CN110627123A - Method for recovering tantalum and niobium from tantalum-niobium alloy - Google Patents
Method for recovering tantalum and niobium from tantalum-niobium alloy Download PDFInfo
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Abstract
The invention provides a method for recovering tantalum and niobium from a tantalum-niobium alloy, which relates to the field of tantalum and niobium recovery and comprises the following steps: s1) providing tantalum-niobium alloy powder as a raw material, and then carrying out chlorination sintering treatment on the tantalum-niobium alloy powder to obtain chlorides containing tantalum and niobium; s2) putting the chloride into alkali liquor for hydrolysis treatment to obtain hydroxide containing tantalum and niobium; s3) performing gravity separation to complete the recovery of tantalum and niobium. By the method, the technical problem that the production environment is seriously threatened due to the fact that HF is volatile and easily generates hydrogen when the HF is used for acid hydrolysis in the existing tantalum-niobium recovery method can be solved, and the purpose of improving the safety of the production environment is achieved.
Description
Technical Field
The invention relates to the field of tantalum-niobium recovery, in particular to a method for recovering tantalum-niobium from a tantalum-niobium alloy.
Background
China is the world with the most abundant mineral resources of rare metals such as tantalum, niobium and the like. However, the tantalum ore deposit in China has low ore taste, fine and dispersed embedded particle size and associated polymetallic, so that the tantalum ore deposit is difficult to collect, separate and select and has low recovery rate. China has no independent niobium mine, and niobium is often associated with rare earth and tantalum.
The tantalum-niobium alloy waste is mainly leftover materials generated in the production process of tantalum-niobium alloy and a large amount of tantalum and niobium component waste which is removed and replaced after equipment is replaced in the fields of spaceflight, aviation, war industry, electronics and the like.
In the prior art, when tantalum-niobium alloy waste is treated, an HF-H2SO4-TBP separation system, an HF-H2SO 4-acetamide separation system, an HF-H2SO4-MIBK separation system and an HF-H2SO 4-sec-octanol separation system are mainly used, and in the four tantalum-niobium separation systems, HF acid hydrolysis is adopted, then extraction separation is carried out, and precipitation recovery is carried out. The HF acid hydrolysis has extremely high requirements on equipment, has strong volatility and is easy to cause pollution to a production site, and in the acid leaching process, a large amount of hydrogen is generated, so that the problems of explosion and the like are easy to occur, and thus the safety of the production site is seriously threatened.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a method for recovering tantalum and niobium from a tantalum-niobium alloy, which aims to solve the technical problem that the production environment is seriously threatened due to the fact that HF is volatile and easily generates hydrogen when the HF is used for acid hydrolysis in the existing tantalum-niobium recovery method.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a method for recovering tantalum and niobium from a tantalum-niobium alloy comprises the following steps:
s1) providing tantalum-niobium alloy powder as a raw material, and then carrying out chlorination sintering treatment on the tantalum-niobium alloy powder to obtain chlorides containing tantalum and niobium;
s2) putting the chloride into alkali liquor for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s3) performing gravity separation to complete the recovery of tantalum and niobium.
Further, in the step S1), the particle size of the tantalum-niobium alloy powder is 0.1 to 1mm, and preferably 0.2 to 0.9 mm.
Further, the preparation method of the tantalum-niobium alloy powder comprises the following steps: firstly, carrying out coarse crushing on the tantalum-niobium alloy by using a jaw crusher, and then carrying out fine grinding on the tantalum-niobium alloy after coarse grinding by using a Raymond mill to obtain the tantalum-niobium alloy powder.
Further, in the step S1), the process parameters of the chlorination sintering include: the chlorination sintering temperature is 500-1200 ℃, and the chlorination sintering time is 1-3 h.
Further, in the step S1), the process parameters of the chlorination sintering include: the chlorination sintering temperature is 600-1100 ℃, and the chlorination sintering time is 1.5-2.5 h.
Further, the chloridizing sintering is carried out in a boiling furnace.
Further, in the step S2), the alkali solution is sodium hydroxide and/or potassium hydroxide.
Further, the molar concentration of the alkali liquor is 1-3 mol/L.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for recovering tantalum and niobium from tantalum-niobium alloy, which takes crushed tantalum-niobium alloy powder as a raw material, firstly performs chlorination and sintering treatment on the raw material to obtain chloride containing tantalum and niobium, then performs hydrolysis treatment on the obtained chloride by using alkali to obtain hydroxide containing tantalum and niobium, and can separate the hydroxide containing tantalum and the hydroxide containing niobium by adopting a gravity separation mode due to larger density difference of the hydroxide containing tantalum and the hydroxide containing niobium, and finally completes the recovery of tantalum and niobium. In the method, the alkali liquor is used for replacing the original HF acid, so that the alkali liquor is not easy to volatilize and has small harm to the production environment; meanwhile, hydrogen is not generated in the hydrolysis process, so that the danger of explosion is avoided. The recovery rate of tantalum and niobium recovered by the method is over 88 percent.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that:
in the present invention, all the embodiments and preferred methods mentioned herein can be combined with each other to form a new technical solution, if not specifically stated.
In the present invention, all the technical features mentioned herein and preferred features may be combined with each other to form a new technical solution, if not specifically stated.
In the present invention, the percentage (%) or parts means the weight percentage or parts by weight with respect to the composition, if not otherwise specified.
In the present invention, the components referred to or the preferred components thereof may be combined with each other to form a novel embodiment, if not specifically stated.
In the present invention, unless otherwise stated, the numerical range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, a numerical range of "6 to 22" means that all real numbers between "6 to 22" have been listed herein, and "6 to 22" is simply a shorthand representation of the combination of these values.
The "ranges" disclosed herein may have one or more lower limits and one or more upper limits, respectively, in the form of lower limits and upper limits.
In the present invention, unless otherwise specified, the individual reactions or operation steps may be performed sequentially or may be performed in sequence. Preferably, the reaction processes herein are carried out sequentially.
Unless otherwise defined, technical and scientific terms used herein have the same meaning as is familiar to those skilled in the art. In addition, any methods or materials similar or equivalent to those described herein can also be used in the present invention.
The invention provides a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) providing tantalum-niobium alloy powder as a raw material, and then carrying out chlorination sintering treatment on the tantalum-niobium alloy powder to obtain chlorides containing tantalum and niobium;
s2) putting the chloride into alkali liquor for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s3) performing gravity separation to complete the recovery of tantalum and niobium.
The invention provides a method for recovering tantalum and niobium from tantalum-niobium alloy, which takes crushed tantalum-niobium alloy powder as a raw material, firstly performs chlorination and sintering treatment on the raw material to obtain chloride containing tantalum and niobium, then performs hydrolysis treatment on the obtained chloride by using alkali to obtain hydroxide containing tantalum and niobium, and can separate the hydroxide containing tantalum and the hydroxide containing niobium by adopting a gravity separation mode due to larger density difference of the hydroxide containing tantalum and the hydroxide containing niobium, and finally completes the recovery of tantalum and niobium. In the method, the alkali liquor is used for replacing the original HF acid, so that the alkali liquor is not easy to volatilize and has small harm to the production environment; meanwhile, hydrogen is not generated in the hydrolysis process, so that the danger of explosion is avoided. The recovery rate of tantalum and niobium recovered by the method is over 88 percent.
In some embodiments of the present invention, gravity sorting may include, but is not limited to, dense media sorting, air sorting, and the like.
The chlorination sintering in the invention refers to sintering treatment of tantalum-niobium alloy powder under a chlorine atmosphere. The specific amount of the introduced chlorine is determined by calculation according to the contents of tantalum and niobium in the tantalum-niobium alloy powder and the content of impurities in the tantalum-niobium alloy powder.
In some embodiments of the present invention, in step S1), the grain size of the tantalum-niobium alloy powder is 0.1 to 1mm, preferably 0.2 to 0.9 mm.
By optimizing the particle size of the tantalum-niobium alloy powder, the chlorination sintering process can be carried out more fully, and meanwhile, the reaction efficiency and the reaction rate in the hydrolysis process can be improved.
In the above embodiment, the particle size of the tantalum-niobium alloy powder may be, for example, 0.1mm, 0.2mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm or 1.0 mm.
In some embodiments of the present invention, the method for preparing the tantalum-niobium alloy powder comprises: firstly, carrying out coarse crushing on the tantalum-niobium alloy by using a jaw crusher, and then carrying out fine grinding on the tantalum-niobium alloy after coarse grinding by using a Raymond mill to obtain the tantalum-niobium alloy powder.
The coarse crushing and fine crushing are combined, so that tantalum-niobium alloy powder with the required particle size can be obtained, the operation is convenient, and the reaction efficiency and the reaction rate in the hydrolysis process can be improved.
In some embodiments of the present invention, in step S1), the process parameters of the chlorination sintering include: the chlorination sintering temperature is 500-1200 ℃, and the chlorination sintering time is 1-3 h; in a further embodiment, in the step S1), the process parameters of the chlorination sintering include: the chlorination sintering temperature is 600-1100 ℃, and the chlorination sintering time is 1.5-2.5 h.
By optimizing the sintering process, the chlorination sintering process can be carried out more fully, so that the hydrolysis effect in the hydrolysis process is improved, and the recovery rate of tantalum and niobium is improved.
In the above embodiment, the chlorination sintering temperature may be, for example, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃, 1100 ℃ or 1200 ℃; the chlorination sintering time may be, for example, 1h, 1.5h, 2h, 2.5h, or 3 h.
In some embodiments of the invention, the chloridizing sintering is performed in a fluidized bed furnace. The chlorination sintering is carried out in a fluidized bed furnace, so that the sintering is more sufficient.
In some embodiments of the present invention, in the step S2), the alkali solution is sodium hydroxide and/or potassium hydroxide. In a further embodiment, the molar concentration of the alkali liquor is 1-3 mol/L.
The sodium hydroxide or potassium hydroxide is selected as the hydrolysis alkali liquor, so that the efficiency in the hydrolysis process can be improved, and the recovery rate is improved. Meanwhile, the reaction efficiency in the hydrolysis process can be improved by optimizing the molar concentration of the alkali liquor.
In the above embodiment, the molar concentration of the alkali solution may be, for example, 1mol/L, 1.5mol/L, 2mol/L, 2.5mol/L, or 3 mol/L.
The present invention will be described in further detail with reference to examples and comparative examples.
Example 1
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of less than 0.1 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at 1000 ℃ for 2 hours to obtain chlorides containing tantalum and niobium;
s3) putting chloride containing tantalum and niobium into sodium hydroxide with the molar concentration of 2mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the recovery of tantalum and niobium.
Example 2
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of 0.1-0.3 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at 1000 ℃ for 2 hours to obtain chlorides containing tantalum and niobium;
s3) putting chloride containing tantalum and niobium into sodium hydroxide with the molar concentration of 2mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the recovery of tantalum and niobium.
Example 3
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of 0.3-1 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at 1000 ℃ for 2 hours to obtain chlorides containing tantalum and niobium;
s3) putting chloride containing tantalum and niobium into sodium hydroxide with the molar concentration of 2mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the recovery of tantalum and niobium.
Example 4
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of more than 1 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at 1000 ℃ for 2 hours to obtain chlorides containing tantalum and niobium;
s3) putting chloride containing tantalum and niobium into sodium hydroxide with the molar concentration of 2mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the recovery of tantalum and niobium.
Example 5
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of 0.3-1 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at the sintering temperature of 700 ℃ for 3 hours to obtain chlorides containing tantalum and niobium;
s3) putting the oxide containing tantalum and niobium into sodium hydroxide with the molar concentration of 2mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the recovery of tantalum and niobium.
Example 6
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of 0.3-1 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at 1200 ℃ for 2h to obtain chlorides containing tantalum and niobium;
s3) putting the oxide containing tantalum and niobium into sodium hydroxide with the molar concentration of 2mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the recovery of tantalum and niobium.
Example 7
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of 0.3-1 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at 1000 ℃ for 2 hours to obtain chlorides containing tantalum and niobium;
s3) putting chloride containing tantalum and niobium into sodium hydroxide with the molar concentration of 3mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the separation of tantalum and niobium.
Example 8
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of 0.3-1 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at 1000 ℃ for 2 hours to obtain chlorides containing tantalum and niobium;
s3) putting the oxide containing tantalum and niobium into sodium hydroxide with the molar concentration of 4mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the recovery of tantalum and niobium.
Example 9
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of 0.3-1 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at 1000 ℃ for 2 hours to obtain chlorides containing tantalum and niobium;
s3) putting chloride containing tantalum and niobium into sodium hydroxide with the molar concentration of 1mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the recovery of tantalum and niobium.
Example 10
The embodiment is a method for recovering tantalum and niobium from a tantalum-niobium alloy, which comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of 0.3-1 mm;
s2) placing the tantalum-niobium alloy powder obtained in the step S1) into a fluidized bed furnace for chlorination sintering at 1000 ℃ for 2 hours to obtain chlorides containing tantalum and niobium;
s3) putting chloride containing tantalum and niobium into sodium hydroxide with the molar concentration of 0.5mol/L for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s4) performing gravity separation to complete the recovery of tantalum and niobium.
Comparative example 1
The comparative example is a method for recovering tantalum and niobium from a tantalum-niobium alloy, and comprises the following steps:
s1) firstly, coarsely crushing the tantalum-niobium alloy by using a jaw crusher, wherein the particle size of the crushed tantalum-niobium alloy is about 2-5cm, and then, finely grinding the coarsely ground tantalum-niobium alloy by using a Raymond mill to obtain tantalum-niobium alloy powder with the particle size of 0.3-1 mm;
s2) putting the tantalum-niobium alloy powder obtained in the step S1) into an HF solution with the molar concentration of 5mol/L for leaching treatment to obtain a leaching solution containing tantalum and niobium;
s3) extracting the leaching solution containing tantalum and niobium by using an extraction technology to respectively obtain a tantalum-containing solution and a niobium-containing solution;
s4) sequentially carrying out precipitation, washing and calcination treatment on the tantalum-containing liquid to obtain tantalum oxide; and precipitating, washing and calcining the niobium-containing solution in sequence to obtain niobium oxide, and recovering tantalum and niobium.
The tantalum and niobium recovery rates in examples 1 to 10 and comparative example 1 were measured, respectively, and the results are shown in Table 1.
TABLE 1
| Serial number | Recovery/% of tantalum and niobium |
| Example 1 | 87.2 |
| Example 2 | 88.6 |
| Example 3 | 91.4 |
| Example 4 | 89.5 |
| Example 5 | 83.4 |
| Example 6 | 86.7 |
| Example 7 | 89.6 |
| Example 8 | 89.1 |
| Example 9 | 87.5 |
| Example 10 | 84.1 |
| Comparative example 1 | 87.9 |
As can be seen from the data in table 1, the method provided by the present invention can achieve the same recovery effect as the conventional recovery method using HF acid. As can be seen from the data in examples 1-10, when the particle size of the tantalum-niobium alloy powder is 0.3-1mm, the recovery efficiency is higher; when the molar concentration of the sodium hydroxide is 1-3mol/L, the recovery efficiency is higher.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (8)
1. A method for recovering tantalum and niobium from a tantalum-niobium alloy is characterized by comprising the following steps:
s1) providing tantalum-niobium alloy powder as a raw material, and then carrying out chlorination sintering treatment on the tantalum-niobium alloy powder to obtain chlorides containing tantalum and niobium;
s2) putting the chloride into alkali liquor for hydrolysis treatment to obtain hydroxide containing tantalum and niobium;
s3) performing gravity separation to complete the recovery of tantalum and niobium.
2. The method of claim 1, wherein in step S1), the tantalum-niobium alloy powder has a particle size of 0.1-1 mm, preferably 0.3-1 mm.
3. The method of claim 2, wherein the tantalum-niobium alloy powder is prepared by a method comprising: firstly, carrying out coarse crushing on the tantalum-niobium alloy by using a jaw crusher, and then carrying out fine grinding on the tantalum-niobium alloy after coarse grinding by using a Raymond mill to obtain the tantalum-niobium alloy powder.
4. The method according to any one of claims 1 to 3, wherein in the step S1), the process parameters of the chlorination sintering comprise: the chlorination sintering temperature is 500-1200 ℃, and the chlorination sintering time is 1-3 h.
5. The method as claimed in claim 4, wherein in the step S1), the process parameters of the chlorination sintering include: the chlorination sintering temperature is 600-1100 ℃, and the chlorination sintering time is 1.5-2.5 h.
6. The method of claim 4, wherein the chloridizing sintering is performed in a fluidized bed furnace.
7. The method according to any one of claims 1 to 3, wherein in step S2), the lye is sodium hydroxide and/or potassium hydroxide.
8. The method according to claim 7, wherein the molar concentration of the alkali liquor is 1-3 mol/L.
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