The preparation system of the blue tungsten of a kind of high-specific surface area and method
Technical field
The present invention relates to a kind of preparation method of blue tungsten, particularly the preparation method of the blue tungsten of a kind of high-specific surface area.
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.
Produce in the process of metal tungsten powder in tungsten oxide hydrogen reduction, the quality of character on reduction process and final tungsten powder of Tungsten oxide 99.999 used has larger impact.The specific surface area of Tungsten oxide 99.999 refers to the total surface area that unit mass oxidation tungsten powder has, conventional m
2/ g represents, its is the granularity of reflection oxidation tungsten powder and granule-morphology indirectly, 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 99.999 greatly then means that reduction process has good dynamic conditions, is conducive to the infiltration of hydrogen and the effusion of water vapour when hydrogen reduction, and also require that when producing the lamp tungsten filament of doping tungsten oxide specific surface area is large, crackle is many, so that doping.Simultaneously because the Tungsten oxide 99.999 chemically reactive of high-specific surface area is high, reduction rate is large, therefore can accelerate to push away boat speed and strengthen boat charge (or improving the feeding coal of converter), thus the significant production efficiency improving tungsten powder.Also the Tungsten oxide 99.999 of bigger serface is conducive to producing the thinner tungsten powder of granularity, tungsten carbide powder to have a large amount of documents and production practice to show.Current tungsten powder, tungsten carbide powder technology are just towards ultra-fine (nanometer) change, super alligatoring, ultrapureization, centralization future development.The Tungsten oxide 99.999 of bigger serface will promote the development of ultrafine tungsten powder, tungsten carbide powder further.
Summary of the invention
The object of this invention is to provide preparation system and the method for the blue tungsten of a kind of high-specific surface area, the preparation system possessing multiple temperature band control region is adopted 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:
The preparation system of the blue tungsten of a kind of high-specific surface area, it is characterized in that, comprise raw material feed bin, feeding machine, calcining furnace, Tungsten oxide 99.999 feed bin and sieve shaker, described raw material feed bin is connected to the feeding port of calcining furnace by feeding machine, the discharge port of described calcining furnace is connected to Tungsten oxide 99.999 feed bin entrance, described Tungsten oxide 99.999 bin outlet is connected to sieve shaker, described calcining furnace is provided with multiple temperature band control region, described calcining furnace is rotary kiln, described feeding machine is screw feeder, and described calcining furnace is provided with 3-6 temperature band control region.
A preparation method for the blue tungsten of high-specific surface area, is characterized in that, comprise the following steps:
S1, by ammonium tungsten compound raw material from raw material feed bin by sending in calcining furnace in screw feeder;
S2, calcining furnace are calcined raw material under negative pressure closed environment, and described calcining furnace fire box temperature adopts and controlled by height gradient type temperature control cincture on earth, and thermograde is 800 DEG C-500 DEG C;
Material after S3, calcining carries out cooling and sieves, and obtains specific surface area>=10m
2the blue tungsten of high-specific surface area of/g.
Preferably, in step S1, calcining raw materials ammonium tungsten compound is APT.
Preferably, in step S2, calcining furnace is rotary kiln.
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, the front temperature band of gradient type temperature control cincture and rear temperature band form 0 DEG C of-300 DEG C of thermograde.
Preferably, vacuum tightness (0.5-1.3) × 10 in burner hearth in step S2
4pa.
Preferably, step S2 is also included in calcining burner hearth and is filled with protective gas, and described gas is nitrogen.
Preferably, in step S1, the feeding speed of screw feeder is 100-250kg/h.
The principal feature of present method produces its specific surface area>=10m of blue tungsten obtained
2/ g.
Beneficial effect of the present invention: the blue tungsten produced has high-specific surface area, the blue tungsten chemically reactive of high-specific surface area is large, and hydrogen reduction speed, effectively improves the production efficiency of tungsten powder and be more conducive to producing rear end product ultrafine tungsten powder, tungsten carbide powder.
Accompanying drawing explanation
Accompanying drawing 1 is the preparation system schematic diagram of the blue tungsten of a kind of high-specific surface area of the present invention.
Embodiment
In the specification, term " ammonium tungsten compound " is the general designation of same (mixing) the polyacid ammonium salt compound of tungsten and calcinate 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 and embodiment, the invention will be further described
The preparation system of the blue tungsten of a kind of high-specific surface area, comprise raw material feed bin 1, feeding machine, calcining furnace 2, Tungsten oxide 99.999 feed bin 3 and sieve shaker 4, described raw material feed bin 1 is connected to the feeding port of calcining furnace by feeding machine, the discharge port of described calcining furnace is connected to Tungsten oxide 99.999 feed bin entrance, described Tungsten oxide 99.999 bin outlet is connected to sieve shaker, and described calcining furnace is provided with 3-6 temperature band control region for carrying out the calcining of differing temps to raw material.
embodiment 1
Being inserted by APT in feeding warehouse, is 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: 750 DEG C, a band, 750 DEG C, two band, 660 DEG C, three band, 630 DEG C, four band, five are with 610 DEG C, 610 DEG C, six band.After rotary kiln calcining, cooling is sieved, and can obtain specific surface area is 12.35m
2the blue tungsten of/g.
embodiment 2
Being inserted by APT in feeding warehouse, is that speed sends into vacuum tightness (0.5-0.8) × 10 by screw feeder with 225kg/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, 700 DEG C, three band, 640 DEG C, four band, five are with 640 DEG C, 610 DEG C, six band.After rotary kiln calcining, cooling is sieved, and can obtain specific surface area is 12.65m
2the blue tungsten of/g.
embodiment 3
Being inserted by APT in feeding warehouse, is 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, 630 DEG C, four band, five are with 595 DEG C, 560 DEG C, six band.After rotary kiln calcining, cooling is sieved, and can obtain specific surface area is 10.91m
2the blue tungsten of/g.
The preparation method of the blue tungsten of a kind of high-specific surface area according to the present invention, can obtain specific surface area>=10m
2the blue tungsten of/g.