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Method for preparing ammonia borane by wet chemical process

An ammonia borane and wet chemical technology, applied in the field of ammonia borane preparation, can solve the problems of reducing the particle size of ammonium salt, low reaction efficiency, slow surface erosion of ammonium salt, etc. Effect

Inactive Publication Date: 2012-07-04
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the conventional solution stirring method does not help to reduce the particle size of the ammonium salt, the reaction can only be carried out slowly through the erosion of the solution on the surface of the ammonium salt, and the reaction efficiency is low

Method used

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  • Method for preparing ammonia borane by wet chemical process
  • Method for preparing ammonia borane by wet chemical process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Weigh 19 g of NaBH in an argon glove box 4 , 24.8 grams (NH 4 ) 2 CO 3 (Slight excess to avoid NaBH 4 excess and soluble in THF to make it difficult to separate from ammonia borane), and measure THF 500 milliliters. Put the three together into a self-designed ball mill jar (volume 2 liters). After sealing the tank body, put it into a planetary ball mill (Fischt PM-400), accurately control the temperature of the ball milling chamber at 45° C., and ball mill at 100 rpm for 45 minutes. The ball mill tank was connected with a pressure gauge, and the pressure in the tank was measured at 128psi. The amount of hydrogen calculated by the ideal gas equation was 0.5 mol, which confirmed that the reaction had been fully completed. The hydrogen in the tank was vented, and the white slurry was removed to a 600 ml centrifuge tank. After centrifugation at 3000r / min for 15min, the obtained supernatant was transferred to a 1-liter round-bottom bottle and placed in a rotary evapora...

Embodiment 2

[0018] Weigh the pre-milled NaBH in an argon glove box 4 1.9 g, (NH 4 ) 2 CO 3 2.5 grams (the ball milling condition is 200 rpm, the particle size of the sample is 100 nanometers), and 30 milliliters of THF is measured. The three were put together into a commercial autoclave (volume 100 ml). Seal the tank and connect it to a magnetic stirrer for stirring. At the same time, control the temperature of the reactor at 50°C. After 5 hours of reaction, connect the autoclave to the pressure gauge, measure the pressure in the tank at 60 psi, and calculate the amount of hydrogen with the help of the ideal gas equation. 0.0108mol, confirming that the degree of progress of the reaction is only 21.6%. It can be seen that the conventional stirring reaction is difficult to complete the preparation reaction even for the samples processed by ball milling. Although increasing the reaction temperature can further increase the reaction rate, it also brings the risk of ammonia borane produc...

Embodiment 3

[0020] Weigh 19 g NaBH4, 33.5 g (NH 4 ) 2 SO 4 (Slight excess to avoid NaBH 4 remaining and dissolved in THF), and measure 500 ml of THF. Put the three into a self-processed ball mill jar (volume 2 liters). After sealing the tank body, put it into a planetary ball mill (Fischt PM-400), accurately control the temperature of the ball milling chamber at 45° C., and ball mill at 100 rpm for 60 minutes. The ball mill tank was connected with a pressure gauge, and the pressure in the tank was measured at 128psi. The amount of hydrogen calculated by the ideal gas equation was 0.5 mol, which confirmed that the reaction had been fully completed. The hydrogen in the tank was vented, and the white slurry was removed to a 600 ml centrifuge tank. After centrifugation at 3000r / min for 15min, the obtained supernatant was transferred to a 1-liter round-bottom bottle and placed in a rotary evaporator for distillation under reduced pressure. After THF was removed, white ammonia borane crys...

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Abstract

The invention provides a new method for preparing ammonia borane, which synthesizes ammonia borane with high efficiency by using an ammonium salt and a boron hydride as raw materials and an organic solvent as a reaction medium and by a wet chemical process. The method is characterized in that the chemical reaction between the starting raw materials is directly promoted by wet-process heating ball milling to form ammonia borane. Subsequently, ball milled pulp is subjected to centrifugal separation and reduced-pressure distillation, the clear liquid is obtained, and thus, high-purity ammonia borane crystal is obtained. The centrifugally separated and ball milled solid is subjected to multiple times of solvent extraction to achieve high yield.

Description

technical field [0001] The invention relates to the preparation technology of ammonia borane, in particular to invent a high-efficiency and low-cost preparation method of ammonia borane. Background technique [0002] Ammoniaborane is the most basic boron-nitrogen compound with the molecular formula H 3 NBH 3 . The research on it began in the 1950s, but the research was stagnant due to the lack of suitable application background. In recent years, with the increasing global energy demand, the development and utilization of various emerging energy sources have gradually received attention. Among them, hydrogen energy, as a clean, safe and efficient renewable energy, is regarded as an important component of the new energy structure in the 21st century. The utilization of hydrogen energy needs to be combined with the research and development of a series of new technologies such as hydrogen production and hydrogen storage. One of the future development directions of the curre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/13
Inventor 熊智涛陈萍吴国涛胡大强
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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