CN103510107B - A kind of method reclaiming copper from brown oxide waste liquid - Google Patents
A kind of method reclaiming copper from brown oxide waste liquid Download PDFInfo
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Abstract
The invention discloses a kind of method reclaiming copper from brown oxide waste liquid, in the scope of temperature 30 ~ 100 DEG C, alkaline matter is added in brown oxide waste liquid, make the pH of waste liquid in the scope of 2 ~ 3 by the add-on controlling alkaline matter, then filter, in filtrate, add electrolysis additive again, at 30 ~ 60 DEG C, carry out electrolysis.The copper in brown oxide waste liquid can be reclaimed by the present invention efficiently, reduce heavy metal contamination; In the present invention, copper recovery reaches 99%, and after process, copper content is at below 100mg/L.After reclaiming copper, in brown oxide waste liquid, the subsequent treatment cost of organic waste reduces greatly.
Description
Technical field
The invention belongs to resource reclaim and clearer production technology field, be specifically related to a kind of method reclaiming copper from brown oxide waste liquid.
Background technology
Printed-wiring board (PWB) (PCB) ensures that various electronic component forms the platform of electric interconnection.The polymeric substrate used in PCB can be the epoxy resin that glass-fiber-fabric strengthens, or the polymkeric substance such as phenol, polymeric amide, also can be other resins etc.By covering the thin copper of one deck at polymeric substrate single or double, copper face covering photoresist material, after exposure, development, etching, line pattern can be formed on copper face, so can produce the wiring board of single or double.Because single dual platen provides the density of electric interconnection very limited, so developed now widely used multilayer circuit board.Above-mentioned dual platen, also known as inner plating, is piled up dual platen get up, is separated, after hot pressing, form multi-ply wood between dual platen with the resin of semicure.In order to realize the electric interconnection between each laminate, need to bore via, blind hole or buried via hole.
In multiple-plate making, the traditional process of surface treatment of inner layer circuit board is melanism (BlackOxide).Along with the demand with market that develops rapidly of PCB industry, PCB enterprise in manufacturing technology constantly to while high precision, light weight, slim future development, also making great efforts to raise the efficiency, reduce costs, environmental protect, and adapt to the demand of multi items, small serial production, and traditional blackening craft is difficult to realize level production, and it makes the ability of thin plate, long flow path, technology controlling and process is complicated, operating environment is poor, cost of sewage disposal is high, and development is restricted, and brown (BrownOxidereplacement) is exactly arise at the historic moment in this case.
Brown technology is the indispensable operation of PCB inner plating.Along with the needs of high precision, highly dense unicircuit, the multilayer circuit board that the manufacturing technology trend of track making sheet is more accurate develops.Thus increase the consumption of brown oxide waste liquid and the generation of brown oxide waste liquid.
Brown process is a chemistry erosion copper reaction process, along with the carrying out that brown is produced, copper ion concentration in brown oxide waste liquid constantly rises, and after cupric ion is more than a threshold quantity, brown oxide waste liquid just can brown copper face turns white, the unequal quality problem of brown copper face color and luster because cupric ion too much produce.Therefore, must process brown tank liquor, cupric ion is controlled within the specific limits, thus ensure the quality of brown product.Usually when copper ion concentration reaches a threshold quantity in brown process after, need constantly to discharge brown oxide waste liquid, supplement annex solution to reduce copper ion concentration simultaneously, to keep stablizing of each active principle content in brown groove.
The macromole with lone-pair electron such as N, S, P such as a large amount of triazole classs, polyethylene glycols is comprised containing many toxic organic compounds in useless brown oxide waste liquid, cupric ion also containing 25 ~ 50g/L in waste liquid, its part forms title complex with cupric ion, and part is free deposits in the solution.At present, have some data to process it, wherein chemical deposition method is not welcome by market owing to there is the low and secondary pollution problems of large, the heavy copper poor quality of reagent consumption, economic benefit.
Disclose in patent documentation CN201713399U " a kind of brown oxide waste liquid regeneration device ", this technology is successively by brown oxide waste liquid collection, underpressure distillation, crystallisation by cooling copper removal, automatic analysis, Automatic Dosing and backflow method again, realize process to useless brown oxide waste liquid, but the equipment price realizing underpressure distillation step that this technical scheme relates to is expensive, energy consumption is high and can re-treatment limited.Therefore, this technology can't realize large-scale promotion application at present.Disclose one " light/ozone-electricity-absorption reaction device and method of copper is carried in brown oxide waste liquid degraded " in patent documentation CN102583840A, this technology first by making with the organism in the useless brown oxide waste liquid of light ozone cooperative degraded, and then carries out copper electrowinning.Although this technology provides a kind of good process and to give up the method for brown oxide waste liquid, this technical scheme be realized, need to configure ozonizer, device for absorbing tail gas and ultraviolet source, be not suitable for industrialization large-scale application.Patent documentation CN102603102A and patent documentation CN102560533A adds cationic polymers to form the metallic compound of eletrolyzable complex copper or tool oxidation capacity and tensio-active agent for decomposing organic matter and improve the brightness of heavy copper in waste liquid, but does not solve the impact of brown oxide waste liquid in electrode surface film forming.By adding ionic catalyst in waste liquid, the while of organic in catalyzing oxidizing degrading waste liquid under the effect of electricity, at catholyte copper in 201210587062.X.But the mutual relationship of electric drive and concentration difference affects whole reaction efficiency in electrocatalysis process.
Summary of the invention
The object of invention
The object of the present invention is to provide a kind of method reclaiming copper from brown oxide waste liquid, the present invention can copper in high efficiente callback brown oxide waste liquid by rational design, reduce the heavy metal content in brown oxide waste liquid, from waste liquid, obtain the copper of high added value, make the subsequent processes of brown oxide waste liquid more easy.
Concrete technical scheme
From brown oxide waste liquid, reclaim a method for copper, concrete steps are: in the scope of temperature 30 ~ 100 DEG C, add alkaline matter and controlled by the pH of waste liquid, in the scope of 2 ~ 3, then to filter in brown oxide waste liquid; In filtrate, add electrolysis additive again, at 30 ~ 60 DEG C, carry out electrolysis.
The electrolysis additive added is selected from sodium polydithio-dipropyl sulfonate, AESS acid copper walks by force agent, mercaptoimidazole propanesulfonate, dimethyl formamide base propane sulfonic acid sodium, dimethyl-two formyl sulfide amine sodium sulfonate, propane sulfonic acid sodium, 3-sulphur-isothiourea propanesulfonic acid inner salt, thiazolinyl dithio propane sulfonic acid sodium, one or several in hexyl benzylamine salts, add 0.001 ~ 0.1g electrolysis additive in every 1L waste liquid.Wherein AESS is that a kind of powerful sour copper walks agent; The effect adding electrolysis additive is the crystallization of refinement copper, increases cathodic polarization, current efficiency during electrolysis is improved, copper smooth on negative electrode.Additive addition is proportional with the volume filtering rear brown oxide waste liquid, and the larger addition of volume is more.
The alkaline matter added is preferably sodium hydroxide, sodium carbonate, ammoniacal liquor, one or more of calcium hydroxide etc., preferably adds 5 ~ 20g alkaline matter in every 1L waste liquid.
Anode in electrolytic process is preferably insoluble titanium coating iridium tantalum anode, and negative electrode is preferably stainless steel cathode or Ti cathode, and the spread of electrodes in electrolyzer is preferably 3 ~ 10cm.
The reaction principle of invention
In the prior art, by Direct Electrolysis brown oxide waste liquid can not on negative electrode precipitating metal copper, and the present invention is by adopting pre-treatment-Direct Electrolysis technique, the complex state of copper in brown oxide waste liquid is destroyed in preprocessing process, and by passing through to add special electrolysis additive in electrolytic process, obtain the metallic copper of separating out at negative electrode.
The present invention by adding alkaline matter to brown oxide waste liquid, adjusted to ph.Time unprocessed, the organism in brown liquid is dissolved in water, and after adding alkaline matter to brown liquid, the organism of sticky shape, not by filter paper, remains on filter paper.Copper in brown oxide waste liquid is separated into eletrolyzable ionic state from complex state.Solution filters after showing to add alkali by detection again, obtains the settled solution of rich copper.Electrolysis is carried out to solution, separates out elemental copper.By the complex state of copper in the brown liquid of destruction, the copper in brown oxide waste liquid is ionic state, and in electrolytic process, negative electrode only separates out copper and indivisible hydrogen, and current efficiency is high.And the cationic polymers itself owing to adding in prior art is a kind of organism, cause electrode surface film forming, being formed with cupric ion after adding cationic polymers can the complex copper of electrolysis, and during the complex copper electrolysis of this state, current efficiency is not high.
In electrolytic process, utilize the reduction reaction of negative electrode, metallic copper is separated out from copper-containing wastewater.Anode adopts insoluble titanium coating iridium tantalum anode, and negative electrode adopts stainless steel plate or Titanium board; During electrolysis, by adding special electrolysis additive, improving current density and current efficiency, making cupric ion in cathodic deposition, obtain the electrolytic copper plate that purity is greater than 99%, make copper content in last waste liquid be low to moderate 100mg/L.
Reaction formula during electrolysis:
Negative electrode Cu
2++ 2e
-=Cu
Anode 2OH
--2e
-=H
2↑+O
2↑
The effect of invention
The copper in brown oxide waste liquid can be reclaimed by the present invention efficiently, reduce heavy metal contamination.The present invention is by adding alkaline matter dexterously, and the temperature of waste liquid and pH value when controlling to add alkaline matter, carry out electrolysis again after the complex copper in brown liquid being converted into cupric ion, current efficiency is high, copper recovery reaches 99%, and after process, in waste liquid, copper content is at below 100mg/L.When reclaiming copper, organic complex state is destroyed, and the subsequent treatment cost of brown oxide waste liquid is reduced greatly, and reduce secondary pollution, sludge quantity reduces to minute quantity.In addition, the raw material used in the present invention is common agents, low price, is applicable to large-scale commercial production.And processing technological flow of the present invention is simple, processing parameter easily controls, and the rate of recovery of copper is up to 99%, and added value is high, production process environmental protection, and the present invention has good economic benefit and social benefit, wide market.
Embodiment
Embodiment 1
At 30 DEG C, get brown liquid 500L, copper content is 25g/L, theoretical copper content 12.5kg, in 500L brown liquid, add 2.5kg sodium hydroxide, pH is 2, filtering solution, add 5g mercaptoimidazole propanesulfonate, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 220A/m
2under carry out electrolysis, peel the copper on negative electrode, oven dry is weighed, and the actual output of the copper obtained is 12.3kg, and current efficiency is now 98.4%.
Embodiment 2
When temperature is 35 DEG C, get brown liquid 1000L, copper content is 30g/L, theoretical copper content is 30kg, and in brown liquid, add 5kg sodium carbonate, pH is 2.5, filtering solution, add 10g3-sulphur-isothiourea propanesulfonic acid inner salt, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 250A/m
2, after carrying out electrolysis, the actual output of the copper obtained is 29.6kg, and current efficiency is now 98.6%.
Embodiment 3
When temperature is 40 DEG C, get brown liquid 2000L, copper content is 35g/L, theoretical copper content is 70kg, and in brown liquid, add 10kg ammoniacal liquor, pH is 2.3, filtering solution, add 15g thiazolinyl dithio propane sulfonic acid sodium, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 280A/m
2, after carrying out electrolysis, the actual output of the copper obtained is 69.3kg, and current efficiency is now 99%.
Embodiment 4
When temperature is 37 DEG C, get brown liquid 1500L, copper content is 28g/L, theoretical copper content is 42kg, and in brown liquid, add 8kg ammoniacal liquor, pH is 3, filtering solution, add 12g dimethyl-two formyl sulfide amine sodium sulfonate, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 270A/m
2, after carrying out electrolysis, the actual output of the copper obtained is 41.6kg, and current efficiency is now 99%.
Embodiment 5
When temperature is 32 DEG C, get brown liquid 400L, copper content is 26g/L, theoretical copper content is 10.4kg, and in brown liquid, add 3kg calcium hydroxide, pH is 2.6, filtering solution, add 8g thiazolinyl dithio propane sulfonic acid sodium, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 240A/m
2, after carrying out electrolysis, the actual output of the copper obtained is 10.1kg, and current efficiency is now 97.1%.
Embodiment 6
When temperature is 33 DEG C, get brown liquid 300L, copper content is 40g/L, theoretical copper content is 12kg, and in brown liquid, add 2kg calcium hydroxide and 2kg ammoniacal liquor, pH is 2.2, filtering solution, add 7.2g sodium polydithio-dipropyl sulfonate, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 210A/m
2, after carrying out electrolysis, the actual output of the copper obtained is 11.7kg, and current efficiency is now 97.5%.
Embodiment 7
When temperature is 40 DEG C, get brown liquid 800L, copper content is 31g/L, theoretical copper content is 24.8kg, and in brown liquid, add 16kg sodium hydroxide, pH is 2.6, filtering solution, add 8g dimethyl-two formyl sulfide amine sodium sulfonate, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 260A/m
2, after carrying out electrolysis, the actual output of the copper obtained is 24.4kg, and current efficiency is now 98.3%.
Embodiment 8
When temperature is 50 DEG C, get brown liquid 20L, copper content is 45g/L, and theoretical copper content is 0.9kg, in brown liquid, add 16kg sodium hydroxide, pH is 2.9, filtering solution, add 2g propane sulfonic acid sodium, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 230A/m
2, after carrying out electrolysis, the actual output of the copper obtained is 0.87kg, and current efficiency is now 96.6%.
Embodiment 9
When temperature is 48 DEG C, get brown liquid 200L, copper content is 42g/L, theoretical copper content is 8.4kg, and in brown liquid, add 16kg sodium carbonate, pH is 2.9, filtering solution, add 11g propane sulfonic acid sodium and 8gAESS acid copper walks by force agent, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 230A/m
2, after carrying out electrolysis, the actual output of the copper obtained is 8.2kg, and current efficiency is now 97.6%.
Embodiment 10
When temperature is 43 DEG C, get brown liquid 700L, copper content is 35g/L, theoretical copper content is 24.5kg, and in brown liquid, add 16kg ammoniacal liquor, pH is 2.7, filtering solution, add 8g dimethyl-two formyl sulfide amine sodium sulfonate, in insoluble titanium coating iridium tantalum anode and Ti cathode electrolyzer, current density is 280A/m
2, after carrying out electrolysis, the actual output of the copper obtained is 24.4kg, and current efficiency is now 99.5%.
Claims (1)
1. from brown oxide waste liquid, reclaim a method for copper, concrete steps are: in the scope of temperature 30 ~ 100 DEG C, add alkaline matter and controlled, 2 ~ 3, then to filter by the pH of waste liquid in brown oxide waste liquid; In filtrate, add electrolysis additive again, at 30 ~ 60 DEG C, carry out electrolysis;
The electrolysis additive added is selected from sodium polydithio-dipropyl sulfonate, AESS acid copper walks by force agent, mercaptoimidazole propanesulfonate, dimethyl formamide base propane sulfonic acid sodium, dimethyl-two formyl sulfide amine sodium sulfonate, propane sulfonic acid sodium, 3-sulphur-isothiourea propanesulfonic acid inner salt, thiazolinyl dithio propane sulfonic acid sodium, one or several in hexyl benzylamine salts, add 0.001 ~ 0.1g electrolysis additive in every 1L waste liquid;
The alkaline matter added is sodium hydroxide, sodium carbonate, ammoniacal liquor, one or more in calcium hydroxide;
The anode used in electrolytic process is insoluble titanium coating iridium tantalum anode, and negative electrode is stainless steel cathode or Ti cathode, and the spread of electrodes in electrolyzer is 3 ~ 10cm.
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| CN104372376A (en) * | 2014-06-20 | 2015-02-25 | 商实企业有限公司 | Method for recovering copper from brown oxidation waste liquid |
| CN105132947B (en) * | 2015-09-24 | 2018-02-02 | 苏州铂瑞电极工业有限公司 | A kind of copper reclaims electrode group |
| CN106191919A (en) * | 2016-07-13 | 2016-12-07 | 深圳市京中康科技有限公司 | A kind of technique reclaiming copper from brown oxide waste liquid |
| CN106115991A (en) * | 2016-08-12 | 2016-11-16 | 深圳市洁驰科技有限公司 | A kind of brown oxide waste liquid processing means and processing method |
| CN106350678B (en) * | 2016-08-30 | 2018-08-17 | 盛隆资源再生（无锡）有限公司 | A method of recycling corrosion inhibiter and copper from brown oxide waste liquid |
| CN106245058B (en) * | 2016-08-30 | 2018-06-19 | 盛隆资源再生（无锡）有限公司 | A kind of method of copper in electrolytic recovery brown oxide waste liquid |
| CN106241960B (en) * | 2016-08-31 | 2019-07-09 | 航天凯天环保科技股份有限公司 | A kind of processing method of acid heavy metal wastewater |
| 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 |
| CN112808742B (en) * | 2020-12-31 | 2022-05-20 | 深圳星河环境股份有限公司 | Method and system for treating printed circuit board waste |
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| CN102560533A (en) * | 2010-12-28 | 2012-07-11 | 深圳市瑞世兴科技有限公司 | Technology for electrolyzing copper from brown oxide waste liquid |
| CN102603102A (en) * | 2012-03-30 | 2012-07-25 | 湖南万容科技股份有限公司 | Processing method of browning liquid |
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