CN104911349A - Method for one segment leaching recovery of valuable metals in zinc system copper cadmium slag - Google Patents
Method for one segment leaching recovery of valuable metals in zinc system copper cadmium slag Download PDFInfo
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Abstract
The present invention is a method for one segment leaching recovery of valuable metals in zinc system copper cadmium slag, the method comprises the following steps: dissolving copper cadmium slag ore pulp and adjusting PH value, oxidizing with air, completely oxidizing with a strong oxidant, and removing impurities, making copper sponge, displacing zinc and cadmium, producing cadmium sponge and zinc sulfate solution, and the like, and high quality copper sponge, cadmium sponge and zinc sulfate solution can be obtained. By use of the new technology method of addition of the strong oxidant, a lot of zinc and cadmium can be leached into the solution by one segment leaching, copper is left in the slag in the form of copper sponge, the technical process and the reaction time are shortened. The method realizes the efficient comprehensive recovery of zinc, copper and cadmium, and the output product contains few impurities and is high in grade.
Description
Technical field
The present invention relates to and belongs to zinc wet process smelting technique waste residue recovery field, is specifically related to one section and leaches the method reclaiming valuable metal in Zn system copper-cadmium slag.
Background technology
The zinc powder purification copper removal cadmium stage is added at wet zinc-making system, output contains the copper-cadmium slag of valency metallic zinc, copper, cadmium, general containing Zn30% ~ 50%, Cu1% ~ 10%, Cd7% ~ 20%, this wet method slag is smelting intermediate product, direct sale price is cheap, and most of zinc abstraction factory has all carried out synthetical recovery, generally zinc is returned Zn system with zinc sulphate, copper reclaims with sponge copper ashes form, and cadmium reclaims with Spongy Cadmium or pure cadmium ingot forms.
The main method of process copper-cadmium slag can be summarized as two kinds: 1) two sections of lixiviation process: copper-cadmium slag is added waste electrolyte or sulfuric acid carries out two sections of counterflow leachings, Manganse Dioxide is added or pressurized air is oxidized in leaching process, leach liquor sulfur acid zinc and Cadmium Sulphate, send cadmium to replace workshop section and reclaim cadmium, zinc, leached mud is copper ashes; 2) direct leaching: with the sulfuric acid leaching copper-cadmium slag that concentration is high, zinc, copper, cadmium are directly proceeded in solution, and then obtain sponge copper ashes with zinc dust precipitation copper, displacement cadmium obtains Spongy Cadmium, displacement liquid sulfur acid zinc, and retrieval system reclaims zinc.There is following defect in aforesaid method: two sections of lixiviation process long flow paths, speed of response slow (needing 1 ~ 2 day), and Manganse Dioxide consumption is large, and copper ashes grade is low, the impure height of leach liquor; The impure height of leach liquor of direct leaching, and copper is also entered solution by leaching, need consume a large amount of zinc powder to displace copper sponge; Impure high leach liquor need add potassium permanganate and sodium hydroxide be oxidized in and removal of impurities.
Summary of the invention
The object of the invention is to overcome above shortcoming, the invention provides a kind of one section and leach the method reclaiming valuable metal in Zn system copper-cadmium slag, the method shortens technical process and reaction times, and the product impurity of output is few, of high grade.
The object of the invention is to be realized by following technique means, the method is made up of following steps:
A, dissolving regulate pH value: under whipped state, the acid be made up of any one in the waste electrolyte of sulfuric acid, Zn system electrolysis output or mixed solution is added in copper-cadmium slag ore pulp, control pH=0.5 ~ 3, copper-cadmium slag ore pulp is obtain copper-cadmium slag ore pulp after the copper-cadmium slag pulp of wet zinc-making system clean-up stage output when removing the impurity such as copper, cadmium.
B, atmospheric oxidation: pass into pressurized air and add strong mixing and oxidation, pressurized air is the pressurized air of removing carbonic acid gas, and solution is heated to 60 ~ 90 DEG C, and soaking time is 0.5 ~ 4h;
C, strong oxidizer exhaustive oxidation removal of impurities: slowly add strong oxidizer, strong oxidizer can be any one in hydrogen peroxide, potassium permanganate or two kinds, and by the zinc in copper-cadmium slag, the further exhaustive oxidation of cadmium play removal of impurities effect, oxidization time is 0.1 ~ 2h;
D, copper sponge preparation: add the acid be made up of any one in the waste electrolyte of sulfuric acid, Zn system electrolysis output or mixed solution after reaction terminates, control pH=2.5 ~ 4, then filtering solution, obtain zinc cadmium leach liquor and copper sponge.Copper sponge can return chlorine removal from copper residue system and utilize;
E, zinc cadmium are replaced: in zinc cadmium leach liquor, add a certain amount of electric furnace zinc powder, the granularity of electric furnace zinc powder is 100 ~ 400 orders, metallic zinc content is greater than 80%, detect the content of Cd in zinc cadmium leach liquor, then the calculation formula of electric furnace zinc powder add-on is: the metallic zinc content in electric furnace zinc powder amount g/L=0.6 × Cd content g/L ÷ electric furnace zinc powder, carries out cadmium displacement;
Producing of F, Spongy Cadmium and solution of zinc sulfate: filtering solution, obtains solution of zinc sulfate and Spongy Cadmium, and obtain Spongy Cadmium cake after Spongy Cadmium pressure group, solution of zinc sulfate can return Zn system and recycle.
The present invention has the following advantages and effect:
(1) by adding strong oxidizer, only need one section of leaching can leach in solution by a large amount of zinc, cadmium, copper is then stayed in slag, exists with the form of copper sponge, shortens technical process and reaction times.
(2) by first reducing the consumption of point strong oxidizer with atmospheric oxidation, reduce costs, strong oxidizer also plays deimpurity effect, does not therefore need deimpurity operation, further shorten technical process and reaction times.
(3) the copper sponge product cupric obtained is of high grade, directly can return chlorine removal from copper residue system and utilize, replace copper sulfate and zinc powder, save great amount of cost.
(4) obtained the input amount of best zinc by practice, the cadmium in leach liquor can disposablely replace by the electric furnace zinc powder dropping into theoretical amount, and the Spongy Cadmium cake of output is of high grade, impure few, is conducive to follow-up deep processing process.
(5) to replace the solution of zinc sulfate that obtains high, impure few containing zinc for cadmium, can return Zn system and recycle.
(6) rate of recovery of rate of recovery higher copper of the present invention, cadmium, zinc is all greater than 99%.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
The present invention is further illustrated below, but limited the present invention never in any form, based on the conversion that the present invention does, all belongs to protection scope of the present invention.
embodiment one:
A gets the copper-cadmium slag ore pulp 1L of certain smeltery, and its main component crossing filter residue is: Zn 45.68%, Cu 7.28%, Cd 17.59%.Under whipped state, in copper-cadmium slag ore pulp, add sulfuric acid, control pH=1.
B passes into pressurized air and adds strong mixing and oxidation, and solution is heated to 70 DEG C, and soaking time is 1.5h.
C slowly adds hydrogen peroxide 50ml, by the zinc in copper-cadmium slag, cadmium oxidation.Oxidization time is 0.2h.
Add waste electrolyte, control pH=3.5, then filtering solution after D reaction terminates, obtain zinc cadmium leach liquor and copper sponge.Copper sponge main component: Cu 62.25%, Zn 7.56%, Cd 9.12%, can return chlorine removal from copper residue system and utilize.Zinc cadmium leach liquor is 4L, impure low, do not need to add potassium permanganate and sodium hydroxide be oxidized in and removal of impurities, main component: Zn 110.02g/l, Cu 0.11mg/l, Cd 52.55 g/l, As 0.063 mg/l, Sb1.23 mg/l, Fe 0.19mg/l.
E adds 146.65g electric furnace zinc powder in 4L zinc cadmium leach liquor, adds zinc powder gauge and calculates by 0.6 × 52.55g/L ÷ 0.86 × 4, carry out cadmium displacement.The granularity of electric furnace zinc powder is 325 orders, and metallic zinc content is 86%.
F filtering solution, obtains solution of zinc sulfate and Spongy Cadmium.Solution of zinc sulfate main component Zn 146.51g/l, Cu 0.04mg/l, Cd 20.13mg/l, can return Zn system and recycle.Spongy Cadmium cake is obtained, main component Zn 1.91%, Cu 0.052%, Cd 89.19% after Spongy Cadmium pressure group.The rate of recovery of copper, cadmium, zinc is all greater than 99%.
embodiment two:
A gets the copper-cadmium slag ore pulp 1L of certain smeltery, and its main component crossing filter residue is: Zn 45.68%, Cu 7.28%, Cd 17.59%.Under whipped state, in copper-cadmium slag ore pulp, add sulfuric acid, control pH=2.
B passes into pressurized air and adds strong mixing and oxidation, and solution is heated to 90 DEG C, and soaking time is 0.5h.
C slowly adds potassium permanganate 1g, by the zinc in copper-cadmium slag, cadmium oxidation.Oxidization time is 0.6h.
Add sulfuric acid, control pH=3, then filtering solution after D reaction terminates, obtain zinc cadmium leach liquor and copper sponge.Copper sponge main component: Cu 59.19%, Zn 7.19%, Cd 8.91%, can return chlorine removal from copper residue system and utilize.Zinc cadmium leach liquor is 4L, impure low, do not need to add potassium permanganate and sodium hydroxide be oxidized in and removal of impurities, main component: Zn 113.56g/l, Cu 0.19mg/l, Cd 53.89 g/l, As 0.091 mg/l, Sb1.14 mg/l, Fe 0.27mg/l.
E adds 148.67g electric furnace zinc powder in 4L zinc cadmium leach liquor, adds zinc powder gauge and calculates by 0.6 × 553.89g/L ÷ 0.87 × 4, carry out cadmium displacement.The granularity of electric furnace zinc powder is 120 orders, and metallic zinc content is 87%.
F filtering solution, obtains solution of zinc sulfate and Spongy Cadmium.Solution of zinc sulfate main component Zn 149.16g/l, Cu 0.02mg/l, Cd 17.38mg/l, can return Zn system and recycle.Spongy Cadmium cake is obtained, main component Zn 2.28%, Cu 0.046%, Cd 88.16% after Spongy Cadmium pressure group.The rate of recovery of copper, cadmium, zinc is all greater than 99%.
embodiment three:
A gets the copper-cadmium slag ore pulp 1L of certain smeltery, and copper-cadmium slag ore pulp is obtain copper-cadmium slag ore pulp after the copper-cadmium slag pulp of wet zinc-making system clean-up stage output when removing the impurity such as copper, cadmium
,its main component crossing filter residue is: Zn 46.68%, Cu 7.58%, Cd 18.09%.Under whipped state, in copper-cadmium slag ore pulp, add the waste electrolyte of Zn system electrolysis output, control pH=0.5.
B passes into the pressurized air removing carbonic acid gas and adds strong mixing and oxidation, and solution is heated to 60 DEG C, and soaking time is 4h.
C slowly adds hydrogen peroxide 25ml and potassium permanganate 0.5g, by the zinc in copper-cadmium slag, cadmium oxidation.Oxidization time is 0.1h.
Add sulfuric acid, control pH=2.5, then filtering solution after D reaction terminates, obtain zinc cadmium leach liquor and copper sponge.Copper sponge main component: Cu 60.19%, Zn 6.29%, Cd 7.81%, can return chlorine removal from copper residue system and utilize.Zinc cadmium leach liquor is 4L, impure low, do not need to add potassium permanganate and sodium hydroxide be oxidized in and removal of impurities, main component: Zn 135.56g/l, Cu 0.17mg/l, Cd 54.89 g/l, As 0.081 mg/l, Sb1.04 mg/l, Fe 0.37mg/l.
E adds 164.67g electric furnace zinc powder in 4L zinc cadmium leach liquor, adds zinc powder gauge and calculates by 0.6 × 54.89g/L ÷ 0.80 × 4, carry out cadmium displacement.The granularity of electric furnace zinc powder is 100 orders, and metallic zinc content is 80%.
F filtering solution, obtains solution of zinc sulfate and Spongy Cadmium.Solution of zinc sulfate main component Zn 168.25g/l, Cu 0.01mg/l, Cd 15.77mg/l, can return Zn system and recycle.Spongy Cadmium cake is obtained, main component Zn 1.18%, Cu 0.026%, Cd 89.00% after Spongy Cadmium pressure group.The rate of recovery of copper, cadmium, zinc is all greater than 99%.
embodiment four:
A gets the copper-cadmium slag ore pulp 1L of certain smeltery, and copper-cadmium slag ore pulp is obtain copper-cadmium slag ore pulp after the copper-cadmium slag pulp of wet zinc-making system clean-up stage output when removing the impurity such as copper, cadmium
,its main component crossing filter residue is: Zn 47.33%, Cu 6.95%, Cd 17.33%.Under whipped state, in copper-cadmium slag ore pulp, add sulfuric acid, control pH=3.
B passes into the pressurized air removing carbonic acid gas and adds strong mixing and oxidation, and solution is heated to 80 DEG C, and soaking time is 3h.
C slowly adds hydrogen peroxide 50ml, by the zinc in copper-cadmium slag, cadmium oxidation.Oxidization time is 2h.
Add the waste electrolyte of Zn system electrolysis output and the mixed solution of sulfuric acid after D reaction terminates, control pH=4, then filtering solution, obtain zinc cadmium leach liquor and copper sponge.Copper sponge main component: Cu 60.01%, Zn 6.21%, Cd 6.99%, can return chlorine removal from copper residue system and utilize.Zinc cadmium leach liquor is 4L, impure low, do not need to add potassium permanganate and sodium hydroxide be oxidized in and removal of impurities, main component: Zn 131.53g/l, Cu 0.15mg/l, Cd 55.01 g/l, As 0.071 mg/l, Sb1.21mg/l, Fe 0.30mg/l.
E adds 146.69g electric furnace zinc powder in 4L zinc cadmium leach liquor, adds zinc powder gauge and calculates by 0.6 × 55.01g/L ÷ 0.90 × 4, carry out cadmium displacement.The granularity of electric furnace zinc powder is 400 orders, and metallic zinc content is 90%.
F filtering solution, obtains solution of zinc sulfate and Spongy Cadmium.Solution of zinc sulfate main component Zn 169.95g/l, Cu 0.02mg/l, Cd 16.75mg/l, can return Zn system and recycle.Spongy Cadmium cake is obtained, main component Zn 1.07%, Cu 0.015%, Cd 88.76% after Spongy Cadmium pressure group.The rate of recovery of copper, cadmium, zinc is all greater than 99%.
embodiment five:
A gets the copper-cadmium slag ore pulp 1L of certain smeltery, and copper-cadmium slag ore pulp is obtain copper-cadmium slag ore pulp after the copper-cadmium slag pulp of wet zinc-making system clean-up stage output when removing the impurity such as copper, cadmium
,its main component crossing filter residue is: Zn 35.28%, Cu 9.18%, Cd 9.35%.Under whipped state, in copper-cadmium slag ore pulp, add sulfuric acid, control pH=2.
B passes into pressurized air and adds strong mixing and oxidation, and solution is heated to 70 DEG C, and soaking time is 2h.
C slowly adds hydrogen peroxide 50ml, by the zinc in copper-cadmium slag, cadmium oxidation.Oxidization time is 1h.
Add waste electrolyte, control pH=3.2, then filtering solution after D reaction terminates, obtain zinc cadmium leach liquor and copper sponge.Copper sponge main component: Cu 68.24%, Zn 6.46%, Cd 6.12%, can return chlorine removal from copper residue system and utilize.Zinc cadmium leach liquor is 4L, impure low, do not need to add potassium permanganate and sodium hydroxide be oxidized in and removal of impurities, main component: Zn 99.02g/l, Cu 0.12mg/l, Cd 46.53 g/l, As 0.061 mg/l, Sb0.93 mg/l, Fe 0.15mg/l.
E adds 121.38g electric furnace zinc powder in 4L zinc cadmium leach liquor, adds zinc powder gauge and calculates by 0.6 × 46.53g/L ÷ 0.92 × 4, carry out cadmium displacement.The granularity of electric furnace zinc powder is 300 orders, and metallic zinc content is 92%.
F filtering solution, obtains solution of zinc sulfate and Spongy Cadmium.Solution of zinc sulfate main component Zn 108.51g/l, Cu 0.02mg/l, Cd 17.13mg/l, can return Zn system and recycle.Spongy Cadmium cake is obtained, main component Zn 0.91%, Cu 0.042%, Cd 88.56% after Spongy Cadmium pressure group.The rate of recovery of copper, cadmium, zinc is all greater than 99%.
Claims (8)
1. one section is leached the method reclaiming valuable metal in Zn system copper-cadmium slag, it is characterized in that the method is made up of following steps:
A, dissolving regulate pH value: under whipped state, in copper-cadmium slag ore pulp, add acid, control pH=0.5 ~ 3;
B, atmospheric oxidation: pass into pressurized air and add strong mixing and oxidation, and solution is heated to 60 ~ 90 DEG C, soaking time is 0.5 ~ 4h;
C, strong oxidizer exhaustive oxidation removal of impurities: slowly add strong oxidizer, by the zinc in copper-cadmium slag, the further exhaustive oxidation removal of impurities of cadmium, oxidization time is 0.1 ~ 2h;
D, copper sponge preparation: add acid control pH=2.5 ~ 4, then filtering solution after reaction terminates, obtain zinc cadmium leach liquor and copper sponge, copper sponge can return chlorine removal from copper residue system and utilize;
E, zinc cadmium are replaced: in zinc cadmium leach liquor, add a certain amount of electric furnace zinc powder, carry out cadmium displacement;
Producing of F, Spongy Cadmium and solution of zinc sulfate: filter, obtain solution of zinc sulfate and Spongy Cadmium, obtain Spongy Cadmium cake after Spongy Cadmium pressure group, solution of zinc sulfate can return Zn system and recycle.
2. according to claim 1 a kind of one section leach the method reclaiming valuable metal in Zn system copper-cadmium slag, it is characterized in that the copper-cadmium slag ore pulp described in steps A is obtain copper-cadmium slag ore pulp after the copper-cadmium slag pulp of wet zinc-making system clean-up stage output when removing the impurity such as copper, cadmium.
3. according to claim 1 a kind of one section leach the method reclaiming valuable metal in Zn system copper-cadmium slag, it is characterized in that the acid described in steps A and D is any one in the waste electrolyte of sulfuric acid, Zn system electrolysis output or mixed solution.
4. according to claim 1 a kind of one section leach the method reclaiming valuable metal in Zn system copper-cadmium slag, it is characterized in that the strong oxidizer described in step C is any one in hydrogen peroxide, potassium permanganate or two kinds of mixing.
5. the method for valuable metal in Zn system copper-cadmium slag is reclaimed in a kind of one section of leaching according to claim 4, it is characterized in that the add-on of described hydrogen peroxide adds 50ml for often liter of copper-cadmium slag ore pulp, or potassium permanganate add-on adds 1g for often liter of copper-cadmium slag ore pulp, or add 25ml hydrogen peroxide and 0.5g potassium permanganate simultaneously.
6. the method for valuable metal in Zn system copper-cadmium slag is reclaimed in a kind of one section of leaching according to claim 1, and it is characterized in that the granularity of the electric furnace zinc powder described in step e is 100 ~ 400 orders, metallic zinc content is greater than 80%.
7. the method for valuable metal in Zn system copper-cadmium slag is reclaimed in a kind of one section of leaching according to claim 1, it is characterized in that the electric furnace zinc powder add-on described in step e obtains like this: the content detecting cadmium in zinc cadmium leach liquor, then the calculation formula of electric furnace zinc powder add-on is: the metallic zinc content in electric furnace zinc powder amount g/L=0.6 × cadmium content g/L ÷ electric furnace zinc powder.
8. the method for valuable metal in Zn system copper-cadmium slag is reclaimed in a kind of one section of leaching according to claim 1, it is characterized in that the pressurized air described in step B is the pressurized air of removing carbonic acid gas.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105349782A (en) * | 2015-10-26 | 2016-02-24 | 株洲冶炼集团股份有限公司 | Novel efficient xanthate purifying technology |
| CN106011466A (en) * | 2016-05-25 | 2016-10-12 | 白银有色集团股份有限公司 | Method for improving copper slag level in zinc hydrometallurgy process |
| CN107287432A (en) * | 2017-06-23 | 2017-10-24 | 贵州省兴安环保科技有限公司 | Zinc, copper, the method for cadmium are reclaimed in a kind of copper-cadmium slag from zinc hydrometallurgy |
| WO2017193725A1 (en) * | 2016-05-10 | 2017-11-16 | 中国恩菲工程技术有限公司 | System and method for treating cadmium-containing solution |
| CN108893609A (en) * | 2018-06-14 | 2018-11-27 | 青海华信环保科技有限公司 | A method of recycling copper cadmium zinc from copper-cadmium slag obtained by zinc hydrometallurgy |
| CN109161688A (en) * | 2018-09-13 | 2019-01-08 | 白银有色集团股份有限公司 | A method of recycling copper, cadmium from copper-cadmium slag |
| CN110699547A (en) * | 2019-08-23 | 2020-01-17 | 白银有色集团股份有限公司 | Method for recovering zinc and cadmium from waste alkaline residues |
| CN113337713A (en) * | 2021-05-11 | 2021-09-03 | 湖南博一环保科技有限公司 | Method for recovering zinc, lead, indium, cadmium and bismuth from zinc-containing wastewater |
| CN115161491A (en) * | 2022-08-17 | 2022-10-11 | 昆明理工大学 | Method for leaching copper and cadmium slag through ultrasonic-ozone oxidation |
| CN115261622A (en) * | 2022-03-18 | 2022-11-01 | 广西科技师范学院 | Method for recovering high-purity zinc sulfate from copper-cadmium-zinc slag |
| CN115449640A (en) * | 2022-09-05 | 2022-12-09 | 中冶瑞木新能源科技有限公司 | Recovery processing method for separating and purifying copper slag |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105349782A (en) * | 2015-10-26 | 2016-02-24 | 株洲冶炼集团股份有限公司 | Novel efficient xanthate purifying technology |
| WO2017193725A1 (en) * | 2016-05-10 | 2017-11-16 | 中国恩菲工程技术有限公司 | System and method for treating cadmium-containing solution |
| CN106011466A (en) * | 2016-05-25 | 2016-10-12 | 白银有色集团股份有限公司 | Method for improving copper slag level in zinc hydrometallurgy process |
| CN107287432A (en) * | 2017-06-23 | 2017-10-24 | 贵州省兴安环保科技有限公司 | Zinc, copper, the method for cadmium are reclaimed in a kind of copper-cadmium slag from zinc hydrometallurgy |
| CN108893609B (en) * | 2018-06-14 | 2019-12-24 | 青海华信环保科技有限公司 | Method for recovering copper, cadmium and zinc from copper and cadmium slag obtained by zinc hydrometallurgy |
| CN108893609A (en) * | 2018-06-14 | 2018-11-27 | 青海华信环保科技有限公司 | A method of recycling copper cadmium zinc from copper-cadmium slag obtained by zinc hydrometallurgy |
| CN109161688A (en) * | 2018-09-13 | 2019-01-08 | 白银有色集团股份有限公司 | A method of recycling copper, cadmium from copper-cadmium slag |
| CN110699547A (en) * | 2019-08-23 | 2020-01-17 | 白银有色集团股份有限公司 | Method for recovering zinc and cadmium from waste alkaline residues |
| CN113337713A (en) * | 2021-05-11 | 2021-09-03 | 湖南博一环保科技有限公司 | Method for recovering zinc, lead, indium, cadmium and bismuth from zinc-containing wastewater |
| CN115261622A (en) * | 2022-03-18 | 2022-11-01 | 广西科技师范学院 | Method for recovering high-purity zinc sulfate from copper-cadmium-zinc slag |
| CN115261622B (en) * | 2022-03-18 | 2023-11-07 | 广西科技师范学院 | Method for recovering high-purity zinc sulfate from copper-cadmium-zinc slag |
| CN115161491A (en) * | 2022-08-17 | 2022-10-11 | 昆明理工大学 | Method for leaching copper and cadmium slag through ultrasonic-ozone oxidation |
| CN115449640A (en) * | 2022-09-05 | 2022-12-09 | 中冶瑞木新能源科技有限公司 | Recovery processing method for separating and purifying copper slag |
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Application publication date: 20150916 |