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Synthetic method of triassic boron nitride

A synthesis method and technology of boron nitride, applied in the direction of nitrogen compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of harsh reaction conditions, many operation steps, and no reaction yield given

Inactive Publication Date: 2012-11-21
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method has harsh reaction conditions, many operating steps, and no specific reaction yield is given.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0012] At a temperature of 15°C to 20°C, add 0.03 mole of trimethylsilazide azide into a 50ml three-necked flask, and slowly add 15g of ethyl acetate solution containing 0.01 mole of boron tribromide dropwise under stirring, until the addition is complete. After the ethyl acetate solution of boron is stirred at a temperature of 5°C to 10°C, react for 6 hours, distill the reaction solution under normal pressure, collect fractions at 42°C to 45°C, and obtain boron triazide as a pale yellow liquid with a yield of 63%.

Embodiment 2

[0014] At a temperature of 25°C to 30°C, add 0.03 mole of trimethylsilazide azide into a 50ml three-necked flask, and slowly add 15g of ethyl acetate solution containing 0.01 mole of boron tribromide dropwise under stirring, until the addition is complete. After the ethyl acetate solution of boron was stirred at a temperature of 25°C to 30°C, reacted for 7 hours, distilled the reaction solution under normal pressure, collected fractions at 42°C to 45°C, and obtained light yellow liquid boron triazide with a yield of 65 %.

Embodiment 3

[0016] At a temperature of 20°C to 25°C, add 0.035 mole of trimethylsilazide azide into a 50ml three-necked flask, slowly add 15g of acetonitrile solution containing 0.01 mole of boron tribromide dropwise under stirring, and finish adding 0.01 mole of boron tribromide After the acetonitrile solution, react for 6 hours under stirring at a temperature of 45°C-50°C, distill the reaction solution under normal pressure, collect fractions at 42°C-45°C to obtain a light yellow liquid, and the yield of boron triazide is 79%.

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Abstract

The invention discloses a synthetic method of triassic boron nitride. The method comprises the steps of: adding trimethyl azide silane into a reactor at 15-30 DEG C; adding an organic solvent containing boron tribromide under agitation; reacting for 2-9 hours at 0-70 DEG C after the organic solvent containing boron tribromide is added; distilling reaction liquid at normal pressure; collecting fraction at 42-45 DEG C; and obtaining triassic boron nitride, wherein the molar ratio of boron tribromide to triassic boron nitride is 1 to 3-4, and the organic solvent is ethyl acetate, trichloromethane or acetonitrile. The synthetic method is mainly applied to synthesis of triassic boron nitride.

Description

technical field [0001] The invention relates to a synthesis method of boron triazide, belonging to the field of chemical synthesis. Background technique [0002] Boron triazide has the characteristics of high nitrogen content, its nitrogen content is as high as 91.97%, and it has a strong energy storage capacity. In the field of military industry, it can be used as a high-efficiency detonating explosive, and can also be used as a raw material for energetic adhesives, energetic bonding agents, and high-energy-density materials. In the field of civil industry, it can be used to prepare high-hardness material cubic boron nitride (hardness second only to diamond), high-wear-resistant material hexagonal boron nitride film and wide-bandgap semiconductor boron nitride material, which has become one of the hotspots in the field of new materials. one. In 1954, people such as E.Wiberg disclosed a kind of synthetic method of boron triazide on the 497th page of "Naturforsch" volume 96...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064
Inventor 李陶琦丁可伟葛忠学毕富强刘庆刘愆苏海鹏陈晓芳许诚郝晓春卜建华肖啸
Owner XIAN MODERN CHEM RES INST
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