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Preparation method for boron carbide precursor

A technology of precursors and boron carbide, which is applied in the field of preparation of boron carbide precursors, can solve the problems of poor solubility, low yield and high production cost of boron carbide precursors, and achieve good solubility, low price and low manufacturing cost Effect

Inactive Publication Date: 2013-10-16
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantages of the existing precursor conversion method are: high production cost, poor solubility of the prepared boron carbide precursor, and low yield

Method used

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  • Preparation method for boron carbide precursor
  • Preparation method for boron carbide precursor

Examples

Experimental program
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Effect test

Embodiment 1

[0021] This embodiment includes the following steps:

[0022] (1) Take 40ml of borane complex and 20g of 1,5-hexadiene for later use;

[0023] (2) Add the 1,5-hexadiene described in step (1) into a 250ml three-necked flask with a stirring and distillation device; then vacuumize the three-necked flask and fill it with dry nitrogen until the pressure gauge returns to zero, repeat three times, To get rid of the air and moisture in it, and then pre-cool the reactor to -10°C;

[0024] (3) In the reactor described in step (2), add the borane described in step (1); 2 Under the protection of the atmosphere, the reaction was continuously stirred at room temperature, the stirring rate was 240r / min, and the reaction was carried out for 7h;

[0025] (4) in N 2 Under the protection of the atmosphere, the temperature of the system was raised to 260°C at a heating rate of 2°C / min, and the solvent component in the system was distilled off under reduced pressure; cooled to room temperature,...

Embodiment 2

[0028] (1) Take 40ml of pentaborane and 20g of 1-octene for later use;

[0029] (2) In a 250ml three-necked flask with a stirring and distillation device, add 1-octene described in step (1); then vacuumize the three-necked flask, fill it with dry nitrogen until the pressure gauge returns to zero, and repeat it three times to eliminate the air and moisture, and then pre-cool the reactor to -5°C;

[0030] (3) In the reactor described in step (2), add the pentaborane described in step (1); 2 Under the protection of the atmosphere, the reaction was continuously stirred at room temperature, the stirring rate was 200r / min, and the reaction was carried out for 10h;

[0031] (4) in N 2 Under the protection of the atmosphere, the temperature of the system was raised to 240°C at a heating rate of 3°C / min, and the solvent in the system was removed by distillation under reduced pressure; cooled to room temperature, it was ready.

[0032] After analysis, the obtained polymer mainly cont...

Embodiment 3

[0034] (1) Take 60ml of borane complex, 20g of 1,5-hexadiene, 10g of 1-octene, set aside;

[0035] (2) Add 1-octene and 1,5-hexadiene described in step (1) into a 250ml three-necked flask with a stirring and distillation device; then vacuumize the three-necked flask and fill it with dry nitrogen until the pressure gauge returns Zero, repeat three times to get rid of the air and moisture, and then pre-cool the reactor to -15°C;

[0036] (3) In the reactor described in step (2), add the borane complex described in step (1); 2 Under the protection of the atmosphere, the reaction was continuously stirred at room temperature, the stirring rate was 180r / min, and the reaction was carried out for 11h;

[0037] (4) in N 2 Under the protection of the atmosphere, the temperature of the system was raised to 250°C at a heating rate of 2°C / min, and the solvent components in the system were removed by distillation under reduced pressure; cooled to room temperature, and the product was read...

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Abstract

A preparation method for a boron carbide precursor includes the steps: (1) taking borane, mono-functional olefin and bi-functional olefin in the mass ratio of 1: (0.1-20): (0.1-20); (2) adding the mono-functional olefin or / and the bi-functional olefin into a reactor with stirring and distilling devices, repeatedly vacuumizing and filling dried nitrogen into the reactor for at least three times, and pre-cooling the reactor to the temperature ranging from -2 DEG C to -35 DEG C; (3) adding the borane, and continuously carrying out stirring reaction at the room temperature under the protection of the N2 atmosphere, wherein the stirring rate is 60-240r / min, and reaction time ranges from 2h to 72h; and (4) increasing the temperature of the system at the temperature rise rate of 0.1-30 DEG C / min to 30-400 DEG C, removing solvent composition in the system by means of reduced pressure distillation, and cooling to the room temperature so that the boron carbide precursor is prepared. The preparation method for the boron carbide precursor is low in production cost, and the boron carbide precursor prepared by the method is good in solubility and high in productivity.

Description

technical field [0001] The invention relates to a preparation method of a boron carbide precursor. Background technique [0002] Currently, the widely accepted boron carbide model is: B 11 The icosahedron composed of C and the rhombohedron composed of C-B-C chains. Since carbon atoms and boron atoms have similar radii, there is a homogeneous substitution in the same phase, so the carbon-boron ratio in boron carbide is not fixed, and mostly changes around 1:4, and when the carbon-boron ratio=1:4, each of the boron carbide item performs best. Boron carbide (B 4 C) is a compound with strong covalent bonds (covalent bonds account for more than 90%), high melting point (2450 ° C), low density (2.519g / cm 3 , is the lightest material in ceramic materials), and has a high modulus of elasticity, which is ideal for engineering ceramics, aerospace, military armor and nuclear industry. Because its hardness is second only to diamond and cubic boron nitride, it ranks third in the cur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/08C04B35/563
Inventor 王浩任武荣王军刘贵宝简科
Owner NAT UNIV OF DEFENSE TECH
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