CN114988423A - Method for removing magnesium and purifying amorphous boron powder by microwave heating and ultrasonic-assisted acid leaching - Google Patents
Method for removing magnesium and purifying amorphous boron powder by microwave heating and ultrasonic-assisted acid leaching Download PDFInfo
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- CN114988423A CN114988423A CN202210735234.5A CN202210735234A CN114988423A CN 114988423 A CN114988423 A CN 114988423A CN 202210735234 A CN202210735234 A CN 202210735234A CN 114988423 A CN114988423 A CN 114988423A
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000002253 acid Substances 0.000 title claims abstract description 46
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 45
- 239000011777 magnesium Substances 0.000 title claims abstract description 45
- 238000002386 leaching Methods 0.000 title claims abstract description 42
- 238000010438 heat treatment Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012535 impurity Substances 0.000 claims abstract description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052786 argon Inorganic materials 0.000 claims abstract description 9
- 239000012065 filter cake Substances 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000008602 contraction Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000007935 neutral effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 11
- 229910052796 boron Inorganic materials 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000008901 benefit Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000007123 defense Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000003380 propellant Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for removing magnesium and purifying amorphous boron powder by microwave heating and ultrasonic-assisted acid leaching, which is characterized by comprising the following steps of: placing amorphous crude boron powder in a microwave oven, introducing argon for microwave heating, preserving heat and cooling to room temperature; adding a hydrochloric acid solution into a sample, and carrying out ultrasonic-assisted acid leaching treatment under a heating condition; filtering the boron powder suspension while the suspension is hot to obtain a filter cake, washing until the pH value is close to neutral, and drying to obtain the amorphous boron powder product with low magnesium. According to the invention, the amorphous boron powder and impurities are selectively heated by microwaves, the impurities are exposed under the principle of thermal expansion and cold contraction, and the hydrochloric acid is promoted to enter the amorphous boron powder along cracks under the assistance of ultrasonic waves by using ultrasonic-assisted acid leaching and react with the impurities, so that the impurities remained in a reaction blind area are better removed; greatly improves the removal efficiency of magnesium impurities, has simple operation, stability, reliability, low cost and high added value, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of chemical impurity removal and purification, and particularly relates to a method for removing magnesium and purifying amorphous boron powder by microwave heating and ultrasonic-assisted acid leaching.
Background
Amorphous boron powder is an important chemical raw material and is widely applied to the fields of national defense, industry, advanced science and the like. The amorphous boron powder has the advantages of high mass calorific value and volume calorific value, clean combustion, no pollution and the like. With the development of science and technology, the national defense, aerospace, aviation and automobile industries are rapidly developed. The demand of the high-tech field for amorphous boron powder is more and more, and the demand for high-purity amorphous boron powder raw materials is continuously increased.
The magnesium thermal reduction is widely applied to producing amorphous boron powder due to high technical maturity, suitability for large-scale production and short reaction time. However, the amorphous boron powder produced by the magnesiothermic reduction method contains a lot of magnesium impurities, and the existence of magnesium directly influences the use value of the amorphous boron powder and reduces the quality of the product. For example, amorphous boron powders are used to make boron-containing fuel-rich propellants because they contain a certain amount of magnesium impurities that hinder the ignition of the boron particles during ignition, have a high level of combustion residues that do not release its high heat, and severely affect the activity and calorific value of the amorphous boron powder, making the boron particles incompatible with the propellant system. Therefore, the magnesium content in the amorphous boron powder needs to be as low as possible in the application. Therefore, it is required to increase the efficiency of removing magnesium as much as possible and to reduce the content of magnesium in the amorphous boron powder.
The method for purifying amorphous boron powder mainly comprises acid leaching and fire purification. The acid leaching method is used for treating amorphous boron powder, and researches show that the mixture of several acids can generate synergistic effect in the reaction process, and the effect of the acid leaching method is better than that of single acid. Wujun et al uses hydrochloric acid, nitric acid and hydrofluoric acid to leach amorphous boron powder to purify boron powder, but only remove impurities which are easily dissolved in acid on the surface of boron powder. (see "university of Kunming' a wet purification method for amorphous crude boron powder: CN202011392138.2[ P ]. 2021-03-12.") since only part of the magnesium impurities in amorphous boron powder are located on the surface of amorphous boron powder and part of the magnesium impurities are located inside the amorphous boron powder particles, they cannot be contacted with acid solution, and thus the magnesium content in amorphous boron powder cannot be reduced to a very low level by means of acid leaching alone. The method of pyrogenic purification by adding diboron trioxide can obtain better purification effect than the acid leaching method. Wujunjunjun et al adds diboron trioxide powder into crude boron powder, mixes and briquettes, purifies the boron powder at a certain temperature, cools the boron powder, and then uses hydrochloric acid for acid leaching to achieve the purpose of boron powder purification, but the method needs a large amount of boron oxide and is not economical (refer to Kunming technology university. a method for purifying crude boron powder: CN201010130202.X [ P ].2010-07-21. ").
With the development of science and technology, the requirement on the purity of amorphous boron powder is higher and higher, how to economically and efficiently remove magnesium impurities in the amorphous boron powder is also more and more important, and the prior art is difficult to meet the requirement on efficiently and rapidly removing magnesium.
Therefore, in order to solve the above problems, a method for purifying amorphous boron powder by removing magnesium through microwave heating and ultrasonic-assisted acid leaching is proposed herein.
Disclosure of Invention
In order to solve the technical problems, the invention designs a method for purifying amorphous boron powder by removing magnesium through microwave heating and ultrasonic-assisted acid leaching, according to the advantage that microwaves selectively heat certain elements in a multiphase material, the amorphous boron powder has strong wave-absorbing capacity and can be heated quickly, while impurities have weak wave-absorbing capacity and can be heated slowly, and due to the principle of thermal expansion and cold contraction, a boron shell wrapping the impurities generates cracks to expose the impurities, and the impurities are removed through acid leaching; the ultrasonic wave is vibration wave with strong energy and high frequency, and the ultrasonic wave assisted acid leaching can promote hydrochloric acid to enter amorphous boron powder along cracks under the assistance of the ultrasonic wave to react with impurities, so that impurities remained in a reaction blind area can be better removed.
In order to achieve the technical effects, the invention is realized by the following technical scheme: a method for removing magnesium and purifying amorphous boron powder by microwave heating and ultrasonic-assisted acid leaching is characterized by comprising the following steps:
step 1: taking amorphous crude boron powder produced by a magnesiothermic reduction method, placing the crude boron powder in a microwave oven, introducing argon gas, performing microwave heating, keeping the temperature for a period of time, closing the microwave power, and cooling to room temperature;
step 2: adding the amorphous boron powder sample obtained in Step1 into a hydrochloric acid solution, then placing the solution into ultrasonic cleaning equipment, carrying out ultrasonic auxiliary acid leaching treatment under a heating condition or at room temperature, and turning off the ultrasonic after the acid leaching treatment is finished;
step 3: filtering the boron powder suspension in Step2 while the suspension is hot, filtering the separated filter cake, washing the filter cake with deionized water until the pH value is close to neutral, and then putting the filter cake into a vacuum drying box for drying to obtain the amorphous boron powder product with low magnesium.
Further, the content of the amorphous crude boron powder magnesium impurities in Step1 is 3-8%.
Further, in the Step1, the microwave heating temperature is 400-1000 ℃; the heating rate is 200-400 ℃/min; the microwave treatment and heat preservation time is 1-5 h.
Further, in Step2, the liquid-solid ratio in the acid leaching process is 4-10: 1, the concentration of hydrochloric acid is 0.05-1 mol/L, the acid leaching temperature is 20-80 ℃, and the acid leaching time is 2-4 h.
The invention has the beneficial effects that:
according to the advantage that microwaves have the effect of selectively heating certain elements in a multiphase material, the amorphous boron powder has strong wave-absorbing capacity and can be heated quickly, while impurities have weak wave-absorbing capacity and can be heated slowly, and under the principle of thermal expansion and cold contraction, a boron shell wrapping the impurities generates cracks to expose the impurities, so that the impurities can be removed by acid leaching; the ultrasonic wave is a vibration wave with strong energy and high frequency, and the ultrasonic wave assisted acid leaching can promote hydrochloric acid to enter the amorphous boron powder along cracks under the assistance of the ultrasonic wave to react with impurities, so that impurities remaining in a reaction blind area are better removed; greatly improves the removal efficiency of magnesium impurities, has simple operation, stability, reliability, low cost and high added value, and is suitable for industrial production.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, the method for purifying amorphous boron powder by removing magnesium through microwave heating and ultrasonic-assisted acid leaching is characterized by comprising the following steps:
placing 5g of amorphous boron powder sample with the magnesium content of 5.67 percent and the purity of 87.86 percent in a ceramic crucible, heating to 800 ℃ by using a microwave oven, introducing argon gas in the heating process to protect the boron powder from being oxidized, preserving heat for 4 hours, and raising the temperature at the speed of 300 ℃/min. And (3) carrying out ultrasonic-assisted acid leaching on the heat-treated sample for 2 hours by using 0.5mol/L hydrochloric acid at the temperature of 80 ℃ in a water bath. And then the hot filtered material is dried in vacuum to obtain purified boron powder. Wherein the content of magnesium can be reduced to 1.06 percent by once removal, the removal rate is as high as 81.31 percent, and the purity of the obtained boron powder can reach 95.81 percent.
Example 2:
placing 5g of amorphous boron powder sample with the magnesium content of 6.87% and the purity of 85.86% in a ceramic crucible, heating to 800 ℃ by using a microwave oven, introducing argon gas in the heating process to protect the boron powder from being oxidized, and preserving heat for 2h at the heating rate of 300 ℃/min. And (3) carrying out ultrasonic-assisted acid leaching on the heat-treated sample for 2 hours by using 0.5mol/L hydrochloric acid at the temperature of 80 ℃ in a water bath. And then the hot filtered material is dried in vacuum to obtain purified boron powder. Wherein the content of magnesium can be reduced to 2.09% by one-time removal, the removal rate reaches 69.58%, and the purity of the obtained boron powder can reach 93.03%.
Example 3:
5g of amorphous boron powder sample with the magnesium content of 6.27% and the purity of 86.36% is placed in a ceramic crucible, heated to 400 ℃ by a microwave oven, argon is introduced in the heating process to protect the boron powder from being oxidized, the temperature is kept for 2h, and the heating rate is 300 ℃/min. And (3) carrying out ultrasonic-assisted acid leaching on the heat-treated sample for 2 hours by using 0.5mol/L hydrochloric acid at the temperature of 80 ℃ in a water bath. And then the hot filtered material is dried in vacuum to obtain purified boron powder. Wherein the content of magnesium can be reduced to 4.02% by once removing, the removal rate reaches 35.90%, and the purity of the obtained boron powder can reach 91.54%.
Example 4:
placing 5g of amorphous boron powder sample with the magnesium content of 7.57% and the purity of 85.34% in a ceramic crucible, heating to 1000 ℃ by using a microwave oven, introducing argon gas in the heating process to protect the boron powder from being oxidized, and keeping the temperature for 2h at the heating rate of 300 ℃/min. And (3) carrying out ultrasonic-assisted acid leaching on the heat-treated sample for 2 hours by using 0.5mol/L hydrochloric acid at the temperature of 80 ℃ in a water bath. And then the hot filtered material is dried in vacuum to obtain purified boron powder. Wherein the content of magnesium can be reduced to 3.26% by once removing, the removal rate reaches 56.93%, and the purity of the obtained boron powder can reach 92.88%.
Example 5:
placing a 5g amorphous boron powder sample with the magnesium content of 5.47% and the purity of 87.64% in a ceramic crucible, heating to 800 ℃ by using a microwave oven, introducing argon gas in the heating process to protect the boron powder from being oxidized, preserving heat for 1h, and raising the temperature at a rate of 300 ℃/min. And (3) carrying out ultrasonic-assisted acid leaching on the heat-treated sample for 2 hours by using 0.5mol/L hydrochloric acid at the temperature of 80 ℃ in a water bath. And then the hot filtered material is dried in vacuum to obtain purified boron powder. Wherein the content of magnesium can be reduced to 2.48% by once removing, the removal rate reaches 54.66%, and the purity of the obtained boron powder can reach 92.36%.
Example 6:
placing 5g of amorphous boron powder sample with the magnesium content of 6.82% and the purity of 86.18% in a ceramic crucible, heating to 800 ℃ by using a microwave oven, introducing argon gas in the heating process to protect the boron powder from being oxidized, and preserving heat for 5h at the heating rate of 300 ℃/min. And (3) carrying out ultrasonic-assisted acid leaching on the heat-treated sample for 2 hours by using 0.5mol/L hydrochloric acid at the temperature of 80 ℃ in a water bath. And then the hot filtered material is dried in vacuum to obtain purified boron powder. Wherein the content of magnesium can be reduced to 1.35% by once removing, the removal rate reaches 80.20%, and the purity of the obtained boron powder can reach 94.12%.
Example 7:
a5 g amorphous boron powder sample with 5.74 percent of magnesium and 85.86 percent of purity is subjected to ultrasonic assisted acid leaching for 2h by 0.5mol/L hydrochloric acid at 80 ℃ in a water bath. And then the hot filtered material is dried in vacuum to obtain purified boron powder. Through direct ultrasonic assisted acid leaching, the magnesium content can only be reduced to 5.12%, the removal rate is only 5.57%, and the purity of the obtained boron powder can reach 87.32%.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (4)
1. The method for purifying amorphous boron powder by removing magnesium through microwave heating and ultrasonic-assisted acid leaching is characterized by comprising the following steps of:
step 1: taking amorphous crude boron powder produced by a magnesiothermic reduction method, placing the crude boron powder in a microwave oven, introducing argon gas, carrying out microwave heating, keeping the temperature for a period of time, and then closing the microwave power and cooling to room temperature;
step 2: adding the amorphous boron powder sample obtained in Step1 into a hydrochloric acid solution, then placing the solution into ultrasonic cleaning equipment, carrying out ultrasonic auxiliary acid leaching treatment under a heating condition or at room temperature, and turning off the ultrasonic after the acid leaching treatment is finished;
step 3: filtering the boron powder suspension in Step2 while the suspension is hot, filtering the separated filter cake, washing the filter cake with deionized water until the pH value is close to neutrality, and then putting the filter cake into a vacuum drying oven for drying to obtain the amorphous boron powder product with low magnesium.
2. The method of claim 1 for purifying amorphous boron powder by removing magnesium by microwave heating and ultrasonic-assisted acid leaching, wherein: the content of the amorphous crude boron powder magnesium impurities in the Step1 is 3-8%.
3. The method for purifying amorphous boron powder by removing magnesium through microwave heating and ultrasonic-assisted acid leaching according to claim 1, is characterized in that: in the Step1, the microwave heating temperature is 400-1000 ℃; the heating rate is 200-400 ℃/min; the microwave treatment and heat preservation time is 1-5 h.
4. The method of claim 1 for purifying amorphous boron powder by removing magnesium by microwave heating and ultrasonic-assisted acid leaching, wherein: in Step2, the liquid-solid ratio in the acid leaching process is 4-10: 1, the concentration of hydrochloric acid is 0.05-1 mol/L, the acid leaching temperature is 20-80 ℃, and the acid leaching time is 2-4 h.
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Citations (4)
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|---|---|---|---|---|
| CN103864077A (en) * | 2014-02-17 | 2014-06-18 | 东北大学 | Production process of boron carbide powder for sapphire wafer grinding |
| EP3553199A1 (en) * | 2018-04-13 | 2019-10-16 | North University of China | A method of preparing magnesium-zinc-yttrium quasicrystal and boron carbide mixed reinforced magnesium-based composite material |
| CN111153409A (en) * | 2020-01-15 | 2020-05-15 | 中国科学院合肥物质科学研究院 | Method for purifying quartz sand by removing iron through microwave heating and ultrasonic-assisted acid leaching |
| CN112125316A (en) * | 2020-09-29 | 2020-12-25 | 昆明理工大学 | Purification method of low-purity amorphous boron powder |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864077A (en) * | 2014-02-17 | 2014-06-18 | 东北大学 | Production process of boron carbide powder for sapphire wafer grinding |
| EP3553199A1 (en) * | 2018-04-13 | 2019-10-16 | North University of China | A method of preparing magnesium-zinc-yttrium quasicrystal and boron carbide mixed reinforced magnesium-based composite material |
| CN111153409A (en) * | 2020-01-15 | 2020-05-15 | 中国科学院合肥物质科学研究院 | Method for purifying quartz sand by removing iron through microwave heating and ultrasonic-assisted acid leaching |
| CN112125316A (en) * | 2020-09-29 | 2020-12-25 | 昆明理工大学 | Purification method of low-purity amorphous boron powder |
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