CN106191919A - A kind of technique reclaiming copper from brown oxide waste liquid - Google Patents
A kind of technique reclaiming copper from brown oxide waste liquid Download PDFInfo
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- CN106191919A CN106191919A CN201610548758.8A CN201610548758A CN106191919A CN 106191919 A CN106191919 A CN 106191919A CN 201610548758 A CN201610548758 A CN 201610548758A CN 106191919 A CN106191919 A CN 106191919A
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- waste liquid
- copper
- oxide waste
- brown oxide
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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 invention discloses a kind of technique reclaiming copper from brown oxide waste liquid, it comprises the steps: a, adds additive in brown oxide waste liquid, the quality of additive accounts for 5 ‰ the 2% of brown liquid quality, by percentage to the quality, additive includes that the complex of 0.01 20% substitutes salt, the surfactant of 0.01 10%, the leveling agent of 0.1 5%, and surplus is solvent；It is electrolysed while b, stirring, obtains copper simple substance.The hydrogen peroxide in brown liquid is removed by the way of adding additive to brown liquid and use electrolysis, its concentration is made to be reduced to an acceptable scope, at this moment the cation during complex substitutes salt swaps with the copper ion being complexed to replace the form with Organic substance complexation in the solution, the copper ion being displaced under the effect of electric current by electrolytic deposition out, become copper simple substance, this method organic efficiency is high, technological process is simple, without the heating that heats up, energy-saving and emission-reduction, do not produce solid waste and cause secondary pollution, without follow-up further process, simplify treatment process.
Description
Technical field
The invention belongs to technical field of resource recovery, relate in particular to a kind of technique reclaiming copper from brown liquid.
Background technology
In printed circuit board (PCB) production process, in order to prevent the copper face of internal layer circuit plate from aoxidizing and strengthening pressing
Adhesion in journey, need to use brown treatment technology to improve the stability of inner plating, and brown technology is by containing sulphuric acid
With the brown liquid of hydrogen peroxide etc. PCB copper face carried out microetch, and under organic additive participates in, form one layer increase interlayer pressing
Performance and the brown film of protection copper face.Containing many toxic organic compounds in brown liquid, such as triazole, polyethylene glycols etc., copper from
The easy formed coordination compound of son.When content of copper ion constantly rises, after exceeding certain limit, brown copper face will be affected and cause copper
Turning white and the unequal quality problem of color and luster in face, it is necessary to adjusts brown tank liquor in time and discharge, thereby produce a large amount of brown and give up
Liquid.
Containing harmful toxic matters such as a large amount of copper ions, triazoles in brown oxide waste liquid, can be to raw as processed not up to emission request
State environment brings high risks, particularly heavy metal copper ion, and it is the noxious substance of a kind of difficult degradation, easily micro-by water body
Biological and algae absorbs and passes through nutrition accumulation and biological chain harm animals and plants and the mankind.Therefore for solve in brown oxide waste liquid copper from
The problem of son harm, recovery copper resource, the most worked out multiple processing method, mainly included chemical deposition method, electrolysis, suction
Attached method, ion exchange, extraction etc..Wherein chemical deposition method needs to add that to have the complex of strong sequestering power relatively low at pH
In the environment of obtain copper precipitation, add technological process and equipment investment, other technique generally require intensification run, add energy
Consumption, the precipitation that reaction produces too increases substantial amounts of solid waste, subsequent treatment adds some technological difficulty.And
And owing to the bivalent cupric ion in brown oxide waste liquid is together with the Organic substance complexation in solution, its chemical property is more steady
Fixed, it is not easy to directly being electrolysed out, prior art there is also the problem that copper ion organic efficiency is relatively low.
Summary of the invention
To this end, the technical problem to be solved is existing copper ion recovery technology process complexity, processing cost
High, organic efficiency is low and there is solid waste causes secondary pollution, thus propose a kind of with low cost, technique simple, reclaim
Efficiency is high, the technique reclaiming copper from brown oxide waste liquid of non-secondary pollution.
For solving above-mentioned technical problem, the technical scheme is that
The present invention provides a kind of technique reclaiming copper from brown oxide waste liquid, and it comprises the steps:
A, in brown oxide waste liquid add additive, the quality of described additive accounts for 5 ‰-the 2% of described brown liquid quality, with
Mass percent, described additive includes that the complex of 0.01-20% substitutes salt, the surfactant of 0.01-10%, 0.1-
The leveling agent of 5%, surplus is solvent；
Being electrolysed while the mixture that b, whipping step a obtain, in electrolytic process, electric current density is 150-400A/m2,
To copper simple substance.
As preferably, it is at least one in inorganic metal salt, organic metal salt that described complex substitutes salt.
As preferably, described inorganic metal salt is sulfate, halogenide, nitrate, chlorate, manganate, sulphite
In at least one.
As preferably, described organic metal salt be formates, acetate, propionate, butyrate, oxalates, citrate,
At least one in sulfonate, sulfinate, sulfur carboxylic salt.
As preferably, the metal ion in described inorganic metal salt, organic metal salt be sodium ion, potassium ion, iron ion,
At least one in manganese ion, aluminium ion, calcium ion, magnesium ion, zinc ion, nickel ion.
As preferably, described surfactant and described leveling agent be Triaethanolamine, polyethyleneimine amino-compound,
In pyridinium hydroxy propyl sulfobetaine, alkylphenol polyoxyethylene, sodium lauryl sulphate and nonyl polyoxyethylene ether at least
A kind of.
As preferably, described solvent is water.
As preferably, described step b also includes the step inflated.
As preferably, in described step b, the speed of stirring is 15-550L/min.
The technique scheme of the present invention has the advantage that compared to existing technology
The technique reclaiming copper from brown oxide waste liquid of the present invention, it comprises the steps: a, adds in brown oxide waste liquid
Entering additive, the quality of described additive accounts for 5 ‰-the 2% of described brown liquid quality, by percentage to the quality, described additive
Complex including 0.01-20% substitutes salt, the surfactant of 0.01-10%, the leveling agent of 0.1-5%, and surplus is solvent；
Being electrolysed while b, stirring, in electrolytic process, electric current density is 150-400A/m2, obtain copper simple substance.By adding in brown liquid
Add complex and substitute salt, surfactant and leveling agent, copper complex is destroyed, and uses the mode of electrolysis to remove palm fibre
Changing the hydrogen peroxide in liquid so that it is concentration is reduced to an acceptable scope, the cation during at this moment complex substitutes salt exists
Swapping to replace the form with Organic substance complexation with the copper ion being complexed in solution, the copper ion being displaced is at electric current
Effect under by electrolytic deposition out, become copper simple substance, the copper simple substance that electrolysis gone out is collected and is dried, and this method is due to first general
Copper ion is replaced in inorganic or organic salt, is more prone to be electrolysed, and organic efficiency is high, and technological process is simple, it is not necessary to heats up and adds
Heat, energy-saving and emission-reduction, and do not produce solid waste and cause secondary pollution, it is not necessary to follow-up further process, simplify place's science and engineering
Sequence.
Detailed description of the invention
In order to make present disclosure be more likely to be clearly understood, below according to the specific embodiment of the present invention to this
Bright it is described in further detail.
Embodiment 1
The present embodiment provides a kind of technique reclaiming copper from brown oxide waste liquid, and it comprises the steps:
A, in brown oxide waste liquid add additive, the quality of described additive accounts for the 5 ‰ of described brown liquid quality, with quality
Percentages, described additive includes that the complex of 0.01% substitutes salt, the surfactant of 0.01%, the leveling agent of 0.1%,
Surplus is solvent, and it is magnesium sulfate that described complex substitutes salt, and described surfactant is Triaethanolamine, and described leveling agent is poly-
Aziridinyl compound--PVOH amine, described solvent is water；
B, electrolysis while the mixing speed stirring of 15L/min, in whipping process, also inflate, to add in electrolysis bath
Strong mixing, promotes that in solution, various ions can be stirred after localized concentrations under the function of current again, electricity in electrolytic process
Current density is 150A/m2, peel the copper of negative electrode drying after being electrolysed to copper simple substance.
Embodiment 2
The present embodiment provides a kind of technique reclaiming copper from brown oxide waste liquid, and it comprises the steps:
A, in brown oxide waste liquid add additive, the quality of described additive accounts for the 1% of described brown liquid quality, with quality
Percentages, described additive includes that the complex of 20% substitutes salt, the surfactant of 10%, the leveling agent of 5%, and surplus is
Solvent, it is sodium chloride and zinc nitrate that described complex substitutes salt, and wherein sodium chloride accounts for described complex and substitutes salt gross mass
30%, described surfactant is sodium lauryl sulphate, and described leveling agent is pyridinium hydroxy propyl sulfobetaine, described solvent
For water；
B, electrolysis while the mixing speed stirring of 550L/min, in whipping process, also inflate, to add in electrolysis bath
Strong mixing, promotes that in solution, various ions can be stirred after localized concentrations under the function of current again, electricity in electrolytic process
Current density is 400A/m2, peel the copper of negative electrode drying after being electrolysed to copper simple substance.
Embodiment 3
The present embodiment provides a kind of technique reclaiming copper from brown oxide waste liquid, and it comprises the steps:
A, in brown oxide waste liquid add additive, by percentage to the quality, described additive include 1% complex substitute
Salt, the surfactant of 5.0%, the leveling agent of 0.8%, surplus is solvent, and it is calcium formate and oxalic acid that described complex substitutes salt
Nickel, wherein calcium formate accounts for described complex and substitutes the 50% of salt gross mass, and described surfactant is nonyl polyoxyethylene ether, institute
Stating leveling agent is alkylphenol polyoxyethylene, and described solvent is water；
B, electrolysis while the mixing speed stirring of 50L/min, in whipping process, also inflate, to add in electrolysis bath
Strong mixing, promotes that in solution, various ions can be stirred after localized concentrations under the function of current again, electricity in electrolytic process
Current density is 300A/m2, peel the copper of negative electrode drying after being electrolysed to copper simple substance.
Embodiment 4
The present embodiment provides a kind of technique reclaiming copper from brown oxide waste liquid, and it comprises the steps:
A, in brown oxide waste liquid add additive, by percentage to the quality, described additive includes that the complex of 10% replaces
For salt, the surfactant of 2%, the leveling agent of 2%, surplus is solvent, described complex substitute salt be potassium chlorate, butanoic acid aluminum,
The mixture of manganese citrate, wherein potassium chlorate accounts for described complex and substitutes the 50% of salt gross mass, and described butanoic acid aluminum accounts for described network
Compound substitutes the 5% of salt gross mass, and remaining is manganese citrate, and described surfactant is alkylphenol polyoxyethylene, described whole
Flat agent is alkylphenol polyoxyethylene, and described solvent is water；
B, electrolysis while the mixing speed stirring of 25L/min, in whipping process, also inflate, to add in electrolysis bath
Strong mixing, promotes that in solution, various ions can be stirred after localized concentrations under the function of current again, electricity in electrolytic process
Current density is 250A/m2, peel the copper of negative electrode drying after being electrolysed to copper simple substance.
Embodiment 5
The present embodiment provides a kind of technique reclaiming copper from brown oxide waste liquid, and it comprises the steps:
A, in brown oxide waste liquid add additive, by percentage to the quality, described additive includes that the complex of 16% replaces
For salt, the surfactant of 1%, the leveling agent of 4%, surplus is solvent, and it is aluminium potassium sulfate and sulfur carboxylic that described complex substitutes salt
Magnesium, wherein aluminium potassium sulfate accounts for described complex and substitutes the 25% of salt gross mass, and described surfactant is sodium lauryl sulphate,
Described leveling agent is pyridinium hydroxy propyl sulfobetaine, and described solvent is water；
B, electrolysis while the mixing speed stirring of 50L/min, in whipping process, also inflate, to add in electrolysis bath
Strong mixing, promotes that in solution, various ions can be stirred after localized concentrations under the function of current again, electricity in electrolytic process
Current density is 300A/m2, peel the copper of negative electrode drying after being electrolysed to copper simple substance.
Embodiment 6
The present embodiment provides a kind of technique reclaiming copper from brown oxide waste liquid, and it comprises the steps:
A, in brown oxide waste liquid add additive, by percentage to the quality, described additive includes that the complex of 11% replaces
For salt, the surfactant of 1.2%, the leveling agent of 3.5%, surplus is solvent, described complex substitute salt be magnesium chloride potassium and
Butanoic acid zinc-aluminium, wherein magnesium chloride potassium accounts for described complex and substitutes the 38% of salt gross mass, and described surfactant is nonyl polyoxy
Vinyl Ether, described leveling agent is alkylphenol polyoxyethylene, and described solvent is water；
B, electrolysis while the mixing speed stirring of 45L/min, in whipping process, also inflate, to add in electrolysis bath
Strong mixing, promotes that in solution, various ions can be stirred after localized concentrations under the function of current again, electricity in electrolytic process
Current density is 200A/m2, peel the copper of negative electrode drying after being electrolysed to copper simple substance.
Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.Right
For those of ordinary skill in the field, can also make on the basis of the above description other multi-form change or
Variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or
Change among still in the protection domain of the invention.
Claims (9)
1. the technique reclaiming copper from brown oxide waste liquid, it is characterised in that comprise the steps:
A, in brown oxide waste liquid add additive, the quality of described additive accounts for 5 ‰-the 2% of described brown liquid quality, with quality
Percentages, described additive includes that the complex of 0.01-20% substitutes salt, the surfactant of 0.01-10%, 0.1-5%
Leveling agent, surplus is solvent；
Being electrolysed while the mixture that b, whipping step a obtain, in electrolytic process, electric current density is 150-400A/m2, obtain copper list
Matter.
The technique reclaiming copper from brown oxide waste liquid the most according to claim 1, it is characterised in that described complex substitutes salt
For at least one in inorganic metal salt, organic metal salt.
The technique reclaiming copper from brown oxide waste liquid the most according to claim 2, it is characterised in that described inorganic metal salt is
At least one in sulfate, halogenide, nitrate, chlorate, manganate, sulphite.
The technique reclaiming copper from brown oxide waste liquid the most according to claim 2, it is characterised in that described organic metal salt is
In formates, acetate, propionate, butyrate, oxalates, citrate, sulfonate, sulfinate, sulfur carboxylic salt at least one
Kind.
The technique reclaiming copper from brown oxide waste liquid the most according to claim 2, it is characterised in that described inorganic metal salt,
Metal ion in organic metal salt be sodium ion, potassium ion, iron ion, manganese ion, aluminium ion, calcium ion, magnesium ion, zinc from
At least one in son, nickel ion.
6. according to the technique reclaiming copper from brown oxide waste liquid described in any one of claim 2-5, it is characterised in that described surface
Activating agent and described leveling agent are Triaethanolamine, polyethyleneimine amino-compound, pyridinium hydroxy propyl sulfobetaine, alkyl
At least one in phenol polyethenoxy ether, sodium lauryl sulphate and nonyl polyoxyethylene ether.
The technique reclaiming copper from brown oxide waste liquid the most according to claim 6, it is characterised in that described solvent is water.
The technique reclaiming copper from brown oxide waste liquid the most according to claim 7, it is characterised in that also wrap in described step b
Include the step inflated.
The technique reclaiming copper from brown oxide waste liquid the most according to claim 8, it is characterised in that stir in described step b
Speed be 15-550L/min.
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| CN201610548758.8A CN106191919A (en) | 2016-07-13 | 2016-07-13 | A kind of technique reclaiming copper from brown oxide waste liquid |
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| CN201610548758.8A CN106191919A (en) | 2016-07-13 | 2016-07-13 | A kind of technique reclaiming copper from brown oxide waste liquid |
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Cited By (3)
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| CN105839140A (en) * | 2014-09-29 | 2016-08-10 | 马丽 | Method for electrolysis recovery of metal from metal-containing organic matter |
| CN110106523A (en) * | 2019-05-13 | 2019-08-09 | 深圳市祺鑫天正环保科技有限公司 | The method of copper is recycled from brown oxide waste liquid |
| CN112573726A (en) * | 2020-11-24 | 2021-03-30 | 苏州美源达环保科技股份有限公司 | Brown liquid wastewater treatment method |
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Application publication date: 20161207 |