CN104263941A - Process for comprehensively recovering valuable metals from electroplating sludge - Google Patents
Process for comprehensively recovering valuable metals from electroplating sludge Download PDFInfo
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- CN104263941A CN104263941A CN201410484290.1A CN201410484290A CN104263941A CN 104263941 A CN104263941 A CN 104263941A CN 201410484290 A CN201410484290 A CN 201410484290A CN 104263941 A CN104263941 A CN 104263941A
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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 process for comprehensively recovering valuable metals from electroplating sludge, and the method comprises the following steps: after dissolving raw materials, filtering the obtained object so as to achieve solid-liquid separation; recovering nickel and copper from filter liquor; putting filter residues into a solution containing 3-5 mol/L of Cl<-1>, adjusting the pH value of the filter residues to 1.0-2.0 by using HCl until the filter residues are dissolved, stirring the obtained object until the obtained object is reacted completely, and filtering the obtained object so as to achieve solid-liquid separation; reducing filter liquor by using a reducing agent, and carrying out filtration and separation on the obtained product; after filter residues are dissolved by using a hydrochloric acid, and sodium chlorate and hydrogen peroxide solutions, carrying out adsorption by using activated gold-absorbing resin, eluting by using eluent, and enriching and recovering gold. The method is applicable to electroplating sludge simultaneously containing metals such as nickel, copper, gold and silver, so that while conventional metals such as nickel and copper are recovered, gold and silver in the electroplating sludge also can be comprehensively recovered. The method has the advantages of low operation cost, strong applicability, large handling capacity, simplicity in operation, small energy consumption, and the like, so that the method is a good method for comprehensively recovering valuable metals from electroplating sludge.
Description
Technical field
The present invention relates to a kind of processing method extracting several valuable metal from electroplating sludge, particularly the electroplating sludge treatment process of a kind of process containing nickel, copper, gold and the multiple valuable metal such as silver-colored.
Background technology
Reclaiming from electroplating sludge and extracting various valuable metal resource is research emphasis both domestic and external always, but because the comparison of ingredients of mud is complicated, such as, containing nickel, copper gold and the various metals such as silver-colored in starting material herein, this gives and extracts valuable metal and add technical difficulty.
At present, the technique reclaiming valuable metal from electroplating sludge is mainly divided into pyrogenic process and wet method:
1. pyrogenic process reclaims: it is a kind of more traditional method that pyrogenic process reclaims.Electroplating sludge through pre-treatments such as removal of impurities, enrichment, oven dry, will add metal target sometimes to increase the metal content in mud, improves smelting efficiency before melting.The flue gas produced in fusion process is entrained with heavy metal and sulfurous gas, need carry out vent gas treatment, and this method power consumption is high, and facility investment is large, and environmental pollution is serious.
2. hydrometallurgic recovery: wet method is first leached by electroplating sludge, and the valuable metal in mud is transformed into metal ion or complexing ion, finally reclaims with metal simple-substance or with the form of metal-salt.Its operational path is: wet-leaching → metal is separated from each other → reclaims.This technique such as to have in cost is low, secondary pollution is little, be applicable to middle and small scale electroplating sludge place at the feature compared with pyrogenic process technology.
Current most domestic reclaims the metal such as nickel, copper in producer's use wet processing recovery electroplating sludge, but for the electroplating sludge simultaneously containing metals such as nickel, copper, gold and silver, not yet has a kind of composite technology, gold recovering and silver while recovery nickel, copper.
Summary of the invention
The object of the present invention is to provide a kind of technique of the valuable metal such as comprehensive recovery nickel, copper, gold and silver from electroplating sludge.
The technical solution used in the present invention is:
From electroplating sludge, a technique for comprehensively recovering valuable metal, comprises the steps:
(1) material dissolution: be added to the water by electroplating sludge waste material, adds strong acid and controls solution ph to 0 ~ 3 in solution, after stirring reaction is complete, adds hydrogen peroxide, stirring reaction;
(2) solution that obtains of filtration step (1), makes solid-liquid separation;
(3) the further filtrate that obtains for the treatment of step (2), reclaims nickel, copper;
(4) filter residue that obtains of step (2) is at Cl
-in the solution of=3 ~ 5mol/L, adjust pH to 1.0 ~ 2.0 to dissolve this slag with HCl, after stirring reaction is complete, filters and make solid-liquid separation;
(5) filtrate that step (4) obtains is reduced with reductive agent, filtering separation, and filtrate cycle uses, and filter residue is raw Ag powder;
(6) with the filter residue that hydrochloric acid, sodium chlorate and hydrogen peroxide solution dissolving step (4) obtain, then with suction gold resin absorption, the elution enriching and recovering gold after activation.
As preferably, in step (1), the ratio of electroplating sludge waste material and water is 1:2 ~ 1:3.
As preferably, step (1) described strong acid is the vitriol oil.
As preferably, in step (1), the add-on of 27% industrial hydrogen peroxide is that raw material per ton adds 30L ~ 50L.
The concrete steps that nickel described in step (3) reclaims are: deironing aluminium → abstraction impurity removal → extracting and separating ambrose alloy → nickel sulfate solution → crystallization obtains nickel sulfate hexahydrate crystal.
The concrete steps that copper reclaims are: deironing aluminium → abstraction impurity removal → extracting and separating ambrose alloy → sulfuric acid back extraction → copper-bath → crystallization obtains copper sulfate crystal.
As preferably, being operating as of deironing aluminium: add alkali and adjust solution ph to 3.5 ~ 4.0 except de-iron aluminium.
Reductive agent described in step (5) is iron powder, zinc powder or aluminium flake.
As preferably, the filter residue that (6) obtain with hydrochloric acid, sodium chlorate and hydrogen peroxide solution dissolving step (4), lysate current potential >900mV keeps 1 hour.
As preferably, the concentration of step (6) described hydrochloric acid, sodium chlorate and hydrogen peroxide solution is respectively: 4mol/L, 1mol/L and 1mol/L.
As preferably, step (6) described elutriant is made up of the thiocarbamide of 7% ~ 15% and the HCl of 1% ~ 5%.
The invention has the beneficial effects as follows:
The method is applicable to the electroplating sludge simultaneously containing metals such as nickel, copper, gold and silver, can while common metal such as recovery nickel, copper etc., synthetical recovery gold and silver wherein.The method has the advantages such as running cost is low, suitability is strong, treatment capacity is large, simple to operate, energy consumption is little, is a kind of better method of comprehensively recovering valuable metal from electroplating sludge.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but be not limited thereto.
embodiment 1
Electroplating sludge waste material metal content: Ni:3.65%, Cu:3.52%, Fe:0.837%, Mn:0.065%, Ag:0.2857%, Au:0.0056%, moisture: 48%.
Electroplating sludge waste material is added water by solid-to-liquid ratio 1:3, and the pH to 1.54 then slowly adding vitriol oil control solution under 80 DEG C of agitation conditions no longer rises, then insulated and stirred 1 hour.After reacting completely, add the metal such as nickel, copper of the non-stripping of 27% industrial hydrogen peroxide oxidation part by 30L/t raw material, then insulated and stirred 1 hour.More than Filter Examination the leaching yield of several metal is respectively Ni:99.91%, Cu:99.14%, Fe:99.99%, Mn:99.99%, Ag:0.0001%, does not detect gold in solution, thus realizes being separated of ambrose alloy and gold and silver.
Solution processes according to the following steps: add adjusting PH with base value to 4.0 except de-iron aluminium → P204 abstraction impurity removal → CP150 extracting and separating ambrose alloy, obtain 143g/L NiSO respectively
4solution, 52g/L CuSO
4solution.NiSO
4solution crystallization obtains electronic-grade NiSO
46H
2o crystal.52g/L CuSO
4solution obtains through electrodeposition the copper coin that copper content is 99.96%.
85 DEG C, pH=1.52, Cl is used under agitation containing gold and silver slag
-=3.5mol/L Industrial Salt solubilize, detects that Ag leaching yield is 99.39% after filtration, Au is without leaching.Containing golden slag under 70 DEG C of agitation conditions, be that 1:8 adds containing golden slag in 3mol/L hydrochloric acid by solid-to-liquid ratio, then in molar ratio for 1:1 slowly adds hydrogen peroxide and sodium chlorate (current potential >900mV keeps 1 hour) simultaneously, keep reaction 1 hour, leaching yield reaches 98.91%.
Ag-containing solution zinc powder reduces, in molar ratio m
zn: m
ag=1.5 slowly add zinc powder, after completion of the reaction Ag concentration <5mg/L in mother liquor.The silver powder obtained obtains the raw Ag powder of argentiferous 94% after dilute hydrochloric acid washing by soaking.In Gold leaching liquid, add the D301G resin after activation by the adsorptive capacity of 250mg/g (doing), adsorb after 5 hours, the adsorption rate of gold is 98.04%.Saturated D301G resin 9% thiocarbamide+3%HCl wash-out, the reduction of elutriant oxalic acid obtains the thick bronze that gold content is 97.51%.
embodiment 2
Electroplating sludge waste material metal content: Ni:3.65%, Cu:3.52%, Fe:0.837%, Mn:0.065%, Ag:0.2857%, Au:0.0056%, moisture: 48%.
Electroplating sludge waste material is added water by solid-to-liquid ratio 1:3, and the pH to 1.42 then slowly adding vitriol oil control solution under 80 DEG C of agitation conditions no longer rises, then insulated and stirred 1 hour.After reacting completely, add the metal such as nickel, copper of the non-stripping of 27% industrial hydrogen peroxide oxidation part by 30L/t raw material, then insulated and stirred 1 hour.More than Filter Examination the leaching yield of several metal is respectively Ni:99.96%, Cu:99.24%, Fe:99.99%, Mn:99.99%, Ag:0.0001%, does not detect gold in solution, thus realizes being separated of ambrose alloy and gold and silver.
Solution processes according to the following steps: add adjusting PH with base value to 3.9 except de-iron aluminium → P204 abstraction impurity removal → CP150 extracting and separating ambrose alloy, obtain 145g/L NiSO respectively
4solution, 54g/L CuSO
4solution.NiSO
4solution crystallization obtains electronic-grade NiSO
46H
2o crystal.54g/L CuSO
4solution obtains through electrodeposition the copper coin that copper content is 99.97%.
85 DEG C, pH=1.64, Cl is used under agitation containing gold and silver slag
-=3.8mol/L Industrial Salt solubilize, detects that Ag leaching yield is 99.39% after filtration, Au is without leaching.Containing golden slag under 70 DEG C of agitation conditions, be that 1:8 adds containing golden slag in 3mol/L hydrochloric acid by solid-to-liquid ratio, then in molar ratio for 1:1 slowly adds hydrogen peroxide and sodium chlorate (current potential >900mV keeps 1 hour) simultaneously, keep reaction 1 hour, leaching yield reaches 98.86%.
Ag-containing solution aluminium flake reduces, in molar ratio m
al: m
ag=2 slowly add aluminium flake, after completion of the reaction Ag concentration <5mg/L in mother liquor.The silver powder obtained obtains the raw Ag powder of argentiferous 94.7% after dilute hydrochloric acid washing by soaking.In Gold leaching liquid, add the D301G resin after activation by the adsorptive capacity of 250mg/g (doing), adsorb after 5 hours, the adsorption rate of gold is 98.14%.Saturated D301G resin 10% thiocarbamide+5%HCl wash-out, the reduction of elutriant oxalic acid obtains the thick bronze that gold content is 97.71%.
embodiment 3
Electroplating sludge waste material metal content: Ni:7.17%, Cu:4.92%, Fe:0.421%, Mn:0.007%, Ag:0.0014%, Au:0.0146%, moisture: 53%.
Raw material is added water by solid-to-liquid ratio 1:3, and the pH to 0.97 then slowly adding vitriol oil control solution under 85 DEG C of agitation conditions no longer rises, then insulated and stirred 1 hour.After reacting completely, add the metal such as nickel, copper of the non-stripping of 27% industrial hydrogen peroxide oxidation part by 35L/t raw material, then insulated and stirred 1 hour.More than Filter Examination the leaching yield of several metal is respectively Ni:99.73%, Cu:99.54%, Fe:99.04%, Mn:99.99%, does not detect gold and silver in solution, thus realizes being separated of ambrose alloy and gold and silver.
Solution processes according to the following steps: add adjusting PH with base value to 3.8 except de-iron aluminium → P204 abstraction impurity removal → CP150 extracting and separating ambrose alloy, obtain 132g/L NiSO respectively
4solution, 57g/L CuSO
4solution.NiSO
4solution crystallization obtains electronic-grade NiSO
46H
2o crystal.57g/L CuSO
4solution obtains through electrodeposition the copper coin that copper content is 99.93%.
Because silver content is too low, this material directly enters to extract gold.By golden slag under 70 DEG C of agitation conditions, be that 1:8 adds containing golden slag in 3mol/L hydrochloric acid by solid-to-liquid ratio, then in molar ratio for 1:1 slowly adds hydrogen peroxide and sodium chlorate (current potential >900mV keeps 1 hour) simultaneously, keep reaction 1 hour, leaching yield reaches 99.18%.
Do by 250mg/g() adsorptive capacity in Gold leaching liquid, add the D301G resin after activation, adsorb after 5 hours, gold adsorption rate reach 98.74%.Saturated D301G resin 9% thiocarbamide+3%HCl wash-out, the reduction of elutriant oxalic acid obtains the thick bronze that gold content is 96.09%.
embodiment 4
Electroplating sludge waste material metal content: Ni:3.97%, Cu:7.91%, Fe:0.112%, Mn:0.219%, Ag:0.4857%, Au:0.0006%, moisture: 61%.Raw material is added water by solid-to-liquid ratio 1:2, and the pH to 1.14 then slowly adding vitriol oil control solution under 80 DEG C of agitation conditions no longer rises, then insulated and stirred 1 hour.After reacting completely, add the metal such as nickel, copper of the non-stripping of 27% industrial hydrogen peroxide oxidation part by 50L/t raw material, then insulated and stirred 1 hour.More than Filter Examination the leaching yield of several metal is respectively Ni:99.24%, Cu:99.03%, Fe:99.99%, Mn:99.99%, Ag:0.0002%, does not detect gold in solution, thus realizes being separated of ambrose alloy and gold and silver.
Solution processes according to the following steps: add alkali and improve pH value to 3.5 except de-iron aluminium → P204 abstraction impurity removal → CP150 extracting and separating ambrose alloy, obtain 137g/L NiSO respectively
4solution, 54g/L CuSO
4solution.NiSO
4solution crystallization obtains electronic-grade NiSO
46H
2o crystal.54g/L CuSO
4solution obtains through electrodeposition the copper coin that copper content is 99.92%.
85 DEG C, pH=1.67, Cl is used under agitation containing gold and silver slag
-=4mol/L Industrial Salt solubilize, the leaching yield detecting Ag is after filtration 99.07%.
Ag-containing solution zinc powder reduces, by m
zn: m
ag=1.5 slowly add zinc powder, after completion of the reaction Ag concentration <5mg/L in mother liquor.The silver powder obtained obtains the raw Ag powder of argentiferous 91.5% after dilute hydrochloric acid washing by soaking.
embodiment 5
Electroplating sludge waste material metal content: Ni:3.97%, Cu:7.91%, Fe:0.112%, Mn:0.219%, Ag:0.4857%, Au:0.0006%, moisture: 61%.Raw material is added water by solid-to-liquid ratio 1:3, and the pH to 1.29 then slowly adding vitriol oil control solution under 80 DEG C of agitation conditions no longer rises, then insulated and stirred 1 hour.After reacting completely, add the metal such as nickel, copper of the non-stripping of 27% industrial hydrogen peroxide oxidation part by 50L/t raw material, then insulated and stirred 1 hour.More than Filter Examination the leaching yield of several metal is respectively Ni:99.14%, Cu:99.17%, Fe:99.99%, Mn:99.99%, Ag:0.0002%, does not detect gold in solution, thus realizes being separated of ambrose alloy and gold and silver.
Solution processes according to the following steps:: add alkali and improve pH value to 3.7 except de-iron aluminium → P204 abstraction impurity removal → CP150 extracting and separating ambrose alloy, obtain 141g/L NiSO respectively
4solution, 53g/L CuSO
4solution.NiSO
4solution crystallization obtains electronic-grade NiSO
46H
2o crystal.54g/L CuSO
4solution obtains through electrodeposition the copper coin that copper content is 99.95%.
85 DEG C, pH=1.52, Cl is used under agitation containing gold and silver slag
-=3.8mol/L Industrial Salt solubilize, the leaching yield detecting Ag is after filtration 99.02%.
Ag-containing solution iron powder reduces, in molar ratio m
zn: m
ag=2 slowly add iron powder, after completion of the reaction Ag concentration <5mg/L in mother liquor.The silver powder obtained obtains the raw Ag powder of argentiferous 92.1% after dilute hydrochloric acid washing by soaking.
Above embodiment is only introduces preferred case of the present invention, to those skilled in the art, not deviating from any apparent changes and improvements of carrying out in the scope of spirit of the present invention, all should be regarded as a part of the present invention.
Claims (10)
1. the technique of comprehensively recovering valuable metal from electroplating sludge, comprises the steps:
(1) material dissolution: be added to the water by electroplating sludge waste material, adds strong acid and controls solution ph to 0 ~ 3 in solution, after stirring reaction is complete, adds hydrogen peroxide, stirring reaction;
(2) solution that obtains of filtration step (1), makes solid-liquid separation;
(3) the further filtrate that obtains for the treatment of step (2), reclaims nickel, copper;
(4) filter residue that obtains of step (2) is at Cl
-in the solution of=3 ~ 5mol/L, adjust pH to 1.0 ~ 2.0 to dissolve this slag with HCl, after stirring reaction is complete, filters and make solid-liquid separation;
(5) filtrate that step (4) obtains is reduced with reductive agent, filtering separation, and filtrate cycle uses, and filter residue is raw Ag powder;
(6) with the filter residue that hydrochloric acid, sodium chlorate and hydrogen peroxide solution dissolving step (4) obtain, then with suction gold resin absorption, the elution enriching and recovering gold after activation.
2. the technique of comprehensively recovering valuable metal from electroplating sludge according to claim 1, is characterized in that, in step (1), the ratio of electroplating sludge waste material and water is 1:2 ~ 1:3.
3. the technique of comprehensively recovering valuable metal from electroplating sludge according to claim 1, is characterized in that, step (1) described strong acid is the vitriol oil.
4. the technique of comprehensively recovering valuable metal from electroplating sludge according to claim 1, is characterized in that, in step (1), the add-on of 27% industrial hydrogen peroxide is that raw material per ton adds 30L ~ 50L.
5. the technique of comprehensively recovering valuable metal from electroplating sludge according to claim 1, it is characterized in that, the concrete steps that nickel described in step (3) reclaims are: deironing aluminium → abstraction impurity removal → extracting and separating ambrose alloy → nickel sulfate solution → crystallization obtains nickel sulfate hexahydrate crystal;
The concrete steps that copper reclaims are: deironing aluminium → abstraction impurity removal → extracting and separating ambrose alloy → sulfuric acid back extraction → copper-bath → crystallization obtains copper sulfate crystal.
6. the technique of comprehensively recovering valuable metal from electroplating sludge according to claim 5, is characterized in that, the technique of deironing aluminium is: add alkali and adjust solution ph to 3.5 ~ 4.0 except de-iron aluminium.
7. the technique of comprehensively recovering valuable metal from electroplating sludge according to claim 1, is characterized in that, the reductive agent described in step (5) is iron powder, zinc powder or aluminium flake.
8. the technique of comprehensively recovering valuable metal from electroplating sludge according to claim 1, it is characterized in that, (6) with the filter residue that hydrochloric acid, sodium chlorate and hydrogen peroxide solution dissolving step (4) obtain, lysate current potential >900mV, keeps 1 hour.
9. the technique of comprehensively recovering valuable metal from electroplating sludge according to claim 1, is characterized in that, the concentration of step (6) described hydrochloric acid, sodium chlorate and hydrogen peroxide solution is respectively: 4mol/L, 1mol/L and 1mol/L.
10. the technique of comprehensively recovering valuable metal from electroplating sludge according to claim 1, is characterized in that, step (6) described elutriant is made up of the thiocarbamide of 7% ~ 15% and the HCl of 1% ~ 5%.
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CN106244811A (en) * | 2016-08-24 | 2016-12-21 | 盛隆资源再生(无锡)有限公司 | The recoverying and utilizing method of the electroplating sludge that a kind of copper iron content is low, stannum nickel content is high |
CN110923456A (en) * | 2019-12-13 | 2020-03-27 | 陕西易莱德新材料科技有限公司 | Method for preparing high-purity copper and copper sulfate by adsorption from copper-plating sludge |
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CN110923456A (en) * | 2019-12-13 | 2020-03-27 | 陕西易莱德新材料科技有限公司 | Method for preparing high-purity copper and copper sulfate by adsorption from copper-plating sludge |
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Address after: 529060 Jiangmen long excellent Industrial Co., Ltd., No. two, 73 East Road, courtesy street, Jianghai District, Guangdong, Jiangmen Applicant after: Jiangmen Chancsun Umicore Industry Co., Ltd. Address before: 529060 Jiangmen long excellent Industrial Co., Ltd., No. two, 73 East Road, courtesy street, Jianghai District, Guangdong, Guangzhou Applicant before: Jiangmen Chancsun Umicore Industry Co., Ltd. |
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