Method for preparing sodium borohydride by chemical mechanical mechanics method

A technology of sodium borohydride and chemical machinery, applied in the direction of borane/diborane hydride, etc., can solve the problems of sodium borohydride environmental pollution, harsh operating conditions, etc., achieve temperature reduction, low raw material cost, simple and safe process Effect

Inactive Publication Date: 2009-09-02
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In order to solve the above problems, the present invention provides a method for preparing sodium borohydride by chemomechanical method, using a high-energy ball mill to

Method used

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  • Method for preparing sodium borohydride by chemical mechanical mechanics method
  • Method for preparing sodium borohydride by chemical mechanical mechanics method
  • Method for preparing sodium borohydride by chemical mechanical mechanics method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Raw material handling

[0024] Dry the borax in a drying oven at 500±30°C for more than 4 hours, remove all the crystal water, then ball mill and grind it, and take it through 150 meshes for later use.

[0025] 2. Synthesis of magnesium hydride

[0026] Weigh 60g of magnesium powder (over 200 mesh) into the autoclave (GCF-1 autoclave), seal the autoclave, fill it with argon and vacuumize, repeat 3 times, then turn on the power and heat the autoclave to 300°C, then fill it with hydrogen To 6.0MPa, react for 24h. After the reaction, stop heating, cool to room temperature, release the pressure to normal pressure, and fill with argon to protect the product.

[0027] 3. Synthesis of sodium borohydride

[0028] Weigh 2.0g of anhydrous borax, 1.3g of magnesium hydride and 0.2g of anhydrous sodium carbonate, put them into a ball mill tank (QM-3A high-speed vibrating ball mill), and put them into Steel balls, then evacuated, filled with argon, repeated three times, finall...

Embodiment 2

[0031] The difference from Example 1 is:

[0032] The magnesium powder is mechanically ground at 200°C and the hydrogen pressure is 4.5MPa to react with hydrogen to produce magnesium hydride; put 2.0g of anhydrous borax, 0.3g of anhydrous sodium carbonate, and 1.3g of magnesium hydride into the ball milling equipment, Keep the hydrogen pressure at 100kPa and the mass ratio of ball to material at 60:1, and the grinding time is 2h.

[0033] The yield is 27%, and the purity is greater than 97% (calculated by active hydrogen).

Embodiment 3

[0035] The difference from Example 1 is:

[0036] Take 100 meshes of dry anhydrous borax for later use, carry out mechanical grinding on magnesium powder at 300°C and hydrogen pressure of 3 MPa to react with hydrogen to produce magnesium hydride; prepare 2.0 g of anhydrous borax, 0.1 g of anhydrous sodium carbonate, and magnesium hydride 1.1g, put it into the ball milling equipment, keep the hydrogen pressure 100kPa, the mass ratio of ball to material 50:1 and the grinding time 1.5h.

[0037] The yield is 18%, and the purity is greater than 97% (calculated by active hydrogen).

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Abstract

The invention relates to a method for preparing alkali borohydride, in particular to a method for preparing sodium borohydride by a chemical mechanical mechanics method and solving the problems of environmental pollution, severe operation condition and the like during the preparation process of the sodium borohdride in the prior art. The method takes magnesium hydride as a hydrogen source, takes borax as a boron source and prepares the sodium borohydride by combining mechanical grinding with chemical reaction. In the hydrogen atmosphere, under a certain temperature and pressure, the magnesium powder is mechanically grinded and generates hydrogenation reaction with the hydrogen, thus preparing magnesium hydride; subsequently, the borax, sodium carbonate and magnesium hydride are arranged in a ball mill with a certain proportion; certain hydrogen pressure, ball material ratio and grinding time are kept, thus obtaining the sodium borohydride. The purity of the sodium borohydride prepared by the method can achieve more than 97%. The chemical mechanical mechanics method is adopted to prepare the sodium borohydride, and compared with the currently general Schlesinger method and Baeyer method, the method has the advantages of low raw material cost, simple, convenient and safe process, no pollution and the like.

Description

technical field [0001] The present invention relates to the preparation method of alkali metal borohydride, specifically the method for preparing sodium borohydride by chemomechanical method. Background technique [0002] Sodium borohydride is known as an excellent reducing agent and hydrogen storage material. As a strong reducing agent, it is widely used in pharmaceuticals, fine organic synthesis, paper bleaching, textiles, chemical coating of non-metallic and metal materials, magnetic material manufacturing, precious metal recovery, wastewater treatment, etc.; as a hydrogen storage material, it can be used It is a new energy material for the manufacture of high-energy fuel and hydrogen source fuel cells. [0003] There are two types of techniques for synthesizing sodium borohydride today: the Schlesinger method and the Bayer method using trimethyl borate and borax as the main raw materials respectively. [0004] Schlesinger method (see US Pat, 1950.2534533; US Pat, 1961....

Claims

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Application Information

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IPC IPC(8): C01B6/21
Inventor 熊天英李铁藩吴杰金花子孔令艳崔新宇吕保军
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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