CN104722767A - Tungsten powder preparation method - Google Patents
Tungsten powder preparation method Download PDFInfo
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- CN104722767A CN104722767A CN201510177510.0A CN201510177510A CN104722767A CN 104722767 A CN104722767 A CN 104722767A CN 201510177510 A CN201510177510 A CN 201510177510A CN 104722767 A CN104722767 A CN 104722767A
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Abstract
The invention relates to tungsten powder preparation method. The tungsten powder preparation method includes: dissolving Na2WO4.5H2O into distilled water and adding CTAB (cetyltrimethyl ammonium bromide); then dropwise adding a hydrochloric acid solution and magnetically stirring and mixing evenly; placing a mixed solution in a high-pressure reactor for heating reaction; cooling to indoor temperature prior to filtering to obtain sediment; washing the sediment and drying the same; placing the dried sediment into a muffle furnace for firing to obtain tungsten trioxide powder; placing the tungsten trioxide powder in a plasma reaction chamber to form a high-temperature plasma through an ionized inert gas in the reaction chamber and allowing the tungsten trioxide powder to be heated by the high-temperature plasma to be reduced to tungsten powder under the reduction atmosphere. Tungsten oxide is prepared by adopting sodium tungstate, the CTAB and hydrochloric acid, the tungsten powder is prepared through a plasma arc method, large temperature difference exists between the tungsten powder and a cooling medium, nucleation is promoted while growth of crystal nucleus is effectively restrained, and the prepared tungsten powder can reach nanoscale; meanwhile, the method is simple in process, preparation time is short, and mass production is easy to realize.
Description
Technical field
The present invention relates to the preparation method of tungsten powder.
Background technology
In the Extraction metallurgy of tungsten, the importance that metal tungsten powder is produced is apparent, and the performance of tungsten powder affects the performance of tungsten product to a great extent.The quality of tungsten powder is the guarantee to tungsten and tungsten alloy superior function, tungsten powder industry faces great challenge, it must meet the market requirement more and more high to it, the production of tungsten powder is not only had to the requirement of chemical purity aspect, and having the requirement of physical property and processing performance aspect, the technology of preparing especially meeting the ultrafine tungsten powder of some specific uses need to solve.
The method of producing tungsten powder is a lot, adopts tungstic acid to be that to prepare tungsten powder by hydrogen reduction reaction be wherein a kind of to raw material; Traditional Process of Hydrogen Reduction flow process is tungstic acid ammonium tungstate roasting obtained, then obtains tungsten powder through two stage of reduction, uses conventional method to prepare tungsten powder and there is following problems: 1, reduction temperature is low, and the reaction time is long, time-consuming; 2, adopt tubulose reduction furnace, equipment is complicated, not energy-conservation; 3, product purity is low, more difficult continuous prodution.
Summary of the invention
For above-mentioned technical problem, the invention provides the tungsten powder preparation method that a kind of preparation time is short, easily accomplish scale production.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of preparation method of tungsten powder, and it comprises the following steps:
(1) by Na
2wO
45H
2o is dissolved in distilled water, adds CTAB;
(2) drip hydrochloric acid solution again, magnetic agitation mixes;
(3) mixed solution is placed in autoclave and adds thermal response;
(4) filter after being cooled to room temperature again, be precipitated thing; Washing precipitate, and dry;
(5) sediment of oven dry is put into Muffle furnace calcination, obtain tungstic acid powder;
(6) tungstic acid powder is placed in plasma reaction chamber, in this reative cell, form high-temperature plasma by ionization inert gas, tungstic acid powder is reduced into tungsten powder after being heated by high-temperature plasma under reducing atmosphere.
Alternatively, after long-time magnetic agitation is even, centrifugal sedimentation is carried out to solution, then washing precipitate, and dry, then carry out step (5) and (6).
As preferably, described Na
2wO
45H
2the mass ratio of O, CTAB, hydrochloric acid is 1:(0.002-0.01): (0.1-0.5).
As preferably, the heating-up temperature of reactor is 80 DEG C--120 DEG C, the reaction time is 20h-24h.
As preferably, filter in reactor reaction the sediment obtained afterwards and can adopt distilled water and absolute ethyl alcohol cyclic washing; The sediment obtained by sedimentation is seen and is adopted distilled water and acetone cyclic washing.
As preferably, during oven dry, adopt 50 DEG C--dry 8h-10h for 70 DEG C.
As preferably, in Muffle furnace, adopt 400 DEG C--the temperature calcination 2h-4h of 500 DEG C.
As preferably, plasma reaction is indoor is plasma working gas with argon gas, and hydrogen is reducing atmosphere; With tungstic acid powder for positive pole, plasma gun is negative pole, the electric arc ionization inert gas produced between a positive electrode and a negative electrode after energising, thus formation high-temperature plasma heats tungstic acid powder.
As preferably, operating voltage during energising is 60v--90v, and operating current is 400A--700A.
As preferably, be 1000 DEG C to the heating-up temperature of tungstic acid powder--1800 DEG C.
As can be known from the above technical solutions, after this method adopts sodium tungstate, CTAB and hydrochloric acid to prepare tungsten oxide, by plasma-arc legal system for tungsten powder, owing to there being very large temperature difference between tungsten powder and cooling medium, while impelling forming core, also effectively inhibit the growth of nucleus, obtained tungsten powder can reach nanoscale; Meanwhile, this method technique is comparatively simple, and preparation time is shorter, easily accomplish scale production.
Detailed description of the invention
Introduce the preparation method of tungsten powder in detail below in conjunction with embodiment, it carries out according to the following steps:
First, by Na
2wO
45H
2o is dissolved in distilled water, and add CTAB (softex kw), slowly drip hydrochloric acid solution, room temperature stirs 1h--2h under magnetic stirring, then by reacted solution centrifugal sedimentation, with distilled water, acetone cyclic washing; Also after magnetic agitation 30min, solution can be placed in autoclave, reactor is put as 80 DEG C--react 20h-24h in the baking oven of 120 DEG C; Be cooled to room temperature after reaction, filter and be precipitated thing, and with distilled water, absolute ethyl alcohol cyclic washing sediment; Wherein, Na
2wO
45H
2the mass ratio of O, CTAB, hydrochloric acid thinks 1:(0.002-0.01): (0.1-0.5) is advisable.
Then, the sediment after washing is put into 50 DEG C--70 DEG C of dry 8h-10h of baking oven; The sediment of oven dry is put into 400 DEG C--the Muffle furnace calcination 2h-4h of 500 DEG C, obtained nano tungsten trioxide superfine powder.
Then, tungstic acid powder is placed in plasma reaction chamber, plasma reaction is indoor is plasma working gas with argon gas, and hydrogen is reducing atmosphere, with tungstic acid powder for positive pole, plasma gun is negative pole, operating voltage is 60v--90v, operating current is 400A--700A, the electric arc ionization inert gas produced between a positive electrode and a negative electrode, thus formation high-temperature plasma heats tungstic acid powder, heating-up temperature maintains 1000 DEG C--between 1800 DEG C, tungstic acid powder is steam by high-temperature plasma heating and gasifying, high-temperature steam is reduced into tungsten powder under the effect of reducing atmosphere hydrogen, and under the cooling effect of reactor interlayer taking circulating water as cooling medium, spontaneous nucleation, cohesion forms the nano particle of tungsten, and fall in gathering-device.
Embodiment 1
Get 600gNa
2wO
45H
2o is dissolved in 2L distilled water, adds 5gCTAB; 180g hydrochloric acid is configured to solution, slowly drops in above-mentioned solution, room temperature lower magnetic force stirs 1-2h.Reacted solution is carried out centrifugal sedimentation, with distilled water, acetone cyclic washing sediment; Gained precipitation puts into 50 DEG C of dry 10h of baking oven, then puts into the Muffle furnace calcination 4h of 400 DEG C; Then powder is placed in plasma reaction chamber, take operating voltage as 60v, and operating current is the electric arc ionization argon gas that the condition of 400A produces, and plasma maintains about 1000 DEG C to tungstic acid powder heating-up temperature, and the tungsten powder average grain diameter of collection is 36nm.
Embodiment 2
Get 600gNa
2wO
45H
2o is dissolved in 2L distilled water, adds 6gCTAB, and 60g hydrochloric acid is configured to solution, slowly drops in above-mentioned solution, and room temperature lower magnetic force stirs 30min; Stir and be placed in the autoclave of inner liner polytetrafluoroethylene, baking oven reactor being put into 80 DEG C reacts 20h; Be cooled to room temperature after reaction, filter and use distilled water, absolute ethyl alcohol cyclic washing sediment, then putting into 60 DEG C of dry 9h of baking oven; Gained sediment puts into the Muffle furnace calcination 3h of 450 DEG C; Then powder is placed in plasma reaction chamber, take operating voltage as 75v, and operating current is the electric arc ionization argon gas that the condition of 550A produces, and plasma maintains about 1500 DEG C to tungstic acid powder heating-up temperature, and the tungsten powder average grain diameter of collection is 51nm.
Embodiment 3
Get 600gNa
2wO
45H
2o is dissolved in 2L distilled water, adds 1.2gCTAB, and 300g hydrochloric acid is configured to solution, slowly drops in above-mentioned solution, and room temperature lower magnetic force stirs 30min; Stir and be placed in the autoclave of inner liner polytetrafluoroethylene, baking oven reactor being put into 120 DEG C reacts 24h; Be cooled to room temperature after reaction, filter and use distilled water, absolute ethyl alcohol cyclic washing sediment, then putting into 70 DEG C of dry 10h of baking oven; Gained sediment puts into the Muffle furnace calcination 2h of 500 DEG C; Then powder is placed in plasma reaction chamber, take operating voltage as 90v, and operating current is the electric arc ionization argon gas that the condition of 700A produces, and plasma maintains about 1800 DEG C to tungstic acid powder heating-up temperature, and the tungsten powder average grain diameter of collection is 27nm.
Above-mentioned embodiment is used for illustrative purposes only, and be not limitation of the present invention, the those of ordinary skill of relevant technical field, without departing from the spirit and scope of the present invention, can also make various change and modification, therefore all equivalent technical schemes also should belong to category of the present invention.
Claims (10)
1. a preparation method for tungsten powder, it comprises the following steps:
(1) by Na
2wO
45H
2o is dissolved in distilled water, adds CTAB;
(2) drip hydrochloric acid solution again, magnetic agitation mixes;
(3) mixed solution is placed in autoclave and adds thermal response;
(4) filter after being cooled to room temperature again, be precipitated thing; Washing precipitate, and dry;
(5) sediment of oven dry is put into Muffle furnace calcination, obtain tungstic acid powder;
(6) tungstic acid powder is placed in plasma reaction chamber, in this reative cell, form high-temperature plasma by ionization inert gas, tungstic acid powder is reduced into tungsten powder after being heated by high-temperature plasma under reducing atmosphere.
2. method according to claim 1, is characterized in that: after adopting step (2), the solution stirred is carried out centrifugal sedimentation, then washing precipitate, and dry, then carry out step (5) and (6).
3. method according to claim 1 and 2, is characterized in that: described Na
2wO
45H
2the mass ratio of O, CTAB, hydrochloric acid is 1:(0.002-0.01): (0.1-0.5).
4. method according to claim 1, is characterized in that: the heating-up temperature of reactor is 80 DEG C--120 DEG C, the reaction time is 20h-24h.
5. method according to claim 1, is characterized in that: adopt distilled water and absolute ethyl alcohol cyclic washing during washing.
6. method according to claim 1 and 2, is characterized in that: adopt 50 DEG C during oven dry--dry 8h-10h for 70 DEG C.
7. method according to claim 1 and 2, is characterized in that: in Muffle furnace, adopt 400 DEG C--the temperature calcination 2h-4h of 500 DEG C.
8. method according to claim 1 and 2, is characterized in that: plasma reaction is indoor is plasma working gas with argon gas, and hydrogen is reducing atmosphere; With tungstic acid powder for positive pole, plasma gun is negative pole, the electric arc ionization inert gas produced between a positive electrode and a negative electrode after energising, thus formation high-temperature plasma heats tungstic acid powder.
9. method according to claim 8, is characterized in that: operating voltage during energising is 60v--90v, and operating current is 400A--700A.
10. method according to claim 8, is characterized in that: be 1000 DEG C to the heating-up temperature of tungstic acid powder--1800 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105798317A (en) * | 2016-03-31 | 2016-07-27 | 宇辰新能源材料科技无锡有限公司 | Preparation method for polyhedral submicron tungsten powder |
| CN105855561A (en) * | 2016-04-29 | 2016-08-17 | 九江有色金属冶炼有限公司 | Preparing method of superfine/nano tantalum tungsten composite powder and superfine/nano tantalum tungsten composite powder prepared through same |
| CN107570724A (en) * | 2017-08-15 | 2018-01-12 | 崇义章源钨业股份有限公司 | The continuous method for preparing nano-tungsten powder of industrialization |
| CN107626930A (en) * | 2017-09-27 | 2018-01-26 | 崇义章源钨业股份有限公司 | The method that nano-tungsten powder is prepared using ammonium tungstate |
| CN109079151A (en) * | 2018-08-16 | 2018-12-25 | 南昌大学 | A kind of method of high temperature solution phase reduction method tungsten oxide preparation extra-coarse tungsten powder |
| CN109396456A (en) * | 2018-12-28 | 2019-03-01 | 西安赛隆金属材料有限责任公司 | A kind of preparation facilities and method at globular tungsten powder end |
| CN110170659A (en) * | 2019-05-29 | 2019-08-27 | 宁波广新纳米材料有限公司 | The production method of ball-type nano-tungsten powder |
| CN112222421A (en) * | 2020-12-07 | 2021-01-15 | 西安稀有金属材料研究院有限公司 | Preparation method and application of nano tungsten trioxide and nano tungsten powder |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105798317B (en) * | 2016-03-31 | 2017-08-25 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of polyhedron Sub-micron Tungsten Powder |
| CN105798317A (en) * | 2016-03-31 | 2016-07-27 | 宇辰新能源材料科技无锡有限公司 | Preparation method for polyhedral submicron tungsten powder |
| CN105855561A (en) * | 2016-04-29 | 2016-08-17 | 九江有色金属冶炼有限公司 | Preparing method of superfine/nano tantalum tungsten composite powder and superfine/nano tantalum tungsten composite powder prepared through same |
| CN105855561B (en) * | 2016-04-29 | 2022-01-25 | 九江有色金属冶炼有限公司 | Preparation method of superfine/nano tantalum-tungsten composite powder and superfine/nano tantalum-tungsten composite powder prepared by same |
| CN107570724A (en) * | 2017-08-15 | 2018-01-12 | 崇义章源钨业股份有限公司 | The continuous method for preparing nano-tungsten powder of industrialization |
| CN107626930A (en) * | 2017-09-27 | 2018-01-26 | 崇义章源钨业股份有限公司 | The method that nano-tungsten powder is prepared using ammonium tungstate |
| CN107626930B (en) * | 2017-09-27 | 2019-07-26 | 崇义章源钨业股份有限公司 | The method for preparing nano-tungsten powder using ammonium tungstate |
| CN109079151B (en) * | 2018-08-16 | 2021-09-28 | 南昌大学 | Method for preparing ultra-coarse tungsten powder by high-temperature liquid-phase reduction of tungsten oxide |
| CN109079151A (en) * | 2018-08-16 | 2018-12-25 | 南昌大学 | A kind of method of high temperature solution phase reduction method tungsten oxide preparation extra-coarse tungsten powder |
| CN109396456A (en) * | 2018-12-28 | 2019-03-01 | 西安赛隆金属材料有限责任公司 | A kind of preparation facilities and method at globular tungsten powder end |
| CN109396456B (en) * | 2018-12-28 | 2024-02-13 | 西安赛隆金属材料有限责任公司 | A device and method for preparing spherical tungsten powder |
| CN110170659A (en) * | 2019-05-29 | 2019-08-27 | 宁波广新纳米材料有限公司 | The production method of ball-type nano-tungsten powder |
| CN112222421A (en) * | 2020-12-07 | 2021-01-15 | 西安稀有金属材料研究院有限公司 | Preparation method and application of nano tungsten trioxide and nano tungsten powder |
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