CN112125316A - Purification method of low-purity amorphous boron powder - Google Patents
Purification method of low-purity amorphous boron powder Download PDFInfo
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- CN112125316A CN112125316A CN202011052612.7A CN202011052612A CN112125316A CN 112125316 A CN112125316 A CN 112125316A CN 202011052612 A CN202011052612 A CN 202011052612A CN 112125316 A CN112125316 A CN 112125316A
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- boron powder
- acid leaching
- purity
- low
- boron
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000000746 purification Methods 0.000 title abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 34
- 238000002386 leaching Methods 0.000 claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000007670 refining Methods 0.000 claims abstract description 27
- 229910052796 boron Inorganic materials 0.000 claims abstract description 19
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002893 slag Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 16
- 239000010935 stainless steel Substances 0.000 description 16
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/023—Boron
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for purifying low-purity amorphous boron powder, belonging to the technical field of boron purification. The method comprises the steps of pressing low-purity amorphous boron powder into blocky boron, placing the blocky boron in a vacuum furnace for vacuum refining, cooling along with the furnace, then grinding into boron powder, adding hydrochloric acid into the boron powder for acid leaching and impurity removal to obtain acid leaching solution and acid leaching residue, washing the acid leaching residue to be neutral by deionized water, and performing vacuum drying to obtain the high-purity amorphous boron powder. The method has the advantages of short process, simple and reliable process, easy operation, low preparation cost, suitability for large-scale production, industrial potential, good purification effect and high value of the purified high-purity boron powder product.
Description
Technical Field
The invention relates to a method for purifying low-purity amorphous boron powder, belonging to the technical field of boron purification.
Background
The boron powder is an important boron fine chemical product and can be widely applied to the fields of nuclear energy, aerospace, war industry, chemical industry, energy and the like. At present, the preparation method of boron powder mainly comprises a molten salt electrolysis method, an diborane cracking method, a hydrogen reduction method, a thermal decomposition method, a self-propagating magnesiothermic reduction method, a self-propagating aluminothermic reduction method and the like. The former three can realize the direct synthesis of high-purity boron powder, but the synthesis efficiency is low, and the industrial production cannot be realized. Therefore, the magnesium thermal self-propagating reduction method is the mainstream method for industrially producing boron powder in China at present due to high reaction speed, low cost and the like.
The paper "boron powder is prepared by a self-propagating metallurgical method", namely, magnesium powder is adopted to reduce diboron trioxide to obtain amorphous boron powder with the purity of 92.43%; in the thesis of "preparation of amorphous boron powder by magnesiothermic reduction method and industrialization", amorphous boron powder with 93.13% content is obtained by pilot plant production, and the thesis of "preparation of ultrafine amorphous boron powder by magnesiothermic reduction method" adopts self-propagating high-temperature synthesis method, uses ultrafine magnesium powder to reduce diboron trioxide, and then obtains amorphous boron powder with 94.6% purity by hydrochloric acid leaching. The amorphous boron powder with the purity of 85-95% can be obtained by reducing diboron trioxide by using magnesium powder industrially, and for low-purity (85-92%) boron powder with a large impurity content, the physicochemical property of the amorphous boron powder cannot reach the use standard in the fields of nuclear energy, aerospace, military industry, chemical industry, energy and the like. Therefore, purification of low-purity amorphous boron powder is very important for the boron fine chemical industry, but a process method for purifying low-purity boron powder is not available at present.
Disclosure of Invention
The invention provides a method for purifying low-purity amorphous boron powder, which aims at solving the problems in the prior art in the purification of low-purity amorphous boron powder.
A method for purifying low-purity amorphous boron powder comprises the following specific steps:
(1) pressing the low-purity amorphous boron powder into blocky boron;
(2) putting the blocky boron in the step (1) into a vacuum furnace for vacuum refining, cooling along with the furnace, and then grinding into boron powder;
(3) and (3) adding hydrochloric acid into the boron powder obtained in the step (2) to carry out acid leaching and impurity removal to obtain acid leaching solution and acid leaching slag, washing the acid leaching slag to be neutral by deionized water, and carrying out vacuum drying to obtain high-purity amorphous boron powder.
The pressure of the vacuum refining in the step (2) is 10-3~10-2Pa, the vacuum refining temperature is 800-1200 ℃, and the vacuum refining time is 2-4 h.
The concentration of the hydrochloric acid in the step (3) is 1-2 mol/L, the acid leaching temperature is 80-100 ℃, and the acid leaching time is 2-4 h.
And (4) the solid-to-liquid ratio g: mL of the boron powder to the hydrochloric acid in the step (3) is 1: 5-20.
The invention discloses a principle of phase transformation of impurities in amorphous boron powder by vacuum refining, which comprises the following steps: purifying low-purity amorphous boron powder which is produced by magnesiothermic reduction and has the purity of below 92 percent sold in the market, so that acid insoluble impurities consisting of Mg, Fe, Si, O and the like in the boron powder are subjected to phase structure transformation in a high-temperature and vacuum environment and converted into a soluble phase structure; meanwhile, in a vacuum environment, volatile impurities such as Mg and O in the boron powder are volatilized in different gaseous states, so that the purposes of reducing the impurities in the amorphous boron powder and improving the boron content are achieved.
The invention has the beneficial effects that:
the purification method of vacuum refining and acid washing has the characteristics of short flow, simple and reliable process, easy operation, low preparation process cost, suitability for large-scale production, industrial potential and good purification effect.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a method for purifying low-purity amorphous boron powder comprises the following specific steps:
(1) pressing commercial amorphous boron powder with the purity of 85.61 percent into massive boron under the pressure of 2 MPa;
(2) putting the blocky boron in the step (1) into a stainless steel crucible, then putting the stainless steel crucible into a vacuum furnace for vacuum refining, cooling the stainless steel crucible along with the furnace, then grinding the stainless steel crucible, and sieving the boron powder by a 200-mesh sieve to obtain boron powder; wherein the pressure of vacuum refining is 10-3Pa, the vacuum refining temperature is 800 ℃, and the vacuum refining time is 4 hours;
(3) adding hydrochloric acid with the concentration of 1mol/L into the boron powder in the step (2), then carrying out acid leaching at the temperature of 80 ℃ for 2h to remove impurities to obtain acid leaching solution and acid leaching slag, washing the acid leaching slag to be neutral by deionized water, and carrying out vacuum drying at the temperature of 80 ℃ for 24h to obtain high-purity amorphous boron powder; wherein the solid-to-liquid ratio g: mL of the boron powder to the hydrochloric acid is 1: 5;
the purity of the high-purity amorphous boron powder of this example was 91.86% by ICP analysis.
Example 2: a method for purifying low-purity amorphous boron powder comprises the following specific steps:
(1) pressing commercial amorphous boron powder with the purity of 85.61 percent into massive boron under the pressure of 5 MPa;
(2) putting the blocky boron in the step (1) into a stainless steel crucible, then putting the stainless steel crucible into a vacuum furnace for vacuum refining, cooling the stainless steel crucible along with the furnace, then grinding the stainless steel crucible, and sieving the boron powder by a 200-mesh sieve to obtain boron powder; wherein the pressure of vacuum refining is 10-2Pa, the vacuum refining temperature is 1200 ℃, and the vacuum refining time is 2 hours;
(3) adding hydrochloric acid with the concentration of 2mol/L into the boron powder in the step (2), then carrying out acid leaching at the temperature of 100 ℃ for 4h to remove impurities to obtain acid leaching solution and acid leaching residue, washing the acid leaching residue to be neutral by deionized water, and carrying out vacuum drying at the temperature of 60 ℃ for 36h to obtain high-purity amorphous boron powder; wherein the solid-to-liquid ratio g: mL of the boron powder to the hydrochloric acid is 1: 20;
the purity of the high-purity amorphous boron powder of this example was 95.22% by ICP analysis.
Example 3: a method for purifying low-purity amorphous boron powder comprises the following specific steps:
(1) pressing commercially available amorphous boron powder with the purity of 90.44% into blocky boron under the pressure of 3 MPa;
(2) putting the blocky boron in the step (1) into a stainless steel crucible, then putting the stainless steel crucible into a vacuum furnace for vacuum refining, cooling the stainless steel crucible along with the furnace, then grinding the stainless steel crucible, and sieving the boron powder by a 200-mesh sieve to obtain boron powder; wherein the pressure of vacuum refining is 0.5 × 10-3Pa, the vacuum refining temperature is 1000 ℃, and the vacuum refining time is 3 hours;
(3) adding hydrochloric acid with the concentration of 1.5mol/L into the boron powder in the step (2), then carrying out acid leaching for 3h at the temperature of 90 ℃ to remove impurities to obtain acid leaching solution and acid leaching slag, washing the acid leaching slag to be neutral by deionized water, and carrying out vacuum drying for 36h at the temperature of 60 ℃ to obtain high-purity amorphous boron powder; wherein the solid-to-liquid ratio g: mL of the boron powder to the hydrochloric acid is 1: 8;
the purity of the high-purity amorphous boron powder of this example was 95.90% by ICP analysis.
Example 4: a method for purifying low-purity amorphous boron powder comprises the following specific steps:
(1) pressing commercially available amorphous boron powder with the purity of 90.44% into blocky boron under the pressure of 3 MPa;
(2) putting the blocky boron in the step (1) into a stainless steel crucible, then putting the stainless steel crucible into a vacuum furnace for vacuum refining, cooling the stainless steel crucible along with the furnace, then grinding the stainless steel crucible, and sieving the boron powder by a 200-mesh sieve to obtain boron powder; wherein the pressure of vacuum refining is 10-3Pa, the vacuum refining temperature is 1200 ℃, and the vacuum refining time is 4 hours;
(3) adding hydrochloric acid with the concentration of 2mol/L into the boron powder in the step (2), then carrying out acid leaching at the temperature of 95 ℃ for 4h to remove impurities to obtain acid leaching solution and acid leaching residue, washing the acid leaching residue to be neutral by deionized water, and carrying out vacuum drying at the temperature of 70 ℃ for 30h to obtain high-purity amorphous boron powder; wherein the solid-to-liquid ratio g: mL of the boron powder to the hydrochloric acid is 1: 15;
the purity of the high-purity amorphous boron powder of this example was 97.40% by ICP analysis.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (4)
1. A method for purifying low-purity amorphous boron powder is characterized by comprising the following specific steps:
(1) pressing the low-purity amorphous boron powder into blocky boron;
(2) putting the blocky boron in the step (1) into a vacuum furnace for vacuum refining, cooling along with the furnace, and then grinding into boron powder;
(3) and (3) adding hydrochloric acid into the boron powder obtained in the step (2) to carry out acid leaching and impurity removal to obtain acid leaching solution and acid leaching slag, washing the acid leaching slag to be neutral by deionized water, and carrying out vacuum drying to obtain high-purity amorphous boron powder.
2. The method of purifying a low-purity amorphous boron powder according to claim 1, characterized in that: the pressure of the vacuum refining in the step (2) is 10-3~10-2Pa, the vacuum refining temperature is 800-1200 ℃, and the vacuum refining time is 2-4 h.
3. The method of purifying a low-purity amorphous boron powder according to claim 1, characterized in that: the concentration of the hydrochloric acid in the step (3) is 0.5-2 mol/L, the acid leaching temperature is 80-100 ℃, and the acid leaching time is 2-4 h.
4. The method of purifying a low-purity amorphous boron powder according to claim 1, characterized in that: and (3) the solid-to-liquid ratio g/mL of the boron powder to the hydrochloric acid is 1: 5-20.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011052612.7A CN112125316A (en) | 2020-09-29 | 2020-09-29 | Purification method of low-purity amorphous boron powder |
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| CN202011052612.7A CN112125316A (en) | 2020-09-29 | 2020-09-29 | Purification method of low-purity amorphous boron powder |
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| CN112125316A true CN112125316A (en) | 2020-12-25 |
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| CN202011052612.7A Pending CN112125316A (en) | 2020-09-29 | 2020-09-29 | Purification method of low-purity amorphous boron powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114988423A (en) * | 2022-06-27 | 2022-09-02 | 昆明理工大学 | Method for removing magnesium and purifying amorphous boron powder by microwave heating and ultrasonic-assisted acid leaching |
| CN116282055A (en) * | 2023-04-04 | 2023-06-23 | 昆明理工大学 | Method for purifying and modifying amorphous boron powder by acid quenching |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB747287A (en) * | 1954-02-22 | 1956-03-28 | Hermann C Starck Ag | Improvements in or relating to the production of boron |
| CN101780960A (en) * | 2010-03-23 | 2010-07-21 | 昆明理工大学 | Method for purifying crude boron powder |
| 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 |
| CN106276940A (en) * | 2016-07-26 | 2017-01-04 | 深圳市赛普戴蒙德科技有限公司 | A kind of pure boron purifying plant and method |
| CN108069431A (en) * | 2016-11-15 | 2018-05-25 | 王婉婷 | A kind of synthetic method of high-purity amorphous boron powder |
| CN108069433A (en) * | 2016-11-15 | 2018-05-25 | 王婉婷 | A kind of technique of quick synthesis high-purity amorphous boron powder |
-
2020
- 2020-09-29 CN CN202011052612.7A patent/CN112125316A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB747287A (en) * | 1954-02-22 | 1956-03-28 | Hermann C Starck Ag | Improvements in or relating to the production of boron |
| CN101780960A (en) * | 2010-03-23 | 2010-07-21 | 昆明理工大学 | Method for purifying crude boron powder |
| 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 |
| CN106276940A (en) * | 2016-07-26 | 2017-01-04 | 深圳市赛普戴蒙德科技有限公司 | A kind of pure boron purifying plant and method |
| CN108069431A (en) * | 2016-11-15 | 2018-05-25 | 王婉婷 | A kind of synthetic method of high-purity amorphous boron powder |
| CN108069433A (en) * | 2016-11-15 | 2018-05-25 | 王婉婷 | A kind of technique of quick synthesis high-purity amorphous boron powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114988423A (en) * | 2022-06-27 | 2022-09-02 | 昆明理工大学 | Method for removing magnesium and purifying amorphous boron powder by microwave heating and ultrasonic-assisted acid leaching |
| CN116282055A (en) * | 2023-04-04 | 2023-06-23 | 昆明理工大学 | Method for purifying and modifying amorphous boron powder by acid quenching |
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