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Preparation method of boron carbide precursor with high boron content

A boron carbide and precursor technology, applied in the field of preparation of high boron content polyboron carbide precursor, can solve the problems of staying in theoretical simulation, lack of boron carbide precursor, lack of boron carbide hollow microsphere preparation process, etc.

Active Publication Date: 2015-09-09
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the use of boron carbide as a target pellet material is still in the theoretical simulation stage. The main problem is the lack of a suitable preparation process for boron carbide hollow microspheres. One of the most basic problems is the lack of a suitable boron carbide precursor.

Method used

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  • Preparation method of boron carbide precursor with high boron content
  • Preparation method of boron carbide precursor with high boron content
  • Preparation method of boron carbide precursor with high boron content

Examples

Experimental program
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Effect test

Embodiment 1

[0041] This embodiment includes the following steps:

[0042] (1) In a 3L glass round bottom flask with a stirring and heating device, add 1000g of toluene and 100g of decaborane; then add 1,5-hexadiene, decaborane and 1,5-hexadiene moles The ratio is 1:2, the reactor is repeatedly evacuated and filled with dry nitrogen three times, and the nitrogen is selected as high-purity nitrogen with a purity of 99.999% to remove the air and moisture in it;

[0043] (2) Add the catalyst to the reactor, the catalyst is selected from (Cp) 2 Ti(CO) 2 , (Cp) 2 Ti(CO) 2 The molar ratio of catalyst to decaborane is 1:5;

[0044] (3) Raise the temperature to 120°C at a heating rate of 1°C / min, continue to stir the reaction, the stirring rate is 60r / min, and react for 96h; the product that has completed the reaction is poured into a round-bottomed flask, and the solvent is removed by rotary evaporation to obtain viscous thick liquid;

[0045] (4) take sherwood oil as eluting agent, the vis...

Embodiment 2

[0054] This embodiment includes the following steps:

[0055] (1) In a 3L glass round bottom flask with a stirring and heating device, add 1000g of toluene and 150g of decaborane; then add 1,4-cyclohexadiene, decaborane and 1,4-cyclohexanedi The ene molar ratio is 1:3, and the reactor is repeatedly evacuated and filled with dry nitrogen three times. The nitrogen gas is high-purity nitrogen with a purity of 99.999% to remove the air and moisture;

[0056] (2) Add the catalyst to the reactor, the catalyst is selected from (Cp) 2 Ti(CO) 2 , (Cp) 2 Ti(CO) 2 The molar ratio of catalyst to decaborane is 1:7.5;

[0057] (3) Heat up to 125°C at a heating rate of 1°C / min, continue to stir the reaction, the stirring rate is 90r / min, and react for 96h; the product that has completed the reaction is poured into a round-bottomed flask, and the solvent is removed by rotary evaporation to obtain viscous thick liquid;

[0058] (4) take sherwood oil as eluting agent, the viscous liquid t...

Embodiment 3

[0065] This embodiment includes the following steps:

[0066] (1) In a 3L glass round bottom flask with a stirring and heating device, add 1000g of xylene and 150g of decaborane; then add 1,5-cyclooctadiene, decaborane and 1,5-cyclooct The molar ratio of diene is 1:4. The reactor is repeatedly evacuated and filled with dry nitrogen three times. The nitrogen gas is high-purity nitrogen with a purity of 99.999% to remove the air and moisture;

[0067] (2) Add the catalyst to the reactor, the catalyst is selected from (Cp) 2 Ti(CO) 2 , (Cp) 2 Ti(CO) 2 The molar ratio of catalyst to decaborane is 1:7.5;

[0068] (3) Heat up to 125°C at a heating rate of 2°C / min, continue to stir the reaction, the stirring rate is 90r / min, and react for 120h; the product that has been reacted is poured into a round-bottomed flask, and the solvent is removed by rotary evaporation to obtain viscous thick liquid;

[0069] (4) take sherwood oil as eluting agent, the viscous liquid that step (3) o...

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Abstract

A preparation method of a boron carbide precursor with high boron content comprises the steps of: (1) adding a solvent in a reactor, then adding decaborane and diene organic compound, and vacuumizing and drying the reactor; (2) adding a catalyst to the reactor; (3) heating, stirring continuously for reaction under nitrogen atmosphere protection, evaporating the reaction products to remove the solvent, to obtain a viscous liquid; (4) rinsing with n-hexane or petroleum ether and removing residual catalyst and solvent in the obtained viscous liquid, to obtain a monomer; (5) placing the monomer in the reactor, and adding a solvent and a catalyst; (6) repeatedly vacuumizing the reactor; (7) heating and continuously stirring for reaction under a nitrogen atmosphere protection; and (8) removing the solvent in the reaction products. The boron carbide precursor prepared by the invention has high ceramic yield and high boron content, and is applicable to the preparation of boron carbide capsule for nuclear fusion, as well as the preparation of high performance carbide matrix composite.

Description

technical field [0001] The invention relates to a preparation method of a polyboron carbide precursor with high boron content. Background technique [0002] Laser-driven inertial confinement fusion mainly uses high-energy laser drivers to heat and compress fusion fuel hollow microspheres (target pellets) to high temperature and high density in a very short time, so that they can be "ignited" in the center, and the subsequent nuclear reaction can be controlled by ignition. Nuclear fusion, so as to obtain clean fusion energy. As a deuterium-tritium fuel and diagnostic gas container, the design and preparation technology of the target pellet has always been the core technology in the research of laser inertial confinement fusion. [0003] According to materials, the current main target pellet systems mainly include hollow glass microspheres, hollow plastic microspheres, hollow Be-Cu microspheres, etc. And through a variety of computing software, such as ILESTA (Osaka Universi...

Claims

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Application Information

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IPC IPC(8): C01B31/36
Inventor 简科王浩王军陈舟邵长伟黄坚苟燕子
Owner NAT UNIV OF DEFENSE TECH
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