Solid-phase synthesis method for magnesium borohydride ammoniates

The technology of magnesium borohydride ammine compound and magnesium borohydride solid phase is applied in the field of preparation of hydrogen storage materials, and can solve the problems of carcinogenicity of benzene, low purity, difficult operation, etc. simple effect

Active Publication Date: 2012-09-12
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the benzene and ether used in this reaction route have certain toxicity, and benzene is a carcinogen
In addition, the synthetic route also needs to undergo subsequent treatments such as filtration, solvent washing and vacuum drying, which is not conducive to large-scale promotion
At the same time, the method needs to accurately control the amount of liquid magnesium borohydride ether complex and gaseous ammonia, which is difficult to achieve in industrial production and will lead to increased production costs.
[0010] In addition, the existing methods for synthesizing magnesium borohydride ammonium compounds can only synthesize diammine magnesium borohydride, triammine magnesium borohydride and hexaammine magnesium borohydride, and the ammonia complex number is not equal to two, three or six

Method used

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  • Solid-phase synthesis method for magnesium borohydride ammoniates
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  • Solid-phase synthesis method for magnesium borohydride ammoniates

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In the glove box, the Mg(BH 4 ) 2 Put it into a stainless steel ball mill tank that can be sealed and have a switch valve. After the ball mill tank is evacuated, fill it with ammonia with a pressure of 10 atmospheres (if there is no special description in the present invention, the atmospheric pressure refers to standard atmospheric pressure). , ball milling on a planetary ball mill, the ball-to-material ratio is 120:1, the rotating speed is 300rpm, and the ball milling time is 36h. After the ball milling is finished, the product is subjected to XRD testing (the XRD of the sample is measured on a Philips X'Pert Pro X-ray diffractometer ).

[0039] figure 1 It is the XRD pattern of the product, and the product has and only has the characteristic diffraction peak of hexaammine magnesium borohydride.

Embodiment 2

[0041] Magnesium borohydride ammonium was prepared according to the method described in Example 1, and the differences in preparation conditions are shown in Table 1.

[0042] After the preparation, the product was weighed, and the ammonium complex number of magnesium borohydride in the product was calculated. Table 1 lists the ratio of product weight increase and the type of product. It was found that by changing the preparation conditions, monoammine magnesium borohydride, diammine magnesium borohydride, triammine magnesium borohydride, tetraammine magnesium borohydride and pentaammine magnesium borohydride can be obtained respectively.

[0043] Table 1 The experimental conditions and products of ball milling magnesium borohydride under ammonia atmosphere

[0044]

Embodiment 3

[0046]In the glove box, the Mg(BH 4 ) 2 and Mg(BH 4 ) 2 6NH 3 Mix according to the molar ratio of 5:1, put it into a stainless steel ball mill tank that can be sealed and have a switch valve, and ball mill it on a planetary ball mill under an argon atmosphere of 1 atmosphere pressure, the ball-to-material ratio is 60:1, and the speed is 550rpm. The time is 18h. After the ball milling, the product was tested by XRD.

[0047] figure 2 It is the XRD pattern of the product, and the product has and only one characteristic diffraction peak of ammine magnesium borohydride.

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Abstract

The invention discloses a solid-phase synthesis method for magnesium borohydride ammoniates. The solid-phase synthesis method comprises the following step of: performing ball milling on magnesium borohydride and an ammonia source under the atmosphere of protective gas to obtain the magnesium borohydride ammoniate. According to the solid-phase synthesis method for the magnesium borohydride ammoniates, the complicated operation processes of filtration, distillation and solvent removal in traditional methods are avoided, and the problem that organic waste liquid needs to be specially treated is solved; the product yield is increased; a series of magnesium borohydride ammoniates with different ammonia complexing numbers can be prepared; the operation is simple; the product purity is high; the yields of the magnesium borohydride ammoniates are respectively higher than 95 percent; the dehydriding temperature of the obtained product is about 130 DEG C; and the hydrogen discharge amount is higher than 13 weight percent (wt%).

Description

technical field [0001] The invention relates to the preparation of hydrogen storage materials, in particular to a solid-phase synthesis method of magnesium borohydride ammonium hydrogen storage materials. Background technique [0002] Magnesium borohydride ammonium compound has the advantages of large hydrogen storage capacity (>13wt%), low hydrogen release temperature, and insensitivity to oxygen. It is widely used in hydrogen energy utilization and is one of the research hotspots of hydrogen storage materials at present. [0003] At present, for the synthesis method of magnesium borohydride ammonium compound in the world, there are mainly used ammonia gas and magnesium borohydride ether solution to prepare hexaammine magnesium borohydride, hexaammine magnesium borohydride decomposition to prepare diammine magnesium borohydride, and benzene, respectively. React with magnesium borohydride and ammonia gas in a near-stoichiometric ratio in ether to generate diammine magnesi...

Claims

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Application Information

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IPC IPC(8): C01B6/21
Inventor 刘永锋杨燕京潘洪革高明霞
Owner ZHEJIANG UNIV
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