Method for directly synthesizing sodium borohydride by solid phase ball milling at room temperature

A room temperature solid-phase, sodium borohydride technology, applied in the direction of borane/diborane hydride, etc., can solve the problems of difficult large-scale application, high requirements for preparation conditions, high energy consumption, etc., and achieves a controllable reaction process. The effect of adjustment, simple process and low energy consumption

Active Publication Date: 2018-09-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But what is more worthy of attention is that this method uses expensive magnesium hydride as a reducing agent. In addition to the high price of magnesium hydride, its production requires the synthesis of magnesium and hydrogen under high temperature and high pressure, which not only consumes a lot of energy, but also uses extra hydrogen. source; and the boron source used in this method is anhydrous borax, which needs to be prepared by removing water from natural borax.
Therefore, the method for preparing sodium borohydrid

Method used

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  • Method for directly synthesizing sodium borohydride by solid phase ball milling at room temperature
  • Method for directly synthesizing sodium borohydride by solid phase ball milling at room temperature
  • Method for directly synthesizing sodium borohydride by solid phase ball milling at room temperature

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Effect test

Embodiment 1

[0054] In a 0.1MPa argon atmosphere glove box, weigh magnesium, sodium carbonate and sodium tetraborate decahydrate with a molar ratio of 28:1:1, mix them into a ball mill jar and place the ball mill jar in a high-energy pendulum ball mill ( In QM-3C), the ball-to-material ratio is 50:1, the ball milling speed is 1000 rpm, and ball milling is performed directly in the argon atmosphere for 20 hours. figure 1 It is the XRD spectrum of the ball milling product. The diffraction peaks at 25.1, 28.9, and 41.4° in the curve belong to sodium borohydride crystals, which proves that sodium borohydride crystals are generated; the mixture is dissolved in ethylenediamine and filtered to obtain a clear filtrate, and the filtrate is subjected to A white powder was obtained after vacuum drying, Image 6 It is the XRD pattern of white powder, the diffraction peaks appearing at 25.1, 28.9, 41.4, 49.0, 51.3, 60.0, 66.0, 68.0° belong to sodium borohydride crystal, which proves that the white powd...

Embodiment 2

[0056] In a 0.1MPa argon atmosphere glove box, weigh magnesium, sodium carbonate and sodium tetraborate decahydrate with a molar ratio of 22:1:1, mix them into a ball mill jar and place the ball mill jar in a high-energy pendulum ball mill ( In QM-3C), the ball-to-material ratio is 30:1, the ball milling speed is 1000 rpm, and the ball milling is directly carried out in the argon atmosphere for 10 hours. The XRD pattern and figure 1 Similarly, the diffraction peaks at 25.1, 28.9, and 41.4° in the curve belong to sodium borohydride crystals, which proves that sodium borohydride crystals are formed; the mixture is dissolved in ethylenediamine and filtered to obtain a clear filtrate, which is vacuum-dried to obtain a white powder , the quantitative yield was 42% by iodine titration.

Embodiment 3

[0058] In a 0.1MPa argon atmosphere glove box, weigh magnesium, sodium carbonate and sodium tetraborate decahydrate with a molar ratio of 18:1:1, mix them into a ball mill jar and place the ball mill jar in a high-energy pendulum ball mill ( In QM-3C), the ball-to-material ratio is 5:1, the ball milling speed is 1000 rpm, and ball milling is performed directly in the argon atmosphere for 5 hours. The XRD pattern and figure 1 Similarly, the diffraction peaks at 25.1, 28.9, and 41.4° in the curve belong to sodium borohydride crystals, which proves that sodium borohydride crystals are formed; the mixture is dissolved in ethylenediamine and filtered to obtain a clear filtrate, which is vacuum-dried to obtain a white powder , the quantitative yield by iodometric titration was 21%.

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Abstract

The invention discloses a method for directly synthesizing sodium borohydride by solid phase ball milling at room temperature. Under the condition of the room temperature, a ball mill is used for solid phase ball milling of a mixture of a reducing agent, a sodium supplement and a reduced material and purification to obtain the sodium borohydride; the reducing agent comprises one or more of magnesium, magnesium hydride, aluminum, calcium silicide and magnesium silicide; the sodium supplement includes at least one of sodium hydroxide, sodium hydride and sodium carbonate; the reduced material iscrystal water-contained sodium tetraborate or sodium tetraborate or a mixture of the crystal water-contained sodium tetraborate or the sodium tetraborate, the solid phase ball milling is carried out in a mixed atmosphere of argon and hydrogen or an argon atmosphere or a hydrogen atmosphere. The method has the advantages of short production process, mild reaction condition, low cost, high output, no pollution, high safety factor and easy industrial production.

Description

technical field [0001] The invention relates to a preparation method of sodium borohydride, in particular to a method for directly synthesizing sodium borohydride by solid-phase ball milling at room temperature. Background technique [0002] The application of hydrogen energy is restricted by its storage technology. The hydrolysis hydrogen production technology realizes the integration of hydrogen production and hydrogen storage. Among them, the hydrogen production by hydrolysis of sodium borohydride is expected to solve the problem of hydrogen storage. Sodium borohydride is a traditional coordination hydride. It has a high hydrogen storage capacity and a large amount of hydrogen release by hydrolysis (theoretical hydrogen release amount can reach 10.8wt%). The hydrolysis reaction is controllable, and the hydrogen produced is of high purity. The product is non-toxic and harmless. However, sodium borohydride is not a substance that directly exists in nature. At the same time...

Claims

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Application Information

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IPC IPC(8): C01B6/21
CPCC01B6/21C01P2002/72
Inventor 欧阳柳章钟浩刘江文王辉朱敏
Owner SOUTH CHINA UNIV OF TECH
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