CN103911512A - Method for removing arsenic and antimony from zinc smelting leaching solution - Google Patents
Method for removing arsenic and antimony from zinc smelting leaching solution Download PDFInfo
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- CN103911512A CN103911512A CN201410174729.0A CN201410174729A CN103911512A CN 103911512 A CN103911512 A CN 103911512A CN 201410174729 A CN201410174729 A CN 201410174729A CN 103911512 A CN103911512 A CN 103911512A
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Abstract
A method for removing arsenic and antimony from zinc smelting leaching solution, relating to zinc smeltingIn the course of preparation, the solution is purified to remove arsenic and antimony. The method is characterized in that zinc smelting low-acid leachate is used as a raw material in the treatment process, and valuable components such as zinc, indium, iron and the like are comprehensively recovered by adopting the processes of pre-reduction, neutralization and indium precipitation and hematite arsenic removal and antimony purification. The low-acid leachate adopts zinc concentrate, zinc sulfite, sulfur dioxide and the like as reducing agents to convert high-valence iron into low-valence iron, and the high-valence iron (Fe) in the solution after reduction3+) The content is lower than 2g/L, lime, limestone, secondary zinc oxide, calcine and zinc oxide are adopted to perform two-stage neutralization and adjustment on the pH value of the solution after reduction to 4.0-5.4, so that indium is precipitated and enriched, and the solution after indium precipitation is subjected to arsenic and antimony removal by a hematite method, so that the aim of efficiently and cleanly purifying the solution is achieved. The method has the advantages of high indium metal recovery rate, high arsenic and antimony removal rate, small slag amount, stable performance and environmental friendliness.
Description
Technical field
The invention belongs to zinc metallurgical technology field, relate to a kind of method of smelting arsenic removal leach liquor, antimony from zinc.
Background technology
The metallurgical main raw material of zinc is the zinc sulfide concentrates that zink sulphide and high-iron sphalerite ore dressing obtain, and a small amount of is zincite, smithsonite and lapis calaminaris etc., and zinc metallurgical technology is divided into two large classes: pyrogenic process and Zinc hydrometallurgy process.At present, the more than 80% zinc metallurgy method in the world is zinc hydrometallurgy.Zinc hydrometallurgy is mainly divided three classes: the first kind is the conventional Zinc hydrometallurgy process flow process leaching, and Equations of The Second Kind is that hot acid leaches zinc metallurgy flow process, and the 3rd class is pressure leaching flowsheet of wet zinc smelting.Hot acid zinc hydrometallurgy main flow is zinc sulfide concentrates " roasting-leaching-purification-electrodeposition ", it is on the basis of conventional lixiviation process, to carry out the high Ore Leaching of high temperature that hot acid leaches flow process, make zinc soak impurity (as iron, cobalt, arsenic, antimony) in slag etc. and also enter leach liquor, in zinc metallurgical process, must carry out purification and impurity removal to obtain the zinc of high-quality and realize comprehensive utilization of resources.In Zinc Hydrometallurgy Process, not only in material, contain the impurity elements such as arsenic, also can add the element such as arsenic, antimony in various degree in smelting process, the technique of arsenic removal in Zinc Hydrometallurgy Process, antimony is mainly to adopt siderotil method, neutralisation, sulfurization-precipitation method etc. at present.
Siderotil method and neutralisation process that the quantity of slag producing is large, valuable element content is low, complicated component, is unfavorable for the comprehensive utilization of valuable metal; At present industrially all comprehensively reclaiming, store up processing, thereby environment is affected greatly but adopt, is also a kind of wasting of resources.Although sulfurization-precipitation method has stronger avidity to part ion, can effectively arsenic, antimony etc. are carried out to sedimentation, improve valuable element content in slag, reclaim economic base is provided for it is comprehensive; But vulcanizing agent very easily generates the virose hydrogen sulfide of tool in acidic solution, causes environmental pollution, improve labour intensity.
Summary of the invention
The object of the invention is the technical deficiency existing in order to overcome existing arsenic removal, antimony method in zinc metallurgical process, provide that a kind of equipment and process is simple, high, the eco-friendly arsenic removal of comprehensive utilization of resources rate, antimony method.
The present invention smelts low acid leaching liquor as raw material take zinc, adopts prereduction---neutralization heavy indium---hematite process arsenic removal, antimony purification process.Be that its process is to reduce under the condition that low acid leaching liquor is existed at reductive agent, make high price iron change iron at a low price into; Adopt again neutralizing agent to neutralize and regulate pH value, reclaim the indium in leach liquor simultaneously; Reach by hematite process arsenic removal, antimony the object that purifies low acid leaching liquor again.The concrete technical scheme of the present invention is as follows.
A method of smelting arsenic removal leach liquor, antimony from zinc, comprises the following steps:
(1) smelt low acid leaching liquor as raw material take zinc, under the condition existing, reduce at reductive agent, make high price iron ion change iron ion at a low price into, the zinc after being reduced is smelted leach liquor;
(2) zinc after reduction being smelted to leach liquor adopts neutralizing agent to carry out one section of neutralization adjusting pH value, liquid after solid-liquid separation obtains one section of neutralization;
(3) adopt neutralizing agent to carry out two sections of neutralizations liquid after one section of neutralization, make the indium precipitate and separate in leach liquor simultaneously, obtain liquid and indium slag after heavy indium;
(4) will sink after indium liquid by hematite process arsenic removal, antimony, obtain leach liquor after arsenic removal, antimony and containing arsenic antimony scum;
(5) indium slag of step (3) is extracted to indium, the leach liquor after arsenic removal, the antimony of step (4) is returned to neutral Leaching Zinc smelting procedure.
Further, described zinc is smelted low acid leaching liquor main component and is: zinc: 60～120g/L, iron: 10～40g/L, indium: 0.05～0.5g/L, arsenic: 0.1～2.0g/L, copper: 0.5～5g/L, antimony: 0.01～2g/L.
Further, reductive agent in step (1) is one or more that are selected from zinc ore concentrate, zinc sulfite, sulfurous gas, its consumption is 1.0～1.5 times of theoretical amount, under 80～100 ℃ of conditions, reduce 1～5h, make the zinc after reduction smelt the high price iron (Fe in leach liquor
3+) content is lower than 2g/L.
Further, one section of neutralizing agent described in step (2) is one or more that are selected from lime, Wingdale, secondary zinc oxide, calcining, zinc oxide, neutral temperature be 40～90 ℃, in and time 20～120min, more than neutralization end of a period sulfuric acid concentration 5g/L.
Further, two sections of neutralizing agents described in step (3) are one or more that are selected from calcining, secondary zinc oxide, zinc oxide, neutral temperature be under 80～100 ℃ of conditions, carry out in and 0.5～2h, neutralization end of a period pH value is 4.0～5.4, makes indium precipitate enrichment.
Further, the temperature of the hematite process arsenic removal described in step (4), antimony is 120～180 ℃, and oxygen partial pressure is 0.1～0.5MPa, and stagnation pressure is 1.1～1.7MPa, and arsenic removal, antimony time are 1～4h.
In the inventive method, in and operation adopt the residual acid in lime, Wingdale neutralization solution, waste residue physical and chemical performance cheap, that produce is stable, environmentally friendly.Adopt calcining, secondary zinc oxide, zinc oxide etc. as reductive agent, can effectively utilize the residual acid of leach liquor, reduce the acid consumption of technique, reduce production costs, and produce without solid waste.
In the inventive method, adopt in the indium slag that two sections of neutralization precipitations separate out valuable metal content high, can directly carry out comprehensive recovery of indium.
In the inventive method, adopt oxygen clean, inexpensive, that easily get to carry out hematite process as oxygenant and remove arsenic, antimony, the decreasing ratio of arsenic is greater than 99%, and the decreasing ratio of antimony is greater than 90%, and in slag, iron level is greater than 62%; The arsenic of technique output, the stable performance of antimony slag, strainability is good, and the quantity of slag is few, and valuable metal content is high, is conducive to the comprehensive reutilization of rhombohedral iron ore slag; Content after arsenic removal simultaneously, antimony in liquid, respectively 0.5 with below 6mg/L, meets the requirement of emission standard.
Accompanying drawing explanation
Accompanying drawing is the process flow sheet of a kind of arsenic removal from zinc smelting leach liquor of the present invention, antimony method.
Embodiment
A method of smelting arsenic removal leach liquor, antimony from zinc, is to smelt low acid leaching liquor as raw material take zinc, adopts reductive agent, comprises zinc ore concentrate, zinc sulfite, sulfurous gas etc., and solution is carried out to prereduction, makes Fe
3+be reduced to the higher Fe of hydrolytic precipitation pH value
2+; By in the neutralizing agents such as lime, Wingdale, secondary zinc oxide, calcining, zinc oxide and free acid, then adopt the neutralizing agent precipitation valuable metal indiums such as calcining, secondary zinc oxide, zinc oxide, to recycle; Finally carry out hematite process arsenic removal, antimony with Purifying Zinc solution by oxygen clean, cheap, that easily get.
Method of the present invention is further described with following indefiniteness embodiment, to contribute to understanding content of the present invention and advantage thereof, and not as limiting the scope of the present invention, protection scope of the present invention is determined by claims.
Embodiment 1
To in the low acid leaching liquor of Zn104g/L, Fe21g/L, In0.15g/L, As0.10g/L, Sb0.05g/L, add zinc ore concentrate to carry out prereduction, concentrate add-on is 1.2 times of theoretical amount, 95 ℃ are reacted 3 hours, the about 0.9g/L of ferric iron, reduction ratio 95.7% in liquid after reduction, solid-liquid separation must be reduced rear liquid; At 90 ℃, Wingdale is slowly joined after reduction to regulator solution pH value in liquid, continue to react 120min in the time that pH is stabilized in 1.0 left and right, solid-liquid separation obtains liquid after one section of neutralization; With in secondary zinc oxide and remaining acid, control endpoint pH approximately 4.5 at 90 ℃, after reaction 2h, solid-liquid separation obtains liquid (i.e. liquid after neutralization) after indium slag and heavy indium; The liquid that will sink after indium is that 170 ℃, oxygen partial pressure are to react 3h under 0.3MPa, stagnation pressure 1.7MPa condition in temperature, and solid-liquid separation obtains liquid after rhombohedral iron ore and arsenic removal, antimony, and after arsenic removal, antimony, liquid is respectively 0.2mg/L and 1mg/L containing arsenic, antimony.
Embodiment 2
To in the low acid leaching liquor of Zn104g/L, Fe21g/L, In0.15g/L, As0.15g/L, Sb0.1g/L, add zinc sulfite to carry out prereduction, zinc sulfite add-on is 1.1 times of theoretical amount, 95 ℃ are reacted 3 hours, the about 0.6g/L of ferric iron, reduction ratio 97.1% in liquid after reduction, solid-liquid separation must be reduced rear liquid; At 90 ℃, calcining is slowly joined after reduction to regulator solution pH value in liquid, continue to react 120min in the time that pH is stabilized in 1.0 left and right, solid-liquid separation obtains liquid after one section of neutralization; With in secondary zinc oxide and remaining acid, control endpoint pH approximately 4.5 at 80 ℃, after reaction 2h, solid-liquid separation obtains liquid (i.e. liquid after neutralization) after indium slag and heavy indium; The liquid that will sink after indium is that 120 ℃, oxygen partial pressure are to react 3h under 0.1MPa, stagnation pressure 1.2MPa condition in temperature, and solid-liquid separation obtains liquid after rhombohedral iron ore and arsenic removal, antimony, and after arsenic removal, antimony, liquid is respectively 0.5mg/L and 6mg/L containing arsenic, antimony.
Embodiment 3
To in the low acid leaching liquor of Zn104g/L, Fe21g/L, In0.15g/L, As1g/L, Sb1g/L, add zinc sulfite to carry out prereduction, zinc sulfite add-on is 1.1 times of theoretical amount, 95 ℃ are reacted 3 hours, the about 0.6g/L of ferric iron, reduction ratio 97.1% in liquid after reduction, solid-liquid separation must be reduced rear liquid; At 90 ℃, zinc oxide is slowly joined after reduction to regulator solution pH value in liquid, continue to react 120min in the time that pH is stabilized in 1.0 left and right, solid-liquid separation obtains liquid after one section of neutralization; By in secondary zinc oxide and remaining acid, control endpoint pH approximately 4.5 at 90 ℃, after reaction 2h, solid-liquid separation obtains liquid (i.e. liquid after neutralization) after indium slag and heavy indium; The liquid that will sink after indium is that 170 ℃, oxygen partial pressure are to react 3h under 0.3MPa, stagnation pressure 1.7MPa condition in temperature, and solid-liquid separation obtains liquid after rhombohedral iron ore and arsenic removal, antimony, and after arsenic removal, antimony, liquid is respectively 0.3mg/L and 3mg/L containing arsenic, antimony.
Embodiment 4
To in the low acid leaching liquor of Zn104g/L, Fe21g/L, In0.15g/L, As2g/L, Sb1.5g/L, add zinc sulfite to carry out prereduction, zinc sulfite add-on is 1.1 times of theoretical amount, 95 ℃ are reacted 3 hours, the about 0.6g/L of ferric iron, reduction ratio 97.1% in liquid after reduction, solid-liquid separation must be reduced rear liquid; At 90 ℃, zinc oxide is slowly joined after reduction to regulator solution pH value in liquid, continue to react 60min in the time that pH is stabilized in 1.0 left and right, solid-liquid separation obtains liquid after one section of neutralization; With in inferior calcining and remaining acid, control endpoint pH approximately 5.4 at 85 ℃, after reaction 1h, solid-liquid separation obtains liquid (i.e. liquid after two sections of neutralizations) after indium slag and heavy indium; The liquid that will sink after indium is that 170 ℃, oxygen partial pressure are to react 1h under 0.3MPa, stagnation pressure 1.7MPa condition in temperature, and solid-liquid separation obtains liquid after rhombohedral iron ore and arsenic removal, antimony, and after arsenic removal, antimony, liquid is respectively 0.2mg/L and 3mg/L containing arsenic, antimony.
Embodiment 5
To in the low acid leaching liquor of Zn104g/L, Fe21g/L, In0.15g/L, As1.5g/L, Sb2g/L, add zinc sulfite to carry out prereduction, zinc sulfite add-on is 1.1 times of theoretical amount, 40 ℃ are reacted 3 hours, the about 1.5g/L of ferric iron, reduction ratio 92.9% in liquid after reduction, solid-liquid separation must be reduced rear liquid; At 40 ℃, zinc oxide is slowly joined after reduction to regulator solution pH value in liquid, continue to react 20min in the time that pH is stabilized in 1.0 left and right, solid-liquid separation obtains liquid after one section of neutralization; With in secondary zinc oxide and remaining acid, control endpoint pH approximately 4.0 at 100 ℃, after reaction 2h, solid-liquid separation obtains liquid (i.e. liquid after two sections of neutralizations) after indium slag and heavy indium; The liquid that will sink after indium is that 180 ℃, oxygen partial pressure are to react 3h under 0.2MPa, stagnation pressure 1.7MPa condition in temperature, and solid-liquid separation obtains liquid after rhombohedral iron ore and arsenic removal, antimony, and after arsenic removal, antimony, liquid is respectively 0.1mg/L and 0.5mg/L containing arsenic, antimony.
Embodiment 6
To in the low acid leaching liquor of Zn104g/L, Fe21g/L, In0.15g/L, As1.0g/L, Sb1.0g/L, pass into SO
2carry out prereduction, keep 95 ℃ of temperature of reaction recording solution current potentials simultaneously, in the time that solution potential is reduced to a stationary value, reduction reaction completes substantially, the about 0.4g/L of ferric iron, reduction ratio 98.1% in liquid after reduction, and solid-liquid separation must be reduced rear liquid; At 90 ℃, zinc oxide is slowly joined after reduction to regulator solution pH value in liquid, continue to react 120min in the time that pH is stabilized in 1.0 left and right, solid-liquid separation obtains liquid after one section of neutralization; With in secondary zinc oxide and remaining acid, control endpoint pH approximately 4.5 at 95 ℃, after reaction 2h, solid-liquid separation obtains liquid (i.e. liquid after two sections of neutralizations) after indium slag and heavy indium; The liquid that will sink after indium is that 170 ℃, oxygen partial pressure are to react 3h under 0.3MPa, stagnation pressure 1.7MPa condition in temperature, and solid-liquid separation obtains liquid after rhombohedral iron ore and arsenic removal, antimony, and after arsenic removal, antimony, liquid is respectively 0.2mg/L and 2mg/L containing arsenic, antimony.
Claims (9)
1. a method of smelting arsenic removal leach liquor, antimony from zinc, is characterized in that, comprises the following steps:
(1) smelt low acid leaching liquor as raw material take zinc, under the condition existing, reduce at reductive agent, make high price iron ion change iron ion at a low price into, the zinc after being reduced is smelted leach liquor;
(2) zinc after reduction being smelted to leach liquor adopts neutralizing agent to carry out one section of neutralization adjusting pH value, liquid after solid-liquid separation obtains one section of neutralization;
(3) adopt neutralizing agent to carry out two sections of neutralizations liquid after one section of neutralization, make the indium precipitate and separate in leach liquor simultaneously, obtain liquid and indium slag after heavy indium;
(4) will sink after indium liquid by hematite process arsenic removal, antimony, obtain leach liquor after arsenic removal, antimony and containing arsenic antimony scum;
(5) indium slag of step (3) is extracted to indium, the leach liquor after arsenic removal, the antimony of step (4) is returned to neutral Leaching Zinc smelting procedure.
2. method according to claim 1, is characterized in that, described zinc is smelted low acid leaching liquor main component and is: zinc: 60～120g/L, iron: 10～40g/L, indium: 0.05～0.5g/L, arsenic: 0.1～2.0g/L, copper: 0.5～5g/L, antimony: 0.01～2g/L.
3. method according to claim 1, is characterized in that, the reductive agent in step (1) is one or more that are selected from zinc ore concentrate, zinc sulfite, sulfurous gas.
4. method according to claim 1, it is characterized in that, reductive agent consumption in step (1) is theoretical amount 1.0～1.5 times, under 80～100 ℃ of conditions, reduce 1～5h, make zinc after reduction smelt high price iron ion content in leach liquor lower than 2g/L.
5. method according to claim 1, is characterized in that, one section of neutralizing agent described in step (2) is one or more that are selected from lime, Wingdale, secondary zinc oxide, calcining, zinc oxide.
6. method according to claim 1, is characterized in that, neutral temperature is 40～90 ℃ in step (2), in and time 20～120min, more than neutralization end of a period sulfuric acid concentration 5g/L.
7. method according to claim 1, is characterized in that, two sections of neutralizing agents described in step (3) are one or more that are selected from calcining, secondary zinc oxide, zinc oxide.
8. method according to claim 1, is characterized in that, neutral temperature is 80～100 ℃ in step (3), in and time 0.5～2h, neutralization end of a period pH value is 4.0～5.4, makes indium precipitate enrichment.
9. method according to claim 1, is characterized in that, the temperature of the hematite process arsenic removal described in step (4), antimony is 120～180 ℃, and oxygen partial pressure is 0.1～0.5MPa, and stagnation pressure is 1.1～1.7MPa, and arsenic removal, antimony time are 1～4h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105039697A (en) * | 2015-08-07 | 2015-11-11 | 贵州宏达环保科技有限公司 | Method for reducing ferric ions in pickle liquor containing Ge, In and Zn into ferrous ions |
| CN106011476A (en) * | 2016-06-21 | 2016-10-12 | 昆明冶金研究院 | New process for extracting scandium in gas ash |
| CN106834698A (en) * | 2017-01-19 | 2017-06-13 | 昆明理工大学 | A kind of method of enriching and reclaiming indium in acid solution containing indium from low concentration |
| CN108823405A (en) * | 2018-07-09 | 2018-11-16 | 刘罗平 | A kind of dilute immersion liquid method of wet process refining indium |
| CN110352254A (en) * | 2018-02-01 | 2019-10-18 | 高丽亚铅株式会社 | From the method for solution of zinc sulfate recycling iron |
| CN112575189A (en) * | 2020-11-20 | 2021-03-30 | 金川集团股份有限公司 | Treatment method of high-chromium high-magnesium platinum group metal ore dressing concentrate strengthening leaching solution |
| CN112708760A (en) * | 2020-12-29 | 2021-04-27 | 金川集团股份有限公司 | Method for removing antimony in nickel refining system |
| CN112981116A (en) * | 2021-01-28 | 2021-06-18 | 江西铜业股份有限公司 | Method for separating copper, zinc, cadmium and arsenic in white smoke dust |
| CN114606400A (en) * | 2022-01-28 | 2022-06-10 | 云锡文山锌铟冶炼有限公司 | Method for treating arsenic-zinc-containing leaching residues of high-iron |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105039697A (en) * | 2015-08-07 | 2015-11-11 | 贵州宏达环保科技有限公司 | Method for reducing ferric ions in pickle liquor containing Ge, In and Zn into ferrous ions |
| CN106011476A (en) * | 2016-06-21 | 2016-10-12 | 昆明冶金研究院 | New process for extracting scandium in gas ash |
| CN106011476B (en) * | 2016-06-21 | 2018-01-12 | 昆明冶金研究院 | The technique of scandium in a kind of extraction gas ash |
| CN106834698A (en) * | 2017-01-19 | 2017-06-13 | 昆明理工大学 | A kind of method of enriching and reclaiming indium in acid solution containing indium from low concentration |
| US11001507B2 (en) | 2018-02-01 | 2021-05-11 | Korea Zinc Co., Ltd. | Method of recovering iron from zinc sulphate solution |
| CN110352254A (en) * | 2018-02-01 | 2019-10-18 | 高丽亚铅株式会社 | From the method for solution of zinc sulfate recycling iron |
| EP3719146A4 (en) * | 2018-02-01 | 2021-03-31 | Korea Zinc Co., Ltd. | Method for recovering iron from zinc sulfate solution |
| CN110352254B (en) * | 2018-02-01 | 2021-06-11 | 高丽亚铅株式会社 | Method for recovering iron from zinc sulfate solution |
| CN108823405A (en) * | 2018-07-09 | 2018-11-16 | 刘罗平 | A kind of dilute immersion liquid method of wet process refining indium |
| CN112575189A (en) * | 2020-11-20 | 2021-03-30 | 金川集团股份有限公司 | Treatment method of high-chromium high-magnesium platinum group metal ore dressing concentrate strengthening leaching solution |
| CN112708760A (en) * | 2020-12-29 | 2021-04-27 | 金川集团股份有限公司 | Method for removing antimony in nickel refining system |
| CN112708760B (en) * | 2020-12-29 | 2022-11-25 | 金川集团股份有限公司 | Method for removing antimony in nickel refining system |
| CN112981116A (en) * | 2021-01-28 | 2021-06-18 | 江西铜业股份有限公司 | Method for separating copper, zinc, cadmium and arsenic in white smoke dust |
| CN114606400A (en) * | 2022-01-28 | 2022-06-10 | 云锡文山锌铟冶炼有限公司 | Method for treating arsenic-zinc-containing leaching residues of high-iron |
| CN114606400B (en) * | 2022-01-28 | 2023-09-22 | 云锡文山锌铟冶炼有限公司 | Treatment method of high-iron arsenic-zinc-containing leaching residues |
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