CN101104884A - Method for leaching, enriching and reclaiming indium from lead-zinc smelting by-product zinc oxide - Google Patents
Method for leaching, enriching and reclaiming indium from lead-zinc smelting by-product zinc oxide Download PDFInfo
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- CN101104884A CN101104884A CNA2007100355333A CN200710035533A CN101104884A CN 101104884 A CN101104884 A CN 101104884A CN A2007100355333 A CNA2007100355333 A CN A2007100355333A CN 200710035533 A CN200710035533 A CN 200710035533A CN 101104884 A CN101104884 A CN 101104884A
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Abstract
The invention discloses a method for leaching, enriching and recovering indium from zinc oxide byproduct in the lead and zinc smelting process. The invention is implemented by the following technical proposal: by using three-step leaching process and adding oxidizing agent in the leached slurry, the problem of low indium leaching rate is solved; intermittent slag feeding mode is used to prevent the over-high acidity due to the leached strong acids and the excessive iron production and thus to avoid the production of indium-conjugated jarosite in the next preneutralization process, which may influence the recovery of indium; the high-acidity solution is neutralized with a neutralizer such as zinc oxide or zinc calcine, so that the problem of high-acidity solution disposal is solved; when the low-acidity and high-acidity leach slurry are fed into the concentration machine, the compound flocculant is added to solve the technical problems of difficulty in settlement clarification of ore slurry, poor fluidity of thickened underflow and serious hardening. With this method, the indium leaching rate is increased up to 70-80 percent and the recovery rates of indium and zinc are also increased. Additionally, the method allows the disposal of lead-containing materials (lead slag) in the lead system and helps to reduce the discharge of waste slag, gas and water, protecting the environment.
Description
Technical field
The present invention relates to a kind of production method of indium, particularly a kind ofly from lead-zinc smelting by-product zinc oxide, leach, the method for enriching and reclaiming indium.
Background technology
Indium metal does not have independent mineral at occurring in nature, follow in lead, zinc, tin and copper mine, and content is seldom, and indium content in metallic ore generally is ten thousand/several.The leaching process of indium generally can be divided into 4 stages, and the one, make the enrichment of indium in its main METAL EXTRACTION process; The 2nd, produce the indium enriched substance; The 3rd, make thick indium by a series of chemical metallurgy processes; The 4th, thick indium electrolysis gets smart indium ingot.The approach that extracts indium in the present prior art mainly contains following several: the one, from the leaching residue extraction indium of zinc hydrometallurgy, for comprehensively putting forward the topmost approach of indium; The 2nd, from the byproduct-hard zinc (zinc-iron alloy) of pyrometallurgy of zinc, extract indium; The 3rd, from lead bullion scum silica frost and copper converter dirt, extract indium; The 4th, from solder electrolytic liquid, extract indium.On the increasingly extensive basis of the application of indium, further exploitation improves indium leaching, recovery technology, has very high economic worth.For reducing the refinement cost of indium, those skilled in the art are exploring new refinement cost method one's own profession.The by-product zinc oxide that for example produces in the lead-zinc smelting process has been finished the enrichment of indium to a certain extent, by-product zinc oxide generally contains In0.02～0.5%, other composition can be: Zn30～80%Pb1～30%Fe0.2～15% also has a spot of As, Sb, Ge, Cu, Au, Ag, Cd, Bi, Ni etc.The method of taking the extracting method of wet method to produce the indium enriched substance from lead-zinc smelting by-product zinc oxide is: indium is leached, and make every effort to reach zinc content reduction in the lead skim, the effect that lead tolerance raises, the rate of recovery of raising indium, zinc.This method generally adopts two sections extract technologies at present, and promptly first section neutral leaching controlled and leached 4.0～5.2, second section acid leaching of terminal point pH value, control leaching terminal point acidity 15～30g/l.The leaching yield of this technology only is 30～60% generally, and the rate of recovery of indium, zinc is low excessively, causes the serious wasting of resources.Three sections extract technologies are the improvement on the basis of two sections extract technologies, and it increases by one section peracid extract technology, is about to the leaching that acid leached mud carries out higher acidity again, and it is 30～100g/l that terminal point acidity is leached in control.Three sections existing bibliographical informations of extract technology (are seen literary composition " Development of Zinc Hydrometallurgy Technology in China " Liu Jiefeng, [periodical name] Hunan non-ferrous metal, 03 phase of calendar year 2001), but still be in laboratory stage or pilot-plant test stage, in suitability for industrialized production, also exist peracid leach the liquid-solid separation difficulty of ore pulp, peracid thickened underflow mobile poor, harden seriously, contain technical problems such as the high acid solution of indium is difficult, the industrialized producing technology flow process is Success in Experiment not as yet, do not have actual operability, can't apply, suitability for industrialized production is unrealized.How to solve the problems of the technologies described above, make three sections extract technologies to realize that industrial production is a difficult problem that remains to be explored.
Summary of the invention
The objective of the invention is to overcome the prior art deficiency, provide a kind of and new leach from lead-zinc smelting by-product zinc oxide, the method for enriching and reclaiming indium, it adopts three sections extract technologies, improves leaching yield, the rate of recovery of indium, the minimizing wasting of resources.
Technical scheme of the present invention is:
A kind ofly from lead-zinc smelting by-product zinc oxide, leach, the method for enriching and reclaiming indium, it is characterized in that comprising successively following steps:
Step 1: by-product zinc oxide through the neutral leaching of sulfuric acid, is obtained containing the neutral leach liquor and the neutral leached mud that contains indium 0.05～1.5% of indium 0.005～0.05g/l;
Step 2: the neutral leached mud that step 1 is obtained goes out with the low acidleach of sulfuric acid, leach initial acidity 60～300g/l, low acidleach after the leaching goes out ore pulp and carry out liquid-solid separation in separating device, add and mix flocculation agent, clarification obtains containing indium 0.1～2.0g/l, contains acid 15～30g/l acidic solution and contains the acid leached mud of indium 0.05～1.5%;
Step 3: the acid leached mud that step 2 is obtained carries out high temperature, peracid leaching with sulfuric acid, in leaching ore pulp, add oxygenant, it is 100～400g/l that initial acidity is leached in control, leaching terminal point acidity is 30～100g/l, temperature of reaction is 70～100 ℃, reaction times is 4～24h, obtains peracid and leaches ore pulp;
Step 4: the peracid leaching ore pulp that step 3 is obtained carries out liquid-solid separation in separating device, add and mix flocculation agent, clarification, obtain containing indium 0.1～2.0g/l, contain the high acid solution of acid 30～100g/l and contain indium 0.02～0.5%, contain zinc 2～15%, leaded 20～60% lead skim;
Step 5: the high acid solution that step 4 is obtained carries out neutralization reaction with neutralizing agent, stir, terminal point acid concentration to solution is 15～30g/l, in separating device, carry out liquid-solid separation again, add and mix flocculation agent, clarification obtains containing indium 0.1～2.0g/l, contains the pre-neutralization slag that acid 15～30g/l contains solution of indium and contains indium 0.05～1.5%, the pre-neutralization slag is returned step 3 handle.
Step 6: the low acid that step 5 is obtained contains low acid that solution of indium and step 2 obtain and contains solution of indium and be mixed into the line replacement reaction, adds the indium in the zinc dust precipitation solution, obtains containing the indium slag of indium 0.5～10%.
As to further improvement of the present invention, the oxygenant in the described step 3 is potassium permanganate or Manganse Dioxide, and potassium permanganate weight is 0.02～0.5kg/m with leaching the ore pulp volume ratio
3, Manganse Dioxide weight is 0.2～5kg/m with leaching the ore pulp volume ratio
3
As to further improvement of the present invention, to join the slag input mode in the conversion unit be that intermittent type adds in batches to acid leached mud in the described step 3, promptly at first add the acid leached mud of 10～70% volumes, add required sulfuric acid again, add the acid leached mud of residual volume at last.
As to further improvement of the present invention, the neutral leach liquor that obtains after the reaction in the described step 1 is back to before the reaction and mixes use with sulfuric acid.
As to further improvement of the present invention, the neutralizing agent that is adopted in the described step 5 is zinc oxide or zinc baking sand, and the neutralization reaction time is 0.5～8 hour.
As to further improvement of the present invention, described mixing flocculation agent is mixed by polyacrylamide and gelatin, and its weight ratio is 50: 1～4: 1, and mixing flocculation agent weight is 0.2～2kg/m with peracid leaching ore pulp volume ratio
3
Beneficial effect of the present invention is:
The present invention adopts three sections extract technologies to extract to the valuable metal in the by-product zinc oxide that produces in the lead-zinc smelting process, has adopted to add oxygenant solved the low problem of indium leaching yield in leaching ore pulp; Adopt step slag input mode, prevent that peracid from leaching initial acid and spending height, prevent that iron from too much being leached, form the indium siderotil when avoiding next step pre-neutralization, influence the recovery of indium; High acid solution is adopted neutralizing agents such as zinc oxide or zinc baking sand carry out neutralization reaction, solved how disposal concerns of high acid solution, when low acidleach goes out ore pulp, peracid and leaches ore pulp and enter thickener, add to mix flocculation agent, solved difficult heavy clear, the thickened underflow of ore pulp mobile poor, serious technical problem hardens.
The present invention is increased to 70%～80% with the leaching yield of indium in the by-product zinc oxide that produces in the lead-zinc smelting process, make simultaneously and contain the reduction of zinc rate in the lead skim, leaded rate raises, and has not only improved the rate of recovery of indium, zinc, has created condition for lead system processing lead-containing material (lead skim) simultaneously.Its expendable material is that common material and consumption are less.Reduced production cost, improved recovery rate of valuable metals, made three sections extract technologies have economic feasibility, promoted the use of the production practice from the laboratory.The present invention does not increase waste residue, waste gas, discharge of wastewater, non-environmental-pollution.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Further specify the present invention by the following examples.
Implement example 1:
Adopt the present invention to the lead-zinc smelting by-product zinc oxide calcining leach, enriching and reclaiming indium, contain indium 0.02% in its zinc-oxide calcine, contain zinc 58.75%, leaded 9.98%.Zinc-oxide calcine is obtained ore pulp according to a conventional method behind ore deposit, ball milling, ore pulp is carried out successively according to the following steps:
Step 1: through the neutral leaching of sulfuric acid, the neutral leached mud that obtains containing the neutral leach liquor of indium 0.005g/l and contain indium 0.05%, neutral leach liquor return with sulfuric acid and are mixed for the neutral leaching of by-product zinc oxide with the zinc-oxide calcine ore pulp;
Step 2: the neutral leached mud that step 1 is obtained goes out with the low acidleach of sulfuric acid, leach initial acidity 60g/l, low acidleach after the leaching goes out ore pulp and carry out liquid-solid separation in separating device, add the mixing flocculation agent that polyacrylamide and gelatin mix, its weight ratio is 50: 1, clarification obtains containing indium 0.1g/l, contains sour 15g/l acidic solution and contains the acid leached mud of indium 0.05%;
Step 3: the acid leached mud that step 2 is obtained carries out high temperature, peracid leaching with sulfuric acid, the slag input mode is that intermittent type adds in batches, promptly at first add the acid leached mud of 10% volume, add required sulfuric acid again, the acid leached mud that adds residual volume at last, add potassium permanganate in leaching ore pulp, potassium permanganate weight is 0.02kg/m with leaching the ore pulp volume ratio
3, it is 100g/l that initial acidity is leached in control, and leaching terminal point acidity is 30g/l, and temperature of reaction is 70 ℃, and the reaction times is 4h, obtains peracid and leaches ore pulp;
Step 4: the peracid leaching ore pulp that step 3 is obtained carries out liquid-solid separation in separating device, add the mixing flocculation agent that is mixed by polyacrylamide and gelatin, and its weight ratio is 50: 1, and mixing flocculation agent weight and peracid leaching ore pulp volume ratio is 0.2kg/m
3, behind the pulp clarification, obtain containing indium 0.1g/l, contain the high acid solution of sour 30g/l and contain indium 0.02%, contain zinc 15%, leaded 20% lead skim;
Step 5: the high acid solution that step 4 is obtained carries out neutralization reaction with the zinc oxide neutralizing agent, stir, terminal point acid concentration to solution is 15g/l, the neutralization reaction time is 0.5 hour, in separating device, carry out liquid-solid separation again, the mixing flocculation agent that adding is mixed by polyacrylamide and gelatin, its weight ratio are 50: 1, and mixing flocculation agent weight and peracid leaching ore pulp volume ratio is 0.2kg/m
3, clarification obtains containing indium 0.1g/l, contains the pre-neutralization slag that sour 15g/l contains solution of indium and contains indium 0.05%, the pre-neutralization slag is returned step 3 handle.
Step 6: the low acid that step 5 is obtained contains low acid that solution of indium and step 2 obtain and contains solution of indium and be mixed into the line replacement reaction, adds the indium in the zinc dust precipitation solution, obtains containing the indium slag of indium 0.5%.
Implement example 2:
Adopt the present invention to the lead-zinc smelting by-product zinc oxide calcining leach, enriching and reclaiming indium, its zinc-oxide calcine contains indium 0.5%, contains zinc 50.53%, leaded 12.46%.Zinc-oxide calcine is obtained ore pulp according to a conventional method behind ore deposit, ball milling, ore pulp is carried out successively according to the following steps:
Step 1: through the neutral leaching of sulfuric acid, the neutral leached mud that obtains containing the neutral leach liquor of indium 0.05g/l and contain indium 1.5%, neutral leach liquor return and are used for sulfuric acid the neutral leaching of by-product zinc oxide with zinc-oxide calcine;
Step 2: the neutral leached mud that step 1 is obtained goes out with the low acidleach of sulfuric acid, leach initial acidity 300g/l, low acidleach after the leaching goes out ore pulp and carry out liquid-solid separation in separating device, the mixing flocculation agent that adding is mixed by polyacrylamide and gelatin, its weight ratio is 4: 1, clarification obtains containing indium 2.0g/l, contains sour 30g/l acidic solution and contains the acid leached mud of indium 1.5%;
Step 3: the acid leached mud that step 2 is obtained carries out high temperature, peracid leaching with sulfuric acid, the slag input mode is that intermittent type adds in batches, promptly at first add the acid leached mud of 70% volume, add required sulfuric acid again, the acid leached mud that adds residual volume at last, add Manganse Dioxide in leaching ore pulp, Manganse Dioxide weight is 5kg/m with leaching the ore pulp volume ratio
3, it is 400g/l that initial acidity is leached in control, and leaching terminal point acidity is 100g/l, and temperature of reaction is 100 ℃, and the reaction times is 24h, obtains peracid and leaches ore pulp;
Step 4: the peracid leaching ore pulp that step 3 is obtained carries out liquid-solid separation in separating device, add the mixing flocculation agent that is mixed by polyacrylamide and gelatin, and its weight ratio is 4: 1, and mixing flocculation agent weight and peracid leaching ore pulp volume ratio is 2kg/m
3, behind the pulp clarification, obtain containing indium 2.0g/l, contain the high acid solution of sour 100g/l and contain indium 0.5%, contain zinc 2%, leaded 60% lead skim;
Step 5: the high acid solution that step 4 is obtained carries out neutralization reaction with the zinc baking sand neutralizing agent, stir, terminal point acid concentration to solution is 30g/l, the neutralization reaction time is 8 hours, in separating device, carry out liquid-solid separation again, the mixing flocculation agent that adding is mixed by polyacrylamide and gelatin, its weight ratio are 4: 1, and mixing flocculation agent weight and peracid leaching ore pulp volume ratio is 2kg/m
3, clarification obtains containing indium 2.0g/l, contains the pre-neutralization slag that sour 30g/l contains solution of indium and contains indium 1.5%, the pre-neutralization slag is returned step 3 handle.
Step 6: the low acid that step 5 is obtained contains low acid that solution of indium and step 2 obtain and contains solution of indium and be mixed into the line replacement reaction, adds the indium in the zinc dust precipitation solution, obtains containing the indium slag of indium 10%.
Claims (6)
- One kind from lead-zinc smelting by-product zinc oxide, leach, the method for enriching and reclaiming indium, it is characterized in that comprising successively following steps:Step 1: by-product zinc oxide through the neutral leaching of sulfuric acid, is obtained containing the neutral leach liquor and the neutral leached mud that contains indium 0.05～1.5% of indium 0.005～0.05g/l;Step 2: the neutral leached mud that step 1 is obtained goes out with the low acidleach of sulfuric acid, leach initial acidity 60～300g/l, low acidleach after the leaching goes out ore pulp and carry out liquid-solid separation in separating device, add and mix flocculation agent, clarification obtains containing indium 0.1～2.0g/l, contains acid 15～30g/l acidic solution and contains the acid leached mud of indium 0.05～1.5%;Step 3: the acid leached mud that step 2 is obtained carries out high temperature, peracid leaching with sulfuric acid, in leaching ore pulp, add oxygenant, it is 100～400g/l that initial acidity is leached in control, leaching terminal point acidity is 30～100g/l, temperature of reaction is 70～100 ℃, reaction times is 4～24h, obtains peracid and leaches ore pulp;Step 4: the peracid leaching ore pulp that step 3 is obtained carries out liquid-solid separation in separating device, add and mix flocculation agent, clarification, obtain containing indium 0.1～2.0g/l, contain the high acid solution of acid 30～100g/l and contain indium 0.02～0.5%, contain zinc 2～15%, leaded 20～60% lead skim;Step 5: the high acid solution that step 4 is obtained carries out neutralization reaction with neutralizing agent, stir, terminal point acid concentration to solution is 15～30 g/l, in separating device, carry out liquid-solid separation again, add and mix flocculation agent, clarification obtains containing indium 0.1～2.0g/l, contains the pre-neutralization slag that acid 15～30 g/l contain solution of indium and contain indium 0.05～1.5%, the pre-neutralization slag is returned step 3 handle;Step 6: the low acid that step 5 is obtained contains low acid that solution of indium and step 2 obtain and contains solution of indium and be mixed into the line replacement reaction, adds the indium in the zinc dust precipitation solution, obtains containing the indium slag of indium 0.5～10%.
- 2. according to claim 1ly from lead-zinc smelting by-product zinc oxide, leach, the method for enriching and reclaiming indium, it is characterized in that: the oxygenant in the described step 3 is potassium permanganate or Manganse Dioxide, and potassium permanganate weight is 0.02～0.5kg/m with leaching the ore pulp volume ratio 3, Manganse Dioxide weight is 0.2～5kg/m with leaching the ore pulp volume ratio 3
- 3. according to claim 1ly from lead-zinc smelting by-product zinc oxide, leach, the method for enriching and reclaiming indium, it is characterized in that: to join the slag input mode in the conversion unit be that intermittent type adds in batches to acid leached mud in the described step 3, promptly at first add the acid leached mud of 10～70% volumes, add required sulfuric acid again, add the acid leached mud of residual volume at last.
- 4. according to claim 1ly from lead-zinc smelting by-product zinc oxide, leach, the method for enriching and reclaiming indium, it is characterized in that: the neutral leach liquor that obtains after the reaction in the described step 1 is back to neutral leach before the reaction and mixes use with sulfuric acid.
- 5. according to claim 1ly from lead-zinc smelting by-product zinc oxide, leach, the method for enriching and reclaiming indium, it is characterized in that: the neutralizing agent that is adopted in the described step 5 is zinc oxide or zinc baking sand, the neutralization reaction time is 0.5～8 hour.
- 6. according to claim 1ly from lead-zinc smelting by-product zinc oxide, leach, the method for enriching and reclaiming indium, it is characterized in that: described mixing flocculation agent is mixed by polyacrylamide and gelatin, polyacrylamide and gelatin weight ratio are 50: 1～4: 1, and mixing flocculation agent weight and peracid leaching ore pulp volume ratio is 0.2～2kg/m 3
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101994009A (en) * | 2010-12-10 | 2011-03-30 | 株洲冶炼集团股份有限公司 | Method for enriching and recovering indium from zinc oxide acid supernate |
| CN101798639B (en) * | 2009-12-16 | 2011-06-08 | 株洲冶炼集团股份有限公司 | Method for recovering indium from indium-containing neutralized dregs directly leached from zinc concentrate |
| CN103173625A (en) * | 2013-04-19 | 2013-06-26 | 长沙矿冶研究院有限责任公司 | Method for efficiently leaching indium from zinc oxide smoke |
| CN103898335A (en) * | 2014-03-24 | 2014-07-02 | 中国恩菲工程技术有限公司 | System for processing zinc roasting ore |
| CN104141046A (en) * | 2014-07-24 | 2014-11-12 | 安阳市岷山有色金属有限责任公司 | Method for carrying out indium and zinc recycling on indium zinc oxide soot |
| US8906947B2 (en) | 2008-02-01 | 2014-12-09 | Zhejiang Hisun Pharmaceutical Co., Ltd. | Method for the separation and purification of epothilones |
| CN105087927A (en) * | 2015-08-11 | 2015-11-25 | 湖南水口山有色金属集团有限公司 | Method for increasing leaching rate of zinc and indium in second zinc oxide |
| CN108048659A (en) * | 2017-11-22 | 2018-05-18 | 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 | A kind of leaching method of zinc replacement slag |
| CN111270091A (en) * | 2020-02-29 | 2020-06-12 | 河南豫光锌业有限公司 | Method for reducing indium content in indium leaching slag |
| CN114836627A (en) * | 2022-06-01 | 2022-08-02 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of indium-containing zinc oxide smoke dust |
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2007
- 2007-08-09 CN CNB2007100355333A patent/CN100537796C/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8906947B2 (en) | 2008-02-01 | 2014-12-09 | Zhejiang Hisun Pharmaceutical Co., Ltd. | Method for the separation and purification of epothilones |
| CN101798639B (en) * | 2009-12-16 | 2011-06-08 | 株洲冶炼集团股份有限公司 | Method for recovering indium from indium-containing neutralized dregs directly leached from zinc concentrate |
| CN101994009B (en) * | 2010-12-10 | 2012-10-03 | 株洲冶炼集团股份有限公司 | Method for enriching and recovering indium from zinc oxide acid supernate |
| CN101994009A (en) * | 2010-12-10 | 2011-03-30 | 株洲冶炼集团股份有限公司 | Method for enriching and recovering indium from zinc oxide acid supernate |
| CN103173625A (en) * | 2013-04-19 | 2013-06-26 | 长沙矿冶研究院有限责任公司 | Method for efficiently leaching indium from zinc oxide smoke |
| CN103173625B (en) * | 2013-04-19 | 2014-12-10 | 长沙矿冶研究院有限责任公司 | Method for efficiently leaching indium from zinc oxide smoke |
| CN103898335A (en) * | 2014-03-24 | 2014-07-02 | 中国恩菲工程技术有限公司 | System for processing zinc roasting ore |
| CN104141046A (en) * | 2014-07-24 | 2014-11-12 | 安阳市岷山有色金属有限责任公司 | Method for carrying out indium and zinc recycling on indium zinc oxide soot |
| CN105087927A (en) * | 2015-08-11 | 2015-11-25 | 湖南水口山有色金属集团有限公司 | Method for increasing leaching rate of zinc and indium in second zinc oxide |
| CN108048659A (en) * | 2017-11-22 | 2018-05-18 | 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 | A kind of leaching method of zinc replacement slag |
| CN111270091A (en) * | 2020-02-29 | 2020-06-12 | 河南豫光锌业有限公司 | Method for reducing indium content in indium leaching slag |
| CN114836627A (en) * | 2022-06-01 | 2022-08-02 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method of indium-containing zinc oxide smoke dust |
| CN114836627B (en) * | 2022-06-01 | 2024-01-30 | 长沙有色冶金设计研究院有限公司 | Oxygen pressure leaching method for indium-containing zinc oxide smoke dust |
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|---|---|
| CN100537796C (en) | 2009-09-09 |
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