CN100387733C - Method of extractin zinc from low grade zinc ore - Google Patents
Method of extractin zinc from low grade zinc ore Download PDFInfo
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- CN100387733C CN100387733C CNB2006100486015A CN200610048601A CN100387733C CN 100387733 C CN100387733 C CN 100387733C CN B2006100486015 A CNB2006100486015 A CN B2006100486015A CN 200610048601 A CN200610048601 A CN 200610048601A CN 100387733 C CN100387733 C CN 100387733C
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Abstract
The present invention relates to a process for extracting zinc from low-grade zinc ore. Said technological process includes the methods of leaching-out, extraction and electrowinning. Said invention provides technical support for reasonably utilizing zinc oxide zinc ore whose zinc content is less than 15% and zinc sulfide zinc ore whose zinc content is less than 8%. It is characterized by that said invention adopts mixed microorganism of sulfur oxide thiobacillus and ferrous oxide ferrobacillus which are collected and cultured in place to effectively leach out low-grade zinc ore. Said invention also provides the concrete steps of said leaching-out process.
Description
Technical field
The invention belongs to the zinc hydrometallurgy field, specifically, is the method for extracting zinc from low-grade zinc.
Background technology
The metallurgical method of low grade zinc ore resources is many, but energy is economical, efficiently utilize the method for low grade zinc resource not have substantially, the metallurgical new technology that needs the new low-grade zinc of exploitation realizes that low-grade zinc makes full use of, for the metallurgical Sustainable development of zinc provides technical support.
At present in the hydrometallurgical processes of the low-grade zinc oxide ore that adopts, alkalescence leaches, comprise that ammonia soaks, do not need reductive agent, reduce the quantity discharged of room temperature air to a certain extent, reduced environmental pollution, but alkali reagent expense height in the leaching process, the reagent rate of recovery are low, quality product is bad, finally causes the smelting cost height of zinc; Agitation leach need be carried out ore fine grinding and supporting whipping device, leaching process energy consumption height, expense height.No matter adopt which kind of mode to leach, the concentration of zine ion is all lower in the leach liquor, and leach liquor must carry out enrichment and just can enter in the existing hydrometallurgical processes flow process.The method of enrichment zinc is more, but its shortcoming is respectively arranged: evaporation concentration energy consumption height, heavy sour reagent consumption is big, causes the expense height.Both economical method is to adopt extraction and separation technology to carry out enrichment, make zine ion in the solution be able to carry out the level of zinc electrodeposition, but the leach liquor of low-grade zinc is extracting zinc directly, suitable arts demand oxidation make wherein iron with extract again after zinc separates, if directly extracting iron will be extracted simultaneously, so just make the extractant regeneration complex process, and a large amount of little spent acid of purposes of output, increase the extraction cost of zinc.At present, zinc ore leaching-solvent extraction-electrodeposition technology is still blank in China, though China is many to the research of zinc solution extraction, but research concentrates on extraction and removes in the impurity of solution of zinc sulfate, and most extraction system is hydrochloric acid system, systematic study is not carried out in solution of zinc sulfate extraction in the zinc smelting technology, do not adopted zinc leachings-extraction-electrodeposition process to carry out systematic study and yet with the smeltery of this technology construction zinc.In order to satisfy metallurgical stably manufactured of zinc and development, just must fully utilize various zinc resources, particularly the low grade zinc ore resources of China's abundant will be realized the utilization of these resources, just must develop the corresponding Technology of cost-effective these zinc resources of processing of energy.
Summary of the invention
Problem and shortage at above-mentioned prior art existence, the invention provides a kind of method of from low-grade zinc, extracting zinc, this new technological flow adopts the method for leaching-extraction-electrodeposition, can efficient, economic treatment low-grade zinc, contain zinc less than 15% zinc oxide zinc ore with contain zinc and provide technical support for rationally utilizing less than 8% zinc sulphide zinc ore.
The present invention will contain zinc less than 8% zinc sulfide ore or contain zinc and be processed into the granularity less than 30mm less than 15% zinc oxide ore, build heap, dump leaching, the heap leaching solution that leaches is carried out enrichment after electrodeposition obtain electric zinc, the steps include:
(1) will contain zinc and carry out the bacterium leaching less than 8% low grade zinc sulfide ore deposit, the dump leaching time is 10～12 months, the used leach liquor of dump leaching is raffinate after extracting and additional an amount of sulfuric acid, the used bacterium of dump leaching is that the mixt bacteria of the open-air thiobacillus thiooxidans cultivated of in-site collecting, thiobacillus thioparus, iron protoxide Ferrobacillus, the little Helicobacter pylori of iron protoxide is through cultivating the domestication back as leaching bacterium, the pH value that remains leach liquor in the heap leaching process is 1.0～1.5, to the deep infiltration, spraying intensity is 10～121/ (m to leach liquor from top to bottom
2.h), the spray system is 16 hours sprays, and 8 hours idle, handles with cleaning section in entering when zinc ion concentration reaches 8～12g/l in the heap leaching solution; Perhaps will contain zinc and directly carry out dump leaching less than 15% low-grade zinc oxide ore, the dump leaching time is 8～10 months, the used leach liquor of dump leaching is raffinate after extracting and additional an amount of sulfuric acid, adopt the sulfuric acid slaking when building heap, leach then, the pH value that remains leach liquor in the heap leaching process is 2.0～2.5, and to the deep infiltration, spraying intensity is 10～151/ (m to leach liquor from top to bottom
2.h), the spray system is 16 hours sprays, and 8 hours idle, handles with cleaning section in entering when zinc ion concentration reaches 8～12g/l in the heap leaching solution;
(2) carry out in the oxidation heap leaching solution that leaches and iron purification, oxygenant is industrial Manganse Dioxide, presses Fe in the solution
2+The amount and according to the reaction 2Fe
2++ MnO
2+ 4H
+=2Fe
3++ Mn
2++ 2H
2O carries out theory and consumes metering, calculate by weight consumption and be theoretical amount 1.1～1.2 times, add Wingdale in the oxidation N-process as neutralizing agent, the add-on of Wingdale is calculated by weight to 10～12g/l, the oxidation N-process carries out at ambient temperature, and in the control and the pH value of terminal point be 5.1～5.3, content＜5mg/l of Fe in the scavenging solution, the purification slag after the purification returns the dump leaching operation of zinc oxide ore; The rate of loss that purifies general zinc in the slag is 2～3%;
(3) with the scavenging solution after the deironing with 35～45%P
2O
4The mixed extractant of forming with 55～65% kerosene extracts, extraction conditions is a room temperature, extraction progression is 5～10 grades, the extraction terminal point is in pH=1.0～1.5, and compare (O/A)=1: (1.0～2.0), mixing time are 5～10min, settling time 20～40min, the percentage extraction of zinc is 80～90% during extraction, and the load organic phases of output contains zinc 10～15g/l, and raffinate contains zinc 1.5～3g/l;
(4) the zinciferous load organic phases in extraction back is directly stripped with zinc electrodeposition waste liquid, strip liquor contains zinc 50～55g/l, acid is 130～150g/l, the back extraction condition: back extraction progression is 3～5 grades, compares (O/A)=(3～4): 1, and mixing time is 5～10min, settling time 20～40min, normal temperature, the back extraction ratio of zinc＞99%, the organic phase after the back extraction is returned the front and is made extracted organic phase;
(5) solution after the back extraction carries out removing of organic phase with gac, the consumption of gac is 20～40g/l, granularity-40 order, normal temperature stirs 2～3 hours absorption organic phases down, clean liquid after the absorption organic phase mixes with the electrodeposition waste liquid, and the gelatine content 20～30mg/l in the maintenance mixed solution can carry out the electrodeposition acquisition 1# electricity zinc of zinc.
Beneficial effect of the present invention: the technical process dump leaching is adopted is mixed strainss such as the thiobacillus thiooxidans cultivated of in-site collecting and iron protoxide Ferrobacillus, can effectively leach low-grade zinc, each element and extracted organic phase do not influence the leaching of bacterium in the leaching process, zinc bacterium year leaching yield greater than 80%, the zinc leaching rate of dump leaching is greater than 90% and flow process is short, operation is few, facility simple production cost is low.The extraction decreasing ratio that can make iron in the present invention is greater than 99%, and the concentration of iron is below 5mg/l in the solution, and the rate of loss of zinc is less than 2.5%, for the di (isooctyl) phosphate P of liquid employing after the deironing in the iron removal
2O
4Mix as extraction agent with kerosene, during extraction process does not carry out and free acid, simplified purification process, save production cost.The electrodeposition waste liquid is directly used in back extraction, and the solution after the back extraction carries out electrodeposition can obtain the above cathode zinc of 1#, and current efficiency reaches 91%, and zinc electrodeposition direct current consumption is about 3100kw.h/t.
Description of drawings
The 1st, process flow diagram of the present invention.
Embodiment
Embodiment one
Zinc content is 8% low grade zinc sulfide ore deposit, ore storage proportion 1.30g/cm
3, 1.05t altogether, earlier with ore reduction to building heap below the 25mm, use the sulfuric acid slaking then, and leach.The little Helicobacter pylori mixt bacteria of the thiobacillus thiooxidans from the field, thiobacillus thioparus, iron protoxide Ferrobacillus, iron protoxide with laboratory culture is leached inoculum size 10%.Remain the pH value of solution value in the heap leaching process 1.0～1.5, to the deep infiltration, spraying intensity is 10L/ (m to leach liquor from top to bottom
2.h), the spray system is 16 hours sprays, and 8 hours idle.Leach zine ion mean concns 10.14g/L in the later stage every month heap leaching solution, iron mean concns 4.78g/L, wherein Fe
2+Be 3.45g/L.Through leaching in 12 months, zinc leaching rate reached 82.14%.The dump leaching solution of this leaching adds the industrial Manganse Dioxide 4.92g/L (being 1.1 times of theoretical amount) of 60% grade, and limestone powder 10g/L stirs 3h at ambient temperature, and the pH value of terminal point is 5.15.Fe 2.1mg/L, Zn 9.89g/L in the solution of in the oxidation and back, the rate of loss of zinc is 2.5%., with solution 40%P after this deironing
2O
4Mixing extracts as extraction agent with 60% kerosene.In the extraction process or not and free acid.Extraction conditions is that room temperature, extraction progression are 6 grades, compares (O/A)=1: 1.5, and mixing time is 5min, settling time 30min.Extraction terminal point pH=1.45, the percentage extraction of zinc is 84.21% during extraction, and load organic phases contains zinc 12.49g/L, and raffinate contains zinc 1.56g/L.Load organic phases is directly stripped with zinc electrodeposition waste liquid, and strip liquor contains zinc 52.14g/L, and acid is 140.27g/L.The back extraction condition: back extraction progression is 3 grades, compares (O/A)=3.5: 1, and mixing time is 5min, settling time 25min, normal temperature.The back extraction ratio 99.14% of zinc.Organic phase contains zinc 0.11g/L after the back extraction, and strip liquor contains zinc 95.48g/L.This strip liquor stirred 2.5 hours under the consumption 35g/L, normal temperature with granularity-40 purpose gac, and organic phase is removed substantially in the solution.Mix by 9.8: 1 with useless electric effusion then, and add gelatin 25mg/L, at 500A/m
2, electrodeposition under 40 ℃ and the bath voltage 3.25V condition, obtain 1# zinc, direct current consumption 3167.83kwh/t.
Embodiment two
Zinc content is 7.83% low grade zinc sulfide ore deposit, ore storage proportion 1.31g/cm
3, 16.51t builds heap with ore with being crushed to earlier below the 30mm altogether, uses the sulfuric acid slaking then, and leaches.The bacterium from the field with laboratory culture is leached, inoculum size 15%.Remain the pH value of solution value in the heap leaching process 1.0～1.5, to the deep infiltration, spraying intensity is 12L/ (m to leach liquor from top to bottom
2H), the spray system is 16 hours sprays, and 8 hours idle.Leach zine ion mean concns 11.17g/L in the later stage every month leach liquor, iron mean concns 5.69g/L, wherein Fe
2+Be 3.66g/L.Through leaching in 12 months, zinc leaching rate reached 80.43%.This infusion solution adds industrial Manganse Dioxide (60% grade) 5.70g/L (1.2 times of theoretical amount), and limestone powder 12g/L stirs 3h at ambient temperature, and the pH value of terminal point is 5.23.Fe 1.87mg/L, Zn 10.87g/L in the solution of in the oxidation and back, the rate of loss that purifies zinc in the slag is 2.67%., with solution 40%P after this deironing
2O
4+ 60% kerosene extracts as extraction agent.In the extraction process or not and free acid.Extraction conditions is that room temperature, extraction progression are 8 grades, compares (O/A)=1: 1.4, and mixing time is 5min, settling time 30min.Extraction terminal point pH=1.31, the percentage extraction of zinc is 84.07% during extraction, and load organic phases contains zinc 12.79g/L, and raffinate contains zinc 1.73g/L.Load organic phases is directly stripped with zinc electrodeposition waste liquid, and strip liquor contains zinc 52.11g/L, and acid is 143.47g/L.The back extraction condition: back extraction progression is 2 grades, compares (O/A)=3.0: 1, and mixing time is 5min, settling time 25min, normal temperature.The back extraction ratio 99.08% of zinc.Organic phase contains zinc 0.12g/L after the back extraction, and strip liquor contains zinc 90.13g/L.This strip liquor stirred 3 hours under the consumption 40g/L, normal temperature with granularity-40 purpose gac, and organic phase is removed substantially in the solution.Mix by 8.5: 1 with useless electric effusion then, and add gelatin 30mg/L, at 500A/m
2, electrodeposition under 40 ℃ and the bath voltage 3.27V condition, obtain 1# zinc, direct current consumption 3151.44kwh/t.
Embodiment three
Zinc content is 15% low-grade zinc oxide ore, ore storage proportion 1.26g/cm
3, 1.47t altogether, this zinc oxide ore is an earthy, natural particle size is built heap, uses the sulfuric acid slaking then, and leaches.Remain the pH value of solution value in the heap leaching process 2.0～2.5, to the deep infiltration, spraying intensity is 14.5L/ (m to leach liquor from top to bottom
2.h), the spray system is 16 hours sprays, and 8 hours idle.Leach zine ion mean concns 11.89g/L in per 10 days leach liquors, iron mean concns 4.21g/L, wherein Fe
2+Be 3.87g/L.Through leaching in 10 months, zinc leaching rate reached 92.35%.This infusion solution adds industrial Manganse Dioxide (60% grade) 5.52g/L (1.1 times of theoretical amount), and limestone powder 11g/L stirs 2.5h at ambient temperature, and the pH value of terminal point is 5.19.Fe 1.93mg/L, Zn 11.56g/L in the solution of in the oxidation and back, the rate of loss that purifies slag zinc is 2.81%, with solution 42%P after this deironing
2O
4+ 58% kerosene extracts as extraction agent.In the extraction process or not and free acid.Extraction conditions is that room temperature, extraction progression are 10 grades, compares (O/A)=1: 1.5, and mixing time is 5min, settling time 30min.Extraction terminal point pH=1.11, the percentage extraction of zinc is 85.31% during extraction, and load organic phases contains zinc 14.79g/L, and raffinate contains zinc 1.70g/L.Load organic phases is directly stripped with zinc electrodeposition waste liquid, and strip liquor contains zinc 51.85g/L, and acid is 141.62g/L.The back extraction condition: back extraction progression is 3 grades, compares (O/A)=3.0: 1, and mixing time is 5min, settling time 25min, normal temperature.The back extraction ratio 99.23% of zinc.Organic phase contains zinc 0.11g/L after the back extraction, and strip liquor contains zinc 95.87g/L.This strip liquor stirred 3 hours under the consumption 40g/L, normal temperature with granularity-40 purpose gac, and organic phase is removed substantially in the solution.Mix by 11: 1 with useless electric effusion then, and add gelatin 30mg/L, at 500A/m
2, electrodeposition under 40 ℃ and the bath voltage 3.26V condition, obtain 1# zinc, direct current consumption 3129.44kwh/t.
Embodiment four
Zinc content is 12.17% low-grade zinc oxide ore, ore storage proportion 1.29g/cm
3, 15.13t altogether, this zinc oxide ore are block, are crushed to-below the 30mm, build heap then, use the sulfuric acid slaking again, and leach.Remain the pH value of solution value in the heap leaching process 2.0～2.5, to the deep infiltration, spraying intensity is 12L/ (m to leach liquor from top to bottom
2.h), the spray system is 16 hours sprays, and 8 hours idle.Leach zine ion mean concns 10.12g/L in per 10 days leach liquors, iron mean concns 4.13g/L, wherein Fe
2+Be 3.74g/L.Through leaching in 10 months, zinc leaching rate reached 91.27%.This infusion solution adds industrial Manganse Dioxide (60% grade) 5.82g/L (1.2 times of theoretical amount), and limestone powder 12g/L stirs 3.0h at ambient temperature, and the pH value of terminal point is 5.24.Fe 0.97mg/L, Zn 9.84g/L in the solution of in the oxidation and back, the rate of loss that purifies slag zinc is 2.73%, with solution 38%P after this deironing
2O
4+ 62% kerosene extracts as extraction agent.In the extraction process or not and free acid.Extraction conditions is that room temperature, extraction progression are 10 grades, compares (O/A)=1: 1.8, and mixing time is 5min, settling time 40min.Extraction terminal point pH=1.27, the percentage extraction of zinc is 84.03% during extraction, and load organic phases contains zinc 14.88g/L, and raffinate contains zinc 1.57g/L.Load organic phases is directly stripped with zinc electrodeposition waste liquid, and strip liquor contains zinc 53.16g/L, and acid is 148.27g/L.The back extraction condition: back extraction progression is 3 grades, compares (O/A)=3.5: 1, and mixing time is 5min, settling time 40min, normal temperature.The back extraction ratio 99.47% of zinc.Organic phase contains zinc 0.08g/L after the back extraction, and strip liquor contains zinc 104.96g/L.This strip liquor stirred 3 hours under the consumption 35g/L, normal temperature with granularity-40 purpose gac, and organic phase is removed substantially in the solution.Mix by 12.95: 1 with useless electric effusion then, and add gelatin 20mg/L, at 500A/m
2, electrodeposition under 40 ℃ and the bath voltage 3.23V condition, obtain 1# zinc, direct current consumption 3148.31kwh/t.
Claims (7)
1. method of from low-grade zinc, extracting zinc, to contain zinc less than 8% zinc sulfide ore or contain zinc and be processed into granularity less than 30mm less than 15% zinc oxide ore, build heap, dump leaching, adopt the sulfuric acid slaking when building heap, leach then, electrodeposition obtained electric zinc after the heap leaching solution that leaches carried out enrichment, it is characterized in that:
(1) will contain zinc and carry out the bacterium leaching less than 8% low grade zinc sulfide ore deposit, the dump leaching time is 10～12 months, the used leach liquor of dump leaching also replenishes an amount of sulfuric acid for the raffinate after extracting, and handles with cleaning section in entering when zinc ion concentration reaches 8～12g/l in the heap leaching solution; Perhaps will contain zinc and directly carry out dump leaching less than 15% low-grade zinc oxide ore, the dump leaching time is 8～10 months, the used leach liquor of dump leaching also replenishes an amount of sulfuric acid for the raffinate after extracting, and handles with cleaning section in entering when zinc ion concentration reaches 8～12g/l in the heap leaching solution;
(2) heap leaching solution that leaches is carried out in and iron purification, the oxidation N-process carries out at ambient temperature, and in the controlled oxidation and the pH value of terminal point be 5.1～5.3, content＜5mg/l of Fe in the scavenging solution;
(3) with the scavenging solution after the deironing with 35～45%P
2O
4The mixed extractant of forming with 55～65% kerosene extracts, and extraction conditions is a room temperature, and the load organic phases of output contains zinc 10～15g/l, and raffinate contains zinc 1.5～3g/l;
(4) the zinciferous load organic phases in extraction back is directly stripped with zinc electrodeposition waste liquid, and strip liquor contains zinc 50～55g/l, and acid is 130～150g/l, the back extraction ratio of zinc＞99%, and the organic phase after the back extraction is returned the front and is made extracted organic phase;
(5) solution after the back extraction carries out removing of organic phase with gac, and the clean liquid after the absorption organic phase mixes with the electrodeposition waste liquid, and the gelatine content 20～30mg/l in the maintenance mixed solution can carry out the electrodeposition acquisition 1# electricity zinc of zinc.
2. extract the method for zinc in the low-grade zinc according to claim 1, it is characterized in that: zinc sulfide ore adopts the mixt bacteria dump leaching, used bacterium is the little Helicobacter pylori mixt bacteria of open-air thiobacillus thiooxidans, thiobacillus thioparus, iron protoxide Ferrobacillus, iron protoxide that in-site collecting is cultivated, through cultivating the domestication back as leaching bacterium.
3. extract the method for zinc in the low-grade zinc according to claim 1, it is characterized in that: the pH value that remains leach liquor in the zinc sulfide ore heap leaching process is 1.0～1.5, and to the deep infiltration, spraying intensity is 10～12/ (m to leach liquor from top to bottom
2.h), the spray system is 16 hours sprays, and 8 hours idle.
4. extract the method for zinc in the low-grade zinc according to claim 1, it is characterized in that: the pH value that remains leach liquor in the zinc oxide ore heap leaching process is 2.0～2.5, and to the deep infiltration, spraying intensity is 10～15l/ (m to leach liquor from top to bottom
2.h), the spray system is 16 hours sprays, and 8 hours idle.
5. extract the method for zinc in the low-grade zinc according to claim 1, it is characterized in that: heap leaching solution carries out in the oxidation and deironing, and oxygenant is industrial Manganse Dioxide, presses Fe in the solution
2+The amount and according to reaction formula 2Fe
2++ MnO
2+ 4H
+=2Fe
3++ Mn
2++ 2H
2O carries out theory and consumes metering, calculate by weight consumption and be theoretical amount 1.1～1.2 times; Add Wingdale in the oxidation N-process as neutralizing agent, the add-on of Wingdale is calculated by weight to 10～12g/l, and the purification slag after the purification returns the dump leaching operation of zinc oxide ore.
6. extract the method for zinc in the low-grade zinc according to claim 1, it is characterized in that: back extraction progression is 3～5 grades, compares (O/A)=(3～4): 1, and mixing time is 5～10min, settling time 20～40min.
7. extract the method for zinc in the low-grade zinc according to claim 1, it is characterized in that: the consumption of gac is 20～40g/L, granularity-40 order, and whip attachment organic phase under the normal temperature, churning time are 2～3 hours.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942560A (en) * | 2010-10-15 | 2011-01-12 | 毕节学院 | Method for directly leaching low-grade germanic lead oxide and zinc oxide ores |
| CN102477488A (en) * | 2010-11-29 | 2012-05-30 | 厦门紫金矿冶技术有限公司 | Method for fractional neutralization and extraction of zinc |
| CN103146918A (en) * | 2013-03-29 | 2013-06-12 | 云南金鼎锌业有限公司 | Process for directly producing electrolytic zinc from zinc extraction liquid |
| CN103966448A (en) * | 2014-05-22 | 2014-08-06 | 北京矿冶研究总院 | Method for comprehensively recovering zinc from jarosite slag |
| CN104962755B (en) * | 2015-06-08 | 2017-09-12 | 长沙矿冶研究院有限责任公司 | Flotation of Zinc Oxide concentrate pre-processes extract technology |
| CN105063355B (en) * | 2015-08-18 | 2018-01-05 | 云南驰宏锌锗股份有限公司 | A kind of heap leaching method of lead Zinc oxide |
| CN109943717B (en) * | 2017-12-20 | 2020-09-15 | 有研工程技术研究院有限公司 | Method for comprehensively recovering zinc and iron from high-iron low-zinc sulfuric acid solution |
| CN111519039B (en) * | 2020-04-26 | 2022-02-01 | 郑州大学 | Process method for recovering zinc from low-grade zinc oxide ore |
| CN114672665B (en) * | 2022-03-24 | 2023-08-22 | 中宁县宁华再生资源循环利用科技有限公司 | Processing technology for preparing zinc ingot by electrodeposition method |
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| CA2104736A1 (en) * | 1993-08-24 | 1995-02-25 | Lucy Rosato | Process for high extraction of zinc from zinc ferrites |
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