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Polymetalcarbosilane, and preparation method and application thereof

A carbosilane and metal technology, applied in the field of polymetallic carbosilane and its preparation, can solve the problems of long reaction process, long time consumption, harsh process conditions, etc., and achieve the effects of low preparation cost, simple reaction steps and high product conversion rate

Active Publication Date: 2014-12-17
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are mainly the defects of long reaction process, long time consumption, harsh process conditions and the formation of a large number of by-products

Method used

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  • Polymetalcarbosilane, and preparation method and application thereof
  • Polymetalcarbosilane, and preparation method and application thereof
  • Polymetalcarbosilane, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] At room temperature and under the protection of nitrogen, add 12 grams of Na flakes and 250 mL of toluene into a 500 mL four-neck flask, stir at 110°C for 5 minutes at high speed to beat the sodium flakes into sodium sand, stop stirring, cool down to 100°C, and add 20.46 grams (0.07 mol) zirconocene dichloride, slowly drop in 27.10 g (0.21 mol) dichlorodimethylsilane, then stir for 5 hours under nitrogen protection and heating at 100°C until the solution is neutral, stop heating, and naturally cool to room temperature , to obtain solution G1. At -0.1MPa and 60°C, use a rotary evaporator to remove the toluene solvent in solution G1 to obtain 24.35 grams of dark brown viscous polymer, i.e. polyzirconium carbosilane A1, with a yield of 88.03wt% (based on the obtained polymetallic The theoretical yield of carbosilane is used as a basis for calculation).

[0044] Adopt KBr tablet method to carry out infrared spectroscopic analysis to solid product A1, the result is as follo...

Embodiment 2

[0049] At room temperature, under the protection of nitrogen, 12.88 grams of metal K and 150 mL of xylene were added to a 500 mL four-neck flask, and 4.38 grams (0.015 mol) of zirconocene dichloride was added under stirring conditions at 60°C, and 28.67 grams ( 0.15mol) of dichloromethylphenylsilane, then stirred at 60°C for 5 hours until the clear liquid was neutral, stopped heating, and naturally cooled to room temperature to obtain solution G2. The solvent in solution G2 was removed to obtain 20.24 g of a viscous polymer, namely polyzirconium carbosilane A2, with a yield of 87.13%.

[0050] Adopt KBr tabletting method to carry out infrared spectroscopic analysis to this viscous polymer A2, the result is as follows image 3 As shown, at wavenumber 1448cm -1 , wave number 1080cm -1 The absorption peak at corresponds to the absorption peak of cyclopentadienyl in zirconocene; at wavenumber 2091cm -1 place, wave number 879cm -1 The absorption peak at corresponds to the absor...

Embodiment 3

[0054] At room temperature and under the protection of nitrogen, 11.5 grams of Na and 280 mL of xylene were added to a 500 mL four-necked flask, and 2.49 grams (0.01 mol) of titanocene dichloride was added under stirring conditions at 110°C, and 25.81 grams (0.2 mol) dichlorodimethylsilane, and then stirred at 140° C. for 8 hours until the solution was neutral, then stopped heating, and naturally cooled to room temperature to obtain solution G3. The solvent in solution G3 was removed to obtain 10.2 g of a viscous polymer, namely polytitacarbosilane A3, with a yield of 76.23%.

[0055] The solid product A3 was analyzed by infrared spectroscopy using the KBr tablet method, and the results showed that at wavenumber 1452cm -1 , wave number 1080cm -1 The absorption peak at corresponds to the absorption peak of cyclopentadienyl in zirconocene; at wave number 2089cm -1 place, wave number 877cm -1 The absorption peak at corresponds to the absorption peak of the Si-H bond; wavenumbe...

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Abstract

The invention relates to polymetalcarbosilane, and a preparation method and an application thereof. The structural formula of the polymetalcarbosilane is shown in the specification. In the formula, R is a methyl group, an ethyl group, a propyl group, a vinyl group, a chloromethyl group, a phenyl group or a phenylethyl group; M is Ti, Zr or Hf; and m is an integer not less than 1, n is an integer not less than 0, and Cp1 and Cp2 respectively represent a cyclopentadienyl group or a substituted cyclopentadienyl group. The method for generating polymetalcarbosilane through catalyzing an organosilane addition polymerization reaction by metallocene has the advantages of adjustability of the content of metals in polymer, simple reaction step, mild reaction conditions and low preparation cost. The polymetalcarbosilane undergoes heat treatment at above 1100DEG C in inert atmosphere to form highly pure SiC.MC diphase ceramic.

Description

technical field [0001] The present invention generally relates to polymetallocarbosilane and its preparation method and application, in particular to polymetallocarbosilane (Ti, Zr, Hf) and its preparation method and application. Background technique [0002] SiC ceramics have excellent properties such as high strength, high modulus, high temperature resistance, corrosion resistance, oxidation resistance, low density, high thermal conductivity, small thermal expansion coefficient, and good wear resistance. Has a wide range of applications. [0003] The preparation of SiC mainly includes inorganic method and organic precursor method. Among them, the main steps of preparing SiC by the organic precursor method are: preparing polydimethylsilane or six-membered ring body through the condensation method of alkali metal or alkaline earth metal, and then preparing polydimethylsilane and six-membered ring body in an argon atmosphere After high temperature and high pressure treatmen...

Claims

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Application Information

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IPC IPC(8): C08G77/60C04B35/571C04B35/622
Inventor 张伟刚戈敏田跃龙于守泉吕晓旭
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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