CN1686788A - Method for removing tellurium from coarse selenium - Google Patents
Method for removing tellurium from coarse selenium Download PDFInfo
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- CN1686788A CN1686788A CN 200510033967 CN200510033967A CN1686788A CN 1686788 A CN1686788 A CN 1686788A CN 200510033967 CN200510033967 CN 200510033967 CN 200510033967 A CN200510033967 A CN 200510033967A CN 1686788 A CN1686788 A CN 1686788A
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- tellurium
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Abstract
The present invention relates to a method for removing tellurium from crude selenium. Said method is characterized by that it includes the following steps: adding crude selenium into sodium hydroxide solution to make reaction, then making dilution and filtration, introducing air or oxygen gas into the filtrate to make oxidation, using dilute sulfuric acid to regulate pH of solution so as to obtain selenium powder precipitate, filtering, washing and drying so as to obtain selenium powder. The selenium percent recovery can be up to above 95%, purity of selenuim is 95-99% and tellurium content is less than or equal to 0.5%.
Description
Technical field
The present invention relates to a kind of recovery purification process of chemical element.
Background technology
Selenium is a kind of dissipated metal element, and very difficult formation independently has the mineral deposit that commercial mining is worth, so selenium all is comprehensively to retrieve from the by product of nonferrous metallurgical process.Mainly be from the anode sludge such as copper, nickel, lead and produce the fume mud of sulfuric acid or paper pulp or the body refuse of drip washing extract.Selenium, tellurium element character are close, normal association.The sulfurization roasting method is often adopted in the recovery of selenium, and selenium content is 80～95% in the thick selenium that obtains, and wherein elemental tellurium content is 5～20%.
At present, the industrial main method of removing tellurium from thick selenium is oxygen combustion-reduction method, promptly under hot conditions, aerating oxygen burning, selenium are the tin anhydride volatilization, collect through condensation, again that tin anhydride is water-soluble, regulating pH with sodium hydroxide is 4～5, and tellurium precipitates with tellurous acid, filter, it is 1～0.5 that filtrate is regulated pH with dilute sulphuric acid, feeds the reduction of sulfurous gas or S-WAT, filtration washing, oven dry obtains selenium powder.In high-temperature oxidation process, the rate of recovery of selenium, tellurium only reaches 85-92%, and in reduction process, the rate of recovery of selenium reaches 95-98%, and the rate of recovery of tellurium reaches more than 99%.In whole production, the rate of recovery of selenium reaches 85-90%, and the rate of recovery of tellurium reaches about 90%, and the rate of recovery of this method selenium is lower, the cost height.Simultaneously because the effusion of tin anhydride and emitting of a large amount of sulfurous gas are arranged, contaminate environment, etching apparatus is serious.
Summary of the invention
The rate of recovery height that the purpose of this invention is to provide a kind of selenium, pollute little, simple to operate, the method for from thick selenium, removing tellurium that cost is low.
Method of the present invention is realized by following measure: it is 20～50% sodium hydroxide solution that thick selenium is added concentration, solid-to-liquid ratio 1: 1～3,60～90 ℃ of temperature of reaction, 4～4 hours reaction times, dilute 0.5～1 times, filter filtrate bubbling air or dioxygen oxidation, 10～40 hours time, pH with the dilute sulphuric acid regulator solution is 11～13, obtain selenium powder precipitation, after filtration, washing, oven dry, obtain selenium powder.The pH that regulates filtrate with dilute sulphuric acid is 4～5, obtains the tellurium dioxide precipitation.The rate of recovery of this method selenium＞95%, the tellurium rate of recovery reaches more than 95%, and the purity of selenium is 95～99%, tellurium content≤0.5%.Fig. 1 is the schema of the inventive method.
Embodiment
Embodiment 1
To contain selenium 90%, contain the thick selenium of 100g of tellurium 7.5%, add concentration and be 40% sodium hydroxide solution, solid-to-liquid ratio 1: 2.5,90 ℃ of temperature of reaction, in 4 hours reaction times, 0.75 times of volume dilution is filtered, filtrate joins logical dioxygen oxidation in the oxidation furnaces, oxidization time 30 hours is 12 with the pH of dilute sulphuric acid regulator solution, obtains the selenium powder precipitation, after filtration, the washing, the oven dry, selenium powder 87.27g.The pH that regulates filtrate with dilute sulphuric acid is 5, obtains the tellurium dioxide precipitation.The rate of recovery of selenium, tellurium is respectively 96%, 95.5%, and selenium powder contains selenium 99%, contains tellurium 0.35%.
Embodiment 2
With embodiment 1.The thick selenium of 100g contains selenium 82.5%, contains tellurium 12.6%, and concentration of sodium hydroxide solution is 30%, solid-to-liquid ratio 1: 1.5,85 ℃ of temperature of reaction, in 5 hours reaction times, 1 times of volume dilution is filtered, the oxidation of filtrate blowing air, time is 35 hours, is 13 with the pH of dilute sulphuric acid regulator solution, obtains the selenium powder precipitation, the pH that regulates filtrate is 4.5, obtains the tellurium dioxide precipitation.Selenium powder is heavy 81.4g after washing and drying, and selenium powder contains selenium 96.4%, contains tellurium 0.43%.The rate of recovery of selenium, tellurium is respectively 95.1%, 95.8%.
Embodiment 3
With embodiment 1.The thick selenium of 100g contains selenium 80.2%, contains tellurium 17.5%, and concentration of sodium hydroxide solution is 35%, solid-to-liquid ratio 1: 2,75 ℃ of temperature of reaction, in 6 hours reaction times, 0.5 times of volume dilution is filtered, filtrate is led to dioxygen oxidation, time is 25 hours, is 13 with the pH of dilute sulphuric acid regulator solution, obtains the selenium powder precipitation, the pH that regulates filtrate is 5, obtains the tellurium dioxide precipitation.Selenium powder is heavy 80.54g after washing and drying, and selenium powder contains selenium 95.6%, contains tellurium 0.5%.The rate of recovery of selenium, tellurium is respectively 96%, 96.2%.
The selenium of the inventive method, the rate of recovery of tellurium all are higher than oxygen combustion-reducing process. Avoided high temperature oxygen The effusion of selenium dioxide and a large amount of sulfur dioxide emits contaminated environment and the equipment that causes in the change process Corrosion.
Claims (1)
1. method of removing tellurium from thick selenium is characterized in that it is 20～50% sodium hydroxide solution that thick selenium is added concentration, solid-to-liquid ratio 1: 1～3,60～90 ℃ of temperature of reaction in 4～6 hours reaction times, are diluted 0.5～1 times, filter filtrate bubbling air or dioxygen oxidation, 10～40 hours time, pH with the dilute sulphuric acid regulator solution is 11～13, obtain selenium powder precipitation, after filtration, washing, oven dry, obtain selenium powder, the pH that regulates filtrate with dilute sulphuric acid is 4～5, obtains the tellurium dioxide precipitation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100339670A CN1298619C (en) | 2005-04-07 | 2005-04-07 | Method for removing tellurium from coarse selenium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100339670A CN1298619C (en) | 2005-04-07 | 2005-04-07 | Method for removing tellurium from coarse selenium |
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| Publication Number | Publication Date |
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| CN1686788A true CN1686788A (en) | 2005-10-26 |
| CN1298619C CN1298619C (en) | 2007-02-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005100339670A Expired - Fee Related CN1298619C (en) | 2005-04-07 | 2005-04-07 | Method for removing tellurium from coarse selenium |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060275A (en) * | 2010-11-12 | 2011-05-18 | 清远先导稀有材料有限公司 | Method for treating precious metal-selenium raw material |
| CN102086029A (en) * | 2010-12-04 | 2011-06-08 | 金川集团有限公司 | Method for extracting selenium from selenium-contained material |
| CN103588181A (en) * | 2013-10-30 | 2014-02-19 | 四川鑫龙碲业科技开发有限责任公司 | Wet method for preparing low-sulfur refined selenium |
| CN108251643A (en) * | 2018-03-05 | 2018-07-06 | 云南驰宏锌锗股份有限公司 | A kind of method of trace selenium and tellurium in oxidizing process removing solution of zinc sulfate |
| CN109336068A (en) * | 2018-12-14 | 2019-02-15 | 昆明鼎邦科技股份有限公司 | The method of tellurium is removed in a kind of impure selenium slag |
| CN112479163A (en) * | 2020-12-08 | 2021-03-12 | 昆明理工大学 | Method for preparing high-purity tellurium dioxide powder by quickly removing impurity selenium |
| CN113003548A (en) * | 2021-04-02 | 2021-06-22 | 昆明鼎邦科技股份有限公司 | Method for preparing high-purity selenium by removing tellurium from crude selenium |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1096588A (en) * | 1977-05-24 | 1981-03-03 | Kohur N. Subramanian | Recovery of selenium |
| RU1820888C (en) * | 1990-11-26 | 1993-06-07 | Щелковское предприятие Агрохима | Process for profound purification of selenium |
-
2005
- 2005-04-07 CN CNB2005100339670A patent/CN1298619C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060275A (en) * | 2010-11-12 | 2011-05-18 | 清远先导稀有材料有限公司 | Method for treating precious metal-selenium raw material |
| CN102086029A (en) * | 2010-12-04 | 2011-06-08 | 金川集团有限公司 | Method for extracting selenium from selenium-contained material |
| CN103588181A (en) * | 2013-10-30 | 2014-02-19 | 四川鑫龙碲业科技开发有限责任公司 | Wet method for preparing low-sulfur refined selenium |
| CN103588181B (en) * | 2013-10-30 | 2015-04-22 | 四川鑫龙碲业科技开发有限责任公司 | Wet method for preparing low-sulfur refined selenium |
| CN108251643A (en) * | 2018-03-05 | 2018-07-06 | 云南驰宏锌锗股份有限公司 | A kind of method of trace selenium and tellurium in oxidizing process removing solution of zinc sulfate |
| CN109336068A (en) * | 2018-12-14 | 2019-02-15 | 昆明鼎邦科技股份有限公司 | The method of tellurium is removed in a kind of impure selenium slag |
| CN112479163A (en) * | 2020-12-08 | 2021-03-12 | 昆明理工大学 | Method for preparing high-purity tellurium dioxide powder by quickly removing impurity selenium |
| CN113003548A (en) * | 2021-04-02 | 2021-06-22 | 昆明鼎邦科技股份有限公司 | Method for preparing high-purity selenium by removing tellurium from crude selenium |
| CN113003548B (en) * | 2021-04-02 | 2022-11-11 | 昆明鼎邦科技股份有限公司 | Method for preparing high-purity selenium by removing tellurium from crude selenium |
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| Publication number | Publication date |
|---|---|
| CN1298619C (en) | 2007-02-07 |
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Granted publication date: 20070207 Termination date: 20140407 |