CN113186399A - Method for extracting tantalum and niobium - Google Patents

Method for extracting tantalum and niobium Download PDF

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CN113186399A
CN113186399A CN202110272586.7A CN202110272586A CN113186399A CN 113186399 A CN113186399 A CN 113186399A CN 202110272586 A CN202110272586 A CN 202110272586A CN 113186399 A CN113186399 A CN 113186399A
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tantalum
niobium
acid
extracting
roasting
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CN113186399B (en
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杨建参
崔奇
席晓丽
马立文
蔡圆圆
聂祚仁
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Beijing University of Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G33/00Compounds of niobium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G35/00Compounds of tantalum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/20Obtaining niobium, tantalum or vanadium
    • C22B34/24Obtaining niobium or tantalum
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
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Abstract

The invention relates to the technical field of hydrometallurgy, in particular to a method for extracting tantalum and niobium; the method comprises the following steps: (1) oxidizing and roasting the material containing tantalum and niobium to prepare oxides of tantalum and niobium; (2) mixing the tantalum oxide and the niobium oxide with alkali, and then roasting to obtain alkali fusion conversion products of the tantalum oxide and the niobium oxide; (3) leaching the alkali fusion conversion products of the tantalum and the niobium by adopting mixed organic acid to obtain leachate containing the tantalum and the niobium; (4) extracting the leachate containing tantalum and niobium by using triisooctylamine, and back-extracting niobium by using pure water or dilute sulfuric acid to obtain a niobium-containing solution and a tantalum-containing organic phase; (5) and back-extracting the tantalum in the tantalum-containing organic phase by using concentrated nitric acid to obtain a tantalum-containing solution. The method not only reduces the extremely high requirements of the reaction on equipment, but also reduces the serious harm to the environment, and provides a new research idea for the field of tantalum-niobium metallurgical separation.

Description

Method for extracting tantalum and niobium
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a method for extracting tantalum and niobium.
Background
Tantalum and niobium belong to rare metals, are important strategic reserve resources, and have wide application in the fields of medicine, military, aerospace and the like. Tantalum and niobium have excellent chemical stability, and do not react with inorganic acid (dehydrofluoric acid) at normal temperature and normal pressure, so that the tantalum and niobium leaching difficulty is high.
At present, there are known methods for effectively leaching tantalum and niobium, such as a hydrofluoric acid method, a sulfuric acid method (high temperature), an alkali fusion method, and an alkaline solution method; among them, the hydrofluoric acid method is most widely used.
Currently, in the field of tantalum-niobium metallurgy, the mainstream method for leaching tantalum and niobium is hydrofluoric acid, which is to directly leach tantalum-niobium ore or dissolve metatantalate (niobate) after alkali conversion by using hydrofluoric acid, and is recorded in detail in chinese patent documents CN102952951A and CN 103898331A. Specifically, in chinese patent document CN102952951A, when treating a tantalum-niobium ore with hydrofluoric acid, the method first crushes the tantalum-niobium ore to below 50 mesh, then removes impurity elements such as iron and manganese in the tantalum-niobium ore by leaching with concentrated hydrochloric acid, and then leachates with hydrofluoric acid to obtain a tantalum-niobium leachate; when the alkali conversion product is treated by hydrofluoric acid, firstly, the tantalum-niobium raw material is oxidized, then, the oxide and the alkali are mixed and roasted to obtain the alkali conversion product, and then, the alkali conversion product is leached by the hydrofluoric acid to obtain the tantalum-niobium leaching solution. In chinese patent document CN103898331A, nonmagnetic tantalum-niobium slag, sodium hydroxide and sodium carbonate are mixed and then melted at 500 to 800 ℃, then the melted block is crushed, heated and stirred with hydrochloric acid to leach out impurities such as calcium, aluminum, iron, etc., and the acid leaching slag is subjected to acid leaching with a mixture of hydrofluoric acid and nitric acid to leach out tantalum-niobium. However, in the above tantalum-niobium leaching process, a large amount of hydrofluoric acid is consumed, the hydrofluoric acid is an acid with extremely high corrosiveness, the requirement on equipment is extremely high, the method generates a large amount of three wastes containing fluorine, and the wastes and the hydrofluoric acid have high toxicity and are very harmful to the environment and the body of an operator.
In order to avoid the use of hydrofluoric acid during the leaching process, chinese patent document CN104745807A discloses a sulfuric acid leaching method. The method comprises the steps of firstly crushing tantalum niobium ore to be less than 200 meshes, then mixing concentrated sulfuric acid and potassium bisulfate with the tantalum niobium ore according to a certain proportion, roasting to obtain roasting slag, and then leaching the roasting slag with sulfuric acid to obtain a tantalum niobium leaching solution. The method avoids the use of hydrofluoric acid in the whole process, obtains breakthrough progress in environmental protection, has large sulfuric acid consumption, is only suitable for treating titanium-tantalum-niobium composite concentrate, and has a small application range.
With the rapid development of the aerospace and military fields, the demand of tantalum-niobium resources is increasing day by day, and the extraction of tantalum-niobium resources from materials containing tantalum and niobium (including tantalum-niobium-containing alloys, spray coatings, additive manufacturing materials and the like) is of great importance. The material containing tantalum and niobium has high tantalum and niobium content, the mass percentage of the material is different from 4 to 99 percent, and the material is far higher than the tantalum and niobium content in the ore. At present, the research blank of tantalum-niobium metallurgy is about extracting high-content tantalum-niobium materials through a fluorine-free process.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention makes up the defects of the prior art, provides the fluorine-free tantalum-niobium extraction method with wider tantalum-niobium content range, reduces the extremely high requirements of the reaction on equipment, reduces the serious harm to the environment and provides a new research idea for the field of tantalum-niobium metallurgical separation.
Specifically, the invention adopts the following technical scheme:
the invention provides a method for extracting tantalum and niobium, which comprises the following steps:
(1) oxidizing and roasting the material containing tantalum and niobium to prepare oxides of tantalum and niobium;
(2) mixing the tantalum oxide and the niobium oxide with alkali, and then roasting to obtain alkali fusion conversion products of the tantalum oxide and the niobium oxide;
(3) leaching the alkali fusion conversion products of the tantalum and the niobium by adopting mixed organic acid to obtain leachate containing the tantalum and the niobium;
(4) extracting the leachate containing tantalum and niobium by using triisooctylamine, and back-extracting niobium by using pure water or dilute sulfuric acid to obtain a niobium-containing solution and a tantalum-containing organic phase;
(5) and back-extracting the tantalum in the tantalum-containing organic phase by using concentrated nitric acid to obtain a tantalum-containing solution.
The invention unexpectedly discovers that materials containing tantalum and niobium are crushed, the main components of the materials are simple substances and hydrides of tantalum and niobium, oxides of tantalum and niobium are prepared by oxidizing roasting, then the oxides are uniformly mixed with alkali and roasted again to realize alkali fusion conversion of tantalum and niobium, and then the alkali fusion conversion products are leached by adopting mixed organic acid to obtain leachate containing tantalum and niobium; extracting tantalum and niobium from the leachate by using triisooctylamine, and performing back extraction on the niobium by using pure water or dilute sulfuric acid to realize the separation of the tantalum and the niobium and obtain a solution containing the niobium; and (3) back-extracting the tantalum by using concentrated nitric acid to obtain a tantalum-containing solution.
In order to further improve the extraction rate of tantalum and niobium, the extraction method is optimized as follows:
preferably, in the step (1), the oxidizing roasting is carried out at 600-800 ℃ for 1.5-2.5 h.
Preferably, in step (2), the base is potassium hydroxide; preferably, the roasting is carried out for 1-4 hours at the temperature of 360-500 ℃.
In the technical scheme, the alkali used in the alkali fusion conversion process is potassium hydroxide, and in the process of mixing and roasting with oxides, oxides of tantalum and niobium react with potassium hydroxide to generate various potassium tantalite and potassium niobate.
In addition, the alkali-fusion process of tantalum and niobium, which first converts to soluble potassium tantalate (niobate) and then to insoluble potassium metatantalate (niobate), is controlled by the reaction temperature and reaction time, and occurs more rapidly at higher reaction temperatures. In order to control the reaction progress and reduce the generation of insoluble substances, the highest reaction temperature should not exceed 500 ℃. The melting point of the potassium hydroxide is 360 ℃, and the reaction temperature is not lower than 360 ℃ in order to ensure the fluidity of the potassium hydroxide in the reaction process. In the reaction temperature range, all conversion products contain insoluble potassium metatantalate (niobate) when the conversion time reaches 4 hours, so the conversion time is controlled within 4 hours.
Preferably, in the step (3), the mixed organic acid is oxalic acid and tartaric acid; preferably, the molar ratio of the oxalic acid to the tartaric acid is 1-5: 1.
in the technical scheme, the mixed organic acid is oxalic acid and tartaric acid, in the process of leaching by adopting the mixed acid of oxalic acid and tartaric acid, oxalic acid reacts with alkali fusion conversion products of tantalum and niobium to generate a soluble tantalum-niobium oxalic acid complex, and tartaric acid can enhance the stability of tantalum and niobium in a solution and reduce hydroxide precipitates of tantalum and niobium generated by side reactions, so that the leaching rate is improved.
In addition, since oxalic acid is more acidic than tartaric acid and serves as the main leaching acid, the amount of oxalic acid used should not be less than tartaric acid; meanwhile, tartaric acid is used as auxiliary acid for leaching, provides functional groups, and mainly aims to improve the stability of the complex of tantalum and niobium in a solution without adding excessive acid; that is, when the molar ratio of the oxalic acid to the tartaric acid is 1-5: 1, the effect is best.
Preferably, the leaching is carried out at 50-70 ℃ for 1-4 h.
In the technical scheme, because the oxalic acid complex of tantalum and niobium is unstable at high temperature, when the temperature is higher than 70 ℃, the oxalic acid complex is accelerated to be decomposed into hydroxide, and therefore, the leaching temperature is not higher than 70 ℃; further, from the viewpoint of dynamics, the reaction temperature should be increased as much as possible to accelerate the reaction rate, and therefore, the leaching temperature is preferably 50 to 70 ℃.
In addition, because tantalum and niobium have strong chemical stability and relatively slow reaction rate, the leaching time should be properly prolonged; specifically, most of tantalum and niobium leaching can be completed within 1-2 h before the reaction, and then as the leaching time is increased, the leaching rate of tantalum and niobium is still improved, but the increase amplitude is gradually reduced.
Preferably, in the step (4), the oil-water ratio of the extraction is 1-5: 1; preferably, the extraction time is 5-10 min; after the extraction is complete, the tantalum and niobium are mostly transferred to the organic phase.
Preferably, the pH of the pure water or the dilute sulfuric acid is 1-7; after the back extraction is finished, the niobium enters a water phase, and most of tantalum is left in an organic phase, so that the separation of tantalum and niobium is realized.
Preferably, in the step (5), the concentrated nitric acid is 10M concentrated nitric acid; in the process of stripping tantalum, the stripping agent is 10M concentrated nitric acid, and the stripping of most of tantalum can be realized after multi-stage extraction.
Preferably, the method further comprises the step of post-processing; the post-treatment comprises the following steps: and respectively adding ammonia water into the niobium-containing solution and the tantalum-containing solution, and roasting the obtained precipitates for 1.5-2.5 hours at 600-800 ℃ after washing.
In the technical scheme, ammonia water is added into a niobium water phase to obtain a niobium hydroxide precipitate, and the precipitate is filtered, washed and then placed in a 600-800 ℃ muffle furnace to be roasted for 1.5-2.5 hours to obtain niobium pentoxide; and adding ammonia water into the tantalum water phase to obtain a tantalum hydroxide precipitate, filtering and washing the precipitate, and roasting the precipitate in a muffle furnace at the temperature of 600-800 ℃ for 1.5-2.5 h to obtain tantalum pentoxide.
As a preferred technical solution, the method comprises the following steps:
(1) oxidizing and roasting the material containing tantalum and niobium at 600-800 ℃ for 1.5-2.5 h to prepare oxides of tantalum and niobium;
(2) mixing the tantalum and niobium oxides with potassium hydroxide, and roasting at 360-500 ℃ for 1-4 h to obtain alkali fusion conversion products of tantalum and niobium;
(3) the method comprises the following steps of (1-5): 1, leaching the alkali fusion conversion products of the tantalum and the niobium for 1-4 hours at 50-70 ℃ to obtain a leaching solution containing the tantalum and the niobium;
(4) extracting the leachate containing tantalum and niobium by using triisooctylamine for 5-10 min, then back-extracting niobium by using pure water or dilute sulfuric acid, and obtaining a niobium-containing solution and a tantalum-containing organic phase through multi-stage extraction; the oil-water ratio of extraction is 1-5: 1;
(5) back-extracting the tantalum in the tantalum-containing organic phase by using 10M concentrated nitric acid to obtain a tantalum-containing solution;
(6) and respectively adding ammonia water into the niobium-containing solution and the tantalum-containing solution, washing the obtained precipitate, and roasting at 600-800 ℃ for 1.5-2.5 h to obtain tantalum pentoxide and niobium pentoxide.
Preferably, the material containing tantalum and niobium is a tantalum-niobium alloy, a spray coating, an additive manufacturing material and the like.
The invention has the beneficial effects that:
(1) the range of the tantalum-niobium materials which can be processed by the method is wider, and the tantalum-niobium materials comprise tantalum materials, niobium materials and tantalum-niobium mixture materials, wherein the content of tantalum or niobium is up to 99 wt%;
(2) the invention is a fluorine-free process, the alkali fusion conversion products of tantalum and niobium are leached by adopting the mixed acid of oxalic acid and tartaric acid, the oxalic acid is used as the main leaching acid, the tartaric acid is used as the leaching auxiliary acid, the mixed acid has the leaching capacity of the oxalic acid and the stabilizing capacity of the tartaric acid, the leaching rate and the solution stability are higher, and the fluorine-free process has great significance for environmental protection and green production;
(3) the method provided by the invention has good extraction effect of tantalum and niobium, the leaching rates of tantalum and niobium can respectively reach 98.6% and 99.8%, the extraction rates of tantalum and niobium can respectively reach 97.2% and 93.1%, the back extraction rates of tantalum and niobium can respectively reach 94.4% and 99.3%, and the method has technical advance for extraction of tantalum and niobium, especially for extraction of materials with high content of tantalum and niobium.
Drawings
FIG. 1 is a flow chart of a process for extracting tantalum and niobium in an embodiment of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Example 1
The embodiment provides a method for extracting tantalum and niobium from a tantalum-niobium-containing material, as shown in fig. 1, comprising the following steps:
the tantalum-niobium content (wt%) of a certain tantalum-niobium containing material powder was 80.59% and 4.08%, respectively, and was designated as powder I. And (3) putting 1g of the powder I into dilute hydrochloric acid and dilute sulfuric acid to remove impurities to obtain tantalum-niobium enriched slag, and roasting the enriched slag in a muffle furnace at 700 ℃ for 2 hours to obtain oxide powder. Uniformly mixing the oxide powder with 4g of KOH, then placing the mixture into a muffle furnace to be roasted for 2 hours at 500 ℃, and leaching roasted slag for 2 hours at 60 ℃ by using 30g of mixed acid of 15% of oxalic acid and 5% of tartaric acid to obtain leachate containing tantalum and niobium; the leaching rate of tantalum is 98.6 percent, and the leaching rate of niobium is 99.8 percent. And mixing an extracting agent triisooctylamine with a leaching solution according to an extraction ratio of O to A of 3 to 1, shaking for extraction for 8min, separating liquid after centrifugation, wherein the extraction rate of tantalum is 97.2 percent, and the extraction rate of niobium is 93.1 percent. The extracted organic phase is mixed with pure water with the same volume, and the niobium back extraction rate is 96.9 percent after four-stage back extraction. The tantalum organic phase is subjected to three-stage extraction by using concentrated nitric acid of 10M, and the tantalum back extraction rate is 93.1%. Respectively adding ammonia water into tantalum and niobium water phases to obtain precipitates, respectively filtering and washing the precipitates, and then placing the precipitates in a muffle furnace at 800 ℃ for roasting for 2 hours to obtain tantalum pentoxide and niobium pentoxide products.
Example 2
The embodiment provides a method for extracting tantalum and niobium from a tantalum-niobium-containing material, which comprises the following steps:
the tantalum-niobium content (wt%) of a certain tantalum-niobium-containing material powder was 9.15% and 1.23%, respectively, and was designated as powder II. 1.163g of powder II was calcined in a muffle furnace at 700 ℃ for 2h to give 1g of oxide powder. The oxide powder is uniformly mixed with 2g of KOH and then is placed in a muffle furnace to be roasted for 2 hours at the temperature of 400 ℃, the roasted slag is leached out for 2 hours at the temperature of 70 ℃ by using 30g of mixed acid of 15 percent oxalic acid and 5 percent tartaric acid, and leachate containing tantalum and niobium is obtained, wherein the leaching rate of the tantalum is 98.7 percent, and the leaching rate of the niobium is 76.3 percent. And mixing an extracting agent triisooctylamine with the leaching solution according to the extraction ratio of O to A of 1 to 1, shaking for extraction for 5min, separating liquid after centrifugation, wherein the extraction rate of tantalum is 96.2 percent, and the extraction rate of niobium is 91.7 percent. The extracted organic phase is mixed with pure water with the same volume, and the niobium back extraction rate is 97.2 percent after four-stage back extraction. The tantalum organic phase is subjected to three-stage extraction by using 10M concentrated nitric acid, and the tantalum back extraction rate is 94.4%. Respectively adding ammonia water into tantalum and niobium water phases to obtain precipitates, respectively filtering and washing the precipitates, and then placing the precipitates in a muffle furnace at 800 ℃ for roasting for 2 hours to obtain tantalum pentoxide and niobium pentoxide products.
Example 3
The embodiment provides a method for extracting tantalum and niobium from a tantalum-niobium-containing material, which comprises the following steps:
the tantalum-niobium content (wt%) of a certain tantalum-niobium containing material powder was 1.5% and 93.7%, respectively, and was designated as powder III. And (3) putting 1g of the powder III into a muffle furnace at 700 ℃ for roasting for 2h to obtain oxide powder. The oxide powder is uniformly mixed with 4g of KOH and then is placed in a muffle furnace to be roasted for 2 hours at the temperature of 400 ℃, the roasted slag is leached out for 2 hours at the temperature of 70 ℃ by using 30g of mixed acid of 15 percent oxalic acid and 5 percent tartaric acid, and leachate containing tantalum and niobium is obtained, wherein the leaching rate of tantalum is 97.9 percent, and the leaching rate of niobium is 96.8 percent. And mixing an extracting agent triisooctylamine with a leaching solution according to an extraction ratio of O to A of 5 to 1, shaking for extraction for 10min, separating liquid after centrifugation, wherein the extraction rate of tantalum is 98.1 percent, and the extraction rate of niobium is 91.7 percent. The extracted organic phase is mixed with the same volume of dilute sulfuric acid, and the mixture is subjected to shaking back extraction for 10min, wherein the niobium back extraction rate is 98.8 percent. The tantalum organic phase is subjected to three-stage extraction by using 10M concentrated nitric acid, and the tantalum back extraction rate is 96.1%. Respectively adding ammonia water into tantalum and niobium water phases to obtain precipitates, respectively filtering and washing the precipitates, and then placing the precipitates in a muffle furnace at 800 ℃ for roasting for 2 hours to obtain tantalum pentoxide and niobium pentoxide products.
Comparative example 1
This comparative example provides a process for extracting tantalum and niobium from a tantalum-niobium containing material, differing from example 1 only in that: triisooctylamine was replaced with sec-octanol.
The extraction rate of tantalum is 1.98 percent, and the extraction rate of niobium is 1.02 percent.
Comparative example 2
This comparative example provides a process for extracting tantalum and niobium from a tantalum-niobium containing material, differing from example 1 only in that: triisooctylamine was replaced with n-heptane.
The extraction rate of tantalum is 0.99 percent, and the extraction rate of niobium is 0.4 percent.
Comparative example 3
This comparative example provides a process for extracting tantalum and niobium from a tantalum-niobium containing material, differing from example 1 only in that: triisooctylamine was replaced with toluene.
The extraction rate of tantalum is 1.37%, and the extraction rate of niobium is 1.52%.
Comparative example 4
This comparative example provides a process for extracting tantalum and niobium from a tantalum-niobium containing material, differing from example 1 only in that: the triisooctylamine is replaced by P204, P507, N235 and N263.
After extraction, the phenomenon of severe emulsification occurs, and the oil phase and the water phase are difficult to separate.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. A method for extracting tantalum and niobium, comprising the steps of:
(1) oxidizing and roasting the material containing tantalum and niobium to prepare oxides of tantalum and niobium;
(2) mixing the tantalum oxide and the niobium oxide with alkali, and then roasting to obtain alkali fusion conversion products of the tantalum oxide and the niobium oxide;
(3) leaching the alkali fusion conversion products of the tantalum and the niobium by adopting mixed organic acid to obtain leachate containing the tantalum and the niobium;
(4) extracting the leachate containing tantalum and niobium by using triisooctylamine, and back-extracting niobium by using pure water or dilute sulfuric acid to obtain a niobium-containing solution and a tantalum-containing organic phase;
(5) and back-extracting the tantalum in the tantalum-containing organic phase by using concentrated nitric acid to obtain a tantalum-containing solution.
2. The method of claim 1, wherein in the step (1), the oxidizing roasting is performed at 600 to 800 ℃ for 1.5 to 2.5 hours.
3. The method according to claim 1 or 2, wherein in step (2), the base is potassium hydroxide; preferably, the roasting is carried out for 1-4 hours at the temperature of 360-500 ℃.
4. The method according to any one of claims 1 to 3, wherein in the step (3), the mixed organic acid is oxalic acid and tartaric acid; preferably, the molar ratio of the oxalic acid to the tartaric acid is 1-5: 1.
5. a method according to claim 4, wherein the leaching is carried out at 50-70 ℃ for 1-4 hours.
6. The method according to any one of claims 1 to 5, wherein in the step (4), the oil-water ratio of the extraction is 1 to 5: 1; preferably, the extraction time is 5-10 min.
7. The method according to claim 6, wherein the pH of the pure water or the dilute sulfuric acid is 1 to 7.
8. The method according to any one of claims 1 to 7, wherein in the step (5), the concentrated nitric acid is 10M concentrated nitric acid.
9. The method according to any one of claims 1 to 8, further comprising a step of post-treatment; the post-treatment comprises the following steps: and respectively adding ammonia water into the niobium-containing solution and the tantalum-containing solution, and roasting the obtained precipitates for 1.5-2.5 hours at 600-800 ℃ after washing.
10. The method of claim 1, comprising the steps of:
(1) oxidizing and roasting the material containing tantalum and niobium at 600-800 ℃ for 1.5-2.5 h to prepare oxides of tantalum and niobium;
(2) mixing the tantalum and niobium oxides with potassium hydroxide, and roasting at 360-500 ℃ for 1-4 h to obtain alkali fusion conversion products of tantalum and niobium;
(3) the method comprises the following steps of (1-5): 1, leaching the alkali fusion conversion products of the tantalum and the niobium for 1-4 hours at 50-70 ℃ to obtain a leaching solution containing the tantalum and the niobium;
(4) extracting the leachate containing tantalum and niobium by using triisooctylamine for 5-10 min, then back-extracting niobium by using pure water or dilute sulfuric acid, and obtaining a niobium-containing solution and a tantalum-containing organic phase through multi-stage extraction; the oil-water ratio of extraction is 1-5: 1;
(5) back-extracting the tantalum in the tantalum-containing organic phase by using 10M concentrated nitric acid to obtain a tantalum-containing solution;
(6) and respectively adding ammonia water into the niobium-containing solution and the tantalum-containing solution, washing the obtained precipitate, and roasting at 600-800 ℃ for 1.5-2.5 h to obtain tantalum pentoxide and niobium pentoxide.
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