CN102990076A - Stirring water-washing method and device for producing tantalum powder by reducing potassium fluotantalate via metallic sodium - Google Patents
Stirring water-washing method and device for producing tantalum powder by reducing potassium fluotantalate via metallic sodium Download PDFInfo
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- CN102990076A CN102990076A CN2012105481013A CN201210548101A CN102990076A CN 102990076 A CN102990076 A CN 102990076A CN 2012105481013 A CN2012105481013 A CN 2012105481013A CN 201210548101 A CN201210548101 A CN 201210548101A CN 102990076 A CN102990076 A CN 102990076A
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Abstract
The invention relates to a stirring water-washing method and device for producing tantalum powder by reducing potassium fluotantalate via metallic sodium. The water-washing method comprises the following steps of: performing stirring water-washing on the tantalum powder obtained by reducing potassium fluotantalate (K2TaF7) via metallic sodium (Na) which removes alkali metal haloids in an electrolyte solution, so as to remove harmful and indissolvable ultrafine-particle impurities in the tantalum powder; and then performing acid-washing and drying to obtain the initial tantalum powder. The method is high in the yield of tantalum powder; and the obtained tantalum powder is high in purity, good in particle size distribution and porosity, and especially suitable for manufacturing a tantalum electrolytic capacitor.
Description
Technical field
The present invention relates to the hydrometallurgy field, particularly relate to a kind of sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) produce stirring method for washing and the device of tantalum powder.
Background technology
Tantalum is a kind of rare metal, is mainly used in the industries such as electronics industry, chemical industry equipment, metal cutting processing, Aero-Space, the consumption rapid growth of tantalum in recent years, but scarcity of resources.Therefore, effectively utilizing the waste of tantalum resource, minimizing tantalum is a kind of development trend of tantalum industry.
In electronics industry, the main application of tantalum powder is to make tantalum electrolytic capacitor, and capacitor required the miniaturization of height, the reliability of height and the compatibility of sheet piece in recent years.On high end capacitor market, tantalum electrolytic capacitor can constantly satisfy the development trend of above-mentioned capacitor, improves constantly its volume specific volume, reliability, high frequency performance, have simultaneously Low ESR, so the tantalum capacitor share increases constantly.Tantalum powder as tantalum electrolytic capacitor anode main material, require its surface area constantly to increase, to improve the tantalum electrolytic capacitor volumetric capacitance, purity and the physical property of tantalum powder also must constantly be improved simultaneously, reliability, high frequency performance to improve tantalum electrolytic capacitor reduce impedance simultaneously.
Usually, adopt chemical method to produce the tantalum powder, namely adopt sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) method, generating in the product has tantalum powder, sodium fluoride and potassium fluoride, its chemical equation is:
K
2TaF
7+5Na=Ta+5NaF+2KF
In order to obtain the tantalum powder of bigger serface, often in raw material, add alkali halide, such as one or more salt-mixture of sodium chloride (NaCl), potassium chloride (KCl) and potassium fluoride (KF) as diluent; On the other hand, in order to ensure above-mentioned sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) sufficient reacting is thorough, often needs to add excessive sodium metal.Above-mentioned reaction is generally being carried out more than 700 ℃, excessive sodium metal (Na) can be reduced to metallic potassium (K) with potassium ion (K+) under this condition, simultaneously in the molten salt system owing to there is the impurity such as O, generation is insoluble in inclined to one side potassium tantalate and the sodium tantalate/sodium metatantalate of water, they often exist with the form of ultra-fine grain (particle diameter 100nm following), make the content of K, O in the resulting tantalum powder and Na higher.Above-mentioned sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) the tantalum powder that generates of course of reaction is suspended in the melt of alkali halide that sodium fluoride (NaF), potassium fluoride (KF) and diluting salt form and remaining alkali metallic sodium (Na), potassium (K), become tantalum powder and above-mentioned alkali halide mixture after the cooling and be entrained with alkali metallic sodium (Na), the potassium (K) of surplus and be insoluble in the inclined to one side potassium tantalate of water and the condensation piece of sodium tantalate/sodium metatantalate.
At sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) produce in the purification process of tantalum powder, the condensation piece is broken into granule, separate first alkali halide soluble in water and remaining sodium metal, the potassium of reaction.This process, remaining sodium metal, potassium meeting and steeping in water for reconstitution are given birth to following reaction:
2K+2H
2O=2KOH+H
2
2Na+2H
2O=2NaOH+H
2
Form strong alkali solution, strong base solution and tantalum powder are insoluble in inclined to one side potassium tantalate and the sodium tantalate/sodium metatantalate of water with generation together, form again and are harmful to indissoluble ultra-fine grain impurity in the tantalum powder.So, by prior art, sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) to produce the tantalum powder be the tantalum finely starched thing of carrying harmful indissoluble ultra-fine grain impurity secretly before stirring washing.
Chinese patent CN102191389A provides a kind of method for washing: with sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) to be broken into granularity be the following granule of 15mm for the condensation piece of product, in the diafiltration groove, arrive neutral with 15 ℃～35 ℃ cold deionized water diafiltration first, and then carry out diafiltration with the deionized water of 40 ℃～100 ℃ of heat, the electrical conductivity of washing diafiltration groove bottom efflux is lower than 10 μ s/cm, then change over to and stir in the rinsing bowl with the washing of deionized water high-speed stirred, and then through overpickling, oven dry and sieve powder, then carry out subsequent treatment and obtain tantalum powder product.This washing methods more and more can not satisfy the production of the increasing tantalum powder of specific area.Along with the increase of tantalum powder specific area, it is more and more thinner that the tantalum powder directly becomes, and sedimentation is more and more difficult in stirring water-washing process.If in the stirring water-washing process sedimentation time too short, part runs off serious greater than the 100nm tantalum powder, the tantalum powder yield reduces, the parts of fine particle diameter tantalum powder of Effective Raise tantalum powder specific volume runs off simultaneously, can cause the product specific volume to reduce; If the sedimentation time prolongs in the stirring water-washing process, can extend manufacture cycle, a large amount of ultra-fine impurity particles of harmful indissoluble also enters the tantalum powder simultaneously, to have a strong impact on the physical property of product, cause the tantalum electrolytic capacitor leakage current of making to increase, specific volume reduces, impedance increases, and reliability reduces; Simultaneously also can make tantalum powder oxygen (O), potassium (K), sodium (Na) and fluorine (F) increased content, have a strong impact on the electric property of tantalum powder.And the stirring water washing device that Chinese patent CN102191389A provides, adopt the upright mode that stirs of paddle, form easily whirlpool in the whipping process, make stirring insufficient, clean result is bad, can not fully remove the impurity that is mingled with in the tantalum powder, make oxygen in the tantalum powder (O), potassium (K), sodium (Na), carbon (C) and fluorine (F) increased content high, have a strong impact on the electric property of tantalum powder.Especially, F, the K in the tantalum powder and C have a strong impact on the electric property of tantalum powder.
Summary of the invention
Purpose of the present invention is exactly some or all defectives that overcome above-mentioned prior art, and a kind of stirring water washing device of the tantalum powder of purifying out from sodium metal (Na) reduction potassium floutaramite (K2TaF7) product is provided.
Another object of the present invention provides the stirring method for washing of the tantalum powder of purifying out from the product (can be considered raw material) of sodium metal (Na) reduction potassium floutaramite (K2TaF7).
In one aspect of the invention, a kind of stirring water washing device of the tantalum powder of purifying out from the product of sodium metal (Na) reduction potassium floutaramite (K2TaF7) is provided, it is characterized in that: comprise that top is that cylindrical shape, bottom are conical cell body, this cell body is used for holding the mixture that comprises described product and the aqueous solution, this cell body top is provided with the washing water inlet pipe, the bottom is provided with adjutage and baiting valve, be provided with baffle plate on the cell body inwall, the agitating device that is comprised of puddler and stirrer paddle is arranged in the cell body.
In a preferred embodiment of the invention, baffle plate evenly is arranged on the cell body inwall.
In one embodiment of the invention, this device and described mixture contact portion by the various materials of wear-resisting and acid and alkali-resistance salt corrosion for example stainless steel make.
In one embodiment of the invention, this device has 2～4 baffle plates, and its length is preferably 1/5～3/4 of cell body height.
In one embodiment of the invention, the length of wherein said stirrer paddle is 1/3～2/3 of cell body diameter;
In one embodiment of the invention, stir the angle that loom and cylinder cell wall are 30～60 degree, stirrer paddle is in the position, boundary of cell body bucket section and cone.
In another aspect of this invention, provide a kind of purification of products from sodium metal (Na) reduction potassium floutaramite (K2TaF7) to go out the stirring method for washing of tantalum powder, comprised the steps:
1) will remove in the above-mentioned stirring water washing device of Ta powder (being raw material) input of alkali metal haloid with the pure water dissolving first, this Ta powder obtains with sodium metal (Na) reduction potassium floutaramite (K2TaF7);
2) pure water is added in the stirring water washing device of the present invention's design, add electrolyte solution;
3) the starting device agitating device stirs, and then stops to stir, and carries out sedimentation;
4) sedimentation 5～60min emits liquid phase;
5) repetition above-mentioned steps 2), 3), 4) repeatedly;
6) mixture of above-mentioned tantalum powder and liquid is put into filter, suction filtration is removed most of moisture content, then sends to pickling, oven dry, obtains initial tantalum powder.
In one embodiment of the invention, described step 2) tantalum grain weight amount is 1:10～2000 with the ratio that adds pure water weight in, preferred 1:30～200, and this ratio is also referred to as solid-to-liquid ratio.
In one embodiment of the invention, described step 2) electrolyte solution refers to one or more mixed solution of various acid, alkali, salt in, the mixed solution of one or more of preferred sodium chloride (NaCl), potassium chloride (KCl), potassium fluoride (KF), sodium fluoride (NaF) and inorganic acid, more preferably hydrochloric acid.
In one embodiment of the invention, mixing speed is 0.01～3000 rev/min in the described step 3); Preferred 50～300 rev/mins.
In one embodiment of the invention, mixing time is 0.01～200 minute in the described step 3), preferred 3～20 minutes, and preferred 3～15 minutes.
In one embodiment of the invention, number of repetition is to surpass 1 time in the described step 5), preferred 1～30 time, and preferred 5～20 times.
Description of drawings
Fig. 1 is the structural representation that agitator treating sodium metal (Na) reduction potassium floutaramite (K2TaF7) is produced the stirring rinsing bowl of tantalum powder among the present invention, and Reference numeral wherein is explained as follows:
1 water inlet pipe; 2 cell bodies; 3 baffle plates; 4 stirrer paddles; 5 tantalum powder; 6 baiting valves; 7 adjutages; 8 puddlers; 9 liquid phases
Fig. 2 is tantalum powder Granularity Distribution figure, and the curve that wherein peak is the highest is corresponding to sample 1, and the minimum curve in peak is corresponding to comparison specimen 2, and another curve is corresponding to comparison specimen 1.
The specific embodiment
Fig. 1 is the device example schematic that the present invention is used for tantalum powder agitator treating, stirring rinsing bowl body and function stainless steel makes, comprise that top is cylindrical shape cylinder section, the bottom is the cell body 2 in conical tapering, stainless steel puddler 8 by the driving of motor (not shown), the lower end of puddler is stirrer paddle 4, and stirrer paddle 4 is welded on puddler 8 lower ends, and stirrer paddle is in cylinder section and the position, boundary, tapering of cell body 2; On the lower position on 2 section's inwalls of cell body is provided with 4 uniform baffle plates 3, and baffle plate 3 is with making with the cell body same material; Tantalum powder 5 is deposited in the tank diameter bottom after the sedimentation, and tank diameter 2 tops are the liquid phases 9 that contain tantalum compound; There is adjutage 7 centre of tank diameter 2 on the lower position, its height on the cylindrical shell depend on stir washing after height after the sedimentation of tantalum powder, the position of operated by rotary motion high 10～20cm of horizontal plane of tantalum powder after than sedimentation; The above has water inlet pipe 1, adds electrolyte solution when stirring washing; It is baiting valve 6 below the tapering; Amount of water generally be tantalum grain weight amount with the ratio of solution weight is 1:30～1:150 when stirring washing; Mixing speed is 50～200 rev/mins when stirring washing; Stir general 5～20 times of washing, each stirring washing 3～15 minutes that continue; By stirring washing, the tantalum powder particles fully contacts with the aqueous solution, makes wherein impurity by flush away.The electrolyte that adds 500～2000ml during the stirring washing is controlled the rear tantalum powder sinking speed of stirring washing, within the relatively-stationary time, particle diameter is deposited to greater than the tantalum powder particles of 100mn stirs the rinsing bowl bottom, put into the waste recovery system through the liquid phase of sedimentation from adjutage 7 after will stirring washing.Stirring sedimentation goes out after the washing tantalum powder puts into by baiting valve 6 and changes descaling bath over to after the diafiltration groove is drained and proceed further processing, for example pickling.
Embodiment
Following examples adopt device as shown in Figure 1 to carry out, the interior diameter 120cm of cylindrical shape cylinder section wherein, and high 250cm, stirrer paddle make with stainless steel, and baffle plate 3 is with making with the cell body same material, being of a size of 40cm * 15cm * 2cm.
Use first sodium metal (Na) reduction potassium floutaramite (K2TaF7) to obtain Ta powder, then remove the alkali metal haloid with the pure water dissolving.With the tantalum powder of gained be divided into sample 1, comparison specimen 1 is carried out respectively agitator treating with comparison specimen 2.
In above-mentioned sample 1 input stirring rinsing bowl as shown in Figure 1, in solid: liquid is that the ratio of 1:50 adds deionized water, the HCl 500ml that adds again 4.0mol/L, start paddle, stirred 10 minutes with 120 rev/mins rotating speeds, stop to stir, leave standstill, after the sedimentation 5 minutes, the suspension that stirs rinsing bowl top is put into accumulator tank; So repeatedly carry out 10 times, change pickling over to.The pickling post-drying is sieved with 150 mesh sieves.Press GB/T 15076.1～15 tantalum niobium chemical analysis methods and analyze tantalum powder O, C, K, Na, Fe, Ni, Cr, F, the results are shown in Table 1.
Comparative example 1
Above-mentioned comparison specimen 1 is dropped in the vertical stirring rinsing bowl of placing of paddle, in solid: liquid is that the ratio of 1:20 adds deionized water, start paddle, stirred 10 minutes with 120 rev/mins rotating speeds, stop to stir, leave standstill, sedimentation was put into accumulator tank with the suspension that stirs rinsing bowl top after 5 minutes; So repeatedly carry out 10 times, change pickling over to.The pickling post-drying is sieved with 150 mesh sieves.Press O, K, C, F, Na, Fe, Ni, the Cr of embodiment 1 methods analyst tantalum powder, the results are shown in Table 1.
Comparative example 2
Above-mentioned comparison specimen 2 is dropped in the vertical stirring rinsing bowl of placing of paddle, in solid: liquid is that the ratio of 1:20 adds deionized water, start paddle, stirred 10 minutes with 120 rev/mins rotating speeds, stop to stir, leave standstill, sedimentation was put into accumulator tank with the suspension that stirs rinsing bowl top after 30 minutes; So repeatedly carry out 10 times, change pickling over to.The pickling post-drying is sieved with 150 mesh sieves.Press O, K, C, F, Na, Fe, Ni, the Cr of embodiment 1 methods analyst tantalum powder, the results are shown in Table 1.
The initial tantalum powder sample 1, comparison specimen 1 and the comparison specimen 2 that obtain are carried out granulation, the while was 1150 ℃ of heat treatments 30 minutes after the granulation, obtain heat treatment tantalum powder, the magnesium powder that adds tantalum grain weight amount 4% in the tantalum powder after the heat treated, 820 ℃ of deoxidations 4 hours, obtain the tantalum powder for the tantalum electrolytic capacitor anode.With embodiment 1 methods analyst tantalum efflorescence impurity, the results are shown in Table 2.Press the bioassay standard funnel method (Hall flowmeter) of GB/T1482 metal dust flowability and measure tantalum powder flowability, the results are shown in Table 2.Analyze the tantalum Powder Particle Size with U.S. Beckman laser particle size analyzer LS 230 and distribute particle size distribution figure such as Fig. 2.
With above-mentioned heat treatment, the tantalum powder 100mg behind the oxygen falls, be pressed into diameter 3.0mm, density is the briquet of 5.0g/cm3, with above-mentioned briquet 1200 ℃ of sintering 20 minutes in vacuum drying oven, form sintered body, above-mentioned agglomerate in 0.1wt%H3PO4 aqueous solution middle-jiao yang, function of the spleen and stomach polarization, is boosted to 20V with the current density of 110mA/g, and constant voltage formed anode block in 180 minutes.With above-mentioned anode block 14V in 0.1wt%H3PO4 aqueous solution electric current that leaks hunting, 120Hz test capacity (CV) and loss (tg δ) value the results are shown in table 3 in the 30.5wt%H2SO4 aqueous solution.
Can find out that from table 1, table 2, table 3 data comparison specimen 1 is because the sedimentation of tantalum powder is inadequate, it is more that the contributive parts of fine tantalum of product specific volume powder is run off, and therefore initial tantalum powder O is low, and final products CV is low; Comparison specimen 2 is because the sedimentation time is long, and superfine powder is many, and the initial powder impurity content is higher, because superfine powder is too many, the product physical property is poor, poor fluidity, and simultaneously, superfine powder is little to the contribution of tantalum powder specific volume, and is large on the leakage current impact, so the product specific volume is not high, and leakage current is poor.Adopt method of the present invention to stir the sample 1 of washing owing to stir washing fully with stirring water washing device, effect of settling is good, and impurity is low, and physical property is superior, and the product leakage current is low, and specific volume is high.
Table 1: initial tantalum powder analysis result
As can be seen from the table, the F content of sample 1, K content and C content obviously F content and the C content than comparison specimen 1 and 2 are lower, and whole impurity content is lower.
Table 2: heat treatment, fall tantalum powder analysis result behind the oxygen
Table 3: electrical analysis result
| Leakage current (nA/ μ FV) | Capacity C V (μ FV/g) | Loss tg δ (%) | |
| |
0.68 | 144215 | 46.0 |
| |
0.55 | 128038 | 44.8 |
| |
0.73 | 136202 | 50.5 |
Claims (12)
1. one kind from sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) product in purify out the stirring water washing device of tantalum powder, it is characterized in that: comprise that top is that cylindrical shape, bottom are conical cell body, this cell body is used for holding the mixture that comprises described product and the aqueous solution, this cell body top is provided with the washing water inlet pipe, the bottom is provided with adjutage and baiting valve, be provided with baffle plate on the cell body inwall, wherein be provided with the agitating device that is formed by puddler and stirrer paddle in the cell body.
2. according to stirring water washing device claimed in claim 1, wherein the part that contacts with described mixture of this device by the material of wear-resisting and acid and alkali-resistance salt corrosion for example stainless steel make.
3. according to stirring water washing device claimed in claim 1, wherein this device has 2～4 baffle plates, and its length is preferably 1/5～3/4 of cell body height.
4. according to stirring water washing device claimed in claim 1, the length of wherein said stirrer paddle is 1/3～2/3 of cell body diameter.
5. according to stirring water washing device claimed in claim 1, wherein stir the angle that loom and cylinder cell wall are 30～60 degree, stirrer paddle is in the position, boundary of cell body bucket section and cone.
6. use as among the claim 1-5 each device reduce potassium floutaramite (K from sodium metal (Na)
2TaF
7) product in purify out the method for tantalum powder.
7. one kind from sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) product in purify out the stirring method for washing of tantalum powder, comprise the steps:
1) will dissolve the Ta powder of having removed the alkali metal haloid with pure water and drop into as in each described device among the claim 1-5, this Ta powder is with sodium metal (Na) reduction potassium floutaramite (K
2TaF
7) obtain;
2) pure water is dropped in the described device, add electrolyte solution;
3) the starting device agitating device stirs, and then stops to stir, and carries out sedimentation;
4) sedimentation 5～60min emits liquid phase;
5) repetition above-mentioned steps 2), 3), 4) repeatedly;
6) mixture of above-mentioned tantalum powder and liquid is put into filter, suction filtration is removed most of moisture content, then sends to pickling, oven dry, obtains initial tantalum powder.
8. tantalum grain weight amount is 1:10～2000 with the ratio that adds pure water weight in accordance with the method for claim 7, wherein said step 2), preferred 1:30～200;
9. in accordance with the method for claim 7, wherein said step 2) electrolyte solution refers to one or more mixed solution of various acid, salt in, the mixed solution of one or more of preferred sodium chloride (NaCl), potassium chloride (KCl), potassium fluoride (KF), sodium fluoride (NaF) and inorganic acid, more preferably hydrochloric acid;
10. according to the method described in the claim 7, mixing speed is 0.01～3000 rev/min in the wherein said step 3); Preferred 50～300 rev/mins.
11. according to the method described in the claim 7, mixing time is 0.01～200 minute in the wherein said step 3), preferred 3～20 minutes, and preferred 3～15 minutes.
12. according to the method described in the claim 7, number of repetition is to surpass 1 time in the wherein said step 5), preferred 1～30 time, and preferred 5～20 times.
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|---|---|---|---|
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Cited By (5)
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| WO2015096048A1 (en) * | 2013-12-25 | 2015-07-02 | 宁夏东方钽业股份有限公司 | Capacitor grade high specific volume tantalum powder improving electrical performance and preparation method therefor |
| WO2015100519A1 (en) * | 2013-12-30 | 2015-07-09 | 宁夏东方钽业股份有限公司 | Preparation method of high-nitrogen-content capacitor grade tantalum powder and tantalum powder prepared therefrom and tantalum capacitor |
| CN105583406A (en) * | 2016-03-29 | 2016-05-18 | 宁夏东方钽业股份有限公司 | Preparation method of metal powder with low oxygen content |
| CN106312084A (en) * | 2016-09-14 | 2017-01-11 | 从化钽铌冶炼厂 | Accurate control method of tantalum powder reduction system |
| CN109468473A (en) * | 2018-12-29 | 2019-03-15 | 株洲硬质合金集团有限公司 | A kind of method of tantalum metallurgy by-product complex salt recycling and reusing |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015096048A1 (en) * | 2013-12-25 | 2015-07-02 | 宁夏东方钽业股份有限公司 | Capacitor grade high specific volume tantalum powder improving electrical performance and preparation method therefor |
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| WO2015100519A1 (en) * | 2013-12-30 | 2015-07-09 | 宁夏东方钽业股份有限公司 | Preparation method of high-nitrogen-content capacitor grade tantalum powder and tantalum powder prepared therefrom and tantalum capacitor |
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| CN106312084A (en) * | 2016-09-14 | 2017-01-11 | 从化钽铌冶炼厂 | Accurate control method of tantalum powder reduction system |
| CN106312084B (en) * | 2016-09-14 | 2018-08-03 | 广东广晟稀有金属光电新材料有限公司 | A kind of accuracy control method of tantalum powder also original system |
| CN109468473A (en) * | 2018-12-29 | 2019-03-15 | 株洲硬质合金集团有限公司 | A kind of method of tantalum metallurgy by-product complex salt recycling and reusing |
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