Method for preparing liquid anaerobic polytitanocarbosilane

An oxygen-free polytitanocarbosilane technology, which is applied in the field of compound preparation, can solve the problems of uneven dispersion of titanium elements, low ceramic yield, high dielectric loss, etc., and achieve low resistivity, high dielectric loss, Ease of engineering

Inactive Publication Date: 2013-09-04
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The titanium element in the prepared polytitanium carbosilane is bonded to the main chain of the polymer molecule through chemical bonds, which realizes the dispersion of the titanium element at the atomic level, and can be used as a polymer impregnation cracking method to prepare titanium-containing silicon carbide ceramic matrix composites. The pr

Method used

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  • Method for preparing liquid anaerobic polytitanocarbosilane
  • Method for preparing liquid anaerobic polytitanocarbosilane
  • Method for preparing liquid anaerobic polytitanocarbosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Under the protection of an inert atmosphere, put 92.0g of chloromethyltrichlorosilane, 40.9g of (chloromethyl)methyldichlorosilane, 0.93g of titanocene dichloride and 500g 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 100°C for 2h.

[0029] (2) Under the protection of an inert atmosphere, 15.2 g of lithium aluminum hydride was added in batches to the reaction material obtained in step (1), stirred mechanically, and reacted at 100° C. for 2 hours.

[0030] (3) Under the protection of an inert atmosphere, add about 1000g of n-hexane to the reaction material obtained in step (2), after mechanical stirring for 0.5h, let it stand for 0.5h, separate the upper organic phase, remove the organic solvent, and obtain light ink Green viscous liquid product, yield 83.4%.

[0031] From the NMR spectrum ( 1 H-NMR, 13 C-NMR and 29 Si-NMR) to characterize ...

Embodiment 2

[0033] (1) Under the protection of an inert atmosphere, place 46.0g of chloromethyltrichlorosilane, 40.9g of (chloromethyl)methyldichlorosilane, 6.3g of titanocene dichloride and 500g of anhydrous ether in a 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 36h.

[0034] (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 12 hours.

[0035] (3) Under the protection of an inert atmosphere, add about 500g heptane to the reaction material obtained in step (2), after mechanical stirring for 0.5h, let it stand for 0.5h, separate the upper organic phase, remove the organic solvent, and obtain light ink Green viscous liquid product, yield 79.5%.

[0036] Through nuclear magnetic resonance data, it was confirmed that the liquid product was an ox...

Embodiment 3

[0038] (1) Under the protection of an inert atmosphere, mix 92.0g of chloromethyltrichlorosilane, 40.9g of (chloromethyl)methyldichlorosilane, 5.6g of titanocene dichloride 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.

[0039] (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.

[0040] (3) Under the protection of an inert atmosphere, add about 500g of petroleum ether to the reaction material obtained in step (2), after mechanical stirring for 0.5h, 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%.

[0041] Through nuclear ...

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Abstract

The invention discloses relates to a preparation method of a compound, in particular to a method for preparing liquid anaerobic polytitanocarbosilane, and provides a method for directly preparing the liquid anaerobic polytitanocarbosilane 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 polytitanocarbosilane is obtained.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for preparing a liquid oxygen-free polytitanocarbosilane. 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 a...

Claims

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Application Information

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IPC IPC(8): C08G79/00C08G77/60C04B35/571
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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