CN106566927B - High efficiency gradient process for separating and recovering for copper anode mud leachate - Google Patents
High efficiency gradient process for separating and recovering for copper anode mud leachate Download PDFInfo
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- CN106566927B CN106566927B CN201610896839.7A CN201610896839A CN106566927B CN 106566927 B CN106566927 B CN 106566927B CN 201610896839 A CN201610896839 A CN 201610896839A CN 106566927 B CN106566927 B CN 106566927B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G28/00—Compounds of arsenic
- C01G28/008—Sulfides
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses the efficient ladder grade process for separating and recovering for copper anode mud leachate, it includes the following steps：（1）, eddy flow electrical integration copper：Copper anode mud leachate is entered into eddy flow Winning cell, electrodeposition is carried out and obtains liquid after the copper and electrodeposition of initial gross separation；（2）, substep vulcanization decopper(ing), divide arsenic；（3）, neutralize salinization：Liquid after decopper(ing) arsenic is added sulfuric acid and adjusts acid concentration to 45~50wt%, alkali compounds neutralization reaction is then added, and after the completion of reaction, purified and separation of solid and liquid obtains solid nickel ore concentrate；（4）, Crystallization Separation, drying：Sulfuric acid is added after being recycled to nickel in liquid and adjusts pH value to 6~7, temperature is cooled to 30~40 DEG C, stands still for crystals, crystallization is centrifuged and washs, dry after obtain epsom salt product.The beneficial effects of the invention are as follows all can effectively be recycled to copper, arsenic, nickel and the sulfuric acid in copper anode mud leachate, overall process can be realized " zero-emission ", pollution-free, produce clean and effective.
Description
Technical field
The present invention relates to metallurgical engineerings and environmental project crossing domain, more particularly to the separation of recycling copper anode mud leachate
Recovery process.
Background technology
In the technical process of domestic and foreign current copper sun mud processing extraction noble metal, copper removal of impurities is divided to be using sulfuric acid solution leaching
A wherein important ring, during acidleach, outside the metals such as copper removal, arsenic, nickel, remaining is a concentration of 20~30% sulfuric acid.This leaching
Currently common treating method is liquid, recycles copper and 80% or so arsenic by evoked electrode, remaining part enters sewage disposal work
Sequence is handled, wherein a large amount of sulfuric acid and the higher copper of concentration, nickel resources also fail to effectively be recycled, causes the wave of resource
Take, waste acid processing cost is on the one hand caused to increase in order of magnitude formula, increases entreprise cost expenditure, or even control the warp of enterprise
Ji benefit.
Chinese invention patent application number CN201510995426.X discloses a kind of height that copper anode mud processing procedure generates
The method of valuable metal recovery in acid waste liquid mainly includes the following steps that the rare precious metals such as (1), selective absorption Gold, Silver, Platinum, Palladium；
(2), diffusion dialysis separation and recovery acid；(3), chlorine oxygen bismuth is recycled in neutralizing hydrolysis；(4), copper arsenic recovering copper；(5), high performance vulcanization
Deeply removing arsenic；(6), the metals such as neutralisation recycling zinc, nickel, tin；(7), high-salt wastewater recycles salt using multiple-effect evaporation after neutralizing.
Chinese invention patent application number CN201110159984.4 discloses the technique for the treatment of black copper slag through electrolytic, and belonging to has
Non-ferrous metal technical field of smelting.The technique is in a kettle, by black copper slag solvent and solute weight ratio 6:1~10:1, concentration 80 ~
The sulfuric acid solution of 250g/L leaches 3 ~ 4 hours in 70 ~ 80 DEG C；Air is blasted to reaction kettle carry out Oxidation Leaching in leaching process；
Secondary filter obtains being electrolysed preceding liquid；Liquid before electrolysis is electrolysed using cyclone electrolytic cell mode again, output criteria tough cathode and low
The high arsenic residual electrolyte of copper.
But arsenic, the rate of recovery of nickel be not high in both methods, and sulfuric acid is not recycled effectively, and the waste of resource is still deposited
Waste acid processing cost is higher, influences the economic benefit of enterprise.
Invention content
The technical problem to be solved by the present invention is to arsenic, nickel existing for the existing recovery process for copper anode mud leachate
The rate of recovery it is not high, sulfuric acid is not recycled effectively, a kind of efficient step for copper anode mud leachate is provided thus
Process for separating and recovering.
The technical scheme is that：For the efficient ladder grade process for separating and recovering of copper anode mud leachate, it include with
Lower step：（1）, eddy flow electrical integration copper：Copper anode mud leachate is entered into eddy flow Winning cell, control temperature is in 40~60 DEG C, electricity
Current density is in 600~700A/m2It carries out electrodeposition and obtains liquid after the copper and electrodeposition of initial gross separation；（2）, substep vulcanization decopper(ing), divide arsenic：
The control of liquid temperature is slowly introducing pure hydrogen sulfide gas at 60~90 DEG C after electrodeposition, the depth recycling of copper is realized, after controlling decopper(ing)
40~50 DEG C of liquid temperature continues to be passed through hydrogen sulfide gas, 80~90min of reaction time, and sampling analysis detects arsenic in solution and is less than
When 1mg/L, reaction terminating obtains the sulfide of arsenic through filtration washing；（3）, neutralize salinization：Liquid after decopper(ing) arsenic is added sulfuric acid and adjusts
Then alkali compounds neutralization reaction is added to 45~50wt% in acid concentration, controlling reaction temperature at 60~70 DEG C, pH value 7~
8, after the completion of reaction, purified and separation of solid and liquid obtains solid nickel ore concentrate；（4）, Crystallization Separation, drying：After being recycled to nickel in liquid
Sulfuric acid is added and adjusts pH value to 6~7, temperature is cooled to 30~40 DEG C, stands still for crystals, and crystallization is centrifuged and washs, dries
After obtain epsom salt product.
Step described in said program（1）Middle copper anode mud leachate 35~50g/L of cupric, liquid copper content is 3 after electrodeposition
~10g/L.
Step described in said program（2）Middle copper sulphur molar ratio 1.0~1.5:1, pozzuolite molar ratio 1：2.0~3.0.
Step described in said program（3）Medium alkaline compound is one kind or more of magnesia, magnesium hydroxide, magnesium carbonate
Kind.
The beneficial effects of the invention are as follows all can effectively being recycled to copper, arsenic, nickel and the sulfuric acid in copper anode mud leachate,
The arsenic rate of recovery is up to 99% or more, and up to 85% or more, sulfuric acid is recycled nickel recovery in the form of epsom salt, liquid cycle profit after crystallization
With overall process can be realized " zero-emission ", pollution-free, produce clean and effective.
Description of the drawings
Fig. 1 is flow diagram of the present invention.
Specific implementation mode
The present invention will be further described below in conjunction with the accompanying drawings.
As shown in Figure 1, the present invention includes the following steps：（1）, eddy flow electrical integration copper：Copper anode mud leachate is entered into rotation
Winning cell is flowed, control temperature is in 40~60 DEG C, current density in 600~700A/m2Carry out electrodeposition obtain initial gross separation copper and
Liquid after electrodeposition；（2）, substep vulcanization decopper(ing), divide arsenic：The control of liquid temperature is slowly introducing pure hydrogen sulfide at 60~90 DEG C after electrodeposition
Gas realizes the depth recycling of copper, controls 40~50 DEG C of liquid temperature after decopper(ing), continue to be passed through hydrogen sulfide gas, reaction time 80
~90min, sampling analysis, detect solution in arsenic be less than 1mg/L when, reaction terminating obtains the sulfide of arsenic through filtration washing；
（3）, neutralize salinization：Liquid after decopper(ing) arsenic is added sulfuric acid and adjusts acid concentration to 45~50wt%, alkali compounds is then added and neutralizes
Reaction, controlling reaction temperature is at 60~70 DEG C, and for pH value after the completion of 7~8, reaction, purified and separation of solid and liquid obtains solid nickel
Concentrate；（4）, Crystallization Separation, drying：Sulfuric acid is added after being recycled to nickel in liquid and adjusts pH value to 6~7, temperature is cooled to 30~40
DEG C, stand still for crystals, crystallization be centrifuged and wash, dry after obtain epsom salt product.
Eddy flow electrodeposition technology is the difference based on each metal ion theory deposition potential, if the metal to be extracted with
Other metal ions have larger potential difference in solution system, then the metal of current potential calibration is easy to preferentially be precipitated in cathode.It is closed
Key is detained or unhurried current and the metal target brought to eliminate solution in traditional electrolyte technology by the swiftly flowing means of solution
Ion concentration is gradually reduced, and causes concentration polarization etc. to the unfavorable factor of electrolysis, is avoided in traditional electrolyte process by many factors
（Ion concentration, deposition potential, concentration polarization, pH value etc.）The limitation of influence can produce height by simple technical conditions
The metal product of quality.Existing eddy flow electrowinning plant, be all cathode outside, including anode, the two be in coaxial columnar.Cathode one
As collectively constituted by cylinder and starting sheet two parts, starting sheet is fitted tightly on cathode cylinder inboard wall, target in electrolytic deposition process
Metal deposit is attached on starting sheet.
Embodiment 1：For the efficient ladder grade process for separating and recovering of copper anode mud leachate, it includes the following steps：（1）、
Eddy flow electrical integration copper：Copper anode mud leachate is entered into eddy flow Winning cell, copper anode mud leachate cupric 35g/L controls temperature
In 40 DEG C, current density in 600A/m2It carries out electrodeposition and obtains liquid after the copper and electrodeposition of initial gross separation, liquid copper content is after electrodeposition
3g/L；（2）, substep vulcanization decopper(ing), divide arsenic：The control of liquid temperature is slowly introducing pure hydrogen sulfide gas, copper sulphur at 60 DEG C after electrodeposition
Molar ratio 1:1, it realizes the depth recycling of copper, controls 40 DEG C of liquid temperature after decopper(ing), continue to be passed through hydrogen sulfide gas, pozzuolite molar ratio
1：2.0, reaction time 80min, sampling analysis, detect solution in arsenic be less than 1mg/L when, reaction terminating obtains arsenic through filtration washing
Sulfide；（3）, neutralize salinization：Liquid after decopper(ing) arsenic is added sulfuric acid and adjusts acid concentration to 45wt%, magnesia, hydrogen is then added
One or more carry out neutralization reactions of magnesia, magnesium carbonate, controlling reaction temperature at 60 DEG C, pH value after the completion of 7, reaction,
Purified and separation of solid and liquid obtains solid nickel ore concentrate；（4）, Crystallization Separation, drying：Sulfuric acid is added after being recycled to nickel in liquid and adjusts PH
Value to 6, temperature is cooled to 30 DEG C, stands still for crystals, crystallization be centrifuged and wash, dry after obtain epsom salt product.
Embodiment 2：For the efficient ladder grade process for separating and recovering of copper anode mud leachate, it includes the following steps：（1）、
Eddy flow electrical integration copper：Copper anode mud leachate is entered into eddy flow Winning cell, copper anode mud leachate cupric 40g/L controls temperature
In 50 DEG C, current density in 650A/m2It carries out electrodeposition and obtains liquid after the copper and electrodeposition of initial gross separation, liquid copper content is after electrodeposition
6g/L；（2）, substep vulcanization decopper(ing), divide arsenic：The control of liquid temperature is slowly introducing pure hydrogen sulfide gas, copper sulphur at 75 DEG C after electrodeposition
Molar ratio 1.2:1, it realizes the depth recycling of copper, controls liquid temperature 45 C after decopper(ing), continue to be passed through hydrogen sulfide gas, pozzuolite mole
Than 1：2.5, reaction time 85min, sampling analysis, detect solution in arsenic be less than 1mg/L when, reaction terminating is obtained through filtration washing
The sulfide of arsenic；（3）, neutralize salinization：Liquid after decopper(ing) arsenic is added sulfuric acid and adjusts acid concentration to 47wt%, be then added magnesia,
One or more carry out neutralization reactions of magnesium hydroxide, magnesium carbonate, controlling reaction temperature is at 65 DEG C, and pH value 7.5, complete by reaction
Afterwards, purified and separation of solid and liquid obtains solid nickel ore concentrate；（4）, Crystallization Separation, drying：Sulfuric acid tune is added after being recycled to nickel in liquid
For whole pH value to 6.5, temperature is cooled to 35 DEG C, stands still for crystals, crystallization be centrifuged and wash, dry after obtain epsom salt
Product.
Embodiment 3：For the efficient ladder grade process for separating and recovering of copper anode mud leachate, it includes the following steps：（1）、
Eddy flow electrical integration copper：Copper anode mud leachate is entered into eddy flow Winning cell, copper anode mud leachate cupric 50g/L controls temperature
In 60 DEG C, current density in 700A/m2It carries out electrodeposition and obtains liquid after the copper and electrodeposition of initial gross separation, liquid copper content is after electrodeposition
10g/L；（2）, substep vulcanization decopper(ing), divide arsenic：The control of liquid temperature is slowly introducing pure hydrogen sulfide gas, copper at 90 DEG C after electrodeposition
Sulphur molar ratio 1.5:1, it realizes the depth recycling of copper, controls liquid temperature 50 C after decopper(ing), continue to be passed through hydrogen sulfide gas, pozzuolite rubs
That ratio 1：3.0, reaction time 90min, sampling analysis, when detecting that arsenic is less than 1mg/L in solution, reaction terminating, through filtration washing,
Obtain the sulfide of arsenic；（3）, neutralize salinization：Liquid after decopper(ing) arsenic is added sulfuric acid and adjusts acid concentration to 50wt%, oxidation is then added
One or more carry out neutralization reactions of magnesium, magnesium hydroxide, magnesium carbonate, at 70 DEG C, pH value has reacted controlling reaction temperature 8
Cheng Hou, purified and separation of solid and liquid obtain solid nickel ore concentrate；（4）, Crystallization Separation, drying：Sulfuric acid is added in liquid after being recycled to nickel
Adjust pH value to 7, temperature is cooled to 40 DEG C, stands still for crystals, crystallization be centrifuged and wash, dry after obtain epsom salt
Product.
The present invention is close by controlling liquid copper content after the copper content of copper anode mud leachate, electrodeposition, the electric current of eddy flow electrodeposition
Degree, control temperature, copper sulphur molar ratio, pozzuolite molar ratio so that copper overall recovery is up to 99% or more, and the arsenic rate of recovery is up to 99% or more；
The concentration realization that sulfuric acid in salinization is neutralized by control reaches 85% or more to nickel recovery.It realizes to copper, arsenic, nickel and sulfuric acid
Substep recycling, realize overall process zero-emission.
Claims (2)
1. for the efficient ladder grade process for separating and recovering of copper anode mud leachate, it is characterized in that it includes the following steps：（1）, rotation
Galvanic electricity integrates copper：Copper anode mud leachate is entered into eddy flow Winning cell, copper anode mud leachate 35~50g/L of cupric, control temperature
Degree is in 40~60 DEG C, current density in 600~700A/m2It carries out electrodeposition and obtains the copper of initial gross separation and copper content to be 3~10g/L
Electrodeposition after liquid；（2）, substep vulcanization decopper(ing), divide arsenic：The control of liquid temperature is slowly introducing pure vulcanization at 60~90 DEG C after electrodeposition
Hydrogen realizes the depth recycling of copper, controls 40~50 DEG C of liquid temperature after decopper(ing), continue to be passed through hydrogen sulfide gas, reaction time
80~90min, sampling analysis, detect solution in arsenic be less than 1mg/L when, reaction terminating obtains the sulfide of arsenic through filtration washing,
Copper sulphur molar ratio 1.0~1.5:1, pozzuolite molar ratio 1：2.0~3.0；（3）, neutralize salinization：Sulfuric acid tune is added in liquid after decopper(ing) arsenic
Acid concentration is saved to 45~50wt%, alkali compounds neutralization reaction is then added, controlling reaction temperature is at 60~70 DEG C, and pH value is 7
~8, after the completion of reaction, purified and separation of solid and liquid obtains solid nickel ore concentrate；（4）, Crystallization Separation, drying：Liquid after being recycled to nickel
Middle addition sulfuric acid adjusts pH value to 6~7, and temperature is cooled to 30~40 DEG C, stands still for crystals, and crystallization is centrifuged and washs, does
Epsom salt product is obtained after dry.
2. the efficient ladder grade process for separating and recovering of copper anode mud leachate is used for as described in claim 1, it is characterized in that described
Step（3）Medium alkaline compound be magnesia, magnesium hydroxide, magnesium carbonate it is one or more.
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| CN107090587B (en) * | 2017-04-25 | 2018-12-04 | 云南锡业股份有限公司铜业分公司 | A method of control potential electrodeposition removes copper arsenic |
| CN107227466A (en) * | 2017-06-26 | 2017-10-03 | 郴州市金贵银业股份有限公司 | A kind of method that chlorine oxygen copper dechlorination carries copper |
| CN109485023B (en) * | 2018-12-18 | 2021-10-22 | 阳谷祥光铜业有限公司 | Method for recovering tellurium from copper-tellurium-containing waste liquid |
| CN110283999A (en) * | 2019-07-02 | 2019-09-27 | 株洲三特环保节能股份有限公司 | A kind of processing method of waste solution of copper electrolysis |
| CN110983376B (en) * | 2019-12-31 | 2020-08-28 | 广西南国铜业有限责任公司 | Copper electrolyte purification process |
| CN111575491B (en) * | 2020-06-29 | 2021-11-19 | 株洲冶炼集团股份有限公司 | Resource comprehensive utilization method for purifying cobalt-nickel slag by zinc hydrometallurgy arsenic salt |
| CN113401995A (en) * | 2021-05-27 | 2021-09-17 | 南方环境有限公司 | Method for treating and recycling heavy metal contaminated soil leaching waste liquid |
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| WO2007039665A1 (en) * | 2005-10-03 | 2007-04-12 | Outotec Oyj. | Method for processing nickel bearing raw material in chloride-based leaching |
| CN101328538A (en) * | 2008-08-04 | 2008-12-24 | 云南嘉明科技实业有限公司 | Method for extracting copper, cobalt and nickel from cupric oxide cobalt ore |
| CN105441685B (en) * | 2015-12-28 | 2017-10-17 | 中南大学 | The method of valuable metal recovery in the high acid waste liquid that a kind of copper anode mud processing procedure is produced |
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