Process for producing elemental boron with 99%-99.99% high purity

A process method and elemental boron technology, applied in the direction of boron, boron/boride, etc., can solve the problems of complex process, high impurities, harsh production conditions, etc., and achieve the effect of simple impurity removal process, reduced technical difficulty, and uniform particle size distribution.

Pending Publication Date: 2019-02-15
董克胜
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Among them, the first and second methods are more suitable for laboratory preparation, and only the molten electrolysis method is suitable for large-scale production, but the disadvantage of this method is that the impurities are high, and it is difficult to obtain high-purity products
In addition, even with the reduction method of boron oxide and magnesium or aluminum, the products produced cannot meet the technical requirements for the preparation of high-purity elemental boron due to the effect of impurities, and it is difficult to control the particle size of elemental boron, which limits the direction and scope of use and reduces production costs. also higher
[0008] High-purity products can also be prepared by reducing boron halides with hydrogen, but this method is complicated in process, high in cost, low in recovery rate, relatively polluting to the environment, and harsh in production conditions.
[0009] High-purity boron can also be obtained by borane cracking method, but borane is active, flammable, explosive, highly toxic, and safety protection problems are difficult to solve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation method of the present embodiment comprises the steps:

[0032] (1) Weigh 122.6kg of boric acid, wash with 85°C hot water, add EDTA to remove metal impurities, filter 3 times, recrystallize the filtrate to obtain high-purity boric acid crystals as a precursor, and then mix it with The melamine of 126.12kg is mixed in the sealed mixer;

[0033] (2) Place the mixed boric acid crystals and melamine in a drying oven, dehydrate at 300° C., and press the dehydrated materials into blocks;

[0034] (3) The dehydrated material is placed in a high-temperature vacuum furnace for calcination. The calcination temperature is 1700 ° C. The mixture of boric acid and melamine is heated, and polycrystals form hexagonal boron nitride white powder, namely product A;

[0035] (4) Rinse the product A with hot water for 3 times, filter and dry it, then place it in a graphite crucible, place the graphite crucible in a high-temperature vacuum furnace, and calcinate it in a high-...

Embodiment 2

[0040] The preparation method of the present embodiment comprises the steps:

[0041] (1) take by weighing the anhydrous borax of 150kg and the dicyandiamide of 75kg to mix in the sealed mixer;

[0042] (2) Place the mixed anhydrous borax and dicyandiamide in a drying oven and dehydrate at 300°C;

[0043] (3) The dehydrated material is placed in a high-temperature vacuum furnace for calcination. The calcination temperature is 1750 ° C. The mixture of anhydrous borax and dicyandiamide is heated, and polycrystals form hexagonal boron nitride white powder, which is product A;

[0044] (4) Rinse the product A with hot water for 3 times, filter and dry it, then place it in a graphite crucible, place the graphite crucible in a high-temperature vacuum furnace, and calcinate it in a high-temperature vacuum at 1950° C. to decompose to obtain a powdery product B; Product B is elemental boron powder; elemental boron powder is elemental B-type boron powder;

[0045] (5) Classify and cla...

Embodiment 3

[0049] The preparation method of the present embodiment comprises the steps:

[0050] (1) The metaboric acid of 150kg and the ammonium chloride of 100kg are mixed in the sealed mixer;

[0051] (2) Place the mixed metaboric acid and ammonium chloride in a drying oven and dehydrate at 300°C;

[0052] (3) The dehydrated material is placed in a high-temperature vacuum furnace for calcination. The calcination temperature is 1700 ° C. The mixture of metaboric acid and ammonium chloride is heated, and the polycrystal forms hexagonal boron nitride white powder, which is product A;

[0053] (4) Rinse the product A with hot water for 3 times, filter and dry it, then place it in a graphite crucible, place the graphite crucible in a high-temperature vacuum furnace, and calcinate it in a high-temperature vacuum at 2000° C. to decompose to obtain a powdery product B; Product B is elemental boron powder; elemental boron powder is type B boron powder;

[0054] (5) Classify and classify the ...

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Abstract

The invention provides a method for producing elemental boron with 99%-99.99% high purity, and belongs to the technical field of chemical substance preparation. Powdery hexagonal boron nitride is prepared from boride and nitride as raw materials by low-temperature dehydration and high-temperature synthesis, hexagonal boron nitride powder is purified and subjected to pyrolysis, and fine boron powder is obtained finally. The purity of elemental boron prepared with the method is as high as 99%-99.99%, particle size is smaller than or equal to 30 mu m, and the method is simple in process, environmentally friendly and nontoxic.

Description

technical field [0001] The invention relates to the technical field of elemental boron preparation, in particular to a process for producing 99%-99.99% high-purity elemental boron. Background technique [0002] Elemental boron is a widely used chemical raw material mineral. In addition to producing borax, boric acid and various boron compounds, it is also an important material in metallurgy, building materials, machinery, electrical appliances, chemicals, light wool, nuclear industry, medicine, agriculture and other departments. raw material. High-purity elemental boron can be used in the electronics industry, especially in the manufacturing process of heat-flow lithium-boron batteries, which can improve the upgrading of military equipment. In the nuclear industry, high-purity elemental boron can make shielding materials miniaturized. In military equipment, high-purity elemental boron plays an important role in upgrading propellants. Among metal materials, high-purity ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/02
CPCC01B35/023
Inventor 董克胜
Owner 董克胜
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