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Method for synthesizing high-capacity solid hydrogen storage material ammonia borane by using amino complex

A technology of hydrogen storage materials and complexes, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, metal hydrides, etc., can solve high operating costs, low operating risks, and complex processes and other problems, to achieve the effect of mild preparation conditions, broaden the range of raw materials, and high product purity

Active Publication Date: 2011-09-07
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The borane method uses borane as a boron source and reacts with liquid ammonia to directly generate products (S. G. Shore, K. W.B?ddeker, Inorg. Chem.1963, 3, 914-915), wherein B 2 h 6 It is a kind of flammable and highly toxic compound, the production is very dangerous, the process is complicated, and the operation cost is high; in the sodium borohydride method, borohydride (NaBH 4 or LiBH 4 ) and ammonium salts (such as NH 4 Cl, (NH 4 ) 2 SO 4 , (NH 4 ) 2 CO 3 etc.) reaction (P. V. Ramachandran, P. D. Gagare, Inorg. Chem. 2007, 46, 7810-7817), the operation risk is small, the environment is friendly, but the raw material source is single
[0005] Although some progress has been made in the preparation of ammonia borane, there is still a lack of a simple, economical and effective synthetic method

Method used

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  • Method for synthesizing high-capacity solid hydrogen storage material ammonia borane by using amino complex
  • Method for synthesizing high-capacity solid hydrogen storage material ammonia borane by using amino complex
  • Method for synthesizing high-capacity solid hydrogen storage material ammonia borane by using amino complex

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Preparation of hexammine nickel chloride:

[0029] 18.6mmol NH 4 Cl was added to ammonia water, stirred and dissolved, and 5mmol Ni-Cl was slowly added to it 2 . 6H 2 O. Stirring was continued for 10 hours, and then the blue-purple solid was isolated by filtration, washed 2-3 times with absolute ethanol, and finally dried at 60° C. for 4 hours. The X-ray diffraction pattern shows that the prepared Ni(NH 3 ) 6 Cl 2 Corresponds exactly to the standard spectrum with good purity, such as figure 1 shown.

[0030] Preparation of high-capacity solid-state hydrogen storage material ammonia borane:

[0031] Add 0.64g hexaammine nickel chloride to the purified tetrahydrofuran solvent and stir thoroughly, then add 0.21g of sodium borohydride according to the molar ratio of hexaamine nickel chloride and sodium borohydride is 1:2, and continue stirring For 12 hours, the system maintained an argon atmosphere during the reaction. After centrifugation, the supernatant was ev...

Embodiment 2

[0037] The preparation of hexaammine nickel chloride is the same as in Example 1, after 0.64g hexaammine nickel chloride is added to the purified tetrahydrofuran solvent and fully stirred, then according to the hexaammine nickel chloride and sodium borohydride mol ratio is 1: Add 0.32 g of sodium borohydride in an amount of 3, and heat to reflux for 5 hours. During the reaction, the system maintains an argon atmosphere. After centrifugation, the supernatant was evaporated to obtain a white powder, and finally vacuum-dried at 40°C for 12 hours. The product was denoted as AB(1:3-H). Figure 7 For the X-ray diffraction pattern of ammonia borane prepared according to the above method, the pattern shows that there are no impurity peaks such as sodium borohydride and hexammine nickel chloride, and the purity is good.

Embodiment 3

[0039] The preparation of hexaammine nickel chloride is the same as in Example 1. After adding 0.64g hexaammine nickel chloride to the purified 1.4-dioxane solvent and fully stirring, then hexaammine nickel chloride and sodium borohydride Add 0.21 g of sodium borohydride at a molar ratio of 1:2. Insulated at 40° C. for 10 hours, and the system maintained an argon atmosphere during the reaction. The product was isolated, solvent removed, and dried to give the product, which was designated as AB(1:2-D). While maintaining a good purity of the product, the output is significantly increased.

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Abstract

The invention discloses a method for synthesizing a high-capacity solid hydrogen storage material ammonia borane by using an amino complex. The ammonia borane is obtained by reacting the amino complex serving as an ammonia source and borohydride serving as a boron source. The borohydride is sodium borohydride (NaBH4), the amino complex is powdery hexammine nickel chloride, and the molar ratio of the NaBH4 to the hexammine nickel chloride is 1: 0.1 to 1. The ammonia borane with high hydrogen capacity is prepared by using the NaBH4 as the boron source and the amino complex as the ammonia source. Compared with the conventional preparation method of the ammonia borane, the method has the advantages that: the range of raw materials of the ammonia borane is widened; the advantages of hydrogen reversible storage of ammine are fully utilized; preparation condition is mild, operation is simple, and the purity of a product is relatively high (99 percent); obtained nickel (Ni) metal is amorphous nano-particles with a diameter of 5 to 30 nm; and the method has a potential application value for catalysis of the ammonia borane and hydrolysis of hydrogen.

Description

technical field [0001] The invention relates to the technical field of preparation of hydrogen storage materials, in particular to a method for synthesizing high-capacity solid hydrogen storage material ammonia borane with an amino complex. Background technique [0002] Due to the worldwide energy shortage and the urgent need of environmental protection, it is imminent to find renewable green energy to replace traditional fossil energy. Hydrogen energy has the advantages of abundant reserves, wide range of sources, high energy density, recyclability, and environmental friendliness, and has become one of the energy carriers with the most development potential in the future energy structure. The development and utilization of hydrogen energy involves cheap hydrogen production, safe and efficient storage and transportation, and large-scale application. Due to the characteristics of hydrogen, such as flammability, explosion, easy diffusion, and low volumetric energy density at ...

Claims

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Application Information

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IPC IPC(8): C01B6/13B01J23/755
Inventor 陶占良邹少爽马华马建丽梁静程方益陈军
Owner NANKAI UNIV
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