CN104801725A - Reaction device for reducing potassium fluotantalate by sodium and method for manufacturing tantalum powder by reaction device - Google Patents
Reaction device for reducing potassium fluotantalate by sodium and method for manufacturing tantalum powder by reaction device Download PDFInfo
- Publication number
- CN104801725A CN104801725A CN201510253215.9A CN201510253215A CN104801725A CN 104801725 A CN104801725 A CN 104801725A CN 201510253215 A CN201510253215 A CN 201510253215A CN 104801725 A CN104801725 A CN 104801725A
- Authority
- CN
- China
- Prior art keywords
- sodium
- pipe
- tantalum powder
- reaction vessel
- potassium
- 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.)
- Granted
Links
Abstract
The invention discloses a device for reducing potassium fluotantalate by sodium. The device comprises a reaction container and a reaction container cover which is in matched sealing with the reaction container; a sodium collecting device is arranged below the reaction container cover; a cooler is arranged at the position, corresponding to the sodium collecting device, on the reaction container cover. The invention further discloses a method for producing tantalum powder by using the device. The device and the method disclosed by the invention are safe and reliable; the tantalum powder produced by reducing the potassium fluotantalate by the sodium is low in impurity content.
Description
Technical field
The present invention relates to the process units of tantalum powder, particularly a kind of reaction unit of the sodium reduction potassium floutaramite with collection sodium device and the method with described device production tantalum powder.
Background technology
The fusing point of metal tantalum is high, steam forces down, cold-forming property is good, chemical stability is high, anti-liquid metal and acid and alkali corrosion ability strong, surface film oxide dielectric constant values is high, metal tantalum and alloy thereof are important functional materials, have important use at the industrial departments such as electronics, integrated circuit, iron and steel, metallurgy, chemical industry, carbide alloy, atomic energy, space flight and aviation and the technical field such as strategic arms, medicine equipment.High-purity is required, especially for electrolytic capacitor and sputter tantalum target in the application of tantalum.
The production of tantalum powder generally adopts the method for sodium reduction potassium floutaramite.
Sodium metal reduction potassium floutaramite, its chemical equation is:
K
2TaF
7+Na＝Ta+2KF+5NaF (1)
In above formula, sodium metal also can use metallic potassium or sodium-potassium-sodium alloy.
Sodium reduction potassium floutaramite produces tantalum powder, has disclosed multinomial technology, makes diluent, preparing tantalum powder by stirring sodium and reducing potassium fluotantalate as US Patent No. 3829310 proposes with sodium chloride; US4149876 notes sodium and stirs and reduce after alkali metal and potassium floutaramite melting, blows cooling to reaction vessel simultaneously; US5442978 discloses by high diluent ratio, adds solid metal sodium reduction, utilizes the heat that the high thermal capacity of sodium metal is released to absorb reduction reaction.
In the process of actual production tantalum powder, in order to obtain the tantalum powder of relatively fine particle, add diluent in the feed, as sodium chloride, potassium chloride, potassium fluoride and grain refiner etc.The product be obtained by reacting is the coagula of the melt parcel tantalum powder of sodium chloride, potassium chloride, potassium fluoride and sodium fluoride.This coagula of usual pure water soaking and water washing, makes tantalum powder be separated with sodium chloride, potassium chloride, potassium fluoride and sodium fluoride and obtains tantalum powder.
When sodium reduction potassium floutaramite, if the sodium quantity not sufficient added, a small amount of potassium floutaramite will be had not to be reduced, and the yield of metal tantalum is low, and such obtained tantalum powder oxygen content is high, and potassium, sodium content are also high.In order to make above-mentioned reacting completely, improving the yield of metal tantalum, often excessively will add sodium metal.After sodium reduction potassium floutaramite has carried out, superfluous sodium metal is actually and is present in product with the form of sodium-potassium eutectic.When reduzate is washed, the tantalates of potassium sodium and/or inclined tantalates can be produced.Particularly when producing the tantalum powder of high-specific surface area, because the specific area of tantalum powder is high, in strong alkali solution, producing a large amount of tantalates and/or inclined tantalates, so just cause the loss of tantalum metal, and oxygen content and the potassium sodium content of tantalum powder being high.The high container to manufacturing tantalum of potassium sodium content of tantalum powder is very unfavorable, the leakage current of tantalum capacitor can be made to increase, still require that potassium sodium content is low just like the tantalum powder of the sputter tantalum target for microelectronic.
And, to environment in the toxic emission containing alkali metal vapour to air.When washing the product of strong basicity sodium reduction potassium floutaramite, use a large amount of water, a large amount of waste water containing alkali also can to environment.
CN101879603 discloses a kind of method that sodium reduction potassium floutaramite manufactures minuteness particle tantalum powder, this method can reach the object reducing tantalum powder potassium sodium content, but owing at high temperature finding time to the reaction vessel after sodium reduction, high-temperature sodium steam is gone out in a large number under decompression suddenly, and because sodium vapor temperature is high, thermal capacity is large, taking a large amount of heat out of makes pipeline, valve all redden heat, valve inconvenience opens and closes, and sometimes also occurs blocking and sodium vapor leakage phenomenon, occurs safety problem.
Summary of the invention
In view of the problems referred to above of the prior art, an object of the present invention is to provide a kind of device of sodium reduction potassium floutaramite.Another object of the present invention is to provide a kind of method of producing tantalum powder.
For achieving the above object, the present invention is by the following technical solutions:
A kind of device of sodium reduction potassium floutaramite, comprise reaction vessel and be mated the container cover of sealing, by the through hole in described container cover, described container cover is provided with stirring arm, thermocouple, sodium injection tube, charge pipe, inert gas inleting pipe, downtake pipe and second exhaust pipe, also comprise: collection sodium device, be located at below described container cover, be provided with bottom described collection sodium device and put sodium pipe, cooler, be located at above described collection sodium device, this cooler has coolant inlet pipe, coolant outlet pipe and coolant flow channel.
Further, described inert gas inleting pipe extends in reaction vessel until sodium reduction reacts the height of on the rear liquid level containing the melt of tantalum powder about 5-15 centimetre.
Further, described inert gas inleting pipe extends in reaction vessel the degree of depth extending under the rear liquid level containing the melt of tantalum powder of sodium reduction reaction about 10-25 centimetre.
Further, described downtake pipe is arranged in described cooler area, and it is overseas that second exhaust pipe is arranged on described cooler zone.
Further, described downtake pipe is arranged in the cooler area of container cover, be placed in coolant inlet pipe and coaxially arrange with coolant inlet pipe, the length at least 15 centimetres of described downtake pipe and coolant inlet pipe coaxial parts, it is overseas that second exhaust pipe is arranged on described cooler zone, and it is near the marginal position of described container cover.
A kind of method utilizing said apparatus to produce tantalum powder comprises step:
1) using Fluoride for Raw Material potassium tantalate be selected from as in sodium chloride, potassium chloride, potassium fluoride, the alkali metal salt of at least one joins in reaction vessel as diluent, argon gas circulation heating is filled with after finding time, inert gas enters reaction vessel from gas tube, by the blast pipe exhaust outside cooler, circulate with the inert gas of 0.1-10 liter/min of flow;
2) by the above-mentioned reaction vessel heating that raw material is housed, material is melted, to 800 DEG C-1050 DEG C, stirs the material of fusing, injection liquid metal sodium makes sodium metal and potassium floutaramite react and generates tantalum powder;
3) row's sodium is carried out after having reacted: passed into by cooling agent in cooler and circulate, constantly inert gas is passed in reactor simultaneously, pressure in reactor is made to remain on 0.1 ~ 0.11MPa, by being in the blast pipe exhaust in cooler, gas outflow is 0.1 liter/min-5 liters/min, at least keeps 30 minutes-3 hours the temperature of 880 DEG C or more; Then make pressure in reactor remain on 0.1 ~ 0.11MPa, gas flow is 5 liters/min-50 liters/min, keeps 30 minutes-2 hours the temperature of 880 DEG C or more, makes to be gasified totally in fact containing the sodium metal in the melt of tantalum powder, is collected in collection sodium device;
4) by product cool to room temperature, reaction vessel lid being hung out, releasing liquid metal sodium from putting sodium pipe; Product in reaction vessel is taken out carry out washing, pickling, oven dry.
Further, step 3) described in sodium metal comprise sodium-potassium-sodium alloy.
Further, it is characterized in that step 3) row's sodium temperature be 880 DEG C-1050 DEG C
According to the present invention, there is following beneficial effect:
(1) according to the present invention, the tantalum powder impurity content that sodium reduction potassium floutaramite is produced is low, can be used as powder metallurgy sputter tantalum target and from the specific volume 3000 μ FV/g for high voltage to the Ta powder used in capacitor of each grade of low voltage Fabrication of High Specific Capacitance 150000 μ FV/g.
(2) according to the present invention, the method safety that sodium reduction potassium floutaramite produces tantalum powder is reliable.
(3) according to the present invention, sodium reduction potassium floutaramite production tantalum powder can reduce the pollution to air, reclaims alkali metal recycling, reduces production cost.
Accompanying drawing explanation
Fig. 1 is the reaction unit schematic diagram of sodium reduction potassium floutaramite of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing and preferred embodiment, the present invention will be further described.
In this manual, unless otherwise expressly noted, unit ppm refers to " 1,000,000/" that represent with mass ratio.
Cooling agent described in this description, comprises gaseous coolant and liquid coolant, as inert gas, nitrogen, air, water and the aqueous solution, cold oil or their mixture.Circulation cooling agent also can first circulated gases cooling agent, then circulating liquid cooling agent, or first circulating liquid cooling agent, then circulated gases cooling agent.
Fig. 1 is the schematic diagram of the reaction unit example of a sodium reduction potassium floutaramite of the present invention, well formula reduction furnace 1 li for the heating of sodium reduction reactor has resistance heater 2, reduction furnace is generally provided with the temperature that exhausting cooling device is used for reducing exothermic heat of reaction rising, the not shown exhausting cooling device of Fig. 1.According to the present invention, the reaction unit of sodium reduction potassium floutaramite comprises reaction vessel 3, reaction vessel lid 31; Described reaction vessel lid 31 is provided with sodium injection tube 5, adds the feed pipe 11 of the raw materials such as potassium floutaramite, thermocouples tube 8, inert gas plenum pipe 4, cooler 6 and the paddle 10 that passes from cooler center.
As shown in Figure 1, inert gas plenum pipe 4 wherein extends to the degree of depth certain in reaction vessel, to make Na-K alloy unnecessary in melt under inert gas flow drives after sodium reduction reaction, be removed fully, an example is the position that gas tube 4 is deep into about 6 centimetres on fused salt 12 liquid level containing tantalum powder after whole potassium floutaramite has reacted.
As shown in Figure 1, reaction vessel lid 3-1 is also provided with blast pipe 71 and blast pipe 72, blast pipe 71 is in cooler 6 region, and described blast pipe 72 is outside described cooler 6 region; Wherein, blast pipe 72 is arranged on the edge of reaction vessel lid, is provided with coolant seal circle (not shown in figure 1) around blast pipe 72, cooling water is wherein had to circulate, before reduction reaction and between the stage of reaction, close blast pipe 71, open blast pipe 7-2 and be vented; During note sodium reduction, even if there is a small amount of sodium vapor to enter blast pipe 72, after the water quench that also can be cooled in sealing ring, be back to reaction vessel 3 li.
As shown in Figure 1, in coolant inlet pipe 61, coaxial setting is deep in reactor 3 blast pipe 71 with coolant inlet pipe 61, the length about 20 centimetres of blast pipe 71 and coolant inlet pipe 61 coaxial parts; At potassium floutaramite by Restore All reacted row's sodium process, close blast pipe 72, be vented with blast pipe 71, make sodium vapor by liquefaction instillation collection sodium device 9 li fully cooled during blast pipe 71.
As shown in Figure 1, a collection sodium device 9 is hung in the below of described reaction vessel lid 31, collection sodium device 9 comprises the bottom surface sections of a ring-type, the container that the outer cylinder that inner cylinder and be connected with plane perpendicular and with bottom surface inner ring is connected with plane perpendicular and with bottom surface outer shroud forms, the shape size of collection sodium device is had no particular limits, as long as just passable containing the remaining sodium in the melt of tantalum powder after effectively can collecting sodium reduction reaction completely, as shown in Figure 1, the internal diameter of inner cylinder is about 10 centimetres, the external diameter of outer cylinder to be about on reaction vessel diametrically 1/2, the height of inner cylinder and outer cylinder is about 8 centimetres.Be provided with bottom collection sodium device 9 and put sodium pipe 92.
As shown in Figure 1, collection sodium device 9 is fixed on reaction vessel lid 3-1 below through collecting the auricle with holes that bottom sodium device 9, relevant position is stretched out in bottom surface by collection sodium device 9 by the fixed bar 9-1 of 4 suspension rods and nut composition, and the distance between the upper edge of inner cylinder and outer cylinder and the lower surface of container cover is about 5 centimetres.The alloy of collection sodium device 9-0 heat-resistant anticorrosion, as nickel or nickel-base alloy manufacture.
As shown in Figure 1, on the reaction vessel lid corresponding with collection sodium device 9, be provided with cooler 6, cooling agent enters from inlet tube 61, along blast pipe 71 toward dirty, by the coolant channel of ring-type, then flow out from coolant outlet 62, ring-type coolant channel can make cooling agent unimpeded.Form coolant channel, can be processed to form annular recess above reaction vessel lid, then weld the sealing of lastblock annular cover plate, surface raises up.One embodiment of the present invention correspond to position subsides weldering one piece of metallic plate of cooler 6 to lower convexity at the lower surface of container cover 31.When after sodium reduction reaction, paddle continues to stir, argon gas is filled with to reactor from inert gas inleting pipe 4, circulate from bottom to top argon gas in reaction vessel 3, discharge from blast pipe 71, and by 6 li, cooler circulation cooling agent, the Na-K alloy steam cooled instillation below cooler making product contain the alkali metal halide melt 12 li of tantalum powder collects in sodium device 9, part sodium vapor enters into blast pipe 71 li, flows to collection sodium device 9 li under being also cooled.
According to the present invention, after product 12 is cooled to room temperature, after opening reaction vessel lid 31, from putting sodium pipe 92, the Na-K alloy collection sodium device 9 can be released, also first with corrosion-resistant flexible pipe, Na-K alloy can be extracted out, then from putting sodium pipe, remaining sodium being put only.The sodium metal reclaimed can be used again.
The present invention also provides a kind of method of producing tantalum powder, using Fluoride for Raw Material potassium tantalate be selected from as the alkali halide salts of at least one in sodium chloride, potassium chloride, potassium fluoride joins reaction vessel 3 li as Fig. 1 as diluent, install container cover 31 to seal, reaction vessel 3 is placed in the reduction furnace 1 li of having heaters 2, find time from blast pipe 71, then be filled with inert gas from inert gas inleting pipe 4, open blast pipe 72 air bleeding valve exhaust circulation argon gas.Described raw material also comprises and adds the appropriate oxygenatedchemicals that can be dissolved in alkali halide salts as grain refiner, when sodium reduction potassium floutaramite produces the tantalum powder period of the day from 11 p.m. to 1 a.m, makes particle surface form one deck tantalum oxide, thus suppresses tantalum particle growth.
According to the inventive method, by regulating pulp furnish and reduction reaction conditions, can produce and comprise high-purity metallurgical Ta powder and specific volume is each grade Ta powder used in capacitor of 3000-120000 μ FV/g.
According to the present invention, first part material potassium floutaramite can be added reaction vessel 3 li, remaining raw material joins reaction vessel 3 from charge door 11 again and reduces in note sodium reduction process.
According to the present invention, in reaction mass temperature-rise period, close blast pipe 71 valve, be vented from blast pipe 72, gas flow is 0.1-10 liter/min, fully can remove the magazines such as metallic iron, nickel, chromium brought into by the corrosion reaction containers such as halide, water, carbon dioxide and the oxygen in raw material " acid " property material to tantalum powder like this.
According to the present invention, the heating raw materials be equipped with in above-mentioned reaction vessel 3 is melted to 800 DEG C-1050, stirs the material of fusing, inject the liquid metal sodium of stoichiometry 1.01-1.08, potassium floutaramite is thoroughly reduced and generates tantalum powder.In note sodium reduction process, due to exothermic heat of reaction, make pressure increase in reaction vessel, preferred reaction container inner pressure remains on 0.1 ~ 0.12MPa, if hypertonia, from blast pipe 72 Exhaust Gas, if hypotony, supplements argon gas from air inlet pipe.
According to the present invention, in reaction vessel, have potassium floutaramite to deposit in case, sodium metal and potassium floutaramite react, and seldom have sodium vapor to discharge, even if there is a small amount of sodium vapor to enter blast pipe 72, cooled backflow entered reaction vessel 3 li and continue to react with potassium floutaramite.
According to the present invention, row's sodium is carried out: cooling agent is passed into 6 li, cooler and circulate after having reacted, pressure in reactor is made to remain on 0.1 ~ 0.11MPa, close air bleeding valve 72, be vented from air bleeding valve 71, simultaneously constantly be passed into reactor by inert gas from air inlet 4, gas outflow is 0.1 liter/min-5 liters/min, at least keeps 30 minutes-3 hours the temperature of 880 DEG C or more; Then make pressure in reactor remain on 0.1 ~ 0.11MPa, gas outflow is 5 liters/min-50 liters/min, keeps 30 minutes-2 hours the temperature of 880 DEG C or more.
According to the present invention, in row's sodium process, gas flow in reaction vessel increases gradually from little, during beginning, in reaction vessel, sodium vapor is more, and sodium vapor runs into the cooler that reaction vessel covers and is condensed into liquid sodium instillation collection sodium device 9 li, after sodium vapor in reaction vessel reduces, increase gas flow gradually, make more sodium vapor instill collection sodium device 9 li.To last, the Na-K alloy containing the melt 12 li of tantalum powder is made substantially all to be collected into collection sodium device 9 li.
According to the present invention, row's sodium temperature is 880 DEG C-1050 DEG C, and the boiling point due to sodium metal is 881.4 DEG C, and temperature is higher, and the vapour pressure of sodium is higher, improves temperature in the final stage of row's sodium, and the Na-K alloy of the melt 12 li containing tantalum powder can be made substantially all to be discharged.
According to the present invention, after row's sodium terminates, by the material cool to room temperature of reaction vessel 3 li, reaction vessel lid 31 being hung out, releasing liquid metal sodium from putting sodium pipe 92; Taking out the condensation of reaction vessel 3 li containing tantalum powder product 12.
According to the present invention, the product of the sodium reduction potassium floutaramite of above-mentioned taking-up is carried out fragmentation, dry to sieve obtain tantalum powder through washing, pickling.
According to the present invention, optionally the tantalum powder that above-mentioned sodium reduction potassium floutaramite obtains is heat-treated and deoxidation treatment further.
In the methods of the invention, known technology can be adopted, if Chinese Patent Application No. is method disclosed in CN201010204181, CN201210518042 and CN201210517836, by reference above-mentioned file be introduced the application in full.
Embodiment
The present invention will clearly by following examples, and these embodiments are exemplary in the present invention purely.
Embodiment 1
Use device as shown in Figure 1, the sodium chloride of the potassium floutaramite of 200kg and 150kg is loaded in sodium reduction reaction vessel 3-0, argon gas is filled with from air inlet pipe 4 after blast pipe 7-2 finds time, the valve opening blast pipe 7-2 circulates, and throughput is 0.1-10 liter/powder, is heated by resistive device 2 and material 12 in reaction vessel 3 is warmed up to 960 DEG C, start paddle 10, being incubated after 1 hour starts from sodium injection tube 5 note sodium, injects 60.92kg sodium metal altogether, completes reaction.Cooling agent is entered from import 61, by passage 63, discharges from outlet 62; By blast pipe 72 valve closing, open blast pipe 71 valve, make the pressure in reaction vessel be maintained at about 0.1-0.105MPa, the flow of Exhaust Gas was 0.1-5 liter/min, continues stirring 10,960 DEG C of insulations 1 hour; Then in maintenance reaction vessel, pressure was 0.1-0.105MPa, and the flow of Exhaust Gas is 5-20 liter/min, 1020 DEG C of insulations 1 hour.Then cool to room temperature, hangs out reaction vessel lid 31, releases from putting sodium pipe 92 Na-K alloy collected.Taking out condensation from reaction vessel 3 containing tantalum powder product 12, through fragmentation, washing, pickling, dries and obtains tantalum powder.Heat-treated and deoxidation treatment by above-mentioned tantalum powder, the content data analyzing the oxygen content of tantalum powder, potassium, sodium, iron, nickel, chromium and silicon lists in table 1.
The above-mentioned tantalum powder obtained has lower specific area, has high-purity, is suitable as the raw material of powder metallurgy sputter tantalum target.
Collect alkali metal 0.8kg from alkali metal collector, return purification and use again.
Embodiment 2
Use device as shown in Figure 1, by the potassium floutaramite of 160kg, the sodium chloride of 100kg and 60kg potassium chloride and the oxygenatedchemicals grain refiner being dissolved in alkali halide salts on a small quantity load in sodium reduction reaction vessel 3, argon gas is filled with from air inlet pipe 4 after blast pipe 72 is found time, the valve opening blast pipe 72 circulates, gas flow is 0.1 liter/min-10 liters/min, be heated by resistive device 2 and material 12 in reaction vessel 3-0 is warmed up to 900 DEG C, paddle 10 is stirred, being incubated after 1 hour starts from sodium injection tube 5 note sodium, inject 48.7kg liquid metal sodium altogether, complete reaction.Cooling agent is circulated in cooler 6-0, by blast pipe 7-2 valve closing, opens blast pipe 7-1 valve, the pressure in reaction vessel is made to be maintained at about 0.1-0.105MPa, the flow of Exhaust Gas was 0.1 liter/min-5 liters/min, continues stirring 10,950 DEG C of insulations 1 hour; Then in maintenance reaction vessel, pressure was 0.1-0.105MPa, and the flow of Exhaust Gas is 5 liters/min-20 liters/min, 950 DEG C of insulations 1 hour.Then cool to room temperature, hangs out reaction vessel lid 31, releases from putting sodium pipe 92 Na-K alloy collected.Taking out condensation from reaction vessel 3-0 containing tantalum powder product 12, through fragmentation, washing, pickling, dries and obtains tantalum powder, by above-mentioned tantalum powder through Overheating Treatment and deoxidation treatment.The content data analyzing the oxygen content of tantalum powder, potassium, sodium, iron, nickel, chromium and silicon lists in table 1.Get the tantalum powder after above-mentioned deoxidation and carry out Electrical analysis,
Above-mentioned tantalum powder is pressed into electrolytic capacitor anode briquet, every grain weight 480mg, the diameter of briquet is about 5.0mm, and height is 2.83mm about, and briquet density is about 5.0g/cm3, and in vacuum drying oven, 1520 DEG C of sintering obtain agglomerate in 30 minutes.By described agglomerate in the phosphoric acid solution of 0.1% (Vol) of 90 DEG C with 60mA/g up voltage to 100V constant voltage 3 hours, carry out anodization and form anode, by above-mentioned anode 2 minutes electric currents that leak hunting in the phosphate aqueous solution of 10%, side capacity in the sulfuric acid of 30%, the specific capacitance and the DC leakage current that obtain described anode are listed in table 2.This tantalum powder has the capacitor being suitable for manufacturing the lower specific volume of high voltage.
The metals content impurities (ppm) such as O, K, Na, Ni, Cr, Fe of table 1 tantalum powder
| O | K | Na | Ni | Cr | Fe | Si | W | Mo | Cu | |
| Embodiment 1 | 1200 | 2 | 3 | 5 | 4 | 5 | ＜5 | ＜2 | ＜2 | ＜2 |
| Embodiment 2 | 2100 | 7 | 3 | 6 | 5 | 5 | 5 | ＜2 | ＜2 | ＜2 |
The electrical result of table 2 tantalum powder
| Specific capacitance (μ FV/g) | DC leakage current (nA/ μ FV) | |
| Embodiment 2 | 17200 | 0.18 |
As can be seen from the result of table 1 and table 2, the tantalum powder produced according to the inventive method has high-purity, may be used for sputter tantalum target and each grade capacitor.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, any those skilled in the art, do not departing within the scope of technical solution of the present invention, make many changes when the technology contents of above-mentioned announcement can be utilized or be modified to the equivalent example of equivalent variations, all still belonging within the scope of the new technical scheme of the present invention.
Claims (8)
1. the device of a sodium reduction potassium floutaramite, comprise reaction vessel and be mated the container cover of sealing, by the through hole in described container cover, described container cover is provided with stirring arm, thermocouple, sodium injection tube, charge pipe, inert gas inleting pipe, downtake pipe and second exhaust pipe, it is characterized in that, also comprise:
Collection sodium device, is located at below described container cover, is provided with and puts sodium pipe bottom described collection sodium device,
Cooler, be located at above described collection sodium device, this cooler has coolant inlet pipe, coolant outlet pipe and coolant flow channel.
2. the device of a kind of sodium reduction potassium floutaramite as claimed in claim 1, is characterized in that, described inert gas inleting pipe extends in reaction vessel until sodium reduction reacts the height of on the rear liquid level containing the melt of tantalum powder about 5-15 centimetre.
3. the device of a kind of sodium reduction potassium floutaramite as claimed in claim 1, is characterized in that, described inert gas inleting pipe extends in reaction vessel the degree of depth extending under the rear liquid level containing the melt of tantalum powder of sodium reduction reaction about 10-25 centimetre.
4. the device of a kind of sodium reduction potassium floutaramite as claimed in claim 1, is characterized in that, described downtake pipe is arranged in described cooler area, and it is overseas that second exhaust pipe is arranged on described cooler zone.
5. the device of a kind of sodium reduction potassium floutaramite as claimed in claim 4, it is characterized in that, described downtake pipe is arranged in the cooler area of container cover, be placed in coolant inlet pipe and coaxially arrange with coolant inlet pipe, the length at least 15 centimetres of described downtake pipe and coolant inlet pipe coaxial parts, it is overseas that second exhaust pipe is arranged on described cooler zone, and it is near the marginal position of described container cover.
6. the method utilizing the device of the sodium reduction potassium floutaramite described in any one claim of claim 1-5 to produce tantalum powder comprises step:
1) using Fluoride for Raw Material potassium tantalate be selected from as in sodium chloride, potassium chloride, potassium fluoride, the alkali metal salt of at least one joins in reaction vessel as diluent, argon gas circulation heating is filled with after finding time, inert gas enters reaction vessel from gas tube, by the blast pipe exhaust outside cooler, circulate with the inert gas of 0.1-10 liter/min of flow;
2) by the above-mentioned reaction vessel heating that raw material is housed, material is melted, to 800 DEG C-1050 DEG C, stirs the material of fusing, injection liquid metal sodium makes sodium metal and potassium floutaramite react and generates tantalum powder;
3) row's sodium is carried out after having reacted: passed into by cooling agent in cooler and circulate, constantly inert gas is passed in reactor simultaneously, pressure in reactor is made to remain on 0.1 ~ 0.11MPa, by being in the blast pipe exhaust in cooler, gas outflow is 0.1 liter/min-5 liters/min, at least keeps 30 minutes-3 hours the temperature of 880 DEG C or more; Then make pressure in reactor remain on 0.1 ~ 0.11MPa, gas flow is 5 liters/min-50 liters/min, keeps 30 minutes-2 hours the temperature of 880 DEG C or more, makes to be gasified totally in fact containing the sodium metal in the melt of tantalum powder, is collected in collection sodium device;
4) by product cool to room temperature, reaction vessel lid being hung out, releasing liquid metal sodium from putting sodium pipe; Product in reaction vessel is taken out carry out washing, pickling, oven dry.
7. tantalum powder producing method according to claim 6, is characterized in that step 3) described in sodium metal comprise sodium-potassium-sodium alloy.
8. tantalum powder producing method as claimed in claim 6, is characterized in that step 3) row's sodium temperature be 880 DEG C-1050 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510253215.9A CN104801725B (en) | 2015-05-18 | 2015-05-18 | A kind of reaction unit of sodium reduction potassium floutaramite and manufacture the method for tantalum powder with it |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510253215.9A CN104801725B (en) | 2015-05-18 | 2015-05-18 | A kind of reaction unit of sodium reduction potassium floutaramite and manufacture the method for tantalum powder with it |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104801725A true CN104801725A (en) | 2015-07-29 |
| CN104801725B CN104801725B (en) | 2018-01-23 |
Family
ID=53687153
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510253215.9A Active CN104801725B (en) | 2015-05-18 | 2015-05-18 | A kind of reaction unit of sodium reduction potassium floutaramite and manufacture the method for tantalum powder with it |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104801725B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107052329A (en) * | 2017-05-18 | 2017-08-18 | 江门富祥电子材料有限公司 | A kind of heat treatment method of tantalum powder |
| CN108080654A (en) * | 2018-01-23 | 2018-05-29 | 江门富祥电子材料有限公司 | A kind of production technology of ultra-fine flake type mesohigh tantalum powder |
| CN110315088A (en) * | 2019-08-16 | 2019-10-11 | 广东广晟稀有金属光电新材料有限公司 | A kind of preparation method of the high-purity tantalum powder of coralliform |
| CN113122830A (en) * | 2021-04-25 | 2021-07-16 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Tungsten sheet or tungsten crucible surface tantalum coating layer and preparation method thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2950185A (en) * | 1958-06-13 | 1960-08-23 | Nat Res Corp | Production of tantalum powder |
| US3829310A (en) * | 1973-04-30 | 1974-08-13 | Norton Co | High surface area valve metal powder |
| JPS5312758A (en) * | 1976-07-21 | 1978-02-04 | Enuaarushii Inc | Metal powder manufacturing |
| US4149876A (en) * | 1978-06-06 | 1979-04-17 | Fansteel Inc. | Process for producing tantalum and columbium powder |
| US5442978A (en) * | 1994-05-19 | 1995-08-22 | H. C. Starck, Inc. | Tantalum production via a reduction of K2TAF7, with diluent salt, with reducing agent provided in a fast series of slug additions |
| CN1240688A (en) * | 1998-07-07 | 2000-01-12 | 宁夏有色金属冶炼厂 | Technology for making tantalum powder |
| CN101879603A (en) * | 2010-06-18 | 2010-11-10 | 江门富祥电子材料有限公司 | Production method and production device of tantalum powder |
| CN201693182U (en) * | 2010-06-18 | 2011-01-05 | 江门富祥电子材料有限公司 | Production device for tantalum powder |
| CN103084568A (en) * | 2012-12-05 | 2013-05-08 | 江门富祥电子材料有限公司 | 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 |
| CN204108313U (en) * | 2014-04-18 | 2015-01-21 | 宁夏东方钽业股份有限公司 | Sodium metal reduction potassium floutaramite produces the reduction reaction container of tantalum powder |
| CN204700313U (en) * | 2015-05-18 | 2015-10-14 | 江门富祥电子材料有限公司 | A kind of device of sodium reduction potassium floutaramite |
-
2015
- 2015-05-18 CN CN201510253215.9A patent/CN104801725B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2950185A (en) * | 1958-06-13 | 1960-08-23 | Nat Res Corp | Production of tantalum powder |
| US3829310A (en) * | 1973-04-30 | 1974-08-13 | Norton Co | High surface area valve metal powder |
| JPS5312758A (en) * | 1976-07-21 | 1978-02-04 | Enuaarushii Inc | Metal powder manufacturing |
| US4149876A (en) * | 1978-06-06 | 1979-04-17 | Fansteel Inc. | Process for producing tantalum and columbium powder |
| US5442978A (en) * | 1994-05-19 | 1995-08-22 | H. C. Starck, Inc. | Tantalum production via a reduction of K2TAF7, with diluent salt, with reducing agent provided in a fast series of slug additions |
| CN1240688A (en) * | 1998-07-07 | 2000-01-12 | 宁夏有色金属冶炼厂 | Technology for making tantalum powder |
| CN101879603A (en) * | 2010-06-18 | 2010-11-10 | 江门富祥电子材料有限公司 | Production method and production device of tantalum powder |
| CN201693182U (en) * | 2010-06-18 | 2011-01-05 | 江门富祥电子材料有限公司 | Production device for tantalum powder |
| CN103084568A (en) * | 2012-12-05 | 2013-05-08 | 江门富祥电子材料有限公司 | 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 |
| CN204108313U (en) * | 2014-04-18 | 2015-01-21 | 宁夏东方钽业股份有限公司 | Sodium metal reduction potassium floutaramite produces the reduction reaction container of tantalum powder |
| CN204700313U (en) * | 2015-05-18 | 2015-10-14 | 江门富祥电子材料有限公司 | A kind of device of sodium reduction potassium floutaramite |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107052329A (en) * | 2017-05-18 | 2017-08-18 | 江门富祥电子材料有限公司 | A kind of heat treatment method of tantalum powder |
| CN107052329B (en) * | 2017-05-18 | 2019-08-23 | 江门富祥电子材料有限公司 | A kind of heat treatment method of tantalum powder |
| CN108080654A (en) * | 2018-01-23 | 2018-05-29 | 江门富祥电子材料有限公司 | A kind of production technology of ultra-fine flake type mesohigh tantalum powder |
| CN110315088A (en) * | 2019-08-16 | 2019-10-11 | 广东广晟稀有金属光电新材料有限公司 | A kind of preparation method of the high-purity tantalum powder of coralliform |
| CN113122830A (en) * | 2021-04-25 | 2021-07-16 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Tungsten sheet or tungsten crucible surface tantalum coating layer and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104801725B (en) | 2018-01-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4149876A (en) | Process for producing tantalum and columbium powder | |
| CN104801725A (en) | Reaction device for reducing potassium fluotantalate by sodium and method for manufacturing tantalum powder by reaction device | |
| CN105803233B (en) | The smelting process of nickel-base alloy containing aluminium titanium boron zirconium | |
| CN105648278B (en) | The smelting process of nickel base superalloy | |
| CN105734314B (en) | The vacuum metling technique of nickel base superalloy | |
| CN102465209B (en) | Method and vacuum distillation device for preparing high-purity neodymium | |
| CN105506318B (en) | A kind of production technology of extra super duralumin alloy | |
| CN204700313U (en) | A kind of device of sodium reduction potassium floutaramite | |
| JP7437813B2 (en) | Production method of high-purity metallic lithium using vacuum thermal reduction method | |
| CN105948122B (en) | A kind of method for preparing high-purity molybdenum trioxide | |
| CN108913922A (en) | The sublimate method of smelting of Ni-based directional solidification cylindrulite, single crystal super alloy master alloy | |
| CN111097920B (en) | Method for producing magnesium-lithium alloy by gaseous co-condensation method | |
| CN204770680U (en) | Reduction potassium fluorotantalate's reaction unit | |
| CN107523701A (en) | A kind of method of normal pressure silicothermic reduction magnesium metal | |
| Tian et al. | One-step and selective extraction of nickel from nickel-based superalloy by molten zinc | |
| CN105624473B (en) | The vacuum metling technique of high temperature alloy | |
| CN105603226B (en) | The vacuum smelting method of nickel base superalloy | |
| CN109110789B (en) | Method for preparing beryllium fluoride and method for preparing ultra-pure metallic beryllium | |
| CN204700312U (en) | A kind of process units of tantalum powder | |
| Kroll et al. | Large‐scale laboratory production of ductile zirconium | |
| TWI429792B (en) | Method and apparatus for producing solid product | |
| US2165742A (en) | Process for separating magnesium and like metals which sublime from their ores and compounds | |
| CN107739892A (en) | The vacuum metling technique of nickel-base cast superalloy | |
| CN107760903A (en) | The smelting process of high chromium nickel-base cast superalloy | |
| CN107794386A (en) | The vacuum smelting method of high chromium nickel-base cast superalloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |