CN107059012A - A kind of electrolytic reaction system, acidic etching liquid regeneration and copper-extracting process - Google Patents
A kind of electrolytic reaction system, acidic etching liquid regeneration and copper-extracting process Download PDFInfo
- Publication number
- CN107059012A CN107059012A CN201710301200.4A CN201710301200A CN107059012A CN 107059012 A CN107059012 A CN 107059012A CN 201710301200 A CN201710301200 A CN 201710301200A CN 107059012 A CN107059012 A CN 107059012A
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- anode
- reaction system
- cathode chamber
- chamber
- electrolytic
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/46—Regeneration of etching compositions
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
Abstract
The present invention relates to electroplating technology field, and in particular to a kind of electrolytic reaction system, acidic etching liquid regeneration and copper-extracting process.The electrolytic reaction system of the present invention, including：It is provided for placing the cathode chamber of minus plate and the anode chamber for placing positive plate in electrolytic cell, electrolytic cell, the anode chamber is surrounded using cationic membrane, and the cationic membrane make it that cathode chamber and anode chamber are mutually isolated；Housed in the cathode chamber and dilute sulfuric acid is housed in etching waste liquor, anode chamber.Also disclose and acidic etching liquid regeneration and copper-extracting process are carried out using above-mentioned electrolytic reaction system.The present invention is due to the presence of cationic membrane, Cl‑The migration to anode can not be realized, therefore will not discharge to form chlorine in anode, without supplementing chlorion again in the etching solution of regeneration；Meanwhile, whole operation process of the present invention do only need supplement be water, system need not supplement other absorption plants and absorbing material, the more environmentally friendly energy-conservation of technical process.
Description
Technical field
The present invention relates to electrolysis tech field, and in particular to a kind of electrolytic reaction system, acidic etching liquid regenerate and carried copper
Technique.
Background technology
The circuit etching process of circuit board industry can produce substantial amounts of etching waste liquor, and etching waste liquor is the danger that country keeps under strict control
Waste, containing heavy metal, acid and oxidant, wherein heavy metal is mainly copper, and copper content reaches as high as 160 gram per liters.Current is logical
It is to handle these waste liquids to our factory by Automobile Transportation by the unit with hazardous waste business licence with way, reclaims
Copper, tail washings is discharged after sewage disposal, and copper-extracting process is mainly neutralisation and displacement method, belongs to chemical method, and extract
Need to add new chemical substance while copper, high risks are caused to surrounding environment.
With the enhancing of people's environmental consciousness, a kind of etching waste liquid regeneration circulates, puies forward copper system and unite and arise at the historic moment, many scales
The wiring board enterprise of change begins attempt to this nominal clean environment firendly equipment, and the objective of the equipment is etching solution circulation to be realized
Use, carry copper and regenerate all online completion, no discharge.But actual conditions are that this kind equipment come into operation at present is unable to reach
All on-line is circulated, and has the etching solution for being not less than half to be discharged and can not all regenerate after carrying copper, and this kind equipment exists
Substantial amounts of chlorine is produced again in regeneration electrolytic process, chlorine is toxic gas, in order to prevent chlorine from endangering, and system adds chlorine again
The ferrous absorption and Alkali absorption device of gas, these devices not only increase equipment cost, at the same with when generate new danger again
Waste, these newly-increased hazardous wastes add the half spent etching solution above discharged, and the total amount of waste alreadys exceed etching waste liquor
Total amount, and environmentally friendly objective runs in the opposite direction.
It can be seen that prior art is further improved.
The content of the invention
In view of this, it is necessary to for it is above-mentioned the problem of there is provided a kind of electrolytic reaction system produced without chlorine, acid lose
Carve liquid regeneration and copper-extracting process.
To achieve the above object, the present invention takes following technical scheme：
The electrolytic reaction system of the present invention, including：Be provided in electrolytic cell, electrolytic cell place minus plate cathode chamber and
Anode chamber for placing positive plate, the anode chamber is surrounded using cationic membrane, and the cationic membrane causes cathode chamber and sun
Pole room is mutually isolated；
Housed in the cathode chamber and dilute sulfuric acid is housed in etching waste liquor, anode chamber.
Further, the electrolytic reaction system also includes：Anolyte regulating tank, waste tank and regenerated liquid regulation tank；
The outlet of the anolyte regulating tank and the entrance of anode chamber are connected；Anode compartment outlet enters with anolyte regulating tank
Mouth connection, so as to form the closed cycle of anolyte；
The outlet of the waste tank and the entrance of cathode chamber are connected, and the outlet of cathode chamber is connected with regenerated liquid regulation tank.
Further, the cathode chamber and anode chamber are set to multigroup.
Further, the thickness of the cationic membrane is 0.6-0.7mm.
Further, the reaction system also includes oxygen catheter, the oxygen catheter connection anode chamber and cathode chamber, will
The oxygen produced by anode is injected into cathode chamber.
Further, the positive plate is analysis oxygen type DSA iridium titanium anode plates, and the minus plate is Ti electrode plate.
The acidic etching liquid regeneration produced without chlorine carried out using above-mentioned electrolytic reaction system and copper-extracting process, including with
Lower step：
Step 1) dilute sulfuric acid is added in anode chamber, etching waste liquor to be regenerated is added in cathode chamber；
Step 2) connection power supply be electrolysed；
Step 3) electrolytic process is continuously replenished water in the anode compartment, to keep the balance of anode chamber's acidity.
Further, the current density of electrolytic process is 3-4A/dm2；The concentration range of the dilute sulfuric acid is 10%-
30%.
It is preferred that, the current density of electrolytic process is 4A/dm2；The concentration range of the dilute sulfuric acid is 20%.
Beneficial effects of the present invention are：
Anode region and cathodic region have been separated into two independences by cation-exchange membrane but can carry out thing by the present invention
The space that matter is selectively exchanged, makes the electrotransport process of ion by artificial control；
Make anolyte with dilution heat of sulfuric acid, it is ensured that there is passing through for ion in anode region and cathodic region, but not release chlorine；
The oxidant that the oxygen of precipitation exactly regenerated liquid needs, can apply to cathodic region oxidation monovalence copper；
By the etching solution of the system regeneration, active ingredient does not have any loss, on the contrary, the H consumed in etching process+, supplemented in the system regenerative process.
Brief description of the drawings
Fig. 1 is the structural representation of electrolytic cell 1 of present system；
Fig. 2 is present system catholyte and anolyte closed cycle structural representation；
Fig. 3 is that online production process etching solution regenerates FB(flow block).
Reference：1st, electrolytic cell；11st, cathode chamber；12nd, anode chamber；13rd, cationic membrane；14th, minus plate；15th, anode
Plate；2nd, anolyte regulating tank；3rd, waste tank；4th, regenerated liquid regulation tank.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical scheme is made further clearly and completely to describe.It should be noted that described embodiment is only the present invention one
Section Example, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not doing
Go out the every other embodiment obtained under the premise of creative work, belong to the scope of protection of the invention.
Amberplex be the one kind invented by Ion America Inc. w.juda in nineteen fifty-three can make in solution solute from
The film that sub- selectivity passes through, cationic membrane abbreviation anode membrane, anode membrane can allow cation to pass through；Anionic membrane abbreviation cavity block, and cavity block
Anion can be allowed to pass through, cation can not then pass through.Cationic membrane employed in the present embodiment produces for Ion America Inc.
CR61CMP-447 cationic membranes.
The present invention has found that the reason for prior art processes process produces chlorine is chlorion by the analysis to regenerative system
Oxidation electric discharge is take part in the anode of electrolytic cell, this results in the spilling of chlorine in system, the spilling of chlorine causes circulation again
Changing not to be known where to begin, because chlorion is the Main Components of etching, chlorion is reduced in system, it is necessary to is supplemented, is caused
The input of material is added, amount of liquid in system is continuously increased, the part accommodated beyond system has to discharge.For the above
Situation, the present invention proposes a set of improved electrolytic reaction system, can solve chlorion the problem of anode discharge.
As shown in figure 1, the electrolytic cell 1 in invention, using dilute sulfuric acid as anolyte, etching waste liquor to be regenerated is catholyte,
The Cl of cathode chamber 11-Due to the effect of cationic membrane 13, it is impossible to realize the migration to anode, therefore will not discharge to form chlorine,
The ion that anode can be uniquely oxidized only has OH-, select analysis oxygen type DSA iridium titanium anode plate 15 to make anode, OH-In anode discharge
Discharge oxygen；In cathode chamber 11, Cu2+It is reduced, forms elemental copper and separate out.H in anode chamber 12+Because the effect of electromigration is led to
Anode membrane is crossed to cathodic migration, but is not discharged, but is assembled in cathode chamber 11, the acidity of regenerated liquid is improved, this is exactly desired
Effect.The electrode reaction of this electrolytic cell 1 is as follows：
Anode：OH--e→O2 (1)
Negative electrode：Cu2++e→Cu (2)
The oxygen that anode chamber 12 is produced is introduced into the medium of cathode chamber 11 by conduit, as in oxidizing catholyte
Monovalence copper, is allowed to be converted into cupric, chemical equation is：
Cu+-e→Cu2+ (3)
Reaction (2) realizes the recovery of copper, and reaction (3) realizes the regeneration of etching waste liquor, and previous reaction is on battery lead plate
Carry out, latter reaction is carried out in the liquid medium in cathodic region, and being converted into the copper of divalence can continue to obtain copper in cathodic discharge
(monovalence copper has certain reproducibility to simple substance, and its discharge capability on negative electrode is very weak, in the far super monovalence copper of divalence copper concentration
When, monovalence copper will not discharge generation copper simple substance in negative electrode, only by reoxidizing, when being converted into divalence, and just formation is in negative electrode
Electric discharge), with cupprous reduction, the redox ability of etching solution strengthens (i.e. ORP value is improved), and etch capabilities are able to extensive
It is multiple, that is, reach regeneration purpose；Too high cupric, into copper coin, by the control of flow velocity, can be existed cupric control by electrodeposition
Rational level, to meet the proportion index and Cu of etching solution2+Concentration index.
As shown in Figures 2 and 3, as a kind of electrolytic reaction system of embodiment of the invention, cathode chamber 11 and anode chamber
12 are spaced setting, each cathode chamber 11 and an anode chamber 12 as one group, can according to need arrangement it is multigroup.Set
One anolyte regulating tank 2, anolyte regulating tank 2 is respectively connecting to each anode chamber 12, the circulation for completing anolyte,
And the acidity of anolyte can be adjusted and moisturizing in anolyte regulating tank 2；The etching discharged by etching production line
Waste liquid flows into waste tank 3, and waste tank 3 is then respectively connecting to each cathode chamber 11 distribution catholyte, through electrolytic recovery Cu2+
Catholyte afterwards is flow in regenerated liquid regulation tank 4, and qualified regeneration etching solution is stored in regeneration liquid storage tank and is recycled to production line
Use, underproof etching solution is then recycled in the anti-system of electrolysis and handled again.From mass transfer in liquid phase the need for, the present invention
Anodic liquid and catholyte employ independent closed circuit circulatory system, keep the quick diffusion of ion in same system, realize high
The electrolytic process of effect.
Embodiment
Etching waste liquor to be regenerated is positioned in cathode chamber 11；Dilute sulfuric acid is positioned in anode chamber 12, and sets dilute sulphur
Acid concentration is in 20-25%, to analyse oxygen type DSA iridium titanium plate as positive plate 15, and Ti electrode plate is minus plate 14, thick using 0.6mm
CR61CMP-447 cationic membranes surround each anode chamber 12, power supply are connected, in 4A/dm2It is electrolysed under current density.Electrolysis
During catholyte and anolyte each constantly circulate.
The chemical reaction process of above-mentioned electrolytic process is anode：OH--e→O2；Negative electrode：Cu2++e→Cu。
The univalent copper ion of part is there is in etching waste liquor, the oxygen separated out in anode is imported into the moon by conduit
In the solution of pole, univalent copper ion is oxidized to bivalent cupric ion：Cu+-e→Cu2+。
The forward and backward liquid etching composition of regeneration and parameter are shown in Table 1：
Table 1 regenerates forward and backward etching waste liquor composition and parameter list
Detection Cl before and after electrolysis-Significant change does not occur for concentration, and etching solution is regenerated, while having reclaimed portion
Divide Cu.
In the whole course of reaction of the present invention, due to the presence of cationic membrane 13, Cl-The migration to anode can not be realized,
Therefore it will not discharge to form chlorine at anode, without supplementing chlorion again in the etching solution of regeneration；Meanwhile, the whole behaviour of the present invention
Done as process only need supplement be water, system need not increase other absorption plants and absorbing material, the more environmentally friendly energy-conservation of technical process.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (9)
1. be provided in a kind of electrolytic reaction system, it is characterised in that electrolytic cell, electrolytic cell place minus plate cathode chamber and
Anode chamber for placing positive plate, the anode chamber is surrounded using cationic membrane, and the cationic membrane causes cathode chamber and sun
Pole room is mutually isolated；
Housed in the cathode chamber and dilute sulfuric acid is housed in etching waste liquor, anode chamber.
2. electrolytic reaction system according to claim 1, it is characterised in that also include：Anolyte regulating tank, waste tank
Tank is adjusted with regenerated liquid；
The outlet of the anolyte regulating tank and the entrance of anode chamber are connected；The entrance of anode compartment outlet and anolyte regulating tank connects
Connect, so as to form the closed cycle of anolyte；
The outlet of the waste tank and the entrance of cathode chamber are connected, and the outlet of cathode chamber is connected with regenerated liquid regulation tank.
3. electrolytic reaction system according to claim 1 or 2, it is characterised in that cathode chamber and the anode interventricular septum is set
It is set to multigroup.
4. electrolytic reaction system according to claim 1 or 2, it is characterised in that the thickness of the cationic membrane is 0.6-
0.7mm。
5. electrolytic reaction system according to claim 1 or 2, it is characterised in that the reaction system is also led including oxygen
Pipe, the oxygen catheter connection anode chamber and cathode chamber, the oxygen produced by anode is injected into cathode chamber.
6. electrolytic reaction system according to claim 1 or 2, it is characterised in that the positive plate is analysis oxygen type DSA iridium titaniums
Positive plate, the minus plate is Ti electrode plate.
7. the acidic etching liquid carried out using the electrolytic reaction system described in the claims 1-6 any one regenerates and carried copper
Technique, it is characterised in that comprise the following steps：
Step 1) dilute sulfuric acid is added in anode chamber, etching waste liquor to be regenerated is added in cathode chamber；
Step 2) connection power supply be electrolysed；
Step 3) electrolytic process is continuously replenished water in the anode compartment, to keep the balance of anode chamber's acidity.
8. acidic etching liquid regeneration according to claim 7 and copper-extracting process, it is characterised in that the electric current of electrolytic process is close
Spend for 3-4A/dm2；The concentration range of the dilute sulfuric acid is 10%-30%.
9. acidic etching liquid regeneration according to claim 8 and copper-extracting process, it is characterised in that the electric current of electrolytic process is close
Spend for 4A/dm2；The concentration range of the dilute sulfuric acid is 20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710301200.4A CN107059012A (en) | 2017-05-02 | 2017-05-02 | A kind of electrolytic reaction system, acidic etching liquid regeneration and copper-extracting process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710301200.4A CN107059012A (en) | 2017-05-02 | 2017-05-02 | A kind of electrolytic reaction system, acidic etching liquid regeneration and copper-extracting process |
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| CN201710301200.4A Pending CN107059012A (en) | 2017-05-02 | 2017-05-02 | A kind of electrolytic reaction system, acidic etching liquid regeneration and copper-extracting process |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108411304A (en) * | 2018-03-19 | 2018-08-17 | 华南理工大学 | Utilize the method for the chlorine synergistic oxidation regenerated acidic etching waste liquor that the hydrogen peroxide that oxygen cathodic reduction generates is generated with anodic oxidation |
| CN110408936A (en) * | 2019-07-18 | 2019-11-05 | 惠州市臻鼎环保科技有限公司 | A kind of method of electrolytic circuit board acidic etching waste liquor |
| CN110964923A (en) * | 2019-12-24 | 2020-04-07 | 中南大学 | Device and method for deep replacement copper extraction under multi-field coupling |
| CN110983375A (en) * | 2019-12-24 | 2020-04-10 | 广东臻鼎环境科技有限公司 | Method for depositing copper by using waste etching solution of electrolytic printed circuit board |
| RU2763856C1 (en) * | 2021-05-13 | 2022-01-11 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Российский химико-технологический университет имени Д.И. Менделеева (РХТУ им. Д.И. Менделеева) | Method for processing the spent solution of copper brightening |
| CN114808042A (en) * | 2022-06-07 | 2022-07-29 | 赵坤 | Cation membrane continuous electrolysis device and use method thereof |
| CN114808039A (en) * | 2021-12-02 | 2022-07-29 | 广州合凯环保科技有限公司 | Acid etching solution regeneration system with chlorine-free gas evolution and low cost |
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| JPS63297583A (en) * | 1987-05-29 | 1988-12-05 | Nippon Mining Co Ltd | Manufacture of high-purity electrolytic copper |
| CN102732888A (en) * | 2012-07-19 | 2012-10-17 | 湖南万容科技股份有限公司 | Method and system for regenerating and recycling acidic etching waste liquor |
| CN102912375A (en) * | 2012-11-06 | 2013-02-06 | 赣州聚环科技有限公司 | Method for recovering copper from acid etching liquid and special device for method |
| CN103757664A (en) * | 2013-12-13 | 2014-04-30 | 陶克（苏州）机械设备有限公司 | Electrolytic tank, etching liquid regeneration equipment using same and regeneration method |
| CN104313584A (en) * | 2014-10-10 | 2015-01-28 | 南京舜业环保科技有限公司 | Method and system for electrolyzing copper-containing etching liquid to obtain copper plate and regenerating and recycling etching liquid |
| CN205062205U (en) * | 2014-09-18 | 2016-03-02 | 龙济时代(北京)新能源科技有限公司 | It configures integrative electrolytic cell assembly to replace filtering of positive pole diaphragm effect in copper electrolysis |
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2017
- 2017-05-02 CN CN201710301200.4A patent/CN107059012A/en active Pending
Patent Citations (6)
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| JPS63297583A (en) * | 1987-05-29 | 1988-12-05 | Nippon Mining Co Ltd | Manufacture of high-purity electrolytic copper |
| CN102732888A (en) * | 2012-07-19 | 2012-10-17 | 湖南万容科技股份有限公司 | Method and system for regenerating and recycling acidic etching waste liquor |
| CN102912375A (en) * | 2012-11-06 | 2013-02-06 | 赣州聚环科技有限公司 | Method for recovering copper from acid etching liquid and special device for method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108411304A (en) * | 2018-03-19 | 2018-08-17 | 华南理工大学 | Utilize the method for the chlorine synergistic oxidation regenerated acidic etching waste liquor that the hydrogen peroxide that oxygen cathodic reduction generates is generated with anodic oxidation |
| CN110408936A (en) * | 2019-07-18 | 2019-11-05 | 惠州市臻鼎环保科技有限公司 | A kind of method of electrolytic circuit board acidic etching waste liquor |
| CN110964923A (en) * | 2019-12-24 | 2020-04-07 | 中南大学 | Device and method for deep replacement copper extraction under multi-field coupling |
| CN110983375A (en) * | 2019-12-24 | 2020-04-10 | 广东臻鼎环境科技有限公司 | Method for depositing copper by using waste etching solution of electrolytic printed circuit board |
| CN110964923B (en) * | 2019-12-24 | 2023-09-19 | 中南大学 | Device and method for extracting copper by deep replacement under multi-field coupling |
| RU2763856C1 (en) * | 2021-05-13 | 2022-01-11 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Российский химико-технологический университет имени Д.И. Менделеева (РХТУ им. Д.И. Менделеева) | Method for processing the spent solution of copper brightening |
| CN114808039A (en) * | 2021-12-02 | 2022-07-29 | 广州合凯环保科技有限公司 | Acid etching solution regeneration system with chlorine-free gas evolution and low cost |
| CN114808039B (en) * | 2021-12-02 | 2024-01-02 | 广州合凯环保科技有限公司 | Acid etching solution regeneration system without chlorine precipitation and low in cost |
| CN114808042A (en) * | 2022-06-07 | 2022-07-29 | 赵坤 | Cation membrane continuous electrolysis device and use method thereof |
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Application publication date: 20170818 |