CN102764894A - Method for preparing high-purity vanadium powder - Google Patents
Method for preparing high-purity vanadium powder Download PDFInfo
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- CN102764894A CN102764894A CN201210267471XA CN201210267471A CN102764894A CN 102764894 A CN102764894 A CN 102764894A CN 201210267471X A CN201210267471X A CN 201210267471XA CN 201210267471 A CN201210267471 A CN 201210267471A CN 102764894 A CN102764894 A CN 102764894A
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title abstract description 27
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 48
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 43
- -1 vanadium hydride Chemical compound 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 28
- 239000001257 hydrogen Substances 0.000 claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000007872 degassing Methods 0.000 claims abstract description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000009837 dry grinding Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000012856 packing Methods 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 19
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 9
- 238000003801 milling Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000003795 desorption Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 17
- 239000012535 impurity Substances 0.000 abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000004663 powder metallurgy Methods 0.000 abstract 1
- 229920006395 saturated elastomer Polymers 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000000428 dust Substances 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010297 mechanical methods and process Methods 0.000 description 2
- 229910052987 metal hydride Inorganic materials 0.000 description 2
- 150000004681 metal hydrides Chemical class 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a method for preparing high-purity vanadium powder. The method aims to solve the problem that contents of impurities, particularly contents of O and N, in vanadium powder are high, and requirements of powder metallurgy on purity of raw materials and the like are met. The method includes activating surfaces of a vanadium block by saturated NaO alkali liquor, distilled water and ethanol or acetone sequentially, feeding the vanadium block in a closed container, placing the closed container with the vanadium block in a hydrogenation hydrogen absorbing system, drying and degassing the vanadium block and hydrogenating the degassed vanadium block at the temperature ranging from 200 DEG C to 500 DEG C to obtain high-purity vanadium hydride grains; placing the high-purity vanadium hydride grains in a planetary ball mill for dry grinding; and feeding vanadium hydride powder obtained in the previous step in the closed container for dehydrogenization at a high temperature. The granularity of the submicron vanadium powder prepared by the method can be smaller than 30 micrometers, oxygen content can be controlled to be within 600ppm, nitrogen content is lower than 250ppm, and the problem that the high-purity vanadium powder is prepared difficultly is effectively solved.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity vanadium powder.
Background technology
Along with the development and the progress of PM technique, the application of its main raw material(s) metal dust constantly to be expanded, the market demand sharply increases, and demonstrates to high-purity, ultra-fine direction Development Trend.The metal powder preparation method of comparative maturity mainly contains Mechanical Method and physics method at present, and two kinds of methods all have certain shortcoming and defect.
Mechanical Method is a kind of processing method that bulk metal is broken into required particle diameter powder by means of mechanical force.Difference according to mechanical force is divided into mechanical shock formula comminuting method, airflow milling comminuting method, ball-milling method and ultrasonic-wave crushing method etc. with it.The method of generally using at present still is ball-milling method and the broken method of air-flow abrasive dust, and its advantage is that technology is simple, output is big, can prepare the refractory metal that some conventional methods are difficult to obtain and the superfine nano powder of alloy.The physics method generally be through high temperature, high pressure with the fusing of reguline metal material, and be broken into tiny drop, and condensation and obtain metal dust in gatherer, chemical change does not take place in this process.The powder sphericity that this method makes is high, powder size is controlled, oxygen content is relatively low., the prepared metal dust of above-mentioned two kinds of methods influences the shortcoming of properties of product but all existing impurity in the easy introducing environment.
The V powder activity is high, very easily adsorb impurity element such as O in the environment, N and form oxide on the surface, and the thinner specific area of powder is big more, is not easy to control impurity contents such as O, N more.Therefore, high-purity, ultra-fine vanadium powder preparation is more difficult.The hydrogenation dehydriding utilizes the easy hydrogen of inhaling of feed metal to increase crisp characteristic, makes metal and hydrogen generation hydrogenation generate metal hydride at a certain temperature, and is by mechanical means that the gained metal hydride is broken then, thereby obtains metal dust.Hydrogen can also and purify atmosphere as protection when playing fragmentation, the control vanadium powder contacts with impurity such as O, N, avoids the formation of oxide, thereby makes high-purity vanadium powder.
Summary of the invention
The objective of the invention is to solve vanadium powder impurity content particularly O, problem that N content is high; Satisfy the demand of PM technique at aspects such as material purities; A kind of preparation method of high-purity vanadium powder is provided, and the granularity of the submicron order vanadium powder that makes through this method can be less than 30um, and oxygen content can be controlled in the 600ppm; Nitrogen content is lower than 250ppm, efficiently solves the problem that high-purity vanadium powder is difficult to prepare.
For achieving the above object, the technical scheme that the present invention adopts is: a kind of preparation method of high-purity vanadium powder comprises the following steps:
A, vanadium piece surface active: with saturated NaOH alkali lye, distilled water and ethanol the vanadium piece is carried out surface active in order, or replace ethanol with acetone, and then with its closed container of packing into;
B, the hydrogenation of vanadium piece: hydrogen system is inhaled in the hydrogenation of packing into of the above-mentioned closed container that is placed with the vanadium piece, and dry degasification is carried out hydrogenation with the vanadium piece after the degasification and is made high-purity Vanadium hydride particle under 200 ℃～500 ℃;
C, Vanadium hydride's refinement: high-purity Vanadium hydride particle of above-mentioned prepared in reaction inserted carry out dry grinding on the planetary ball mill;
D, the dehydrogenation of hydrogenation vanadium powder: the above-mentioned Vanadium hydride's powder that the makes closed container of packing into is carried out dehydrogenation at high temperature.
In technique scheme, among the said step b, said dry degasification is to be superior to 1 * 10 in vacuum
-3Pa, temperature are to carry out under 500 ℃～800 ℃ the condition.
In technique scheme, among the said step b, the purity of the High Purity Hydrogen that adopts during said hydrogenation is greater than 99.999%.
In technique scheme, among the said step c, the ratio of grinding media to material during said dry grinding is 4～10:1, and the batch can rotating speed is 200r/min～320r/min, and milling time is 4h～8h.
In technique scheme, in the said steps d, said desorption temperature is 500 ℃～800 ℃, and the time is 1h～10h.
Can find out that from each item technical characterictic of the invention described above its advantage is: the present invention carries out hydrogenation-ball milling-dehydrogenation with the vanadium piece of commercialization, under the effect of protective atmosphere, prepares high-purity, submicron order vanadium powder.This preparation method can effectively control the impurity content in the vanadium, and the vanadium powder oxygen content of preparation is lower than 600ppm, and nitrogen content is lower than 250ppm.The present invention carries out refinement with commercial vanadium piece; The all operations process is all carried out under protective atmosphere; Guaranteed that powder material do not introduce new impurity in thinning process, and got rid of the influence of ambiance as much as possible, finally can prepare high-purity submicron order vanadium powder.This preparation method's technological parameter is easy to control, and is easy to operate, is fit to suitability for industrialized production.
The specific embodiment
Through embodiment the present invention is done further explanation below.
Embodiment 1
A kind of preparation method of high-purity vanadium powder comprises the following steps:
A, vanadium piece surface active: with saturated NaOH alkali lye, distilled water and ethanol the vanadium piece is carried out surface active in order, or replace ethanol with acetone, and then with its closed container of packing into;
B, the hydrogenation of vanadium piece: hydrogen system is inhaled in the hydrogenation of packing into of the above-mentioned closed container that is placed with the vanadium piece, be superior to 1 * 10 in vacuum
-3Pa, temperature are dry degasification under 500 ℃ the condition; Because the suction hydrogen temperature of vanadium is higher; Vanadium piece after the degasification is carried out hydrogenation make high-purity Vanadium hydride particle under 200 ℃, for reducing the impurity such as O, N in the high-purity hydrogen, the purity of the High Purity Hydrogen that adopts during hydrogenation is greater than 99.999%;
C, Vanadium hydride's refinement: high-purity Vanadium hydride particle of above-mentioned prepared in reaction inserted carry out dry grinding on the planetary ball mill, the ratio of grinding media to material during dry grinding is 4:1, and the batch can rotating speed is 200r/min, and milling time is 4h;
D, the dehydrogenation of hydrogenation vanadium powder: the above-mentioned Vanadium hydride's powder that the makes closed container of packing into is carried out dehydrogenation at high temperature, and said desorption temperature is 500 ℃, and the time is 1h.
Making oxygen content through above-mentioned steps is 600ppm, and particle mean size is the hydrogenation vanadium powder of 30mm.
Embodiment 2
A kind of preparation method of high-purity vanadium powder comprises the following steps:
A, vanadium piece surface active: with saturated NaOH alkali lye, distilled water and ethanol the vanadium piece is carried out surface active in order, or replace ethanol with acetone, and then with its closed container of packing into;
B, the hydrogenation of vanadium piece: hydrogen system is inhaled in the hydrogenation of packing into of the above-mentioned closed container that is placed with the vanadium piece, be superior to 1 * 10 in vacuum
-3Pa, temperature are dry degasification under 600 ℃ the condition; Because the suction hydrogen temperature of vanadium is higher; Vanadium piece after the degasification is carried out hydrogenation make high-purity Vanadium hydride particle under 300 ℃, for reducing the impurity such as O, N in the high-purity hydrogen, the purity of the High Purity Hydrogen that adopts during hydrogenation is greater than 99.999%;
C, Vanadium hydride's refinement: high-purity Vanadium hydride particle of above-mentioned prepared in reaction inserted carry out dry grinding on the planetary ball mill, the ratio of grinding media to material during dry grinding is 6:1, and the batch can rotating speed is 220r/min, and milling time is 5h;
D, the dehydrogenation of hydrogenation vanadium powder: the above-mentioned Vanadium hydride's powder that the makes closed container of packing into is carried out dehydrogenation at high temperature, and said desorption temperature is 600 ℃, and the time is 3h.
Making oxygen content through above-mentioned steps is 600ppm, and particle mean size is the hydrogenation vanadium powder of 29mm.
Embodiment 3
A kind of preparation method of high-purity vanadium powder comprises the following steps:
A, vanadium piece surface active: with saturated NaOH alkali lye, distilled water and ethanol the vanadium piece is carried out surface active in order, or replace ethanol with acetone, and then with its closed container of packing into;
B, the hydrogenation of vanadium piece: hydrogen system is inhaled in the hydrogenation of packing into of the above-mentioned closed container that is placed with the vanadium piece, be superior to 1 * 10 in vacuum
-3Pa, temperature are dry degasification under 650 ℃ the condition; Because the suction hydrogen temperature of vanadium is higher; Vanadium piece after the degasification is carried out hydrogenation make high-purity Vanadium hydride particle under 350 ℃, for reducing the impurity such as O, N in the high-purity hydrogen, the purity of the High Purity Hydrogen that adopts during hydrogenation is greater than 99.999%;
C, Vanadium hydride's refinement: high-purity Vanadium hydride particle of above-mentioned prepared in reaction inserted carry out dry grinding on the planetary ball mill, the ratio of grinding media to material during dry grinding is 7:1, and the batch can rotating speed is 250r/min, and milling time is 6h;
D, the dehydrogenation of hydrogenation vanadium powder: the above-mentioned Vanadium hydride's powder that the makes closed container of packing into is carried out dehydrogenation at high temperature, and said desorption temperature is 700 ℃, and the time is 6h.
Making oxygen content through above-mentioned steps is 600ppm, and particle mean size is the hydrogenation vanadium powder of 28mm.
Embodiment 4
A kind of preparation method of high-purity vanadium powder comprises the following steps:
A, vanadium piece surface active: with saturated NaOH alkali lye, distilled water and ethanol the vanadium piece is carried out surface active in order, or replace ethanol with acetone, and then with its closed container of packing into;
B, the hydrogenation of vanadium piece: hydrogen system is inhaled in the hydrogenation of packing into of the above-mentioned closed container that is placed with the vanadium piece, be superior to 1 * 10 in vacuum
-3Pa, temperature are dry degasification under 700 ℃ the condition; Because the suction hydrogen temperature of vanadium is higher; Vanadium piece after the degasification is carried out hydrogenation make high-purity Vanadium hydride particle under 450 ℃, for reducing the impurity such as O, N in the high-purity hydrogen, the purity of the High Purity Hydrogen that adopts during hydrogenation is greater than 99.999%;
C, Vanadium hydride's refinement: high-purity Vanadium hydride particle of above-mentioned prepared in reaction inserted carry out dry grinding on the planetary ball mill, the ratio of grinding media to material during dry grinding is 8:1, and the batch can rotating speed is 300r/min, and milling time is 7h;
D, the dehydrogenation of hydrogenation vanadium powder: the above-mentioned Vanadium hydride's powder that the makes closed container of packing into is carried out dehydrogenation at high temperature, and said desorption temperature is 700 ℃, and the time is 8h.
Making oxygen content through above-mentioned steps is 600ppm, and particle mean size is the hydrogenation vanadium powder of 26mm.
Embodiment 5
A kind of preparation method of high-purity vanadium powder comprises the following steps:
A, vanadium piece surface active: with saturated NaOH alkali lye, distilled water and ethanol the vanadium piece is carried out surface active in order, or replace ethanol with acetone, and then with its closed container of packing into;
B, the hydrogenation of vanadium piece: hydrogen system is inhaled in the hydrogenation of packing into of the above-mentioned closed container that is placed with the vanadium piece, be superior to 1 * 10 in vacuum
-3Pa, temperature are dry degasification under 800 ℃ the condition; Because the suction hydrogen temperature of vanadium is higher; Vanadium piece after the degasification is carried out hydrogenation make high-purity Vanadium hydride particle under 500 ℃, for reducing the impurity such as O, N in the high-purity hydrogen, the purity of the High Purity Hydrogen that adopts during hydrogenation is greater than 99.999%;
C, Vanadium hydride's refinement: high-purity Vanadium hydride particle of above-mentioned prepared in reaction inserted carry out dry grinding on the planetary ball mill, the ratio of grinding media to material during dry grinding is 10:1, and the batch can rotating speed is 320r/min, and milling time is 8h;
D, the dehydrogenation of hydrogenation vanadium powder: the above-mentioned Vanadium hydride's powder that the makes closed container of packing into is carried out dehydrogenation at high temperature, and said desorption temperature is 800 ℃, and the time is 10h.
Making oxygen content through above-mentioned steps is 600ppm, and particle mean size is the hydrogenation vanadium powder of 25mm.
Disclosed all characteristics in this specification except mutually exclusive characteristic, all can make up by any way.
Disclosed arbitrary characteristic in this specification (comprising any accessory claim, summary) is only if special narration all can be replaced by other equivalences or the alternative features with similar purpose.That is, only if special narration, each characteristic is an example in a series of equivalences or the similar characteristics.
Claims (5)
1. the preparation method of a high-purity vanadium powder is characterized in that comprising the following steps:
A, vanadium piece surface active: with saturated NaOH alkali lye, distilled water and ethanol the vanadium piece is carried out surface active in order, or replace ethanol with acetone, and then with its closed container of packing into;
B, the hydrogenation of vanadium piece: hydrogen system is inhaled in the hydrogenation of packing into of the above-mentioned closed container that is placed with the vanadium piece, and dry degasification is carried out hydrogenation with the vanadium piece after the degasification and is made high-purity Vanadium hydride particle under 200 ℃～500 ℃;
C, Vanadium hydride's refinement: high-purity Vanadium hydride particle of above-mentioned prepared in reaction inserted carry out dry grinding on the planetary ball mill;
D, the dehydrogenation of hydrogenation vanadium powder: the above-mentioned Vanadium hydride's powder that the makes closed container of packing into is carried out dehydrogenation at high temperature.
2. the preparation method of a kind of high-purity vanadium powder according to claim 1 is characterized in that among the said step b, and said dry degasification is to be superior to 1 * 10 in vacuum
-3Pa, temperature are to carry out under 500 ℃～800 ℃ the condition.
3. the preparation method of a kind of high-purity vanadium powder according to claim 1 is characterized in that among the said step b, and the purity of the High Purity Hydrogen that adopts during said hydrogenation is greater than 99.999%.
4. the preparation method of a kind of high-purity vanadium powder according to claim 1 is characterized in that among the said step c, and the ratio of grinding media to material during said dry grinding is 4～10:1, and the batch can rotating speed is 200r/min～320r/min, and milling time is 4h～8h.
5. the preparation method of a kind of high-purity vanadium powder according to claim 1 is characterized in that in the said steps d, and said desorption temperature is 500 ℃～800 ℃, and the time is 1h～10h.
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| CN201210267471.XA CN102764894B (en) | 2012-07-30 | 2012-07-30 | Method for preparing high-purity vanadium powder |
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| CN201210267471.XA CN102764894B (en) | 2012-07-30 | 2012-07-30 | Method for preparing high-purity vanadium powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018129868A1 (en) | 2017-01-11 | 2018-07-19 | 中国科学院过程工程研究所 | System for extracting vanadium from leaching solution containing vanadium chromium silicon and for preparing vanadium pentoxide and processing method therefor |
| CN109277429A (en) * | 2018-09-03 | 2019-01-29 | 重庆材料研究院有限公司 | The preparation method of high purity vanadium silk |
| CN110340369A (en) * | 2019-08-08 | 2019-10-18 | 南昌大学 | A kind of Ultra Low Cost spherical shape vanadium powder preparation method |
| CN111266597A (en) * | 2020-03-23 | 2020-06-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of metal vanadium powder |
| CN111957984A (en) * | 2020-08-25 | 2020-11-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of metal vanadium powder |
| CN113732297A (en) * | 2021-09-04 | 2021-12-03 | 湖南众鑫新材料科技股份有限公司 | High-purity vanadium purification process |
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| CN102430759A (en) * | 2011-12-03 | 2012-05-02 | 常州六九新材料科技有限公司 | Preparation method of high-purity titanium powder for large-scale integrated circuit |
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| EP1174385A2 (en) * | 2000-05-31 | 2002-01-23 | Honda Giken Kogyo Kabushiki Kaisha | Process for producing hydrogen absorbing alloy powder, hydrogen absorbing alloy powder, and hydrogen-storing tank for mounting in vehicle |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018129868A1 (en) | 2017-01-11 | 2018-07-19 | 中国科学院过程工程研究所 | System for extracting vanadium from leaching solution containing vanadium chromium silicon and for preparing vanadium pentoxide and processing method therefor |
| CN109277429A (en) * | 2018-09-03 | 2019-01-29 | 重庆材料研究院有限公司 | The preparation method of high purity vanadium silk |
| CN109277429B (en) * | 2018-09-03 | 2020-01-10 | 重庆材料研究院有限公司 | Preparation method of high-purity vanadium wire |
| CN110340369A (en) * | 2019-08-08 | 2019-10-18 | 南昌大学 | A kind of Ultra Low Cost spherical shape vanadium powder preparation method |
| CN111266597A (en) * | 2020-03-23 | 2020-06-12 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of metal vanadium powder |
| CN111957984A (en) * | 2020-08-25 | 2020-11-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of metal vanadium powder |
| CN113732297A (en) * | 2021-09-04 | 2021-12-03 | 湖南众鑫新材料科技股份有限公司 | High-purity vanadium purification process |
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| CN102764894B (en) | 2014-10-29 |
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