CN109179444A - A kind of preparation method of amorphous boron powder - Google Patents
A kind of preparation method of amorphous boron powder Download PDFInfo
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- CN109179444A CN109179444A CN201811185344.9A CN201811185344A CN109179444A CN 109179444 A CN109179444 A CN 109179444A CN 201811185344 A CN201811185344 A CN 201811185344A CN 109179444 A CN109179444 A CN 109179444A
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Abstract
The present invention relates to a kind of preparation methods of amorphous boron powder.Its technical solution is: by reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.2~3.6): (0.2~16.0); the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed; 0.5~8h is heat-treated under the conditions of protective atmosphere and 600~1300 DEG C; then it is dissolved under the conditions of room temperature~250 DEG C with water or aqueous slkali; filtering; washing, it is dry, amorphous boron powder is made.The present invention has the characteristics that production cost is low, environmental-friendly, easy to industrialized production, byproduct of reaction can recycle and the rate of recovery of boron is high, and prepared amorphous boron powder partial size is small, narrow particle size distribution and purity is high.
Description
Technical field
The invention belongs to pure boron field of material technology.More particularly to a kind of preparation method of amorphous boron powder.
Background technique
Amorphous boron powder has many advantages, such as that large specific surface area and combustion heat value are high, be mainly used for Metallic Materials Held In Shanghai synthesis and
The boron-rich fuel of aerospace field, also serves as the initiator of air bag.
Currently, the preparation of boron powder mainly has borine cracking process, halogenation boron hydrogen thermal reduction, fused salt electrolysis process, metal fever
Reduction method etc..Borine cracking process is that redox reaction occurs using sodium hydride and boron trifluoride etherate to generate second boron
Then alkane carries out cracking to diborane under the conditions of 300~900 DEG C and prepares amorphous boron.Though purity is high can be made in this method
Amorphous boron powder, but diborane is in gaseous state and has severe toxicity at normal temperature, and so that production environment is harsh, and production cost is higher, difficult
It is generated with industrializing.Halogenation boron hydrogen thermal reduction is with pure H2BBr of the reduction by purification3Or BCl3, made from this method
Though boron powder purity with higher, high production cost, the boron rate of recovery are low and very high to the requirement for anticorrosion of environmental protection facility and equipment,
Also it cannot achieve industrialized production.Fused salt electrolysis process is that the compound of electrolysis boron under the conditions of high-temperature molten salt prepares pure boron, electricity
Solution prepares boron powder, and most distinct issues are that electrode material is difficult to resolve certainly, and (Peng Cheng, Chen Song, Wu Yanke wait for low yield and energy consumption height
Fused salt electrolysis process prepares the research rare metal of boron powder, 2010,34 (2): 264-270.).Metallothermic processes is existed with magnesium powder
Thick boron (beans will river, Zhang Tingan Preparation of boron powder by self-propagating high temperature synthesis metallurgy China YouSe metallography is made in reduction-oxidation boron under high temperature
Report, 2004,14 (12): 2137-2143.), amorphous pure boron powder, metal fever are then prepared using HCl, NaOH and HF processing
Prepared by reduction method, though boron powder technical maturity, yield are big, and product purity is low, size distribution is uneven, in subsequent processes
Hydrochloric acid need to be largely used, the by-product added value of generation is low, has stronger corrosiveness to equipment, and have serious pollution.
Summary of the invention
The present invention is directed to overcome prior art defect, provide a kind of production cost it is low, it is environmental-friendly, be easy to industrial metaplasia
Production, the amorphous boron powder that byproduct of reaction can recycle and the boron rate of recovery is high preparation method, prepared amorphous boron powder
Partial size is small, narrow particle size distribution and purity is high.
To achieve the above object, the technical solution adopted by the present invention is that: press reducing agent: boron-containing compound: alkali metal containing
The mass ratio 1.0 of object fused salt: (1.2~3.6): (0.2~16.0) is closed, by the reducing agent, the boron-containing compound and described
Alkali metal-containing compound fused salt is uniformly mixed, and 0.5~8h is heat-treated under the conditions of protective atmosphere and 600~1300 DEG C, then
It is dissolved, is filtered under the conditions of room temperature~250 DEG C with water or aqueous slkali, washed, it is dry, amorphous boron powder is made.
The reducing agent be silicon powder or be aluminium powder or be silicon powder and aluminium powder mixture.
The boron-containing compound is one or more of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
One or more of potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
The aqueous slkali be one of sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution with
On.
SiO in the sodium metasilicate2With Na2Molar ratio≤1 of O.
SiO in the potassium silicate2With K2Molar ratio≤1 of O.
SiO in the lithium metasilicate2With Li2Molar ratio≤1 of O.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art:
(1), the boracics chemical combination such as boric acid, sodium tetraborate, dipotassium tetraborate, lithium tetraborate can be used in addition to boron oxide in the present invention
Object has widened raw material sources as boron source, and production cost is low.
(2), the alkali metal-containing compound fused salt that the present invention uses can participate in chemically reacting, and improve the thermodynamics of chemical reaction
Condition, the progress for promoting reduction reaction improve yield and improve the rate of recovery.Product after heat treatment can directly wash or alkali cleaning,
Simple process, byproduct recoverable avoid traditional acid cleaning process and cause the drawbacks of seriously polluting to environment, production process
No pollution to the environment, it is easy to industrialized production.
(3), the present invention introduces alkali metal-containing compound fused salt in the reaction system, and alkali metal-containing compound fused salt is deposited
Liquid phase can be being formed at a lower temperature, is strengthening mass transport process, is improving the dynamic conditions of chemical reaction, and it is anti-to improve reduction
Answer efficiency.In addition, alkali metal-containing compound fused salt can participate in chemically reacting, improve the thermodynamic condition of chemical reaction, promotes also
The progress of original reaction, improves yield and the rate of recovery, the rate of recovery of boron are above 90%.After introducing alkali metal compound fused salt, instead
It should carry out in the liquid phase, reaction condition is mild, and the boron powder of generation has the characteristics that partial size is small and narrow particle size distribution.
(4), boron powder produced by the present invention is amorphous boron powder, and B content >=95wt%, preferred process conditions can obtain B
Content is greater than the high purity boron powder of 98.5wt%.Boron powder uniform particle diameter obtained forms agglomerate particle.
Therefore, with production cost, low, environmental-friendly, easy to industrialized production, byproduct of reaction can recycle benefit to the present invention
With the feature high with the rate of recovery of boron, prepared amorphous boron powder partial size is small, narrow particle size distribution and purity is high.
Detailed description of the invention
Fig. 1 is a kind of XRD spectrum of amorphous boron powder prepared by the present invention；
Fig. 2 is the SEM photograph of another amorphous boron powder prepared by the present invention.
Specific embodiment
In order to better understand the present invention, below by the drawings and examples content that the present invention is further explained, but this
Invention is not limited solely to the following examples.
It is first that material Unify legislation involved in present embodiment is as follows to avoid repeating, it is no longer superfluous in embodiment
It states:
SiO in the sodium metasilicate2With Na2Molar ratio≤1 of O.
SiO in the potassium silicate2With K2Molar ratio≤1 of O.
SiO in the lithium metasilicate2With Li2Molar ratio≤1 of O.
Embodiment 1
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.5~2.5): (3.5~
8.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protective atmosphere
It is heat-treated 6~8h under the conditions of with 1000~1300 DEG C, is then dissolved under the conditions of 95~200 DEG C with water, filters, washs, it is dry,
Amorphous boron powder is made.
The reducing agent be silicon powder or be aluminium powder or be silicon powder and aluminium powder mixture.
The boron-containing compound is one or more of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
One or more of potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
Embodiment 2
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.5~2.5): (3.5~
8.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protective atmosphere
It is heat-treated 6~8h under the conditions of with 1000~1300 DEG C, is then dissolved under the conditions of 95~200 DEG C with aqueous slkali, filters, washing,
It is dry, amorphous boron powder is made.
The reducing agent is silicon powder.
The boron-containing compound is one of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
One of potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
The aqueous slkali is one of sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
Embodiment 3
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.5~2.5): (3.5~
8.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protective atmosphere
It is heat-treated 6~8h under the conditions of with 1000~1300 DEG C, is then dissolved under the conditions of 95~200 DEG C with aqueous slkali, filters, washing,
It is dry, amorphous boron powder is made.
The reducing agent is aluminium powder.
The boron-containing compound is two kinds of substances in boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Mixture.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
The mixture of two kinds of substances in potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
The aqueous slkali is two kinds of substances in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
Mixture.
Embodiment 4
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.5~2.5): (3.5~
8.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protective atmosphere
It is heat-treated 6~8h under the conditions of with 1000~1300 DEG C, is then dissolved under the conditions of 95~200 DEG C with aqueous slkali, filters, washing,
It is dry, amorphous boron powder is made.
The reducing agent is the mixture of silicon powder and aluminium powder.
The boron-containing compound is boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate, three kinds or more objects in lithium tetraborate
The mixture of matter.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
Potassium, lithium hydroxide, lithium carbonate, lithium metasilicate, three kinds or more substances in sodium aluminate mixture.
The aqueous slkali be sodium hydrate aqueous solution, potassium hydroxide aqueous solution, three kinds of substances of lithium hydroxide aqueous solution it is mixed
Close object.
Embodiment 5
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (2.4~3.6): (7.5~
12.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protectiveness gas
It is heat-treated 4.5~7h under the conditions of atmosphere and 600~800 DEG C, is then dissolved under the conditions of 45~100 DEG C with water, filters, washs, does
It is dry, amorphous boron powder is made.
The reducing agent be silicon powder or be aluminium powder or be silicon powder and aluminium powder mixture.
The boron-containing compound is one or more of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
One or more of potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
Embodiment 6
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (2.4~3.6): (7.5~
12.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protectiveness gas
It is heat-treated 4.5~7h under the conditions of atmosphere and 600~800 DEG C, is then dissolved under the conditions of 45~100 DEG C with aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made.
The reducing agent is silicon powder.
The boron-containing compound is one of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
One of potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
The aqueous slkali is one of sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
Embodiment 7
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (2.4~3.6): (7.5~
12.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protectiveness gas
It is heat-treated 4.5~7h under the conditions of atmosphere and 600~800 DEG C, is then dissolved under the conditions of 45~100 DEG C with aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made.
The reducing agent is aluminium powder.
The boron-containing compound is two kinds of substances in boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Mixture.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
The mixture of two kinds of substances in potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
The aqueous slkali is two kinds of substances in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
Mixture.
Embodiment 8
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (2.4~3.6): (7.5~
12.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protectiveness gas
It is heat-treated 4.5~7h under the conditions of atmosphere and 600~800 DEG C, is then dissolved under the conditions of 45~100 DEG C with aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made.
The reducing agent is the mixture of silicon powder and aluminium powder.
The boron-containing compound is boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate, three kinds or more objects in lithium tetraborate
The mixture of matter.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
Potassium, lithium hydroxide, lithium carbonate, lithium metasilicate, three kinds or more substances in sodium aluminate mixture.
The aqueous slkali be sodium hydrate aqueous solution, potassium hydroxide aqueous solution, three kinds of substances of lithium hydroxide aqueous solution it is mixed
Close object.
Embodiment 9
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.2~1.8): (11.0~
16.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protectiveness gas
It is heat-treated 2.5~5h under the conditions of atmosphere and 750~1000 DEG C, is then dissolved under the conditions of room temperature~50 DEG C with water, filters, washing,
It is dry, amorphous boron powder is made.
The reducing agent be silicon powder or be aluminium powder or be silicon powder and aluminium powder mixture.
The boron-containing compound is one or more of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
One or more of potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
Embodiment 10
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.2~1.8): (11.0~
16.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protectiveness gas
It is heat-treated 2.5~5h under the conditions of atmosphere and 750~1000 DEG C, is then dissolved under the conditions of room temperature~50 DEG C with aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made.
The reducing agent is silicon powder.
The boron-containing compound is one of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
One of potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
The aqueous slkali is one of sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
Embodiment 11
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.2~1.8): (11.0~
16.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protectiveness gas
It is heat-treated 2.5~5h under the conditions of atmosphere and 750~1000 DEG C, is then dissolved under the conditions of room temperature~50 DEG C with aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made.
The reducing agent is aluminium powder.
The boron-containing compound is two kinds of substances in boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Mixture.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
The mixture of two kinds of substances in potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
The aqueous slkali is two kinds of substances in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
Mixture.
Embodiment 12
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.2~1.8): (11.0~
16.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protectiveness gas
It is heat-treated 2.5~5h under the conditions of atmosphere and 750~1000 DEG C, is then dissolved under the conditions of room temperature~50 DEG C with aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made.
The reducing agent is the mixture of silicon powder and aluminium powder.
The boron-containing compound is boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate, three kinds or more objects in lithium tetraborate
The mixture of matter.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
Potassium, lithium hydroxide, lithium carbonate, lithium metasilicate, three kinds or more substances in sodium aluminate mixture.
The aqueous slkali be sodium hydrate aqueous solution, potassium hydroxide aqueous solution, three kinds of substances of lithium hydroxide aqueous solution it is mixed
Close object.
Embodiment 13
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.8~2.8): (0.2~
4.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protective atmosphere
It is heat-treated 0.5~3h under the conditions of with 850~1200 DEG C, is then dissolved under the conditions of 195~250 DEG C with water, filters, washs, does
It is dry, amorphous boron powder is made.
The reducing agent be silicon powder or be aluminium powder or be silicon powder and aluminium powder mixture.
The boron-containing compound is one or more of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
One or more of potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
Embodiment 14
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.8~2.8): (0.2~
4.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protective atmosphere
It is heat-treated 0.5~3h under the conditions of with 850~1200 DEG C, is then dissolved under the conditions of 195~250 DEG C with aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made.
The reducing agent is silicon powder.
The boron-containing compound is one of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
One of potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
The aqueous slkali is one of sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
Embodiment 15
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.8~2.8): (0.2~
4.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protective atmosphere
It is heat-treated 0.5~3h under the conditions of with 850~1200 DEG C, is then dissolved under the conditions of 195~250 DEG C with aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made.
The reducing agent is aluminium powder.
The boron-containing compound is two kinds of substances in boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate
Mixture.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
The mixture of two kinds of substances in potassium, lithium hydroxide, lithium carbonate, lithium metasilicate and sodium aluminate.
The aqueous slkali is two kinds of substances in sodium hydrate aqueous solution, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution
Mixture.
Embodiment 16
A kind of preparation method of amorphous boron powder.Preparation method described in the present embodiment is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.8~2.8): (0.2~
4.0), the reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protective atmosphere
It is heat-treated 0.5~3h under the conditions of with 850~1200 DEG C, is then dissolved under the conditions of 195~250 DEG C with aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made.
The reducing agent is the mixture of silicon powder and aluminium powder.
The boron-containing compound is boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate, three kinds or more objects in lithium tetraborate
The mixture of matter.
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, silicic acid
Potassium, lithium hydroxide, lithium carbonate, lithium metasilicate, three kinds or more substances in sodium aluminate mixture.
The aqueous slkali be sodium hydrate aqueous solution, potassium hydroxide aqueous solution, three kinds of substances of lithium hydroxide aqueous solution it is mixed
Close object.
Present embodiment has following good effect compared with prior art:
(1), boric acid, sodium tetraborate, dipotassium tetraborate, lithium tetraborate etc. can be used in addition to boron oxide in present embodiment
Boron-containing compound has widened raw material sources as boron source, reduces production cost.
(2), the alkali metal-containing compound fused salt that present embodiment uses can participate in chemically reacting, and improve chemical reaction
Thermodynamic condition, promote reduction reaction progress, improve yield and improve the rate of recovery.Product after heat treatment can be washed directly
Or alkali cleaning, simple process, byproduct of reaction recoverable, it avoids traditional acid cleaning process and causes the disadvantage seriously polluted to environment
End, production process no pollution to the environment are easy to industrialized production.
(3), present embodiment introduces alkali metal-containing compound fused salt in the reaction system, and alkali metal-containing compound is molten
The presence of salt can form liquid phase at a lower temperature, strengthen mass transport process, improve the dynamic conditions of chemical reaction, improve
Reduction reaction efficiency.In addition, alkali metal-containing compound fused salt can participate in chemically reacting, improve the thermodynamic condition of chemical reaction,
Promote the progress of reduction reaction, improves yield and the rate of recovery, the rate of recovery of boron are above 90%.Introduce alkali metal compound fused salt
Afterwards, reaction carries out in the liquid phase, and reaction condition is mild, and the boron powder of generation has the characteristics that partial size is small and narrow particle size distribution.
(4), boron powder made from present embodiment is amorphous boron powder, B content >=95wt%, preferred process conditions
High-purity boron powder can be obtained.Fig. 1 is the XRD spectrum of boron powder made from embodiment 10, it will be seen from figure 1 that boron powder obtained
For amorphous boron powder, B content is 98.54% to chemical composition analysis as the result is shown；Fig. 2 is the SEM of boron powder made from embodiment 16
Photo, figure it is seen that boron powder uniform particle diameter obtained, forms agglomerate particle.
Therefore, present embodiment has that production cost is low, environmental-friendly, easy to industrialized production, byproduct of reaction
It can recycle and the high feature of the rate of recovery of boron, prepared amorphous boron powder partial size is small, narrow particle size distribution and purity is high.
Claims (5)
1. a kind of preparation method of amorphous boron powder, it is characterised in that the preparation method is:
By reducing agent: boron-containing compound: the mass ratio 1.0 of alkali metal-containing compound fused salt: (1.2~3.6): (0.2~16.0),
The reducing agent, the boron-containing compound and the alkali metal-containing compound fused salt are uniformly mixed, in protective atmosphere and 600
It is heat-treated 0.5~8h under the conditions of~1300 DEG C, is then dissolved under the conditions of room temperature~250 DEG C with water or aqueous slkali, filters, washes
It washs, it is dry, amorphous boron powder is made；
The reducing agent be silicon powder or be aluminium powder or be silicon powder and aluminium powder mixture；
The boron-containing compound is one or more of boron oxide, boric acid, sodium tetraborate, dipotassium tetraborate and lithium tetraborate；
The alkali metal-containing compound fused salt is sodium hydroxide, sodium carbonate, sodium metasilicate, potassium hydroxide, potassium carbonate, potassium silicate, hydrogen
One or more of lithia, lithium carbonate, lithium metasilicate and sodium aluminate.
2. the preparation method of amorphous boron powder according to claim 1 is characterized in that the aqueous slkali is that sodium hydroxide is water-soluble
One or more of liquid, potassium hydroxide aqueous solution and lithium hydroxide aqueous solution.
3. the preparation method of amorphous boron powder according to claim 1, the SiO being characterized in that in the sodium metasilicate2With Na2O's
Molar ratio≤1.
4. the preparation method of amorphous boron powder according to claim 1, the SiO being characterized in that in the potassium silicate2With K2O's
Molar ratio≤1.
5. the preparation method of amorphous boron powder according to claim 1, the SiO being characterized in that in the lithium metasilicate2With Li2O's
Molar ratio≤1.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020073806A1 (en) * | 2018-10-11 | 2020-04-16 | 武汉科技大学 | Method for preparing amorphous boron powder |
| CN112250081A (en) * | 2020-10-10 | 2021-01-22 | 中北大学 | Preparation method and application of boron oxide quantum dots |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20130045152A1 (en) * | 2011-08-15 | 2013-02-21 | Ind Llc | Elemental Boron by Reduction of Boron Halides by metals and their borides |
| CN108439422A (en) * | 2018-03-13 | 2018-08-24 | 东北大学 | A kind of method that aluminothermic reduction prepares boronation titanium alloy |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104402014B (en) * | 2014-11-07 | 2016-04-20 | 上海九鼎粉体材料有限公司 | The production technique of amorphous boron powder |
| CN108069432A (en) * | 2016-11-15 | 2018-05-25 | 王婉婷 | A kind of method of low content amorphous boron powder Fast Purification |
| CN109179444B (en) * | 2018-10-11 | 2020-08-25 | 武汉科技大学 | Preparation method of amorphous boron powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130045152A1 (en) * | 2011-08-15 | 2013-02-21 | Ind Llc | Elemental Boron by Reduction of Boron Halides by metals and their borides |
| 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 |
| CN108439422A (en) * | 2018-03-13 | 2018-08-24 | 东北大学 | A kind of method that aluminothermic reduction prepares boronation titanium alloy |
Non-Patent Citations (1)
| Title |
|---|
| 王晓玲: ""熔盐介质中二硼化钛超细粉体的制备研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020073806A1 (en) * | 2018-10-11 | 2020-04-16 | 武汉科技大学 | Method for preparing amorphous boron powder |
| CN112250081A (en) * | 2020-10-10 | 2021-01-22 | 中北大学 | Preparation method and application of boron oxide quantum dots |
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