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.