐任慕苏孙晋良
Owner SHANGHAI UNIV
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