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Preparation method of nano-particle type borohydride ammonate

A borohydride and nanoparticle technology is applied in the field of preparation of hydrogen storage materials, which can solve the problems of influence of hydrogen storage performance, large size of hexaammine magnesium borohydride, influence of sample purity, etc., and achieves simple operation and low impurity content. Effect

Active Publication Date: 2015-05-06
ZHEJIANG UNIV
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  • Abstract
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Problems solved by technology

However, this method also has the following disadvantages: First, the hexaammine magnesium borohydride prepared by this method has a large particle structure and a large size, which has a certain impact on the hydrogen storage performance; secondly, due to the hexaammine magnesium borohydride prepared by this method Magnesium borohydride still contains a certain amount of solvent ether, the purity of the sample will be affected
At present, the existing preparation methods cannot realize the preparation of nanoparticulate hexaammine magnesium borohydride with controllable particle size

Method used

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  • Preparation method of nano-particle type borohydride ammonate
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Experimental program
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Effect test

Embodiment 1

[0029] In an argon atmosphere, manually stir and mix 1 gram of magnesium borohydride and 1 liter of organic solvent ether through a glass rod. The stirring time is 60 minutes, and the rotation speed is 60 rpm. After fully mixing, the complex of magnesium borohydride is obtained. compound solution; feed ammonia gas with a pressure of 0.6 bar into the complex solution, ultrasonically stir and mix, the rotating speed is 400 rpm, and the stirring time is 1 hour to form the ammonia complex of magnesium borohydride; adopt dynamic vacuum The solvent diethyl ether is removed by a method to obtain hexaamminemagnesium borohydride.

[0030] Such as figure 1 As shown, the hexaamminemagnesium borohydride and the figure 1 The medium standard hexaammine magnesium borohydride sample has the same infrared spectrum, that is, the prepared product is hexaammine magnesium borohydride. The particle size of the obtained product is in the range of 150-300 nanometers, the initial hydrogen desorption...

Embodiment 2

[0032] In an argon atmosphere, 1 gram of magnesium borohydride and 2 liters of organic solvent methyl sulfide were mixed by ultrasonic stirring, the stirring time was 10 minutes, and the rotation speed was 100 rpm. After fully mixing, the complex of magnesium borohydride was obtained. compound solution; into the complex solution, a pressure of 1.5bar ammonia gas is passed into the complex solution, magnetically stirred and mixed, the rotating speed is 100 rpm, and the stirring time is 40 minutes to form the ammonia complex of magnesium borohydride; adopt suction filtration The solvent methyl sulfide is removed by the method, and hexaammine magnesium borohydride is obtained.

[0033] Such as figure 2 As shown, the obtained hexaammine magnesium borohydride and figure 2 The X-ray diffraction pattern of the standard hexaammine magnesium borohydride sample is the same, indicating that the prepared product is hexaammine magnesium borohydride. The particle size of the obtained he...

Embodiment 3

[0035] In an argon atmosphere, 0.5 grams of magnesium borohydride and 3 liters of organic solvent ether were mixed by ultrasonic stirring, the stirring time was 10 minutes, and the rotation speed was 400 rpm. After thorough mixing, the complex of magnesium borohydride was obtained. solution; the ammonia gas with a pressure of 0.8 bar is passed into the complex solution, stirred and mixed by ultrasonic, the rotating speed is 300 rpm, and the stirring time is 30 minutes, and the solvent ether is removed by dynamic vacuum to obtain boron hexaamine magnesium hydride.

[0036] Such as Figure 4 As shown, the prepared magnesium hexaammine borohydride has a nanoparticle structure, and the particle size is about 20 nanometers to 100 nanometers. Its initial hydrogen release temperature is 66°C, and when heated to 500°C, the hydrogen release amount can reach 11.8wt%.

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Abstract

The invention discloses a preparation method of nano-particle type borohydride ammonate. The preparation method comprises the following steps: (1) at the atmosphere of a protective gas, mixing borohydride and an excess organic solvent to obtain a complex solution; and (2) mixing the complex solution and an ammonia source to obtain the nano-particle type borohydride ammonate. According to the preparation method disclosed by the invention, the borohydride and the excess organic solvent are mixed to obtain the complex solution, and then mixing is carried out in the process of introducing the ammonia source into the complex solution to obtain the nano-particle type borohydride ammonate, so that the problem of poor hydrogen storage property of the large-particle borohydride ammonate prepared by the traditional method is solved.

Description

technical field [0001] The invention relates to the preparation of hydrogen storage materials, in particular to a method for preparing nanoparticle-shaped borohydride ammonium compounds. Background technique [0002] Hydrogen energy, as a clean and non-polluting green energy with rich resources, wide sources and high combustion calorific value, has been paid more and more attention by people, and it is also considered as one of the ideal fuels in the future. Finding an efficient and safe method of hydrogen storage and transportation is the key to the application of hydrogen energy. The solid-state hydrogen storage method using hydrogen storage materials and hydrogen reaction can effectively overcome the shortcomings of gas and liquid hydrogen storage methods, and has the characteristics of safety, high efficiency, and low cost, and is considered to be a promising hydrogen storage method. [0003] Among many hydrogen storage materials, magnesium borohydride ammonium compound...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B6/21C01B6/23B82Y30/00
CPCC01B6/21C01B6/23C01P2002/72C01P2002/82C01P2004/03C01P2004/64C01P2006/80
Inventor 刘永锋李由高明霞潘洪革
Owner ZHEJIANG UNIV