CN109179444B - Preparation method of amorphous boron powder - Google Patents
Preparation method of amorphous boron powder Download PDFInfo
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Abstract
The invention relates to a preparation method of amorphous boron powder. The technical scheme is as follows: uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.2-3.6) to (0.2-16.0), carrying out heat treatment for 0.5-8 h under the condition of a protective atmosphere and 600-1300 ℃, then dissolving the mixture by using water or an alkali solution at the room temperature-250 ℃, filtering, washing and drying to obtain the amorphous boron powder. The method has the characteristics of low production cost, environmental friendliness, easiness in industrial production, capability of recycling reaction byproducts and high boron recovery rate, and the prepared amorphous boron powder has small particle size, narrow particle size distribution and high purity.
Description
Technical Field
The invention belongs to the technical field of elemental boron materials. In particular to a preparation method of amorphous boron powder.
Background
The amorphous boron powder has the advantages of large specific surface area, high combustion heat value and the like, is mainly used for synthesis of new metallurgical materials and boron-rich fuels in the field of aerospace, and is also used as an initiator of safety airbags.
Currently, boron powder is mainly prepared by a borane cracking method, a boron halide gas-thermal reduction method, a molten salt electrolysis method, a metallothermic reduction method and the like. The borane cracking method is to perform oxidation-reduction reaction on sodium hydride and boron trifluoride diethyl etherate complex to generate diborane, and then crack the diborane at 300-900 ℃ to prepare amorphous boron. Although the method can prepare amorphous boron powder with high purity, diborane is in a gaseous state at normal temperature and has high toxicity, so that the production environment is harsh, the production cost is high, and industrial production is difficult. The hydroboration method is a gas-thermal reduction method using pure H2Reduction of refined BBr3Or BCl3Although the boron powder prepared by the method has higher purity, the production cost is high, the boron recovery rate is low, the corrosion prevention requirement on environmental protection facilities and equipment is high, and the industrial production cannot be realized. The molten salt electrolysis method is to electrolyze boron compound to prepare simple substance boron under the condition of high temperature molten salt, and the electrolysis method is to prepare boron powder, the most outstanding problems are that electrode materials are difficult to solve, the yield is low and the energy consumption is high (Pengtong, Chensong, Wuyanke, etc. research on preparing boron powder by the molten salt electrolysis method, rare metals, 2010,34(2): 264-. The metallothermic reduction method is to reduce boron oxide with magnesium powder at high temperature to obtain crude boronThe boron powder is prepared by a self-propagating metallurgical method, namely 2137-.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the preparation method of the amorphous boron powder, which has the advantages of low production cost, environmental friendliness, easiness in industrial production, capability of recycling reaction byproducts and high boron recovery rate, and the prepared amorphous boron powder has small particle size, narrow particle size distribution and high purity.
In order to achieve the purpose, the invention adopts the technical scheme that: uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.2-3.6) to (0.2-16.0), carrying out heat treatment for 0.5-8 h under the condition of a protective atmosphere and 600-1300 ℃, then dissolving the mixture by using water or an alkali solution at the room temperature-250 ℃, filtering, washing and drying to obtain the amorphous boron powder.
The reducing agent is silicon powder, or aluminum powder, or a mixture of silicon powder and aluminum powder.
The boron-containing compound is more than one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is more than one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is more than one of sodium hydroxide aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
SiO in the sodium silicate2With Na2The molar ratio of O is less than or equal to 1.
SiO in the potassium silicate2And K2Mole of OThe ratio is less than or equal to 1.
SiO in the lithium silicate2With Li2The molar ratio of O is less than or equal to 1.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
(1) besides boron oxide, boric acid, sodium tetraborate, potassium tetraborate, lithium tetraborate and other boron-containing compounds can be used as boron sources, so that the raw material sources are widened, and the production cost is low.
(2) The alkali metal compound-containing molten salt adopted by the invention can participate in chemical reaction, improve the thermodynamic condition of the chemical reaction, promote the reduction reaction, improve the yield and improve the recovery rate. The product after heat treatment can be directly washed by water or alkali, the process is simple, the by-product can be recycled, the defect of serious pollution to the environment caused by the traditional acid washing process is avoided, the production process has no pollution to the environment, and the industrial production is easy to realize.
(3) The invention introduces the alkali metal compound-containing molten salt into the reaction system, and the existence of the alkali metal compound-containing molten salt can form a liquid phase at a lower temperature, strengthen the mass transfer process, improve the dynamic condition of the chemical reaction and improve the reduction reaction efficiency. In addition, the alkali metal compound-containing molten salt can participate in chemical reaction, improve the thermodynamic condition of the chemical reaction, promote the reduction reaction, improve the yield and the recovery rate, and the recovery rate of boron is higher than 90 percent. After the alkali metal compound molten salt is introduced, the reaction is carried out in a liquid phase, the reaction condition is mild, and the generated boron powder has the characteristics of small particle size and narrow particle size distribution.
(4) The boron powder prepared by the invention is amorphous boron powder, the B content is more than or equal to 95 wt%, and the high-purity boron powder with the B content of more than 98.5 wt% can be obtained under the optimal process conditions. The prepared boron powder has uniform particle size and forms agglomerate particles.
Therefore, the method has the characteristics of low production cost, environmental friendliness, easiness in industrial production, capability of recycling reaction byproducts and high boron recovery rate, and the prepared amorphous boron powder has small particle size, narrow particle size distribution and high purity.
Drawings
FIG. 1 is an XRD pattern of an amorphous boron powder prepared in accordance with the present invention;
FIG. 2 is an SEM photograph of another amorphous boron powder prepared according to the present invention.
Detailed Description
For a better understanding of the invention, the contents of the invention are further illustrated below by means of the figures and examples, but the invention is not limited to the following examples.
In order to avoid repetition, the materials related to this specific embodiment are described in a unified manner, which is not described in the embodiments again:
SiO in the sodium silicate2With Na2The molar ratio of O is less than or equal to 1.
SiO in the potassium silicate2And K2The molar ratio of O is less than or equal to 1.
SiO in the lithium silicate2With Li2The molar ratio of O is less than or equal to 1.
Example 1
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.5-2.5) to (3.5-8.0), carrying out heat treatment for 6-8 h under the condition of protective atmosphere and 1000-1300 ℃, then dissolving the mixture with water at the temperature of 95-200 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is silicon powder, or aluminum powder, or a mixture of silicon powder and aluminum powder.
The boron-containing compound is more than one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is more than one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
Example 2
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.5-2.5) to (3.5-8.0), carrying out heat treatment for 6-8 h under the condition of protective atmosphere and 1000-1300 ℃, then dissolving with an alkali solution at the temperature of 95-200 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is silicon powder.
The boron-containing compound is one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is one of a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a lithium hydroxide aqueous solution.
Example 3
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.5-2.5) to (3.5-8.0), carrying out heat treatment for 6-8 h under the condition of protective atmosphere and 1000-1300 ℃, then dissolving with an alkali solution at the temperature of 95-200 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is aluminum powder.
The boron-containing compound is a mixture of two substances of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is a mixture of two substances of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is a mixture of two substances in a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a lithium hydroxide aqueous solution.
Example 4
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.5-2.5) to (3.5-8.0), carrying out heat treatment for 6-8 h under the condition of protective atmosphere and 1000-1300 ℃, then dissolving with an alkali solution at the temperature of 95-200 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is a mixture of silicon powder and aluminum powder.
The boron-containing compound is a mixture of more than three of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is a mixture of more than three substances of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is a mixture of three substances of sodium hydroxide aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
Example 5
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (2.4-3.6) to (7.5-12.0), carrying out heat treatment for 4.5-7 h under the condition of a protective atmosphere and 600-800 ℃, then dissolving with water at the temperature of 45-100 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is silicon powder, or aluminum powder, or a mixture of silicon powder and aluminum powder.
The boron-containing compound is more than one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is more than one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
Example 6
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (2.4-3.6) to (7.5-12.0), carrying out heat treatment for 4.5-7 h under the conditions of protective atmosphere and 600-800 ℃, then dissolving with an alkali solution at the temperature of 45-100 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is silicon powder.
The boron-containing compound is one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is one of a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a lithium hydroxide aqueous solution.
Example 7
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (2.4-3.6) to (7.5-12.0), carrying out heat treatment for 4.5-7 h under the conditions of protective atmosphere and 600-800 ℃, then dissolving with an alkali solution at the temperature of 45-100 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is aluminum powder.
The boron-containing compound is a mixture of two substances of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is a mixture of two substances of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is a mixture of two substances in a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a lithium hydroxide aqueous solution.
Example 8
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (2.4-3.6) to (7.5-12.0), carrying out heat treatment for 4.5-7 h under the conditions of protective atmosphere and 600-800 ℃, then dissolving with an alkali solution at the temperature of 45-100 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is a mixture of silicon powder and aluminum powder.
The boron-containing compound is a mixture of more than three of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is a mixture of more than three substances of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is a mixture of three substances of sodium hydroxide aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
Example 9
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.2-1.8) to (11.0-16.0), carrying out heat treatment for 2.5-5 h under the condition of protective atmosphere and 750-1000 ℃, then dissolving the mixture with water at the room temperature of 50 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is silicon powder, or aluminum powder, or a mixture of silicon powder and aluminum powder.
The boron-containing compound is more than one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is more than one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
Example 10
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.2-1.8) to (11.0-16.0), carrying out heat treatment for 2.5-5 h under the conditions of protective atmosphere and 750-1000 ℃, then dissolving with an alkali solution at the temperature of room temperature-50 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is silicon powder.
The boron-containing compound is one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is one of a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a lithium hydroxide aqueous solution.
Example 11
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.2-1.8) to (11.0-16.0), carrying out heat treatment for 2.5-5 h under the conditions of protective atmosphere and 750-1000 ℃, then dissolving with an alkali solution at the temperature of room temperature-50 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is aluminum powder.
The boron-containing compound is a mixture of two substances of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is a mixture of two substances of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is a mixture of two substances in a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a lithium hydroxide aqueous solution.
Example 12
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.2-1.8) to (11.0-16.0), carrying out heat treatment for 2.5-5 h under the conditions of protective atmosphere and 750-1000 ℃, then dissolving with an alkali solution at the temperature of room temperature-50 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is a mixture of silicon powder and aluminum powder.
The boron-containing compound is a mixture of more than three of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is a mixture of more than three substances of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is a mixture of three substances of sodium hydroxide aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
Example 13
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.8-2.8) to (0.2-4.0), carrying out heat treatment for 0.5-3 h under the condition of protective atmosphere and 850-1200 ℃, then dissolving with water at 195-250 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is silicon powder, or aluminum powder, or a mixture of silicon powder and aluminum powder.
The boron-containing compound is more than one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is more than one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
Example 14
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.8-2.8) to (0.2-4.0), carrying out heat treatment for 0.5-3 h under the condition of protective atmosphere and 850-1200 ℃, then dissolving with an alkali solution at 195-250 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is silicon powder.
The boron-containing compound is one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is one of a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a lithium hydroxide aqueous solution.
Example 15
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.8-2.8) to (0.2-4.0), carrying out heat treatment for 0.5-3 h under the condition of protective atmosphere and 850-1200 ℃, then dissolving with an alkali solution at 195-250 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is aluminum powder.
The boron-containing compound is a mixture of two substances of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is a mixture of two substances of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is a mixture of two substances in a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a lithium hydroxide aqueous solution.
Example 16
A method for preparing amorphous boron powder. The preparation method in this example is:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.8-2.8) to (0.2-4.0), carrying out heat treatment for 0.5-3 h under the condition of protective atmosphere and 850-1200 ℃, then dissolving with an alkali solution at 195-250 ℃, filtering, washing and drying to obtain amorphous boron powder.
The reducing agent is a mixture of silicon powder and aluminum powder.
The boron-containing compound is a mixture of more than three of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate.
The alkali metal compound-containing molten salt is a mixture of more than three substances of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate.
The alkali solution is a mixture of three substances of sodium hydroxide aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
Compared with the prior art, the specific implementation mode has the following positive effects:
(1) in the embodiment, boric acid, sodium tetraborate, potassium tetraborate, lithium tetraborate and other boron-containing compounds can be used as a boron source besides boron oxide, so that the raw material source is widened, and the production cost is reduced.
(2) The alkali metal compound-containing molten salt adopted by the embodiment can participate in the chemical reaction, improve the thermodynamic condition of the chemical reaction, promote the reduction reaction, improve the yield and improve the recovery rate. The product after heat treatment can be directly washed by water or alkali, the process is simple, the reaction by-product can be recycled, the defect of serious pollution to the environment caused by the traditional acid washing process is avoided, the production process has no pollution to the environment, and the industrial production is easy to realize.
(3) The specific embodiment introduces the alkali metal compound-containing molten salt into the reaction system, and the existence of the alkali metal compound-containing molten salt can form a liquid phase at a lower temperature, strengthen the mass transfer process, improve the dynamic conditions of the chemical reaction and improve the reduction reaction efficiency. In addition, the alkali metal compound-containing molten salt can participate in chemical reaction, improve the thermodynamic condition of the chemical reaction, promote the reduction reaction, improve the yield and the recovery rate, and the recovery rate of boron is higher than 90 percent. After the alkali metal compound molten salt is introduced, the reaction is carried out in a liquid phase, the reaction condition is mild, and the generated boron powder has the characteristics of small particle size and narrow particle size distribution.
(4) The boron powder prepared by the specific embodiment is amorphous boron powder, the content of B is more than or equal to 95 wt%, and high-purity boron powder can be obtained under the optimal process conditions. Fig. 1 is an XRD spectrum of the boron powder prepared in example 10, and as can be seen from fig. 1, the prepared boron powder is amorphous boron powder, and the chemical composition analysis result shows that the B content is 98.54%; fig. 2 is an SEM photograph of the boron powder obtained in example 16, and it can be seen from fig. 2 that the obtained boron powder has a uniform particle size and forms agglomerate particles.
Therefore, the specific implementation mode has the characteristics of low production cost, environmental friendliness, easiness in industrial production, capability of recycling reaction byproducts and high boron recovery rate, and the prepared amorphous boron powder has small particle size, narrow particle size distribution and high purity.
Claims (2)
1. A preparation method of amorphous boron powder is characterized in that the preparation method comprises the following steps:
uniformly mixing a reducing agent, a boron-containing compound and an alkali metal-containing compound molten salt according to the mass ratio of the reducing agent to the boron-containing compound to the alkali metal-containing compound molten salt of 1.0 to (1.2-3.6) to (0.2-16.0), carrying out heat treatment for 0.5-8 h at the temperature of 600-1300 ℃ in a protective atmosphere, then dissolving the mixture with water or an alkali solution at the temperature of room temperature-250 ℃, filtering, washing and drying to obtain amorphous boron powder;
the reducing agent is silicon powder, or aluminum powder, or a mixture of silicon powder and aluminum powder;
the boron-containing compound is more than one of boron oxide, boric acid, sodium tetraborate, potassium tetraborate and lithium tetraborate;
the alkali metal compound-containing molten salt is more than one of sodium hydroxide, sodium carbonate, sodium silicate, potassium hydroxide, potassium carbonate, potassium silicate, lithium hydroxide, lithium carbonate, lithium silicate and sodium aluminate;
SiO in the sodium silicate2With Na2The molar ratio of O is less than or equal to 1;
the preparation method of the amorphous boron powder is characterized in that SiO in the potassium silicate2And K2The molar ratio of O is less than or equal to 1;
SiO in the lithium silicate2With Li2The molar ratio of O is less than or equal to 1.
2. The method for producing an amorphous boron powder according to claim 1, characterized in that the alkali solution is one or more of an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution and an aqueous lithium hydroxide solution.
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| CN102491359A (en) * | 2011-12-21 | 2012-06-13 | 昆明理工大学 | Method for purifying amorphous rough boron powder through pressurizing and leaching |
| CN102583420B (en) * | 2012-02-24 | 2013-03-13 | 深圳市新星轻合金材料股份有限公司 | Circulating preparation method for producing simple substance boron and synchronously producing sodium cryolite based on sodium fluoborate as intermediate raw material |
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| CN108439422B (en) * | 2018-03-13 | 2021-10-15 | 东北大学 | Method for preparing titanium boride alloy through aluminothermic reduction |
| CN109179444B (en) * | 2018-10-11 | 2020-08-25 | 武汉科技大学 | Preparation method of amorphous boron powder |
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