Method for synthesizing ammonia borane

A synthesis method, ammonia borane technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve problems such as high cost and complicated process, achieve solvent saving, cost reduction, simple and cheap preparation process Effect

Inactive Publication Date: 2013-09-18
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above preparation methods usually have a complex process and high cost

Method used

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  • Method for synthesizing ammonia borane
  • Method for synthesizing ammonia borane
  • Method for synthesizing ammonia borane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Put 26.21g of ammonium fluoroborate and 9.46g of sodium borohydride (the molar ratio of ammonium fluoroborate and sodium borohydride is 1) into a reactor with a reflux device containing 250 milliliters of dioxane solvent, The prepared ammonium fluoroborate-sodium borohydride-dioxane mixed solution was then heated and stirred for at least 10 hours, and the heating temperature was 40°C;

[0026] (2) Suction filter the mixed solution obtained through the reaction in step (1) to obtain a clear and transparent solution;

[0027] (3) Rotate the clear and transparent solution obtained in step (2) at 70°C to obtain a white light sample, which is ammonia borane;

[0028] Such as figure 1 Shown is the X-ray diffraction (XRD) pattern of the product. Within the measured diffraction angle range, each diffraction peak is very clear and sharp. One-to-one correspondence of diffraction data indicates that it has high purity and crystallinity. There are no diffraction peaks of oth...

Embodiment 2、 example 3

[0030] Change step (1) ammonium fluoroborate in Example 1 to 13.11g and 52.42g (the molar ratios of ammonium fluoroborate and sodium borohydride are 0.5 and 2 respectively), and other operations are the same as in Example 1 to obtain Product is with embodiment 1.

Embodiment 4、 example 5

[0032] Change the amount of sodium borohydride in step (1) in Example 1 to 4.73g and 18.92g respectively (the molar ratios of ammonium fluoroborate and sodium borohydride are 2 and 0.5 respectively), and all other operations are the same as in Example 1 Identical, obtain product with embodiment 1.

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Abstract

The invention discloses a method for synthesizing ammonia borane. The method comprises the following two synthesizing steps of: 1, reacting a mixture of ammonium fluoroborate and sodium borohydride in an experimental container with a reflux unit in which a dioxane solvent is filled, thereby obtaining a dioxane solvent for dissolving ammonia borane; 2, performing heating and spin drying treatment on the solvent by utilizing a rotary evaporator, thereby obtaining the product ammonia borane. In the process, the dioxane recovered by utilizing the rotary evaporator can be repeatedly utilized to serve as the solvent in the ammonia borane preparation process. In the method, the ammonium fluoroborate serves as an ammonium source for the first time, the synthetic method is simple, the product yield is considerable, and the purity is high.

Description

technical field [0001] The technical scheme of the invention relates to a simple and cheap method for synthesizing the chemical hydrogen storage material ammonia borane. Background technique [0002] Ammonium borane compound (NH 3 BH 3 ) is a chemical hydride hydrogen storage material that has received close attention in recent years. Its hydrogen density is as high as 19.6wt.%. It has the advantages of moderate thermal stability and good chemical stability, and has been called for high expectations in the field of vehicle hydrogen energy applications. At the same time, the product after dehydrogenation is a very high-purity boron nitride (BN) ceramic material, which has also attracted people's close attention. [0003] In recent years, quite a number of researchers have devoted themselves to the preparation of ammonia borane with different methods and raw materials. Shore et al. used lithium borohydride and ammonium salts such as NH 4 Cl,(NH 4 ) 2 SO 4 and (NH 4 ) ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/13
Inventor 唐成春薛彦明田冉徐学文
Owner HEBEI UNIV OF TECH
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