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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 severe reaction conditions, prone to explosive polymerization, and difficulty in fine particle dispersion, and achieves mild reaction conditions, easy control, and solution The effect of low yield

Inactive Publication Date: 2011-07-20
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

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Experimental program
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Embodiment 1

[0021] Embodiment 1: 17.66ml (0.15mol) methyl trichlorosilane, 4.09ml (0.05mol) allyl chloride and 2.52ml cyclopentadiene (0.03mol) are put into the electrochemical reaction bottle, add 121ml tetrahydrofuran simultaneously solvent and 1.6 g lithium perchlorate supporting electrolyte. Magnesium blocks are used as cathode and anode. After three times of vacuuming and nitrogen filling, start stirring and ultrasonic waves, and then turn on electricity to start the reaction. When reaching 4% (536mA h) of theoretical electricity, add 3.49g (0.015mol) titanium tetrachloride to continue the reaction until the reaction electricity reaches At 5% (670mA·h), stop the power supply, add 200ml of toluene, pass through a bag of ammonia gas, neutralize the remaining Si-Cl bonds, and undergo secondary pressure filtration and vacuum distillation to obtain a black liquid product.

[0022] As a result, the obtained zirconium-containing polysilane had a viscosity of 10.8 mPa.s, a yield of 76%, a d...

Embodiment 2

[0023] Example 2: Methyltrichlorosilane / allyl chloride, methyltrichlorosilane / cyclopentadiene, methyltrichlorosilane / tetrachloro The infrared spectrogram of the zirconium-containing polysilane prepared by zirconium, such 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; 1270cm -1 for Si-CH 3 Middle CH 3 Deformation vibration; 1100cm -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, zirconium-containing polysilane also has some special double bond absorp...

Embodiment 3

[0024] Example 3: Methyltrichlorosilane / allyl chloride, methyltrichlorosilane / cyclopentadiene, methyltrichlorosilane / tetrachloro Zirconium is the ultraviolet spectrogram of the zirconium-containing polysilane prepared by monomer, such as figure 2 shown. There is a maximum absorption wavelength at 300nm, which is the characteristic absorption of the silicon backbone. where the strong peak at 300 nm is attributed to σ→σ * transition, while the weak peak at 350nm–400nm is attributed 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 has also been significantly strengthened. This is because the introduction of zirconium forms a π-bond complex in the system, resulting in the formation of a similar crosslinking system , thus broadening the delocalized system and broadening 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 hassimple 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 polymers. Background technique [0002] Polysilane is a kind of polymer containing only silicon atoms in the chain skeleton. The delocalization of the σ-bond electrons in the Si-Si chain enables the σ-electrons to be widely delocalized along the main chain. , thermal stability, ultraviolet absorption, thermochromism and fluorescence, etc. present unique properties. Based on its unique properties, it has broad application prospects in photoresists, photoinitiators, waveguides, photoconductors and nonlinear optical materials. In addition, polysilane is also used to prepare SiC, Si 3 N 4 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 to prepare carbon / carbon-silicon carb...

Claims

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Application Information

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Patent Type & Authority Patents(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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