CN113151695A - Method for decomposing low-grade tantalum-niobium resource and extracting tantalum-niobium by acid method - Google Patents

Method for decomposing low-grade tantalum-niobium resource and extracting tantalum-niobium by acid method Download PDF

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CN113151695A
CN113151695A CN202110466596.4A CN202110466596A CN113151695A CN 113151695 A CN113151695 A CN 113151695A CN 202110466596 A CN202110466596 A CN 202110466596A CN 113151695 A CN113151695 A CN 113151695A
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niobium
tantalum
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CN113151695B (en
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韩桂洪
刘兵兵
黄艳芳
曹亦俊
王益壮
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Zhengzhou University
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/24—Obtaining niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
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    • C22B1/06—Sulfating roasting
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    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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Abstract

The invention discloses a method for decomposing low-grade tantalum-niobium resources and extracting tantalum-niobium by an acid method, which is characterized in that ground low-grade tantalum-niobium resources, persulfate and bisulfate are uniformly mixed and then are roasted to obtain a roasted product; leaching the roasted product at a high temperature by adopting low acid to obtain leachate containing the tantalum-niobium peroxy complex; carrying out decomposition reaction on the leachate containing the tantalum-niobium peroxy complex to obtain hydrous tantalum-niobium oxide precipitate; the method has the advantages that the recovery rate of tantalum and niobium is as high as 94-98%, super-strong hydrofluoric acid is avoided, the concentration and the dosage of sulfuric acid are reduced, the method is environment-friendly, the process flow is simple, the requirement on equipment is low, and the method is favorable for large-scale popularization and application.

Description

Method for decomposing low-grade tantalum-niobium resource and extracting tantalum-niobium by acid method
Technical Field
The invention relates to a method for processing low-grade tantalum-niobium resources, in particular to a method for decomposing the low-grade tantalum-niobium resources and extracting tantalum-niobium by an acid method, and belongs to the field of rare and precious metal metallurgy.
Background
Tantalum (Ta) and niobium (Nb) belong to rare precious metals, have the advantages of high melting point, corrosion resistance, good cold processing performance, large dielectric constant of an oxide film on the surface of metal and the like, and are widely applied to the fields of electronics, steel, aerospace, chemical industry, nuclear industry and the like. Currently, 60-70% of the world's tantalum production is used to fabricate tantalum capacitors, which have high specific capacity, long life, thin and stable dielectric films, and the like. More than 90% of the niobium yield is used in the steel industry, and the performance of the steel can be greatly improved by adding a very small amount of niobium into the common steel.
The tantalum and niobium belong to indissolvable metals, and are leached by strong acid and strong alkali under the condition of low temperature (below 100 ℃), and the leaching rate is lower than 30 percent. Methods for extracting niobium from niobium-tantalum ores are generally classified into pyrogenic and wet processes. The pyrogenic process includes an acidic reagent melting process, an alkaline reagent melting process, a chlorination process, and the like. The wet process includes a hydrofluoric acid process, a sulfuric acid process, a hydrofluoric acid-sulfuric acid process, and the like. The hydrofluoric acid is favorable for separating and purifying tantalum-niobium ores by an extraction method, and an alkali fusion method is gradually eliminated. When the tantalum-niobium concentrate is decomposed by hydrofluoric acid, tantalum, niobium and part of impurities enter a solution to be separated by a subsequent extraction process, elements such as alkaline earth, rare earth, uranium and the like generate insoluble fluoride precipitates, the decomposition rate can reach more than 98%, but because the hydrofluoric acid is volatile, about 10% of the hydrofluoric acid is volatilized in a fluorine-containing waste gas form in an acidolysis process, serious pollution is caused to the ecological environment, the cost is high, and the method is not suitable for treating low-grade ores. At present, the hydrofluoric acid-sulfuric acid method widely applied in industry greatly reduces the consumption of hydrofluoric acid, the leaching rate is more than 85 percent, but still has the problem of environmental pollution, the concentration of sulfuric acid is high, the requirement on equipment is high, and the production cost is increased. Therefore, the development of a fluorine-free process is the key to the problem of decomposing tantalum-niobium ores. The Chinese patent (CN104745807A) adopts sulfuric acid-bisulfate to leach out tantalum-niobium ores, avoids using hydrofluoric acid, has no pollution to the environment, and has leaching rates of niobium and tantalum of more than 95 percent and rare earth elements close to 100 percent.
Some tantalum-niobium ores belong to refractory minerals, and after the previous beneficiation is finished, a part of low-grade ores containing 2-15% of tantalum and niobium can be generated, and the low-grade refractory minerals are quite complex in components and contain elements such as alkaline earth metals, rare earth metals, titanium, zirconium, tin, tungsten and the like. In addition, the tantalum-niobium-containing slag generated in smelting other metals uses the traditional hydrofluoric acid-sulfuric acid method to cause the heavy use of acid, the impurity separation effect is not good, and the recovery rate of tantalum and niobium is low. Chinese patent (CN103352117A) adopts ammonium bifluoride to roast low-grade niobium-containing ore, acid-soaks and then alkali-soaks the roasted product, and a multi-step separation process is carried out to separate niobium from various impurities, wherein the leaching rate of niobium can reach more than 97%. But the whole process still generates a large amount of fluorine-containing waste residue and waste water, and the environmental pollution is serious.
Disclosure of Invention
Aiming at the technical defects in the prior art, the invention aims to provide a method for decomposing low-grade tantalum-niobium resources by using acidic oxidizing roasting and converting the low-grade tantalum-niobium resources into tantalum-niobium peroxy complex which is easy to dissolve in low-concentration acid and generating aqueous tantalum-niobium oxide precipitate by using low-temperature decomposition of the tantalum-niobium peroxy complex so as to realize efficient separation of tantalum-niobium and other metals.
In order to realize the technical purpose, the invention provides a method for decomposing low-grade tantalum-niobium resources and extracting tantalum-niobium by an acid method, which comprises the following steps:
1) uniformly mixing the ground low-grade tantalum-niobium resource with persulfate and bisulfate, and then roasting to obtain a roasted product;
2) leaching the roasted product at a high temperature by adopting low acid to obtain leachate containing the tantalum-niobium peroxy complex;
3) and (3) carrying out decomposition reaction on the leachate containing the tantalum-niobium peroxy complex to obtain hydrous tantalum-niobium oxide precipitate.
According to the technical scheme, in the roasting process of the low-grade tantalum-niobium resource, the oxidizing persulfate and the acidic bisulfate are added as the additive components, so that tantalum and niobium in the low-grade tantalum-niobium resource can be selectively converted into a tantalum-niobium peroxy complex (H) which is easy to leach in low-concentration acid liquor in the high-temperature solid-phase reaction process2TaO2(O2) And H2NbO2(O2) Etc.) to combine low-concentration acid liquor and high-temperature leaching, under the condition, the high-efficiency leaching of the tantalum-niobium peroxy complex can be ensured, only a small amount of impurities such as titanium is contained, and silicon dioxide, zirconium, rare earth elements and the like are precipitated in a slag phase, so that the primary enrichment of tantalum and niobium can be realized, the stability of the tantalum-niobium peroxy complex is relatively poor, and the tantalum-niobium peroxy complex can be selectively decomposed and converted into aqueous tantalum-niobium oxide (Ta, Nb) at a proper temperature2O5·nH2And precipitating O, and remaining other impurities in the acid solution, so that high-purity hydrous tantalum-niobium oxide can be obtained, and the tantalum-niobium oxide can be obtained through simple high-temperature dehydration.
As a preferable scheme, the low-grade tantalum-niobium resource is ground until the mass percentage content of the fraction with the particle size of less than 0.043mm accounts for more than 90%. After the low-grade tantalum-niobium resources are ground to a proper granularity, the interaction between persulfate and bisulfate in the high-temperature solid-phase reaction and the low-grade tantalum-niobium resources is facilitated, and the high-temperature solid-phase reaction efficiency is improved.
In a preferred embodiment, the persulfate is at least one of sodium persulfate, potassium persulfate, and ammonium persulfate. The preferable persulfate has strong oxidizing property, and can selectively convert tantalum and niobium in low-grade tantalum and niobium resources into a tantalum and niobium peroxy complex which is easy to leach out in low-concentration acid liquor in the high-temperature solid-phase reaction process.
In a preferred embodiment, the bisulfate salt is at least one of potassium bisulfate, sodium bisulfate, ammonium bisulfate, and magnesium bisulfate. The bisulfate provides an acid environment for high-temperature solid-phase reaction, which is beneficial to the destruction of the mineral structure of low-grade tantalum-niobium resources, and on the other hand, the bisulfate can be used as a fluxing agent, thereby greatly reducing the roasting temperature and the roasting time.
As a preferable scheme, the mass ratio of the low-grade tantalum-niobium resource to the persulfate and the bisulfate is 1.0: (0.5-3): (2-4). The mass ratio of the low-grade tantalum-niobium resource to the persulfate and the bisulfate is further preferably 1.0: (0.5-2): (2-3).
As a preferred embodiment, the conditions of the roasting treatment are as follows:the temperature is 300-500 ℃ and the time is 2-3 hours. Under the condition of using persulfate and bisulfate together and the preferable roasting treatment, the method can ensure that the tantalum and niobium in the low-grade tantalum and niobium resource is selectively converted into a tantalum and niobium peroxy complex (H) which is easily dissolved in low-concentration acid liquid2TaO2(O2) And H2NbO2(O2) Etc.). The calcination temperature is preferably 400 to 500 ℃.
As a preferred scheme, the conditions of the low-acid high-temperature leaching are as follows: sulfuric acid with the concentration of less than or equal to 45 wt% is used as a leaching agent, the solid-liquid mass ratio is 1: 3-1: 5, the leaching temperature is 150-300 ℃, and the time is 1-2 hours. Under the optimized leaching condition, the tantalum-niobium can be efficiently and selectively leached by a tantalum-niobium peroxy complex, and silicon dioxide, zirconium, rare earth elements and the like are precipitated in a slag phase, so that the primary enrichment of the tantalum-niobium can be realized. The concentration of sulfuric acid is more preferably 20 to 45 wt%. The leaching temperature is further preferably 200-300 ℃.
As a preferred embodiment, the decomposition reaction conditions are: the temperature is 70-100 ℃, and the time is 1-3 hours. Under the optimized conditions, the method can ensure that metal impurities such as titanium and the like are still dissolved in acid liquor, and the tantalum-niobium peroxy complex is selectively decomposed and converted into hydrous tantalum-niobium oxide (Ta, Nb)2O5·nH2And (4) precipitating O. The decomposition reaction temperature is more preferably 90 to 98 ℃.
The low-grade tantalum-niobium resource is refractory low-grade ore containing tantalum and niobium or smelting slag containing tantalum and niobium generated in the process of smelting other metals, wherein the mass percentage content of tantalum and niobium is generally within the range of 2-15%.
The method for decomposing low-grade tantalum-niobium resources and extracting tantalum-niobium by the acid method comprises the following specific steps:
(1) grinding a low-grade tantalum-niobium raw material until the granularity is less than 0.043mm (the mass percentage content is more than 90%), and mixing the ground raw material with persulfate and hydrogen sulfate according to the mass ratio of 1.0: (0.5-3): (2-4) uniformly mixing;
(2) and (2) roasting the mixed material obtained in the step (1) in a muffle furnace at the roasting temperature of 300-500 ℃ for 2-3 hours to obtain a roasted product.
(3) And (3) performing acid leaching on the roasted product in the step (2), wherein the mass ratio of solid to liquid in the acid leaching is 1: 3-1: 5, the temperature is 150-300 ℃, the sulfuric acid concentration is not higher than 45 wt%, the leaching time is 1-2 hours, and performing solid-liquid separation to obtain acid leaching solution containing tantalum, niobium, titanium and certain impurities and precipitate containing silicon dioxide, zirconium, rare earth elements and the like.
(4) Heating the acid leaching solution obtained in the step (3) at a low temperature of 70-100 ℃ for 2-3 hours to obtain a tantalum-niobium peroxy complex (H)2TaO2(O2) And H2NbO2(O2) Etc.) into hydrous tantalum-niobium oxide, washing with water, press-filtering and drying to obtain hydrous tantalum-niobium oxide (Ta, Nb)2O5·nH2O。
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
according to the technical scheme, the low-grade tantalum-niobium resource is subjected to combined means of acid oxidizing roasting, low-acid high-temperature leaching, decomposition reaction and the like, so that the high-efficiency conversion of tantalum and niobium in the low-grade tantalum-niobium resource and the high-efficiency separation of the tantalum and niobium from metal impurities are realized, and the recovery rate of the obtained tantalum and niobium reaches 94-98%. According to the technical scheme, the tantalum and niobium in the low-grade tantalum and niobium resource are selectively converted into the tantalum and niobium peroxy complex (H) which is easily dissolved in acid liquor with low concentration at high temperature by adopting a special roasting additive2TaO2(O2) And H2NbO2(O2) Etc.) so that the tantalum-niobium can be leached efficiently under low-concentration acid liquor, and the tantalum-niobium peroxy complex with poor stability can be selectively converted into hydrous tantalum-niobium oxide (Ta, Nb) by controlling the temperature condition2O5·nH2And precipitating O, and remaining other impurities in the acid solution, so that further separation of tantalum and niobium from impurities can be realized.
Compared with the existing common acidolysis method, the method for treating the low-grade tantalum-niobium resource in the technical scheme of the invention avoids using hydrofluoric acid with high risk and high pollution for decomposition, reduces the concentration and the using amount of sulfuric acid, and is environment-friendly and low in equipment requirement.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples. These examples are only for better understanding of the present invention and do not limit the scope of the present invention.
In the following examples, the low-grade tantalum-niobium raw material is ground, and the mass percentage content of the low-grade tantalum-niobium raw material with the particle size of less than 0.043mm accounts for more than 90%.
Example 1
100g of ground low-grade tantalum-niobium ore (the components are shown in table 1), 100g of sodium persulfate and 200g of sodium bisulfate are uniformly mixed and put into a muffle furnace for roasting, the roasting temperature is controlled at 400 ℃, and the roasting time is 3 hours. Adding the molten product into a sulfuric acid solution (45 wt%), wherein the solid-liquid ratio is 1: 4, heating the mixture to 250 ℃ for 2 hours, filtering the mixture to obtain pickle liquor containing tantalum, niobium, titanium and certain impurities, heating the pickle liquor at 98 ℃ for 2 hours, washing, filter-pressing and drying the pickle liquor to obtain hydrous oxides (Ta, Nb) of tantalum, niobium2O5·nH2O。
The tantalum recovery rate is 96.0 percent and the niobium recovery rate is 97.3 percent through calculation.
TABLE 1 compositions, in wt%, of certain low grade tantalum niobium ores
Figure BDA0003044297350000051
Example 2
100g of ground low-grade tantalum-niobium ore (the components are shown in table 1), 200g of sodium persulfate and 200g of sodium bisulfate are uniformly mixed and put into a muffle furnace for roasting, the roasting temperature is controlled to be 500 ℃, and the roasting time is 2 hours. Adding the molten product into a sulfuric acid solution (45 wt%), wherein the solid-liquid ratio is 1: 4, heating the mixture at 200 ℃ for 2 hours, filtering the mixture to obtain pickle liquor containing tantalum, niobium, titanium and certain impurities, heating the pickle liquor at 98 ℃ for 3 hours, washing, filter-pressing and drying the pickle liquor to obtain hydrous oxides (Ta, Nb) of tantalum, niobium2O5·nH2O。
The tantalum recovery rate is 96.5 percent and the niobium recovery rate is 97.8 percent through calculation.
Example 3
100g of ground low-grade tantalum-niobium ore (the components are shown in table 1), 50g of potassium persulfate and 200g of potassium bisulfate are uniformly mixed and put into a muffle furnace for roasting, the roasting temperature is controlled at 400 ℃, and the roasting time is 3 hours. Adding the molten product into a sulfuric acid solution (45 wt%), wherein the solid-liquid ratio is 1:5, heating the mixture at 250 ℃ for 2 hours, filtering the mixture to obtain pickle liquor containing tantalum, niobium, titanium and certain impurities, heating the pickle liquor at 95 ℃ for 2 hours, washing, filter-pressing and drying the pickle liquor to obtain hydrous oxides (Ta, Nb) of tantalum, niobium2O5·nH2O。
The tantalum recovery rate is 95.5 percent and the niobium recovery rate is 96.2 percent through calculation.
Example 4
100g of ground low-grade tantalum-niobium ore (the components are shown in table 1), 300g of sodium persulfate and 200g of ammonium bisulfate are uniformly mixed and put into a muffle furnace for roasting, the roasting temperature is controlled at 400 ℃, and the roasting time is 3 hours. Adding the molten product into a sulfuric acid solution (30 wt%), wherein the solid-liquid ratio is 1: 4, heating the mixture to 250 ℃ for 2 hours, filtering the mixture to obtain pickle liquor containing tantalum, niobium, titanium and certain impurities, heating the pickle liquor at 90 ℃ for 3 hours, washing, filter-pressing and drying the pickle liquor to obtain hydrous oxides (Ta, Nb) of tantalum, niobium2O5·nH2O。
The calculated results show that the recovery rate of tantalum is 95.8 percent and the recovery rate of niobium is 96.8 percent.
Example 5
100g of ground low-grade tantalum-niobium ore (the components are shown in table 1), 100g of sodium persulfate and 200g of magnesium bisulfate are uniformly mixed and put into a muffle furnace for roasting, the roasting temperature is controlled at 400 ℃, and the roasting time is 3 hours. Adding the molten product into a sulfuric acid solution (45 wt%), wherein the solid-liquid ratio is 1:5, heating the mixture at 200 ℃ for 2h, filtering the mixture to obtain pickle liquor containing tantalum, niobium, titanium and certain impurities, heating the pickle liquor at 98 ℃ for 3h, washing, filter-pressing and drying the pickle liquor to obtain hydrous oxides (Ta, Nb) of tantalum, niobium2O5·nH2O。
The tantalum recovery rate is 96.8 percent and the niobium recovery rate is 97.3 percent through calculation.
Comparative example 1
100g of ground low-grade tantalum-niobium ore (the components are shown in table 1), 100g of sodium persulfate and 200g of sodium sulfate are uniformly mixed and put into a muffle furnace for roasting, the roasting temperature is controlled to be 400 ℃, and the roasting time is 3 hours. Adding the molten product into a sulfuric acid solution (20 wt%), wherein the solid-liquid ratio is 1: 4, heating at 200 ℃ for 2h, filtering to obtain pickle liquor containing tantalum, niobium, titanium and some impurities, heating the pickle liquor at 90 ℃ for 3h, washing with water, filter-pressing and drying to obtain aqueous oxide (Ta, Nb) of tantalum, niobium2O5·nH2O。
The calculated recovery rate of tantalum is 29.8 percent, and the recovery rate of niobium is 27.9 percent. In the comparative example, acidic sodium bisulfate is not selected as the roasting additive, so that the high-efficiency conversion of tantalum and niobium in low-grade tantalum-niobium ore is difficult to realize.
Comparative example 2
100g of ground low-grade tantalum-niobium ore (the components are shown in table 1), 100g of sodium persulfate and 200g of sodium bisulfate are uniformly mixed and put into a muffle furnace for roasting, the roasting temperature is controlled to be 250 ℃, and the roasting time is 3 hours. Adding the molten product into a sulfuric acid solution (20 wt%), wherein the solid-liquid ratio is 1: 4, heating at 200 ℃ for 2h, filtering to obtain pickle liquor containing tantalum, niobium, titanium and some impurities, heating the pickle liquor at 90 ℃ for 3h, washing with water, filter-pressing and drying to obtain aqueous oxide (Ta, Nb) of tantalum, niobium2O5·nH2O。
The calculated results show that the recovery rate of tantalum is 76.8 percent, and the recovery rate of niobium is 77.5 percent. In the comparative example, the roasting temperature is too low, and the high-efficiency conversion of tantalum and niobium in low-grade tantalum-niobium ore is difficult to realize.
Comparative example 3
100g of ground low-grade tantalum-niobium ore (the components are shown in table 1), 100g of sodium persulfate and 200g of sodium bisulfate are uniformly mixed and put into a muffle furnace for roasting, the roasting temperature is controlled at 400 ℃, and the roasting time is 3 hours. Adding the molten product into a sulfuric acid solution (10 wt%), wherein the solid-to-liquid ratio is 1: 4, heating the mixture at 120 ℃ for 2 hours, filtering the mixture to obtain pickle liquor containing tantalum, niobium, titanium and certain impurities, heating the pickle liquor at 90 ℃ for 3 hours, washing the pickle liquor with water, performing filter pressing and drying to obtain hydrous oxide of tantalum and niobiumThing (Ta, Nb)2O5·nH2O。
The calculated results show that the recovery rate of tantalum is 60.2 percent and the recovery rate of niobium is 68.5 percent. The comparative example shows that the temperature and sulfuric acid concentration during acid leaching are not in the preferred ranges, resulting in a lower tantalum-niobium recovery.
In conclusion, through analysis of comparative examples, for low-grade tantalum-niobium resources, the decomposition efficiency can be obviously improved through the fusion roasting of persulfate and bisulfate and low-temperature leaching of low-concentration sulfuric acid, and the method is simple in process flow, low in requirement on equipment and suitable for industrial large-scale production.

Claims (8)

1. A method for decomposing low-grade tantalum-niobium resources and extracting tantalum-niobium by an acid method is characterized by comprising the following steps: the method comprises the following steps:
1) uniformly mixing the ground low-grade tantalum-niobium resource with persulfate and bisulfate, and then roasting to obtain a roasted product;
2) leaching the roasted product at a high temperature by adopting low acid to obtain leachate containing the tantalum-niobium peroxy complex;
3) and (3) carrying out decomposition reaction on the leachate containing the tantalum-niobium peroxy complex to obtain hydrous tantalum-niobium oxide precipitate.
2. The method for acid decomposition of low-grade tantalum-niobium resources and extraction of tantalum-niobium according to claim 1, characterized in that: the low-grade tantalum-niobium resource is ground until the mass percentage of the grain size of less than 0.043mm accounts for more than 90%.
3. The method for acid decomposition of low-grade tantalum-niobium resources and extraction of tantalum-niobium according to claim 1, characterized in that: the persulfate is at least one of sodium persulfate, potassium persulfate and ammonium persulfate.
4. The method for acid decomposition of low-grade tantalum-niobium resources and extraction of tantalum-niobium according to claim 1, characterized in that: the bisulfate is at least one of potassium bisulfate, sodium bisulfate, ammonium bisulfate and magnesium bisulfate.
5. The method for decomposing low-grade tantalum-niobium resources and extracting tantalum-niobium by an acid method according to any one of claims 1-4, characterized by comprising the following steps: the mass ratio of the low-grade tantalum-niobium resource to the persulfate and the bisulfate is 1.0: (0.5-3): (2-4).
6. The method for acid decomposition of low-grade tantalum-niobium resources and extraction of tantalum-niobium according to claim 1, characterized in that: the roasting treatment conditions are as follows: the temperature is 300-500 ℃ and the time is 2-3 hours.
7. The method for acid decomposition of low-grade tantalum-niobium resources and extraction of tantalum-niobium according to claim 1, characterized in that: the conditions of the low-acid high-temperature leaching are as follows: sulfuric acid with the concentration of less than or equal to 45 wt% is used as a leaching agent, the solid-liquid mass ratio is 1: 3-1: 5, the leaching temperature is 150-300 ℃, and the time is 1-2 hours.
8. The method for acid decomposition of low-grade tantalum-niobium resources and extraction of tantalum-niobium according to claim 1, characterized in that: the conditions of the decomposition reaction are as follows: the temperature is 70-100 ℃, and the time is 1-3 hours.
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GB649342A (en) * 1941-05-19 1951-01-24 Titan Company A S Improvements in or relating to the separation of niobium and tantalum from ores
GB837110A (en) * 1955-12-21 1960-06-09 Andrew Thomas Mccord Process of extracting and recovering columbium and tantalum from their ores and products thereof
AU8224082A (en) * 1981-04-02 1982-10-07 Starck, Hermann C Recovery of niobium and tantalum from radioactive metal ores
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