CN105051223B - Purify out the method and device of target powder - Google Patents
Purify out the method and device of target powder Download PDFInfo
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- CN105051223B CN105051223B CN201280077499.5A CN201280077499A CN105051223B CN 105051223 B CN105051223 B CN 105051223B CN 201280077499 A CN201280077499 A CN 201280077499A CN 105051223 B CN105051223 B CN 105051223B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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Abstract
The method of purification of tantalum powder in a kind of sodium reduction potassium floutaramite product with metal, this method is first to cut off the part that tantalum powder is free of in metal sodium reduction potassium floutaramite product, then by the part containing tantalum powder carry out it is broken after carry out tantalum powder again and detached with comprising tantalum powder alkali metal haloid, remove ultra-fine grain and Ferromagnetic Impurities in tantalum powder, mordant dissolving removal of impurities, the separation of spent acid lotion and tantalum powder, divide disk drying and processing, obtain the tantalum powder for being suitble to subsequent processing, described device can meet tantalum powder and be detached with comprising tantalum powder alkali metal haloid, remove ultra-fine grain and Ferromagnetic Impurities in tantalum powder, pickling dissolving removal of impurities, the separation Four processes of spent acid lotion and tantalum powder, it is low to solve static mode efficiency in prior art, water consumption is big, the inferior separating effect of spent acid lotion and tantalum powder, it is big to solve current technique labor intensity, ineffective problem.
Description
Technical field
The present invention relates to the method and devices that target powder is purified out from the mixture comprising target powder, particularly relate to
And one kind restores potassium floutaramite (K from metallic sodium (Na)2TaF7) method and device of tantalum powder is purified out in products therefrom.
Background technology
In the industry, it is often necessary to from including target powder such as tantalum powder, niobium powder, tantalum-niobium alloy powder, niobium monoxide powder
Target powder is purified out in mixture.For example, it is often desirable to tantalum powder is purified out from the mixture comprising tantalum powder.
In the electronics industry, one of main application of tantalum powder is manufacture tantalum electrolytic capacitor (hereinafter referred to as tantalum capacitor).
The requirement being getting faster to meet the electronic device speed of service, it is desirable to which its volume specific volume, reliability, height is continuously improved in tantalum capacitor
Frequency performance, and with Low ESR.Have increasing need for having following characteristics as the tantalum powder for making tantalum capacitor anodes main material：
Surface area increase improves tantalum capacitor volume specific volume to improve tantalum powder specific volume；Purity is continuously improved to improve tantalum capacitor
Reliability particularly requires relatively low O, C, K, Na, F.In order to ensure that the tantalum powder of high-specific surface area has enough purity, need
Consume a large amount of pure water.But it in order to be pushed further into clean manufacturing, needs to further improve water application efficiency, while reduce labour
Intensity improves working efficiency, constantly meets the production of the increasing high specific capacitance tantalum powder of specific surface area.
Chemical method produces tantalum powder generally use metallic sodium (Na) reduction potassium floutaramite (K2TaF7) method, generate product
In have tantalum powder, sodium fluoride and potassium fluoride, chemical equation is：
K2TaF7+5Na→Ta+5NaF+2KF
Above-mentioned potassium floutaramite (K is restored with metallic sodium (Na)2TaF7) reaction process in, in order to obtain with big ratio
The tantalum powder of surface area, often will be in potassium floutaramite (K2TaF7) it is inner add in alkali halide, such as sodium chloride (NaCl), potassium chloride
(KCl), one or more of mixtures of potassium fluoride (KF), potassium iodide (KI), sodium iodide (NaI) etc. are as diluent.In order to
Ensure K2TaF7It is thoroughly restored, often adds in excessive metallic sodium (Na) in actual production.Above-mentioned reduction reaction generally exists
700 DEG C or more are carried out with molten salt system, and excessive metallic sodium (Na) under this condition can be by potassium ion (K+) it is reduced to metallic potassium
(K).Simultaneously potassium tantalate/inclined potassium tantalate, the sodium tantalate/inclined for being insoluble in water will be generated since there are the impurity such as oxygen in molten salt system
Sodium tantalate, they often exist in the form of ultra-fine grain (below grain size 100nm).If potassium tantalate/inclined potassium tantalate, tantalic acid
Sodium/sodium metatantalate cannot be detached with tantalum powder, then the content of K, O and Na in obtained tantalum powder will be higher.Upper
It states with metallic sodium (Na) reduction potassium floutaramite (K2TaF7) reaction process in the tantalum powder that generates be suspended in by sodium fluoride (NaF), fluorine
The alkali halide and remaining alkali metallic sodium (Na) of change potassium (KF) and diluting salt composition and newly generated alkali metal potassium (K)
Melt in, become the mixture of tantalum powder and above-mentioned alkali halide after cooling and be entrained with superfluous alkali metallic sodium (Na) and
Newly generated alkali metal potassium (K) and it is insoluble in the condensed product of potassium tantalate and sodium tantalate/sodium metatantalate of the potassium tantalate of water/partially.
Chinese patent CN102191389A provides a kind of solution：Above-mentioned condensed product is broken into granularity as 15mm
Following little particle, first in diafiltration slot with 15 DEG C~35 DEG C of cold deionized water diafiltration to neutral, then again with 40 DEG C~
100 DEG C of hot deionized waters carry out diafiltration, and the conductivity for washing diafiltration slot lower part efflux is less than 10 micro-Siemens (μ s/cm),
Then it is transferred to stir in washing trough and be washed with deionized water high-speed stirred, dissolved clean with pickling again later, static diafiltration later is realized
Acid pickle is detached with tantalum powder, using drying and sieving powder, is then carried out subsequent processing and is obtained tantalum powder product.However, this purification
There are many defects for method：First, all alkali metal haloids are integrally handled with tantalum powder, water consumption is big, brings into more
Indissoluble tantalates/inclined tantalates that reduction process generates, causes tantalum powder impurity higher；Second, directly with cold deionized water diafiltration
Restore obtained condensed product block, the alkali metallic sodium (Na) and newly generated alkali metal potassium (K) in condensed product are generated with water
High concentration strong base solution, strong base solution corrosion tantalum powder, makes the reduction of tantalum powder yield, while generation is insoluble in potassium tantalate/inclined tantalum of water
Sour potassium and sodium tantalate/sodium metatantalate increase impurity in tantalum powder；Third, tantalum powder is detached with alkali metal haloid, spent acid after pickling
The processes such as the separation of lotion and tantalum powder are static process, and efficiency is low, and water use efficiency is low, and water consumption is bigger；4th, it gives up after pickling
The separation process of mordant and tantalum powder is static process, is susceptible to flow dead angle in tantalum powder filter cake, spent acid lotion and tantalum powder
Inferior separating effect influences tantalum powder quality；5th, variety of processes uses different device, needs repeatedly to transport, and labor intensity is big,
Working efficiency is low.This method cannot increasingly meet the production of the high specific capacitance tantalum powder of big specific surface area.
As it can be seen that potassium floutaramite (K is restored from metallic sodium (Na) in the prior art2TaF7) tantalum powder is purified out in products therefrom
Method it is big there are still labor intensity, the shortcomings of working efficiency is low, and water consumption is big, and tantalum powder yield is relatively low, and tantalum powder impurity is higher.
Invention content
The defects of it is an object of the invention to overcome the above-mentioned prior art, provides a kind of from the mixture comprising target powder
The middle method for purifying out target powder particularly restores potassium floutaramite (K from metallic sodium (Na)2TaF7) tantalum is purified out in product
The method of powder, this method can obtain the tantalum powder of high-purity.The tantalum powder is especially suitable for manufacturing tantalum electrolytic capacitor anode.
Another object of the present invention, which provides, realizes that carry out tantalum powder in a dynamic fashion detaches and pickling with alkali metal haloid
The device that spent acid lotion is detached with tantalum powder afterwards, and the device can realize that tantalum powder is detached with alkali metal haloid, removed in tantalum powder
Detergent and the separation Four processes of tantalum powder after ultra-fine grain and Ferromagnetic Impurities, pickling dissolving removal of impurities, pickling.
In one embodiment of the invention, it provides and a kind of target is purified out from the mixture comprising target powder
The device of powder, the device include two parts to link together from top to bottom,
Wherein first part is columnar filtration fraction；
Second part is the groove body that top is cylindrical and bottom is rounded or oval, and top carries stirring bar；
Wherein the groove body is equipped with the inlet tube for extending to bottom, outlet tube, and bottom is equipped with baiting valve, stirring is equipped in groove body
Paddle and optional concentration equipment；
Wherein described filtration fraction carries the interlayer that can provide vacuum；The wherein described inlet tube top band for extending to bottom
There is the aperture of dispersing water flow, the outlet tube top can be variously-shaped, and optionally with filter element.
In one embodiment of the invention, the first part and second part flanged joint.
In another embodiment, the first part and second part are integrated.
The target powder is selected from tantalum powder, niobium powder, tantalum-niobium alloy powder, niobium monoxide powder and its mixture.Preferably, it is described
Target powder is tantalum powder, and the mixture comprising tantalum powder is with metallic sodium (Na) reduction potassium floutaramite (K2TaF7) obtain reaction production
Object.
In one embodiment of the invention, the shape of the agitating paddle be selected from bar shaped, disk, rectangle and other
It is variously-shaped.
Preferably, stirring loom and cell wall are in the angle of 0-30 degree.It is highly preferred that agitating paddle and concentration equipment can on
Lower lifting.
In one embodiment of the invention, provide it is a kind of using foregoing device from comprising target powder
The method that target powder is purified out in mixture.
Preferably, the mixture comprising target powder is the mixture for including tantalum powder, which is with metallic sodium (Na)
Restore potassium floutaramite (K2TaF7) obtained reaction product.
Preferably, the mixture comprising tantalum powder obtains in the following way：
With metallic sodium (Na) reduction potassium floutaramite (K in reduction vessel2TaF7), after the completion of reaction, stop before condensation
Stirring makes tantalum powder sedimentation layering, is divided into the part without tantalum powder and the part comprising tantalum powder；
The reaction product is taken out from reduction reaction container, part of the excision without tantalum powder is left comprising tantalum powder
Reaction product is as the mixture comprising tantalum powder；
Optionally, the mixture comprising tantalum powder is broken into granularity as below 20mm blocks or is ground into powder.
It should be understood that " part for being free of tantalum powder " is substantially free of the tantalum of simple substance form mainly comprising tantalates herein.
In a specific embodiment, the method for the present invention includes following steps：
A alkali metal haloid) is removed；
B ultra-fine grain) is removed；
C Ferromagnetic Impurities) are optionally removed；
D) pickling dissolving removal of impurities；With
E tantalum powder) is recycled.
Ultra-fine grain as described herein refers to the particle below grain size 100nm, including the tantalic acid that granularity is below 100nm
The particle of potassium/inclined potassium tantalate, sodium tantalate/sodium metatantalate, they are insoluble in water.Particularly, method of the invention is for removing grain
The particle of below diameter 20nm is especially effective.
In one embodiment of the invention, step A) including following sub-step：
1) mixed acid of for example various inorganic acids of the first acidic electrolyte solution and/or organic acid is added in by inlet tube,
And put into the mixture comprising tantalum powder in described device, while start stirring, preferably described inorganic acid is selected from hydrochloric acid, nitre
In acid, sulfuric acid, hydrofluoric acid and their mixed acid, particularly, the inorganic acid is hydrochloric acid；
2) return pump is connected to the interlayer of the device, and starts return pump；
3) the second acidic electrolyte solution such as various inorganic acids (such as salt is continuously added from bottom by the inlet tube
Acid, nitric acid, sulfuric acid, hydrofluoric acid and their mixed acid, preferably hydrochloric acid) and/or organic acid mixed acid, be kept stirring and take out
Sky makes aqueous solution pass through filter membrane, is detached with powder, and aqueous solution is reduced to pH value after 4-6, to add in pure by alkalinity in the device
Water replaces acidic electrolyte solution, continues to wash, until aqueous solution conductivity is less than 10,000 micro-Siemens (μ s/ in device
Cm), preferably shorter than 2,000 micro-Siemens (μ s/cm), preferably shorter than 500 micro-Siemens (μ s/cm), preferably shorter than 200 micro- west gates
Sub (μ s/cm) then stops stirring, stops adding in pure water, stops evacuating；
4) third electrolyte solution is added in, after tantalum powder is made to settle such as 20-30 minutes, liquid phase is taken out by outlet tube, and
Tantalum powder on filter membrane is flushed to described device bottom.
In sub-step 1) in, the mixture comprising tantalum powder is put into the first acidic electrolyte solution, gold can be neutralized rapidly
Belong to sodium (Na) and metallic potassium (K) reacts the alkali of generation with water, reduce corrosion of the alkali to tantalum powder, reduce and generate harmful precipitation.
In sub-step 2) in, remove alkali metal haloid, effect and the first acid electricity with the second acidic electrolyte solution
Electrolyte solution is identical, but after aqueous solution is reduced to pH value as 4-6 by alkalinity in device, it is molten should not to add acidic electrolyte bath
Liquid, because containing a large amount of F in device in aqueous solution at this time-Ion, will be to tantalum powder if adding acidic electrolyte solution
Generate corrosion.1) and 3) preferably, the mixing speed in is respectively or simultaneously 0.01-3000 revs/min, preferably 0.5-100
Rev/min.
Preferably, described first, second and/or third acidic electrolyte solution pH value ＜ 6, preferably 1-4.It is preferred that
Ground, described first, second and/or third acidic electrolyte solution do not generate precipitation after the addition, in order to avoid precipitation pollution target powder
End.
In one embodiment of the invention, step B is carried out in the following way)：
The 4th electrolyte solution such as acidic electrolyte bath or the salting liquid (preferably hydrochloric acid) of neutrality are added in into described device,
And pass through blender and be stirred such as 0.01-200 minutes, preferably 3-20 minutes, preferably 3-15 minutes, then stop stirring
It mixes and precipitates such as 20-30 minutes, liquid phase is taken out by outlet tube.
Preferably, step B) in the 4th electrolyte solution be acid and/or salt mixed solution.4th acidic electrolyte bath
Solution can cause aqueous solution concentration of electric charges to improve after adding in, but not generate precipitation, in order to avoid precipitation pollution target powder.More preferably
Ground, the 4th electrolyte solution be inorganic acid with selected from sodium chloride (NaCl), potassium chloride (KCl), one kind in potassium fluoride (KF) or
A variety of mixtures.
Be not bound by any theory, it is believed that step B) principle it is as follows：Part ultra-fine grain has glue in tantalum powder mixture
The performance of body, surface electrification in the case of stirring, sinking speed is slow, thus is readily retained in water phase.It is but other
The particle sinking speed of grain size is than comparatively fast, being often deposited to bottom.So ultra-fine grain can be realized by detaching water phase by outlet tube
It is detached with tantalum powder.By being selected electrolyte simultaneously reasonably to adjust its concentration, satisfied separating effect can be reached.It should
Understand, in practical operation, also comprising the ultra-fine tantalum powder of some grain sizes in the ultra-fine grain being removed with water phase, due to these tantalums
Mealiness can be bad, therefore the removal of these superfine tantalum powders is also what can be received, even desired.Step B) it repeatedly can
Relatively thoroughly to remove ultra-fine grain.
In one embodiment of the invention, step C is carried out in the following way)：Magnetic is inserted into electrolyte solution
Screening device simultaneously stirs, and then takes out concentration equipment, takes Ferromagnetic Impurities in tantalum powder out of.
In yet another embodiment of the present invention, in step B) in be stirred by concentration equipment, then take out magnetic
Screening device takes Ferromagnetic Impurities in tantalum powder out of, so as to be carried out at the same time step B) and C).
In a preferred embodiment of the invention, step B is repeated) and/or C) repeatedly, such as 1-200 times, preferably
It is 1-30 times, 5-20 times more preferable.
In one embodiment of the invention, step D) including following sub-step：
I) mordant is added in into described device to be stirred such as 1-6 hours, is then stopped stirring, is precipitated such as 5-
After 50min, most spent acid lotions for including dissolved impurity are taken out by outlet tube；
Ii) in the case of stirring, cold pure water is continuously added from bottom into apparatus of the present invention by inlet tube, starts and take out
Sky pump, makes aqueous solution pass through filter membrane, is detached with tantalum powder；
Iii it) after aqueous solution conductivity is less than 15 micro-Siemens (μ s/cm) in device, adds in hot pure water and substitutes cold pure water,
After aqueous solution conductivity is less than 10 micro-Siemens (μ s/cm) in device, stop stirring, stop adding water, it is anhydrous logical in filter membrane
Later stop evacuating, leave water and the mixture of tantalum powder in the device.
The mordant refers to the mixed liquor comprising hydrofluoric acid and hydrogen peroxide, wherein must also contain hydrochloric acid, nitric acid, sulfuric acid
One or more of to improve total acid molar concentration.In general, mordant preparation design conditions are：In step D) initial operating stage,
Aqueous solution contains 0.25-3.5mol/L hydrofluoric acid, 0.1-1.5%mol/L hydrogen peroxide in device, and total acid molar concentration is 0.6-
10mol/L。
Preferably, it will i) repeat 1-200 times, preferably repeat 1-30 times, more preferably repeat 1-3 times.
Preferably, the pure water is the pure water of the pure water of 7 megaohms of resistivity ＞, preferably 10 megaohms of ＞, more preferably ＞
12 megaohms of pure water is most preferably the pure water of 15 megaohms of resistivity ＞.
In one embodiment of the invention, step E is carried out in the following way)：
Will be from step D) obtained mixture is all put into filter, detach most water, the filter cake that then will be obtained
Divide disk vacuum drying, obtain target powder.
Preferably, drying is carried out by following condition：In negative pressure such as less than atmospheric pressure 0.06MPa or lower
It it is 80 DEG C or more in temperature under pressure.
It should be appreciated that pH test paper and pH meter can be used to measure and monitor the pH value of solution.For the purpose accurately controlled,
PH meter is preferred.
Herein, " room temperature pure water " and " cold pure water " can be used alternatingly.First, second, third He in the present invention
4th electrolyte solution may be the same or different.Preferably, the addition of first, second, third and fourth electrolyte solution
Precipitation is not generated.
Method using the present invention and/or device productive target powder such as tantalum powder has the following advantages in one kind or more
Kind：
1) water consumption is small；
2) impurity and the separation of target powder such as tantalum powder are abundant；With
3) the advantages that labor intensity is low, and working efficiency is high；
In addition, one in being had the following advantages according to the target powder such as tantalum powder that the method for the present invention and/or device produce
Kind is a variety of：
1) advantages such as purity is high, and the impurity containing O, C, K, Na, F is low；
2) specific volume is high；With
3) leakage current is low.
Description of the drawings
Fig. 1 is according to the present invention to restoring potassium floutaramite (K with metallic sodium (Na)2TaF7) product in tantalum powder carry out
The device of purification, wherein legend are as follows：
1. 5. inlet tube flow dispersion apertures of filter membrane 2. hollow sandwich, 3. stirring bar, 4. inlet tube, 6. outlet tube
7. 12. return pump of baiting valve 8. agitating paddle, 9. connecting flange, 10. tantalum powder, 11. water phase, 13. concentration equipment
Specific embodiment
For the purpose this specification, the amount of all expression compositions, reaction condition etc. in the specification and in the claims
Number in all cases it is understood that be modified by term " about ", unless otherwise specified.Correspondingly, the following specification
It is approximation with the numerical parameter provided in the appended claims, the desirable property that can be attempted according to the present invention
And change, unless the contrary indication.At least, and application of the doctrine of equivalents on right is not intended to limit, each
Numerical parameter at least should round up technology and explain according to the digit of the effective digital reported and according to common.
As described above, the inventive system comprises first parts and second part.The effect of first part was mainly
Filter；The effect of second part is mainly dissolved impurity.
Although first part and second part can be made of one, in order to more easily install, split and clearly
It washes, more preferably they is linked together by detachable part such as flange.By flange by first part and second
In the situation point to link together, more easily the first part of top can be disassembled, filter membrane is cleaned or more
It changes.
The exemplary device and not restrictive of the present invention is described in detail below in conjunction with attached drawing.
Fig. 1 is the device for being used to purify out tantalum powder from the mixture comprising tantalum powder of the present invention.The device is from top to bottom
Including two parts, first part is columnar filtration fraction.Second part for top is cylindrical and bottom is rounded or ellipse
Circular groove body.First part and second part flange 9 connect
First part includes filter membrane 1 and can provide the interlayer 2 of vacuum, and vacuum pump 12 evacuates interlayer 2, so as to real
It now filters, tantalum powder is made to be detached with solution.
Cylinder-shaped upper part and rounded or oval bottom, the two with stirring bar is included in second part to be welded on
One integrally shows the shape of groove body.The second part is equipped with and extends to the inlet tube 4 of bottom and outlet tube 6, inlet tube 4
The part for being embedded to solid mixture carries the aperture 5 of flow dispersion.Second part is also equipped with baiting valve 7 in bottom, and in groove body
Equipped with agitating paddle 8 and concentration equipment 13.
An exemplary embodiment and not restrictive according to the present invention described further below.
Specifically, following embodiment is provided by way of illustration, not of limitation.
Embodiment 1
First, by using metallic sodium (Na) reduction potassium floutaramite (K2TaF7) mixture comprising tantalum powder is provided.Specifically
Ground is packed into the mixing of 300kg potassium chloride (KCl), 450kg potassium fluorides (KF), 100kg potassium iodide (KI) in reduction reaction container
Object is heated to start to stir after said mixture melts, and continues to be heated to 900 DEG C, then add in 30kg into reduction reaction vessel
Potassium floutaramite (K2TaF7), about 12kg liquid metals sodium is added, restores potassium floutaramite, so as to generate reaction product.It is reacting
Product stops stirring before beginning to cool down, and tantalum powder is made to be settled in fused salt, and reaction product then is cooled to room temperature obtains condensation production
Object takes out condensed product in reaction vessel.Then, the purple part that tantalum powder is not included in above-mentioned condensed product is cut off, it will
Black portions comprising tantalum powder are broken into the block less than 20mm.
Then, tantalum powder and the separation of alkali metal haloid are carried out.Specifically, in the device of the invention as shown in Figure 1
The hydrochloric acid that the pH value prepared in advance is 1 is added in be added thereto as the first electrolyte solution, and by the block, while rotation is stirred
Mix paddle 8.Then, vacuum pump is connected to the device, and opens return pump 12.Then, it is constantly passed through by inlet tube 4 and matched in advance
Good pH is 4 hydrochloric acid as the second electrolyte solution, is kept stirring and evacuates, aqueous solution is made to pass through filter membrane 1, after taking away dissolving
Alkali metal haloid, and tantalum powder is stayed in the device, is carried out tantalum powder in a dynamic condition and is detached with alkali metal haloid.At this
In the process, because adding hydrochloric acid, the metallic sodium, the alkali of metallic potassium generation that are mingled in mixture are neutralized, and avoid tantalum powder quilt
Corrosion, and reduce potassium tantalate/potassium tantalate and sodium tantalate/the sodium metatantalate generation partially for being insoluble in water.In tantalum powder and alkali metal
In haloid separation process, the alkali that metallic sodium, metallic potassium react generation with water will gradually reduce, and aqueous solution is gradually by alkali in device
Sex reversal is pickling, to pH value of water solution is 4 after the salt pickling for the use of pH being 4 12 minutes, stop being passed through hydrochloric acid at this time and from into
Liquid pipe 4 adds in pure water, and after pure water washes 9 hours, aqueous solution conductivity stops stirring afterwards less than 200 micro-Siemens (μ s/cm) in device
It mixes, stops logical pure water, stop evacuating after waiting the anhydrous outflow of return pumps；Tantalum powder on filter membrane is flushed to the device lower part, is added
Enter the hydrochloric acid of 1.0 liters of a concentration of 4.0mol/L as third electrolyte solution, etc. after tantalum powders settle 30 minutes, pass through outlet tube 6
Liquid phase is sucked out.
Then, ultra-fine grain and the process for removing Ferromagnetic Impurities are removed.Specifically, it is added in by inlet tube 4 pure
Water makes pure water full of device second part, adds the hydrochloric acid of 1.0 liters of a concentration of 4.0mol/L as the 4th electrolyte solution,
And concentration equipment is inserted into electrolyte solution, bottom is extended to, is then stirred 15 minutes, stops stirring and opening later
Begin precipitation, and after tantalum powder settles 30 minutes, liquid phase is taken away by outlet tube 6.Under the stirring of concentration equipment, constantly repeatedly add
Pure water plus hydrochloric acid stir, and precipitation takes out liquid-phase operation 20 times, realizes the removal of ultra-fine grain in tantalum powder.Then, magnetic separation is taken out
Device takes Ferromagnetic Impurities in tantalum powder out of, unloads concentration equipment, and clears up concentration equipment surface outside the present apparatus and inhaled from tantalum powder
Attached ferromagnetic material realizes the removal of Ferromagnetic Impurities in tantalum powder.
Later, pickling dissolving removal of impurities is carried out.Specifically, water is further reduced in the present apparatus to the water surface by outlet tube 6
Close to the sediment surface comprising tantalum powder, the mixture of hydrochloric acid, hydrofluoric acid and hydrogen peroxide is then added in as mordant, makes device
Middle aqueous solution is the mixing containing concentration 5.5mol/L hydrochloric acid, concentration 2.5mol/L hydrofluoric acid, concentration 0.75mol/L hydrogen peroxide
Liquid is stirred 6 hours, carries out pickling dissolving removal of impurities；Then stop stirring, after precipitating 15min, by outlet tube 6 as far as possible
Spent acid lotion in more extraction present apparatus, and by spent acid lotion delivery to waste acidity recovery processing system, due to being carried on outlet tube
Filter element, it is possible to be effectively prevented from tantalum powder and also be pumped.Then, in the case of stirring, by inlet tube 4 constantly from
Cold pure water is passed through in the bottom of device, while starts return pump 12, aqueous solution is made to pass through filter membrane 1, takes away spent acid lotion, and tantalum
Powder is stayed in the device, realizes the separation of spent acid lotion and tantalum powder.After aqueous solution conductivity is less than 15 μ s/cm in device, change
50 DEG C of hot pure water washings after aqueous solution conductivity is less than 10 μ s/cm in device, stop stirring, stopping plus water, when return pump 12
Stop evacuating after anhydrous extraction；The separation used time of spent acid lotion and tantalum powder amounts to 13 hours.
Then, the mixture of tantalum powder in device and water is all put into filter, filters the most water of separation, then will
Obtained filter cake (thickness is less than 30mm) is divided in corrosion resistant stainless steel charging tray, in subatmospheric 0.06MPa or lower
Negative pressure device in, dried at a temperature of 80 DEG C, obtain being suitable for the target powder for being suitble to subsequent processing.
It is to implement sample 1 by above-mentioned tantalum powder number.Sampling analysis implements O, C, K, Na, F content in sample 1, O, C, K, Na content
Analysis uses spectrophotometry using national standard, F content analysis, the use of analytical instrument is spectrophotometer, referring specifically to table
1.Implement impurity content in sample 1 to be listed in subordinate list 2.Statistics from washing be dosed into drying before whole process water consumption, processing time,
Number, tantalum powder yield are transported, is listed in subordinate list 2.
1 chemical impurity analysis method of table
Comparative example 1
First, it is substantially identical with embodiment to provide the mixture process comprising tantalum powder, difference part is not cut off not
Part containing tantalum powder and condensed product is all broken into the block less than 15mm.
Then, according to Chinese patent CN102191389A, with deionized water diafiltration, in start diafiltration 5 hours, diafiltration
Slot lower part efflux is milky turbidity liquid, and pH value reaches 7 or so after pH value reaches 14,7 hours, changes 50 DEG C or so of deionization
Water is washed；Due to tantalum powder large specific surface area, average grain diameter is small, and water velocity is slow, and water in rinsing bowl is just washed till after 22 hours
The conductivity of solution is less than 10 μ s/cm, and the first filter cake is obtained by filtration.
Then, continue to be stirred washing according to Chinese patent CN102191389A.It is average due to tantalum powder large specific surface area
Grain size is small, sedimentation it is difficult in addition can not supernatant, stir after washing and solid mixture be transferred to filter, the second filter cake is obtained by filtration.
Then, continue to carry out pickling according to Chinese patent CN102191389A.It is filtered after pickling, with deionized water filter 23 1
After hour, conductivity is washed till less than 10 μ s/cm, third filter cake is obtained by filtration；
Then, it is recycled.Specifically, filter cake at 120 DEG C is dried in air, dried to after 10 hours or so,
Due to tantalum powder large specific surface area, average grain diameter is small, and activity is too strong, and spontaneous combustion occurs for tantalum powder, tantalum powder firing accident occurs, experiment fails
It completes.Drying temperature in above-mentioned experiment is dropped to 80 DEG C, again involuntary ignition, experiment fails to complete；It will be dried in above-mentioned experiment
Temperature drops to 50 DEG C, and tantalum powder is dried 50 hours, still fails to dry, and experiment fails to complete.Statistics is before washing is dosed into drying
Whole process water consumption, processing time, transhipment number, tantalum powder yield, are represented with comparative sample 1, are listed in subordinate list 1.
Comparative example 2
Treatment process is substantially identical with comparative example 1, and difference part is tantalum powder recovery process.Specifically, filter cake is dispensed
In corrosion resistant charging tray, filter cake thickness is less than 30mm, in the negative pressure device of subatmospheric 0.08MPa, in 80 DEG C of baking
It is dried at dry temperature, sieving obtains initial tantalum powder.
It is comparative sample 2 by above-mentioned tantalum powder number.O, C, K, Na, F content in sampling analysis comparative sample 2.Impurity in comparative sample 2
Content is listed in subordinate list 2.Statistics from washing be dosed into drying before whole process water consumption, processing time, transhipment number, tantalum powder receive
Rate is listed in subordinate list 2.
The implementation sample 1 of acquisition and comparative sample 2 are granulated, adulterated, then while under vacuum at 1050 DEG C of heat
It manages 30 minutes, the tantalum powder after being heat-treated, the magnesium powder of tantalum powder weight 5% is added in the tantalum powder after heat treated, it is de- at 880 DEG C
Oxygen 4 hours obtains the product tantalum powder for tantalum electrolytic capacitor anode, wherein the tantalum powder number for implementing to obtain after sample 1 is handled is
Embodiment product sample 1, the tantalum powder number obtained after the processing of comparative sample 2 is comparative example product sample 2.The chemistry of sampling and measuring tantalum powder is miscellaneous
Matter, the results are shown in Table 3.
Above-mentioned two product sample tantalum powder 50mg is taken respectively, is pressed into diameter 2.0mm, density 5.0g/cm3Briquet, will
Above-mentioned briquet is sintered 20 minutes for 1150 DEG C in vacuum drying oven, sintered body is formed, by 0.0102mol/L of the above-mentioned agglomerate at 80 DEG C
H3PO4Aqueous solution middle-jiao yang, function of the spleen and stomach polarizes, and boosts to 10V with the current density of 110mA/g, constant pressure forms anode block in 60 minutes.By above-mentioned sun
Pole block is in 0.0102mol/L H3PO47V leaks hunting electric current in aqueous solution, in 3.9099mol/L H2SO4120Hz is tested in aqueous solution
Capacity (CV) and loss (tg δ) value, are as a result listed in table 4.
In comparative example 1, due to tantalum powder large specific surface area, average grain diameter is small, is washed using static state, and water velocity is slow, effect
Rate is extremely low；In the case where not using vacuum drying, if temperature is high, due to tantalum powder large specific surface area, average grain diameter is small, activity
Too strong, spontaneous combustion occurs for tantalum powder, firing accident will occurs, if temperature is low, drying efficiency is too low, can not produce.From table 2, table 3,
4 data of table can be seen that in comparative example 2, since all alkali metal haloids and tantalum powder are integrally carried out tantalum powder purification, and
Static water-washing method separation tantalum powder and alkali metal haloid, still tantalum powder and acid solution, tantalum are detached after pickling with static state diafiltration mode
Powder water consumption is big, and processing time is long, and there are dead angle, acid solution and other ion remavals in filter cake to be not thorough, and tantalum powder is caused to dry
Process is corroded and is hydrolyzed again, so impurity content is higher in tantalum powder, these impurity differences are not until final products are also complete
It totally disappeared and remove, and seriously affected tantalum powder electric property, increase tantalum powder leakage current, weight specific volume reduces, loss increase；Comparing
In example 2, acid is not used in washing, the alkali that the metallic sodium being mingled in tantalum powder mixture, metallic potassium generate is made tantalum powder be corroded,
And generation is insoluble in potassium tantalate/inclined potassium tantalate of water and sodium tantalate/sodium metatantalate, tantalum powder yield is greatly lowered, impurity
It is higher；In 2 production process of comparative sample using rinsing bowl, stir washing trough, descaling bath, filter, personnel, which operate, to be needed to throw washing, throws and stir
It washes, throws pickling, throws diafiltration, dividing disk, the operation that washing is dosed into before drying could be completed by transporting 5 times, and embodiment 1 only needs to throw
Expect, divide disk, transporting only 2 times just can complete to be dosed into the operation before drying, greatly reduce labor intensity, improve work effect
Rate.
Table 2：The impurity analysis result of the process conditions and products therefrom of embodiment 1 and comparative example 1-2
Table 3：The impurity analysis result of product sample
Table 4：The electrical properties analysis result of product sample
Embodiment 2
First, it is substantially same as Example 1 to provide the mixture process comprising tantalum powder, difference part is to be heated to 750
DEG C when, add in potassium floutaramite (K2TaF7) and metallic sodium restored, tantalum powder particle is thinner in the mixture obtained in this way.
Then, alkali metal haloid is removed using the technique identical with embodiment.But since tantalum powder is thinner, aqueous solution
Slower by filter membrane speed, the used time is longer.After being 4 to pH value of water solution after the salt pickling for the use of pH value being 4 35 minutes, stop logical
Enter hydrochloric acid and add in pure water from inlet tube 4, after pure water washes 25 hours, aqueous solution conductivity is less than 200 micro-Siemens (μ in device
s/cm)。
Then, it is removed using technique same as Example 1 ultra-fine grain and removal Ferromagnetic Impurities
Process.
Then, it carries out carrying out pickling dissolving removal of impurities using technique same as Example 1.But since tantalum powder is thin, aqueous solution
Slow by filter membrane speed, the separation used time of spent acid lotion and tantalum powder is longer, 39 hours altogether.
Then, recycling tantalum powder is carried out using technique same as Example 1.
It is to implement sample 2 by above-mentioned tantalum powder number.Sampling analysis implements O, C, K, Na, F content in sample 2.Implement impurity in sample 2
Content is listed in subordinate list 5.Statistics from washing be dosed into drying before whole process water consumption, processing time, transhipment number, tantalum powder receive
Rate is listed in subordinate list 5.
Comparative example 3
It is substantially identical with embodiment to provide the mixture process comprising tantalum powder, difference part is not cut off without tantalum powder
Part and above-mentioned condensed product is all broken into the block less than 15mm.
Then, according to Chinese patent CN102191389A, with deionized water diafiltration, in start diafiltration 10 hours, filter
Washing trough lower part efflux is milky turbidity liquid, and after pH value reaches 14,15 hours pH value reaches 8 or so, changes 50 DEG C or so and goes
Ionized water is washed；Due to tantalum powder large specific surface area, average grain diameter is small, and water velocity is slow, and rinsing bowl is just washed till after 87 hours
The conductivity of middle aqueous solution is less than 10 μ s/cm, filters the first filter cake.
Then, continue to be stirred washing according to Chinese patent CN102191389A.It is average due to tantalum powder large specific surface area
Grain size is small, sedimentation it is difficult in addition can not supernatant, stir after washing and the solid mixture comprising tantalum powder be transferred to filter, filter
To the second filter cake.
Then, continue to carry out pickling according to Chinese patent CN102191389A.It is filtered after pickling, 95 is filtered with deionized water
Conductivity is washed till after hour less than 10 μ s/cm, third filter cake is obtained by filtration.
Then, it is recycled.Filter cake is divided in corrosion resistant charging tray, filter cake thickness is less than 30mm, less than air
It presses in 0.08MPa negative pressure devices, is dried under 80 DEG C of drying temperature, sieving obtains initial tantalum powder.It is by above-mentioned tantalum powder number
Comparative sample 3.O, C, K, Na, F content in sampling analysis comparative sample 3.Impurity content is listed in subordinate list 5 in comparative sample 3.It counts from water
Wash be dosed into drying before whole process water consumption, processing time, transhipment number, be listed in subordinate list 5.
The implementation sample 2 of acquisition and comparative sample 3 are granulated, adulterated, then while under vacuum at 1000 DEG C of heat
Reason 30 minutes obtains heat treatment tantalum powder, the magnesium powder of tantalum powder weight 7% is added in the tantalum powder after heat treated, in 750 DEG C of deoxidations 4
Hour, the product tantalum powder for tantalum electrolytic capacitor anode is obtained, the tantalum powder number for implementing to obtain after sample 2 is handled is embodiment production
Product sample 2, the tantalum powder number obtained after the processing of comparative sample 3 is comparative example product sample 3.The chemical impurity of sampling and measuring tantalum powder, as a result
It is listed in Table 6 below.
With above-mentioned two product sample tantalum powder 50mg, it is pressed into diameter 2.0mm, density 5.0g/cm3Briquet, will be above-mentioned
Briquet is sintered 20 minutes for 1050 DEG C in vacuum drying oven, sintered body is formed, by 0.0010mol/L of the above-mentioned agglomerate at 80 DEG C
H3PO4Aqueous solution middle-jiao yang, function of the spleen and stomach polarizes, and boosts to 10V with the current density of 110mA/g, constant pressure forms anode block in 60 minutes.By above-mentioned sun
Pole block is in 0.0102mol/L H3PO47V leaks hunting electric current in aqueous solution, in 3.9099mol/L H2SO4120Hz is tested in aqueous solution
Capacity (CV) and loss (tg δ) value, are as a result listed in table 7.
In comparative example 3, due to tantalum powder large specific surface area, average grain diameter is small, is washed using static state, and water velocity is slow, effect
Rate is extremely low.It can be seen that in comparative example 3 from table 5, table 6,7 data of table, since all alkali metal haloids and tantalum powder are integrated
Tantalum powder purification, and static water-washing method separation tantalum powder and alkali metal haloid are carried out, still with static diafiltration mode after pickling
Tantalum powder and acid solution are detached, tantalum powder water consumption is big, and processing time is long, and there are dead angles in filter cake, and acid solution and other ion remavals are not thorough
Bottom causes tantalum powder to corrode and hydrolyze again in drying course, so impurity content is higher in tantalum powder, these impurity differences are always
It is not also completely eliminated, and seriously affected tantalum powder electric property to final products, increases tantalum powder leakage current, weight specific volume drop
It is low, loss increase；In 3 production process of comparative sample using rinsing bowl, stir washing trough, descaling bath, filter, personnel's operation needs to throw water
It washes, throw to stir and wash, throw pickling, throw diafiltration, dividing disk, transhipment could complete to wash the operation being dosed into before drying for 5 times, and embodiment 2
It only needs to feed intake, divide disk, transporting only 2 times just can complete to be dosed into the operation before drying, greatly reduce labor intensity, improve
Working efficiency.
Table 5：The impurity analysis result of the process conditions and products therefrom of embodiment 2 and comparative example 3
Table 6：Product sample analysis result
Table 7：The electrical properties analysis result of product sample
Embodiment 3
Process conditions are substantially the same manner as Example 2, and difference part is first, second acidic electrolyte solution, third, the
Four electrolyte solutions are all formulated using sulfuric acid.
Embodiment 4
Technique is substantially the same manner as Example 2, and difference part is first, second acidic electrolyte solution, third, the 4th electricity
Electrolyte solution is formulated using nitric acid.
Embodiment 5
Technique is substantially the same manner as Example 2, and difference part is first, second acidic electrolyte solution, third, the 4th electricity
Electrolyte solution is formulated using hydrofluoric acid.
Embodiment 6
Technique is substantially the same manner as Example 2, and difference part is that third, the 4th electrolyte solution use potassium chloride (KCl)
It is formulated.
Embodiment 7
Technique is substantially the same manner as Example 2, and difference part is that the hydrochloric acid in mordant replaces with sulfuric acid and is formulated.
Embodiment 8
Technique is substantially the same manner as Example 2, and difference part is that the hydrochloric acid in mordant replaces with nitric acid and is formulated, and
And pickling dissolving dedoping step i) operations are repeated 2 times.
The target powder that embodiment 3-8 is obtained by embodiment 2 is sampled, statistical correlation index, and carried out by same process
Subsequent processing prepares and implements product sample 3-8 and analyze its electric property, is as a result included in table 8, table 9, table 10.
Table 8：The process conditions of embodiment 3-8 and the impurity analysis result of products therefrom
Table 9：The analysis result of product sample
Table 10：The electrical properties analysis result of product sample
Claims (6)
1. a kind of method that use device purifies out target powder from the mixture comprising target powder, the mixture is with gold
Belong to sodium (Na) and restore potassium floutaramite (K2TaF7) obtained reaction product, the wherein reaction product obtains in the following way：
With metallic sodium (Na) reduction potassium floutaramite (K in reduction vessel2TaF7), after the completion of reaction, stop stirring before condensation
It mixes, makes tantalum powder sedimentation layering, be divided into the part without tantalum powder and the part comprising tantalum powder；
The reaction product is taken out from reduction reaction container, part of the excision without tantalum powder leaves the reaction comprising tantalum powder
Product is as the mixture comprising tantalum powder；Mixture comprising tantalum powder is broken into granularity as below 20mm blocks,
The method includes the following steps：
A alkali metal haloid) is removed；
B ultra-fine grain) is removed；
C Ferromagnetic Impurities) are removed；
D) pickling dissolving removal of impurities；With
E tantalum powder) is recycled,
Wherein step A) including following sub-step：
1) the first acidic electrolyte solution is added in by inlet tube and puts into the mixture comprising tantalum powder in described device, simultaneously
Start stirring, first acidic electrolyte solution is the various inorganic acid for not generating precipitation and/or does not generate the organic of precipitation
One kind of acid and/or several mixed acid, wherein inorganic acid are in hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid and their mixing
Acid；
2) return pump is connected to the interlayer of the device, and starts return pump；
3) the second acidic electrolyte solution is continuously added as the various inorganic acids for not generating precipitation from bottom by the inlet tube
And/or the mixed acid of the organic acid of precipitation is not generated, it is kept stirring and evacuates, aqueous solution is made to pass through filter membrane, detached with powder,
Aqueous solution is reduced to pH value by alkalinity and replaces acidic electrolyte solution after 4-6, to add in pure water in the device, continues to wash, directly
Aqueous solution conductivity is less than 2,000 micro-Siemens (μ s/cm) in device, then stops stirring, stops adding in pure water, stops taking out
It is empty；
4) the third electrolyte solution for not generating precipitation is added in, after tantalum powder is made to settle 20-30 minutes, liquid is taken out by outlet tube
Phase, and the tantalum powder on filter membrane is flushed to described device bottom,
Wherein step 1) and 3) in mixing speed be 0.01-3000 revs/min respectively or simultaneously,
Step B is wherein carried out in the following way)：
The 4th electrolyte solution for not generating precipitation is added in into described device, and passes through blender and is stirred 3-20 minutes,
Then stop stirring and being precipitated, liquid phase, and step B taken out by outlet tube) it repeats 1-30 times,
Step C is wherein carried out in the following way)：Concentration equipment is inserted into electrolyte solution and is stirred, then takes out magnetic separation
Device takes Ferromagnetic Impurities in tantalum powder, and step C out of) it repeats 1-30 times,
Wherein described device includes upper and lower two parts to be linked together with flange from top to bottom；
Its middle and upper part is divided into columnar filtration fraction；
Lower part is divided into that top is cylindrical and bottom is rounded or oval groove body, and top carries stirring bar；
Wherein the groove body, which is equipped with, extends to the inlet tube of bottom, and outlet tube, bottom is equipped with baiting valve, be equipped in groove body agitating paddle and
Concentration equipment, agitating paddle and cell wall are in the angle of 0-30 degree and being capable of oscilaltions；
Wherein described filtration fraction carries the interlayer that can provide vacuum；The wherein described inlet tube top for extending to bottom, which carries, to be divided
The aperture of aproll stream, the outlet tube top can be variously-shaped, and optionally with filter element, can rise up and down
Drop,
Wherein target powder is selected from tantalum powder, niobium powder, tantalum-niobium alloy powder and niobium monoxide powder,
Wherein the mixture comprising target powder is the mixture for including tantalum powder, which is to go back protofluorine tantalum with metallic sodium (Na)
Sour potassium (K2TaF7) obtained reaction product.
2. the method as described in claim 1, wherein in step B) detailed description in carry out the precipitation 20-30 minutes.
3. method as claimed in claim 1 or 2, wherein being carried out at the same time step B in the following way) and C) or simultaneously repeat to walk
Rapid B) and C)：It is stirred by concentration equipment, then takes out concentration equipment, take Ferromagnetic Impurities in tantalum powder out of.
4. method as claimed in claim 1 or 2, wherein step D) including following sub-step：
I) mordant is added in into described device to be stirred, then stop stirring, after precipitating 5-50min, taken by outlet tube
Go out the spent acid lotion that the overwhelming majority includes dissolved impurity, i) will repeat 1-3 times；
Ii) in the case of stirring, cold pure water is continuously added from bottom into described device by inlet tube, starts return pump,
Aqueous solution is made to pass through filter membrane, is detached with tantalum powder；
Iii it) after aqueous solution conductivity is less than 15 micro-Siemens (μ s/cm) in device, adds in hot pure water and replaces cold pure water, work as dress
Interior aqueous solution conductivity is put less than after 10 micro-Siemens (μ s/cm), stops stirring, stops adding water, it is anhydrous by rear in filter membrane
Stop evacuating, leave water and the mixture of tantalum powder in the device, the pure water is the pure water of 12 megaohms of resistivity ＞.
5. method as claimed in claim 1 or 2, wherein carrying out step E)：
Will be from step D) obtained mixture is all put into filter, and most water are detached, then divide obtained filter cake to disk
Vacuum drying obtains target powder.
6. the mixing time in method as claimed in claim 4, wherein sub-step i) is 1-6 hours.
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| PCT/CN2012/086812 WO2014094220A1 (en) | 2012-12-18 | 2012-12-18 | Target powder purification method and device |
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| CN1023548C (en) * | 1989-11-20 | 1994-01-19 | 宁夏有色金属冶炼厂 | Method for producing ta powder used in capacitor |
| US7182925B2 (en) * | 2003-04-24 | 2007-02-27 | Osram Sylvania Inc. | Tantalum concentrates dissolution and purification method |
| JP2006249449A (en) * | 2005-03-08 | 2006-09-21 | Art Kagaku:Kk | Method for producing metal tantalum nanosheet and metal tantalum nanosheet produced by the method |
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| CN102191389A (en) * | 2011-04-19 | 2011-09-21 | 潘伦桃 | Rinsing method and device of potassium fluotantalate product obtained through sodium reduction |
| CN102382993A (en) * | 2011-10-09 | 2012-03-21 | 广东致远新材料有限公司 | Preparation method of target-grade ultrahigh-purity tantalum metal |
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