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Method for preparing liquid anaerobic polyzirconocarbosilane

A polyzirconium carbosilane, an oxygen-free technology, applied in the field of compound preparation, can solve the problems of uneven dispersion of zirconium elements, low ceramic resistivity, low ceramic yield, etc., to achieve low resistivity, high dielectric loss, Ease of engineering

Inactive Publication Date: 2015-03-25
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The prepared polyzirconium carbosilane can be used as a precursor for the preparation of zirconium-containing silicon carbide ceramic matrix composites by polymer impregnation cracking method, which can improve the existing polytitania carbosilane containing oxygen, uneven dispersion of zirconium elements, and ceramics Low yield and other issues, while making the prepared ceramics have lower resistivity and higher dielectric loss

Method used

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  • Method for preparing liquid anaerobic polyzirconocarbosilane
  • Method for preparing liquid anaerobic polyzirconocarbosilane
  • Method for preparing liquid anaerobic polyzirconocarbosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Under the protection of an inert atmosphere, put 92.0g of chloromethyltrichlorosilane, 40.9g of (chloromethyl)methyldichlorosilane, 10.89g of dichlorozirconocene and 800g of anhydrous tetrahydrofuran in a reaction flask 36.0g of magnesium was added in batches and mechanically stirred; after the magnesium was added, the reaction was kept at 50°C for 12h.

[0024] (2) Under the protection of an inert atmosphere, 28.5 g of lithium aluminum hydride was added in batches to the reaction mixture obtained in step (1), stirred mechanically, and reacted at 50° C. for 12 hours.

[0025] (3) Under the protection of an inert atmosphere, add about 1600g of n-hexane to the reaction material obtained in step (2), stir it mechanically for 1 hour, let it stand for 0.5 hours, separate the upper organic phase, and remove the organic solvent to obtain light dark green viscous Thick liquid product, 76.2% yield.

[0026] Depend on Figure 1~3 The nuclear magnetic resonance spectrum (1H-...

Embodiment 2

[0028] (1) Under the protection of an inert atmosphere, put 46.0g of chloromethyltrichlorosilane, 40.9g of (chloromethyl)methyldichlorosilane, 7.4g of dichlorozirconocene and 500g of anhydrous ether in the reaction flask 18.0g of magnesium was added in batches and mechanically stirred; after the magnesium was added, the reaction was kept at 80°C for 6h.

[0029] (2) Under the protection of an inert atmosphere, 16.9 g of sodium aluminum hydride was added in batches to the reaction material obtained in step (1), stirred mechanically, and reacted at 60° C. for 36 hours.

[0030] (3) Under the protection of an inert atmosphere, add about 500g of heptane to the reaction material obtained in step (2), stir mechanically for 0.5h, then let it stand for 0.5h, separate the upper organic phase, remove the organic solvent, and obtain light ink Green viscous liquid product, yield 77.5%.

[0031] Through nuclear magnetic resonance data, it is confirmed that the liquid product is an oxygen-...

Embodiment 3

[0033] (1) Under the protection of an inert atmosphere, mix 92.0g of chloromethyltrichlorosilane, 40.9g of (chloromethyl)methyldichlorosilane, 6.6g of dichlorozirconocene and 1000g of anhydrous ethylene glycol dimethyl ether The solution was placed in a reaction bottle, and 19.2 g of magnesium was added in batches, and mechanically stirred; after the magnesium was added, the reaction was kept at 100° C. for 2 hours.

[0034] (2) Under the protection of an inert atmosphere, 18.5 g of lithium aluminum hydride was added in batches to the reaction material obtained in step (1), stirred mechanically, and reacted at 80° C. for 12 hours.

[0035] (3) Under the protection of an inert atmosphere, add about 500g of petroleum ether to the reaction material obtained in step (2), stir mechanically for 0.5h, then let it stand for 0.5h, separate the upper organic phase, remove the organic solvent, and obtain light ink Green viscous liquid product, yield 80.3%.

[0036] Through nuclear magne...

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Abstract

The invention relates to a preparation method of a compound, in particular to a method for preparing liquid anaerobic polyzirconocarbosilane, relates to a preparation method of a compound, and provides a method for directly preparing the liquid anaerobic polyzirconocarbosilane through binary or ternary polymerization of chloromethylsilane and zirconocene dichloride. The method comprises the steps as follows: 1), under the protection of an inert atmosphere, the chloromethylsilane and the zirconocene dichloride are mixed simultaneously and dissolved in absolute ether; 2), magnesium metals are added into a mixed solution obtained in the step 1) in batches for reaction; 3), under the protection of the inert atmosphere, a reducing agent is added in batches into a reaction mixed material obtained in the step 2) for reaction; and 4), under the protection of the inert atmosphere, an organic solvent is added into a reaction mixed material obtained in the step 3), an organic phase is extracted, standing is performed, an upper-layer organic phase is separated, the organic solvent is removed through filtration, and the liquid anaerobic polyzirconocarbosilane is obtained.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for preparing liquid oxygen-free polyzirconium carbosilane. 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, it is a typical microwave transmission material (Journal of Inorganic Materials, 2006, 21:103-108). To make silicon carbide ceramics an excellent dielectric absorbing material, the resistivity must be reduced and the dielectric loss increased. Introducing heterogeneous elements such as titanium and zirconium into the polycarbosilane precursor can significantly reduce the resistivity of silicon carbide ceramics, increase the dielectric loss, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60C04B35/565
Inventor 余兆菊闵浩杨乐周聪詹俊英郑强夏海平陈立富
Owner XIAMEN UNIV
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