CN105399062A - Method for extracting tellurium dioxide from anode slime produced through tellurium electro-deposition - Google Patents
Method for extracting tellurium dioxide from anode slime produced through tellurium electro-deposition Download PDFInfo
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- CN105399062A CN105399062A CN201510858719.3A CN201510858719A CN105399062A CN 105399062 A CN105399062 A CN 105399062A CN 201510858719 A CN201510858719 A CN 201510858719A CN 105399062 A CN105399062 A CN 105399062A
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- tellurium
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- dioxide
- sodium hydroxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/004—Oxides; Hydroxides
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a method for extracting tellurium dioxide from anode slime produced through tellurium electro-deposition. The method comprises the following steps that 1, the anode slime is put into a reaction kettle, water and sodium hydroxide are added, heating and mixing are performed for two hours, and filter pressing is performed to obtain filter residues, namely the tellurium dioxide; 2, the filter residues are put into the reaction kettle, water is added, a PH value is regulated to be 1.0-1.5 by using sulfuric acid, heating is performed to reach 85 DEG C, stirring is performed for two hours, and filter pressing is performed to obtain filtrate; 3, the filtrate is added into the reaction kettle, and iron powder is added and stirred for three hours; 4, sodium hydroxide is added after the solution is clarified and transparent, the PH value is regulated to be 7.0, then sodium hydroxide with the tellurium metal content 70% is added and stirred for an hour, filter pressing is performed to obtain a sodium tellurite solution, the PH value is regulated to be 5-5.5 by using sulfuric acid, and filter pressing is performed to obtain tellurium dioxide. In the step 3, the amount of the iron powder is determined according to the tellurium content in the filtrate and meets the requirements of a reaction equation: Te<6+> + Fe<0>= Te<4+> + Fe<2+>.
Description
Technical field
The present invention relates to a kind of method extracting tellurium dioxide, particularly relate to a kind of method extracting tellurium dioxide from the anode sludge that tellurium electrodeposition produces.
Background technology
Electrodeposition method is produced containing a large amount of tellurium trioxide and a small amount of tellurium dioxide in the anode sludge produced in smart tellurium process, and these tellurium dioxide can utilize in advance.
Produce in the anode sludge produced smart tellurium process from electrodeposition method at present and extract the method for tellurium dioxide mainly: with high-concentration sulfuric acid, tellurium trioxide is changed into sulfuric acid tellurium solution, add a large amount of sodium-chlor again, under peracid height chlorization condition, add S-WAT sexavalence tellurium ion reduction is become tetravalence tellurium ion, then adjust pH value to be extracted with the form of tellurium dioxide by tellurium with alkali.Adopt the shortcoming of this method to be the low conversion rate of tetravalence tellurium, transformation efficiency generally about 60%, tellurium is stayed in slag in a large number with the form of zeroth order tellurium and sexavalence tellurium, and adopts the chlorination of peracid height, and labor condition is severe, and equipment corrosion is large, and cost is high.
Summary of the invention
The object of the present invention is to provide that a kind of transformation efficiency of tetravalence tellurium is high, cost is low, the method extracting tellurium dioxide from the anode sludge that tellurium electrodeposition produces of Environmental Safety.
In order to solve the problems of the technologies described above, the method that the present invention extracts tellurium dioxide from the anode sludge that tellurium electrodeposition produces comprises the following steps:
(1) anode sludge is put into reactor and add water and sodium hydroxide, heated and stirred press filtration in two hours, obtains filter residue and tellurium trioxide;
(2) dropped in reactor by filter residue and add water, adjust pH value to 1.0-1.5 with sulfuric acid, be heated to 85 DEG C of stirrings two hours, press filtration, obtains filtrate;
(3) filtrate is joined in reactor, add iron powder, stir three hours;
(4) after solution clear, add sodium hydroxide adjusts pH value to 7.0, then adds the sodium hydroxide of tellurium metal amount 70%, and stir one hour, press filtration, obtains sodium tellurite solution, and adjust pH value to 5-5.5 with sulfuric acid, press filtration, obtains tellurium dioxide.
Step (3), the amount of added iron powder is determined according to the tellurium content in filtrate, meet reaction equation requires: Te
6++ Fe
0=Te
4++ Fe
2+.
Step (2), described pH value is 1.5.
Step (1) gained filtrate is sodium tellurite solution, with in sulfuric acid and adjust pH value to 5-5.5, press filtration, obtains tellurium dioxide.
Method of the present invention adopts iron powder as reductive agent, and step (2) adjusts pH value to combine to 7.0 with adding sodium hydroxide after sulfuric acid tune pH value to 1.0-1.5, step (4) solution clear, sexavalence tellurium can be made to dissolve fully, improve the transformation efficiency of tetravalence tellurium, especially when pH value, to be transferred to the sodium hydroxide effect adding tellurium metal amount 70% after 7.0 better, adopts the transformation efficiency of aforesaid method tellurium dioxide of the present invention to reach 93% through test.Step (2), when described pH value is 1.5, best results, the transformation efficiency of tellurium dioxide can reach 94%.Adopt iron powder method for determination of amount in the inventive method, can improve the transformation efficiency of tellurium dioxide further, the transformation efficiency of tellurium dioxide can reach 96%.
Adopt method of the present invention, tetravalence tellurium transformation efficiency is high, and it is few that slag remains tellurium, and works under low sour condition, and Working environment have also been obtained improvement, and cost also reduced, and avoids the various defects of prior art.
Embodiment
Below method of the present invention is described in detail.
The method extracting tellurium dioxide from the anode sludge that tellurium electrodeposition produces comprises the following steps:
(1) anode sludge is put into reactor to add water and make solid-to-liquid ratio be 1:6, then add the sodium hydroxide that weight is anode sludge dry measure 5%, heated and stirred press filtration in two hours, obtains filter residue and tellurium trioxide;
(2) dropped in reactor by filter residue and add water and make solid-to-liquid ratio be 1:6, adjust pH value to 1.5 with sulfuric acid, be heated to 85 DEG C and stir two hours, press filtration, obtains filtrate;
(3) filtrate is joined in reactor, add iron powder, stir three hours;
(4) after solution clear, add sodium hydroxide adjusts pH value to 7.0, then adds the sodium hydroxide of tellurium metal amount 70%, and stir one hour, press filtration, obtains sodium tellurite solution, and adjust pH value to 5 with sulfuric acid, press filtration, obtains tellurium dioxide.
Step (3), the amount of added iron powder is determined according to the tellurium content in filtrate, meet reaction equation requires: Te
6++ Fe
0=Te
4++ Fe
2+.
Step (1) gained filtrate is sodium tellurite solution, with in sulfuric acid and adjust pH value to 5, press filtration, obtains tellurium dioxide.Like this, the transformation efficiency of tellurium dioxide can be improved further.
Adopt aforesaid method to reclaim tellurium dioxide, the transformation efficiency of tellurium dioxide can reach more than 96%.
Claims (4)
1. from the anode sludge that tellurium electrodeposition produces, extract a method for tellurium dioxide, it is characterized in that comprising the following steps:
(1) anode sludge is put into reactor and add water and sodium hydroxide, heated and stirred press filtration in two hours, obtains filter residue and tellurium trioxide;
(2) dropped in reactor by filter residue and add water, adjust pH value to 1.0-1.5 with sulfuric acid, be heated to 85 DEG C of stirrings two hours, press filtration, obtains filtrate;
(3) filtrate is joined in reactor, add iron powder, stir three hours;
(4) after solution clear, add sodium hydroxide adjusts pH value to 7.0, then adds the sodium hydroxide of tellurium metal amount 70%, and stir one hour, press filtration, obtains sodium tellurite solution, and adjust pH value to 5-5.5 with sulfuric acid, press filtration, obtains tellurium dioxide.
2. method according to claim 1, is characterized in that: step (3), and the amount of added iron powder is determined according to the tellurium content in filtrate, meet reaction equation requires: Te
6++ Fe
0=Te
4++ Fe
2+.
3. method according to claim 1, is characterized in that: step (2), and described pH value is 1.5.
4. method according to claim 1, is characterized in that: step (1) gained filtrate is sodium tellurite solution, with in sulfuric acid and adjust pH value to 5-5.5, press filtration, obtains tellurium dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510858719.3A CN105399062B (en) | 2015-12-01 | 2015-12-01 | The method that tellurium dioxide is extracted in the earth of positive pole produced from tellurium electrodeposition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510858719.3A CN105399062B (en) | 2015-12-01 | 2015-12-01 | The method that tellurium dioxide is extracted in the earth of positive pole produced from tellurium electrodeposition |
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| Publication Number | Publication Date |
|---|---|
| CN105399062A true CN105399062A (en) | 2016-03-16 |
| CN105399062B CN105399062B (en) | 2017-07-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510858719.3A Active CN105399062B (en) | 2015-12-01 | 2015-12-01 | The method that tellurium dioxide is extracted in the earth of positive pole produced from tellurium electrodeposition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107190272A (en) * | 2017-04-25 | 2017-09-22 | 中南大学 | A kind of method for preparing tellurium powder |
| CN107313063A (en) * | 2017-05-26 | 2017-11-03 | 湖南省金润碲业有限公司 | 5N high purity tellurium smelting processes |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627609A (en) * | 1985-07-02 | 1987-01-14 | Sumitomo Metal Mining Co Ltd | Method for recovering tellurium from anode slime produced by electrolysis of tellurium |
| JP2001011547A (en) * | 1999-06-24 | 2001-01-16 | Nippon Mining & Metals Co Ltd | Method for separating tellurium and lead |
| CN101259956A (en) * | 2007-12-20 | 2008-09-10 | 金川集团有限公司 | Deep impurity-removing method for crude tellurium powder |
| CN102390819A (en) * | 2011-08-10 | 2012-03-28 | 辽宁大学 | Method for preparing tellurium dioxide from tellurium slag |
| CN103112833A (en) * | 2013-02-26 | 2013-05-22 | 江西理工大学 | Method for recycling tellurium from copper anode slime |
-
2015
- 2015-12-01 CN CN201510858719.3A patent/CN105399062B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS627609A (en) * | 1985-07-02 | 1987-01-14 | Sumitomo Metal Mining Co Ltd | Method for recovering tellurium from anode slime produced by electrolysis of tellurium |
| JP2001011547A (en) * | 1999-06-24 | 2001-01-16 | Nippon Mining & Metals Co Ltd | Method for separating tellurium and lead |
| CN101259956A (en) * | 2007-12-20 | 2008-09-10 | 金川集团有限公司 | Deep impurity-removing method for crude tellurium powder |
| CN102390819A (en) * | 2011-08-10 | 2012-03-28 | 辽宁大学 | Method for preparing tellurium dioxide from tellurium slag |
| CN103112833A (en) * | 2013-02-26 | 2013-05-22 | 江西理工大学 | Method for recycling tellurium from copper anode slime |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107190272A (en) * | 2017-04-25 | 2017-09-22 | 中南大学 | A kind of method for preparing tellurium powder |
| CN107190272B (en) * | 2017-04-25 | 2019-05-17 | 中南大学 | A method of preparing tellurium powder |
| CN107313063A (en) * | 2017-05-26 | 2017-11-03 | 湖南省金润碲业有限公司 | 5N high purity tellurium smelting processes |
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| Publication number | Publication date |
|---|---|
| CN105399062B (en) | 2017-07-11 |
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