CN101974689A - Method for processing material containing copper - Google Patents
Method for processing material containing copper Download PDFInfo
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- CN101974689A CN101974689A CN2010102913209A CN201010291320A CN101974689A CN 101974689 A CN101974689 A CN 101974689A CN 2010102913209 A CN2010102913209 A CN 2010102913209A CN 201010291320 A CN201010291320 A CN 201010291320A CN 101974689 A CN101974689 A CN 101974689A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a method for processing materials containing copper. The method comprises the following steps: leaching out spongy copper, black copper slag and various solid materials containing copper by using a microbubble copper dissolving device; and respectively producing electrodeposited copper, cupric sulfate, nickel sulfate and other products by using the whirl electrolysis technology and the combined process of extraction, impurity removal, evaporation and crystallization. The method is suitable for processing black copper slag generated in the copper electrolysis purification process, spongy copper generated by nickel electrolysis, and various waste acids containing copper, can be used for comprehensively recycling copper, nickel and other valuable metals in various complex materials containing copper, can also be used for recycling various industrial waste acids, and has the advantages of low operating cost, environment friendliness and the like.
Description
Technical field
The present invention relates to a kind of method of handling smelting process gained waste material, relate in particular to a kind of method of Treatment of Copper material.
Background technology
The various copper-contained material treatment process of smelting process output are more, mainly contain following several:
1, copper sulfate is produced in oxidizing roasting → leaching → evaporation → crystallization.The product purity that this technology obtains is difficult to reach requirement.
2, sulfurization roasting adds sulfuric acid again and leaches, and evaporative crystallization is produced the copper sulfate product after filtration.This technology environmental pollution is more serious, and product purity is difficult to reach requirement.
3, adopt the atmospheric oxidation dissolving, evaporative crystallization is produced the production of copper sulfate product basis, and production efficiency is lower, and the leaching yield of copper is lower.
4, thick copper sulfate and the atomized copper powder with the copper electrolyte output is raw material, by dissolving → leaching → evaporation → crystallization → exsiccant explained hereafter feed and plating grade bluestone product.This technology is had relatively high expectations to raw material, and production cost is higher.
5, adopt dissolving with hydrochloric acid, then with ammonia precipitation process → washing → dissolving → evaporation → crystalline explained hereafter feed grade and common copper sulfate product.But the production cost of this technology is higher.
More than the common issue with that exists of several processing methodes be: the one, environmental pollution is more serious; The 2nd, can not comprehensively reclaim other valuable metals in the copper-contained material; The 3rd, product purity is relatively poor, can not satisfy the high-end user demand; The 4th, production cost is higher, and to the having relatively high expectations of raw material, technology is relatively poor to the adaptability of raw material.
Summary of the invention
In view of this, the purpose of this invention is to provide a kind of method of Treatment of Copper material, this method can address the above problem.
Above-mentioned purpose realizes by following proposal:
A kind of method of Treatment of Copper material is characterized in that, described method comprises the steps:
(1) adopt the molten copper equipment utilization of microvesicle spent acid as infusion solution, in the leaching of no external heat source condition realization solid copper-contained material, by the liquid-solid ratio of the hierarchy of control, the pH value that makes infusion solution is at 1.0-2.0;
(2) infusion solution that obtains of filtration step (1) is removed insoluble substance wherein, obtains settled solution;
(3) 10-50% that will filter back settled solution volume adopts the eddy flow electrolysis tech to produce electro deposited copper;
(4) 50-90% that will filter back settled solution volume adopts chemical subtraction, the separation of solvent extraction deep impurity-removing copper nickel, evaporative crystallization technique to produce the copper sulfate product;
(5) the single nickel salt raffinate of solvent extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate;
And, in step (3), adopt the eddy flow electrolysis tech to produce in the process of electro deposited copper, when copper ion concentration in the solution during, return the leaching operation of step (1) and use as leaching acid less than 10g/L; The mother liquor of producing output in the copper sulfate process in step (4) returns and leaches operation as leaching the acid use.
Method according to above-mentioned is characterized in that, described extraction solvent is the P204 extraction agent, and control solution and the organic 4:1-6:1 that is in a ratio of.
Method according to above-mentioned is characterized in that: in step (1), spent acid is the spent acid that contains copper, nickel, iron, calcium, magnesium, plumbous impurity, and the concentration of acid is at 30-500g/L; Described solid copper-contained material is to comprise copper, nickel, iron contamination to contain the difficult solid materials that leaches mutually.
Method according to above-mentioned is characterized in that, described solid copper-contained material is black copper slag or copper sponge.
According to above-mentioned method, it is characterized in that: in step (3), the 10-50% of described settled solution volume adopts the eddy flow electrolysis tech to produce electro deposited copper, the copper ion concentration scope of solution is 1-110 g/L before the electrolysis, the acid concentration scope is 10-300 g/L, solution can contain a kind of in nickel, iron, calcium, magnesium, lead, arsenic, antimony, the bismuth impurity or some kinds before the electrolysis, and the concentration range of each foreign ion is all at 0.01-10g/L, and current density is controlled at 600-800A/m
2, bath voltage is controlled at 3.0-3.2V; Liquid copper ion concentration scope is 0.05-10g/L behind the electrodeposition.
According to above-mentioned method, it is characterized in that: in step (4), the step that the other 50-90% of described settled solution volume carries out chemical subtraction comprises: adopt time clorox as oxygenant, add-on is 5-6 a times of arsenic content in the solution, pH is at 2.0-2.5 in control, reaction times 2-3 hour, add yellow soda ash then the pH value of solution value is transferred to the 4.0-4.5 after-filtration, remove iron, calcium, magnesium, arsenic impurities in the solution simultaneously with the form of ferric arsenate, Tricalcium arsenate magnesium.
Method according to above-mentioned is characterized in that: in step (3), the solution copper ion concentration returns the leaching operation and does leaching acid use behind the electrodeposition when 1-10 g/L.
This method is applicable to the black copper slag of cupric electrolysis scavenging process output, the copper sponge of nickel electrowinning generation and the processing of various copper-containing waste acids, valuable metals such as the copper in both can the various complicated copper-contained materials of comprehensive reutilization, nickel, again can the various industrial waste acids of recycle, and advantage such as it is low to have running cost, environmentally friendly.
Embodiment
Embodiment 1
The copper electrolyte (vitriolic concentration is 180 g/L) that in the molten bronze, brass or copper ware of microvesicle, adds the cupric electrolysis output, add the copper sponge of smelting output then and leach reaction, the concentration that the reaction end solution acid is leached in control is 20 g/L, copper ion concentration is 80 g/L, then solution is filtered, obtain as clear as crystal filtered liquid, 50% of the liquor capacity after the filtration adopts the eddy flow electrolysis tech to produce electro deposited copper, and current density is controlled at 600-800A/m
2, bath voltage is controlled at 3.0-3.2V, and when copper ion concentration is reduced to 10 g/L, sulfuric acid concentration is to 115 g/L, liquid behind this part electrodeposition returned leach operation and recycle as leaching acid; Filter other 50% of back solution and add hypochlorite oxidation, pH is at 2.0-2.5 in control, reaction times 2-3 hour, add yellow soda ash then pH value of solution is transferred to the 4.0-4.5 after-filtration, impurity such as arsenic in the solution, iron, calcium, magnesium are removed with forms such as ferric arsenate, Tricalcium arsenates, and the decreasing ratio of arsenic is more than 98%; Solution after will filtering then carries out solvent extraction removal of impurities (using the P204 extraction agent), control solution and the organic 6:1 that is in a ratio of, load is organic to be that the sulfuric acid of 2.5N is stripped as back extraction acid with hydrogen ion concentration, obtains copper ion concentration and be the copper sulfate strip liquor about 90 g/L; Evaporative crystallization obtains the copper sulfate product then, and the mother liquor after the evaporation returns and leaches process configurations leaching acid; The single nickel salt raffinate of P204 extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate.
Embodiment 2
Liquid (vitriolic concentration is 115 g/L) after the electrolysis of adding eddy flow electrolytic process output in the molten bronze, brass or copper ware of microvesicle, the black copper slag that adds copper smelting electrolytic cleaning process output then leaches reaction, the concentration that the reaction end solution acid is leached in control is 30 g/L, copper ion concentration is 65 g/L, then solution is filtered, obtain as clear as crystal filtered liquid, 50% of the liquor capacity after the filtration adopts the eddy flow electrolysis tech to produce electro deposited copper, and current density is controlled at 600-800A/m
2, bath voltage is controlled at 3.0-3.2V, and when copper ion concentration is reduced to 5 g/L, sulfuric acid concentration is raised to 120 g/L, liquid behind this part electrodeposition is returned leach operation and recycle as leaching acid; The another part that filters back solution adds hypochlorite oxidation, pH is at 2.0-2.5 in control, reaction times 2-3 hour, add yellow soda ash then pH value of solution is transferred to the 4.0-4.5 after-filtration, impurity such as arsenic in the solution, iron, calcium, magnesium are removed with forms such as ferric arsenate, Tricalcium arsenates, and the decreasing ratio of arsenic is more than 98%; Solution after will filtering then carries out solvent extraction removal of impurities (using the P204 extraction agent), control solution and the organic 6:1 that is in a ratio of, load is organic to be that the sulfuric acid of 3.0N is stripped as back extraction acid with hydrogen ion concentration, obtains copper ion concentration and be the copper sulfate strip liquor about 90 g/L; Evaporative crystallization obtains the copper sulfate product then, and the mother liquor after the evaporation returns and leaches process configurations leaching acid; The single nickel salt raffinate of P204 extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate.
Embodiment 3
The wet dust collector liquid (vitriolic concentration is 300 g/L) that in the molten bronze, brass or copper ware of microvesicle, adds copper fusion process output, add the copper sponge of smelting output then and leach reaction, the concentration that the reaction end solution acid is leached in control is 10 g/L, copper ion concentration is 100 g/L, then solution is filtered, obtain as clear as crystal filtered liquid, 10% of the liquor capacity after the filtration adopts the eddy flow electrolysis tech to produce electro deposited copper, and current density is controlled at 800A/m
2, bath voltage is controlled at 3.0-3.2V, and when copper ion concentration is reduced to 0.05 g/L, sulfuric acid concentration is to 160 g/L, liquid behind this part electrodeposition returned leach operation and recycle as leaching acid; Filter other 90% of back solution and add hypochlorite oxidation, pH is at 2.0-2.5 in control, reaction times 2-3 hour, add yellow soda ash then pH value of solution is transferred to the 4.0-4.5 after-filtration, impurity such as arsenic in the solution, iron, calcium, magnesium are removed with forms such as ferric arsenate, Tricalcium arsenates, and the decreasing ratio of arsenic is more than 98%; Solution after will filtering then carries out solvent extraction removal of impurities (using the P204 extraction agent), control solution and the organic 6:1 that is in a ratio of, load is organic to be that the sulfuric acid of 2.8N is stripped as back extraction acid with hydrogen ion concentration, obtains copper ion concentration and be the copper sulfate strip liquor about 90 g/L; Evaporative crystallization obtains the copper sulfate product then, and the mother liquor after the evaporation returns and leaches process configurations leaching acid; The single nickel salt raffinate of P204 extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate.
Embodiment 4
In the molten bronze, brass or copper ware of microvesicle, add the electrodeposition raffinate (vitriolic concentration is 90g/L) of producing electrolytic copper powder process output, the black copper slag that adds copper smelting electrolytic cleaning process output then leaches reaction, the concentration that the reaction end solution acid is leached in control is 20 g/L, copper ion concentration is 50 g/L, then solution is filtered, obtain as clear as crystal filtered liquid, 30% of the liquor capacity after the filtration adopts the eddy flow electrolysis tech to produce electro deposited copper, and current density is controlled at 600A/m
2, bath voltage is controlled at 3.0-3.2V, and when copper ion concentration is reduced to 10g/L, sulfuric acid concentration is to 80g/L, liquid behind this part electrodeposition returned leach operation and recycle as leaching acid; 70% adding hypochlorite oxidation of back liquor capacity will be filtered, pH is at 2.0-2.5 in control, reaction times 2-3 hour, add yellow soda ash then pH value of solution is transferred to the 4.0-4.5 after-filtration, impurity such as arsenic in the solution, iron, calcium, magnesium are removed with forms such as ferric arsenate, Tricalcium arsenates, and the decreasing ratio of arsenic is more than 98%; Solution after will filtering then carries out solvent extraction removal of impurities (using the P204 extraction agent), control solution and the organic 6:1 that is in a ratio of, load is organic to be that the sulfuric acid of 2.5N is stripped as back extraction acid with hydrogen ion concentration, obtains copper ion concentration and be the copper sulfate strip liquor about 80 g/L; Evaporative crystallization obtains the copper sulfate product then, and the mother liquor after the evaporation returns and leaches process configurations leaching acid; The single nickel salt raffinate of P204 extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate.
Embodiment 5
The copper electrolyte (vitriolic concentration is 180 g/L) that in the molten bronze, brass or copper ware of microvesicle, adds the cupric electrolysis output, add the copper sponge of smelting output then and leach reaction, the concentration that the reaction end solution acid is leached in control is 20 g/L, copper ion concentration is 80 g/L, then solution is filtered, obtain as clear as crystal filtered liquid, 50% of the liquor capacity after the filtration adopts the eddy flow electrolysis tech to produce electro deposited copper, and current density is controlled at 600A/m
2, bath voltage is controlled at 3.0-3.2V, and when copper ion concentration is reduced to 10 g/L, sulfuric acid concentration is raised to 115 g/L, liquid behind this part electrodeposition is returned leach operation and recycle as leaching acid; Filter other 50% of back solution and add hypochlorite oxidation, PH is at 2.0-2.5 in control, reaction times 2-3 hour, add yellow soda ash then solution PH is transferred to 4.0 after-filtration, impurity such as arsenic in the solution, iron, calcium, magnesium are removed with forms such as ferric arsenate, Tricalcium arsenates; Solution after will filtering then carries out solvent extraction removal of impurities (using the P204 extraction agent), control solution and the organic 4:1 that is in a ratio of, load is organic to be that the sulfuric acid of 2.5N is stripped as back extraction acid with hydrogen ion concentration, obtains copper ion concentration and be the copper sulfate strip liquor about 100 g/L; Evaporative crystallization obtains the copper sulfate product then, and the mother liquor after the evaporation returns and leaches process configurations leaching acid; The single nickel salt raffinate of P204 extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate.
Embodiment 6
Liquid (vitriolic concentration is 115 g/L) after the electrolysis of adding eddy flow electrolytic process output in the molten bronze, brass or copper ware of microvesicle, the black copper slag that adds copper smelting electrolytic cleaning process output then leaches reaction, the concentration that the reaction end solution acid is leached in control is 30 g/L, copper ion concentration is 65 g/L, then solution is filtered, obtain as clear as crystal filtered liquid, 50% of the liquor capacity after the filtration adopts the eddy flow electrolysis tech to produce electro deposited copper, and current density is controlled at 800A/m
2, bath voltage is controlled at 3.2V, and when copper ion concentration is reduced to 5 g/L, sulfuric acid concentration is raised to 120 g/L, liquid behind this part electrodeposition is returned leach operation and recycle as leaching acid; The another part that filters back solution adds hypochlorite oxidation, PH is at 2.0-2.5 in control, reaction times 2-3 hour, add yellow soda ash then solution PH is transferred to 4.5 after-filtration, impurity such as arsenic in the solution, iron, calcium, magnesium are removed with forms such as ferric arsenate, Tricalcium arsenates; Solution after will filtering then carries out solvent extraction removal of impurities (using the P204 extraction agent), control solution and the organic 5:1 that is in a ratio of, load is organic to be that the sulfuric acid of 3.0N is stripped as back extraction acid with hydrogen ion concentration, obtains copper ion concentration and be the copper sulfate strip liquor about 90 g/L; Evaporative crystallization obtains the copper sulfate product then, and the mother liquor after the evaporation returns and leaches process configurations leaching acid; The single nickel salt raffinate of P204 extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate.
Embodiment 7
The copper electrolyte (vitriolic concentration is 180 g/L) that in the molten bronze, brass or copper ware of microvesicle, adds the cupric electrolysis output, add the copper sponge of smelting output then and leach reaction, the concentration that the reaction end solution acid is leached in control is 20 g/L, copper ion concentration is 80 g/L, then solution is filtered, obtain as clear as crystal filtered liquid, 50% of the liquor capacity after the filtration adopts the eddy flow electrolysis tech to produce electro deposited copper, and current density is controlled at 600A/m
2, bath voltage is controlled at 3.0V, and when copper ion concentration is reduced to 10 g/L, sulfuric acid concentration is raised to 115 g/L, liquid behind this part electrodeposition is returned leach operation and recycle as leaching acid; Filter other 50% of back solution and add hypochlorite oxidation, PH is 2.0 in control, 3 hours reaction times, and add yellow soda ash then solution PH is transferred to 4.0 after-filtration, impurity such as arsenic in the solution, iron, calcium, magnesium are removed with forms such as ferric arsenate, Tricalcium arsenates; Solution after will filtering then carries out solvent extraction removal of impurities (using the P204 extraction agent), control solution and the organic 6:1 that is in a ratio of, load is organic to be that the sulfuric acid of 2.5N is stripped as back extraction acid with hydrogen ion concentration, obtains copper ion concentration and be the copper sulfate strip liquor about 100 g/L; Evaporative crystallization obtains the copper sulfate product then, and the mother liquor after the evaporation returns and leaches process configurations leaching acid; The single nickel salt raffinate of P204 extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate.
Embodiment 8
The copper electrolyte (vitriolic concentration is 180 g/L) that in the molten bronze, brass or copper ware of microvesicle, adds the cupric electrolysis output, add the copper sponge of smelting output then and leach reaction, the concentration that the reaction end solution acid is leached in control is 20 g/L, copper ion concentration is 80 g/L, then solution is filtered, obtain as clear as crystal filtered liquid, 50% of the liquor capacity after the filtration adopts the eddy flow electrolysis tech to produce electro deposited copper, and current density is controlled at 800A/m
2, bath voltage is controlled at 3.2V, and when copper ion concentration is reduced to 10 g/L, sulfuric acid concentration is raised to 115 g/L, liquid behind this part electrodeposition is returned leach operation and recycle as leaching acid; Filter other 50% of back solution and add hypochlorite oxidation, PH is 2.5 in control, 2 hours reaction times, and add yellow soda ash then solution PH is transferred to 4.0 after-filtration, impurity such as arsenic in the solution, iron, calcium, magnesium are removed with forms such as ferric arsenate, Tricalcium arsenates; Solution after will filtering then carries out solvent extraction removal of impurities (using the P204 extraction agent), control solution and the organic 6:1 that is in a ratio of, load is organic to be that the sulfuric acid of 2.5N is stripped as back extraction acid with hydrogen ion concentration, obtains copper ion concentration and be the copper sulfate strip liquor about 100 g/L; Evaporative crystallization obtains the copper sulfate product then, and the mother liquor after the evaporation returns and leaches process configurations leaching acid; The single nickel salt raffinate of P204 extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate.
Claims (7)
1. the method for a Treatment of Copper material is characterized in that, described method comprises the steps:
(1) adopt the molten copper equipment utilization of microvesicle spent acid as infusion solution, in the leaching of no external heat source condition realization solid copper-contained material, by the liquid-solid ratio of the hierarchy of control, the pH value that makes infusion solution is at 1.0-2.0;
(2) infusion solution that obtains of filtration step (1) is removed insoluble substance wherein, obtains settled solution;
(3) 10-50% that will filter back settled solution volume adopts the eddy flow electrolysis tech to produce electro deposited copper;
(4) 50-90% that will filter back settled solution volume adopts chemical subtraction, the separation of solvent extraction deep impurity-removing copper nickel, evaporative crystallization technique to produce the copper sulfate product;
(5) the single nickel salt raffinate of solvent extraction process output adopts yellow soda ash precipitation preparation nickelous carbonate;
And, in step (3), adopt the eddy flow electrolysis tech to produce in the process of electro deposited copper, when copper ion concentration in the solution during, return the leaching operation of step (1) and use as leaching acid less than 10g/L; The mother liquor of producing output in the copper sulfate process in step (4) returns and leaches operation as leaching the acid use.
2. method according to claim 1 is characterized in that, described extraction solvent is the P204 extraction agent, and control solution and the organic 4:1-6:1 that is in a ratio of.
3. method according to claim 1 is characterized in that: in step (1), spent acid is the spent acid that contains copper, nickel, iron, calcium, magnesium, plumbous impurity, and the concentration of acid is at 30-500g/L; The solid copper-contained material is to comprise copper, nickel, iron contamination to contain the difficult solid materials that leaches mutually.
4. method according to claim 3 is characterized in that, described solid copper-contained material is black copper slag or copper sponge.
5. method according to claim 1, it is characterized in that: in step (3), the 10-50% of described settled solution volume adopts the eddy flow electrolysis tech to produce electro deposited copper, the copper ion concentration scope of solution is 1-110 g/L before the electrolysis, the acid concentration scope is 10-300 g/L, solution can contain a kind of in nickel, iron, calcium, magnesium, lead, arsenic, antimony, the bismuth impurity or some kinds before the electrolysis, and the concentration range of each foreign ion is all at 0.01-10g/L, and current density is controlled at 600-800A/m
2, bath voltage is controlled at 3.0-3.2V; Liquid copper ion concentration scope is 0.05-10g/L behind the electrodeposition.
6. method according to claim 1, it is characterized in that: in step (4), the step that the other 50-90% of described settled solution volume carries out chemical subtraction comprises: adopt time clorox as oxygenant, add-on is 5-6 a times of arsenic content in the solution, pH is at 2.0-2.5 in control, reaction times 2-3 hour, add yellow soda ash then the pH value of solution value is transferred to the 4.0-4.5 after-filtration, remove iron, calcium, magnesium, arsenic impurities in the solution simultaneously with the form of ferric arsenate, Tricalcium arsenate magnesium.
7. method according to claim 1 is characterized in that: in step (3), the solution copper ion concentration returns the leaching operation and does leaching acid use behind the electrodeposition when 1-10 g/L.
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| CN102242268A (en) * | 2011-06-15 | 2011-11-16 | 金川集团有限公司 | Process for treating black copper slag through electrolytic method |
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| CN102634668A (en) * | 2012-05-04 | 2012-08-15 | 昆明理工大学 | Roasting-free evaporation-free method for producing cupric sulfate from zinc hydrometallurgy acid-wash copper dross |
| CN102758091A (en) * | 2012-07-18 | 2012-10-31 | 中国瑞林工程技术有限公司 | Treatment method for electroplating sludge |
| CN103184333A (en) * | 2011-12-30 | 2013-07-03 | 北京有色金属研究总院 | High grade copper oxide-containing material sulfuric acid leaching and stage extraction technology |
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| CN104047022A (en) * | 2014-06-09 | 2014-09-17 | 广东省工业技术研究院(广州有色金属研究院) | Electrolyzing and recovering method for copper in waste diamond cutter |
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| CN111501065A (en) * | 2020-04-27 | 2020-08-07 | 阳谷祥光铜业有限公司 | Method for purifying copper electrolyte |
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Application publication date: 20110216 |