CN111945009A - Ammonia leaching recycling process for copper and nickel in electroplating sludge - Google Patents

Ammonia leaching recycling process for copper and nickel in electroplating sludge Download PDF

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CN111945009A
CN111945009A CN202010964131.7A CN202010964131A CN111945009A CN 111945009 A CN111945009 A CN 111945009A CN 202010964131 A CN202010964131 A CN 202010964131A CN 111945009 A CN111945009 A CN 111945009A
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ammonia
nickel
leaching
copper
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侯海盟
祁国恕
方晓明
李宝磊
赵岩
孔德勇
曾乐
刘舒
陈明
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Shenyang Academy Environmental Sciences
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/008Wet processes by an alkaline or ammoniacal leaching
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0063Hydrometallurgy
    • C22B15/0065Leaching or slurrying
    • C22B15/0078Leaching or slurrying with ammoniacal solutions, e.g. ammonium hydroxide
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0063Hydrometallurgy
    • C22B15/0084Treating solutions
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0407Leaching processes
    • C22B23/0446Leaching processes with an ammoniacal liquor or with a hydroxide of an alkali or alkaline-earth metal
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0453Treatment or purification of solutions, e.g. obtained by leaching
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to the technical field of electroplating sludge recycling, in particular to an ammonia leaching recycling process for copper and nickel in electroplating sludge, which is technically characterized by comprising the following steps of: 1) mixing, filtering and separating; 2) extracting and treating the leachate; 3) secondary extraction treatment of the leachate; 4) removing impurities from the loaded organic phase; 5) carrying out organic reverse extraction treatment on the first section; 6) carrying out organic reverse extraction treatment on the two-stage load; 7) removing impurities from the strip liquor; 8) and preparing a leaching agent. The process is simple and convenient to operate, does not cause secondary pollution, is low in operation cost, is high in heavy metal recovery rate, and has remarkable environmental benefit and economic benefit.

Description

Ammonia leaching recycling process for copper and nickel in electroplating sludge
Technical Field
The invention relates to the technical field of electroplating sludge recycling, in particular to an ammonia leaching recycling process for copper and nickel in electroplating sludge.
Background
After the electroplating wastewater and waste liquid generated in the electroplating process are neutralized, filtered and precipitated, a large amount of electroplating sludge can be generated, the water content of the electroplating sludge is high, the electroplating sludge contains various heavy metals such as copper, nickel, zinc, chromium, iron and the like, the electroplating sludge is easy to leach out, and if the electroplating sludge is not properly treated, the electroplating sludge can bring serious pollution to the surrounding ecological environment, so the electroplating sludge is classified as dangerous waste.
At present, the electroplating sludge treatment mainly comprises harmless treatment and resource treatment, but the treatment methods have some problems:
1. the harmless treatment of the electroplating sludge is to solidify the electroplating sludge and then bury the electroplating sludge, the method occupies a large amount of land resources, and the risk of leaching heavy metals exists, so that the useful metals in the electroplating sludge cannot be reused, and the resource waste is caused.
2. The electroplating sludge resource treatment is to recover heavy metals by two methods of pyrometallurgy and wet leaching. Wherein, the pyrometallurgical process needs to be carried out under the high-temperature condition, and the conditions of high energy consumption, high cost and low metal yield exist; the wet leaching process adopts a leaching agent to leach and separate heavy metal elements such as copper, nickel, zinc and the like in sludge, and although the process has low cost and small secondary pollution, the prior wet technology has poor selectivity on copper, nickel and chromium, high requirement on process condition control, complex operation, incapability of recycling the leaching agent and high medicament consumption.
Disclosure of Invention
The invention aims to solve the problems and provides an ammonia leaching recycling process for copper and nickel in electroplating sludge, which has the advantages of simple process, convenient operation, no secondary pollution, low operation cost, high heavy metal recovery rate and obvious environmental and economic benefits.
The ammonia leaching recycling process of copper and nickel in electroplating sludge has the technical key points that the process comprises the following steps:
1) mixing, filtering and separating: according to the liquid-solid ratio of 3-4: 1, adding electroplating sludge into an ammoniacal system leaching agent, stirring for 4 hours at the temperature of 60-80 ℃, and filtering and separating leaching liquid and leaching residues;
2) extracting and treating the leachate: taking the leachate separated in the step 1), adjusting the pH value to 9-10, adding an extracting agent according to the mass ratio of 1:1, stirring and oscillating for a certain time, and separating a first-stage loaded organic phase and a first-stage raffinate;
3) secondary extraction treatment of the leachate: taking the first-stage raffinate separated in the step 2), adding an extracting agent according to the mass ratio of 1:1, stirring and oscillating for a certain time, and separating a second-stage loaded organic phase and a second-stage raffinate;
4) removing impurities from a loaded organic phase: carrying out two-stage countercurrent water washing on the first-stage loaded organic phase separated in the step 2) and the second-stage loaded organic phase separated in the step 3) to remove impurity metal ions in the first-stage loaded organic phase;
5) one-stage loaded organic reverse extraction treatment: taking the first-stage loaded organic phase subjected to impurity removal in the step 4), adding a stripping agent according to the volume ratio of 1:1, stirring and oscillating for a certain time, stripping and separating out a copper hydroxide solution for further electrodeposition and copper recovery, and leaving a first-stage stripping raffinate;
6) and (3) carrying out organic reverse extraction treatment on the two stages: taking the second-stage loaded organic phase subjected to impurity removal in the step 4), adding a stripping agent according to the volume ratio of 1:1, stirring and oscillating for a certain time, separating out a nickel hydroxide solution through stripping, using the nickel hydroxide solution to further evaporate and recover nickel, and remaining second-stage stripping raffinate;
7) removing impurities from the strip liquor: taking the first-stage strip raffinate left after the strip processing in the step 5) and the second-stage strip raffinate left after the strip processing in the step 6), adjusting the pH value to 9-10, and adding ammonium phosphate to remove impurity ions such as calcium, magnesium, iron and the like;
8) preparing a leaching agent: and (4) supplementing ammonia and ammonium oxycarbonate to the first-stage strip raffinate and the second-stage strip raffinate which are subjected to impurity removal in the step 7) in the step five until the total ammonia concentration is 8-10mol/L, and using the first-stage strip raffinate and the second-stage strip raffinate as the leaching agent in the step 1).
In the ammonia leaching recycling process of copper and nickel in electroplating sludge, in the step 1), the ammonia system leaching agent is an ammonia-ammonium oxycarbonate system, the total ammonia concentration is 8-10mol/L, and the ammonia-ammonium ratio is 1: 2.
In the ammonia leaching recycling process of copper and nickel in electroplating sludge, in the step 2) and the step 3), the extracting agent is Lix984 with the volume fraction of 9-12%, and the diluting agent is sulfonated kerosene.
In the ammonia leaching recycling process of copper and nickel in electroplating sludge, in the step 4), the volume ratio of the loaded organic phase to the water phase in the secondary countercurrent washing process is 2: 1.
In the ammonia leaching recycling process of copper and nickel in electroplating sludge, in the step 5) and the step 6), the stripping agent is a sulfuric acid solution with the concentration of 1.5-2.5 mol/L.
In the ammonia leaching recycling process of copper and nickel in electroplating sludge, in the step 7), the addition amount of ammonium phosphate is 1.3 times of the theoretical reaction amount.
In the ammonia leaching recycling process of copper and nickel in electroplating sludge, in the step 8), the ammonia-ammonium ratio of the supplemented ammonia and ammonium oxycarbonate is 1: 2.
The invention has the beneficial effects that:
mixing the electroplating sludge and the ammoniacal system leaching agent, separating leaching slag to perform conventional waste residue treatment, obtaining leaching solution containing Cu and Ni, performing impurity removal and back extraction treatment on a loaded organic phase obtained by performing two-stage extraction treatment on the leaching solution to obtain a copper hydroxide solution and a nickel hydroxide solution, recovering copper and nickel further, and supplementing ammonia and ammonium bicarbonate after removing impurities from the residual back extraction raffinate to obtain the ammoniacal system leaching agent. The whole process eliminates the dangerous characteristic of the electroplating sludge on the basis of treating the electroplating sludge to recover copper and nickel, and the electroplating sludge is changed into conventional waste residues after treatment; the recycling of the leaching agent is realized, meanwhile, the second-stage raffinate is a mixed solvent without most heavy metals, and can be partially recycled and used as the extracting agent for recycling, so that the consumption of the medicinal agent in the treatment process is greatly reduced, the treatment cost is reduced, no reagent is left, secondary pollution cannot be caused, and the treatment effect of the leaching agent after recycling is not influenced; the recovery rate of copper is more than 93% and the recovery rate of nickel is more than 90% after the ammonia system leaching agent is firstly treated, the recyclable leaching agent is obtained after ammonia and ammonium oxycarbonate are supplemented, the recovery rate of copper is more than 88% and the recovery rate of nickel is more than 85% after the electroplating sludge is treated, and the recovery rate of heavy metal is obvious in environmental benefit and economic benefit.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are presented herein for the purpose of illustration and explanation and are not intended to be limiting.
As shown in figure 1, the ammonia leaching recycling process of copper and nickel in electroplating sludge comprises the following steps:
1) mixing, filtering and separating: according to the liquid-solid ratio of 3-4: 1, adding electroplating sludge into an ammoniacal system leaching agent, stirring for 4 hours at the temperature of 60-80 ℃, and filtering and separating leaching liquid and leaching residues;
2) extracting and treating the leachate: taking the leachate separated in the step 1), adjusting the pH value to 9-10, adding an extracting agent according to the mass ratio of 1:1, stirring and oscillating for a certain time, and separating a first-stage loaded organic phase and a first-stage raffinate;
3) secondary extraction treatment of the leachate: taking the first-stage raffinate separated in the step 2), adding an extracting agent according to the mass ratio of 1:1, stirring and oscillating for a certain time, and separating a second-stage loaded organic phase and a second-stage raffinate;
4) removing impurities from a loaded organic phase: carrying out two-stage countercurrent water washing on the first-stage loaded organic phase separated in the step 2) and the second-stage loaded organic phase separated in the step 3) to remove impurity metal ions in the first-stage loaded organic phase;
5) one-stage loaded organic reverse extraction treatment: taking the first-stage loaded organic phase subjected to impurity removal in the step 4), adding a stripping agent according to the volume ratio of 1:1, stirring and oscillating for a certain time, stripping and separating out a copper hydroxide solution for further electrodeposition and copper recovery, and leaving a first-stage stripping raffinate;
6) and (3) carrying out organic reverse extraction treatment on the two stages: taking the second-stage loaded organic phase subjected to impurity removal in the step 4), adding a stripping agent according to the volume ratio of 1:1, stirring and oscillating for a certain time, separating out a nickel hydroxide solution through stripping, using the nickel hydroxide solution to further evaporate and recover nickel, and remaining second-stage stripping raffinate;
7) removing impurities from the strip liquor: taking the first-stage strip raffinate left after the strip processing in the step 5) and the second-stage strip raffinate left after the strip processing in the step 6), adjusting the pH value to 9-10, and adding ammonium phosphate to remove impurity ions such as calcium, magnesium, iron and the like;
8) preparing a leaching agent: and (4) supplementing ammonia and ammonium oxycarbonate to the first-stage strip raffinate and the second-stage strip raffinate which are subjected to impurity removal in the step 7) in the step five until the total ammonia concentration is 8-10mol/L, and using the first-stage strip raffinate and the second-stage strip raffinate as the leaching agent in the step 1).
In the step 1), the leaching agent of the ammoniacal system is an ammonia-ammonium oxycarbonate system, the total ammonia concentration is 8-10mol/L, and the ammonia-ammonium ratio is 1: 2. In the step 2) and the step 3), the extracting agent is Lix984 with the volume fraction of 9-12%, and the diluting agent is sulfonated kerosene. In the step 4), the volume ratio of the loaded organic phase to the water phase in the secondary countercurrent water washing process is 2: 1. In the step 5) and the step 6), the stripping agent is sulfuric acid solution with the concentration of 1.5-2.5 mol/L. In the step 7), the adding amount of the ammonium phosphate is 1.3 times of the theoretical reaction amount. In step 8), the ammonia-to-ammonium ratio of the supplemented ammonia and ammonium oxycarbonate is 1: 2.
Example 1
Adding 500g of dry electroplating sludge (mainly containing heavy metals of Cu5.6 percent and Ni4.9 percent) into 2000mL of ammoniacal system leaching agent (containing 25 percent of ammonia water and ammonium bicarbonate and having the total ammonia concentration of 8 mol/L), keeping the temperature at about 70 ℃, stirring for 4 hours, and filtering to separate leaching solution and leaching residues; taking 2100mL of leachate, adding alkali liquor to adjust the pH value to 9.2, adding a Lix984 extracting agent (volume fraction is 9%) according to the mass ratio of 1:1, stirring for 30min at normal temperature, and separating out a first-stage loaded organic phase and a first-stage raffinate; adding a Lix984 extracting agent (volume fraction is 9%) into the first-stage raffinate according to the mass ratio of 1:1, stirring and oscillating, and separating a second-stage loaded organic phase and a second-stage raffinate, wherein the second-stage raffinate can be partially recycled as the extracting agent; carrying out two-stage countercurrent water washing on the first-stage loaded organic phase and the second-stage loaded organic phase, wherein the volume ratio of the organic phase to the water phase is 2:1, and removing impurity metal ions in the organic phase and the water phase; adding a sulfuric acid solution stripping agent with the concentration of 1.5mol/L into the first section of the loaded organic phase after the impurity metal ions are removed according to the volume ratio of 1:1, stirring and oscillating for 1h, separating out a copper hydroxide solution by stripping, and further electrodepositing to recover copper, wherein the recovery rate of the crude copper is 93.83%; adding a sulfuric acid solution stripping agent with the concentration of 1.5mol/L into the two-stage loaded organic phase after the impurity metal ions are removed according to the volume ratio of 1:1, stirring and oscillating for 1h, separating out a nickel hydroxide solution through stripping, and using the nickel hydroxide solution to further evaporate and recover nickel hydroxide to obtain crude nickel with the recovery rate of 92.19%; and (3) adjusting the pH value of all the strip liquor to 9-10, adding ammonium phosphate, and supplementing ammonia and ammonium bicarbonate until the total ammonia concentration is 8mol/L to obtain the ammoniacal leaching agent.
Adding an ammoniacal extracting agent obtained by supplementing ammonia and ammonium oxycarbonate into the untreated electroplating sludge, repeating the steps for treatment, and obtaining an ammoniacal leaching agent again, so that the recycling of the leaching agent is realized, and the recovery rate of crude copper and crude nickel obtained by recovery after treatment is 88.36% and 85.50%.
Example 2
Adding 500g of dry electroplating sludge (mainly containing heavy metals of Cu6.8 percent and Ni5.2 percent) into 2000mL of ammoniacal system leaching agent (containing 25 percent of ammonia water and ammonium bicarbonate and the total ammonia concentration of 9 mol/L), keeping the temperature at about 70 ℃, stirring for 4 hours, and filtering to separate leaching solution and leaching residues; taking 2100mL of leachate, adding alkali liquor to adjust the pH value to 9.2, adding a Lix984 extracting agent (the volume fraction is 10%) according to the mass ratio of 1:1, stirring for 30min at normal temperature, and separating out a first-stage loaded organic phase and a first-stage raffinate; adding a Lix984 extracting agent (the volume fraction is 10%) into the first-stage raffinate according to the mass ratio of 1:1, stirring and oscillating, and separating a second-stage loaded organic phase and a second-stage raffinate, wherein the second-stage raffinate can be partially recycled as the extracting agent; carrying out two-stage countercurrent water washing on the first-stage loaded organic phase and the second-stage loaded organic phase, wherein the volume ratio of the organic phase to the water phase is 2:1, and removing impurity metal ions in the organic phase and the water phase; adding a sulfuric acid solution stripping agent with the concentration of 2 mol/L into the first section of the loaded organic phase after the impurity metal ions are removed according to the volume ratio of 1:1, stirring and oscillating for 1h, separating out a copper hydroxide solution by stripping, and further electrodepositing to recover copper to obtain the recovery rate of the crude copper of 95.34%; adding a sulfuric acid solution stripping agent with the concentration of 2 mol/L into the two-section loaded organic phase after the impurity metal ions are removed according to the volume ratio of 1:1, stirring and oscillating for 1h, separating out a nickel hydroxide solution through stripping, and using the nickel hydroxide solution to further evaporate and recover nickel hydroxide to obtain the crude nickel with the recovery rate of 93.58%; and (3) adjusting the pH value of all the strip liquor to 9-10, adding ammonium phosphate, and supplementing ammonia and ammonium bicarbonate until the total ammonia concentration is 9mol/L to obtain the ammoniacal leaching agent.
Adding an ammoniacal extracting agent obtained by supplementing ammonia and ammonium oxycarbonate into the untreated electroplating sludge, repeating the steps for treatment, and obtaining an ammoniacal leaching agent again, so that the recycling of the leaching agent is realized, and the recovery rate of the crude copper and the crude nickel obtained by recovery after treatment is 89.43% and 85.59%.
Example 3
Adding 500g of dry electroplating sludge (mainly containing heavy metals of Cu8.9 percent and Ni7.2 percent) into 2000mL of ammoniacal system leaching agent (containing 25 percent of ammonia water and ammonium bicarbonate and having a total ammonia concentration of 10 mol/L), keeping the temperature at about 70 ℃, stirring for 4 hours, and filtering to separate leaching solution and leaching residues; taking 2100mL of leachate, adding alkali liquor to adjust the pH value to 9.2, adding a Lix984 extracting agent (the volume fraction is 12%) according to the mass ratio of 1:1, stirring for 30min at normal temperature, and separating out a first-stage loaded organic phase and a first-stage raffinate; adding a Lix984 extracting agent (the volume fraction is 12%) into the first-stage raffinate according to the mass ratio of 1:1, stirring and oscillating, and separating a second-stage loaded organic phase and a second-stage raffinate, wherein the second-stage raffinate can be partially recycled as the extracting agent; carrying out two-stage countercurrent water washing on the first-stage loaded organic phase and the second-stage loaded organic phase, wherein the volume ratio of the organic phase to the water phase is 2:1, and removing impurity metal ions in the organic phase and the water phase; adding a sulfuric acid solution stripping agent with the concentration of 2.5mol/L into the first section of the loaded organic phase after the impurity metal ions are removed according to the volume ratio of 1:1, stirring and oscillating for 1h, separating out a copper hydroxide solution by stripping, and further electrodepositing to recover copper, wherein the recovery rate of the crude copper is 96.72%; adding a sulfuric acid solution stripping agent with the concentration of 2.5mol/L into the two-section loaded organic phase after the impurity metal ions are removed according to the volume ratio of 1:1, stirring and oscillating for 1h, separating out a nickel hydroxide solution through stripping, and further evaporating and recovering the nickel hydroxide to obtain crude nickel with the recovery rate of 95.22%; and (3) adjusting the pH value of all the strip liquor to 9-10, adding ammonium phosphate, and supplementing ammonia and ammonium bicarbonate until the total ammonia concentration is 10mol/L to obtain the ammoniacal leaching agent.
Adding an ammoniacal extracting agent obtained by supplementing ammonia and ammonium oxycarbonate into the untreated electroplating sludge, repeating the steps for treatment, and obtaining an ammoniacal leaching agent again, so that the recycling of the leaching agent is realized, and the recovery rate of the crude copper and the crude nickel obtained by recovery after treatment is 92.42% and 89.87%.
The above embodiments are only used for illustrating the technical solution of the present invention, and not for limiting the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (7)

1. The ammonia leaching recycling process of copper and nickel in electroplating sludge is characterized by comprising the following steps:
1) mixing, filtering and separating: according to the liquid-solid ratio of 3-4: 1, adding electroplating sludge into an ammoniacal system leaching agent, stirring for 4 hours at the temperature of 60-80 ℃, and filtering and separating leaching liquid and leaching residues;
2) extracting and treating the leachate: taking the leachate separated in the step 1), adjusting the pH value to 9-10, adding an extracting agent according to the mass ratio of 1:1, stirring and oscillating for a certain time, and separating a first-stage loaded organic phase and a first-stage raffinate;
3) secondary extraction treatment of the leachate: taking the first-stage raffinate separated in the step 2), adding an extracting agent according to the mass ratio of 1:1, stirring and oscillating for a certain time, and separating a second-stage loaded organic phase and a second-stage raffinate;
4) removing impurities from a loaded organic phase: carrying out two-stage countercurrent water washing on the first-stage loaded organic phase separated in the step 2) and the second-stage loaded organic phase separated in the step 3) to remove impurity metal ions in the first-stage loaded organic phase;
5) one-stage loaded organic reverse extraction treatment: taking the first-stage loaded organic phase subjected to impurity removal in the step 4), adding a stripping agent according to the volume ratio of 1:1, stirring and oscillating for a certain time, stripping and separating out a copper hydroxide solution for further electrodeposition and copper recovery, and leaving a first-stage stripping raffinate;
6) and (3) carrying out organic reverse extraction treatment on the two stages: taking the second-stage loaded organic phase subjected to impurity removal in the step 4), adding a stripping agent according to the volume ratio of 1:1, stirring and oscillating for a certain time, separating out a nickel hydroxide solution through stripping, using the nickel hydroxide solution to further evaporate and recover nickel, and remaining second-stage stripping raffinate;
7) removing impurities from the strip liquor: taking the first-stage strip raffinate left after the strip processing in the step 5) and the second-stage strip raffinate left after the strip processing in the step 6), adjusting the pH value to 9-10, and adding ammonium phosphate to remove impurity ions such as calcium, magnesium, iron and the like;
8) preparing a leaching agent: and (4) supplementing ammonia and ammonium oxycarbonate to the first-stage strip raffinate and the second-stage strip raffinate which are subjected to impurity removal in the step 7) in the step five until the total ammonia concentration is 8-10mol/L, and using the first-stage strip raffinate and the second-stage strip raffinate as the leaching agent in the step 1).
2. The ammonia leaching recycling process of copper and nickel in electroplating sludge according to claim 1, characterized in that: in the step 1), the leaching agent of the ammoniacal system is an ammonia-ammonium oxycarbonate system, the total ammonia concentration is 8-10mol/L, and the ammonia-ammonium ratio is 1: 2.
3. The ammonia leaching recycling process of copper and nickel in electroplating sludge according to claim 1, characterized in that: in the step 2) and the step 3), the extracting agent is Lix984 with the volume fraction of 9-12%, and the diluting agent is sulfonated kerosene.
4. The ammonia leaching recycling process of copper and nickel in electroplating sludge according to claim 1, characterized in that: in the step 4), the volume ratio of the loaded organic phase to the water phase in the secondary countercurrent water washing process is 2: 1.
5. The ammonia leaching recycling process of copper and nickel in electroplating sludge according to claim 1, characterized in that: in the step 5) and the step 6), the stripping agent is sulfuric acid solution with the concentration of 1.5-2.5 mol/L.
6. The ammonia leaching recycling process of copper and nickel in electroplating sludge according to claim 1, characterized in that: in step 7), the amount of ammonium phosphate added is 1.3 times the theoretical reaction amount.
7. The ammonia leaching recycling process of copper and nickel in electroplating sludge according to claim 1, characterized in that: in step 8), the ammonia-to-ammonium ratio of the supplemented ammonia and ammonium oxycarbonate is 1: 2.
CN202010964131.7A 2020-09-15 2020-09-15 Ammonia leaching recycling process for copper and nickel in electroplating sludge Withdrawn CN111945009A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN115491513A (en) * 2022-09-08 2022-12-20 西北矿冶研究院 Process for comprehensively recovering copper, cobalt and nickel from copper-cobalt-nickel-containing solid hazardous waste

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张焕然: "氨法回收电镀污泥中铜镍的工艺研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技I辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115491513A (en) * 2022-09-08 2022-12-20 西北矿冶研究院 Process for comprehensively recovering copper, cobalt and nickel from copper-cobalt-nickel-containing solid hazardous waste
CN115491513B (en) * 2022-09-08 2023-11-17 西北矿冶研究院 Process for comprehensively recovering copper, cobalt and nickel from copper-cobalt-nickel-containing solid hazardous waste

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Application publication date: 20201117