CN105016393B - The preparation system of a kind of high-specific surface area indigo plant tungsten and method - Google Patents
The preparation system of a kind of high-specific surface area indigo plant tungsten and method Download PDFInfo
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- CN105016393B CN105016393B CN201510478011.5A CN201510478011A CN105016393B CN 105016393 B CN105016393 B CN 105016393B CN 201510478011 A CN201510478011 A CN 201510478011A CN 105016393 B CN105016393 B CN 105016393B
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Abstract
The present invention relates to a kind of preparation system and the method for high-specific surface area indigo plant tungsten, described method uses the preparation system with multiple temperature band control zone, and concrete preparation process is: pass through ammonium tungsten compound raw material from raw material feed bin to send in calcining furnace in screw(-type) feeder；Raw material is calcined under negative pressure closed environment by calcining furnace；Material after calcining carries out cooling and sieves, and obtains specific surface area >=10m2The high-specific surface area indigo plant tungsten of/g, can obtain that there is high-specific surface area by this method, the blue tungsten chemism of this high-specific surface area is big, and hydrogen reduction speed is effectively increased the production efficiency of tungsten powder and is more beneficial for producing end product ultrafine tungsten powder, tungsten carbide powder.
Description
Technical field
The present invention relates to the preparation method of a kind of blue tungsten, particularly to the preparation method of a kind of high-specific surface area indigo plant tungsten.
Background technology
Tungsten is the non-ferrous metal of a kind of infusibility, is also a kind of important strategic resource, is used widely because it has the premium properties such as fusing point is high, hardness is big, ductility is strong, wear-resisting and corrosion-resistant.
During metal tungsten powder is produced in tungsten oxide hydrogen reduction, the character of tungsten oxide used has large effect to the quality of reduction process and final tungsten powder.The specific surface area of tungsten oxide refers to the total surface area that unit mass oxidation tungsten powder is had, conventional m2/ g represents, its indirectly granularity of reflection oxidation tungsten powder and granule-morphology, be weigh oxidation tungsten powder in reduction process with the important indicator of gas-solid state substance reaction ability.The specific surface area of tungsten oxide the most then means that reduction process has preferable dynamic conditions, is conducive to the infiltration of hydrogen and the effusion of steam when hydrogen reduction, also requires that when producing the lamp tungsten filament of doping tungsten oxide specific surface area is big, and crackle is many, in order to doping.Simultaneously because the tungsten oxide chemism of high-specific surface area is high, reduction rate is big, therefore can accelerate push away boat speed and strengthen boat charge (or improving the feeding coal of converter), thus significantly improve the production efficiency of tungsten powder.Also the tungsten oxide of bigger serface is conducive to producing the thinner tungsten powder of granularity, tungsten carbide powder to have substantial amounts of document and production practices to show.At present tungsten powder, tungsten carbide powder technology are just changed towards ultra-fine (nanometer), super roughening, ultrapureization, centralization direction are developed.The tungsten oxide of bigger serface will promote the development of ultrafine tungsten powder, tungsten carbide powder further.
Summary of the invention
It is an object of the invention to provide a kind of preparation system and the method for high-specific surface area indigo plant tungsten, the preparation system possessing multiple temperature band control zone is used to be prepared, by improving the dynamic conditions of blue tungsten reduction process, improve the production efficiency of tungsten powder, the method not only improves the doping performance of blue tungsten, also helps and produces ultrafine tungsten powder, tungsten carbide powder.
For achieving the above object, the present invention is achieved through the following technical solutions:
A kind of preparation system of high-specific surface area indigo plant tungsten, it is characterized in that, including raw material feed bin, batcher, calcining furnace, tungsten oxide feed bin and vibrating sieving machine, described raw material feed bin is connected to the feeding port of calcining furnace by batcher, the discharging opening of described calcining furnace is connected to tungsten oxide feed bin entrance, described tungsten oxide bin outlet is connected to vibrating sieving machine, described calcining furnace is provided with multiple temperature band control zone, described calcining furnace is rotary furnace, described batcher is screw(-type) feeder, and described calcining furnace is provided with 3-6 temperature band control zone.
The preparation method of a kind of high-specific surface area indigo plant tungsten, it is characterised in that comprise the following steps:
S1, by ammonium tungsten compound raw material from raw material feed bin by screw(-type) feeder is sent in calcining furnace；
Raw material is calcined under negative pressure closed environment by S2, calcining furnace, and described calcining furnace fire box temperature uses and controlled band by height gradient type temperature on earth and control, and thermograde is 800 DEG C-500 DEG C；
Material after S3, calcining carries out cooling and sieves, and obtains specific surface area >=10m2The high-specific surface area indigo plant tungsten of/g.
Preferably, in step S1, calcining raw materials ammonium tungsten compound is APT.
Preferably, in step S2, calcining furnace is rotary furnace.
Preferably, in step S2, calcining furnace fire box temperature controls with 3-6.
Preferably, calcining furnace feed end temperature 700 DEG C-800 DEG C in step S2.
Preferably, discharge end of furnace temperature 500 DEG C-700 DEG C in step S2.
Preferably, in step S2, gradient type temperature controls front temperature band and rear temperature band 0 DEG C of-300 DEG C of thermograde of formation of band.
Preferably, vacuum (0.5-1.3) × 10 in burner hearth in step S24Pa。
Preferably, step S2 is filled with protective gas in being additionally included in calcining burner hearth, and described gas is nitrogen.
Preferably, in step S1, the feeding speed of screw(-type) feeder is 100-250kg/h.
Being mainly characterized by of this method produces its specific surface area >=10m of blue tungsten obtained2/g。
Beneficial effects of the present invention: the blue tungsten produced has high-specific surface area, the blue tungsten chemism of high-specific surface area is big, and hydrogen reduction speed is effectively increased the production efficiency of tungsten powder and is more beneficial for producing end product ultrafine tungsten powder, tungsten carbide powder.
Accompanying drawing explanation
Accompanying drawing 1 is the preparation system schematic diagram of the present invention a kind of high-specific surface area indigo plant tungsten.
Detailed description of the invention
In the specification, term " ammonium tungsten compound " is that tungsten is with (miscellaneous) polyacid ammonium salt compound and the general designation of calcined product thereof.
In the specification, term " blue tungsten " is that blue tungsten oxide is called for short.
In the specification, term APT is the abbreviation of " ammonium paratungstate ".
Below in conjunction with accompanying drawing, the invention will be further described with embodiment
A kind of preparation system of high-specific surface area indigo plant tungsten, including raw material feed bin 1, batcher, calcining furnace 2, tungsten oxide feed bin 3 and vibrating sieving machine 4, described raw material feed bin 1 is connected to the feeding port of calcining furnace by batcher, the discharging opening of described calcining furnace is connected to tungsten oxide feed bin entrance, described tungsten oxide bin outlet is connected to vibrating sieving machine, and described calcining furnace is provided with 3-6 temperature band control zone for raw material carries out the calcining of different temperatures.
Embodiment
1
APT is inserted in feeding warehouse, send into vacuum (0.5-0.8) × 10 with 200kg/h for speed by screw(-type) feeder4In the rotary furnace of Pa, be passed through protective gas nitrogen, temperature control be: 750 DEG C of a band, 750 DEG C of two band, 660 DEG C of three band, four 630 DEG C of bands, multicolored vaginal discharge 610 DEG C, 610 DEG C of six band.After rotary furnace is calcined, cooling is sieved, and can obtain specific surface area is 12.35m2The blue tungsten of/g.
Embodiment
2
APT is inserted in feeding warehouse, send into vacuum (0.5-0.8) × 10 with 225kg/h for speed by screw(-type) feeder4In the rotary furnace of Pa, be passed through protective gas nitrogen, temperature control be: 800 DEG C of a band, 800 DEG C of two band, 700 DEG C of three band, four 640 DEG C of bands, multicolored vaginal discharge 640 DEG C, 610 DEG C of six band.After rotary furnace is calcined, cooling is sieved, and can obtain specific surface area is 12.65m2The blue tungsten of/g.
Embodiment
3
APT is inserted in feeding warehouse, send into vacuum (0.8-1.2) × 10 with 180kg/h for speed by screw(-type) feeder4In the rotary furnace of Pa, be passed through protective gas nitrogen, temperature control be: 750 DEG C of a band, 750 DEG C of two band, 660 DEG C of three band, four 630 DEG C of bands, multicolored vaginal discharge 595 DEG C, 560 DEG C of six band.After rotary furnace is calcined, cooling is sieved, and can obtain specific surface area is 10.91m2The blue tungsten of/g.
The preparation method of a kind of high-specific surface area indigo plant tungsten according to the present invention, can obtain specific surface area >=10m2The blue tungsten of/g.
Claims (9)
1. a preparation method for high-specific surface area indigo plant tungsten, uses its preparation system following: include raw material
Feed bin, batcher, calcining furnace, tungsten oxide feed bin and vibrating sieving machine, described raw material feed bin is by batcher even
Being connected to the feeding port of calcining furnace, the discharging opening of described calcining furnace is connected to tungsten oxide feed bin entrance, described oxygen
Change tungsten bin outlet be connected to vibrating sieving machine, described calcining furnace is provided with multiple temperature band control zone, described in forge
Burning stove is rotary furnace, and described batcher is screw(-type) feeder, and described calcining furnace is provided with 3-6 temperature band control
District processed, it is characterised in that comprise the following steps:
S1, by ammonium tungsten compound raw material from raw material feed bin by screw(-type) feeder is sent in calcining furnace；
Raw material is calcined under negative pressure closed environment by S2, calcining furnace, and described calcining furnace fire box temperature is adopted
Control with being controlled band by height gradient type temperature on earth, the change of the temperature from calcining furnace feed end to discharge end
Change scope is 800 DEG C-500 DEG C and temperature is successively decreased from high to low；
Material after S3, calcining carries out cooling and sieves, and obtains specific surface area >=10m2The high-specific surface area of/g
Blue tungsten.
The preparation method of a kind of high-specific surface area indigo plant tungsten the most according to claim 1, it is characterised in that
In step S1, calcining raw materials ammonium tungsten compound is APT.
The preparation method of a kind of high-specific surface area indigo plant tungsten the most according to claim 1, it is characterised in that
In step S2, calcining furnace is rotary furnace.
The preparation method of a kind of high-specific surface area indigo plant tungsten the most according to claim 1, it is characterised in that
In step S2, calcining furnace fire box temperature controls with 3-6.
The preparation method of a kind of high-specific surface area indigo plant tungsten the most according to claim 1, it is characterised in that
Calcining furnace feed end temperature 700 DEG C-800 DEG C in step S2, discharge end of furnace temperature 500 DEG C-700 DEG C.
The preparation method of a kind of high-specific surface area indigo plant tungsten the most according to claim 1, it is characterised in that
The front temperature band that in step S2, gradient type temperature controls to carry exceeds 0 DEG C-300 DEG C than rear temperature zone temperature.
The preparation method of a kind of high-specific surface area indigo plant tungsten the most according to claim 1, it is characterised in that
Vacuum (0.5-1.3) × 10 in burner hearth in step S24Pa。
The preparation method of a kind of high-specific surface area indigo plant tungsten the most according to claim 1, it is characterised in that
Step S2 is filled with protective gas in being additionally included in calcining burner hearth, and described gas is nitrogen.
The preparation method of a kind of high-specific surface area indigo plant tungsten the most according to claim 1, it is characterised in that
In step S1, the feeding speed of screw(-type) feeder is 100-250kg/h.
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| CN105016393B true CN105016393B (en) | 2016-09-14 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105645473A (en) * | 2016-03-16 | 2016-06-08 | 江西稀有金属钨业控股集团有限公司 | Preparation system and method for blue tungsten with fine particles |
| CN110722172B (en) * | 2019-11-01 | 2022-08-26 | 厦门金鹭硬质合金有限公司 | Production method of high-pressure billet strength tungsten powder with wide particle size distribution |
| CN111362305B (en) * | 2020-04-21 | 2022-06-28 | 赣州海创钨业有限公司 | Orange tungsten for uniform superfine tungsten powder and preparation method thereof |
| CN111604504A (en) * | 2020-05-26 | 2020-09-01 | 蓬莱市超硬复合材料有限公司 | Undoped ultra-coarse grain tungsten powder and preparation method thereof |
| CN112479259B (en) * | 2020-12-14 | 2023-01-03 | 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 |
| CN116282175B (en) * | 2023-05-09 | 2024-07-05 | 江钨世泰科钨品有限公司 | Preparation method and system of superfine tungsten trioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH02141429A (en) * | 1988-11-22 | 1990-05-30 | Tokyo Tungsten Co Ltd | Method and apparatus for production of tungsten intermediate oxide |
| CN1238259C (en) * | 2003-09-10 | 2006-01-25 | 厦门金鹭特种合金有限公司 | Method and apparatus for preparing blue tungsten oxide by ammonium paratungstate self-reduction |
| CN101642816B (en) * | 2008-08-05 | 2013-03-27 | 江西稀有稀土金属钨业集团有限公司 | Process for producing tungsten powder |
| WO2012129782A1 (en) * | 2011-03-30 | 2012-10-04 | 厦门金鹭特种合金有限公司 | Preparation method of industrial purple nano-needle tungsten oxide |
| CN202688007U (en) * | 2012-05-11 | 2013-01-23 | 江西稀有金属钨业控股集团有限公司 | High-purity ammonium paratungstate preparation system |
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Address after: 330046 No. 118 West Beijing Road, Jiangxi, Nanchang Patentee after: JIANGXI TUNGSTEN HOLDING GROUP CO.,LTD. Address before: 330046 No. 118 West Beijing Road, Jiangxi, Nanchang Patentee before: JIANGXI RARE EARTH & RARE METALS TUNGSTEN GROUP HOLDING Co.,Ltd. |
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Effective date of registration: 20220214 Address after: 341000 Shuixi nonferrous metallurgy industrial base, Zhanggong District, Ganzhou City, Jiangxi Province Patentee after: JIANGWU H.C. STARCK TUNGSTEN PRODUCTS Co.,Ltd. Address before: 330046 No. 118 West Beijing Road, Jiangxi, Nanchang Patentee before: JIANGXI TUNGSTEN HOLDING GROUP CO.,LTD. |
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