CN102491359A - Method for purifying amorphous rough boron powder through pressurizing and leaching - Google Patents
Method for purifying amorphous rough boron powder through pressurizing and leaching Download PDFInfo
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- CN102491359A CN102491359A CN2011104310450A CN201110431045A CN102491359A CN 102491359 A CN102491359 A CN 102491359A CN 2011104310450 A CN2011104310450 A CN 2011104310450A CN 201110431045 A CN201110431045 A CN 201110431045A CN 102491359 A CN102491359 A CN 102491359A
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- boron powder
- amorphous
- purity
- pressurizing
- leaching
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002386 leaching Methods 0.000 title abstract 6
- 239000011777 magnesium Substances 0.000 claims abstract description 24
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 14
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 14
- 238000011946 reduction process Methods 0.000 claims description 13
- 238000013019 agitation Methods 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 abstract description 12
- 239000012535 impurity Substances 0.000 abstract description 11
- 238000000746 purification Methods 0.000 abstract description 8
- 238000009854 hydrometallurgy Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000012847 fine chemical Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000001535 kindling effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N trihydridoboron Substances B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for purifying amorphous rough boron powder through pressurizing and leaching. The method comprises the following steps of: adding diluted hydrochloric acid of a certain proportion to the amorphous rough boron powder, heating and pressurizing during mixing, and carrying out leaching reaction; and naturally cooling down to room temperature to obtain a mixture, filtering the mixture, cleaning filter residue by water, drying and sieving to obtain amorphous boron powder with purity of more than 97%, wherein the contents of impurities, such as Mg, O, Si, Fe and the like are respectively below 0.9%, 0.2%, 1.0% and 0.3%. According to the method for purifying the amorphous rough boron powder through pressurizing and leaching, disclosed by the invention, the purification of rough boron is carried out by a hydrometallurgy pressurizing leaching method, thus the purification process is simple, the cost is low, the additional value is high and the purity of boron power can be over 97%. The method for purifying the amorphous rough boron powder through pressurizing and leaching, disclosed by the invention, has the advantages of novel technique, innovativeness and high additional value, and can solve a problem that the purity of the amorphous boron powder prepared by the current thermal magnesium reduction method is too low.
Description
Technical field
The present invention relates to a kind of method of pressurizeing and leach purifying, being specifically related to a kind of is that raw material pressurizes and leaches the method for purifying with the amorphous thick boron powder that spreads the magnesium reduction process preparation certainly, belongs to boron fine chemical technology field.
Background technology
Amorphous boron powder is a kind of important boron fine chemical product, because the surfactivity of boron is higher, in metallurgical industry, is widely used as altered contents; In the solid-rocket compositepropellent, light metal fuel mainly contains Mg, Al, Be, B, and wherein B has the highest volume calorific value; And amorphous boron is because out-of-shape; Specific surface area reduces its kindling temperature greatly greatly, and simultaneously, amorphous boron powder still prepares TiB
2, LaB
6, B
4The important source material of boride such as C, BN.In recent years, high-purity amorphous boron powder has got into the Aeronautics and Astronautics field, and the SB95 amorphous boron powder that U.S. SB Boron company produces has been applied in the preparation of military fuel such as aircraft, nuclear power, rocket, ammunition, explosive substance and chemical weapons.
Document shows that less relatively to the preparation research of amorphous boron powder, some research institutions are still lower with the amorphous boron powder purity of relevant boronation worker's enterprise's preparation and production both at home and abroad.Nineteen ninety, people such as Y. C Yi on " J.Mater.Sci. ", publish thesis (1990, (25): 1159), utilize metal M g reduction B
2O
3The amorphous boron powder purity of preparing can only reach 90%.Ni Kun (patent No.: 02144932.5) etc. the people utilize burning synthetic method with boron oxide and magnesium powder with 1～2.5 ︰ 1 (weight) mixing after; To obtain purity be 90～97% boron powder that do not wait in reaction in the combustion synthesis reaction device, but most boron powder with purity about 90% is main.People such as beans will river publish thesis " the self-spreading metallurgical legal system is equipped with the boron powder " on " China YouSe Acta Metallurgica Sinica ", and (2004,14 (12): 2137-2143), adopting the boron powder purity of magnesium reduction process preparation is 92.43%.(application number: such as Gu Yunle 201010227137.2) with B
2O
3, Mg and KBH
4Be reaction raw materials, after mixing, under argon shield, under 700～850 ℃, cause self-propagating reaction, the gained reacting coarse product can obtain nano level boron powder after separating purification.
B
2H
6Borine cracking process, BX
3(X=Cl, F, Br) halogenation boron hydrogen reduction method and with fused salt electrolysis process can prepare the high purity boron powder, purity can reach more than 99.9%, prepares the complex technical process of high-purity halogen boride and hydrogenate; Investment is big; And environmental requirement is high, and corrosion on Equipment has also been proposed very high requirement, and production cost is high; Output is little, can't satisfy the demand of modern science development.
From spreading magnesium powder reduction method reduction B
2O
3Can obtain purity at 85～95% amorphous boron powders that do not wait; Mainly contain impurity such as Mg, Si, Fe, O; And the content of these impurity directly has influence on the physical and chemical performance of boron powder, and especially the combustionproperty index does not reach the standard of U.S. SB Boron 95 and is difficult to be applied.Therefore; Utilize the thick boron powder of magnesium reduction process preparation to purify; Remove most of impurity wherein; The boron Fine Chemical Industry is had crucial meaning, and thick boron powder is purified and not only can be made domestic amorphous boron powder be used for fields such as high-tech Aeronautics and Astronautics and military affairs, and can alleviate the pressure that the boron industry of present China faces.
For this reason, domestic researchist has carried out the method that some boron powder are purified.The petty official of Xi'an Inst. of Modern Chemistry can auspiciously wait the people on " fiery explosive journal ", to publish thesis (2007,30 (2): 8-12), with ethanol, zero(ppm) water amorphous boron powder is carried out purification processes, effectively remove the H on boron powder surface
3BO
3Impurity has improved the surface property of boron powder, helps the combustionproperty of boron powder.(application number: 201010130202.x) wait the people is raw material with the amorphous thick boron powder of magnesium reduction process production to Wu Jijun, in thick boron powder, allocates B into
2O
3, can obtain 95～97% boron powder after purifying at a certain temperature.Yet, at present for the purification research work of the thick boron powder of magnesium reduction process production carry out less.
Summary of the invention
In order to realize reaching more than 97% from 85～92% thick boron powder purification, the present invention proposes the method that the amorphous thick boron powder of purifying is leached in a kind of hydrometallurgy pressurization, and this method is less investment not only, and cost is low, and added value of product is high.
The present invention passes through following technical proposal and realizes: a kind of amorphous thick boron powder pressurization is leached the method for purifying, following each step of process:
(1) takes from that to spread purity that magnesium reduction process prepares be 85～92% amorphous thick boron powder;
(2) compound concentration is the Hydrogen chloride of 0.05～0.5mol/L;
(3) in the amorphous thick boron powder of step (1), be the Hydrogen chloride that 4～6 ︰ 1 add step (2), under agitation be warming up to 120～220 ℃ by liquid-solid mass ratio, be forced into 1.0～2.0MPa again after, leach reaction 2～3h;
(4) treat that step (2) reaction finishes after, naturally cool to room temperature, mixture is filtered; After the filter residue water cleans 3～5 times; Place 100～150 ℃, vacuum tightness to be no more than under the 20Pa and to dry 1～3h, sieve again, promptly obtain purity and reach the amorphous boron powder more than 97%.Wherein impurity Mg, O, Si, Fe equal size respectively 0.9%, 0.2%, 1.0%, below 0.3%.
Effect that the present invention possesses and advantage:
The method that method provided by the invention utilizes the hydrometallurgy pressurization to leach is carried out the purification of thick boron, and purification process is simple, with low cost, added value is high, and boron powder purity can reach more than 97%.This invention technology is novel, has novelty, and added value is high, can solve the low excessively problem of amorphous boron powder purity of current magnesium reduction process preparation.
Embodiment
To combine embodiment further to illustrate content of the present invention below, but these instances do not limit protection scope of the present invention.
Embodiment 1
(1) takes from that to spread purity that magnesium reduction process prepares be 90% amorphous thick boron powder;
(2) compound concentration is the Hydrogen chloride of 0.2mol/L;
(3) in the amorphous thick boron powder of step (1), be the Hydrogen chloride that 5 ︰ 1 add step (2), under agitation be warming up to 220 ℃ by liquid-solid mass ratio, be forced into 1.5MPa again after, leach reaction 2.5h;
(4) treat that step (2) reaction finishes after, naturally cool to room temperature, mixture is filtered, after the filter residue water cleans 4 times, place under 120 ℃, vacuum tightness 20Pa and dry 2h, sieve again, promptly obtain purity and reach 97.7% amorphous boron powder.Wherein impurity Mg, O, Si, Fe equal size are respectively 0.7%, 0.13%, 0.8%, 0.25%.
Embodiment 2
(1) takes from that to spread purity that magnesium reduction process prepares be 90% amorphous thick boron powder;
(2) compound concentration is the Hydrogen chloride of 0.05mol/L;
(3) in the amorphous thick boron powder of step (1), be the Hydrogen chloride that 4 ︰ 1 add step (2), under agitation be warming up to 120 ℃ by liquid-solid mass ratio, be forced into 1.0MPa again after, leach reaction 3h;
(4) treat that step (2) reaction finishes after, naturally cool to room temperature, mixture is filtered, after the filter residue water cleans 3 times, place under 100 ℃, vacuum tightness 18Pa and dry 3h, sieve again, promptly obtain purity and reach 97.4% amorphous boron powder.Wherein impurity Mg, O, Si, Fe equal size are respectively 0.9%, 0.2%, 1.0%, 0.25%.
Embodiment 3
(1) takes from that to spread purity that magnesium reduction process prepares be 90% amorphous thick boron powder;
(2) compound concentration is the Hydrogen chloride of 0.5mol/L;
(3) in the amorphous thick boron powder of step (1), be the Hydrogen chloride that 6 ︰ 1 add step (2), under agitation be warming up to 180 ℃ by liquid-solid mass ratio, be forced into 2.0MPa again after, leach reaction 2h;
(4) treat that step (2) reaction finishes after, naturally cool to room temperature, mixture is filtered; After filter residue cleans 5 times with zero(ppm) water; Place under 150 ℃, vacuum tightness 10Pa and dry 1h, sieve again, promptly obtain purity and reach the amorphous boron powder more than 98.1%.Wherein impurity Mg, O, Si, Fe equal size are respectively 0.64%, 0.13%, 0.78%, 0.25%.
Embodiment 4
(1) takes from that to spread purity that magnesium reduction process prepares be 85% amorphous thick boron powder;
(2) compound concentration is the Hydrogen chloride of 0.1mol/L;
(3) in the amorphous thick boron powder of step (1), be the Hydrogen chloride that 5 ︰ 1 add step (2), under agitation be warming up to 150 ℃ by liquid-solid mass ratio, be forced into 1.6MPa again after, leach reaction 2.5h;
(4) treat that step (2) reaction finishes after, naturally cool to room temperature, mixture is filtered, after the filter residue water cleans 4 times, place under 150 ℃, vacuum tightness 15Pa and dry 2h, sieve again, promptly obtain purity and reach the amorphous boron powder more than 97.5%.Wherein impurity Mg, O, Si, Fe equal size are respectively 0.83%, 0.16%, 0.85%, 0.25%.
Embodiment 5
(1) takes from that to spread purity that magnesium reduction process prepares be 92% amorphous thick boron powder;
(2) compound concentration is the Hydrogen chloride of 0.08mol/L;
(3) in the amorphous thick boron powder of step (1), be the Hydrogen chloride that 4 ︰ 1 add step (2), under agitation be warming up to 120 ℃ by liquid-solid mass ratio, be forced into 1.2MPa again after, leach reaction 2h;
(4) treat that step (2) reaction finishes after, naturally cool to room temperature, mixture is filtered, after the filter residue water cleans 3 times, place under 120 ℃, vacuum tightness 20Pa and dry 2h, sieve again, promptly obtain purity and reach the amorphous boron powder more than 97.2%.Wherein impurity Mg, O, Si, Fe equal size are respectively 0.84%, 0.16%, 0.92%, 0.27%.
Claims (1)
1. the method for purifying is leached in an amorphous thick boron powder pressurization, it is characterized in that through following each step:
(1) takes from that to spread purity that magnesium reduction process prepares be 85～92% amorphous thick boron powder;
(2) compound concentration is the Hydrogen chloride of 0.05～0.5mol/L;
(3) in the amorphous thick boron powder of step (1), be the Hydrogen chloride that 4～6 ︰ 1 add step (2), under agitation be warming up to 120～220 ℃ by liquid-solid mass ratio, be forced into 1.0～2.0MPa again after, leach reaction 2～3h;
(4) treat that step (2) reaction finishes after, naturally cool to room temperature, mixture is filtered; After the filter residue water cleans 3～5 times; Place 100～150 ℃, vacuum tightness to be no more than under the 20Pa and to dry 1～3h, sieve again, promptly obtain purity and reach the amorphous boron powder more than 97%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179444A (en) * | 2018-10-11 | 2019-01-11 | 武汉科技大学 | A kind of preparation method of amorphous boron powder |
| CN111423882A (en) * | 2019-11-11 | 2020-07-17 | 殷柳 | Method for removing and preventing oxidation of boron powder surface oxide |
| CN112125316A (en) * | 2020-09-29 | 2020-12-25 | 昆明理工大学 | Purification method of low-purity amorphous boron powder |
| CN112479220A (en) * | 2020-12-02 | 2021-03-12 | 昆明理工大学 | Wet purification method of amorphous crude boron powder |
| CN114933311A (en) * | 2022-06-02 | 2022-08-23 | 安阳工学院 | Method for refining hexaboride powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780960A (en) * | 2010-03-23 | 2010-07-21 | 昆明理工大学 | Method for purifying crude boron powder |
| CN102211777A (en) * | 2011-03-05 | 2011-10-12 | 兰州理工大学 | Method for preparing pure boron |
-
2011
- 2011-12-21 CN CN2011104310450A patent/CN102491359A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101780960A (en) * | 2010-03-23 | 2010-07-21 | 昆明理工大学 | Method for purifying crude boron powder |
| CN102211777A (en) * | 2011-03-05 | 2011-10-12 | 兰州理工大学 | Method for preparing pure boron |
Non-Patent Citations (1)
| Title |
|---|
| KEQIANG XIE ETAL: "Removal of iron from metallurgical grade silicon with pressure leaching", 《ADVANCED MATERIAL SCIENCE AND TECHNOLOGY》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179444A (en) * | 2018-10-11 | 2019-01-11 | 武汉科技大学 | A kind of preparation method of amorphous boron powder |
| CN111423882A (en) * | 2019-11-11 | 2020-07-17 | 殷柳 | Method for removing and preventing oxidation of boron powder surface oxide |
| CN112125316A (en) * | 2020-09-29 | 2020-12-25 | 昆明理工大学 | Purification method of low-purity amorphous boron powder |
| CN112479220A (en) * | 2020-12-02 | 2021-03-12 | 昆明理工大学 | Wet purification method of amorphous crude boron powder |
| CN114933311A (en) * | 2022-06-02 | 2022-08-23 | 安阳工学院 | Method for refining hexaboride powder |
| CN114933311B (en) * | 2022-06-02 | 2023-08-25 | 安阳工学院 | Method for refining hexaboride powder |
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Application publication date: 20120613 |