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Synthesis of boron-contained silicone

A synthesis method and technology of polysilane, which is applied in the field of synthesis of boron-containing polysilane, can solve the problems of difficult control of reaction rate, severe reaction conditions, and lack of commercial production, and achieve high-temperature oxidation resistance improvement, simple operation, and easy control Effect

Inactive Publication Date: 2009-07-08
SHANGHAI UNIV
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  • Summary
  • 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 intense, the reaction rate is difficult to control, and the phenomenon of detonation often occurs
The two monomeric unsaturated organopolysilanes and borane compounds used in the technical route (2) have no commercial production in China

Method used

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  • Synthesis of boron-contained silicone
  • Synthesis of boron-contained silicone
  • Synthesis of boron-contained silicone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: In an electrochemical reaction flask equipped with a ventilation tube, a stirrer and a thermometer, add methylhydrogendichlorosilane and boron trifluoride ether solutions in different molar ratios. 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 gas bag of ammonia to neutralize the remaining Si-Cl bonds. At this time, observe the change of the thermometer in the reaction bottle, and the temperature will increase with the introduction of ammonia gas. When the thermometer shows a stable reading an...

Embodiment 2

[0031] Example 2: Using boron-containing polysilane as a precursor to prepare a C / C-B-SiC composite material containing a B-SiC matrix, and using H 2 -O2 The ablation properties of C / C and C / C-B-SiC composites were compared by flame method. The density is 1.19g cm -3 The C / C composite material has been impregnated three times, and the density has been increased to 1.50g cm -3 . The change of its density with the number of immersions is shown in Table 2. Figure 4 , Figure 5 The ablation experimental results of C / C-B-SiC composites after dipping three times are given, and the ablation results of C / C are also given for comparison. Density 1.19g·cm -3 The C / C sample was impregnated once to obtain 1.31g·cm -3 C / C-B-SiC, its line ablation rate and mass ablation rate are lower than the density of 1.5g cm -3 C / C. As the density of C / C-B-SiC composites increases, the linear ablation rate and mass ablation rate gradually decrease. When the density of the material increases fro...

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Abstract

The invention relates to a method for synthesizing boron-containing polysilane. The method of the invention adopts an electrochemical synthesis method, uses magnesium blocks as cathode and anode, and polymerizes dihalogen silane or trihalogen and allyl chloride in tetrahydrofuran solution to synthesize boron-containing polysilane. The boron-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 prepared boron-containing polysilane can obviously improve the high-temperature oxidation resistance of C / C composite materials, and is a kind of A kind of ceramic precursor with excellent performance. The method of the invention effectively solves the problems existing in the early research, and is beneficial 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 boron-containing polysilane. Background technique [0002] Polysilane is a kind of high polymer containing only silicon atoms in the chain skeleton, and its main chain is Si-Si bond. The delocalization of the Si-Si chain σ-bond electrons allows the Si-Si bond σ-electrons to move along the main chain to form a large conjugated system σ-conjugate bond. Its unique structure makes it exhibit unique properties in terms of solubility, thermal stability, UV absorption, thermochromism and fluorescence. Based on its unique properties, it has broad application prospects in photoresists, photoinitiators, waveguides, photoconductors and nonlinear optical materials. In addition, polysilane is used as SiC, Si 3 N 4 One of its uses is the preparation of silicon carbide ceramic materials by high temperature pyrolysis, mainly to prepare high temperature resistan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60C08G79/08
Inventor 吴市陈来钱林任慕苏孙晋良
Owner SHANGHAI UNIV
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