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Polysilane containing transition metallic element and preparation method thereof

A technology of transition metal elements and transition metal ions, applied in the field of polysilane and its preparation, to achieve mild reaction conditions, moderate viscosity, and increase the effect of cured gel content

Inactive Publication Date: 2011-07-27
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are no domestic reports about introducing metals into polysilane

Method used

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  • Polysilane containing transition metallic element and preparation method thereof
  • Polysilane containing transition metallic element and preparation method thereof
  • Polysilane containing transition metallic element and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Example 1: Put 17.66ml (0.15mol) of methyltrichlorosilane, 4.09ml (0.05mol) of allyl chloride and 2.52ml of cyclopentadiene (0.03mol) into the electrochemical reaction bottle, and at the same time add 121ml of tetrahydrofuran solvent and 1.6g Lithium perchlorate supports the 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 electricity to start the reaction. When the theoretical electricity reaches 4% (536mA h), add 2.85g (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 to neutralize the residual Si-Cl bonds, and undergo secondary pressure filtration and vacuum distillation to obtain black liquid titanium-containing polysilane.

[0031] The resulting titanium-containing polysilane had a viscosity of 120 mPa·s,...

Embodiment 2

[0032] Example 2: Prepared with methyltrichlorosilane / allyl chloride, methyltrichlorosilane / cyclopentadiene, methyltrichlorosilane / titanium tetrachloride at a molar ratio of 3 / 1, 5 / 1, 10 / 1 The infrared spectrum of titanium-containing polysilane, such as figure 1 shown. Among them 2960, 2920 cm -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; 1100 cm -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; 460 cm -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, titanium-containing polysilane also h...

Embodiment 3

[0033] Example 3: Methyltrichlorosilane / allyl chloride, methyltrichlorosilane / cyclopentadiene, methyltrichlorosilane / titanium tetrachloride at a molar ratio of 3 / 1, 5 / 1, 10 / 1 The ultraviolet spectrum of the titanium-containing polysilane prepared by the body, 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 titanium-containing polysilane in the near-ultraviolet region is broadened, and the absorption at 350nm-400nm is also significantly strengthened, because the introduction of titanium forms a similar cross-linked branch system centered on titanium in the system, thus Broaden the delocalized system and broaden the peak shape.

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Abstract

The invention relates to a polysilane containing a transition metallic element and a preparation method thereof. In the invention, an electrochemical synthesis method is adopted, magnesium blocks are adopted as a cathode and an anode; methyl trichlorosilane, allyl chloride and cyclopentadiene are dissolved in tetrahydrofuran to prepare into an electrolytic solution, lithium perchlorate is added as a supporting electrolyte, transition metal chloride is added, and the electrolytic solution, lithium perchlorate and the transition metal chloride are polymerized to synthesize the polysilane containing double bonds and a metallic element, wherein the constitutional formula of the polysilane is shown in the specification. The result proves that the reaction condition in the invention is mild, and the operation is simple and safe; and the double bonds and the antioxidant metallic element titanium or zirconium or hafnium and the like are introduced into the polysilane, and the polysilane containing a transition metallic element is a ceramic precursor with excellent performance.

Description

technical field [0001] The invention relates to a polysilane and a preparation method thereof, in particular to a synthesis method of polysilane containing transition metal elements. technical background [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 pyrolysis is one of its important uses, mainly to prepare high temperature resistant and oxidation resistant silicon carbide ceramic fibers, or to prepa...

Claims

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Application Information

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IPC IPC(8): C08G77/60C25B3/00C04B35/565
Inventor 高孟姣陈来花永盛张家宝任慕苏孙晋良
Owner SHANGHAI UNIV
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