CN112010348A - Preparation method of high-purity niobium oxide for high-purity niobium sheet for irradiation monitoring tube - Google Patents
Preparation method of high-purity niobium oxide for high-purity niobium sheet for irradiation monitoring tube Download PDFInfo
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Abstract
The application provides a preparation method of high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube, in the preparation process, a multiple acid washing and extraction combined process is adopted, impurities of tantalum, tungsten and molybdenum in the high-purity niobium oxide are removed in a targeted manner, meanwhile, the effect of removing other metal impurities in the high-purity niobium oxide is achieved, the defect that the tantalum, tungsten and molybdenum cannot be removed deeply in the traditional process is effectively overcome, the high-purity niobium oxide with high purity and chemical impurity level superior to the industrial standard is prepared, and the problem that in the traditional method for preparing the high-purity niobium oxide, the tantalum, tungsten and molybdenum in the preparation process are not treated by a special method with high specificity, so that the prepared niobium oxide impurities are high, and the produced high-purity niobium oxide cannot meet the use requirements of superconducting and electronic military materials according to special conditions is solved.
Description
Technical Field
The application relates to the technical field of metal chemical smelting, in particular to a preparation method of high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube.
Background
The high-purity niobium oxide refers to a niobium oxide product with the purity of more than 99.99 percent, is an important functional material in the high-technology new material industry, and is a main raw material of high-purity niobium materials for aerospace industry alloys, superconducting materials, atomic energy industry and military electronic equipment. The preparation method of the high-purity niobium oxide generally comprises the steps of selecting appropriate raw materials, decomposing the raw materials by hydrofluoric acid and sulfuric acid, extracting the raw materials by octanol or methyl isobutyl ketone (MIBK) to obtain a high-purity fluoroniobate solution, and then precipitating, washing, drying and roasting the solution by ammonia gas or ammonia water to prepare the high-purity niobium oxide.
In the related art, in order to prepare high-purity niobium oxide, proper raw materials need to be selected, that is, the raw materials of ores need to be selected, the requirement on impurities such as phosphorus, arsenic, antimony and the like in the ores is high, and because the processing of the ores is continuous, the proper raw materials are difficult to be completely used for producing the high-purity niobium oxide, and part of the high-purity niobium oxide is polluted in the production process. Meanwhile, in the preparation process, specific tantalum, tungsten and molybdenum are not subjected to specific treatment in the production process, so that the requirements of common high-purity niobium oxide targets such as lithium niobate ferroelectric crystals, high-refractive-index optical glass and niobium oxide sputtering targets can be met.
However, when the method is used for preparing high-purity niobium oxide required in a special field, the tantalum, tungsten and molybdenum in the preparation process are not treated by a special method with strong pertinence, so that the prepared niobium oxide has high impurity content, and the produced high-purity niobium oxide cannot meet the use requirements of superconducting and electronic military materials according to special conditions, particularly, high-purity niobium sheets for irradiation monitoring tubes in the nuclear power field, so that the application development of the high-purity niobium oxide as a raw material in the high-technology new material industry is limited.
Disclosure of Invention
The application provides a preparation method of high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube, which aims to solve the problems that in the traditional method for preparing high-purity niobium oxide, tantalum, tungsten and molybdenum in the preparation process are not treated by a special method with strong pertinence, so that the prepared niobium oxide has high impurity content, and the produced high-purity niobium oxide cannot meet the use requirements of superconducting and electronic military materials according to special conditions.
The technical scheme adopted by the application for solving the technical problems is as follows:
a preparation method of high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube comprises the following steps:
extracting a tantalum-niobium-containing solution into methyl isobutyl ketone in an extraction tank to generate a primary loaded organic solution, wherein the tantalum-niobium-containing solution is a tantalum-niobium solution produced by a hydrofluoric acid-sulfuric acid system extraction process;
respectively carrying out primary acid washing on the primary loaded organic solution by adopting an industrial-grade 2-2.5mol/L sulfuric acid solution and 5.5-6mol/L sulfuric acid to obtain a primary loaded organic phase containing tantalum and niobium, wherein the acid washing ratio of the 2-2.5mol/L sulfuric acid solution to the primary loaded organic solution is 4-8:1, the acid washing ratio of the 5.5-6mol/L sulfuric acid solution to the primary loaded organic solution is 4-8:1, the acid washing frequency of the 2-2.5mol/L sulfuric acid solution is not less than 2 times, and the acid washing frequency of the 5.5-6mol/L sulfuric acid solution is not less than 4 times;
carrying out primary niobium-resisting extraction on the primary load organic phase containing tantalum and niobium by using 0.7-0.9mol/L sulfuric acid solution as niobium-resisting solution;
carrying out tantalum-niobium separation on the primary loaded organic phase after the primary anti-niobium extraction to obtain a primary fluoroniobate solution;
adding analytically pure hydrofluoric acid and analytically pure sulfuric acid into the primary fluoroniobate solution for blending, so that the content of niobium oxide in the primary fluoroniobate solution is controlled to be 110-130g/L, the acidity of sulfuric acid is controlled to be 3-3.5mol/L, and the acidity of hydrofluoric acid is controlled to be 4.3-4.8 mol/L;
extracting the prepared primary niobium fluoride solution into methyl isobutyl ketone again in an extraction tank to obtain a high-purity secondary niobium-loaded organic solution;
respectively carrying out secondary acid washing on the secondary niobium-loaded organic solution by adopting an analytically pure sulfuric acid solution with acidity of 1.9-2.1mol/L and an analytically pure sulfuric acid solution with acidity of 4.9-5.1mol/L to obtain a secondary tantalum-containing niobium loaded organic phase, wherein the acid washing frequency of the analytically pure sulfuric acid solution with acidity of 1.9-2.1mol/L is not less than 2 times, and the acid washing frequency of the analytically pure sulfuric acid solution with acidity of 4.9-5.1mol/L is not less than 4 times;
performing secondary niobium-removing extraction on the secondary load organic phase containing tantalum and niobium by using 0.85-0.95mol/L of analytically pure sulfuric acid solution as niobium-removing solution to obtain secondary fluoroniobium acid solution;
performing tantalum-niobium separation on the secondary fluoroniobate solution again to obtain a high-purity fluoroniobate solution;
introducing purified ammonia gas into the high-purity fluoroniobate solution to neutralize and precipitate to obtain niobium hydroxide slurry;
and washing, vacuum drying and roasting the niobium hydroxide slurry in sequence to finally obtain the high-purity niobium oxide with low tantalum content, low tungsten content and low molybdenum content.
Optionally, the sequence of the primary pickling is as follows: firstly, adopting industrial-grade 2-2.5mol/L sulfuric acid solution in an extraction tank, and continuously adopting 5.5-6mol sulfuric acid solution for continuous washing after washing.
Optionally, the acid washing times of the sulfuric acid solution with the acidity of 4.9 to 5.1mol/L are 5 times, and the acid washing times of the analytically pure sulfuric acid solution with the acidity of 5.5 to 6mol/L are 5 times.
Optionally, the niobium hydroxide slurry is sequentially washed, vacuum-dried and roasted to finally obtain the high-purity niobium oxide with low tantalum content, low tungsten content and low molybdenum content, and the method comprises the following steps:
washing the niobium hydroxide slurry by adopting high-purity ammonia water with the temperature of more than 80 ℃ and quartic pure water, and drying for 18-24 hours at 80-180 ℃ by adopting a vacuum drying box after washing is finished to obtain high-purity niobium hydroxide powder;
and roasting the high-purity niobium hydroxide powder in a push-boat furnace at a controlled temperature, wherein the high-temperature area of the push-boat furnace is controlled at 950-.
The technical scheme provided by the application comprises the following beneficial technical effects:
the application provides a preparation method of high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube, in the preparation process, a multiple acid washing and extraction combined process is adopted, the impurities of tantalum, tungsten and molybdenum in the high-purity niobium oxide are removed in a targeted manner, meanwhile, the effect of removing other metal impurities in the high-purity niobium oxide is achieved, the defect that the tantalum, tungsten and molybdenum cannot be removed deeply in the traditional process is effectively overcome, the high-purity niobium oxide with high purity and chemical impurity level superior to the industrial standard is prepared, and the problem that in the traditional preparation method of the high-purity niobium oxide, the tantalum, tungsten and molybdenum in the preparation process are not treated by a special method with high specificity, so that the prepared niobium oxide impurities are high, and the produced high-purity niobium oxide cannot meet the use requirements of superconducting, electronic and military materials and the like according to special conditions is solved.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without any creative effort.
FIG. 1 is a flowchart of a method for preparing high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube according to an embodiment of the present disclosure;
fig. 2 is a flowchart of a specific preparation method of a high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube according to an embodiment of the present disclosure.
Detailed Description
In order to make the technical solutions in the present application better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application; it is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Referring to fig. 1, fig. 1 is a flow chart of a method for preparing high purity niobium oxide for a high purity niobium sheet for an irradiation monitoring tube according to an embodiment of the present application, and as shown in the figure, the method for preparing high purity niobium oxide for a high purity niobium sheet for an irradiation monitoring tube according to an embodiment of the present application includes the following steps:
s1, preparation of a primary loaded organic solution:
extracting a tantalum-niobium-containing solution into methyl isobutyl ketone (MIBK) in an extraction tank to generate a primary loaded organic solution, wherein the tantalum-niobium-containing solution is a tantalum-niobium solution produced by a hydrofluoric acid-sulfuric acid system extraction process.
S2, primary pickling:
respectively carrying out primary acid washing on the primary loaded organic solution by using an industrial-grade 2-2.5mol/L sulfuric acid solution and 5.5-6mol/L sulfuric acid to obtain a primary loaded organic phase containing tantalum and niobium, wherein the acid washing ratio of the 2-2.5mol/L sulfuric acid solution to the primary loaded organic solution is 4-8:1, the acid washing ratio of the 5.5-6mol/L sulfuric acid solution to the primary loaded organic solution is 4-8:1, the acid washing frequency of the 2-2.5mol/L sulfuric acid solution is not less than 2 times, and the acid washing frequency of the 5.5-6mol/L sulfuric acid solution is not less than 4 times.
As an embodiment, the sequence of the primary pickling is: firstly, adopting industrial-grade 2-2.5mol/L sulfuric acid solution in an extraction tank, and continuously adopting 5.5-6mol sulfuric acid solution for continuous washing after washing. The pickling sequence is limited mainly because after the primary tantalum-niobium-containing loaded organic phase is pickled by the industrial-grade 2-2.5mol/L sulfuric acid solution, the impurity elements W, Mo and the like in the mixed solution are back-extracted into the water phase, meanwhile, a part of tantalum and niobium (mainly niobium) is also back-extracted into the water phase, the distribution coefficient of the impurity elements W, Mo is much smaller than that of the tantalum and niobium, the acidity is improved by the industrial-grade 5.5-6mol/L sulfuric acid solution, the tantalum and niobium back-extracted into the water phase is extracted into the organic phase, a part of the impurity elements W, Mo does not enter the organic phase, the extraction operation is continuously performed, and the removal of the impurity elements W, Mo in the mixed solution is facilitated.
Meanwhile, the acid washing frequency of the 5.5-6mol/L sulfuric acid solution can be increased to 5 times according to the specific requirements of products.
S3, primary anti-niobium extraction:
and performing primary niobium extraction on the primary load organic phase containing the tantalum-niobium by using 0.7-0.9mol/L sulfuric acid solution as niobium-reflecting liquid.
S4, preparing a primary fluoroniobate solution:
and (4) carrying out tantalum-niobium separation on the primary loaded organic phase after the primary anti-niobium extraction to obtain a primary fluoroniobate solution.
S5, blending
Adding analytically pure hydrofluoric acid and analytically pure sulfuric acid into the primary fluoroniobate solution for blending, so that the content of niobium oxide in the primary fluoroniobate solution is controlled to be 110-130g/L, the acidity of sulfuric acid is controlled to be 3-3.5mol/L, and the acidity of hydrofluoric acid is controlled to be 4.3-4.8 mol/L.
S5, preparation of a high-purity secondary niobium-loaded organic solution:
and extracting the prepared primary niobium fluoride solution into methyl isobutyl ketone again in an extraction tank to obtain a high-purity secondary niobium supported organic solution.
S6, secondary pickling:
respectively carrying out secondary acid washing on the secondary niobium-loaded organic solution by adopting an analytically pure sulfuric acid solution with acidity of 1.9-2.1mol/L and an analytically pure sulfuric acid solution with acidity of 4.9-5.1mol/L to obtain a secondary tantalum-containing niobium loaded organic phase, wherein the acid washing frequency of the analytically pure sulfuric acid solution with acidity of 1.9-2.1mol/L is not less than 2 times, and the acid washing frequency of the analytically pure sulfuric acid solution with acidity of 4.9-5.1mol/L is not less than 4 times;
meanwhile, the acid washing times of the analytically pure sulfuric acid solution with the acidity of 4.9-5.1mol/L can be increased to 5 times according to the specific requirements of the product.
S7, secondary niobium reverse extraction:
and (3) performing secondary niobium-resisting extraction on the secondary tantalum-niobium-containing load organic phase by using 0.85-0.95mol/L of analytically pure sulfuric acid solution as niobium-resisting solution to obtain a secondary fluoroniobium acid solution.
S8, separating tantalum and niobium:
and carrying out tantalum-niobium separation on the secondary fluoroniobate solution again to obtain the high-purity fluoroniobate solution.
S9, neutralizing and precipitating:
and introducing purified ammonia gas into the high-purity fluoroniobate solution to neutralize and precipitate, thereby obtaining the niobium hydroxide slurry.
S10, post-processing:
and washing, vacuum drying and roasting the niobium hydroxide slurry in sequence to finally obtain the high-purity niobium oxide for the high-purity niobium sheet for the low-tantalum, tungsten and molybdenum irradiation monitoring tube.
As an embodiment, the niobium hydroxide slurry is sequentially washed, vacuum-dried, and calcined to finally obtain the high-purity niobium oxide with low tantalum, tungsten, and molybdenum contents, and the method comprises the following steps:
washing the niobium hydroxide slurry by adopting high-purity ammonia water with the temperature of more than 80 ℃ and quartic pure water, and drying for 18-24 hours at 80-180 ℃ by adopting a vacuum drying box after washing is finished to obtain high-purity niobium hydroxide powder;
and roasting the high-purity niobium hydroxide powder in a push-boat furnace at a controlled temperature, wherein the high-temperature area of the push-boat furnace is controlled at 950-.
One specific embodiment is given below as a more detailed technical description:
example 1
Referring to fig. 2, fig. 2 shows a specific method flow of the present embodiment.
Extracting the tantalum-niobium-containing solution into methyl isobutyl ketone (MIBK) in an extraction tank to generate a primary loaded organic solution simultaneously containing tantalum and niobium, wherein the content of tantalum and niobium in the loaded organic solution is calculated by tantalum oxide and niobium oxide, and the ratio is tantalum oxide: niobium oxide is 1-3: 3-1, the proportion of tantalum and niobium in the loaded organic solution is different during actual production, the content of tantalum oxide can be floated at 80-220g/l, and the content of niobium oxide can be floated at 80-220 g/l. Wherein the MIBK purity is greater than 99.9%.
The dilute sulfuric acid solution for primary acid washing and primary niobium extraction is prepared by using industrial-grade sulfuric acid (the relative molecular mass is 98%). The sulfuric acid solution for primary acid washing is 2-2.5mol sulfuric acid solution and 5.5-6mol/L sulfuric acid solution, and the sulfuric acid solution for primary niobium reaction is 0.7-0.9mol/L sulfuric acid solution.
The dilute sulfuric acid solution (with the concentration of 95.0-98.0%) obtained by secondary acid washing and secondary niobium-removing extraction is prepared by adopting analytically pure sulfuric acid (with the relative molecular mass of 98%). The concentration of the secondary acid sulfuric acid is 1.9-2.1mol/L and 4.9-5.1mol/L respectively, and the acidity of the secondary anti-niobium sulfuric acid solution is 0.85-0.95 mol/L.
The neutralizing precipitation precipitator is any one of ammonia gas, ammonia water or liquid ammonia.
The washing is carried out by adopting ammonia water and pure water, the purpose of washing is to remove ammonium ions and fluoride ions in the tantalum-niobium hydroxide mixed slurry, other impurity ions are not introduced, the washing mode can adopt a pressure washing mode, and the pressure washing time is 300kg per batch and is not less than 6 hours.
Drying temperature: drying the washed slurry at 80-180 ℃, wherein the drying time is as follows: 18-24 hours.
Roasting temperature: the roasting temperature of the high-purity niobium hydroxide powder is controlled at 950 ℃ and 1100 ℃.
According to the extraction principle, the distribution coefficients of tantalum, tungsten, molybdenum and niobium are different in the extraction process, acid washing and the extraction process respectively enter an organic phase and a water phase, and after acid washing and reverse niobium extraction are carried out for multiple times by utilizing extraction equipment, high-purity niobium oxide with high purity and low tantalum, tungsten and molybdenum is obtained.
The high-purity niobium oxide prepared by the preparation method of the high-purity niobium oxide for the high-purity niobium sheet for the irradiation monitoring tube provided by the embodiment of the application has the impurity level superior to that of product number FNb in industry standard 'high-purity niobium pentoxide' YS/T548-20072O5Provision of-040.
As shown in the following table, the results were obtained by the methods (experimental data 1 and experimental data 2) and the FNb2O5Prepared by the method in-040 StandardHigh-purity niobium oxide impurity content reference table:
TABLE 1 content of impurity component
As can be seen from the above table, the high purity niobium oxide prepared by the method provided in the present application has a purity superior to that using FNb2O5The high-purity niobium oxide prepared by the method in the-040 standard is more outstanding in the effect of removing impurities W and Mo, and therefore, the impurities in the high-purity niobium oxide can be removed in a targeted manner by the method provided in the embodiment of the application, so that the prepared product is superior to the industrial standard.
In summary, the embodiments of the present application provide a method for preparing high purity niobium oxide for high purity niobium sheet for irradiation monitoring tube, in the preparation process, a process of combining acid washing and extraction for many times is adopted, impurities of tantalum, tungsten and molybdenum of the high-purity niobium oxide are pertinently removed, meanwhile, the method also has the effect of removing other metal impurities in the high-purity niobium oxide, effectively avoids the defect that the traditional process can not deeply remove tantalum, tungsten and molybdenum, prepares the high-purity niobium oxide with high purity and chemical impurity level superior to the industrial standard, solves the problem that in the traditional method for preparing the high-purity niobium oxide, the tantalum, tungsten and molybdenum in the preparation process are not treated by a special method with strong pertinence, so that the prepared niobium oxide has high impurity content, and the produced high-purity niobium oxide cannot meet the use requirements of superconducting and electronic military materials and the like according to special conditions.
It is to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that an article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
It will be understood that the present application is not limited to what has been described above and shown in the accompanying drawings, and that various modifications and changes can be made without departing from the scope thereof. The scope of the application is limited only by the appended claims.
Claims (4)
1. A preparation method of high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube is characterized by comprising the following steps:
extracting a tantalum-niobium-containing solution into methyl isobutyl ketone in an extraction tank to generate a primary loaded organic solution, wherein the tantalum-niobium-containing solution is a tantalum-niobium solution produced by a hydrofluoric acid-sulfuric acid system extraction process;
respectively carrying out primary acid washing on the primary loaded organic solution by adopting an industrial-grade 2-2.5mol/L sulfuric acid solution and 5.5-6mol/L sulfuric acid to obtain a primary loaded organic phase containing tantalum and niobium, wherein the acid washing ratio of the 2-2.5mol/L sulfuric acid solution to the primary loaded organic solution is 4-8:1, the acid washing ratio of the 5.5-6mol/L sulfuric acid solution to the primary loaded organic solution is 4-8:1, the acid washing frequency of the 2-2.5mol/L sulfuric acid solution is not less than 2 times, and the acid washing frequency of the 5.5-6mol/L sulfuric acid solution is not less than 4 times;
carrying out primary niobium-resisting extraction on the primary load organic phase containing tantalum and niobium by using 0.7-0.9mol/L sulfuric acid solution as niobium-resisting solution;
carrying out tantalum-niobium separation on the primary loaded organic phase after the primary anti-niobium extraction to obtain a primary fluoroniobate solution;
adding analytically pure hydrofluoric acid and analytically pure sulfuric acid into the primary fluoroniobate solution for blending, so that the content of niobium oxide in the primary fluoroniobate solution is controlled to be 110-130g/L, the acidity of sulfuric acid is controlled to be 3-3.5mol/L, and the acidity of hydrofluoric acid is controlled to be 4.3-4.8 mol/L;
extracting the prepared primary niobium fluoride solution into methyl isobutyl ketone again in an extraction tank to obtain a high-purity secondary niobium-loaded organic solution;
respectively carrying out secondary acid washing on the secondary niobium-loaded organic solution by adopting an analytically pure sulfuric acid solution with acidity of 1.9-2.1mol/L and an analytically pure sulfuric acid solution with acidity of 4.9-5.1mol/L to obtain a secondary tantalum-containing niobium loaded organic phase, wherein the acid washing frequency of the analytically pure sulfuric acid solution with acidity of 1.9-2.1mol/L is not less than 2 times, and the acid washing frequency of the analytically pure sulfuric acid solution with acidity of 4.9-5.1mol/L is not less than 4 times;
performing secondary niobium-removing extraction on the secondary load organic phase containing tantalum and niobium by using 0.85-0.95mol/L of analytically pure sulfuric acid solution as niobium-removing solution to obtain secondary fluoroniobium acid solution;
performing tantalum-niobium separation on the secondary fluoroniobate solution again to obtain a high-purity fluoroniobate solution;
introducing purified ammonia gas into the high-purity fluoroniobate solution to neutralize and precipitate to obtain niobium hydroxide slurry;
and washing, vacuum drying and roasting the niobium hydroxide slurry in sequence to finally obtain the high-purity niobium oxide with low tantalum content, low tungsten content and low molybdenum content.
2. The method for preparing high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube according to claim 1, wherein the sequence of the primary acid washing is as follows: firstly, adopting industrial-grade 2-2.5mol/L sulfuric acid solution in an extraction tank, and continuously adopting 5.5-6mol sulfuric acid solution for continuous washing after washing.
3. The method for preparing high-purity niobium oxide for a high-purity niobium sheet for an irradiation monitoring tube according to claim 1, wherein the acid washing frequency of the sulfuric acid solution of 5.5 to 6mol/L is 5, and the acid washing frequency of the analytically pure sulfuric acid solution having an acidity of 4.9 to 5.1mol/L is 5.
4. The method for preparing high-purity niobium oxide for the high-purity niobium sheet for the irradiation monitoring tube according to claim 1, wherein the step of sequentially washing, vacuum drying and roasting the niobium hydroxide slurry to finally obtain the high-purity niobium oxide with low tantalum, tungsten and molybdenum content comprises the following steps:
washing the niobium hydroxide slurry by adopting high-purity ammonia water with the temperature of more than 80 ℃ and quartic pure water, and drying for 18-24 hours at 80-180 ℃ by adopting a vacuum drying box after washing is finished to obtain high-purity niobium hydroxide powder;
and roasting the high-purity niobium hydroxide powder in a push-boat furnace at a controlled temperature, wherein the high-temperature area of the push-boat furnace is controlled at 950-.
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