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Method for preparing polymerized boron silazane precursor

A technology for polyborosilazane and precursors is applied in the field of preparation of polyborosilazane precursors, which can solve the problems of cumbersome and complicated processes, unfavorable popularization and application, and high cost, and achieves simple reaction process, low cost and reliable source. Effect

Inactive Publication Date: 2008-03-26
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of synthetic route process is cumbersome and complicated, and the cost is high, which is not conducive to popularization and application.

Method used

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  • Method for preparing polymerized boron silazane precursor
  • Method for preparing polymerized boron silazane precursor

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) The 250ml three-neck flask with the electric stirring device in the reactor was repeatedly vacuumized and filled with dry nitrogen three times to remove the air and moisture therein, and then the reactor was pre-cooled to minus 10 degrees;

[0034] (2) Take 0.3mol (34.5g) of methylhydrogendichlorosilane and 0.15mol (17.6g) of boron trichloride into a three-necked flask protected by dry nitrogen with a syringe. The ammonia gas is put into the reaction system, and the system heats up rapidly, and produces a large amount of precipitation; Filter; (4) Place the filtrate obtained in step (3) in a reactor with a condenser tube, a cracking column, and a reflux device, and under the protection of dry nitrogen, slowly heat to carry out cothermal polycondensation, and the reactor temperature is 320°C , the temperature of the pyrolysis column was 450°C, and the temperature was kept for 3 hours; (5) The temperature of the system was lowered to 260°C, and the vacuum distillation...

Embodiment 2

[0041] (1) Same as Example 1; (2) Get 0.3mol (30.3g) of dichlorosilane and 0.3mol (29.0g) of methyl boron dichloride with a syringe and inject them into a three-necked flask protected by dry nitrogen successively, while stirring , while feeding ammonia with a purity of 99.999% into the reaction system, the system heats up rapidly and produces a large amount of precipitation; when the temperature no longer rises, stop the feeding of ammonia; (3) when the temperature of the system drops to room temperature , the system product is filtered in a nitrogen bag; (4) the filtrate obtained in step (3) is placed in a reactor with a condenser tube, a cracking column, and a reflux device, and slowly heated for co-heating under the protection of dry nitrogen Polycondensation, the temperature of the reactor is 270°C, the temperature of the cracking column is 420°C, and the temperature is kept for 2 hours; (5) the temperature of the system is lowered to 200°C, and the vacuum distillation is c...

Embodiment 3

[0043] (1) Same as Example 1; (2) Get 0.3mol (38.7g) of dimethyl dichlorosilane with a syringe, and inject 0.2mol (16.5g) of dichloroborohydroane into a three-necked flask protected by dry nitrogen, While stirring, feed methylamine with a purity of 99.999% into the reaction system, the system heats up rapidly and produces a large amount of precipitation, when the temperature no longer rises, stop the feed of methylamine; (3) until the temperature of the system drops to At room temperature, the system product is filtered in a nitrogen bag; (4) the filtrate obtained in step (3) is placed in a reactor with a condenser tube, a cracking column, and a reflux device, and slowly heated under the protection of dry nitrogen Thermal polycondensation, the temperature of the reactor is 270°C, the temperature of the cracking column is 440°C, and the temperature is kept for 2 hours; (5) The temperature of the system is reduced to 300°C, and the vacuum distillation is carried out for 30 minute...

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Abstract

The process of preparing polyborosilazane precursor with boroalkyl halide, silane halide and alkyl amine as initial material includes the following steps: mixing boroalkyl halide and silane halide in the molar ratio of 0.1-10 and alkyl amine in excessive amount to react; filtering the product to obtain filtrate as low molecular borosilazane; heating the low molecular borosilazane to polymerize and cooling to obtain polyborosilazane precursor. The polyborosilazane precursor has cheap material, simple reaction process, high yield, homogeneous element distribution in atom level, and effectively controlled machining performance and physical performance.

Description

technical field [0001] The invention relates to a preparation method of a polyborosilazane precursor. Background technique [0002] Multi-component ceramics containing Si, B, N, C and other elements have excellent high-temperature strength, high modulus, excellent high-temperature oxidation resistance and high-temperature creep resistance. Therefore, Si-B-N-C system ceramics are used in aviation, aerospace, weapons, Ships and other fields that require high strength, high modulus, high temperature resistance, oxidation resistance, thermal shock resistance, and high temperature creep resistance materials have important application prospects. [0003] Precursor conversion method is an effective way to prepare such ceramic materials. At present, the preparation methods of Si-B-N-C ceramic precursors mainly include polymer route and monomer route. [0004] The polymer route refers to modifying Si-N bond-containing polymers such as polysilazane with boron-containing compounds to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/515
Inventor 王军唐云李效东王浩
Owner NAT UNIV OF DEFENSE TECH
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