CN111362305A - Orange tungsten for uniform superfine tungsten powder and preparation method thereof - Google Patents
Orange tungsten for uniform superfine tungsten powder and preparation method thereof Download PDFInfo
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- CN111362305A CN111362305A CN202010315925.0A CN202010315925A CN111362305A CN 111362305 A CN111362305 A CN 111362305A CN 202010315925 A CN202010315925 A CN 202010315925A CN 111362305 A CN111362305 A CN 111362305A
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- tungsten
- orange
- uniform
- tungsten powder
- ammonium
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 43
- 239000010937 tungsten Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- ZGRBQKWGELDHSV-UHFFFAOYSA-N N.[W+4] Chemical compound N.[W+4] ZGRBQKWGELDHSV-UHFFFAOYSA-N 0.000 claims description 6
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 9
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 description 6
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 4
- 229910001930 tungsten oxide Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011362 coarse particle Substances 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses orange tungsten for uniform superfine tungsten powder and a preparation method thereof. The process is simple, and the prepared orange tungsten ore is beneficial to producing ultrafine tungsten powder/tungsten carbide powder with uniform granularity and stable performance.
Description
Technical Field
The invention relates to the field of powder metallurgy, in particular to orange tungsten oxide for uniform superfine tungsten powder and a preparation method thereof.
Background
Tungsten, a refractory metal, has excellent physical properties and is a well-known strategic resource. The tungsten powder/tungsten carbide powder is not only a main raw material of the cemented carbide, but also a main raw material of the tungsten-based alloy, and is widely applied to the fields of machining, mining, geological drilling, construction tools, bulb lighting, military engineering and the like. In order to continuously improve the performance of the material, the trend is to uniformly refine the powder so as to prepare tungsten related products with more excellent performance. The commonly used preparation method of tungsten powder at present is that ammonium tungsten compound-tungsten oxide-tungsten powder-tungsten carbide powder, the process has strong shape inheritance, therefore, the structure, components and physical and chemical properties of raw materials have important influence on the product performance, for example, tungsten oxide with large specific area is beneficial to preparing tungsten powder with finer granularity. Tungsten oxide raw material selection has been long developed, ranging from the first tungstic and yellow tungsten to the present blue and violet tungsten. The yellow tungsten is not suitable for preparing superfine tungsten powder at present due to small specific surface area; the specific surface area of the purple tungsten is large, the phase composition is single, but the production process has very strict operation requirements, is difficult to control and has lower yield, so that the cost and the process need to be further improved; the blue tungsten has large specific surface area and can be used for preparing the superfine tungsten powder, but the phase is relatively complex, and the prepared superfine tungsten powder has the phenomenon of uneven granularity of coarse particles and fine particles.
Disclosure of Invention
The invention aims to overcome a series of problems of poor uniformity, complex phase composition, uneven fineness of the coarse particles and the fine particles in tungsten powder and tungsten carbide production and the like in the existing process, and seeks a relatively simple and efficient method for preparing uniform superfine tungsten powder from tungsten oxide serving as a raw material for preparing superfine tungsten powder/tungsten carbide powder as an entry point, and orange tungsten with high specific surface area, high particle uniformity and single phase composition is prepared by a low-temperature secondary calcination multi-temperature control zone process method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of orange tungsten for uniform superfine tungsten powder comprises the following steps:
(1) feeding the ammonium-tungsten compound raw material into a rotary furnace from a bin through a screw feeder, and calcining the rotary furnace in a negative-pressure air-ventilation environment;
(2) firstly, carrying out primary multi-zone temperature control calcination on the raw materials, wherein the calcination temperature gradient is 200-500 ℃;
(3) performing secondary multi-zone temperature control calcination on the material produced in the step (2), wherein the calcination temperature gradient is 350-;
(4) cooling and sieving the material after the secondary calcination to obtain orange tungsten with better particle uniformity;
further, the ammonium tungsten compound includes, but is not limited to, ammonium metatungstate, ammonium paratungstate, and the like, and preferably ammonium paratungstate.
Further, in the step (1), the speed of the screw feeder is 30-50 Hz, and the rotating speed of the furnace tube is 20-30 Hz.
Further, the temperature of the plurality of zones in the step (2) is controlled to be 3-6 zones, and the temperature is preferably controlled to be 3 zones.
The orange tungsten prepared by the method is used for preparing tungsten powder/tungsten carbide powder.
Compared with the prior art, the invention has the following beneficial effects: (1) by adjusting the process conditions, the produced orange tungsten has high specific surface area and large chemical activity, has more single phase composition compared with the existing blue tungsten on the market at present, and is beneficial to producing superfine tungsten powder/tungsten carbide powder with uniform granularity and stable performance; (2) the process does not need to be protected by inert gas, and the calcination is directly carried out in the air environment, so that the process is relatively simple and the energy is saved.
Drawings
Fig. 1 is an XRD pattern of orange tungsten prepared in example 1.
Fig. 2 is a prior art high specific surface area blue tungsten XRD pattern.
Detailed Description
The following is a further description of the production of uniform ultrafine tungsten powder/tungsten carbide powder using orange tungsten by means of specific examples.
Example 1: the preparation method of the orange tungsten comprises the following steps:
ammonium paratungstate is poured into the feed bin, and the rotary furnace is sent into with 35Hz input speed through screw feeder again, and the rotary furnace is controlled temperature through three areas and is let in the air and calcine, and the calcination temperature for the first time is: one belt is 300 ℃, two belts are 400 ℃, three belts are 500 ℃, the secondary calcination temperature is 400 ℃, two belts are 500 ℃, three belts are 600 ℃, after the secondary low-temperature calcination is completely carried out, the product can be obtained by cooling and sievingSpecific surface area of 11.268m2Orange tungsten, uniform particle. X-ray diffraction was performed on the orange tungsten prepared in the examples and the existing blue tungsten with high specific surface area, and as can be seen from fig. 1 and 2, the orange tungsten phase composition was: 95.6% WO3And 4.4% WO2.9The blue-tungsten phase comprises: 72.9% WO3、26.8％WO2.9And 0.5% WO2.72The blue tungsten contains a small amount of purple tungsten, so that the uniformity of particles of the superfine tungsten powder prepared by the blue tungsten is poor, the phase composition of the orange tungsten prepared by the embodiment is more single, the superfine tungsten powder/tungsten carbide powder is favorably produced, the particle size is uniform, and the performance is more stable.
Example 2: the preparation method of the orange tungsten comprises the following steps:
ammonium metatungstate is poured into the feed bin, and the rotary kiln is sent into with 30Hz input speed through screw feeder, and furnace tube rotational speed 20 Hz, rotary kiln control temperature and let in the air through three areas and calcine, and the first calcination temperature is: the first belt is 200 ℃, the second belt is 350 ℃, the third belt is 500 ℃, the second calcining temperature is 350 ℃, the second belt is 450 ℃, the third belt is 600 ℃, after the second low-temperature calcining is completed, the orange tungsten with good particle uniformity and composed of two phases is obtained by cooling and sieving.
Claims (7)
1. The preparation method of the orange tungsten for the uniform superfine tungsten powder is characterized by comprising the following steps:
(1) feeding the ammonium-tungsten compound raw material into a rotary furnace from a bin through a screw feeder, and calcining the rotary furnace in a negative-pressure air-ventilation environment;
(2) firstly, carrying out primary multi-zone temperature control calcination on the raw materials, wherein the calcination temperature gradient is 200-500 ℃;
(3) performing secondary multi-zone temperature control calcination on the material produced in the step (2), wherein the calcination temperature gradient is 350-;
(4) and cooling and sieving the material after the secondary calcination to obtain the orange tungsten with better particle uniformity.
2. The method for preparing orange tungsten for uniform ultrafine tungsten powder according to claim 1, wherein the ammonium tungsten compound is ammonium metatungstate or ammonium paratungstate.
3. The method for preparing orange tungsten for uniform ultrafine tungsten powder according to claim 2, wherein the ammonium tungsten compound is ammonium paratungstate.
4. The method for preparing orange tungsten powder for uniform ultrafine tungsten powder according to claim 3, wherein the speed of the screw feeder in the step (1) is 30-50 Hz, and the rotating speed of the furnace tube is 20-30 Hz.
5. The method for preparing orange tungsten for uniform ultrafine tungsten powder according to claim 1, wherein the temperature of the plurality of zones in step (2) is controlled to 3 to 6 zones.
6. The method for preparing orange tungsten for uniform ultrafine tungsten powder according to claim 5, wherein the temperature control in step (2) is 3 zones.
7. The orange tungsten ore produced by the method for producing orange tungsten for the uniform ultrafine tungsten powder according to any one of claims 1 to 7.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479259A (en) * | 2020-12-14 | 2021-03-12 | 江钨世泰科钨品有限公司 | Yellow tungsten oxide with high specific surface area and low residual ammonia and preparation method thereof |
| CN113912125A (en) * | 2021-11-05 | 2022-01-11 | 赣州海盛钨钼集团有限公司 | Calcination process for preparing yellow tungsten oxide with high specific surface area and low residual ammonia |
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| CN113912125A (en) * | 2021-11-05 | 2022-01-11 | 赣州海盛钨钼集团有限公司 | Calcination process for preparing yellow tungsten oxide with high specific surface area and low residual ammonia |
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Effective date of registration: 20220919 Address after: Office Building, No. 11, Jingsan Road, Hong Kong Industrial Park, Economic and Technological Development Zone, Ganzhou City, Jiangxi Province 341003 Patentee after: GANZHOU SUNNY NON-FERROUS METALS CO.,LTD. Address before: 341599 Xinhua Industrial community, Dayu Industrial Park, Ganzhou City, Jiangxi Province Patentee before: GANZHOU HAICHUANG TUNGSTEN CO.,LTD. |
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Denomination of invention: Orange tungsten for uniform ultrafine tungsten powder and its preparation method Effective date of registration: 20230804 Granted publication date: 20220628 Pledgee: Everbright Xinglong Trust Co.,Ltd. Pledgor: GANZHOU SUNNY NON-FERROUS METALS CO.,LTD. Registration number: Y2023980050936 |
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Address after: 341000 Office Building 15 Songshan Xia Road, Ganzhou Economic and Technological Development Zone, Ganzhou City, Jiangxi Province Patentee after: GANZHOU SUNNY NON-FERROUS METALS CO.,LTD. Country or region after: China Address before: Office Building, No. 11, Jingsan Road, Hong Kong Industrial Park, Economic and Technological Development Zone, Ganzhou City, Jiangxi Province 341003 Patentee before: GANZHOU SUNNY NON-FERROUS METALS CO.,LTD. Country or region before: China |
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