CN113307233A - Method for purifying and selenium-removing tellurium-containing metal material - Google Patents
Method for purifying and selenium-removing tellurium-containing metal material Download PDFInfo
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- CN113307233A CN113307233A CN202110592833.1A CN202110592833A CN113307233A CN 113307233 A CN113307233 A CN 113307233A CN 202110592833 A CN202110592833 A CN 202110592833A CN 113307233 A CN113307233 A CN 113307233A
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Abstract
The invention discloses a method for purifying and selenium-removing tellurium-containing metal materials, which comprises the following steps: (1) leaching of tellurium-containing material: adding tellurium-containing metal materials into the concentrated nitric acid solution step by step at normal temperature in batches for reacting for 1-2 h to obtain tellurium dioxide; (2) leaching tellurium dioxide: adding tellurium dioxide into the pure acidic solution step by step in batches to obtain a tellurium-containing solution; (3) leaching and selenium removal of a tellurium-containing solution: adding a selenium removal reagent into the tellurium-containing solution step by step in batches to obtain a selenium-free or trace selenium-free tellurium-containing solution; the dosage of the adopted selenium removal reagent is 30-45 g/L, the reaction lasts for 1-3 h, and the selenium removal rate can reach 99.8% or above. (4) Reduction of the liquid after selenium removal: the tellurium-containing solution without selenium or trace selenium is reduced by sodium sulfite to obtain high-purity tellurium with selenium content not more than 0.00035 percent and main metal tellurium content not less than 99.997 percent. The method for purifying and removing selenium from the tellurium-containing metal material has the advantages of easily controlled process, simple operation and strong process adaptability, can ensure that the removal rate of selenium in the crude tellurium powder reaches more than 99.8 percent, can recover the selenium from the selenium removal slag, and realizes the purposes of comprehensively recovering valuable metals and improving the purity of pure tellurium products.
Description
Technical Field
The invention relates to the field of nonferrous metallurgy, in particular to a method for purifying and selenium-removing tellurium-containing metal materials.
Background
At present, the methods for purifying and removing selenium from tellurium-containing materials at home and abroad mainly comprise a sodium sulfite method, an electrolysis method and a hydrogenation method. Wherein the sodium sulfite method is mainly used for purifying and selenium removing of reduced tellurium with higher selenium content; the electrolytic method is used as a traditional purification process, although partial selenium can be removed, the purity of the prepared electrolytic tellurium is usually 99.99 percent, and the purity is difficult to further improve; the hydrogenation method is mainly used for further removing trace selenium in high-purity tellurium after vacuum distillation or zone melting. The patent of CN201210286217.4 discloses a process for preparing high-purity tellurium from tellurium-containing materials by a ternary precipitation method, which comprises water chlorination leaching, neutralization precipitation of tellurium ions, oxidation precipitation and reduction precipitation, and realizes removal of impurities such as selenium by matching with a vulcanization impurity removal process. 200710303633.X discloses a method for removing selenium impurity from solid tellurium powder, which adopts the technical method that crude tellurium powder is dissolved in sodium sulfite solution with the weight percentage concentration of 5-40%, and after reaction is carried out for 0.5-5 hours at 80-95 ℃, tellurium powder with the tellurium content of more than 96% is obtained by filtering and washing, and the removal rate of selenium can be more than 90.4%. The patent of CN101844750A discloses a method for preparing high-purity tellurium from tellurium-containing materials, which comprises the processes of oxidation acid leaching for copper removal, step reduction of formic acid or sodium hydrosulfite and the like, hydrogen treatment and the like. There is also reported a method for removing selenium by calcining tellurium dioxide as a raw material. The adopted process technical method has long process flow, and particularly has poor process adaptability when processing raw materials with large selenium content fluctuation, thereby causing large product quality fluctuation. Therefore, it is very important to develop a method for purifying and selenium-removing tellurium-containing metal materials.
Disclosure of Invention
In order to overcome the defects of the technology, the invention aims to provide a method for purifying and selenium-removing tellurium-containing metal materials, which has the advantages of easy control, simple operation and strong technological adaptability, and can greatly reduce the influence of selenium on tellurium products and reduce the quality fluctuation of pure tellurium products.
The purpose of the invention is realized by the following technical scheme:
a method for purifying and selenium-removing tellurium-containing metal materials is characterized by comprising the following steps:
(1) adding the tellurium-containing metal materials into the concentrated nitric acid solution step by step in batches for reacting for 1-2 h to obtain pure tellurium dioxide crystals;
(2) adding the pure tellurium dioxide crystals into the pure acidic solution step by step in batches to obtain a tellurium-containing solution;
(3) adding a selenium removal reagent into the tellurium-containing solution step by step in batches to obtain a selenium-free or trace selenium-containing solution, and reducing the selenium-free or trace selenium-containing solution by using sodium sulfite to obtain high-purity tellurium.
The acidic solution is preferably hydrochloric acid.
The tellurium-containing metal material in the step (1) can be crude tellurium, refined tellurium or other materials containing selenium and tellurium.
The mass concentration of the nitric acid added in the step (1) is 65-68%, and the dosage is 0.95-1.0 time of the theoretical calculation amount.
The mass concentration of the hydrochloric acid added in the step (2) is 36-38%, and the dosage is 1.2-1.4 times of the theoretical calculation amount.
The dosage of the selenium removal reagent added in the step (3) is 30-45 g/L, the reaction lasts for 1-3 h, and the selenium removal rate can reach 99.8% or above.
And (4) reducing the tellurium-containing solution without selenium or trace selenium in the step (3) by using sodium sulfite to obtain high-purity tellurium with selenium content not more than 0.00035% and main metal tellurium content not less than 99.997%.
The invention has the beneficial technical effects that:
the method for purifying and removing selenium from the tellurium-containing metal material has the advantages of easily controlled process, simple operation and strong process adaptability, can ensure that the removal rate of selenium in the crude tellurium powder reaches more than 99.8 percent, can recover the selenium from the selenium removal slag, realizes the comprehensive recovery of valuable metals, and achieves the purposes of reducing the influence of the selenium on tellurium products and improving the purity of pure tellurium products.
The whole process only introduces nitric acid, hydrochloric acid and a selenium removal reagent, does not contain other reagents, has high product purity, short process flow and low production cost, and effectively solves the problems of long process, large consumption of acid and alkali reagents and high impurity content, particularly selenium content, in the preparation of high-purity tellurium by using the existing tellurium-containing metal material.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
Referring to fig. 1, the method for purifying and selenium-removing tellurium-containing metal material of the invention comprises the following steps:
(1) leaching of tellurium-containing material: and (3) adding the tellurium-containing metal materials into the concentrated nitric acid solution step by step and in batches at normal temperature to react for 1-2 h to obtain tellurium dioxide. The mass concentration of the nitric acid is 65-68%, and the dosage of the nitric acid is 0.95-1.0 time of the theoretical calculation amount.
(2) Leaching tellurium dioxide: adding pure tellurium dioxide into the pure acidic solution step by step in batches to obtain a tellurium-containing solution; the mass concentration of the hydrochloric acid is 36-38%, and the dosage of the hydrochloric acid is 1.2-1.4 times of the theoretical calculation amount.
(3) Leaching and selenium removal of a tellurium-containing solution: adding a selenium removal reagent into the tellurium-containing solution step by step in batches to obtain a selenium-free or trace selenium-free tellurium-containing solution; the dosage of the adopted selenium removal reagent is 30-45 g/L, the reaction lasts for 1-3 h, and the selenium removal rate can reach 99.8% or above.
(4) Reduction of the liquid after selenium removal: the tellurium-containing solution without selenium or trace selenium is reduced by sodium sulfite to obtain high-purity tellurium with selenium content not more than 0.00035% and main metal tellurium content not less than 99.997%.
Example 1
The crude tellurium is leached by 65% nitric acid for 1h, the amount of the nitric acid is 0.95 times of the theoretical calculation amount, and the chemical components of the trial-produced tellurium dioxide are shown in Table 1.
TABLE 1 tellurium dioxide chemical composition (%)
Leaching tellurium dioxide with 36% hydrochloric acid for 1h, wherein the dosage is 1.2 times of the theoretical calculation amount, adding 30g/L of a selenium removal reagent after complete dissolution, and reacting for 1h, wherein the chemical compositions of the solution before and after selenium removal are shown in Table 2.
TABLE 2 chemical composition of solution before and after selenium removal (g/L)
The chemical components of the high-purity tellurium obtained by reducing the selenium-removed liquid with sodium sulfite are shown in Table 3.
TABLE 3 high purity tellurium chemical composition (%)
Example 2
The crude tellurium is leached by 65% nitric acid for 1.5h, the amount of the nitric acid is 0.98 times of the theoretical calculated amount, and the chemical components of the trial-produced tellurium dioxide are shown in Table 4.
TABLE 4 tellurium dioxide chemical composition (%)
Leaching tellurium dioxide with 36% hydrochloric acid for 1h, wherein the dosage is 1.3 times of the theoretical calculation amount, adding 40g/L of a selenium removal reagent after complete dissolution, and reacting for 1h, wherein the chemical compositions of the solution before and after selenium removal are shown in Table 5.
TABLE 5 chemical composition of solution before and after selenium removal (g/L)
The chemical components of the high-purity tellurium obtained by reducing the selenium-removed liquid with sodium sulfite are shown in Table 6.
TABLE 6 high purity tellurium chemical composition (%)
Example 3
The crude tellurium is leached by 68 percent nitric acid for 2 hours, the dosage of the nitric acid is 1.0 time of the theoretical calculation amount, and the chemical components of the trial-produced tellurium dioxide are shown in a table 7.
TABLE 7 tellurium dioxide chemical composition (%)
Leaching tellurium dioxide with 38% hydrochloric acid for 1h, wherein the dosage is 1.4 times of the theoretical calculation amount, adding 45g/L of a selenium removal reagent after complete dissolution, and reacting for 1h, wherein the chemical compositions of the solution before and after selenium removal are shown in Table 8.
TABLE 8 chemical composition of solution before and after selenium removal (g/L)
The chemical components of the high-purity tellurium obtained by reducing the selenium-removed liquid with sodium sulfite are shown in Table 9.
TABLE 9 high purity tellurium chemical composition (%)
Claims (6)
1. A method for purifying and selenium-removing tellurium-containing metal materials is characterized by comprising the following steps:
(1) adding the tellurium-containing metal materials into the concentrated nitric acid solution step by step in batches for reacting for 1-2 h to obtain pure tellurium dioxide crystals;
(2) adding the pure tellurium dioxide crystals into the pure acidic solution step by step in batches to obtain a tellurium-containing solution;
(3) adding a selenium removal reagent into the tellurium-containing solution step by step in batches to obtain a selenium-free or trace selenium-containing solution, and reducing the selenium-free or trace selenium-containing solution by using sodium sulfite to obtain high-purity tellurium.
2. The method for purifying and diselenating a tellurium-containing metal material as claimed in claim 1, wherein the tellurium-containing metal material in the step (1) is crude tellurium, or refined tellurium, or other selenium-tellurium-containing material.
3. The method for purifying and removing selenium from tellurium-containing metal materials as claimed in claim 1, wherein the mass concentration of the nitric acid adopted in the step (1) is 65% -68%, and the amount is 0.95-1.0 times of the theoretical calculation amount.
4. The method for purifying and selenium-removing tellurium-containing metal material as claimed in claim 1, wherein the hydrochloric acid used in the step (2) has a mass concentration of 36% to 38% and an amount of 1.2 to 1.4 times of the theoretical amount.
5. The method for purifying and removing selenium from tellurium-containing metal materials as claimed in claim 1, wherein the dosage of the selenium removing reagent used in the step (3) is 30 g/L-45 g/L, the reaction time is 1-3 h, and the selenium removing rate can reach 99.8% or more.
6. The method of claim 1, wherein the tellurium-containing solution without selenium or trace selenium in step (3) is reduced with sodium sulfite to obtain high-purity tellurium with selenium content of not more than 0.00035% and main metal tellurium content of not less than 99.997%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11147703A (en) * | 1997-11-12 | 1999-06-02 | Nippon Telegr & Teleph Corp <Ntt> | Production of high-purity tellurilim dioxide |
| CN101259956A (en) * | 2007-12-20 | 2008-09-10 | 金川集团有限公司 | Deep impurity-removing method for crude tellurium powder |
| CN101844750A (en) * | 2010-06-04 | 2010-09-29 | 中南大学 | Method for preparing high-purity tellurium by material containing tellurium |
| CN102153054A (en) * | 2011-05-03 | 2011-08-17 | 嘉兴市达泽光电技术有限公司 | Preparation method of high purity tellurium |
| CN109704295A (en) * | 2019-03-14 | 2019-05-03 | 阳谷祥光铜业有限公司 | A method of producing smart tellurium |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11147703A (en) * | 1997-11-12 | 1999-06-02 | Nippon Telegr & Teleph Corp <Ntt> | Production of high-purity tellurilim dioxide |
| CN101259956A (en) * | 2007-12-20 | 2008-09-10 | 金川集团有限公司 | Deep impurity-removing method for crude tellurium powder |
| CN101844750A (en) * | 2010-06-04 | 2010-09-29 | 中南大学 | Method for preparing high-purity tellurium by material containing tellurium |
| CN102153054A (en) * | 2011-05-03 | 2011-08-17 | 嘉兴市达泽光电技术有限公司 | Preparation method of high purity tellurium |
| CN109704295A (en) * | 2019-03-14 | 2019-05-03 | 阳谷祥光铜业有限公司 | A method of producing smart tellurium |
Non-Patent Citations (3)
| Title |
|---|
| ZHAO-MING SUN等: "Preparation of high pure tellurium from raw tellurium containing Cu and Se by chemical method", 《TRANSACTIONS OF NONFERROUS METALS SOCIETY OF CHINA》, vol. 21, no. 3, 31 March 2011 (2011-03-31), pages 665 - 672 * |
| 肖鹏等: "稀散金属硒、碲回收工艺现状与展望", 《金属矿山》, no. 04, 30 April 2020 (2020-04-30), pages 52 - 60 * |
| 韩汉民: "高纯碲的制备", 《精细化工》, no. 6, 30 June 1997 (1997-06-30), pages 55 * |
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Application publication date: 20210827 |