CN116102065A - Preparation method of high-purity niobium pentoxide superfine powder - Google Patents
Preparation method of high-purity niobium pentoxide superfine powder Download PDFInfo
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- CN116102065A CN116102065A CN202310137992.1A CN202310137992A CN116102065A CN 116102065 A CN116102065 A CN 116102065A CN 202310137992 A CN202310137992 A CN 202310137992A CN 116102065 A CN116102065 A CN 116102065A
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- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 title claims abstract description 55
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000000843 powder Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 42
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 claims abstract description 30
- 238000001354 calcination Methods 0.000 claims abstract description 25
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 claims abstract description 25
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 20
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 20
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000012528 membrane Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 16
- 239000013078 crystal Substances 0.000 description 11
- 239000002245 particle Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- 239000012535 impurity Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000010955 niobium Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- 229910000484 niobium oxide Inorganic materials 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- -1 iron Chemical compound 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 229910000592 Ferroniobium Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 206010049155 Visual brightness Diseases 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 229910001439 antimony ion Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- ZFGFKQDDQUAJQP-UHFFFAOYSA-N iron niobium Chemical compound [Fe].[Fe].[Nb] ZFGFKQDDQUAJQP-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of high-purity niobium pentoxide superfine powder, which comprises the steps of dissolving niobium hydroxide in oxalic acid to support niobium oxalate solution, then reacting the solution with ammonia water through a microreactor, aging, dehydrating, washing, drying and calcining the product to obtain the niobium pentoxide superfine powder with good dispersibility and high purity, wherein the purity of the powder is greatly improved compared with that of the raw materials, and the percentage content of niobium pentoxide is more than 99.995 percent.
Description
Technical Field
The invention relates to the field of high-purity ultrafine powder preparation, in particular to a preparation method of high-purity niobium pentoxide ultrafine powder.
Background
Niobium (Nb) is a metal with a silver gray luster, typically a metal body centered cubic structure. Niobium is in VB group of periodic table, has the advantages of soft quality, good ductility, low vapor pressure, large heat conductivity, high melting point boiling point, strong corrosion resistance, etc., and is widely applied to steel, electronics, chemistry, nuclear energy, superconductivity and aerospaceAnd the like in various industrial fields. The high-purity niobium pentoxide is used as an important raw material and a functional material in the high and new technology material industry, and is widely applied to various tip technical fields such as new energy sources, optics, communication, military, electronics, chemical industry, biomedicine and the like. At present, the domestic niobium pentoxide production process generally takes tantalum-niobium concentrate as raw material, adopts HF and H 2 SO 4 The hydrometallurgical process for preparing niobium oxide by decomposing ore with mixed acid includes such steps as mechanical grinding, regulating acidity with decomposing liquid, extracting with organic solvent to obtain organic phase containing tantalum and niobium, acid washing to remove impurities, extracting with organic solvent again, neutralizing with ammonia, depositing, filtering, baking and calcining. Due to the large number of process steps and the presence of a large amount of fluoride and sulfate ions in the solution during the synthesis of the product, the niobium hydroxide produced in the precipitation step is contaminated and difficult to clean, and finally remains partially in the product powder to affect the purity of niobium pentoxide. The niobium pentoxide powder obtained by the process has the general purity of 99.9 percent. The process of optimizing extraction stage number, extractant, acid concentration and the like can also be used for obtaining the niobium pentoxide with higher purity, such as the method for preparing the niobium pentoxide by taking ferroniobium as raw material in Chinese patent publication No. CN102424420A, which discloses a method for preparing the niobium pentoxide with purity up to 99.99%. However, the process requires strict control of process parameters of each step in the process, and the control conditions are severe, so that the control deviation can lead to the product purity not reaching the standard.
With the rapid development of touch screen displays in recent years, metal oxide targets have also rapidly developed. The 2021 global touch screen display market size was about 4247 gigabytes, of which about 50% came from china production. In addition, china is the most important application market. Therefore, the development of targets in China puts more demands. The niobium oxide target is an important material for preparing shadow-eliminating ITO (indium tin oxide) glass. The shadow-eliminating ITO glass is prepared by plating a layer of anti-reflection and anti-reflection film between an ITO film and glass in a liquid crystal display, and has the following advantages when the ITO conductivity is satisfied: 1) The glass has high transmittance, and better visual brightness can be obtained by reducing the influence of ambient light on the premise of the same backlight source; 2) The available high transmittance reduces the visual contrast of the work area and the non-work area, lightens the work line of the capacitive screen and improves the visual effect. With the continuous development of touch screen displays, higher requirements are put on the purity and the compactness of niobium pentoxide targets. This in fact puts higher demands on the purity and particle size, dispersibility, etc. of the raw materials of the target, i.e., the niobium pentoxide powder, on the one hand, it is required that the niobium pentoxide powder has a higher purity, and on the other hand, it is also required that the niobium pentoxide powder has a smaller particle size and a better dispersibility, which the current process has failed to meet.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity niobium pentoxide superfine powder, aiming at the defects that the purity of niobium pentoxide powder prepared by the prior art is difficult to improve, the dispersibility is insufficient and the like. The method comprises the following steps:
(1) Dissolving niobium hydroxide in oxalic acid at high temperature to form niobium oxalate solution;
(2) Respectively feeding a niobium oxalate solution with a certain concentration and an ammonia solution into a membrane dispersion microreactor to enable the niobium oxalate solution to react with the ammonia solution to generate niobium hydroxide precipitate, wherein the concentration of the niobium oxalate is 0.1-0.3mol/L, the concentration of the ammonia solution is 10-35wt%, and the pH of the reaction end point is 8.5-10.0;
(3) Aging, dehydrating and washing the precipitate, and drying and calcining the precipitate to obtain the high-purity niobium pentoxide superfine powder, wherein the calcining temperature is 500-1200 ℃.
The membrane-dispersed microreactor used in the step (1) may be a flat plate membrane or a tubular membrane.
The pore size of the membrane used in the step (2) is between 1 μm and 100 μm.
The film material used in the step (2) can be plastic, metal, glass or ceramic.
The temperature of the reaction in the step (2) is 10-80 ℃.
The aging temperature in the step (3) is 50-90 ℃ and the aging time is 0.5-3 hours.
The niobium hydroxide used in the patent is a precursor obtained through precipitation reaction in the current process for preparing the niobium pentoxide product, and the niobium pentoxide is obtained through further calcination. In the method, the prior niobium hydroxide product is dissolved by oxalic acid to prepare niobium oxalate, and metal ions in the niobium hydroxide, such as iron, antimony ions and the like, and fluoride ions and sulfate ions are dissolved along with the niobium hydroxide; in the precipitation process, iron and antimony plasma only partially precipitate due to the solubility product, and most of the main impurity anions such as fluoride and sulfate are left in the solution, so that little precipitation occurs, and part of metal impurities and most of anion impurities are removed in the prepared niobium hydroxide precipitate. Although some ammonia and oxalic acid root are mixed in the precipitate, most of the ammonia and oxalic acid root are removed in the washing process, and the residual ammonia and oxalic acid root are decomposed and removed in the calcining process, so that no new impurities are brought, and the purity of the prepared niobium pentoxide is higher and higher than 99.995%. In addition, the patent adopts the membrane dispersion microreactor to carry out reaction precipitation, so that the niobium oxalate and the ammonia water can be uniformly mixed and reacted in a very short time, and the formation of relatively uniform supersaturation degree is facilitated, and the niobium hydroxide powder with relatively uniform particle size and relatively good dispersibility is obtained; the particle size of the niobium hydroxide powder can be controlled by controlling the conditions of reactant concentration, membrane pore diameter, reaction temperature, aging temperature and the like, and finally the niobium pentoxide powder with controllable particle size and good dispersibility is obtained by roasting.
Drawings
Fig. 1 is an XRD pattern of niobium pentoxide powder prepared in this patent.
Fig. 2 is a transmission electron microscope image of niobium pentoxide powder prepared in this patent.
Fig. 3 is a transmission electron microscope image of niobium pentoxide powder prepared in comparative example.
Detailed Description
The invention provides a preparation method of high-purity niobium pentoxide superfine powder. The method comprises the following steps:
(1) Dissolving niobium hydroxide in oxalic acid at high temperature to form niobium oxalate solution;
(2) Respectively feeding a niobium oxalate solution with a certain concentration and an ammonia solution into a membrane dispersion microreactor to enable the niobium oxalate solution to react with the ammonia solution to generate niobium hydroxide precipitate, wherein the concentration of the niobium oxalate is 0.1-0.3mol/L, the concentration of the ammonia solution is 10-35wt%, and the pH of the reaction end point is 8.5-10.0;
(3) Aging, dehydrating and washing the precipitate, and drying and calcining the precipitate to obtain the high-purity niobium pentoxide superfine powder, wherein the calcining temperature is 500-1200 ℃.
The membrane dispersion microreactor can be a flat plate membrane or a tubular membrane, the pore diameter of the membrane is 1-100 mu m, and the membrane material can be plastic, metal, glass or ceramic.
The reaction temperature in the membrane dispersion microreactor is between 10 ℃ and 80 ℃, the aging temperature of the reaction precipitation is between 50 ℃ and 90 ℃, and the aging time is between 0.5 and 3 hours.
The preparation method of the high-purity niobium pentoxide superfine powder provided by the invention can further purify niobium hydroxide to prepare the niobium pentoxide superfine powder with purity of more than 99.99%, controllable particle size and good dispersibility.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The niobium hydroxide with the purity of 99.9 percent is adopted as a raw material, and oxalic acid is adopted as follows: niobium hydroxide = 2.7:1, and at 90 deg.c, dissolving niobium hydroxide with oxalic acid. The concentration of the prepared niobium oxalate is controlled by controlling the concentration of oxalic acid. At this ratio, only a very small amount of powder particles of niobium pentoxide are insoluble; when the proportion of oxalic acid is low, the residual part of niobium pentoxide is not dissolved, and the solubility of niobium oxalate in water is not high enough at the moment; when the proportion of oxalic acid is high, there are few insoluble particles, but the consumption of oxalic acid and the consumption of ammonia in the reaction are increased, thereby increasing the production cost.
Feeding a niobium oxalate solution with the concentration of 0.3mol/L and an ammonia water solution with the concentration of 30wt% into a membrane dispersion microreactor, taking niobium oxalate as a disperse phase and ammonia water as a continuous phase, enabling the niobium oxalate and the ammonia water to react to generate niobium hydroxide precipitate, controlling the reaction temperature to be 60 ℃, controlling the reaction end point pH to be 9.6, and using a stainless steel flat plate sintered membrane with the pore diameter of 1 mu m as a membrane; aging the obtained precipitate at 90 ℃ for 3 hours, then dehydrating, washing, drying and calcining to obtain the high-purity niobium pentoxide superfine powder, wherein the calcining temperature is 500 ℃, 800 ℃, 1000 ℃ and 1200 ℃ respectively.
The XRD patterns of niobium pentoxide crystals obtained at three calcination temperatures can be seen in FIG. 1, and different crystal forms can be obtained by controlling different calcination temperatures. The T-type niobium pentoxide crystal is obtained at the calcination temperature of 500 ℃, but amorphous components exist; after the calcination temperature is increased to 800 ℃, the peak shape is sharp, the crystal is purer, and niobium hydroxide is basically all converted into T-shaped niobium pentoxide crystal; when the calcination temperature is 1000 ℃, the T-type niobium pentoxide crystal is mainly used, but a small amount of H-type niobium pentoxide crystal begins to appear; when the calcination temperature was raised to 1200 c, substantially all of the niobium pentoxide crystals were converted to form H.
FIG. 2 is a transmission electron microscope picture of niobium pentoxide obtained by calcining at 800 ℃, and the particle size is about 150nm, and the dispersibility is good.
The purity analysis was performed on the 800 c calcined samples, and the results are shown in table 1, with a purity of 99.9972%. In practice, the product purity is mainly determined by impurities in the niobium hydroxide precursor, and the calcination temperature does not affect the product purity, so that the product purity obtained at other calcination temperatures is unchanged.
TABLE 1 detection results of purity of niobium oxide prepared in example 1
| Determination of elements | Measurement result/(%) | Determination of elements | Measurement result/(%) |
| Main component, nb 2 O 5 | 99.9972 | K | 0.00005 |
| Ta | 0.00008 | Mg | 0.00004 |
| AI | 0.00005 | Mn | 0.00002 |
| As | 0.0001 | Mo | 0.00015 |
| B | 0.00006 | Na | 0.0001 |
| Bi | 0.00004 | Ni | 0.00005 |
| Ca | 0.00018 | Pb | 0.00004 |
| Cd | 0.00004 | Sb | 0.00007 |
| Co | 0.00001 | Si | 0.0005 |
| Cr | 0.00003 | Sn | 0.0004 |
| Cu | 0.00006 | Ti | 0.00008 |
| F | 0.0005 | V | 0.00005 |
| Fe | 0.0001 | W | 0.00003 |
| Ga | 0.00002 | Zr | 0.00001 |
Example 2
Preparation of niobium oxalate solution the preparation of the niobium oxalate solution was the same as in example 1, a niobium oxalate solution with a concentration of 0.1mol/L and an aqueous ammonia solution with a concentration of 15wt% were fed into a membrane dispersion microreactor, niobium oxalate was used as a dispersed phase, aqueous ammonia was used as a continuous phase, niobium oxalate and aqueous ammonia were reacted to produce a niobium hydroxide precipitate, the reaction temperature was controlled at 25 ℃, the reaction end point pH was 8.5, and the membrane used was a stainless steel flat plate sintered membrane with a pore diameter of 5 μm; aging the obtained precipitate at 80 ℃ for 3 hours, then dehydrating, washing, drying and calcining to obtain the high-purity niobium pentoxide superfine powder, wherein the calcining temperature is 600 ℃. The obtained T-type niobium pentoxide crystal has a powder particle diameter of about 123nm.
Example 3
Preparation of niobium oxalate solution the preparation of the niobium oxalate solution was the same as in example 1, and a solution of 0.2mol/L niobium oxalate and a solution of 25wt% aqueous ammonia were fed into a membrane dispersion microreactor, niobium oxalate was used as a dispersed phase, aqueous ammonia was used as a continuous phase, niobium oxalate and aqueous ammonia were reacted to produce a niobium hydroxide precipitate, the reaction temperature was controlled at 40 ℃, the reaction end point pH was 9.4, and the membrane used was a stainless steel flat plate sintered membrane having a pore diameter of 10. Mu.m; aging the obtained precipitate at 60 ℃ for 3 hours, then dehydrating, washing, drying and calcining to obtain the high-purity niobium pentoxide superfine powder, wherein the calcining temperature is 800 ℃. The obtained T-type niobium pentoxide crystal has a powder particle diameter of about 195nm.
Comparative example
The niobium hydroxide raw material is directly calcined at 800 ℃, a TEM image of the obtained powder is shown as a figure 3, and the crystal form at the temperature is T-shaped, but the powder agglomeration is serious.
Claims (6)
1. The preparation method of the high-purity niobium pentoxide superfine powder is characterized by comprising the following steps of:
(1) Dissolving niobium hydroxide in oxalic acid at high temperature to form niobium oxalate solution;
(2) Respectively feeding a niobium oxalate solution with a certain concentration and an ammonia solution into a membrane dispersion microreactor to enable the niobium oxalate solution to react with the ammonia solution to generate niobium hydroxide precipitate, wherein the concentration of the niobium oxalate is 0.1-0.3mol/L, the concentration of the ammonia solution is 10-35wt%, and the pH of the reaction end point is 8.5-10.0;
(3) Aging, dehydrating and washing the precipitate, and drying and calcining the precipitate to obtain the high-purity niobium pentoxide superfine powder, wherein the calcining temperature is 500-1200 ℃.
2. The method for preparing high-purity ultrafine niobium pentoxide powder as claimed in claim 1, wherein the membrane-dispersed microreactor used in the step (1) is a flat plate membrane or a tubular membrane.
3. The method for preparing high-purity niobium pentoxide superfine powder according to claim 1, wherein the pore diameter of the membrane used in the step (2) is 1 μm to 100 μm.
4. The method for preparing high-purity niobium pentoxide superfine powder according to claim 1, wherein the film material used in the step (2) is plastic, metal, glass or ceramic.
5. The method for preparing high-purity niobium pentoxide superfine powder according to claim 1, wherein the reaction temperature in the step (2) is 10 ℃ to 80 ℃.
6. The method for preparing high-purity niobium pentoxide superfine powder according to claim 1, wherein the aging temperature in the step (3) is 50-90 ℃ for 0.5-3 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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