Method for synthesizing zirconium-containing polysilane

A technology of polysilane and methyltrichlorosilane, which is applied in the field of synthesis of zirconium-containing polysilane, can solve the problems of difficult dispersion of particles, severe reaction conditions, and prone to implosion, etc., to solve the problems of low yield and reaction conditions. Gentle, manageable effect

Inactive Publication Date: 2010-06-09
SHANGHAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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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
The current metal-containing polysilanes are generally added with metal carbides in the form of doping. The problem is that the fine dispersion of these particles is usually difficult and cannot effectively penetrate into the fiber bundle.

Method used

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  • Method for synthesizing zirconium-containing polysilane
  • Method for synthesizing zirconium-containing polysilane
  • Method for synthesizing zirconium-containing polysilane

Examples

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Embodiment 1

[0021] Example 1: Put 17.66ml (0.15mol) methyltrichlorosilane, 4.09ml (0.05mol) allyl chloride and 2.52ml cyclopentadiene (0.03mol) into the electrochemical reaction flask, and add 121ml tetrahydrofuran at the same time Solvent and 1.6g lithium perchlorate supporting electrolyte. Use magnesium blocks as cathode and anode. After three times of vacuuming and filling with nitrogen, start stirring and ultrasonic, then energize to start the reaction. When it reaches 4% of the theoretical power (536mA·h), add 3.49g (0.015mol) of titanium tetrachloride to continue the reaction until the reaction power reaches Stop energizing at 5% (670mA·h), add 200ml of toluene, and pass in a bag of ammonia gas to neutralize the remaining Si-Cl bonds. After a second pressure filtration and vacuum distillation, a black liquid product is obtained.

[0022] As a result, the obtained zirconium-containing polysilane had a viscosity of 10.8 mPa·s, a yield of 76%, a double bond retention rate of 9.8%, and a ...

Embodiment 2

[0023] Example 2: Methyltrichlorosilane / allyl chloride, methyltrichlorosilane / cyclopentadiene, methyltrichlorosilane / tetrachloride with a molar ratio of 3 / 1, 5 / 1, 10 / 1 The infrared spectrum of zirconium-containing polysilane prepared by zirconium, such as figure 1 Shown. Of which 2960, 2920cm -1 The peak corresponds to polysilane CH 3 -Stretching vibration of saturated C-H; 1450, 1410cm -1 Si-CH 3 Deformation vibration of medium C-H; 1270cm -1 Si-CH 3 Medium CH 3 Deformation vibration; 1100cm -1 It is the characteristic absorption peak of silicon-oxygen bond, which is caused by the inability to completely isolate oxygen during the experiment; 790,690cm -1 Si-CH 3 Stretching vibration; 460cm -1 It is the characteristic absorption peak of silicon-silicon bond. This shows that polysilanes containing double bonds have Si-CH 3 , Saturated C-H, Si-Si and other structural groups. At the same time, zirconium-containing polysilane also has some special double bond absorption peaks: 1640...

Embodiment 3

[0024] Example 3: Methyltrichlorosilane / allyl chloride, methyltrichlorosilane / cyclopentadiene, methyltrichlorosilane / tetrachloride with molar ratios of 3 / 1, 5 / 1, 10 / 1 The UV spectrum of zirconium-containing polysilane prepared by using zirconium as a monomer, such as figure 2 Shown. There is a maximum absorption wavelength at 300nm, which is the characteristic absorption of the silicon backbone. The strong peak at 300nm is attributed to σ→σ * Transition, and the weak peak at 350nm-400nm is due to π→π * Jump. The absorption peak of zirconium-containing polysilane in the near ultraviolet region has been broadened, and the absorption at 350nm to 400nm is also significantly enhanced. This is because the introduction of zirconium forms a π-bonded complex in the system, leading to the formation of a similar cross-linked system , Which broadens the delocalized system and broadens the peak shape.

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Abstract

The invention relates to a method for preparing zirconium-containing polysilane, which is synthesized by the steps of adopting the electrochemical synthesis method, taking magnesium blocks as negative and positive poles, and polymerizing methyl trichlorosilane, allyl chloride, cyclopentadiene and zirconium chloride in tetrahydrofuran solution and electrolyte supported by lithium perchlorate to obtain the polysilane containing double bonds and zirconium. Results show that the polysilane prepared by the method in the invention has high quality retention rate and ceramic yield. The invention has simple and safe operation method; and the zirconium-containing polysilane can improve the ceramic yield of precursors favorably, successfully introduce the antioxidant metal zirconium, and is a ceramic precursor with good performance.

Description

Technical field [0001] The invention relates to a method for synthesizing zirconium-containing polysilane, which belongs to the field of organic high molecular polymers. Background technique [0002] Polysilane is a kind of polymer with only silicon atoms in the chain skeleton. The delocalization of the σ bond electrons in the Si-Si chain allows the σ electrons to be widely delocalized along the main chain. Its unique structure makes it more soluble , Thermal stability, ultraviolet absorption, thermochromic and fluorescence, etc., showing unique properties. Based on its unique properties, it has broad application prospects in photoresist, photoinitiator, waveguide, optical conductor and nonlinear optical materials. In addition, polysilane still prepares SiC, Si 3 N 4 The preparation of silicon carbide ceramic materials by high temperature cracking is one of its important uses, mainly to prepare high temperature resistant and oxidation resistant silicon carbide ceramic fibers, or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/50C04B35/565C04B35/584
Inventor 花永盛陈来高孟娇任慕苏孙晋良
Owner SHANGHAI UNIV
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