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A kind of preparation method of amorphous boron powder

A technology of amorphous boron powder and silicon powder, which is applied in the direction of boron, boron/boride, etc., can solve the problems of high anti-corrosion requirements for environmental protection facilities and equipment, the inability to realize industrial production, and low added value of by-products, so as to improve thermodynamic conditions , Broaden the source of raw materials, narrow the effect of particle size distribution

Active Publication Date: 2020-08-25
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

Although this method can produce high-purity amorphous boron powder, diborane is gaseous and highly toxic at room temperature, making the production environment harsh, and the production cost is high, making it difficult to produce industrially.
Halide borohydrogen gas thermal reduction method, is to use pure H 2 Reduction of refined BBr 3 or BCl 3 Although the boron powder prepared by this method has high purity, the production cost is high, the boron recovery rate is low and the anticorrosion requirements for environmental protection facilities and equipment are very high, and industrial production cannot be realized
The molten salt electrolysis method is to prepare elemental boron by electrolyzing boron compounds under high temperature molten salt conditions. The most prominent problem in the preparation of boron powder by electrolysis is that the electrode material is difficult to solve, the yield is low and the energy consumption is high (Peng Cheng, Chen Song, Wu Yanke, et al. Preparation of boron powder by molten salt electrolysis. Rare Metals, 2010,34(2):264-270.)
The metallothermic reduction method uses magnesium powder to reduce boron oxide at high temperature to obtain coarse boron (Dou Zhihe, Zhang Tingan. Preparation of boron powder by self-propagating metallurgy. Chinese Journal of Nonferrous Metals, 2004, 14(12): 2137-2143. ), and then use HCl, NaOH and HF to prepare amorphous elemental boron powder. Although the metallothermic reduction method prepares boron powder with mature technology and large output, the product has low purity and uneven particle size distribution. A large amount of hydrochloric acid is required in the subsequent treatment process , the by-products produced have low added value, have a strong corrosion effect on equipment, and cause serious pollution

Method used

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Embodiment 1

[0027] A preparation method of amorphous boron powder. The preparation method described in this embodiment is:

[0028] According to the mass ratio of reducing agent: boron-containing compound: molten salt of alkali metal compound: 1.0: (1.5-2.5): (3.5-8.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound are melted The salt is mixed evenly, heat-treated in a protective atmosphere at 1000-1300°C for 6-8 hours, then dissolved in water at 95-200°C, filtered, washed and dried to obtain amorphous boron powder.

[0029] The reducing agent is silicon powder, or aluminum powder, or a mixture of silicon powder and aluminum powder.

[0030] The boron-containing compound is at least one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.

[0031] The molten salt of the alkali metal compound is more than one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbona...

Embodiment 2

[0033] A preparation method of amorphous boron powder. The preparation method described in this embodiment is:

[0034] According to the mass ratio of reducing agent: boron-containing compound: molten salt of alkali metal compound: 1.0: (1.5-2.5): (3.5-8.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound are melted The salt is mixed evenly, heat-treated in a protective atmosphere at 1000-1300°C for 6-8 hours, then dissolved with an alkali solution at 95-200°C, filtered, washed and dried to obtain amorphous boron powder.

[0035] The reducing agent is silicon powder.

[0036] The boron-containing compound is one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.

[0037] The molten salt containing alkali metal compound is one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium si...

Embodiment 3

[0040] A preparation method of amorphous boron powder. The preparation method described in this embodiment is:

[0041] According to the mass ratio of reducing agent: boron-containing compound: molten salt of alkali metal compound: 1.0: (1.5-2.5): (3.5-8.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound are melted The salt is mixed evenly, heat-treated in a protective atmosphere at 1000-1300°C for 6-8 hours, then dissolved with an alkali solution at 95-200°C, filtered, washed and dried to obtain amorphous boron powder.

[0042] The reducing agent is aluminum powder.

[0043] The boron-containing compound is a mixture of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.

[0044] The molten salt of the alkali metal compound is sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silica...

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Abstract

Provided is a method for preparing the amorphous boron powder, comprising uniformly mixing a reducing agent, a boron-containing compound, and an alkali metal compound-containing molten salt which have the mass ratio of 1.0:(1.2-3.6):(0.2-16.0), performing thermal treatment on same for 0.5-8 h at the temperature of 600-1,300ºC in a protective atmosphere, resolving a thermal treatment product with water or the alkali solution at the temperature of 195-250ºC, filtering same, washing same, and drying same to prepare the amorphous boron powder. The method is low in production costs, is environment-friendly, is easily applied to industrial production, makes it possible to recycle a reaction byproduct, and has a high recovery rate of boron. The amorphous boron powder prepared by the method has a small particle size, a narrow granularity distribution, and a high purity.

Description

technical field [0001] The invention belongs to the technical field of elemental boron materials. Specifically relates to a preparation method of amorphous boron powder. Background technique [0002] Amorphous boron powder has the advantages of large specific surface area and high combustion calorific value. It is mainly used in the synthesis of new metallurgical materials and boron-rich fuel in the aerospace field, and is also used as an initiator for airbags. [0003] At present, the preparation of boron powder mainly includes borane cracking method, boron halide hydrogen gas thermal reduction method, molten salt electrolysis method, metal thermal reduction method and so on. The borane cracking method is to use sodium hydride and boron trifluoride ether complex to undergo redox reaction to generate diborane, and then crack diborane at 300-900°C to prepare amorphous boron. Although this method can produce high-purity amorphous boron powder, diborane is gaseous and highly ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/02
CPCC01B35/023C01P2006/80
Inventor 柯昌明张锦化熊思秦智王景然
Owner WUHAN UNIV OF SCI & TECH
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