CN104944472A - Preparation method of high fluidity tungsten oxide - Google Patents

Preparation method of high fluidity tungsten oxide Download PDF

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Publication number
CN104944472A
CN104944472A CN201510339447.6A CN201510339447A CN104944472A CN 104944472 A CN104944472 A CN 104944472A CN 201510339447 A CN201510339447 A CN 201510339447A CN 104944472 A CN104944472 A CN 104944472A
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China
Prior art keywords
furnace
temperature
tungsten oxide
preparation
tungsten
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CN201510339447.6A
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CN104944472B (en
Inventor
廖小丽
谢金明
余春荣
朱亚模
李继红
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Jiangwu HC Starck Tungsten Products Co ltd
Jiangxi Tungsten Holding Group Co ltd
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Jiangxi Rare Earth and Rare Metals Tungsten Group Holding Co Ltd
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Priority to CN201510339447.6A priority Critical patent/CN104944472B/en
Publication of CN104944472A publication Critical patent/CN104944472A/en
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Publication of CN104944472B publication Critical patent/CN104944472B/en
Expired - Fee Related legal-status Critical Current
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Abstract

The invention relates to a preparation method of high fluidity tungsten oxide. According to the preparation method, an ammonium-tungsten compound is taken as a raw material for calcination in a negative-pressure closed calcination furnace; the furnace temperature is controlled in a gradient manner; 2-6 temperature control belts are arranged in a calcination process; the temperature of a feeding end is 700-800 DEG C; the temperature of a discharging end is 500-700 DEG C; the temperature differences of previous temperature control belts and next temperature control belts are temperature gradients of 0-300 DEG C; the furnace vacuum degree is (0.1-0.5)*10<4> Pa; the calcination process in the negative pressure closed calcination furnace lasts for 20-50 min; furnace burden is cooled through a cooling water jacket arranged in the negative pressure closed calcination furnace, and then the cooled furnace burden is discharged for screening, so that a tungsten oxide product of which the fluidity is lower than or equal to 30 s/50 g. Through adoption of the preparation method, the obtained tungsten oxide product is high in fluidity, and the problems that automatic feeding equipment is non-uniform in feeding and the automatic weighing equipment is non-uniform in material weighing can be effectively solved; the automation degree of tungsten powder production is improved, the labor intensity is eased, and the cost in tungsten powder production is reduced.

Description

A kind of preparation method of high workability Tungsten oxide 99.999
Technical field
The present invention relates to the preparation method of Tungsten oxide 99.999, particularly a kind of preparation method of high workability Tungsten oxide 99.999.
In the application, term " ammonium tungsten compound " is the general designation of same (mixing) the polyacid ammonium salt compound of tungsten and calcinate thereof.
In the application, term APT is the abbreviation of " ammonium paratungstate ".
In the application, term " Tungsten oxide 99.999 " refers to blue tungsten oxide or tungstic violet oxide.
Background technology
Tungsten is a kind of non-ferrous metal of infusibility, is also a kind of important strategic resource, is used widely because it has the premium propertiess such as fusing point is high, hardness is large, ductility is strong, wear-resisting and corrosion-resistant.
At present, major equipment mainly pusher reduction furnace and the rotary type reduction furnace of tungsten powder is produced.
The feeding manner of pusher reduction furnace is that Tungsten oxide 99.999 is placed in boat, and the promotion by push rod realizes charging and discharging.This feeding manner relates to the problem of weighing of Tungsten oxide 99.999, and the mode of weighing has two kinds: manually weigh and automatic Weighing.Manually weigh: shoveled from bucket in boat by Tungsten oxide 99.999 with scoop, each shovel 0.5-4kg(is according to actual tungsten powder production technique adjustment charge amount).Such production model causes the labour intensity of workman large, or even woman worker cannot be competent at this work.Automatic Weighing: feed bin Tungsten oxide 99.999 being placed in automatic material weighing machine, utilizes its flow by gravity in boat.Such production model, workman, without the need to shovel material, greatly alleviates the labour intensity of workman.Adopt the production model of automatic Weighing, require high to the mobility of Tungsten oxide 99.999, if the poor fluidity of Tungsten oxide 99.999, gravity flow has some setbacks, and will waste time, and makes automatic weighing equipment become nonsensical, and the weight fluctuation of weighing is large, affects the quality of production of tungsten powder.
The feeding manner of rotary type reduction furnace is opening for feed Tungsten oxide 99.999 being placed in reduction furnace, utilizes himself flow by gravity in boiler tube.Such production model avoids manually shovels material, but requires high to the mobility of Tungsten oxide 99.999.If the poor fluidity of Tungsten oxide 99.999, the inlet amount fluctuation of Tungsten oxide 99.999 so can be caused large, affect the quality of production of tungsten powder.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of high workability Tungsten oxide 99.999, can improve the level of automation that tungsten powder is produced, alleviate the labour intensity of employee, and reduce the production cost of tungsten powder.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of preparation method of high workability Tungsten oxide 99.999, comprising:
[1] with ammonium tungsten compound for raw material, calcine in the calcining furnace that negative pressure is airtight, gradient type is adopted to control fire box temperature, calcination process is provided with 2-6 temperature control cincture, feed end temperature 700 DEG C-800 DEG C, discharge end temperature 500 DEG C-700 DEG C, front temperature band and the rear temperature band temperature difference 0 DEG C of-300 DEG C of thermograde;
[2] vacuum tightness (0.1-1.5) × 10 in calcining furnace burner hearth 4pa, calcining furnace furnace protection atmosphere is non-oxidizing atmosphere;
[3] feed material feed rates 50-250kg/h;
[4] in the airtight calcining furnace of negative pressure, 20-50min is calcined;
[5] furnace charge is come out of the stove after being cooled by the cooling water jecket that calcining furnace is provided with, and sieves subsequently and obtains the Tungsten oxide 99.999 product of mobility≤30s/50g.
Described calcining furnace is rotary kiln or without boat belt continuous calcining stove.The mesh density of sieving after coming out of the stove after described furnace charge cools requires to determine sieve number according to product granularity.
The invention has the beneficial effects as follows: the Tungsten oxide 99.999 that the present invention produces has high workability, efficiently solve the problem of automatic feed equipment charging inequality and the problem of automatic weighing equipment weighing inequality.Improve the level of automation that tungsten powder is produced, alleviate the labour intensity of employee, thus reduce the production cost of tungsten powder.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the schematic diagram of high workability Tungsten oxide 99.999 preparation technology.
Embodiment
embodiment 1 as shown in Figure 1: APT is inserted in feeding warehouse, be that speed sends into vacuum tightness (0.5-0.8) × 10 by screw feeder with 220kg/h 4in the rotary kiln of Pa, pass into protective gas nitrogen, temperature control is: 755 DEG C, a band, 755 DEG C, two band, 650 DEG C, three band, 635 DEG C, four band, five are with 635 DEG C, 635 DEG C, six band.After rotary kiln calcining, cooling is sieved, and can obtain the Tungsten oxide 99.999 that mobility is 26s/50g.
embodiment 2 as shown in Figure 1: APT is inserted in feeding warehouse, be that speed sends into vacuum tightness (0.5-0.8) × 10 by screw feeder with 200kg/h 4in the rotary kiln of Pa, pass into protective gas nitrogen, temperature control is: 800 DEG C, a band, 800 DEG C, two band, 650 DEG C, three band, 640 DEG C, four band, five are with 620 DEG C, 610 DEG C, six band.After rotary kiln calcining, cooling is sieved, and can obtain the Tungsten oxide 99.999 that mobility is 26s/50g.
embodiment 3 as shown in Figure 1: APT is inserted in feeding warehouse, be that speed sends into vacuum tightness (0.8-1.2) × 10 by screw feeder with 180kg/h 4in the rotary kiln of Pa, pass into protective gas nitrogen, temperature control is: 750 DEG C, a band, 750 DEG C, two band, 660 DEG C, three band, 660 DEG C, four band, five are with 550 DEG C, 550 DEG C, six band.After rotary kiln calcining, cooling is sieved, and can obtain the Tungsten oxide 99.999 that mobility is 27s/50g.

Claims (3)

1. a preparation method for high workability Tungsten oxide 99.999, comprising:
[1] with ammonium tungsten compound for raw material, calcine in the calcining furnace that negative pressure is airtight, gradient type is adopted to control fire box temperature, calcination process is provided with 2-6 temperature control cincture, feed end temperature 700 DEG C-800 DEG C, discharge end temperature 500 DEG C-700 DEG C, front temperature band and the rear temperature band temperature difference 0 DEG C of-300 DEG C of thermograde;
[2] vacuum tightness (0.1-1.5) × 10 in calcining furnace burner hearth 4pa, calcining furnace furnace protection atmosphere is non-oxidizing atmosphere;
[3] feed material feed rates 50-250kg/h;
[4] in the airtight calcining furnace of negative pressure, 20-50min is calcined;
[5] furnace charge is come out of the stove after being cooled by the cooling water jecket that calcining furnace is provided with, and sieves subsequently and obtains the Tungsten oxide 99.999 product of mobility≤30s/50g.
2. the preparation method of a kind of high workability Tungsten oxide 99.999 according to claim 1, is characterized in that: described calcining furnace is rotary kiln or without boat belt continuous calcining stove.
3. the preparation method of a kind of high workability Tungsten oxide 99.999 according to claim 1, is characterized in that: the mesh density of sieving after coming out of the stove after described furnace charge cools requires to determine sieve number according to product granularity.
CN201510339447.6A 2015-06-18 2015-06-18 A kind of preparation method of high fluidity tungsten oxide Expired - Fee Related CN104944472B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111362305A (en) * 2020-04-21 2020-07-03 赣州海创钨业有限公司 Orange tungsten for uniform superfine tungsten powder and preparation method thereof
CN116282175A (en) * 2023-05-09 2023-06-23 江钨世泰科钨品有限公司 Preparation method and system of superfine tungsten trioxide

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5125964A (en) * 1990-09-10 1992-06-30 General Electric Company Fluidized bed process for preparing tungsten powder
CN101642816A (en) * 2008-08-05 2010-02-10 江西稀有稀土金属钨业集团有限公司 Process for producing tungsten powder
CN102923649A (en) * 2012-11-05 2013-02-13 江苏和田科技材料有限公司 Reduction hydrogen production compound furnace and device and method for ammonium paratungstate tungsten production by using same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5125964A (en) * 1990-09-10 1992-06-30 General Electric Company Fluidized bed process for preparing tungsten powder
CN101642816A (en) * 2008-08-05 2010-02-10 江西稀有稀土金属钨业集团有限公司 Process for producing tungsten powder
CN102923649A (en) * 2012-11-05 2013-02-13 江苏和田科技材料有限公司 Reduction hydrogen production compound furnace and device and method for ammonium paratungstate tungsten production by using same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111362305A (en) * 2020-04-21 2020-07-03 赣州海创钨业有限公司 Orange tungsten for uniform superfine tungsten powder and preparation method thereof
CN116282175A (en) * 2023-05-09 2023-06-23 江钨世泰科钨品有限公司 Preparation method and system of superfine tungsten trioxide

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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: 20220208

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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