CN1766510A - Ventilated forced drainage type nano tungsten powder reducing furnace for industrial use - Google Patents
Ventilated forced drainage type nano tungsten powder reducing furnace for industrial use Download PDFInfo
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- CN1766510A CN1766510A CN 200510086397 CN200510086397A CN1766510A CN 1766510 A CN1766510 A CN 1766510A CN 200510086397 CN200510086397 CN 200510086397 CN 200510086397 A CN200510086397 A CN 200510086397A CN 1766510 A CN1766510 A CN 1766510A
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Abstract
The invention discloses a poromeric draining pipe type reducing furnace, which comprises the following parts: boating-pushing device (1), firedoor (2), exhaust ignition or recovery pipe (3), poromeric boat-container (4), nanometer tungsten oxide powder (5), boat-container poromeric floor (6), furnace tube (7), positive pressure H 2 supply porous air-cushion (8), heating plate (9), drainage air-flow channel (10), furnace case (11), cold water case (12), positive pressure air-supply system (13) and furnace rack (14), wherein the positive pressure H 2 supply porous air-cushion (8) is set on the bottom of furnace tube (7); the H 2 even pressure chamber is formed between the double-layer boat-container poromeric plate (6) and porous air-cushion (8), which pierces the boat-container poromeric floor (6) after buffering. The average grain size of nanometer tungsten powder is or less than 35.5 nm with the distribution breadth ranged from 45 to 50 nm.
Description
Technical field
The invention belongs to the reduction apparatus technical field, a kind of ventilated forced drainage type nano tungsten powder reducing furnace for industrial use particularly is provided, be applicable to the various career fields that prepare nano metal powder with hydrogen reduction; Reduction as nano metal tungsten powder, nano-cobalt powder, nano-nickel powder, nanometer nickel one ferroalloy powder in the powder technology.
Background technology
By nearly 50 years literature search as can be known, use H
2Reduction WO
3Directly produce tungsten powder or be reduced into the history in existing more than 100 year of technology that blue tungsten, (or tungsten dioxide) restore into tungsten powder earlier, employed reduction furnace mostly is tubular type push boat type reduction furnace, the U.S., the Soviet Union, China and Germany begin to develop mechanical rotary furnace and fluid bed (fluidized bed furnace) reduction furnace after nineteen sixty-five, and China begins to develop the air-flow rotary furnace after 1996.Above-mentioned reduction furnace respectively has pluses and minuses, is that cost simple in structure is low as tubular type push boat type reduction furnace (containing four pipe Muffle furnaces, 12 pipe reduction furnaces etc.) advantage, and the loss of material rate is little.Shortcoming is that the material that is reduced at high temperature is and leaves standstill ground stacking states, H
2Air-flow flows through from the bed of material surface of piling up, and the product steam in the bed of material is difficult for by H
2Air-flow is taken away, and is easy to cause tungsten powder particles to grow up like this, and reduction rate is low, and efficient is poor, is difficult to produce nano-tungsten powder and other nano metal powder.
Mechanical type rotary furnace advantage is the bed of material that does not leave standstill, and material is and stirs, and sheds and flow regime powder energy and H
2Gas mixes preferably, and product steam is easily by H
2The band of gas is walked, and reduction rate is higher, and output is big, and tungsten powder particles is difficult for growing up.Shortcoming is, equipment complexity, cost height, rotating seal life-span are shorter, when producing ultra-fine grain and nano grade tungsten powder, the loss of material rate is higher, and material and tube wall and the frid surface is bonding, wall cling phenomenon is serious, event only is applicable in the production, the fine grained tungsten powder, is not suitable for to produce nano-tungsten powder and other nano metal powder.
The advantage of fluid bed (fluidized bed furnace) is H at high temperature
2Air-flow can with the material that is reduced, form gas one solid multiphase flow fluidized state, the material that is reduced can be with very little granule, even individual particle and H
2The gas contact, so reduction reaction speed is fast, the efficient height, tungsten particle is very difficult close in reduction process, so tungsten powder particles is difficult for growing up.Shortcoming is that loss of material is very big, and dedusting and recovery system are huge.Gas consumption, energy-output ratio are all very big, are difficult to carry out serialization, automatic mass production simultaneously.As the nano-tungsten powder reduction time, often use the thicker Al of granularity
2O
3Spheric granules is as the carrier that carries tungsten powder, to produce the jump action of boiling type.Also need after the reduction Al
2O
3The spheroid sieving separating.So this equipment when being used for producing nano-tungsten powder, is extremely unfavorable.
The air-flow rotary furnace is that the Wu Chengyi of University of Science ﹠ Technology, Beijing professor designed in 1997, and its advantage is in this rotary furnace, material that is reduced and (H
2+ N
2) gas, form uniform gas one solid heterogeneous suspension air-flow, at high temperature this heterogeneous air-flow, along the inwall of vertical furnace tube, screw type moving upward, until the boiler tube top, under suction function, circulate so repeatedly in the boiler tube bottom outside interior boiler tube turns back to then, finish until reduction reaction, tungsten powder is come out of the stove.In whole reduction process, the working gas (H of discharge
2+ N
2) seldom, so there is not dust removal problem, gas consumption, energy-output ratio are very low, tungstic acid and tungsten powder particles are in released state each other in the suspension air-flow in reduction process, do not have particle deposition and assemble the condition of growing up, therefore the tungsten powder particles of producing is very thin, and this equipment is specially adapted to produce the nano level superfine tungsten powder, but its shortcoming is to be difficult to realize serialization large-scale production, and removing water problems still needs external accessory to solve.
From the evolution of the above-mentioned various type of furnaces and strengths and weaknesses analysis as can be known, above all devices, 1. three basic demands that all can not have simultaneously in the time of can not comprehensively solving the reduced nano tungsten powder in other words are that loss of material will be lacked.2. be to want the instant steam that will react in the bed of material to discharge the bed of material fast up hill and dale in the reduction process.3. be the oxide particle that as far as possible will avoid tungsten, particularly tungsten powder particles contacts with each other.
In the process of preparation nano-tungsten powder, because raw material oxide powder is nanometer grade powder, so the strenuous exercise of material, be very disadvantageous to the casting yield of tungsten powder and the dust removal problem of equipment, be unfavorable therefore if select mechanical rotary furnace or ebullated bed.But existing tubular type push boat type reduction furnace, though there is not the problem of loss of material, but maximum shortcoming is the steam in the reaction bed of material can not discharge fast, therefore find over past ten years when producing nano-tungsten powder with tubular type push boat type reduction furnace, the average grain diameter of tungsten powder is high always, be difficult to reach≤100nm, and size distribution bandwidth＞120nm, the particle greater than 100nm in the powder still has 35% (mass fraction).This phenomenon has had a strong impact on the level of production of China's nano-tungsten powder.
A kind of new design that the application's summary of the invention proposes for the problem that solves draining difficulty in the tubular type push boat type reduction furnace just.
Summary of the invention
The object of the present invention is to provide a kind of ventilated forced drainage type nano tungsten powder reducing furnace for industrial use, can be in reduction process, continuously, discharge the bed of material fast up hill and dale, significantly reduced the average grain diameter of the reduction temperature and the tungsten powder of nano-tungsten powder product steam.Equipment manufacturing cost is low, and output is big, is suitable for most applying, and expectation will can be played great impetus to the production of China's nano-tungsten powder.
The present invention includes: push away boat mechanism 1, fire door 2, waste gas igniting or recovery tube 3, ventilative boat 4, nano oxidized tungsten powder 5, the ventilative base plate 6 of boat, boiler tube 7, malleation for H
2Porous air cushion 8, heating plate 9, draining gas channel 10, stove draw a bow to the full 11, water collar 12, malleation air supply system 13, grate 14.The structure of device as shown in Figure 1.
The difference of the type of furnace of the present invention and conventional tubular type push boat type reduction furnace is, the bottom of boiler tube 7 is provided with one in addition and can malleation supplies H
2The porous air cushion 8 of gas, the surface of porous air cushion 8 has a lot of apertures uniformly by different densities, be divided into uniformly in the porous air cushion 8 3～6 road air supply channels and with each aperture UNICOM, be connected with outside malleation air supply system 13 at the right-hand member of porous air cushion, to guarantee the H of air cushion in the stove
2Air pressure falls by linear distribution.This for H
2The characteristics of system and conventional tubular type push boat type stove one end air feed, the mode that flows to the other end is different fully, in the malleation permeability type air supply system of the present invention, for H
2The direction of gas is by the boiler tube bottom vertical upwards and pass the porose boat in each bottom.This malleation compulsory type plenum system not only can make fresh H
2Gas can continuously pass the whole reduction bed of material from bed of material bottom, thereby in can guaranteeing at any time product steam be got rid of the bed of material rapidly, controls H simultaneously strictly
2Under the situation of atmospheric pressure, can prevent nanopowder again, can be by H
2Air-blowing rises or takes away, and easily loses with the nothing of avoiding nanopowder.
Another special character of the present invention is on boat structure, has adopted double-deck permeability type boat.The bottom of boat is built on stilts, forms a H between ventilative base plate 6 of boat and porous air cushion 8
2Gas is all pressed chamber, H
2Gas passes the ventilative base plate 6 of boat again after all pressing buffering.The ventilative base plate of boat is to be that the stainless steel mesh cloth of 40～50 μ m is made with the aperture, nanopowder is reunited because of the electrostatic attraction effect is arranged between particle, be placed directly on the porous screen cloth can not leak down, this permeability type boat, pushing to by burner in the motion process of stove tail, constantly from the air-permeable mattress aperture, obtaining fresh H
2Gas, and be to be upward through the bed of material, H from the boat bottom
2In the process of one tunnel reduction, take product steam out of the boat bed of material fast again, be pooled to the exhausting waste gas passage on boat top, take all steam out of boiler tube by the off-gas flows that forms naturally in the boiler tube upper space then., also can with Luoci pump waste gas and steam be extracted out, preferably under the situation in condition through the recovery H that dewaters in igniting or exhaust gas recycling tube place
2The operation of this external material, push away the boat direction, the direction of coming out of the stove, operation sequence etc. be all identical with conventional tubular type reduction furnace, difference is that reduction rate is obviously accelerated, production efficiency increases substantially, the tungsten powder average grain diameter reduces at double.
The present invention is in the boiler tube of square-section, and malleation is for H
2The porous air cushion is to be formed by the corrosion resistant plate Combination Welding, and it highly is H=9～12mm, and length and width equate that with boiler tube inside is divided into 3-6 gas passage, and the surface has a lot of apertures, the rectangular box of outer image flat.Its closed at both ends and being screwed respectively on the boiler tube base plate, an end has total air inlet, and links with the malleation air supply system of outside.The shared cross-sectional area of porous air cushion in boiler tube: boat cross-sectional area: waste gas passing away sectional area=1.5: 3.5: 1.
Malleation at rectangle boiler tube of the present invention supplies H
2The lip-deep hole diameter of porous air cushion is 1.5～4mm, and the surperficial aperture face distribution density on low temperate zone of boiler tube and zone, middle temperate zone is 5～8 holes/dm
2Surperficial aperture face distribution density on boiler tube high temperature region is 12 ~ 18 holes/dm
2Surperficial aperture face distribution density at the boiler tube salband is 3～5 holes/dm
2In the heating warm area of boiler tube is provided with three bands can be set, the four-tape but also can be removed low, middle warm area section from until six bands, and a band high-temperature region and a cooling section only is set.
In the tee section boiler tube of garden, malleation is for H
2The porous air cushion can be made by the stainless steel tube of 1～2 garden tee section, the confession H on different warm areas
2Aperture can be that garden shape aperture also can be the cutting slotted eye of strip.Garden shape hole diameter is 1.2～2.5mm, and the width of slotted hole is that B=2mm length is 2～4mm.Perforation lines density on low temperature and the middle warm area section is 3～5 holes/dm.Perforation lines density is 4～7 holes/dm on the high temperature section.Perforation lines density is 2～3 holes/dm on the cooling section.
H used in the present invention
2The gas supply gas pressure is the stove inside and outside differential pressure, Δ P=0.003～0.005MPa.
The ground floor Porous Base of boat of the present invention is to make with 40～50 μ m stainless steel mesh cloth, can guarantee that nanometer powder can not spill under ventilative situation.
To discharge direction opposite for boat direction and the waste gas stream that pushes away of boat of the present invention, promptly advances along lighting-up tuyere or the opposite direction of exhaust gas recycling tube away from furnace gas, and finally enter water collar, can come out of the stove after the cooling.Pushing away boat mechanism can be that mechanical type or pneumatic type fluid pressure type all can.
The present invention can use the H of dew point lower (15～-20) ℃
2Gas is as reducing gas, also can use the production of conventional cracked ammonium stove and dewater with molecular sieve after (25%N
2+ 75%H
2) mist as reducing gas.
The present invention can be at 600～650 ℃, and 40～60 minutes, H
2Cross section flow Q=70～90ml/cm
2Divide H
2Atmospheric pressure Δ P=0.003-0.005MPa, boat charge are 0.65～0.7 gram/cm
2Condition under, be 50～70nm with average grain diameter, presoma amorphous tungsten oxide powder or tungsten powder once are reduced into nano-tungsten powder, its SAXS average grain diameter is 30～35.5nm, the BET specific surface is 19～23m
2/ g.
Advantage of the present invention:
1, from production equipment and technical provide a kind of can serialization the device that the oxide powder of nanometer tungsten directly is reduced into nano-tungsten powder of automation, can be used to reduce other nano metal powder simultaneously.
2, under the situation that does not adopt other working gas or aspiration pump, utilize H
2The malleation air feed of gas can be discharged product steam rapidly from the bed of material.Compare with the conventional reduction stove.At H
2Under the identical situation of atmospheric pressure, in fact the plenum system of ventilative cushion from bottom to top of the present invention has improved H local in the bed of material
2The gas dividing potential drop, thus reduction reaction speed improved, and production efficiency obviously improves.
3, the smooth eliminating of product steam, obvious suppression the tungsten powder particles phenomenon of growing up, very favourable to the production of nano-tungsten powder and other nano metal powders.
4, owing to adopted ventilative drainage type boat, thus thoroughly solved the material reduction inhomogeneous and come out of the stove before by the addiction disease of steam repeated oxidation.
5, the nano-tungsten powder of Sheng Chaning, the very narrow 45～50nm scope of average grain diameter≤35.5nm, particle diameter distribution width.
6, device structure is simple, and cost is low, promotes easily.
7, loss of material is few, the casting yield height.
Description of drawings
Fig. 1 is a kind of structural representation of the present invention, wherein pushes away boat mechanism 1, fire door 2, waste gas igniting or recovery tube 3, ventilative boat 4, nano oxidized tungsten powder 5, the ventilative base plate 6 of boat, boiler tube 7, malleation for H
2Porous air cushion 8, heating plate 9, draining gas channel 10, furnace shell 11, water collar 12, malleation air supply system 13, grate 14.
The specific embodiment
Fig. 1 is one embodiment of the present invention.
Embodiment 1
Preparation output is that 1.42 tons/month ventilated forced drainage type nano tungsten powder reducing furnace should be by following design.
1, boiler tube preparation
Cr25Ni20 heat-resistance stainless steel plate or 1Cr18Ni9Ti corrosion resistant plate with thickness δ=4.5mm, Combination Welding is made the rectangle boiler tube of two square-sections, the high H=36mm of its burner hearth cavity, the wide B=146mm of inner chamber, boiler tube heat resisting steel part length overall is 2274mm, the boiler tube in the water collar is long to be 665mm, body of heater is long to be 1824mm, boiler tube high temperature belt length is 1424mm, is made as a band heating 32KW, the long 480mm of cooling jacket.
2, malleation is for H
2The porous air cushion is that the corrosion resistant plate Combination Welding with thickness δ=1mm forms, in 5 gas passages are arranged.The height overall of porous air cushion is 9mm, and wide is 143mm, and long is 2941mm (containing the thick 2mm of flange gasket).Hole diameter φ=the 4mm on air cushion top on high temperature section, surface density is 18 holes/dm
2, hole diameter φ=2.5mm on the burner low temperature section, surface density is 8 holes/dm
2Hole diameter φ=2.5mm on the water collar section, surface density is 5 holes/dm
2
3, Double bottom permeability type boat is to make with Cr25Ni20 or the 1Cr18Ni9Ti corrosion resistant plate of thickness δ=1mm, and going to the bottom has φ=2mm aperture, and surface density is 60 holes/dm
2Upper base is to be that the stainless steel mesh cloth of 40 μ m is made with the aperture.The high H=21mm of the wide B=140mm of the long L=200mm of boat, at a distance of 5mm, so exhaust passage, top height is 6mm, clothes close, the air cushion sectional area: the boat sectional area at two the end: the relation of exhaust passage sectional area=1.5: 3.5: 1.
4, push away the boat mode for the manual boat that pushes away, go out boat by hand.
Embodiment 1 effect
The nano amorphous tungsten oxide precursor powder that adopts the hot conversion process of ullrasonic spraying to produce in the ventilated forced drainage type nano tungsten powder reducing furnace of above-mentioned design is at 600 ℃; 60 minutes; H
2Atmospheric pressure Δ P=0.005MPa; H
2The cross section flow is 90ml/cm
2Divide; H
2Gas dew point-15 ℃; Push away boat speed 7.12 boats/h; Boat charge is 0.65g/cm
2Every boat is adorned under the condition of 185g altogether, and the nano-tungsten powder SAXS average grain diameter=30.3nm of production, BET specific area are 23m
2/ g, the tungsten powder daily output (two-tube) is 47.4kg/ day, meanwhile, in order to contrast reduction effect, the malleation in above-mentioned two boiler tubes is supplied H
2The porous air cushion is removed, and changes the conventional reduction stove into, and plenum system supplies H along the boiler tube axis
2Gas.Boat changes single end into, airtight boat, in other reducing process conditions, under the identical situation, promptly identical, reduction temperature, temperature retention time of the raw meal of Shi Yonging, push away boat speed, boat charge, H
2Gas cross section flow, H
2Gas dew point, the daily output, etc. under the identical situation, the tungsten powder that restores of reduction furnace detects through XRD routinely, reduction not exclusively still contains WO
2Remaining tungsten oxide phase, and SAXS average grain diameter=198nm, BET specific surface are 2.82m
2/ g, both differ greatly, and ventilated forced drainage type nano tungsten powder reducing furnace is described, and when the reduced nano tungsten powder, its reaction speed is fast, and the efficient height can effectively stop the phenomenon of growing up of nanometer tungsten particle.Comprehensive benefit is very remarkable.The nano-tungsten powder monthly output can reach 1.42 tons/month.
Embodiment 2
Prepare a kind of garden shape boiler tube (single tube), the ventilated forced drainage type nano tungsten powder reducing furnace that has a daily output of 8.3kg/ day should be by following design.
1, boiler tube preparation
With thickness is δ=6mm, and internal diameter is the Cr25Ni20 heat-resistance stainless steel pipe of φ 70mm, and length is 2.3 meters, wherein to take length be 450mm to water collar, and body of heater is long to be 1500mm, and the high temperature belt length is 1.1 meters, heating power 10KW only establishes one section high temperate zone, can cool off two boats simultaneously in the water collar.
2, malleation is for H
2The porous air cushion is to be that the garden shape stainless steel tube of φ=12mm wall thickness δ=1.5mm is made with diameter, two stomidiums are the obstruction shape, length L=2.28 meter, and two ends is fixed on shape boiler tube bottom, garden with chuck, the air inlet mouth of pipe of air inlet port and boiler tube outside links, and fixes with dop.Hole diameter φ=the 2.5mm on air cushion top on high temperature section, line distribution density 8 holes/dm.
3, boat thickness is that δ=1mm 1Cr18Ni9Ti corrosion resistant plate is rolled into half garden tube and is welded, the nominal diameter φ=65mm in half garden, and cut along axis the bottom.Make saddle-shaped two pin and ride over porous air cushion steel pipe both sides, at the boat middle part of half garden shape, be welded with the square backing ring of stainless steel of one deck (thick 1.2mm), and stainless steel mesh compressed with another square clamping plate.Screen cloth is the stainless steel mesh cloth of 50 μ m with the aperture.Boat is long to be 220mm, and dress powder place is wide to be 60mm, and every boat can be adorned 92 gram reduction materials, can hold 5 boats in the high temperature section of boiler tube.
4, push away the boat mode for the manual boat that pushes away, go out boat by hand
Embodiment 2 effects
In the ventilated forced drainage type nano tungsten powder reducing furnace of design, the nano amorphous tungsten oxide precursor powder that adopts the hot conversion process of ullrasonic spraying to produce is at 650 ℃ in embodiment 2; 40 minutes; H
2Atmospheric pressure Δ P=0.003MPa; H
2The cross section flow is 70ml/cm
2Divide; Push away boat speed 5 boats/h (or 1 boat/12min); Boat charge is 0.7g/cm
2Every boat is reaction cartridge material 92g/ boat altogether, and the daily output can reach 8.3kg/ day nano-tungsten powder, and its SAXS average grain diameter=35.1nm, BET specific area are 19.2m
2/ g.Similar with embodiment 1, in order to contrast conventional circular single tube reduction furnace, the tungsten powder quality of reduction and granularity situation supply H with malleation
2The air cushion pipe is removed, and boat is also taked the airtight boat in single end, and under the identical situation of other reducing conditions, the tungsten powder of reduction detects through XRD, contains minute quantity WO in the tungsten powder
2SAXS average grain diameter=192nm, BET specific area are 2.78m
2/ g.
Claims (7)
1, a kind of ventilated forced drainage type tubular type reduction furnace comprises pushing away boat mechanism (1), fire door (2), waste gas igniting or recovery tube (3), ventilative boat (4), nano oxidized tungsten powder (5), the ventilative base plate (6) of boat, boiler tube (7), malleation for H
2Porous air cushion (8), heating plate (9), draining gas channel (10), furnace shell (11), water collar (12), malleation air supply system (13), grate (14); It is characterized in that: the bottom of boiler tube (7) is provided with one can malleation supply H
2The porous air cushion (8) of gas, the surface of porous air cushion (8) has a lot of apertures uniformly by different densities, be divided into uniformly in the porous air cushion (8) 3～6 road air supply channels and with each aperture UNICOM, be connected with outside malleation air supply system (13) at the right-hand member of porous air cushion, to guarantee the H of air cushion in the stove
2Air pressure falls by linear distribution; In the malleation permeability type air supply system, for H
2The direction of gas is by the boiler tube bottom vertical upwards and pass the porose boat in each bottom; On the boat structure, adopted double-deck permeability type boat, the bottom of boat is built on stilts, forms a H between ventilative base plate (6) of boat and porous air cushion (8)
2Gas is all pressed chamber, H
2Gas passes the ventilative base plate (6) of boat again after all pressing buffering; On reaction mass is placed at the bottom of the porous boat of upper strata, to guarantee the H of porous air cushion ejection
2Gas once cushions between at the bottom of first second layer boat of boat, pressure equalizing again; H from the ejection of malleation air feed porous air cushion
2Gas is by control H
2The stove inside and outside differential pressure Δ P of gas guarantees fresh H
2Gas can continuously pass the bed of material smoothly.
2, according to the described ventilated forced drainage type nano tungsten powder reducing furnace of claim 1, it is characterized in that:
A, in the boiler tube of square-section, malleation is for H
2The porous air cushion is to be formed by the corrosion resistant plate Combination Welding, and it highly is H=9～12mm, and length and width equate that with boiler tube inside is divided into 3-6 gas passage, and the surface has a lot of apertures, the rectangular box of outer image flat; Its closed at both ends and being screwed respectively on the boiler tube base plate, an end has total air inlet, and links with the malleation air supply system of outside; The shared cross-sectional area of porous air cushion in boiler tube: boat cross-sectional area: waste gas passing away sectional area=1.5: 3.5: 1.
The malleation of b, rectangle boiler tube is for H
2The lip-deep hole diameter of porous air cushion is 1.5～4mm, and the surperficial aperture face distribution density on low temperate zone of boiler tube and zone, middle temperate zone is 5～8 holes/dm
2Surperficial aperture face distribution density on boiler tube high temperature region is 12～18 holes/dm
2, be 3～5 holes/dm in the surperficial aperture face distribution density of boiler tube salband
23 bands～6 bands are set in the heating warm area of boiler tube is provided with, or a band high-temperature region and a cooling section only is set.
In c, the garden tee section boiler tube, malleation is for H
2The porous air cushion can be made by the stainless steel tube of 1～2 garden tee section, the confession H on different warm areas
2Aperture is the cutting slotted eye of garden shape aperture or strip; Garden shape hole diameter is 1.2～2.5mm, and the width of slotted hole is that B=2mm length is 2～4mm; Perforation lines density on low temperature and the middle warm area section is 3～5 holes/dm; Perforation lines density is 4～7 holes/dm on the high temperature section; Perforation lines density is 2～3 holes/dm on the cooling section.
3, according to the described ventilated forced drainage type nano tungsten powder reducing furnace of claim 1, it is characterized in that: employed H
2The gas supply gas pressure is the stove inside and outside differential pressure, Δ P=0.003～0.005MPa.
4, according to the described ventilated forced drainage type nano tungsten powder reducing furnace of claim 1, it is characterized in that: the ground floor Porous Base of boat is to be that the stainless steel mesh cloth of 40～50 μ m is made with the aperture, guarantees that nanometer powder can not spill under ventilative situation.
5, according to the described ventilated forced drainage type nano tungsten powder reducing furnace of claim 1, it is characterized in that: to discharge direction opposite for boat direction and the waste gas stream that pushes away of boat, advance along lighting-up tuyere or the opposite direction of exhaust gas recycling tube, and finally enter water collar, can come out of the stove after the cooling away from furnace gas; Pushing away boat mechanism is mechanical type or pneumatic type or fluid pressure type.
6, according to the described ventilated forced drainage type nano tungsten powder reducing furnace of claim 1, it is characterized in that; Use lower-15～-20 ℃ H of dew point
2Gas is as reducing gas, or use the production of conventional cracked ammonium stove and dewater with molecular sieve after 25%N
2Add 75%H
2Mist as reducing gas.
7, according to the described ventilated forced drainage type nano tungsten powder reducing furnace of claim 1, it is characterized in that: at 600～650 ℃, 40～60 minutes, H
2Cross section flow Q=70～90ml/cm
2Divide H
2Atmospheric pressure Δ P=0.003～0.005MPa, boat charge are 0.65～0.7 gram/cm
2Condition under, be 50～70nm with average grain diameter, presoma amorphous tungsten oxide powder or tungsten powder once are reduced into nano-tungsten powder, its SAXS average grain diameter is 30～35.5nm, the BET specific surface is 19～23m
2/ g.
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| CN102925692A (en) * | 2012-09-29 | 2013-02-13 | 崇义章源钨业股份有限公司 | Method for treating waste hard alloy |
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| CA3228734A1 (en) | 2021-10-14 | 2023-04-20 | Tino Saeuberlich | Method for producing a tungsten metal powder having a high specific surface area |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5125964A (en) * | 1990-09-10 | 1992-06-30 | General Electric Company | Fluidized bed process for preparing tungsten powder |
| DE69315935T2 (en) * | 1992-09-10 | 1998-08-27 | Kao Corp | Method and device for producing magnetic metallic particles |
| CN1126625C (en) * | 2000-04-30 | 2003-11-05 | 北京科技大学 | Preparation process of superfine carbide powder by direct reduction carbonization in pipe furnace |
| US20030121365A1 (en) * | 2001-11-20 | 2003-07-03 | Bruce Dover | Method of producing fine tungsten powder from tungsten oxides |
| CN2652567Y (en) * | 2003-09-10 | 2004-11-03 | 厦门金鹭特种合金有限公司 | Uniform flow type double layer vessel for tungsten powder reduction |
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