Preparation method of boron hydrogen nitrogen energy storage material

A technology of energy storage materials and hydrogen storage materials, which is applied in the production of hydrogen, etc., can solve the problems of boron hydrogen nitrogen material raw materials, low product purity, high processing cost, etc., and achieve high yield, high purity, and reduced pollution. Effect

Active Publication Date: 2013-11-06
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
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Problems solved by technology

[0005] The purpose of the present invention is to provide a method of high-capacity solid-state boron-hydrogen-nitrogen hydrogen storage material in order to solve the disadvantages of raw material risk, complex process, high processing cost, and low product purity in the traditional process of preparing boron-hydrogen-nitrogen materials

Method used

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  • Preparation method of boron hydrogen nitrogen energy storage material
  • Preparation method of boron hydrogen nitrogen energy storage material
  • Preparation method of boron hydrogen nitrogen energy storage material

Examples

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Effect test

Embodiment 1

[0026] (1) Add 1.01mol of (NH 4 ) 2 SO 4 Put it into a 5L three-necked reaction flask, which is equipped with a thermometer, a polytetrafluoroethylene stirring paddle, and a spherical reflux device. The top of the reflux pipe is connected with a moisture-proof tube. anhydrous solvent, stir for 30min;

[0027] (2) Add 2mol NaBH 4 Add to the ammonium salt solution in step (1), stir for 30 minutes, then heat up to 40°C, and react for 5 hours;

[0028] (3) The mixed solution in step (2) was filtered, and the filtrate was subjected to rotary evaporation to obtain 58 g of white solid powder, with a yield of 94%;

[0029] (4) Dissolve the white powder obtained in step (3) in tetrahydrofuran anhydrous solvent to form a saturated solution, add the saturated solution dropwise to petroleum ether solvent, when microcrystals appear, under the condition of -5°C After standing for 24 hours, a white crystalline product was obtained, and the crystallization was repeated 3 times; the cryst...

Embodiment 2

[0033] (1) Add 0.55mol of (NH 4 ) 2 CO 3 Add to the three-necked reaction flask filled with 2L 2-methylfuran anhydrous solvent, and install a spherical reflux condenser, thermometer and Teflon stirring paddle on the three-necked reaction flask, and stir for 30 minutes;

[0034] (2) Add 1mol NaBH 4 Add it to the ammonium salt solution in step (1), stir for 30 minutes, then raise the temperature to 42°C, and react for 4 hours;

[0035] (3) Filter the mixed solution in step (2), and perform rotary evaporation on the filtrate to obtain 29.32 g of white powder, with a yield of 95%;

[0036] (3) Dissolve the white solid powder in tetrahydrofuran anhydrous solvent to form a saturated solution, sublime in an oven at 60°C and a vacuum of 0.02 for 20h to obtain BNH 6 White crystals 21.91g, BNH 6 The purity reaches 99.4%.

Embodiment 3

[0038] (1) Add 0.26mol of (NH 4 ) 2 CO 3 Add it to a 1L four-necked reaction flask, which is equipped with a polytetrafluoroethylene stirring device, a thermometer, a feeding tube, and a spherical reflux device, and the top of the reflux tube is connected with a moisture-proof tube. Anhydrous solvent, stirring for 20min;

[0039] (2) Add 0.5mol LiBH 4 Add to the ammonium salt solution in step (1), stir for 30 minutes, heat up to 43°C, and react for 3.5 hours;

[0040] (3) The mixed solution of (2) was filtered, and the filtrate was subjected to rotary evaporation to obtain 14.5 g of white solid powder, with a yield of 94%;

[0041] (4) Dissolve the white solid powder obtained in step (3) in tetrahydrofuran anhydrous solvent to make a saturated solution, and sublimate the saturated solution in an oven with a temperature of 60°C and a vacuum of 0.02 for 12 hours to obtain white BNH 6 Crystalline product 12.6g, BNH 6 The purity reaches 99.6%.

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Abstract

Belonging to the preparation field of boron hydrogen nitrogen energy storage materials, the invention relates to a preparation method of a boron hydrogen nitrogen energy storage material. The preparation method provided in the invention specifically consists of the steps of: 1) adding an ammonium salt into an anhydrous solvent and conducting stirring; 2) adding a borohydride into the ammonium salt solution obtained in step 1), raising the temperature and letting them react; 3) performing filtration, and subjecting the filtrate to rotary evaporation, thus obtaining white solid powder; 4) dissolving the white solid powder in the anhydrous solvent, and conducting a recrystallization treatment so as to obtain a white crystal; and 5) subjecting the white crystal to vacuum drying, thus obtaining the boron hydrogen nitrogen energy storage material. The preparation method provided in the invention broadens the selection range of the ammonium salt, the reaction conditions are mild, the yield is high and can reach over 94%. The obtained product has high purity, which can reach a maximum of more than 99.9%. The method is of important significance for boosting practical application of the boron hydrogen nitrogen material. At the same time, the anhydrous solvent can be recycled, the cost is saved, and pollution to the environment is reduced.

Description

technical field [0001] The invention relates to a method for preparing boron-hydrogen-nitrogen energy storage materials, and belongs to the field of preparation of boron-hydrogen-nitrogen hydrogen storage materials. Background technique [0002] The energy problem is a major problem facing our country and the world today. With the development of the national economy and the deepening of urbanization, energy issues are increasingly restricting the development of the economy and the improvement of people's quality of life. At present, fossil fuels are the main body of energy. As a kind of non-renewable resources, using them as energy not only has low production efficiency, but also is accompanied by various forms of pollution. Hydrogen energy is a clean and efficient energy source, renewable, high energy density, and easy to convert into energy forms. It is considered as a bridge connecting fossil fuels and renewable resources. It is the most ideal energy carrier and has beco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B3/02
Inventor 刘吉平毕晓露
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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