CN1109021A - Wet process for extracting refined tellurium from primary tellurium ore - Google Patents
Wet process for extracting refined tellurium from primary tellurium ore Download PDFInfo
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- CN1109021A CN1109021A CN 93115389 CN93115389A CN1109021A CN 1109021 A CN1109021 A CN 1109021A CN 93115389 CN93115389 CN 93115389 CN 93115389 A CN93115389 A CN 93115389A CN 1109021 A CN1109021 A CN 1109021A
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- Prior art keywords
- tellurium
- liquid
- teo
- ore
- alkali
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Abstract
The wet process for production of refined tellurium from primary tellurium ore includes such technical steps as high-temp oxidation of broken ore in hydrochlinc acid for obtain Te and Bi contained extractive liquid, reduction with SO2 to obtain coarse Te powder, neutralizing and hydrolizing Bi contaiued reductive liquid to obtain interwediate containing Bi, and chemical and electric purifying of coarse Te powder to obtain high-purity tellurium, and features low cost and high Te recovery rate of over 85%.
Description
This technology is to be raw material with the rare primary tellurium ore in the world, extracts smart tellurium by the hydrometallurgy means, and the primary ore of tellurium leaches by the salt acid oxidase, sulfurous gas sinks tellurium, reach tellurium and separate with bismuth and gangue, the coarse tellurium powder that obtains is purified through chemical purification and electrodeposition, and obtains four nine smart tellurium.
One, background of invention
Tellurium is a kind of rare and scatter element, and tradition is applied to steel smelt additive, can make the undersea cable sheath, makes vulcanization accelerator in the rubber industry, and can be used for petrochemical catalyst, the fragrant toner of glass-ceramic, fields such as sterilant and skin care medicine.Developing rapidly along with new and high technology in recent years, the Application Areas of tellurium constantly enlarges, as on the light-to-current inversion film (Se-As-Te and Zn-Cd-Te) of cadmium-tellurium solar cell, disks stored material (Pb-Te-Se), plain roll (Te-Se), electronics Refrigeration Technique (Te-Bi), television camera tube, Computer Storage material (As-Te-Si), the spaceship satellite as thermoelectric refrigeration machine and thermal electric generator, infrared controller then needs high purity tellurium, and the dissipated metal that comprises tellurium is the supportive material of contemporary high-tech art novel material.China produces tellurium per year only more than two tons at present, therefore, starts to develop and utilizes the exclusive tellurium ore resources of China to have crucial meaning undoubtedly.
Independently have the mineral deposit that commercial mining is worth because tellurium is difficult to formation, therefore the tellurium that produces all is in addition comprehensively recovery in the accessory substance from nonferrous metallurgical process in the world.Mainly extract from copper, lead anode slurry, the technology of taking is traditional technology, and it causes the rate of recovery low, the production cost height.
China's product tellurium producer is zhuzhou,hunan smeltery and Shenyang Smeltery Factory at present, all comprehensively reclaims from copper, lead anode slurry, and the technology of taking also is traditional technology.
The objective of the invention is to from unique primary tellurium ore in the world, extract and reclaim smart tellurium, (comprise China) so far in the world and also from the primary ore of tellurium, do not extract the technology and the experience of smart tellurium.Therefore, it has novelty, creativeness and practicality, reliable, simple, the easy row of this craft science, and adaptability is strong, and production cost is low, and the rate of recovery (from the raw ore to the finished product) of tellurium is more than 85%.
Two, detailed Description Of The Invention
The process flow sheet that extracts smart tellurium from the primary ore of tellurium is seen Figure of description.
The tellurium bismuth separates:
Leaching the first time of operation leaches: the tellurium bismuth primary ore that contains Te 1.2-36%, Bi 3-40% leaches after being crushed to 80 orders, and technical qualification are as follows: HCL concentration 50-200g/L, liquid-solid ratio (3-10): 1,80-95 ℃, add proper amount of oxidant, i.e. KClO
3, NaClO
3, H
2O
2, HNO
3, MnO
2, KMnO
4In one or more, agitation leach 1-3 hour, Te and Bi changed solution over to, most of gangue slag input.
Leach for the second time: a leached mud carries out secondary and leaches, technical qualification are: HCl concentration 50-200g/l, liquid: Gu=(3-10): 1,80-95 ℃, add one or more agitation leachs 1-1.5 hour in the above-mentioned oxygenant, soak after rolling liquid-solid separation, leached mud effluxes after pickling, and leach liquor returns and once leaches dosing.
Te reduces operation: with above-mentioned leach liquor SO
2Heavy tellurium, technical qualification are: 85-100 ℃,
SO
2Joining day 1.5-5 hour, reduction back liquid contained Te＜0.01g/L, and filtered while hot obtains coarse tellurium powder and reduction back liquid.
Heavy Bi operation: reduction back liquid is with the dilution that neutralizes of alkali or milk of lime, service water, and terminal point PH3-4 isolates the intermediates that contain Bi, and liquid, effluxes to 7-8 with milk of lime accent PH behind the heavy bismuth.
The chemical purification of coarse tellurium powder:
Coarse tellurium powder carries out hydrochloric acid and leaches.Technical qualification are: the beginning acid concentration 80-200g/L of hydrochloric acid, and 85-95 ℃, add in the above-mentioned oxygenant one or more, contain tellurium until solution and reach capacity.Filter residue returns leaching, and filtrate neutralizes terminal point PH5-6 with solid caustic soda or liquid caustic soda or soda ash, leave standstill filtration in 1 hour after reaching PH, filtrate is returned tellurobismuthite and is leached operation, and the thick tellurium dioxide that obtains carries out alkali and soaks, liquid-solid ratio (2-5): 1, more than 85 ℃, terminal point free alkali 15-50g/L is leached in agitation leach, best 20-35g/L, the pure sodium sulphite of processing industry purifies, and the filter residue after the filtration returns the isolating leaching operation of tellurium bismuth after washing, and filtrate is used in the industrial sulphuric acid and terminal point PH5-6.Obtain purer TeO
2Powder, filtrate effluxes.
Electrodeposition is purified:
Electrodeposition liquid making operation: with the TeO of above-mentioned gained
2Powder carries out alkali and soaks, and liquid-solid ratio is (3-5): 1, and 85-95 ℃, the processing industry solid caustic soda is to TeO
2Fully till the dissolving, add and analyze the purification of bright sulfur sodium, the electrolytic solution of gained solution preparation requires composition following (g/L): Te180-220g/L, NaoH80-100g/L, Se＜0.3, Pb＜0.003, Bi＜0.020.The technical qualification of tellurium electrodeposition are: 15-35 ℃, and Te＞130g/L, current density 20-50A/m
2, cycle 200-300 hour, the tellurium founding of separating out that obtains became the tellurium ingot.
Claims (9)
1, take full hydrometallurgy from the primary ore of tellurium, to extract smart tellurium.
2, according to claim 1, it is characterized in that leaching condition of breeze is: liquid-solid ratio (3-10): 1, HCl 50-200g/L, 80-95 ℃, oxidizer KClO
3, NaClO
3, H
2O
2, HNO
3, KMnO
4In one or more, agitation leach 1-3 hour.
3, leached mud according to claim 2 carries out the secondary leaching, it is characterized in that liquid-solid ratio (3-10): 1, and 80-95 ℃, Hce 50-200g/L, oxidizer KClO
3, NaClO
3, H
2O
2, HNO
3, KMnO
4In one or more, agitation leach 1-1.5 hour.
4, leach liquor according to claim 1 sulphur dioxide reduction tellurium is characterized in that 80-100 ℃, SO
2Joining day contains Te＜0.01g/L up to reduction back liquid.
5, coarse tellurium powder according to claim 4 carries out the oxidation leaching, it is characterized in that HCl initial concentration 80-200g/L, 85-95 ℃, adds oxygenant KClO
3, NaClO
3, H
2O
2, HNO
3In one or more, agitation leach is saturated to the solution tellurium.
6, leach liquor according to claim 5 is neutralized to PH5-6 with solid caustic soda or liquid caustic soda or soda ash and obtains thick TeO
2
7, thick TeO according to claim 6
2Carry out alkali and soak, it is characterized in that liquid-solid ratio (2-5): more than 1,85 ℃, terminal point free alkali 15-50g/L, the pure sodium sulphite of processing industry purifies.
8, the industrial H of alkali immersion liquid according to claim 7
2SO
4The PH5-6 that neutralizes, TeO that must be purer
2
9, TeO according to claim 8
2Alkali soaks liquid making, it is characterized in that adding analysis bright sulfur sodium and purifies back dosing electrodeposition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115389 CN1109021A (en) | 1993-11-22 | 1993-11-22 | Wet process for extracting refined tellurium from primary tellurium ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115389 CN1109021A (en) | 1993-11-22 | 1993-11-22 | Wet process for extracting refined tellurium from primary tellurium ore |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1109021A true CN1109021A (en) | 1995-09-27 |
Family
ID=4991014
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93115389 Pending CN1109021A (en) | 1993-11-22 | 1993-11-22 | Wet process for extracting refined tellurium from primary tellurium ore |
Country Status (1)
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|---|---|
| CN (1) | CN1109021A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009146647A1 (en) * | 2008-06-02 | 2009-12-10 | Wang Jun | Method of extracting te and bismuth oxide and recovering byproduct |
| CN102020252A (en) * | 2010-12-30 | 2011-04-20 | 成都理工大学 | Biological leaching method of low-grade tellurium mine |
| CN103849777A (en) * | 2012-11-30 | 2014-06-11 | 湖南宇腾有色金属股份有限公司 | Researches on method used for direct preparation of sodium tellurite solution from tellurium smelting waste |
| CN106277037A (en) * | 2016-08-16 | 2017-01-04 | 广东先导稀材股份有限公司 | Tellurium and the method for cadmium is reclaimed from cadmium telluride waste material |
| CN106987706A (en) * | 2017-04-13 | 2017-07-28 | 成都理工大学 | A kind of leaching method of tellurobismuthite |
| CN113699379A (en) * | 2021-08-29 | 2021-11-26 | 中南大学 | Method for recycling copper, tellurium and arsenic from black copper mud for harmless treatment |
-
1993
- 1993-11-22 CN CN 93115389 patent/CN1109021A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009146647A1 (en) * | 2008-06-02 | 2009-12-10 | Wang Jun | Method of extracting te and bismuth oxide and recovering byproduct |
| US8277772B2 (en) | 2008-06-02 | 2012-10-02 | Jun Wang | Method of extracting Te and bismuth oxide and recovering byproducts |
| CN102020252A (en) * | 2010-12-30 | 2011-04-20 | 成都理工大学 | Biological leaching method of low-grade tellurium mine |
| CN102020252B (en) * | 2010-12-30 | 2013-04-10 | 成都理工大学 | Biological leaching method of low-grade tellurium mine |
| CN103849777A (en) * | 2012-11-30 | 2014-06-11 | 湖南宇腾有色金属股份有限公司 | Researches on method used for direct preparation of sodium tellurite solution from tellurium smelting waste |
| CN106277037A (en) * | 2016-08-16 | 2017-01-04 | 广东先导稀材股份有限公司 | Tellurium and the method for cadmium is reclaimed from cadmium telluride waste material |
| CN106987706A (en) * | 2017-04-13 | 2017-07-28 | 成都理工大学 | A kind of leaching method of tellurobismuthite |
| CN113699379A (en) * | 2021-08-29 | 2021-11-26 | 中南大学 | Method for recycling copper, tellurium and arsenic from black copper mud for harmless treatment |
| CN113699379B (en) * | 2021-08-29 | 2022-10-04 | 中南大学 | Method for recycling copper, tellurium and arsenic from black copper mud for harmless treatment |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |