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Method of preparing liquid anaerobic polyferrocarbosilane

A polycarbosilane and oxygen-free technology, which is applied in the field of compound preparation, can solve the problems of insoluble and infusible, uneven dispersion of iron elements, etc., and achieve the effects of high yield, easy engineering and simple process

Inactive Publication Date: 2013-08-21
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The prepared liquid oxygen-free polyironcarbosilane can be used as a precursor for the preparation of iron-containing silicon carbide ceramic matrix composites by polymer dipping and cracking, and can improve the existing polyironcarbosilane insoluble, infusible, oxygen-containing, Problems such as uneven dispersion of iron element

Method used

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  • Method of preparing liquid anaerobic polyferrocarbosilane
  • Method of preparing liquid anaerobic polyferrocarbosilane
  • Method of preparing liquid anaerobic polyferrocarbosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Under the protection of an inert atmosphere, vinyl ferrocene is added to liquid hyperbranched polycarbosilane, and the mass ratio of vinyl ferrocene to liquid hyperbranched polycarbosilane is 1%;

[0019] (2) Under the protection of an inert atmosphere, the mixture described in step (1) was stirred in an oil bath at 70° C. for 48 hours to obtain a liquid oxygen-free polyferrocarbosilane.

[0020] The average structural formula of the raw material liquid hyperbranched polycarbosilane used is—[SiH 1.6 (CH 3 ) 0.3 —(CH 2 CH=CH 2 ) 0.1 —CH 2 ] n —, measure the molecular weight and molecular weight distribution of liquid hyperbranched polycarbosilane by gel permeation chromatography (GPC), the eluent is tetrahydrofuran, the number average molecular weight is 500, and the dispersion coefficient is 1.7; the liquid anaerobic type obtained after the reaction The number-average molecular weight of polyferrocarbosilane is 900, and the dispersion coefficient is 8.7 (see ...

Embodiment 2

[0022] (1) Under the protection of an inert atmosphere, vinyl ferrocene is added to the liquid hyperbranched polycarbosilane, and the mass ratio of vinyl ferrocene to liquid hyperbranched polycarbosilane is 10%;

[0023] (2) Under the protection of an inert atmosphere, the mixture described in step (1) was stirred in an oil bath at 30° C. for 48 hours to obtain a liquid oxygen-free polyferrocarbosilane.

[0024] The average structural formula of the raw material liquid hyperbranched polycarbosilane used is—[SiH 1.5 (CH 3 ) 0.5 —CH 2 ] n -, the number average molecular weight is 600, and the dispersion coefficient is 3.5; the number average molecular weight of the liquid oxygen-free polyironcarbosilane obtained after the reaction is 1000, and the dispersion coefficient is 4.5; the synthesis yield is 95.2wt%. The ceramic yield of liquid oxygen-free polycarbosilane 1200°C pyrolysis product was determined by thermogravimetric analysis (TGA) to be 83.2wt%, while the ceramic yie...

Embodiment 3

[0026] (1) Under the protection of an inert atmosphere, vinyl ferrocene is added to liquid hyperbranched polycarbosilane, and the mass ratio of vinyl ferrocene to liquid hyperbranched polycarbosilane is 20%;

[0027] (2) Under the protection of an inert atmosphere, the mixture described in step (1) was stirred in an ice-water bath at 0° C. for 36 hours to obtain a liquid oxygen-free polyferrocarbosilane.

[0028] The average structural formula of the raw material liquid hyperbranched polycarbosilane used is—[SiH 1.5 (CH 3 ) 0.3 (C≡CH) 0.2 —CH2 ] n -, the number average molecular weight is 600, and the dispersion coefficient is 3.5; the number average molecular weight of the liquid oxygen-free polyironcarbosilane obtained after the reaction is 1500, and the dispersion coefficient is 6.2; the synthesis yield is 85.3wt%. The ceramic yield of liquid oxygen-free polycarbosilane cracked at 1200°C was determined by thermogravimetric analysis (TGA) to be 84.2wt%, while the ceramic...

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Abstract

The invention discloses a method of preparing liquid anaerobic polyferrocarbosilane, relates to a preparation method of a compound, and provides a method of directly preparing liquid anaerobic polyferrocarbosilane by taking anaerobic vinyl ferrocene as an iron source to react with liquid hyperbranched polycarbosilane. The method comprises the steps that 1) vinyl ferrocene is added to liquid hyperbranched polycarbosilane under inert atmosphere protection, wherein a mass ratio of vinyl ferrocene to liquid hyperbranched polycarbosilane is 1-50%; and 2) a mixture obtained in Step 1) is stirred under the inert atmosphere protection, and liquid anaerobic polyferrocarbosilane is obtained. Prepared liquid anaerobic polyferrocarbosilane can serve as a precursor for preparing a ferrous silicon carbide ceramic matrix composite by a high polymer infiltration and pyrolysis method, and can solve the problems that existing polyferrocarbosilane is insoluble, infusible and oxygenous, and an iron element is disperse and nonuniform.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for preparing liquid oxygen-free polyironcarbosilane. Background technique [0002] Silicon carbide (SiC) ceramics prepared by polycarbosilane through the precursor conversion method are a class of high-performance ceramic materials with a wide range of uses (J.Am.Ceram.Soc., 2010,93:1805-1837; Polymer materials Science and Engineering, 2000, 16:7-12). But silicon carbide ceramics have a resistivity of 10 6 About Ω·cm, non-magnetic, is a typical microwave transmission material (Journal of Inorganic Materials, 2006, 21:103-108). To make silicon carbide ceramics have good wave-absorbing characteristics, the resistivity must be reduced and the dielectric loss or magnetic loss must be increased. Introducing heterogeneous elements such as iron, cobalt, and nickel into the polycarbosilane precursor can make the obtained silicon carbide ceramics have both electrical loss ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
Inventor 余兆菊杨乐周聪詹俊英闵浩郑强夏海平陈立富
Owner XIAMEN UNIV
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