CN105018738A - Method for recovering Cu, Cd, Ni, Co and Zn from copper-cadmium slag - Google Patents
Method for recovering Cu, Cd, Ni, Co and Zn from copper-cadmium slag Download PDFInfo
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- CN105018738A CN105018738A CN201510409145.1A CN201510409145A CN105018738A CN 105018738 A CN105018738 A CN 105018738A CN 201510409145 A CN201510409145 A CN 201510409145A CN 105018738 A CN105018738 A CN 105018738A
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Abstract
The invention provides a method for recovering Cu, Cd, Ni, Co and Zn from copper-cadmium slag. The copper-cadmium slag is subjected to two times of oxidizing acid leaching, and Cu is extracted from leach liquor; after Fe in raffinate is removed through neutralization oxidation, Ni and Co are precipitated through cobalt purification reagents, and Co and Ni concentrate is obtained through calcinations; after liquor obtained after Co precipitation is subjected to activated carbon adsorption, an electrolytic metal zinc plate is used for replacing spongy cadmium, and a metal cadmium ingot is obtained through melting; and liquor after replacement is delivered to a zinc electrolyzing system. H2SO4 leaching is adopted during the two times of oxidizing acid leaching, and the final PH value after the first time of oxidizing acid leaching is 2 to 3; in the second time of oxidizing acid leaching, the concentration is 50-100 g/L, time is 2 hours, and an oxidizing agent is MnO2 of 5-10% or H2O2 of 5-10%; extraction agents of copper are Cp180 of 20-40% and kerosene of 60-80%, the extraction PH value is 2 to 3, the concentration of reverse extraction H2SO4 is 250-300 g/L, and three levels of extraction, two levels of reverse extraction and two levels of regeneration from washing are carried out; the amount of the cobalt purification reagents is 1.2-1.4 times the sum of the content of Co and the content of Ni, and the temperature ranges from 50 DEG C to 60 DEG C; the replacement PH value of the spongy cadmium is 3 to 4, and the temperature ranges from 40 DEG C to 50 DEG C. According to the method, the process is short, and the recovery rate is high.
Description
Technical field
The invention belongs to technical field of wet metallurgy, particularly a kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag.
Background technology
The copper-cadmium slag of zinc hydrometallurgy output generally all contains o.5% above Cu, the Cd of more than 2%, o.2% above Ni, the Co of more than 0.03%, the Zn. of more than 40% is along with the prolongation of shelf-time, and all main form with the state of oxidation and vitriol of Cu, Cd, Ni, Co, Zn exists, and is easy to by H
2sO
4leach.Traditional technique first carries out meutral innersion PH5.2 ~ 5.4, first leaches Zn, Cd, then carry out acidleach Cu, Co, a Ni, but facts have proved, also have considerable part Cu at neutral leaching stage, Co, Ni leached, and acid leaching stage Zn and Cd is also higher, does not also reach the requirement of selectively leaching.When therefore using the Cd in zinc dust precipitation in immersion liquid, Cu, Co, Ni are also replaced and produce new copper-cadmium slag, cause the loss of Cu, Co, Ni and can not be separated.The consumption of zinc powder reaches more than 2 times of displacement metal, and the Spongy Cadmium displaced is containing Cd 20 ~ 30%, and reach more than 30 containing Zn, this Spongy Cadmium dissolves again, purify and carry out electrolytic metal cadmium, long flow path, the rate of recovery is low.
In order to overcome the shortcoming of traditional technology, someone have studied with the first extracting copper of extraction agent in the pickling liquor after middle leaching, then with zinc dust precipitation Spongy Cadmium to improve the quality of Spongy Cadmium.This technique just adds the extraction and separation technology of Cu in traditional technology, and still adopts high/low temperature zinc dust precipitation technology to Co, Ni, Cd, thus still there is separation to Co, Ni, Cd not thorough, long flow path, Cu, Cd, Co, Ni
,the shortcoming that the Zn rate of recovery is not high.For simplification of flowsheet has people to adopt vacuum distillation technique to process copper-cadmium slag to scheme first to boil off Zn-Cd alloy, enrichment Cu, Co, Ni slag.But because the Spongy Cadmium in copper-cadmium slag mainly exists with sulphate form, and seldom steam, can not be separated.Even the Spongy Cadmium that fresh Spongy Cadmium slag, zinc dust precipitation go out is very easily oxidized or sulfation also.The vacuum steam rate of cadmium also only has about 5%.Cu, Cd, Co, Ni
,zn still needs wet processing.
Summary of the invention
The object of the present invention is to provide a kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, the method flow process is short, Cu, Cd, Co, Ni
,zn Separation and Recovery rate is high, and waste residue amount is few, and waste water is few, and production cost is low, remarkable in economical benefits.
Object of the present invention and solve its technical problem underlying and realize by the following technical solutions:
A kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, it is characterized in that: by copper-cadmium slag through twice oxidation acid leaching, leach liquor extracting Cu, after removing Fe with oxidation in raffinate, Ni, Co is precipitated with except cobalt agent, and calcining to obtain Co, Ni concentrate, after heavy Co, liquid to obtain metal cadmium ingot, displaced liquid power transmission solution Zn system with electrolysis metallic zinc sheet displacement Spongy Cadmium is also molten after charcoal absorption.
A kind of described method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: twice oxidation acid leaching is H
2sO
4leach, it is 2 ~ 3 that first time leaches terminal pH value; Second time is 50 ~ 100g/L, and the time is 2 hours, and oxygenant is the MnO of 5 ~ 10%
2or the H of 5 ~ 10%
2o
2, the leaching yield of Cu, Cd, Ni, Co, Zn is more than 98%.
A kind of described method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: the extraction agent of copper is the Cp180 of 20 ~ 40%, the kerosene of 60 ~ 80%, extraction pH value is 2 ~ 3, back extraction H
2sO
4be 250 ~ 300g/L, three grades of extractions, secondary back extraction, two-stage regenerated from washing.
A kind of above-mentioned method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: regenerated from washing liquid is the NH of 5 ~ 10%
4hCO
3or NH
4oH.
A kind of described method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: the consumption except cobalt agent is 1.2 ~ 1.4 multiples of Co, Ni content sum; Temperature is 50 ~ 60 DEG C, time 2 h, and heavy Co, Ni slag is 500 ± 50 DEG C of calcinings, and Co, Ni concentrate is more than 15% containing Co, is more than 30% containing Ni.
A kind of described method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: the displacement carrying out Spongy Cadmium with electrolytic zinc plate, displacement pH value 3 ~ 4, temperature 40 ~ 50 DEG C, Spongy Cadmium is greater than 70% containing Cd, is less than 5% containing Zn.
A kind of above-mentioned method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: the Spongy Cadmium cake of press of gained is also with NaOH alkali fusion ingot casting, and the cadmium metal quality of gained is more than 99%.
The present invention compared with prior art has obvious advantage and beneficial effect.From above technical scheme, the present invention has following characteristics:
1, twice H
2sO
4oxidation Leaching fully can leach Cu, Cd, Co, Ni
,zn reaches more than 98%.
2, use Cp180 when PH2 ~ 3, normal temperature extracting Cu reaches more than 99%.
3, neutralization oxidation is used except cobalt agent precipitate C o, Ni except after Fe, and reduce the consumption except cobalt agent, the grade that improve Co, Ni concentrate reaches more than Ni30%, more than Co15%.
4, described separation of C u, Co, Ni
,spongy Cadmium is replaced with electrolytic zinc plate when PH3 ~ 4 after Fe, the consumption of zinc metal sheet is 0.5 ~ 0.8 times of cadmium amount, Spongy Cadmium reaches more than 70% containing Cd, 5% is less than containing Zn, greatly reduce the cost of metallic zinc displacement Spongy Cadmium, substantially increase the quality of Spongy Cadmium, thus the quality that improve cast metal cadmium reaches more than 99%.
5, flow process is short, Cu, Cd, Co, Ni
,zn Separation and Recovery rate is high, and waste residue amount is few, and about 5 ~ 10%, waste water is few, and production cost is low, remarkable in economical benefits.
Accompanying drawing explanation
Fig. 1 is present invention process schema.
Embodiment
Below in conjunction with accompanying drawing and preferred embodiment, to a kind of method embodiment, feature and the effect thereof reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag proposed according to the present invention, be described in detail as follows.
See Fig. 1, a kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, it is characterized in that: by copper-cadmium slag through twice oxidation acid leaching, leach liquor extracting Cu, after removing Fe with oxidation in raffinate, precipitate Ni, Co with except cobalt agent, and calcine to obtain Co, Ni concentrate, after heavy Co, liquid to obtain metal cadmium ingot, displaced liquid power transmission solution Zn system with electrolysis metallic zinc sheet displacement Spongy Cadmium is also molten after charcoal absorption.
A kind of described method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: twice oxidation acid leaching is H
2sO
4leach, it is 2 ~ 3 that first time leaches terminal pH value; Second time is 50 ~ 100g/L, and the time is 2 hours, and oxygenant is the MnO of 5 ~ 10%
2or the H of 5 ~ 10%
2o
2, the leaching yield of Cu, Cd, Ni, Co, Zn is more than 98%.
A kind of described method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: the extraction agent of copper is the Cp180 of 20 ~ 40%, the kerosene of 60 ~ 80%, extraction pH value is 2 ~ 3, back extraction H
2sO
4be 250 ~ 300g/L, three grades of extractions, secondary back extraction, two-stage regenerated from washing.
A kind of above-mentioned method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: regenerated from washing liquid is the NH of 5 ~ 10%
4hCO
3or NH
4oH.
A kind of described method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: the consumption except cobalt agent is 1.2 ~ 1.4 multiples of Co, Ni content sum; Temperature is 50 ~ 60 DEG C, time 2 h, and heavy Co, Ni slag is 500 ± 50 DEG C of calcinings, and Co, Ni concentrate is more than 15% containing Co, is more than 30% containing Ni.
A kind of described method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: the displacement carrying out Spongy Cadmium with electrolytic zinc plate, displacement pH value 3 ~ 4, temperature 40 ~ 50 DEG C, Spongy Cadmium is greater than 70% containing Cd, is less than 5% containing Zn.
A kind of above-mentioned method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag, wherein: the Spongy Cadmium cake of press of gained is also with NaOH alkali fusion ingot casting, and the cadmium metal quality of gained is more than 99%.
Embodiment:
Step 1, uses H
2sO
4at 80 ~ 90 DEG C, manganese mineral powder 10% or H
2o
25%, Gu liquid /=3 ~ 4, leach containing 0.57% Cu, 2.32% Cd, Ni, the Co of 0.044% of 0.19%, the copper-cadmium slag of the Zn of 45.7%.Extraction time is 2 hours; Leaching terminal pH value is 2 ~ 3.Filter containing the leach liquor of Cu 882mg/L, Cd6955mg/L, Ni366mg/L, Co140mg/L, Zn132g/L, filter residue uses the H of 50g/L again
2sO
4, manganese mineral powder 5%, 80 ~ 90 DEG C time, leach Gu second time is carried out in liquid /=3, filtrate returns first time leaching, filter residue rate average 6 ~ 7%, Cu0.039%, Cd0.19%, Ni0.0053%, Co0.0023%, Zn4.1%.
Step 2, carries out Cp180 with time pickling liquor of one of step 1 and extracts Cu, compared/water=1.5 ~ 2, Cp180 30 ~ 40%, kerosene 60 ~ 70%, three grades of extractions, the H of two-stage 250g/L
2sO
4back extraction, one-level 5%NH
4hCO
3regenerated from washing.Raffinate is containing Cu 3mg/L, and percentage extraction 99.6%, strip liquor is containing Cu 5.6g/L, and continuous 60 extractions, back extraction, regenerated from washing circulation, the median extraction rate of Cu is 98.4%, and strip liquor is containing Cu 21 ~ 31g/L.
Step 3, first carries out neutralization oxidation except Fe with the raffinate of step 2, rear liquid containing Fe 8.26mg/L, Cu 4.18mg/L, Cd 6193mg/L, Ni 356mg/L, Co 92.9mg/L, Zn 91.4g/L, As 0.57mg/L, Sb 0.67 mg/L, Ge 0.19 mg/L.Add except cobalt agent by 1.2 times of Co, Ni content sum, in PH2 ~ 3,50 ~ 60 DEG C are carried out calcining Co, Ni concentrate contains Cu 0.49%, Cd5.8%, Co11.6%, Ni 42.57%, Fe 1.37% except Co, Ni must precipitate Ni, Co slag at 500 DEG C in 2 hours.
Step 4, carries out zinc metal sheet displacement Spongy Cadmium through charcoal absorption by step 3 except liquid after Co, Ni.First to the charcoal absorption organism of liquid 1.2g/L after Co, Ni, then carry out Spongy Cadmium displacement in displacement slot, displacement liquid temperature is at 40 ~ 50 DEG C, PH3 ~ 4, within 16 hours, displaced liquid is containing Cu trace, Cd2.25mg/L, Ni 7.6mg/L, Co 0.4 mg/L, Spongy Cadmium wet slag is containing Cd74.38%, Cu 0.037%, Ni0.08%, Co 0.0078%, Zn5.83%.
Step 5, covers step 4 gained Spongy Cadmium NaOH, carries out founding, founding rate more than 70% at 500 ~ 550 DEG C, cadmium metal containing Cd99.67%, containing Zn0.0054%, Co 0.001%, Ni 0.065%, Pb 0.078%, Fe0.182%.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, anyly do not depart from technical solution of the present invention content, the any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (7)
1. one kind is reclaimed the method for Cu, Cd, Ni, Co, Zn from copper-cadmium slag, it is characterized in that: by copper-cadmium slag through twice oxidation acid leaching, leach liquor extracting Cu, after removing Fe with oxidation in raffinate, Ni, Co is precipitated with except cobalt agent, and calcining to obtain Co, Ni concentrate, after heavy Co, liquid to obtain metal cadmium ingot, displaced liquid power transmission solution Zn system with electrolysis metallic zinc sheet displacement Spongy Cadmium is also molten after charcoal absorption.
2. a kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag as claimed in claim 1, is characterized in that: twice oxidation acid leaching is H
2sO
4leach, it is 2 ~ 3 that first time leaches terminal pH value; Second time is 50 ~ 100g/L, and the time is 2 hours, and oxygenant is the MnO of 5 ~ 10%
2or the H of 5 ~ 10%
2o
2, the leaching yield of Cu, Cd, Ni, Co, Zn is more than 98%.
3. a kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag as claimed in claim 1, is characterized in that: the extraction agent of copper is the Cp180 of 20 ~ 40%, the kerosene of 60 ~ 80%, and extraction pH value is 2 ~ 3, back extraction H
2sO
4be 250 ~ 300g/L, three grades of extractions, secondary back extraction, two-stage regenerated from washing.
4. a kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag as claimed in claim 3, is characterized in that: regenerated from washing liquid is the NH of 5 ~ 10%
4hCO
3or NH
4oH.
5. a kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag as claimed in claim 1, is characterized in that: the consumption except cobalt agent is 1.2 ~ 1.4 multiples of Co, Ni content sum; Temperature is 50 ~ 60 DEG C, time 2 h, and heavy Co, Ni slag is 500 ± 50 DEG C of calcinings, and Co, Ni concentrate is more than 15% containing Co, is more than 30% containing Ni.
6. a kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag as claimed in claim 1, is characterized in that: the displacement carrying out Spongy Cadmium with electrolytic zinc plate, displacement pH value 3 ~ 4, and temperature 40 ~ 50 DEG C, Spongy Cadmium is greater than 70% containing Cd, is less than 5% containing Zn.
7. a kind of method reclaiming Cu, Cd, Ni, Co, Zn from copper-cadmium slag as claimed in claim 6, is characterized in that: the Spongy Cadmium cake of press of gained with NaOH alkali fusion ingot casting, the cadmium metal quality of gained is more than 99%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106086439A (en) * | 2016-08-04 | 2016-11-09 | 西北矿冶研究院 | Method for recovering zinc and cobalt from zinc smelting slag |
| CN106756069A (en) * | 2017-02-08 | 2017-05-31 | 陕西理工学院 | A kind of method that valuable metal is reclaimed in the waste residue from zinc abstraction |
| CN106834696A (en) * | 2017-01-14 | 2017-06-13 | 六盘水中联工贸实业有限公司 | The comprehensive recovering process of valuable metal in a kind of copper-cadmium slag |
| CN107512837A (en) * | 2017-09-11 | 2017-12-26 | 云南省环境科学研究院(中国昆明高原湖泊国际研究中心) | The processing method of the river bottom mud containing heavy metal |
| CN109536714A (en) * | 2018-12-01 | 2019-03-29 | 贵州省冶金化工研究所 | A kind of synthetical recovery zinc method of iron content cobalt zinc waste residue |
| CN109592822A (en) * | 2018-12-01 | 2019-04-09 | 六盘水中联工贸实业有限公司 | One kind is based on magnetic field electrolysis processing iron content cobalt method for waste water |
| CN111826525A (en) * | 2020-07-24 | 2020-10-27 | 广西银亿新材料有限公司 | Method for producing metal cobalt by sulfuric acid system electrodeposition |
| CN112410568A (en) * | 2020-10-29 | 2021-02-26 | 广东中金岭南有色冶金设计研究有限公司 | Method for preparing cobalt ferrite from cobalt-containing slag |
| CN113957253A (en) * | 2021-09-27 | 2022-01-21 | 贵州省冶金化工研究所 | Method for recovering valuable metals from copper-cadmium slag through two-step oxidation acid leaching treatment |
| CN114214522A (en) * | 2021-12-23 | 2022-03-22 | 江西自立环保科技有限公司 | Wet treatment process for refined copper slag |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106086439A (en) * | 2016-08-04 | 2016-11-09 | 西北矿冶研究院 | Method for recovering zinc and cobalt from zinc smelting slag |
| CN106834696A (en) * | 2017-01-14 | 2017-06-13 | 六盘水中联工贸实业有限公司 | The comprehensive recovering process of valuable metal in a kind of copper-cadmium slag |
| CN106756069A (en) * | 2017-02-08 | 2017-05-31 | 陕西理工学院 | A kind of method that valuable metal is reclaimed in the waste residue from zinc abstraction |
| CN107512837A (en) * | 2017-09-11 | 2017-12-26 | 云南省环境科学研究院(中国昆明高原湖泊国际研究中心) | The processing method of the river bottom mud containing heavy metal |
| CN109536714A (en) * | 2018-12-01 | 2019-03-29 | 贵州省冶金化工研究所 | A kind of synthetical recovery zinc method of iron content cobalt zinc waste residue |
| CN109592822A (en) * | 2018-12-01 | 2019-04-09 | 六盘水中联工贸实业有限公司 | One kind is based on magnetic field electrolysis processing iron content cobalt method for waste water |
| CN111826525A (en) * | 2020-07-24 | 2020-10-27 | 广西银亿新材料有限公司 | Method for producing metal cobalt by sulfuric acid system electrodeposition |
| CN111826525B (en) * | 2020-07-24 | 2021-11-26 | 广西银亿新材料有限公司 | Method for producing metal cobalt by sulfuric acid system electrodeposition |
| CN112410568A (en) * | 2020-10-29 | 2021-02-26 | 广东中金岭南有色冶金设计研究有限公司 | Method for preparing cobalt ferrite from cobalt-containing slag |
| CN113957253A (en) * | 2021-09-27 | 2022-01-21 | 贵州省冶金化工研究所 | Method for recovering valuable metals from copper-cadmium slag through two-step oxidation acid leaching treatment |
| CN114214522A (en) * | 2021-12-23 | 2022-03-22 | 江西自立环保科技有限公司 | Wet treatment process for refined copper slag |
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