CN111607697B - Method for separating niobium and tantalum and application thereof - Google Patents
Method for separating niobium and tantalum and application thereof Download PDFInfo
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Abstract
The invention discloses a method for separating niobium and tantalum and application thereof, wherein the method comprises the steps of reacting raw materials containing niobium and tantalum to prepare hydroxides of niobium and tantalum, leaching with mixed acid of oxalic acid and tartaric acid, extracting the obtained leachate with N235, back-extracting the extract with nitric acid to prepare niobium oxide, and adjusting acid to precipitate raffinate to obtain tantalum oxide. The method adopts the mixed acid of oxalic acid and tartaric acid to leach the tantalum and the niobium, wherein the oxalic acid is used as the main leaching acid, the tartaric acid is used as the leaching auxiliary acid, and the mixed acid has the leaching capability of the oxalic acid and the stabilizing capability of the tartaric acid, so that the method has higher leaching rate and solution stability, and the total recovery rate of the tantalum and the niobium is improved; the invention further optimizes the alkali liquor decomposition conditions, reduces the reaction temperature and greatly saves the energy consumption; the method has good separation effect of tantalum and niobium, and realizes the separation of tantalum and niobium without fluorination.
Description
Technical Field
The invention relates to the technical field of hydrometallurgy, in particular to a method for separating niobium and tantalum and application thereof.
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 are similar in nature and are often intergrown, and therefore, separation of tantalum and niobium is critical in the field of tantalum and niobium metallurgy and recovery. Tantalum and niobium have excellent chemical stability and similar chemical properties, so that the separation of the two is difficult.
At present, known methods for effectively separating tantalum and niobium include fractional crystallization, chlorination distillation, ion exchange and solvent extraction; among them, the solvent extraction method is most widely used.
At present, in the field of tantalum-niobium metallurgy, the mainstream method for separating tantalum and niobium is a solvent extraction method, which is a flow of hydrofluoric acid leaching-MIBK extraction separation, and the method is recorded in detail in U.S. Pat. No. 3117833; specifically, the method comprises the steps of firstly treating a raw material containing tantalum and niobium by using hydrofluoric acid, then extracting the tantalum and niobium in the solution by using MIBK, back extracting a niobium-fluorine complex in an organic ketone phase by using dilute sulfuric acid, and back extracting the tantalum-fluorine complex by using pure water. However, in the process of separating and recovering tantalum and niobium, 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 can generate a large amount of three wastes containing fluorine, and the wastes and the hydrofluoric acid have high toxicity and are extremely harmful to the environment and the bodies of operators.
In order to solve the problems, the Chinese patent application with the publication number of CN101955228A discloses an improvement method, which is used for reducing the concentration of hydrofluoric acid in the extraction process, thereby reducing the generation amount of fluorine-containing waste liquid and waste residue; however, the method reduces the fluorine pollution to a certain extent, and the traditional end treatment method is converted into source treatment, so that the economic benefit and the environmental benefit are improved, but the fluorine pollution is generated not only in the extraction process, but also in the leaching process, which is an important link for generating the fluorine pollution, the method cannot reduce the fluorine pollution in the leaching process, and the method only can reduce the fluorine pollution properly in quantity, and cannot essentially solve the problem of the fluorine pollution.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention makes up the defects of the prior art, provides a fluorine-free tantalum-niobium separation method, avoids the use of hydrofluoric acid in the separation process, does not generate fluorine-containing three wastes, 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.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method of separating niobium and tantalum, comprising,
reacting raw materials containing niobium and tantalum to prepare niobium and tantalum hydroxide, leaching with mixed acid of oxalic acid and tartaric acid, extracting the obtained leachate by adopting N235, finally back extracting the extract by using nitric acid to prepare niobium oxide, and adjusting acid to precipitate raffinate to obtain tantalum oxide.
Specifically, in the process of leaching by using mixed acid of oxalic acid and tartaric acid, oxalic acid reacts with hydroxides of tantalum and niobium to generate a soluble tantalum niobium oxalic acid complex; the tartaric acid can enhance the stability of tantalum and niobium in the solution and reduce the hydroxide precipitation of tantalum and niobium generated by side reaction, thereby improving the leaching rate.
In the above technical scheme, in the mixed acid, the molar ratio of oxalic acid to tartaric acid is 1-5: 1.
in particular, 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 a leaching auxiliary acid which provides a functional group, and the main purpose is to improve the stability of the tantalum and niobium complex in a solution without adding excessive amount.
Further, in the technical scheme, the leaching temperature and time are 60-68 ℃ and 1-4h respectively.
Specifically, since oxalic acid complexes of tantalum and niobium are unstable at high temperature, the oxalic acid complexes thereof are rapidly decomposed into hydroxides when the temperature reaches 70 ℃, and thus the leaching temperature should be lower 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 60 to 68 ℃. In addition, because tantalum and niobium have strong chemical stability and reaction rate is much slower than that of active metals, the leaching time should be properly prolonged; specifically, most of the leaching of tantalum and niobium can be completed within 1-2h 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.
Further, in the above technical solution, the process of reacting the raw materials containing niobium and tantalum to prepare the hydroxide specifically comprises roasting the raw materials containing niobium and tantalum at high temperature, washing the obtained roasted powder with acid, then placing the roasted powder in a hydrothermal tank, performing alkaline leaching decomposition with sodium hydroxide solution, and finally hydrolyzing the obtained alkaline leaching product with hydrochloric acid to obtain the hydroxide of niobium and tantalum.
In particular, most of the prior art for preparing tantalum and niobium hydroxides uses a method of hydrofluoric acid leaching and then ammonia water precipitation, and the method uses hydrofluoric acid, so that the pollution is large; in addition, there is a method of using alkali liquid for high-pressure decomposition, but the alkali leaching temperature is as high as 205-300 ℃. The method reduces the reaction temperature, reduces the energy consumption and saves the resources under the condition of ensuring the reaction products at the temperature of 150-.
In detail, in the technical scheme, the concentration of the sodium hydroxide solution is 2-5mol/L in the alkaline leaching decomposition process.
Specifically, during alkaline leaching decomposition, increasing the reactant concentration can accelerate the reaction rate, but too high a concentration increases the liquid viscosity; in addition, the concentration of the NaOH solution is also related to the liquid-solid ratio of the reaction, and when a NaOH solution with lower concentration is adopted, a higher solid-liquid ratio is selected to ensure that the actual NaOH amount is more than the theoretical amount.
Preferably, in the above technical solution, in the alkaline leaching decomposition process, the amount of the sodium hydroxide solution added is controlled such that the solid-to-liquid ratio is 3-5: 1.
in detail, in the above technical scheme, in the process of alkaline leaching decomposition, the reaction temperature and the reaction time are 150 ℃ and 200 ℃ and 1-4h respectively.
Specifically, in the alkaline leaching decomposition process, because tantalum and niobium have strong chemical stability, a certain temperature needs to be provided for the decomposition reaction, the reaction can occur in a hydrothermal tank at 150 ℃, and the reaction rate can be increased along with the further increase of the temperature; in addition, the reaction temperature and time have a corresponding relationship, when higher temperature is used, shorter reaction time can be used, the problems of reaction energy consumption and high-temperature deformation of a reaction container are comprehensively considered, and the reaction temperature and the reaction time of alkaline leaching decomposition are respectively controlled to be 150-200 ℃ and 1-4 h.
In detail, in the above technical solution, the acid for cleaning the baked powder is a mixed acid of hydrochloric acid and nitric acid.
Preferably, in the above technical solution, the acid for cleaning the roasted powder is in a molar ratio of 0.5 to 3: 1 hydrochloric acid and nitric acid, and the concentration of the hydrochloric acid in the mixed acid is 1-5 mol/L.
Specifically, the purpose of washing the calcined powder with an acid is to remove active metal impurities in the powder; the nitric acid has strong acidity and oxidizability, and has excellent effect after being mixed with the hydrochloric acid, and the higher the hydrochloric acid concentration in the mixed acid is, the stronger the impurity removal capability is, so that the general active metal impurities can be basically treated after the hydrochloric acid concentration reaches 5mol/L, and meanwhile, the hydrochloric acid concentration is not lower than 1mol/L for ensuring the acidity and the impurity removal effect of the solution.
Further preferably, in the above technical solution, the temperature and time for cleaning the roasted powder are 50-70 ℃ and 0.5-2h, respectively.
In one embodiment, the temperature and time of the high-temperature calcination are 600-1000 ℃ and 0.5-2h, respectively.
In another embodiment, the hydrochloric acid concentration of the hydrolyzed alkaline leach product is from 1 to 2 mol/L.
Still further, in the above technical solution, in the process of extracting the leachate with N235, the O: a is 1-5: 1.
still further, in the above technical solution, in the process of stripping the extract with nitric acid, the concentration of the nitric acid is 0.5-1 mol/L.
The invention also provides the application of the method in separating the metal niobium and the metal tantalum.
The invention has the following advantages:
(1) according to the method, tantalum and niobium are leached by adopting mixed acid of oxalic acid and tartaric acid, the oxalic acid is used as main leaching acid, the tartaric acid is used as auxiliary leaching acid, and the mixed acid has the leaching capacity of the oxalic acid and the stabilizing capacity of the tartaric acid, so that compared with single oxalic acid leaching, the method has higher leaching rate and solution stability, and the total recovery rate of tantalum and niobium is improved;
(2) in the process of decomposing the tantalum-niobium oxide by using the sodium hydroxide solution in the hydrothermal tank, the alkali liquor decomposition condition is further optimized, the reaction temperature is reduced, and the energy consumption is greatly saved;
(3) the method provided by the invention has good separation effect of tantalum and niobium, the purity of the prepared tantalum and niobium product is high and can reach 97%, and a fluoride-free process is realized in the separation and recovery process of tantalum and niobium, so that the method has great significance for environmental protection and green production.
Drawings
Fig. 1 is a flow chart of a process for separating niobium and tantalum in an embodiment of the present invention.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to specific examples.
The following examples are merely illustrative of the present invention and are not intended to limit the scope of the present invention.
The experimental procedures used in the following examples are conventional unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
As shown in figure 1, the powder containing tantalum and niobium is placed in a muffle furnace at 800 ℃ for roasting for 1 h; washing the roasted powder for 1h at 70 ℃ by using 2M hydrochloric acid and 1M nitric acid to remove impurities; putting the powder after impurity removal into a water heating tank filled with 5M sodium hydroxide solution, reacting for 2h at 200 ℃ according to the liquid-solid ratio of 5: 1, cooling to room temperature after the reaction is finished, and taking filter residue; the residue was hydrolyzed with 1M hydrochloric acid at room temperature for 2h and filtered to obtain a solid powder.
Dissolving the powder with mixed organic acid of 40% oxalic acid and 20% tartaric acid at 65 deg.C for 2 hr; preparing an extracting agent from N235 and secondary octanol (a diluent) according to the mass ratio of 3: 7, extracting niobium oxalate in an organic acid solution at room temperature, wherein the extraction ratio of O to A is 5: 1, and extracting for 30min to obtain an extraction liquid and a raffinate.
Carrying out back extraction on the extract liquor by using a 0.5M nitric acid solution, then gradually adding a 5M sulfuric acid solution until no precipitate is generated, filtering and cleaning the obtained precipitate to obtain high-purity niobium oxide with the purity of more than or equal to 99%, gradually adding a 5M sulfuric acid solution into the extract liquor until no precipitate is generated, filtering and cleaning the obtained precipitate to obtain high-purity tantalum oxide with the purity of more than or equal to 98%; further, the total recovery of tantalum and niobium was 97.3%.
Example 2
Placing the powder containing tantalum and niobium in a muffle furnace at 600 ℃ for roasting for 2 h; washing the roasted powder with 3M hydrochloric acid +1M nitric acid at 50 ℃ for 2h to remove impurities; putting the powder after impurity removal into a water heating tank filled with 2M sodium hydroxide solution, reacting for 4 hours at 150 ℃ with the liquid-solid ratio of 3: 1, cooling to room temperature after the reaction is finished, and taking filter residue; the residue was hydrolyzed with 1M hydrochloric acid at room temperature for 2h and filtered to obtain a solid powder.
Dissolving the powder with mixed organic acid of 50% oxalic acid and 10% tartaric acid at 65 deg.C for 4 hr; preparing an extracting agent from N235 and secondary octanol (a diluent) according to the mass ratio of 3: 7, extracting niobium oxalate in an organic acid solution at room temperature, wherein the extraction ratio of O to A is 3: 1, and extracting for 30min to obtain an extraction liquid and a raffinate.
Carrying out back extraction on the extract liquor by using a 0.5M nitric acid solution, then gradually adding a 5M sulfuric acid solution until no precipitate is generated, filtering and cleaning the obtained precipitate to obtain high-purity niobium oxide with the purity of more than or equal to 99%, gradually adding a 5M sulfuric acid solution into the extract liquor until no precipitate is generated, filtering and cleaning the obtained precipitate to obtain high-purity tantalum oxide with the purity of more than or equal to 98%; further, the total recovery of tantalum and niobium was 97.8%.
Example 3
Placing the powder containing tantalum and niobium in a muffle furnace at 1000 ℃ for roasting for 0.5 h; washing the roasted powder with 3M hydrochloric acid +1M nitric acid at 70 deg.C for 0.5h to remove impurities; putting the powder after impurity removal into a water heating tank filled with 5M sodium hydroxide solution, reacting for 1h at 200 ℃ according to the liquid-solid ratio of 5: 1, cooling to room temperature after the reaction is finished, and taking filter residue; the residue was hydrolyzed with 2M hydrochloric acid at room temperature for 2h and filtered to obtain a solid powder.
Dissolving the powder with mixed organic acid of 20% oxalic acid and 20% tartaric acid at 65 deg.C for 1 hr; preparing an extracting agent from N235 and secondary octanol (a diluent) according to the mass ratio of 3: 7, extracting niobium oxalate in an organic acid solution at room temperature, wherein the extraction ratio of O to A is 5: 1, and extracting for 30min to obtain an extraction liquid and a raffinate.
Extracting the extract liquor with 1M nitric acid solution to back extract niobium, then gradually adding 5M sulfuric acid solution until no precipitate is generated, filtering and cleaning the obtained precipitate to obtain high-purity niobium oxide with the purity of more than or equal to 98%, gradually adding 5M sulfuric acid solution into the raffinate until no precipitate is generated, filtering and cleaning the obtained precipitate to obtain high-purity tantalum oxide with the purity of more than or equal to 97%; in addition, the total recovery of tantalum and niobium was 96.2%.
Comparative example 1
Similar to example 1, the powder containing tantalum and niobium was placed in a muffle furnace at 800 ℃ for calcination for 1 h; washing the roasted powder for 1h at 70 ℃ by using 2M hydrochloric acid and 1M nitric acid to remove impurities; putting the powder after impurity removal into a water heating tank filled with 5M sodium hydroxide solution, reacting for 2h at 200 ℃ according to the liquid-solid ratio of 5: 1, cooling to room temperature after the reaction is finished, and taking filter residue; the residue was hydrolyzed with 1M hydrochloric acid at room temperature for 2h and filtered to obtain a solid powder.
Dissolving the powder with 40% oxalic acid at 65 deg.C for 2 h; preparing an extracting agent from N235 and secondary octanol (a diluent) according to the mass ratio of 3: 7, extracting niobium oxalate in an organic acid solution at room temperature, wherein the extraction ratio of O to A is 5: 1, and extracting for 30min to obtain an extraction liquid and a raffinate.
Carrying out back extraction on the extract liquor by using a 0.5M nitric acid solution, then gradually adding a 5M sulfuric acid solution until no precipitate is generated, filtering and cleaning the obtained precipitate to obtain high-purity niobium oxide with the purity of more than or equal to 99%, gradually adding a 5M sulfuric acid solution into the extract liquor until no precipitate is generated, filtering and cleaning the obtained precipitate to obtain high-purity tantalum oxide with the purity of more than or equal to 98%; further, the total recovery of tantalum and niobium was 94.8%.
Finally, the above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for separating niobium and tantalum,
comprises reacting raw materials containing niobium and tantalum to prepare hydroxide of niobium and tantalum, leaching with mixed acid of oxalic acid and tartaric acid, extracting with N235 to obtain leachate, back extracting with nitric acid to obtain niobium oxide, and precipitating with acid to obtain raffinate;
in the mixed acid, the molar ratio of oxalic acid to tartaric acid is 1-5: 1;
the leaching temperature and time are 60-68 ℃ and 1-4h respectively;
the method specifically comprises the steps of roasting raw materials containing niobium and tantalum at high temperature, washing the roasted powder obtained by acid washing, then putting the roasted powder into a hydrothermal tank, performing alkaline leaching decomposition by using a sodium hydroxide solution, and finally hydrolyzing the alkaline leaching product obtained by hydrochloric acid to obtain the hydroxide of niobium and tantalum;
the temperature and the time of the high-temperature roasting are respectively 600-1000 ℃ and 0.5-2 h;
the temperature and the time for cleaning the roasted powder are respectively 50-70 ℃ and 0.5-2 h;
in the alkaline leaching decomposition process, the reaction temperature and the reaction time are respectively 150 ℃ and 200 ℃ and 1-4 h.
2. The method of claim 1,
in the process of the alkaline leaching decomposition, the alkaline leaching solution is added with a solvent,
the concentration of the sodium hydroxide solution is 2-5 mol/L.
3. The method of claim 2,
the addition amount of the sodium hydroxide solution is controlled to be 3-5: 1.
4. the method of claim 1,
the acid for cleaning the roasted powder is a mixed acid of hydrochloric acid and nitric acid.
5. The method of claim 4,
the acid for cleaning the roasted powder is prepared from the following components in a molar ratio of 0.5-3: 1 hydrochloric acid and nitric acid, and the concentration of the hydrochloric acid in the mixed acid is 1-5 mol/L.
6. The method according to any one of claims 1 to 5,
the concentration of the hydrochloric acid of the hydrolysis alkaline leaching product is 1-2 mol/L.
7. The method according to any one of claims 1 to 5,
and in the process of extracting the leaching solution by the N235, controlling the O: a is 1-5: 1;
and/or, in the process of back extraction of the extract by nitric acid, the concentration of the nitric acid is 0.5-1 mol/L.
8. The method of claim 6,
and in the process of extracting the leaching solution by the N235, controlling the O: a is 1-5: 1;
and/or, in the process of back extraction of the extract by nitric acid, the concentration of the nitric acid is 0.5-1 mol/L.
9. Use of the method according to any one of claims 1 to 8 for separating niobium and tantalum metals.
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