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A kind of method for preparing borazine

A borazane and nitrogen filling technology, which is applied in the field of preparing borazane, can solve the problems of low temperature, reduced borazane yield, inability to produce borazane with high yield and high yield, etc., and achieves high yield , the effect of major economic and social benefits

Active Publication Date: 2021-03-09
北京玻钢院复合材料有限公司
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  • Application Information

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Problems solved by technology

The mainstream preparation method of borazine at present is the synthetic method (Inorg.Chem., 1995.34 (4): 1002-1003) of using sodium borohydride and ammonium sulfate to react in tetraethylene glycol dimethyl ether reported by Senddon et al. , but this method needs to react at a temperature of 120-140°C for 3 hours. Since the product borazine has high reactivity, when the temperature exceeds 70°C, the borazine molecules pass through highly active boron-hydrogen bonds (B-H) / nitrogen Hydrogen bond (N-H) reaction occurs self-polymerization, forming white oligomer solid, so that the yield and purity of borazine in the product are greatly reduced, and when using this method to expand the concentration of reactant, the intermolecular concentration of borazine The polymerization reaction is more violent, so that the output of borazine is greatly reduced when the production volume is large
National University of Defense Technology Li Junsheng and others reported the method of using aluminum trichloride as a catalyst to catalyze the reaction of sodium borohydride and ammonium sulfate at 45 °C in tetraethylene glycol dimethyl ether solvent to prepare borazine (Eur.J. Inorg.Chem., 2010,1763-1766), the method catalyzes the reaction of sodium borohydride and ammonium sulfate by adding an aluminum trichloride catalyst, and at a lower temperature of 45°C, a higher conversion is ensured rate, and can effectively avoid the self-polymerization of borazine, but the preparation method has a low temperature, which is not conducive to the efficient collision of borohydride compounds and ammonium salts. Once the amount of a single batch of reactants is increased or the concentration of reactants is enlarged, the reaction The conversion rate of substance and the productive rate of product can reduce greatly, can't guarantee high yield under the situation of single batch high production capacity, the yield of borazine is the borazine prepared by single batch of 60~67%. It is only at the gram level, which cannot be used for high-yield and high-yield production of borazine, and cannot meet the engineering needs of borazine as a precursor to prepare continuous fiber-reinforced boron nitride ceramic matrix composites

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  • A kind of method for preparing borazine
  • A kind of method for preparing borazine
  • A kind of method for preparing borazine

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Embodiment 1

[0029]A kind of method for preparing borazine described in the present embodiment, concrete steps are as follows:

[0030] The first step, mix 22kg tetrahydrofuran and 22kg tetraethylene glycol dimethyl ether, and cool to 0°C, add 28kg ammonium sulfate and 14.5kg sodium borohydride, vacuumize the reaction system, fill it with nitrogen, vacuumize it, and fill it with nitrogen 1. Vacuumize and fill with nitrogen to replace the air in the system, then add liquid ammonia with a molar mass of 1% borohydride ion, and fully stir for 3 hours;

[0031] The second step is to raise the temperature of the reaction system to 25°C and fully stir the reaction for 2.5h;

[0032] The third step is to raise the temperature of the reaction system to 60°C, vacuumize the reaction system while raising the temperature, and fully stir the reaction at 60°C for 3 hours, and collect the gas generated by the reaction;

[0033] The fourth step is to use a cold trap to cool the gas generated by the reacti...

Embodiment 2

[0037] A kind of method for preparing borazine described in the present embodiment, concrete steps are as follows:

[0038] The first step, mix 29kg tetrahydrofuran and 58kg tetraethylene glycol dimethyl ether, and cool to 0°C, add 32kg ammonium sulfate and 14.5kg sodium borohydride, vacuumize the reaction system, fill it with nitrogen, vacuumize it, and fill it with nitrogen 1. Vacuumize and fill with nitrogen to replace the air in the system, then add liquid ammonia with a molar mass of 6% borohydride ion, and fully stir and react for 1.5h;

[0039] The second step is to raise the temperature of the reaction system to 30°C and fully stir the reaction for 0.5h;

[0040] The third step is to raise the temperature of the reaction system to 80°C, vacuumize the reaction system while raising the temperature, and fully stir the reaction at 80°C for 1.5h, and collect the gas generated by the reaction;

[0041] The fourth step is to use a cold trap to cool the gas generated by the r...

Embodiment 3

[0045] A kind of method for preparing borazine described in the present embodiment, concrete steps are as follows:

[0046] The first step, mix 44kg tetrahydrofuran and 22kg tetraethylene glycol dimethyl ether, and cool to 0°C, add 35.4kg ammonium sulfate and 14.5kg sodium borohydride, vacuumize the reaction system, fill with nitrogen, vacuumize, fill Nitrogen, vacuumize, and fill with nitrogen to replace the air in the system, then add liquid ammonia with a molar mass of 3% borohydride ions, and fully stir the reaction for 0.5h;

[0047] In the second step, the temperature of the reaction system is raised to 20°C, and the reaction is fully stirred for 5 hours;

[0048] The third step is to raise the temperature of the reaction system to 100°C, vacuumize the reaction system while raising the temperature, and fully stir the reaction at 100°C for 1.5h, and collect the gas generated by the reaction;

[0049] The fourth step is to use a cold trap to cool the gas generated by the ...

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Abstract

The invention provides a method for preparing borazine, comprising: the first step, dissolving ammonium salt and borohydride in a solvent, then adding liquid ammonia, in an inert atmosphere protection, at a temperature not higher than 0°C The reaction time is 0.5-3h; the second step is to heat up the mixture obtained in the first step to 20-30°C for 0.5-5h; the third step is to heat up the mixture obtained in the second step to 60-100°C while the reaction system Vacuumize, and then react at 60-100°C for 1-3h to obtain borazine. The method for preparing borazine can realize high-yield and high-yield production of borazine, can be used for industrial production of borazine, and can meet borazine as a precursor to prepare continuous fiber-reinforced boron nitride ceramics Engineering needs of matrix composites.

Description

technical field [0001] The invention belongs to the technical field of inorganic material synthesis, and in particular relates to a method for preparing borazine. Background technique [0002] Boron nitride (hexagonal boron nitride) is a strong covalent bond compound with excellent high temperature resistance, oxidation resistance, ablation resistance, thermal shock resistance, chemical corrosion resistance and good high temperature dielectric and wave transmission properties, such as nitriding Boron does not decompose at high temperatures, only sublimes above 3000 ° C, and has a very low dielectric constant and loss tangent, and can maintain stable electrical properties in a wide temperature range. It is a high temperature resistant wave transparent radome material of choice. In the field of high-temperature wave-transmitting materials, compared with silica-based wave-transmitting composite materials, nitride-based wave-transmitting composite materials have better mechanic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/14
CPCC01B35/146C01P2002/87C01P2002/89
Inventor 彭喆李松高龙飞肖沅渝张雪梅路秋勉万业强安楠
Owner 北京玻钢院复合材料有限公司
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