CN105441970A - New method for removing impurities in tellurium electrolyte - Google Patents
New method for removing impurities in tellurium electrolyte Download PDFInfo
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- CN105441970A CN105441970A CN201510797486.0A CN201510797486A CN105441970A CN 105441970 A CN105441970 A CN 105441970A CN 201510797486 A CN201510797486 A CN 201510797486A CN 105441970 A CN105441970 A CN 105441970A
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- tellurium
- sodium
- selenium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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Abstract
The invention relates to the technical field of metallurgy and discloses a new method for removing impurities in tellurium electrolyte. According to the method, the wet process for preparing qualified tellurium electrolyte by removing lead through purification, depositing tellurium through hydrolysis and dissolving tellurium dioxide through sodium hydroxide is adopted; after the lead is removed through sodium sulfide, a solution is subjected to neutralizing treatment through hydrochloric acid, and the pH is adjusted to 5-5.5; sodium tellurite (Na2TeO3) and sodium selenite (Na2SeO3) are hydrolyzed to generate tellurium dioxide (TeO2) and selenium dioxide (SeO2) respectively; the selenium dioxide has good solubility and can be dissolved into water and inorganic acid easily, and the tellurium dioxide has poor solubility within the pH range of 5-5.5; selenium and the tellurium are separated preliminarily; finally, tellurium dioxide is subjected to alkali dissolution and filtration to obtain the qualified tellurium electrolyte. By means of the method, purification and impurity removal of the tellurium electrolyte with high lead and selenium contents are effectively realized; the technological process is simple, the quantity and varieties of adopted raw materials are fewer, and the production cost is effectively lowered; energy consumption is less, and the recovery rate of the tellurium is high.
Description
Technical field
The present invention relates to metallurgical technology field, effectively can reduce the method for a kind of tellurium electrolytic solution removal of impurities of lead, selenium content in tellurium electrolytic solution specifically.
Background technology
Tellurium is a kind of rare metal, is widely used in the industrial circles such as metallurgy, instrument, electronics, chemical industry, glass.Tellurium reclaims primarily of in copper anode mud, and technique used is alkali leaching or acidleach mainly, and leach liquor, after a series of purification, the dedoping step such as purification, neutralization, is prepared into tellurium electrolytic solution, carries out electrowinning with insoluble anode, finally obtains product essence tellurium.This technique is comparatively ripe, stable, and quality product is better.But in the tellurium electrolytic solution of situ production sometimes, impurity element is higher, cannot meet need of production, general treatment process be electrolytic solution after neutralization with in and slag be mixed in proportion laggard row relax, this method long flow path, produce load high, the tellurium rate of recovery is lower.Therefore need the tellurium electrolytic solution treatment process developing a kind of simple possible, can effectively purify tellurium electrolytic solution.
Summary of the invention
The object of this invention is to provide the method for a kind of tellurium electrolytic solution removal of impurities, high with the technical process length, the production load that solve the tellurium electrolytic solution removal of impurities plumbous in prior art, selenium content is higher, the problem that the tellurium rate of recovery is low.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A method for tellurium electrolytic solution removal of impurities, the lead in plumbous, that selenium content is higher tellurium electrolytic solution, selenium are removed by the wet processing that present method adopts the heavy tellurium-sodium hydroxide of purification deleading-hydrolysis to dissolve, and make it comprise the following steps:
A, purification deleading
The sodium sulphite of quality 1.1 times plumbous in solution is added in plumbous, that selenium content is higher tellurium electrolytic solution, 4h is left standstill at normal temperatures after stirring reaction 1h, after solid-liquid layering, supernatant liquid is inclined to, lower sediment carries out filtration makes solid-liquid separation, and lead is deposited in filter residue with the form of lead sulfate, and tellurium and selenium exist in filtrate with the form of sodium tellurite and Sodium Selenite respectively, reclaim filter residue, collect filtrate;
B, the heavy tellurium of hydrolysis
Concentrated hydrochloric acid is added in the filtrate prepared by step a, regulate pH to 4.5 ~ 5, filtrate be heated to 75 ~ 80 DEG C and constantly stir, soaking time 1h, period supplements hydrochloric acid in right amount, makes the pH of filtrate remain on 5 ~ 5.5, standing and reacting liquid at the end of reaction, Sodium Selenite hydrolysis generates tin anhydride and is dissolved in water and mineral acid, and sodium tellurite hydrolysis generates tin anhydride throw out; Question response liquid filters when being cooled to 50 ~ 60 DEG C while hot, filter residue is washed to pH and carries out drying after 6 ~ 7, obtained tellurium dioxide powder;
The molten liquid making of c, alkali
Tellurium dioxide powder obtained by step b is added in sodium hydroxide solution, the mol ratio of tellurium dioxide powder and sodium hydroxide is 1:2.5, and solid-to-liquid ratio is 1:4, is heated to 60 DEG C of reaction 1.5h, after question response completes, electrolytic solution is filtered, obtain qualified tellurium electrolytic solution.
Extend time of repose in the present invention in step a and can increase level of response, improve deposition rate plumbous in solution, can improve again the efficiency of filtration, the chemical reaction that this step occurs is as follows:
Na
2PbO
2+Na
2S+2H
2O=PbS↓+4NaOH
In the present invention, in step b, the conventional sulfuric acid that uses carries out neutralizing heavy tellurium, and the sodium sulfate solubleness of generation is lower, when temperature is low, pipeline latch up phenomenon easily occurs, concentrated hydrochloric acid is now used to replace, because sodium-chlor solubleness is high, can avoid the generation salting out blocking pipe, the chemical reaction occurred in solution is as follows:
Na
2TeO
3+2HCl=TeO
2↓+2NaCl+H
2O
Na
2SeO
3+2HCl=H
2SeO
3+2NaCl
The chemical reaction that in the present invention, step c occurs is as follows:
TeO
2+2NaOH=Na
2TeO
3+H
2O
The present invention is directed to the defect of prior art, adopt the heavy tellurium of purification deleading-hydrolysis-sodium hydroxide dissolving tellurium dioxide to prepare the wet processing of qualified tellurium electrolytic solution, after utilizing sodium sulphite deleading, use hydrochloric acid to solution neutralizing treatment, regulate pH to 5 ~ 5.5, sodium tellurite (Na
2teO
3) and Sodium Selenite (Na
2seO
3) be hydrolyzed generation tellurium dioxide (TeO respectively
2) and tin anhydride (SeO
2), tin anhydride has good solubility, soluble in water and mineral acid, the solvability extreme difference of tellurium dioxide within the scope of this pH, selenium, tellurium initial gross separation, finally by molten for tellurium dioxide alkali, filtration, obtains qualified tellurium electrolytic solution.
Method of the present invention have effectively achieved purification in the higher tellurium electrolytic solution of lead, selenium content, removal of impurities, and technical process is simple and direct, and the amount that starting material use, kind are less, effectively reduce production cost; Energy consumption is less, and the rate of recovery of tellurium is high.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Component analysis and the content of present method Raw tellurium electrolytic solution are as shown in table 1:
Table 1
A tellurium electrolyte purification method for high leaded, selenium, it comprises the following steps:
A, purification deleading
The sodium sulphite of quality 1.1 times plumbous in solution is added in plumbous, that selenium content is higher tellurium electrolytic solution, 4h is left standstill at normal temperatures after stirring reaction 1h, reacted solution is filtered and makes solid-liquid separation, lead is deposited in filter residue with the form of lead sulfate, tellurium and selenium exist in filtrate with the form of sodium tellurite and Sodium Selenite respectively, reclaim filter residue, collect filtrate;
Component and the content of filtrate are as shown in table 2:
Table 2
As can be seen from Table 2, after former tellurium electrolyte purification deleading, the tellurium concentration in solution is 143.22g/L, and the yield of tellurium is 97.4%.
B, the heavy tellurium of hydrolysis
Concentrated hydrochloric acid is added in the filtrate prepared by step a, regulate pH to 4.5 ~ 5 of filtrate, filtrate be heated to 75 ~ 80 DEG C and constantly stir, soaking time 1h, period supplements hydrochloric acid in right amount, makes the pH of filtrate remain on 5 ~ 5.5, standing and reacting liquid at the end of reaction, Sodium Selenite hydrolysis generates tin anhydride and is dissolved in water and mineral acid, and sodium tellurite hydrolysis generates tin anhydride throw out; Question response liquid filters when being cooled to 50 ~ 60 DEG C while hot, filter residue is washed to pH and carries out drying after 6 ~ 7, obtained tellurium dioxide powder;
Component and the content of the rear liquid of hydrolysis are as shown in table 3:
Table 3
Component and the mass percentage content of tellurium dioxide powder are as shown in table 4:
Table 4
As can be seen from table 3, table 4, the content remaining tellurium after hydrolysis in liquid is 0.013g/L, and the yield of tellurium is more than 99.8%.
The molten liquid making of c, alkali
Tellurium dioxide powder obtained by step b is added in sodium hydroxide solution, the mol ratio of tellurium dioxide powder and sodium hydroxide is 1:2.5, and solid-to-liquid ratio is 1:4, is heated to 60 DEG C of reaction 1.5h, after question response completes, electrolytic solution is filtered, obtain qualified tellurium electrolytic solution.
Tellurium electrolytic solution component and content as shown in table 5:
Table 5
As can be seen from the above table, in final obtained tellurium electrolytic solution, the content of tellurium is 267.5g/L, and selenium, tellurium content all meet electrodeposition requirement, and the yield of tellurium can reach more than 97%, and total direct yield of tellurium can reach more than 94%.
Method of the present invention have effectively achieved purification in the higher tellurium electrolytic solution of lead, selenium content, removal of impurities, and technical process is simple and direct, and the amount that starting material use, kind are less, effectively reduce production cost; Energy consumption is less, and the rate of recovery of tellurium is high.
Claims (1)
1. a method for tellurium electrolytic solution removal of impurities, is characterized in that: the lead in plumbous, that selenium content is higher tellurium electrolytic solution, selenium are removed by the wet processing that present method adopts the heavy tellurium-sodium hydroxide of purification deleading-hydrolysis to dissolve, and make it comprise the following steps:
A, purification deleading
The sodium sulphite of quality 1.1 times plumbous in solution is added in plumbous, that selenium content is higher tellurium electrolytic solution, 4h is left standstill at normal temperatures after stirring reaction 1h, after solid-liquid layering, supernatant liquid is inclined to, lower sediment carries out filtration makes solid-liquid separation, and lead is deposited in filter residue with the form of lead sulfate, and tellurium and selenium exist in filtrate with the form of sodium tellurite and Sodium Selenite respectively, reclaim filter residue, collect filtrate;
B, the heavy tellurium of hydrolysis
Concentrated hydrochloric acid is added in the filtrate prepared by step a, regulate pH to 4.5 ~ 5 of filtrate, filtrate be heated to 75 ~ 80 DEG C and constantly stir, soaking time 1h, period supplements hydrochloric acid in right amount, makes the pH of filtrate remain on 5 ~ 5.5, standing and reacting liquid at the end of reaction, Sodium Selenite hydrolysis generates tin anhydride and is dissolved in water and mineral acid, and sodium tellurite hydrolysis generates tin anhydride throw out; Question response liquid filters when being cooled to 50 ~ 60 DEG C while hot, filter residue is washed to pH and carries out drying after 6 ~ 7, obtained tellurium dioxide powder;
The molten liquid making of c, alkali
Tellurium dioxide powder obtained by step b is added in sodium hydroxide solution, the mol ratio of tellurium dioxide powder and sodium hydroxide is 1:2.5, and solid-to-liquid ratio is 1:4, is heated to 60 DEG C of reaction 1.5h, after question response completes, electrolytic solution is filtered, obtain qualified tellurium electrolytic solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105862059A (en) * | 2016-05-12 | 2016-08-17 | 中南大学 | Method for recovering tellurium through cyclone electrolysis of solution containing tellurium |
| CN108315569A (en) * | 2018-03-05 | 2018-07-24 | 云南驰宏锌锗股份有限公司 | A method of trace selenium and tellurium in absorption, deposition removal solution of zinc sulfate |
| CN113528850A (en) * | 2021-07-26 | 2021-10-22 | 中南大学 | Method for purifying gold by controlling potential |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105862059A (en) * | 2016-05-12 | 2016-08-17 | 中南大学 | Method for recovering tellurium through cyclone electrolysis of solution containing tellurium |
| CN108315569A (en) * | 2018-03-05 | 2018-07-24 | 云南驰宏锌锗股份有限公司 | A method of trace selenium and tellurium in absorption, deposition removal solution of zinc sulfate |
| CN108315569B (en) * | 2018-03-05 | 2020-03-31 | 云南驰宏锌锗股份有限公司 | Method for removing trace selenium and tellurium in zinc sulfate solution through adsorption and precipitation |
| CN113528850A (en) * | 2021-07-26 | 2021-10-22 | 中南大学 | Method for purifying gold by controlling potential |
| CN113528850B (en) * | 2021-07-26 | 2022-06-07 | 中南大学 | Method for purifying gold by controlling potential |
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Application publication date: 20160330 |