CN108570560A - A method of recycling copper from copper-bearing waste material - Google Patents
A method of recycling copper from copper-bearing waste material Download PDFInfo
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- CN108570560A CN108570560A CN201810597521.8A CN201810597521A CN108570560A CN 108570560 A CN108570560 A CN 108570560A CN 201810597521 A CN201810597521 A CN 201810597521A CN 108570560 A CN108570560 A CN 108570560A
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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
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0078—Leaching or slurrying with ammoniacal solutions, e.g. ammonium hydroxide
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
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- C—CHEMISTRY; METALLURGY
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The method that the invention discloses a kind of to recycle copper from copper-bearing waste material, copper-bearing waste material is crushed to 20 mesh or more, then use the mixed solution of copper sulphate, ammonium hydroxide and ammonium sulfate as leaching agent, and air is passed through as oxidant, leaching is for a period of time under certain solid-to-liquid ratio, certain temperature, certain rotating speed, selectively leach the copper in copper-bearing waste material, obtain the leachate of cupric, leachate is extracted using extract liquor, it is used in combination dilution heat of sulfuric acid to be stripped, the copper-bath of high concentration is obtained, high purity copper is obtained finally by electrolysis.After extraction process, obtained aqueous phase extracted is the mixed liquor of copper sulphate, ammonium hydroxide and ammonium sulfate, may return to and is continuing with to the leaching stage of copper-bearing waste material；Extract liquor returns to extraction stages and is continuing with after back extraction；After electrolysis due to electrolyte in sulfuric acid concentration it is higher, concentration of copper sulfate is relatively low, can be back to strip stages and be continuing with.Closed cycle is realized in entire technological process, reduces " three wastes " pollution and cost, and the rate of recovery of copper is high.
Description
Technical field
The invention belongs to metal extraction techniques field more particularly to a kind of methods recycling copper from copper-bearing waste material.
Background technology
Mostly use the valuable metals such as lead, copper, silver in acid leaching process and thermal process recycling copper-bearing waste material greatly both at home and abroad at present
Acid leaching process：It can be acted under certain condition with strong acid such as nitric acid, the concentrated sulfuric acids using copper, become soluble-salt and enter aqueous solution
In and achieve the purpose that detach with other insoluble substances, can be obtained later by the precipitation method, displacement method, electrolysis different
Copper product.Advantage is that selectivity is good, and low energy consumption, and leaching effect is good, and production equipment is simple, easy to operate.The disadvantage is that using a large amount of
Toxic, harmful, strong corrosive reagent, liquid waste processing is costly and than more intractable, if direct emission, or deal with improperly very
It may cause secondary pollution, there are serious environmental threat, sour consumption is larger, while also can be one to the corrosion of equipment
Prodigious problem.
Thermal process：Stripping nonmetallic substance is heated using metallurgical furnace high temperature, then obtains composition brass material, uses pyrogenic process essence later
The method of refining is refined.Purpose is to obtain meeting the copper anode plate that electrolysis requires.Advantage is that noble metal loss is few, operation letter
It is single.The disadvantage is that the gas of discharge can pollute air, high energy consumption influences the quality of electrorefining product.In addition, the pottery in copper junk
Porcelain and glass ingredient be easy to cause certain metals and are wrapped in wherein and can not recycle.In addition, a large amount of Non-metallic components are burning
It loses in the process and is unable to get effective utilize etc..
Invention content
The method that the technical problem to be solved by the invention is to provide a kind of to recycle copper from copper-bearing waste material, the method energy
Enough effectively by the copper in copper-bearing waste material at high purity copper.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：It is a kind of to recycle copper from copper-bearing waste material
Method includes the following steps：
Step 1, leaching process
Copper-bearing waste material is crushed to 20 mesh or more, using the mixed solution of copper sulphate, ammonium hydroxide and ammonium sulfate as leaching agent,
And air is passed through as oxidant, 20-30 DEG C of temperature stirring a period of time, obtain the leachate of cupric；Wherein, in mixed solution
Copper ion concentration is 37g/L-48g/L, ammonia concn 4-6mol/L, ammonium sulfate concentrations 0.5-1.5mol/L, in copper junk
The quality of copper content：The mixed solution quality of (copper sulphate+ammonium hydroxide+ammonium sulfate) is 1:30-60；
Step 2, extraction process
The leachate of the cupric obtained in step 1 is extracted using extract liquor, isolated load is organic after standing
Phase and aqueous phase extracted；Extract liquor includes extractant and diluent, and extractant is N910 extractants, and diluent is 260# kerosene；Extraction
Water intaking mutually adds a certain amount of ammonium hydroxide return to step one and is continuing with as leaching agent；
Step 3, stripping process
Load organic phases in step 2 are stripped with dilute sulfuric acid, obtain copper-rich liquid and organic phase；Organic phase returns
Step 2 is continuing with as extract liquor；
Step 4, electrolytic process
It is electrolysed the copper-rich liquid in step 3 to obtain high purity copper；The waste electrolyte that electrolysis generates is sulfuric acid and copper sulphate
Mixed liquor, return to step three is stripped instead of dilute sulfuric acid.
Mixing speed is 750-1250r/min in the step 1, extraction time is 150-180 minutes.
In the step 2, extractant in extract N910 concentration of volume percent is 30%-40%, is 1 compared to O/A:
1。
In the step 2, aqueous phase extracted is added return to step one after a certain amount of ammonium hydroxide makes pH value of solution reach 10.9-12 and makees
It is continuing with for leaching agent.
In the step 3 stripping process, sulfuric acid concentration 2.5-3.5mol/L is 1 compared to O/A:1.
The beneficial effects of the invention are as follows：The present invention is strong to the selectively leaching of copper, and leaching efficiency is high, easy to operate, consumption
The energy is few, and the raw material of leachate is simple, is easy purchase, and cheap, entire technological process can realize closed cycle, drop significantly
It is low " three wastes " pollution and cost of material carry out under alkaline condition due to leaching, thus the cost of manufacture of leaching equipment than
Acid system is cheap, has input cost few, blowdown advantage at low cost.
Description of the drawings
Fig. 1 is the process flow chart for the method that the present invention recycles copper from copper-bearing waste material.
Specific implementation mode
Invention is further described in detail with reference to the accompanying drawings and detailed description：
As shown in Figure 1, the method for recycling copper in the slave copper-bearing waste material of the present invention, includes the following steps：
Step 1, leaching process
Copper-bearing waste material is crushed to 20 mesh or more, using the mixed solution of copper sulphate, ammonium hydroxide and ammonium sulfate as leaching agent,
And air is passed through as oxidant, 20-30 DEG C of temperature stirring a period of time, obtain the leachate of cupric；Wherein, in mixed solution
Copper ion concentration is 37g/L-48g/L, ammonia concn 4-6mol/L, ammonium sulfate concentrations 0.5-1.5mol/L, in copper junk
The quality of copper content：The mixed solution quality of (copper sulphate+ammonium hydroxide+ammonium sulfate) is 1:30-60；
Step 2, extraction process
The leachate of the cupric obtained in step 1 is extracted using extract liquor, isolated load is organic after standing
Phase and aqueous phase extracted；Extract liquor includes extractant and diluent, and extractant is N910 extractants, and diluent is 260# kerosene；Extraction
Water intaking mutually adds a certain amount of ammonium hydroxide return to step one and is continuing with as leaching agent；
Step 3, stripping process
Load organic phases in step 2 are stripped with dilute sulfuric acid, obtain copper-rich liquid and organic phase；Organic phase returns
Step 2 is continuing with as extract liquor；
Step 4, electrolytic process
It is electrolysed the copper-rich liquid in step 3 to obtain high purity copper；The waste electrolyte that electrolysis generates is sulfuric acid and copper sulphate
Mixed liquor, return to step three is stripped instead of dilute sulfuric acid.
Mixing speed is 750-1250r/min in the step 1, extraction time is 150-180 minutes.
In the step 2, extractant in extract N910 concentration of volume percent is 30%-40%, is 1 compared to O/A:
1。
In the step 2, aqueous phase extracted is added return to step one after a certain amount of ammonium hydroxide makes pH value of solution reach 10.9-12 and makees
It is continuing with for leaching agent.
In the step 3 stripping process, sulfuric acid concentration 2.5-3.5mol/L is 1 compared to O/A:1.
After the extraction process of the present invention, obtained aqueous phase extracted is the mixed liquor of copper sulphate, ammonium hydroxide and ammonium sulfate,
In the case of a certain amount of ammonium hydroxide is added, it may return to and be continuing with that (leachate is 20 times recyclable to the leaching stage of copper-bearing waste material
More than)；Extract liquor returns to extraction stages and is continuing with (extract liquor is 10 times or more recyclable) after back extraction；Terminate in electrolysis
Afterwards due in electrolyte sulfuric acid concentration it is higher, concentration of copper sulfate is relatively low, it is possible to be back to strip stages and be continuing with.Entirely
Closed cycle may be implemented in technological process, greatly reduces " three wastes " pollution and cost, and the rate of recovery of copper is high.
In leaching process of the present invention, copper leaching rate can reach 99%；In extraction process, the extraction yield of copper is 40-50%, instead
During extraction, back extraction ratio 99%.
The present invention is strong to the selectively leaching of copper, and leaching efficiency is high, easy to operate, and the consumption energy is few, the raw material of leachate
Simply, it is easy purchase, and cheap, entire technological process can realize closed cycle, greatly reduce " three wastes " pollution and original
Expect cost, carried out under alkaline condition due to leaching, so the cost of manufacture of leaching equipment is cheaper than acid system, have input at
This is few, blowdown advantage at low cost.
Embodiment 1
Step 1：The volumetric flask of 1000ml is taken, the copper sulphate 92.5g that purity is 99.9% is added thereto, purity is added
For 99.9% ammonium sulfate 66g, the ammonium hydroxide 272g that mass concentration is 25% is added, is eventually adding distilled water to graduation mark, configuration
At the leachate that copper ion concentration is 37g/L, ammonia concn 4mol/L, ammonium sulfate concentrations are 0.5mol/L, match according to this method
It is for use to set several leachates.
Step 2：0.5kg copper-bearing waste materials (cupric 72%, plastics 28%) are crushed to 20 mesh or more, 10.8kg is added and matches
The leachate set, is passed through air, and at 20 DEG C, mixing speed leaches 150min under conditions of being 750r/min, obtains cupric leaching
Go out liquid 10L and filter residue, the copper factor of residue is measured by ICP-AES Atomic Absorption Spectrometers, obtains the cupric of residue
By formula, (formula is rate：(copper leaching rate=(copper factor of 0.5*72%- mass of residue * residues)/0.5*72%) calculates
Copper leaching rate is up to 96%.
Step 3：The copper ion concentration of cupric leachate is measured by atomic spectrophotometer, then will be obtained in step 2
To cupric leachate in be added 10L extract liquors extracted (in extract liquor the volumetric concentration of N910 extractants be 30%, 260#
Kerosene volumetric concentration be 70%), low whipping speed 500r/min, extract 6min, after being layered separating and extracting water phase and load have
Machine phase measures the copper ion concentration of aqueous phase extracted by atomic spectrophotometer, and by formula, (formula is：1- aqueous phase extracteds
The copper ion concentration of copper ion concentration/cupric leachate) calculate copper extraction yield be 38%, aqueous phase extracted be added mass concentration
For 25% ammonium hydroxide so that pH value of solution is reached 10.9 after return leaching process be continuing with as leaching agent.
Step 4：The 10L dilute sulfuric acids of load organic phases 10L and a concentration of 2.5mol/L in step 3 are stripped；
Mixing speed is 800r/min, extraction time 6min, and 10L copper-rich liquid and 10L organic phases are obtained after being layered, and passes through atom point
Light photometer measures the copper ion concentration of copper-rich liquid, and by formula, (formula is：Copper-rich liquid copper ion concentration/(cupric leachate
The copper ion concentration of copper ion concentration-aqueous phase extracted)) calculate back extraction ratio be 95%；Three conduct of organic phase return to step
Extract liquor is continuing with；
Step 5：By the copper-rich liquid in step 4 current density be 150A/m2Under conditions of electrolysis 3h obtain purity and be
99% high purity copper 150g, the waste electrolyte for being electrolysed generation is the mixed liquor of sulfuric acid and copper sulphate, and return to step four replaces dilute sulphur
Acid is stripped.
Embodiment 2
Step 1：The volumetric flask of 1000ml is taken, the copper sulphate 107.5g that purity is 99.9% is added thereto, purity is added
For 99.9% ammonium sulfate 132g, the ammonium hydroxide 340g that mass concentration is 25% is added, is eventually adding distilled water to graduation mark, configuration
At the leachate that copper ion concentration is 43g/L, ammonia concn 5mol/L, ammonium sulfate concentrations are 1mol/L, configured according to this method
Several leachates are for use.
Step 2：0.5kg copper-bearing waste materials (cupric 63%, iron 37%) are crushed to 20 mesh or more, 12.6kg configurations are added
Good leachate, is passed through air, and at 25 DEG C, mixing speed leaches 180min under conditions of being 1000r/min, obtains cupric leaching
Liquid 12L and filter residue measure the copper factor of residue by ICP-AES Atomic Absorption Spectrometers, obtain the copper factor of residue
By formula, (formula is：(copper leaching rate=(copper factor of 0.5*63%- mass of residue * residues)/0.5*63%) calculates copper
Leaching rate is up to 99%.
Step 3：The copper ion concentration of cupric leachate is measured by atomic spectrophotometer, then will be obtained in step 2
To cupric leachate in be added 12L extract liquors extracted (in extract liquor the volumetric concentration of N910 extractants be 35%, 260#
Kerosene volumetric concentration be 65%), low whipping speed 500r/min, extract 5min, after being layered separating and extracting water phase and load have
Machine phase measures the copper ion concentration of aqueous phase extracted by atomic spectrophotometer, and by formula, (formula is：1- be (aqueous phase extracted
The copper ion concentration of copper ion concentration/cupric leachate)) calculate copper extraction yield be 36.8%, aqueous phase extracted be added quality
A concentration of 25% ammonium hydroxide returns to leaching process after so that pH value of solution is reached 11.6 and is continuing with as leaching agent.
Step 4：The 12L dilute sulfuric acids of load organic phases 12L and a concentration of 3mol/L in step 3 are stripped；It stirs
Mix speed be 800r/min, extraction time 5min, 12L copper-rich liquid and 12L organic phases are obtained after being layered, is divided by atom
Photometer measures the copper ion concentration of copper-rich liquid, and by formula, (formula is：The copper-rich liquid copper ion concentration/(copper of cupric leachate
The copper ion concentration of ion concentration-aqueous phase extracted)) calculate back extraction ratio be 99%；The organic phase return to step three is as extraction
Liquid is taken to be continuing with；
Step 5：By the copper-rich liquid in step 4 current density be 150A/m2Under conditions of electrolysis 3h obtain purity and be
99% high purity copper 151.5g, the waste electrolyte for being electrolysed generation is the mixed liquor of sulfuric acid and copper sulphate, and return to step four replaces dilute
Sulfuric acid is stripped.
Embodiment 3
Step 1：The volumetric flask of 1000ml is taken, the copper sulphate 120g that purity is 99.9% is added thereto, purity, which is added, is
99.9% ammonium sulfate 198g is added the ammonium hydroxide 408g that mass concentration is 25%, is eventually adding distilled water to graduation mark, is configured to
The leachate that copper ion concentration is 48g/L, ammonia concn 6mol/L, ammonium sulfate concentrations are 1.5mol/L is configured according to this method
Several leachates are for use.
Step 2：0.5kg copper-bearing waste materials (cupric 63%, iron 37%) are crushed to 20 mesh or more, 18.9kg configurations are added
Good leachate, is passed through air, and at 30 DEG C, mixing speed leaches 180min under conditions of being 1250r/min, obtains cupric leaching
Liquid 18.5L and filter residue measure the copper factor of residue by ICP-AES Atomic Absorption Spectrometers, obtain the cupric of residue
By formula, (formula is rate：(copper leaching rate=(copper factor of 0.5*63%- mass of residue * residues)/0.5*63%) calculates
Copper leaching rate is up to 99%.
Step 3：The copper ion concentration of cupric leachate is measured by atomic spectrophotometer, then will be obtained in step 2
To cupric leachate in be added 18.5L extract liquors extracted (in extract liquor the volumetric concentration of N910 extractants be 40%,
260# kerosene volumetric concentrations be 60%), low whipping speed 500r/min, extract 4min30s, after being layered separating and extracting water phase and
Load organic phases measure the copper ion concentration of aqueous phase extracted by atomic spectrophotometer, and by formula, (formula is：1- (extractions
The copper ion concentration of the copper ion concentration of water phase/cupric leachate)) calculate copper extraction yield be 25.7%, extraction water be added
Enter mass concentration be 25% ammonium hydroxide so that pH value of solution is reached 12 after return leaching process be continuing with as leaching agent.
Step 4：The 18.5L dilute sulfuric acids of load organic phases 18.5L and a concentration of 3.5mol/L in step 3 are carried out anti-
Extraction；Mixing speed is 800r/min, extraction time 45s, and 18.5L copper-rich liquid and 18.5L organic phases are obtained after being layered, is passed through
Atomic spectrophotometer measures the copper ion concentration of copper-rich liquid, and by formula, (formula is：Copper-rich liquid copper ion concentration/(cupric soaks
Go out the copper ion concentration of copper ion concentration-aqueous phase extracted of liquid)) calculate back extraction ratio be 99%；The organic phase return to step
Three are continuing with as extract liquor；
Step 5：By the copper-rich liquid in step 4 current density be 150A/m2Under conditions of electrolysis 3h obtain purity and be
99% high purity copper 144g, the waste electrolyte for being electrolysed generation is the mixed liquor of sulfuric acid and copper sulphate, and return to step four replaces dilute sulphur
Acid is stripped.
In conclusion present disclosure is not limited in the above embodiments, the knowledgeable people in same area can
Can propose other embodiments easily within the technological guidance's thought of the present invention, but this embodiment is included in this hair
Within the scope of bright.
Claims (5)
1. a kind of method recycling copper from copper-bearing waste material, which is characterized in that include the following steps：
Step 1, leaching process
Copper-bearing waste material is crushed to 20 mesh or more, using the mixed solution of copper sulphate, ammonium hydroxide and ammonium sulfate as leaching agent, and is led to
Enter air as oxidant, 20-30 DEG C of temperature stirring a period of time, obtains the leachate of cupric；Wherein, in mixed solution copper from
A concentration of 37g/L-48g/L of son, ammonia concn 4-6mol/L, ammonium sulfate concentrations 0.5-1.5mol/L, cupric in copper junk
The quality of amount：The mixed solution quality of (copper sulphate+ammonium hydroxide+ammonium sulfate) is 1:30-60；
Step 2, extraction process
The leachate of the cupric obtained in step 1 is extracted using extract liquor, after standing isolated load organic phases and
Aqueous phase extracted；Extract liquor includes extractant and diluent, and extractant is N910 extractants, and diluent is 260# kerosene；Extraction water
A certain amount of ammonium hydroxide return to step one is mutually added to be continuing with as leaching agent；
Step 3, stripping process
Load organic phases in step 2 are stripped with dilute sulfuric acid, obtain copper-rich liquid and organic phase；Organic phase return to step
Two are continuing with as extract liquor；
Step 4, electrolytic process
It is electrolysed the copper-rich liquid in step 3 to obtain high purity copper；The waste electrolyte that electrolysis generates is the mixed of sulfuric acid and copper sulphate
Liquid is closed, return to step three is stripped instead of dilute sulfuric acid.
2. the method for recycling copper from copper-bearing waste material according to claim 1, which is characterized in that stir speed in the step 1
Degree is 750-1250r/min, extraction time is 150-180 minutes.
3. the method for recycling copper from copper-bearing waste material according to claim 1, which is characterized in that in the step 2, extraction
Extractant N910 concentration of volume percent is 30%-40% in liquid, is 1 compared to O/A:1.
4. the method for recycling copper from copper-bearing waste material according to claim 1, which is characterized in that in the step 2, extraction
Water phase is added return to step one after a certain amount of ammonium hydroxide makes pH value of solution reach 10.9-12 and is continuing with as leaching agent.
5. the method for recycling copper from copper-bearing waste material according to claim 1, which is characterized in that the step 3 stripping process
In, sulfuric acid concentration 2.5-3.5mol/L is 1 compared to O/A:1.
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| CN110029009A (en) * | 2019-04-19 | 2019-07-19 | 金陵科技学院 | It is a kind of to utilize waste and old circuit board recycling copper nanoparticle and selfreparing preparation of greases method |
| CN110759373A (en) * | 2019-10-16 | 2020-02-07 | 长春黄金研究院有限公司 | Method for producing copper sulfate by using low-grade copper oxide ore |
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| CN113136604A (en) * | 2021-03-25 | 2021-07-20 | 深圳市祺鑫环保科技有限公司 | Copper recovery process |
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| CN110029009A (en) * | 2019-04-19 | 2019-07-19 | 金陵科技学院 | It is a kind of to utilize waste and old circuit board recycling copper nanoparticle and selfreparing preparation of greases method |
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| CN113136604A (en) * | 2021-03-25 | 2021-07-20 | 深圳市祺鑫环保科技有限公司 | Copper recovery process |
| CN113136604B (en) * | 2021-03-25 | 2022-09-16 | 深圳市祺鑫环保科技有限公司 | Copper recovery process |
| CN113604669A (en) * | 2021-07-21 | 2021-11-05 | 申能环境科技有限公司 | Method for selectively recovering copper and nickel from electroplating nickel-containing sludge |
| CN115747882A (en) * | 2022-12-06 | 2023-03-07 | 西安诺博尔稀贵金属材料股份有限公司 | Method for recovering molybdenum and copper from molybdenum-copper alloy waste |
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Application publication date: 20180925 |