CN203140761U - Tantalum powder magnesium reduction and oxygen reduction device with cooler and tapered heat insulation screen - Google Patents
Tantalum powder magnesium reduction and oxygen reduction device with cooler and tapered heat insulation screen Download PDFInfo
- Publication number
- CN203140761U CN203140761U CN 201220665415 CN201220665415U CN203140761U CN 203140761 U CN203140761 U CN 203140761U CN 201220665415 CN201220665415 CN 201220665415 CN 201220665415 U CN201220665415 U CN 201220665415U CN 203140761 U CN203140761 U CN 203140761U
- Authority
- CN
- China
- Prior art keywords
- magnesium
- tantalum powder
- cooler
- reaction vessel
- pipe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The utility model discloses a tantalum powder magnesium reduction and oxygen reduction device with a cooler and a tapered heat insulation screen. The tantalum powder magnesium reduction and oxygen reduction device comprises an electric heating pit furnace and a cylindrical reaction vessel placed in the pit furnace, wherein the reaction vessel mainly comprises an inert gas intake pipe, a gas discharge pipe, a thermocouple tube and a crucible containing tantalum powder; a heater is arranged outside the reaction vessel where the crucible is arranged; the crucible is arranged at the lower part of the reaction vessel; a magnesium collector is arranged above the tantalum powder crucible; a lower heat insulation screen is arranged between the magnesium collector and the tantalum powder crucible; a cooler is arranged above the magnesium collector; an upper heat insulation screen is arranged above the cooler; the inverted tapered heat insulation screen which is at least close to the magnesium collector is arranged between the upper heat insulation screen and the magnesium collector; and the inert gas intake pipe leads to the bottom of the reaction vessel. When the tantalum powder magnesium reduction and oxygen reduction device is used for tantalum powder magnesium reduction and oxygen reduction, the loss of tantalum powder is low, the oxygen content of tantalum powder is low, and the reclaimed magnesium metal can be reused, so that environmental pollution is reduced.
Description
Technical field
The utility model relates to the utility model and relates to a kind of tantalum powder magnesium-reduced with cooler and taper heat screen and fall the oxygen device.
Background technology
The tantalum metal is a kind of rare precious metal, and its important use is to make electrolytic capacitor.The tantalum powder of using as capacitor requires very high purity.Producing Ta powder used in capacitor is normally having in the presence of the diluent salt (as NaCl, KCl and KF etc.) with sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) product that comprises tantalum powder, alkali metal and polybasic salt that obtains, its washing reclaimed obtain the tantalum powder, then carry out the pickling washing, the tantalum powder after the washing will carry out vacuum heat, just can reach for the requirement of making electrolytic capacitor.Yet because tantalum metal pair oxygen has very big affinity, the tantalum powder that makes through above-mentioned operation often contains too high oxygen, this is very disadvantageous for making electrolytic capacitor, can cause the condenser leakage current height, proof voltage is poor, handles so must fall oxygen.In addition, the oxygen that also will fall that has at the capacitor base that becomes with the tantalum powder sintering is handled.The oxygen processing falls in the general employing of the oxygen processing magnesium-reduced of falling of tantalum powder.
With the tantalum oxide (Ta in the magnesium-reduced tantalum powder
2O
5+ 5Mg → 5MgO+2Ta) variation of Gibbs free energy is as shown in table 1:
Table 1
From last table data as can be seen, to fall oxygen with magnesium-reduced be very suitable to the tantalum powder.
Based in theory tantalum powder oxygen content being reduced to 0 required amount meter, preferably use 1.1 times to the 3 times reducing agent magnesium that stoichiometry is excessive.Fall after the oxygen, used magnesium and the magnesia that forms during falling oxygen are removed with inorganic acid, preferably use in hydrochloric acid, sulfuric acid, nitric acid, the hydrogen peroxide one or more.
US Patent No. 4483819A, US4537641A have proposed the method that oxygen falls in the tantalum material, and tantalum powder and tantalum sintering are heat-treated at 600 ℃～1200 ℃ having in the presence of reducing agent such as Ca, Mg, the Al etc. soon, and the fast oxygen content of tantalum powder and tantalum sintering is reduced.
In order to effectively reduce the oxygen content of tantalum powder, to add usually based on tantalum powder oxygen content meter, add the magnesium powder of 1.5 times～3 times of stoichiometries, like this, after insulation reaction is intact, in the tantalum powder, also can remain considerable magnesium.Remaining magnesium is very unfavorable to the tantalum powder in the tantalum powder, because magnesium and oxygen have very big affinity, when the tantalum powder is come out of the stove, magnesium will even cause that the tantalum powder catches fire with oxygen kickback and heat release, and when putting into the tantalum powder that contains a large amount of magnesium in the Acidwash solution, because magnesium and dilute acid soln intense reaction also can be emitted big calorimetric, can cause also sometimes and catch fire that this is also unfavorable to environment; And tantalum powder and magnesium form Ta-Mg-O and contain water complex, cause the loss of tantalum powder when pickling, washing, and finally cause Mg, the O content height of tantalum powder.Therefore, people take when oxygen falls in magnesium-reduced to be incubated 1～3 hour under positive pressure 800 ℃～1000 ℃ elder generations in that the tantalum powder is carried out, and find time at 800 ℃～1000 ℃ then.Yet because the fusing point of magnesium is 651 ℃, boiling point is 1107 ℃, and is higher in the vapour pressure of 800 ℃～1000 ℃ of magnesium, and the vapour pressure of magnesium under some temperature sees Table 2.Magnesium unnecessary in the tantalum powder is except having small part by the absorption of tantalum powder surface, all the other major parts are present in crucible bottom with liquid form, so, as at 927 ℃, if the pressure in the reaction vessel is lower than the 134.9mm mercury column when finding time, can make liquid magnesium boiling unnecessary in the tantalum powder crucible and cause that the tantalum powder is ejected in the reaction vessel, on the heat screen, even be pumped to vacuum pipe, blocking pipe, this part the tantalum powder that can collect is also polluted, and produces serious economic loss.
Table 2 magnesium vapor is pressed the relation with temperature
| Temperature/℃ | 427 | 527 | 627 | 651 | 727 | 827 | 927 | 1027 | 1107 |
| Pressure/mm mercury column | 0.0071 | 0.148 | 1.66 | 2.63 | 8.71 | 39.8 | 134.9 | 407.4 | 760 |
The utility model content
The utility model is at the deficiencies in the prior art, provide a kind of tantalum powder loss less, tantalum powder that tantalum powder oxygen content is low falls oxygen technology and the oxygen device falls in the tantalum powder.
For achieving the above object, the utility model by the following technical solutions:
The oxygen device falls in the tantalum powder magnesium-reduced with cooler and taper heat screen, comprise electrical heating shaft furnace and the drum type brake reaction vessel that places this shaft furnace, described reaction vessel mainly includes inert gas and enters pipe, gas outlet pipe, thermocouples tube and the crucible that the tantalum powder is housed, the reaction vessel peripheral hardware having heaters at this crucible position, described crucible places the reaction vessel bottom, above the tantalum powder crucible, be provided with magnesium collecting device, following heat screen is arranged between magnesium collecting device and tantalum crucible, heat screen on having above the cooler, be provided with at least near magnesium collecting device between last heat screen and the magnesium collecting device and be inverted circular cone heat screen, described inert gas enters pipe and is passed into reaction container bottom.In the middle of the described inverted circular cone heat screen through hole, the angle of inverted conical being arranged is 170 °～120 °.
The oxygen device falls in the tantalum powder magnesium-reduced with cooler and taper heat screen of the present utility model, wherein, cooler is arranged on the top of magnesium collecting device, and the form of cooler is had no particular limits, and is to comprise that the route of cooling agent operation and cooling agent enter a kind of device of pipe and coolant discharge pipe; The route of cooling agent operation can be a plurality of annulus lines, is connected to each other; It can be spiral element; Can be that annulus or the helix tube that a plurality of diameters are different is welded on the stainless steel flat plate, be drilled with many through holes on the stainless steel flat plate; Can be to go up lower plate, sealing all around, the inside is the cooling agent running route.
Preferably, described cooler comprise cooling agent enter the operation of pipe, cooling agent pipeline and and coolant discharge pipe, the pipeline of described cooling agent operation comprises:
Manage the cooling inner coil pipe that is communicated with described entering;
Middle coil pipe, it is communicated with described cooling inner coil pipe by first tube connector;
Outer coil pipe, the one end is by second tube connector and described middle coil pipe, and the other end is communicated with described discharge pipe,
Cooling agent enters pipe from cooling agent and enters into the cooling inner coil pipe, separately two-way converges to first tube connector again, enter middle coil pipe by first tube connector, divide two-way again and be pooled to second tube connector at middle coil pipe, enter outer coil pipe then, divide two-way and be pooled to coolant discharge pipe, outside discharge pipe is discharged shaft furnace.
Cooler can use the material manufacturing of corrosion-and high-temp-resistant, considers from the angle that economy is used, and can make with stainless steel or nickel material; Consider the collection of magnesium, cooler radially little than magnesium collecting device internal diameter, preferred little 1～20cm, the bottom of cooler is 0～3cm from the distance that goes up most a magnesium collecting device upper edge.
The oxygen device falls in the tantalum powder magnesium-reduced with cooler and taper heat screen of the present utility model, shape for magnesium collecting device has no particular limits, for the drum type brake reaction vessel, preferred magnesium collecting device is one and comprises chassis and sidewall upper shed disk, more preferably a plurality of chassis and sidewall upper shed disks of comprising stack up and down, these magnesium collecting device disks are in different positions, when the circulation inert gas, the temperature difference of each magnesium collecting device can be collected the magnesium that evaporates up condensation from the reaction vessel bottom effectively.
The oxygen device falls in described tantalum powder magnesium-reduced with cooler and taper heat screen, in order to collect the steam magnesium that rises from reaction container bottom effectively, the diameter of preferred magnesium collecting device disk is less than the about 10～20cm of reaction vessel internal diameter, and its upper edge is 2～5cm to the degree of depth of bottom.The material of making magnesium collecting device is had no particular limits, consider from economical and practical angle, can make with 2～4mm thick corrosion resistant plate or nickel plate.
The oxygen device falls in the tantalum powder magnesium-reduced with cooler and taper heat screen of the present utility model, has a temperature measuring equipment at least between the magnesium collecting device outside and reaction vessel inwall, is used for measuring the temperature at magnesium collecting device position.
The oxygen device falls in the tantalum powder magnesium-reduced with cooler and taper heat screen of the present utility model, wherein the upper edge of the superiors' tantalum powder crucible is from the about 10cm～20cm of distance at the end of the most next magnesium collecting device, 1～3 layer of heat screen arranged below magnesium collecting device, to ensure the small distance between tantalum powder crucible and magnesium collecting device bigger temperature difference is arranged; Cooler is arranged above magnesium collecting device, 2～4 layers of heat screen are arranged above cooler, the diameter of heat screen is less than reaction vessel internal diameter 2～4cm; Reach the 4～10cm that is spaced apart of heat screen and magnesium collecting device between the heat screen.
Like this, at high temperature, when inert gas is passed into reaction container bottom and circulates, cool off cooler with coolant flow simultaneously, inert gas flows from bottom to up, unnecessary magnesium volatilization in the tantalum powder in the tantalum powder crucible under the high temperature, magnesium steam rises along with the air-flow that rises, when magnesium steam rises to the position of magnesium collecting device, the device that is cooled cooling, the magnesium devaporation becomes liquid magnesium, drops onto in the magnesium collecting device.
The beneficial effects of the utility model are: device of the present utility model is simple, transforms a little to get final product on original device basic, implements easily; Use device of the present utility model to carry out the magnesium-reduced of tantalum powder and fall oxygen, tantalum powder loss is few, and tantalum powder oxygen content is low, and the magnesium metal of recovery can recycling, reduces the pollution to environment.
Description of drawings
Fig. 1 is that oxygen device schematic diagram falls in the magnesium-reduced of the utility model tantalum powder.
Fig. 2 is the E_E sectional top view of Fig. 1.
Fig. 3 is that oxygen device schematic diagram falls in the magnesium-reduced of prior art tantalum powder.
To be the utility model fall oxygen is passed to D between the outside, magnesium collecting device middle part that outage measures and reaction vessel inwall from inert gas variations in temperature in the magnesium-reduced of tantalum powder to Fig. 4.
The specific embodiment
Fig. 1 shows the tantalum powder magnesium-reduced of the utility model use and falls the oxygen device, it comprises shaft furnace 14, the bottom heater 141 that the bottom is made up of resistance wire in the burner hearth, the sidewall heater 142 that the cylinder side wall that makes progress from the bottom is made up of 6 sections resistance wires, the top of sidewall heater strip topmost are higher than in the reaction vessel the last layer tantalum powder crucible about 8cm in upper edge;
When carrying out the magnesium-reduced of tantalum powder and fall oxygen, pack into 16 li of tantalum crucibles of the high tantalum powder 17 of the oxygen that is mixed with the magnesium powder, tantalum crucible 16 is placed on the bin 15, then the bin 15 that the tantalum powder crucible is housed is put into the bottom that internal diameter is about the drum type brake reaction vessel 10 of 80cm, drum type brake reaction vessel 10 is placed 14 li of shaft furnaces, and its pallet 12 is seated on the shaft furnace.
The top of reaction vessel 10 is reaction vessel lids 11, and reactor cap 11 has cooling water ring (not shown) corresponding to the sealing ring position on reaction vessel 10 upper flanges; Be provided with at reaction vessel lid 11 find time, blast pipe 20(valve, threeway be not shown), have from the inert gas that is deep into reaction container bottom near the reaction vessel perisporium and enter pipe 19, an end that enters pipe connection inert gas source at inert gas is connected with gas flowmeter 191, and the gas that charges into air (or nitrogen) enters pipe 21; The pressure vacuum ga(u)ge 22 of assaying reaction container inner pressure; Be deep at least 4 thermocouples tube 23A, 23B, 23C and the 23D(Fig. 2 of different depth in the reaction vessel from the same circumference of reaction vessel lid near the reaction vessel perisporium), measure the temperature as 4 positions of A, B, C and the magnesium collecting device disk periphery D different depth of tantalum powder crucible periphery among Fig. 1 respectively; With connecting rod 184 and sleeve pipe last heat screen 181, magnesium collecting device 24 and following heat screen 182 are connected to reaction vessel and cover, wherein on stacked above the magnesium collecting device 24 diameter of heat screen 181 less than reaction vessel internal diameter 5cm, be provided with inverted circular cone heat screen 183 under the last heat screen 181, it is inverted circular cone heat screen 183 near magnesium collecting device 24, circular cone heat screen 183 centers have and are about the manhole that diameter is 6cm, so that the liquid magnesium that makes magnesium vapor run into heat shielding 181 condensations flow into 24 li of magnesium collecting devices, two stacked following heat screens 182 are arranged below magnesium collecting device, its diameter is identical with the magnesium collecting device diameter, the spacing that reaches between heat screen and magnesium collecting device disk between the heat screen is about 6cm, wherein the upper edge of magnesium collecting device disk is about 4cm to the degree of depth of bottom, the about 6cm of spacing between the magnesium collecting device disk, magnesium collecting device disk periphery and the about 8cm of reaction vessel inwall spacing, the bottom of the disk of the bottom of magnesium collecting device is about 12cm from the upper edge of the superiors' tantalum powder crucible; Above magnesium collecting device, be provided with cooler 25, Fig. 2 represents that cooling agent is in the flow direction of 25 li in cooler, cooling agent enters pipe 253 and puts in the reacting furnace 10 from reaction bell 11, cooling agent enters pipe 253 from cooling agent and enters into cooling inner coil pipe 256, separately two-way converges to tube connector 255 again from 256, enter middle coil pipe 251 by tube connector 255, divide two-way again and be pooled to another tube connector 255 at middle coil pipe, enter outer coil pipe 252 then, divide two-way and be pooled to coolant discharge pipe 254, discharge out of the furnace from discharge pipe 254.The external diameter of outer coil pipe is than the approximately little 18cm of magnesium collecting device internal diameter, and the most next heat screen of heat screen bottom on it, cooling coil top is 6cm.
Like this, cover lower side position from tantalum powder crucible position to reaction vessel in reaction vessel interior, form one from top to bottom high temperature to the thermograde of low temperature, temperature in the tantalum crucible position is reaction temperature (as 920 ℃), position between the outside of magnesium collecting device and reaction vessel inwall, temperature is about 600 ℃～800 ℃; And, when circulation cooling agent in condenser, on the plane of cooler, near the reaction vessel inwall in be formed centrally by the thermograde of high temperature to low temperature, like this, the magnesium steam that vaporization at high temperature comes out from the tantalum powder of bottom will arrive the height of condenser from bottom to top, promptly be condensed into liquid magnesium at cooler, drop onto in the magnesium collecting device; When circulating cooling agent in the cooler, the temperature of covering lower side position at reaction vessel is lower than 120 ℃; When not circulating cooling agent, the temperature of reaction vessel lid lower side position is lower than 200 ℃; The magnesium vapour concentration is very low in the gas that the reactor cap bottom is discharged or extracted out.
The utility model also provides the magnesium-reduced of a kind of tantalum powder to fall the method for oxygen, and this method comprises: the high tantalum powder of oxygen is mixed with the magnesium powder of the 1wt%～3wt% of tantalum powder, in the tantalum crucible in the reaction vessel of packing into, the reaction vessel that the tantalum powder is housed is hung in the shaft furnace; Charge into inert gas after reaction vessel found time, in inert atmosphere, pressure is that 0.1～0.2MPa is heated to 800～1000 ℃ and kept 30 minutes～2 hours, and in this step, oxygen reacts in magnesium and the tantalum powder, removes the oxygen in the tantalum powder;
Then, cooling agent circulates in cooler, at A, the tantalum powder crucible position of B and C is 800～1000 ℃, under about 0.1MPa pressure, with inert gas circulation reaction vessel 30 minutes～2 hours, the velocity of liquid assets of inert gas was 10 liters/minute～300 liters/minute, in the meantime, oxygen in magnesium continuation and the tantalum powder reacts, and, because a lasting ascending air is arranged, at tantalum powder crucible position temperature height, magnesium in the tantalum powder in the crucible has higher magnesium vapor presses, and magnesium steam arrives magnesium collecting device top along with ascending air, run into cooler, the temperature here is between 600 ℃～800 ℃, and magnesium steam condenses into liquid rapidly, drops onto in the magnesium collecting device.Wherein the time to the inert gas circulation does not have strict restriction, can according to the tantalum powder of packing in tantalum powder temperature height and the reaction vessel how much, coolant flow speed in the cooler and temperature, what excessive and inert gas circulation speed decides to add the magnesium stoichiometry, general temperature is more high, magnesium vapor is pressed more high, and the inert gas circulation time can be shorter; The heat that the cooler unit interval is taken away is many, and row's magnesium time is short, and inert gas flow is big, and row's magnesium time is short, if excessive magnesium total amount is many in the reaction vessel, Liu Tong time will suitably lengthen so; General circulation 0.5 hour to 2 hours is behind the inert gas that goes into circulation, under the temperature-resistant situation in control tantalum powder crucible position, the magnesium vapor stream that rises takes heat to top, magnesium collecting device position temperature is raise, and still one works as the cooling agent that circulates in the cooler, and temperature just descends rapidly;
After the most of magnesium evaporation in the tantalum powder, stop the circulation of cooling agent in the cooler, the temperature at magnesium collecting device position can return to the temperature that approaches when beginning to carry out the inert gas circulation again, and at this time, the liquid magnesium of the cohesion in the tantalum powder is evaporated completely basically;
Through the inert gas circulation, definite unnecessary liquid magnesium be discharged from basically collect magnesium collecting device after, discharge duct is connect vavuum pump finds time to reduce pressure, the phenomenon that the magnesium spray is taken the tantalum powder out of crucible at this time can not appear, find time is to be 800～1000 ℃ to keep 30 minutes～1 hour at A, B and C place, pressure reaches below about 300Pa, is enough to like this make that the magnesium that is adsorbed on tantalum powder surface also can be taken away;
Continue to find time, coolant flow is stopped, improving the temperature of cooler, the solid-state magnesium fusing that condenses in above the cooler is dropped onto in the magnesium collecting device;
Then, with the cooling of the tantalum powder in the reaction vessel, the magnesium in the magnesium collecting device is collected in discharging after the passivation, and reaction vessel is cleaned, dries together with magnesium collecting device, and next time is stand-by.The tantalum powder is carried out pickling, the oven dry of washing final vacuum, the tantalum powder of the oxygen that has been reduced.
Fig. 3 is that the oxygen device falls in the magnesium-reduced of the employed tantalum powder of prior art, with the utility model tantalum powder magnesium-reduced fall the oxygen device different be drum type brake reaction vessel upper periphery cooling water jecket 13, it comprises water inlet pipe 131 and outlet pipe 132.Have only heat screen above the tantalum powder crucible, do not have magnesium collecting device and cooler, inert gas enters the following position that pipe only is deep into the reaction vessel lid, is not deep into reaction container bottom.
The oxygen that falls of prior art tantalum powder is to carry out in device as shown in Figure 3, to contain the high tantalum powder of oxygen mixes the back and forms and to contain pack into 16 li of tantalum crucibles of magnesium tantalum powder 17 with a certain amount of magnesium powder, find time after adding a cover 11 sealings, charge into argon gas then, by resistance heater 141 and 142 A, B and C place temperature are heated to 800 ℃～1000 ℃ 14 li of shaft furnaces, " vexed jar " insulation in the inert gas atmosphere and/or under the vacuum 2～6 hours, cool to room temperature then, carry out coming out of the stove after the passivation and carry out the pickling washing, oven dry obtains falling oxygen tantalum powder.Between soak, magnesium volatilization in the tantalum powder, magnesium steam rises, and runs into the lower heat screen of temperature and reactor vessel wall, has only small amount of magnesium steam to condense upon on the heat screen with solid-state magnesium, a large amount of magnesium steam condense upon on the heat screen with liquid magnesium and the reaction vessel inwall on, drippage goes down again, continues volatilization, like this, circulation repeatedly hinders the magnesium volatilization in the tantalum powder.
Embodiment
Be the tantalum powder of 6800ppm with the 100kg oxygen content, add 2000 gram magnesium powder, (based in theory oxygen in the tantalum powder all being removed, residue magnesium 980 grams after reaction is finished, need restrain-in fact can not all remove the oxygen in the tantalum powder with magnesium 1020), magnesium powder and tantalum powder are mixed, be respectively charged into 16 li of 10 tantalum crucibles, pack into as described in Figure 1 10 li of reaction vessels of the crucible 16 usefulness bins 15 that the tantalum powder of sneaking into magnesium is housed, reaction vessel 10 is hung in 14 li of shaft furnaces, be evacuated to about 200Pa from exhaust outlet 20, after stopping to find time argon gas is filled into 10 li of reaction vessels from pipeline 19, make 10 li pressure of reaction vessel remain on 0.11MPa～0.14MPa, A, B and C place temperature are warmed up to 920 ℃, are incubated 1.5 hours; Then open argon gas circulation valve, make the argon gas flow velocity remain on 20～60 liters/minute with flowmeter 191, and open air bleeding valve 20, the about 0.1MPa of reaction vessel internal pressure; Open advancing of cooler, outlet valve, enter pipe 253 with chilled nitrogen from cooling agent and enter inner coil pipe 256, through 255 to middle coil pipe 251, arrive outer coil pipe 252 again, discharge from coolant discharge pipe 254 then, meanwhile, keep A, about 920 ℃ of B and C place temperature, by flowmeter 191, enter pipe 19 from argon gas and enter into reactor bottom, discharge circulation argon gas 90 minutes from the exhaust outlet 20 of loam cake, close the argon gas inlet port then, air bleeding valve 20 is connect vavuum pump, found time 30 minutes, allow cooling agent continue in 25 li circulations of cooler simultaneously, the reaction vessel internal pressure is lower than 300Pa, A, about 920 ℃ of B and C place temperature; Then, stop cooling agent and flow for 25 li at cooler, continued to find time 30 minutes, keep about 920 ℃ of A, B and C place temperature, make that the solid-state magnesium on the cooler is melted into liquid magnesium, flow to 24 li of magnesium collecting devices; Show from circulation during inert gas finishes to finding time as Fig. 4, D place variations in temperature between magnesium collecting device middle part magnesium collecting device periphery and reaction vessel inwall stops after finding time to finish heating, and charges into argon gas, makes the reaction vessel internal pressure remain on 0.11～0.14MPa; A, B and C place are cooled near room temperature, enter pipe 21 from gas and slowly charge into air and carry out passivation, then the tantalum powder from 11 li taking-ups of reaction vessel, do not find not have tantalum powder ejection phenomenon.Simultaneously the magnesium in the magnesium collecting device is collected, the tantalum powder is carried out pickling, do not have the intense reaction phenomenon, the tantalum powder is washed neutrality with deionized water, then vacuum drying again through pernitric acid-aqueous hydrogen peroxide solution washing, obtain tantalum powder 99.7kg, the oxygen content of tantalum powder is 3300ppm, and content of magnesium is lower than 3ppm.Collect magnesium 653 grams.
Comparative example 1
With the tantalum powder 100kg identical with embodiment, the same 2000 gram magnesium powder that add, use reaction vessel as shown in Figure 3, after the shove charge reaction vessel is hung in 10 li of shaft furnaces, charge into argon gas after finding time, at 0.11MPa～0.14MPa, intensification makes A, about 920 ℃ of B and C place temperature, be incubated 4 hours, the cooling that has a power failure, cooling back and embodiment 1 carry out passivation equally, then the tantalum powder is taken out in reaction vessel, the tantalum powder is when carrying out pickling, owing in the tantalum powder more residue magnesium is arranged, beginning has intense reaction, and the plain soup phenomenon arranged, obtain tantalum powder 99.1kg after the washing oven dry, the oxygen content of tantalum powder is 3800ppm, and content of magnesium is 6ppm.
Comparative example 2
With the tantalum powder 100kg identical with embodiment, the same 2000 gram magnesium powder that add, use reaction vessel as shown in Figure 3, after the shove charge reaction vessel is hung in 10 li of shaft furnaces, charge into argon gas after finding time, at 0.11MPa～0.14MPa, be warmed up to 920 ℃, be incubated 2 hours, find time from blast pipe 20 then, found time 2 hours 920, the cooling that has a power failure, cooling back and embodiment 1 carry out passivation equally, then the tantalum powder is taken out in reaction vessel, find that on the heat screen, evacuation tube has the tantalum powder in the reaction vessel, collect the tantalum powder 1.1kg of pollution, tantalum powder in the tantalum powder crucible is carried out pickling, obtain tantalum powder 96.4kg after the washing oven dry, the oxygen content of tantalum powder is 3420ppm, and content of magnesium is 3ppm.
Can fully understand superiority of the present utility model from above example, the utility model also is fit to the oxygen that falls of niobium powder to be handled.
The above, it only is preferred embodiment of the present utility model, be not that the utility model is done any pro forma restriction, any those skilled in the art, in not breaking away from the technical solutions of the utility model scope, make many changes or be modified to the equivalent example of equivalent variations when the technology contents that can utilize above-mentioned announcement, all still belong in the new technical scheme scope of the utility model.
Claims (4)
1. the oxygen device falls in the tantalum powder magnesium-reduced that has cooler and taper heat screen, comprise electrical heating shaft furnace and the drum type brake reaction vessel that places this shaft furnace, described reaction vessel mainly includes inert gas and enters pipe, gas outlet pipe, thermocouples tube and the crucible that the tantalum powder is housed, the reaction vessel peripheral hardware having heaters at this crucible position, it is characterized in that: described crucible places the reaction vessel bottom, above the tantalum powder crucible, be provided with magnesium collecting device, following heat screen is arranged between magnesium collecting device and tantalum crucible, above magnesium collecting device, be provided with cooler, heat screen on having above the cooler, be provided with between last heat screen and the magnesium collecting device near magnesium collecting device and be inverted circular cone heat screen, described inert gas enters pipe and is passed into reaction container bottom.
2. the oxygen device falls in the tantalum powder magnesium-reduced with cooler and taper heat screen according to claim 1, it is characterized in that, in the middle of the described inverted circular cone heat screen through hole, the angle of inverted conical being arranged is 170 °～120 °.
3. the oxygen device falls in the tantalum powder magnesium-reduced with cooler and taper heat screen according to claim 1, it is characterized in that, described cooler comprises that cooling agent enters pipeline and the coolant discharge pipe of pipe, cooling agent operation, and the pipeline of described cooling agent operation comprises:
Manage the cooling inner coil pipe that is communicated with described entering;
Middle coil pipe, it is communicated with described cooling inner coil pipe by first tube connector;
Outer coil pipe, the one end is communicated with described middle coil pipe by second tube connector, and the other end is communicated with described discharge pipe,
Cooling agent enters pipe from cooling agent and enters into the cooling inner coil pipe, separately two-way converges to first tube connector again, enter middle coil pipe by first tube connector, divide two-way again and be pooled to second tube connector at middle coil pipe, enter outer coil pipe then, divide two-way and be pooled to coolant discharge pipe, outside discharge pipe is discharged shaft furnace.
4. the oxygen device falls in each described tantalum powder magnesium-reduced with cooler and taper heat screen according to claim 1～3, it is characterized in that having a temperature measuring equipment at least between the magnesium collecting device outside and reaction vessel inwall.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220665415 CN203140761U (en) | 2012-12-05 | 2012-12-05 | Tantalum powder magnesium reduction and oxygen reduction device with cooler and tapered heat insulation screen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220665415 CN203140761U (en) | 2012-12-05 | 2012-12-05 | Tantalum powder magnesium reduction and oxygen reduction device with cooler and tapered heat insulation screen |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN203140761U true CN203140761U (en) | 2013-08-21 |
Family
ID=48968317
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201220665415 Expired - Fee Related CN203140761U (en) | 2012-12-05 | 2012-12-05 | Tantalum powder magnesium reduction and oxygen reduction device with cooler and tapered heat insulation screen |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN203140761U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112276079A (en) * | 2020-06-22 | 2021-01-29 | 江门富祥电子材料有限公司 | Device and method for sintering tantalum briquette and removing binder |
-
2012
- 2012-12-05 CN CN 201220665415 patent/CN203140761U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112276079A (en) * | 2020-06-22 | 2021-01-29 | 江门富祥电子材料有限公司 | Device and method for sintering tantalum briquette and removing binder |
| CN112276079B (en) * | 2020-06-22 | 2021-09-10 | 江门富祥电子材料有限公司 | Device and method for sintering tantalum briquette and removing binder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102923699B (en) | Continuous pyrographite purifying device | |
| CN103084568B (en) | Device used for reducing tantalum powder by using magnesium to reduce oxygen content and provided with cooler and method for reducing tantalum powder by using magnesium to reduce oxygen content | |
| CN105817461B (en) | A kind of device of waste and old circuit board electronic component high added value recycling | |
| CN101999005A (en) | Vacuum circulation molten state silicothermic method for producing magnesium and equipment thereof | |
| CN203227818U (en) | Device for magnesium reduction and deoxidization on tantalum powder with cooler | |
| CN102965525B (en) | Device and method for carrying out magnesium reduction and deoxidization on tantalum powder | |
| CN105970004A (en) | Vacuum induction furnace magnesium smelting system and magnesium smelting method thereof | |
| CN203140761U (en) | Tantalum powder magnesium reduction and oxygen reduction device with cooler and tapered heat insulation screen | |
| CN206418169U (en) | A kind of many metal distillation temperature control condensed components evaporate single crude product vacuum drying oven | |
| CN203245360U (en) | A device used for reducing tantalum powder by using magnesium to reduce oxygen content and provided with conic heat shields | |
| CN202954080U (en) | Magnesium reduction and deoxygenation device of tantalum powder | |
| CN102706144A (en) | Fractional condensation vacuum furnace | |
| CN104325149A (en) | Device and method for adopting electronic reaction beam for making ultrafine metal powder | |
| CN203124743U (en) | Magnesium reduction and deoxygenation device of tantalum powder with inverted cone-shaped heat insulation screen | |
| CN207402110U (en) | A kind of plating cadmia melting continuously zinc powder furnace | |
| CN103937999B (en) | A kind of vacuum distilling ferromanganese extracts method and the device of manganese metal | |
| CN102787246B (en) | Smelting production method and device of antimony trioxide | |
| CN206089779U (en) | Vacuum induction furnace magnesium production system | |
| CN209549735U (en) | Can go out the cyclone dust collectors of flame | |
| CN107218809A (en) | A kind of many metal distillation temperature control condensed components evaporate single crude product vacuum drying oven | |
| CN204898031U (en) | A condenser for thick cadmium vacuum distillation | |
| CN203642666U (en) | High-temperature hydrogen sintering furnace | |
| CN209555329U (en) | Heated by electrodes vacuum distillation furnace | |
| CN103146933A (en) | Method for separating and recycling zinc from secondary zinc resource by using distilling-condensing device | |
| CN104911518A (en) | Heat treatment method of high-performance tungsten-based high-proportion alloy products |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130821 Termination date: 20211205 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |