CN1966773A - Method for simultaneous electrolysis and regeneration of acid etching solution and micro-etching solution - Google Patents
Method for simultaneous electrolysis and regeneration of acid etching solution and micro-etching solution Download PDFInfo
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- CN1966773A CN1966773A CNA2006100620866A CN200610062086A CN1966773A CN 1966773 A CN1966773 A CN 1966773A CN A2006100620866 A CNA2006100620866 A CN A2006100620866A CN 200610062086 A CN200610062086 A CN 200610062086A CN 1966773 A CN1966773 A CN 1966773A
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- microetching
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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
Abstract
The invention relates to a method for electrolysis regenerating acid etching liquid and micro-etching liquid. The anode chamber (11) and the cathode chamber (12) are separated by the cation-exchange membrane. The reservoir of the acid etching liquid containing hydrochloric acid and chloratum culture-medium (17) is connected with the anode chamber (11). The reservoir of micr0-etching liquid containing ammonium persulfate and sulphuric acid is connected with the cathode chamber (12). During the electrolysis reaction, ammonium sulfate formed in the anode chamber (11) by micr0-etching reaction is oxidized to regenerate to ammonium persulfate, meanwhile, divalent copper ions pass through the cation-exchange membrane into the cathode chamber (12), univalent copper ions formed in the cathode chamber (12) through etching reaction is reduced to copper, and divalent copper ions return to acid etching liquid reservoir (17). The technological effects of the invention are: making full use of anode electric energy, copper resource, no creation of pollution and waste, and improving the quality of micro-etching and etching.
Description
The invention relates to a chemical etching technology of metal materials, in particular to a regeneration technology of an etching composition for etching copper.
Background of the inventionprinted circuit boards used in the electronics industry for the placement of components are typically patterned by etching a copper foil overlying an insulating material. The etching solution is usually a mixture of copper chloride and hydrochloric acid, and the copper foil is corroded by the acid in the etching solution to release copper ions. As the etching proceeds, the copper ion concentration increases and the acid concentration decreases due to consumption. Therefore, the etching solution is less and less effective after a period of time, and a new etching solution must be replaced, and the waste etching solution causes environmental pollution. In the prior art, in order to prevent waste etching solution, the electrolytic regeneration of acidic etching solution is one of the better solutions. For example, Japanese patent application laid-open No. Hei 10-18062 entitled "method for regenerating etching liquid, apparatus for regenerating etching liquid, and etching apparatus" discloses such a technical proposal: the electrolytic cell is divided into an anode chamber and a cathode chamber by adopting a perfluorocarbon resin cation exchange membrane, the cathode adopts a copper plate, and the anode adopts a titanium-coated platinum group oxide coating. The liquid in the cathode chamber is high-concentration copper chloride and trace hydrochloric acid solution, and the liquid in the anode chamber is 5% sulfuric acid solution. Through electrolysis, copper ions are reduced into metal copper in the cathode chamber, water in the anode chamber is oxidized to generate oxygen and hydrogen ions, and the hydrogen ions enter the cathode chamber through the cation exchange membrane and react with chloride ions to generate hydrochloric acid. The whole process realizes electrolytic regeneration. However, the technical scheme has the following defects: the anode reaction produces useless oxygen into the air, wasting this portion of the electrical energy.
The production process of the printed circuit board has a microetching procedure, wherein the microetching treatment is carried out on the copper surface by using microetching liquid, so that the copper surface forms a micro rough surface, and the bonding force between the copper surface and a plating layer of the next electroplating procedure is favorably improved. The microetching solution contains 3% of sulfuric acid and 10% of ammonium persulfate. As the etching proceeds, the copper ion concentration rises and the ammonium persulfate concentration falls. When the concentration of copper ions in the microetching solution rises to 20g/l, almost all of the ammonium persulfate has been converted into ammonium sulfate. The method in the prior art treats the ineffective micro-etching solution as wastewater, thereby not only wasting copper resources and increasing the cost of water treatment, but also leading the wastewater to be eutrophicated after the ammonium sulfate enters the wastewater, being beneficial to breeding bacteria and leading the water body to be smelly.
Disclosure of the invention the technical problem to be solved by the invention is to avoid the disadvantages of the prior art mentioned above and to provide a method for producing a composite materialIn the anode chamber, ammonium sulfate in the microetching liquid is oxidized into ammonium persulfate, which is returned to the microetching liquid tank for useCopper ion Cu of2+The anode enters the cathode chamber through the cation membrane and is supplemented as an effective component in the acidic etching solution, so that the anode regeneration micro-etching solution is realized, and the anode electric energy is fully utilized. In the cathode chamber, Cu in the acidic etching solution+Is preferentially reduced to copper at the cathode for recovery, Cu2+Is not reduced, but is returned to the acidic etching solution tank for use.
The technical problem to be solved by the invention can be realized by adopting the following technical scheme:
a method for simultaneously electrolyzing and regenerating acidic etching solution and microetching solution is provided, which comprises separating an anode chamber and a cathode chamber by a cation exchange membrane in an electrolytic bath made of acid-resistant material; communicating an acidic etching solution liquid storage tank with the cathode chamber, wherein the acidic etching solution comprises hydrochloric acid and copper chloride; communicating a microetching liquid storage tank with the anode chamber, wherein the microetching liquid comprises ammonium persulfate and sulfuric acid; during the electrolytic reaction, in the anode chamber, ammonium sulfate formed by the microetching reaction in the microetching solution is oxidized into ammonium persulfate, and then returns to the microetching solution storage tank, and simultaneously divalent copper ions in the microetching solution pass through the cation exchange membrane and enter the cathode chamber; in the cathode chamber, monovalent copper ions formed by etching reaction in the acidic etching solution are preferentially reduced to metallic copper at the cathode, while divalent copper ions are returned to the acidic etching solution reservoir.
Compared with the prior art, the invention has the technical effects that:
1. ammonium sulfate in the micro-etching solution is oxidized into useful ammonium persulfate at the anode, and the electric energy of the anode is fully utilized;
2. copper ion Cu in microetching liquid2+The water enters the cathode chamber after passing through the cation exchange membrane and is effectively supplemented as an oxidant for acid etching, so that copper resources are fully utilized, and pollution and waste are not generated;
3. ineffective component Cu in acidic etching solution entering cathode chamber+The reduction at the cathode is preferred, and the consumed electric energy is only traditional Cu2+Half of the electrolytic reduction saves electric energy on the premise of recovering copper resources;
4. because of adopting the cation exchange membrane, chloride ions in the cathode chamber can not enter the anode chamber, the generation of chlorine gas is controlled, and the whole electrolysis process is pollution-free;
5. because continuous electrolytic regeneration is adopted, the effective concentration in the microetching solution and the acidic etching solution is kept in a better state, and the microetching and etching quality is greatly improved;
6. zero additive agent is realized for micro-etching and acid etching, zero emission pollution is realized, the production cost is greatly reduced, and the production benefit is improved.
Drawings
FIG. 1 is a schematic diagram of the operation of the process of the present invention.
The detailed description is provided below in conjunction with the preferred embodiments illustrated in the accompanying drawings.
As shown in figure 1, the electrolytic cell is a rectangular cell made of polyvinyl chloride plastic plate, a polytetrafluoroethylene cation exchange membrane 15 is used for separating an anode chamber 11 from a cathode chamber 12, the distance between the cathode and the anode is 120mm, the anode adopts a boron-doped diamond membrane electrode, and the cathode adopts 35 mu m thick copper foil as an electrode. An acidic etching solution reservoir 17 is in communication with the cathode chamber 12, the acidic etching solution comprising hydrochloric acid and copper chloride. The microetching liquid storage tank 16 is communicated with the anode chamber 11, and the microetching liquid comprises ammonium persulfate and sulfuric acid. A small amount of copper sulfate can be added into the microetching liquid, and when the microetching process begins, a small amount of copper sulfate is added into the microetching liquid, so that the microetching speed is accelerated. The acid etching solution and the microetching solution respectively enter the cathode chamber 12 and the anode chamber 11 for electrolytic regeneration.
① electrolytic regeneration principle and condition control of anode chamber waste micro-etching liquid
And (3) anode reaction:
anode current density: 50-100A/dm2Temperature: at normal temperature
Because the concentration of ammonium sulfate in the micro-etching solution is not high, in order to improve the current efficiency, the solution in the anode chamber adopts a circulation method to strengthen the ammonium sulfate and the anodeThe opportunity for contact. Cu of anode chamber2+Passes through the cation membrane to enter the cathode chamber under the action of the electrostatic attraction of the cathode.
② electrolytic regeneration principle and condition control of waste acidic etching solution in cathode chamber
The acidic waste etching solution contains a large amount of Cu+And Cu2+The total copper concentration is generally maintained at 120-150g/l, where Cu2+55% of Cu+Accounting for 45 percent. Using E DEG Cu+Cu +0.522V greater than E ° Cu2+/Cu＝+0.34V，Cu+Preferentially reducing to metallic copper Thereby making Cu having etching capability2+Remaining, and adding Cu from the anode chamber2+And are gathered together and returned to the etching tank to work.
The cathode current density is controlled to be 6-15A/dm2The thin copper foil is used as a cathode, the temperature is normal temperature, and in order to make the quality of the upper part and the lower part of the cathode plate consistent, the catholyte adopts a circulation mode to ensure that copper ions are uniformly distributed at all parts of the solution.
In order to realize the purpose of regenerating acidic etching solution at the cathode and microetching solution at the anode in one electrolytic cell, a cation exchange membrane which is corrosion-resistant, oxidation-resistant, high in conductivity and small in membrane resistance is used as a diaphragm material to separate a cathode chamber from an anode chamber. Through repeated test comparison, the effect of selecting the polytetrafluoroethylene cation exchange membrane is optimal. The anode can adopt a platinum anode, a titanium platinum-coated oxide anode and a boron-doped diamond membrane electrode. However, by comparing the platinum anode, the titanium platinum-coated oxide anode and the boron-doped diamond film electrode, the boron-doped diamond film electrode has obvious advantages, and is a long-life anode material with high oxygen evolution overpotential. In 1 mol of sulfuric acid medium, the oxygen evolution potential of the boron-doped diamond membrane electrode is +2.4V, the oxygen evolution potential of the platinum electrode is +1.5V, and the oxygen evolution potential of the titanium platinum-coated oxide electrode is + 1.35V. It can be seen from the oxygen evolution potential that the boron-doped diamond film electrode is not easy to generate oxygen in the anodic oxidation process, and the electric energy is fully used for oxidizing sulfate radicals into persulfate radicals, and more rarely, the boron-doped diamond film hardly consumes electrode materials in the anodic oxidation process, and the cost is too high because 3 g of platinum is consumed for every ton of ammonium persulfate generated by the platinum electrode, so the boron-doped diamond film electrode is selected as the anode material in the embodiment of the invention.
The first embodiment is as follows:
the anode 13 adopts a boron-doped diamond membrane electrode, and the current density of the anode is 75A/dm2Circularly stirring the solution in the anode chamber, and converting 90 percent of ammonium sulfate into ammonium persulfate and Cu after electrolyzing for 1 hour2+And also substantially all of the microetching solution is transferred to the cathode chamber 12, and the regenerated microetching solution is returned to the microetching solution reservoir 16 to be operated. The micro corrosion-resistant pump 18 is used as the power of the circulation.
The cathode 14 adopts 35 μm thick copper foil, and the cathode current density is 8A/dm2Electrolysis for 4 hours, Cu+The residual 5 percent of the regenerated etching solution is returned to the acid etching liquid storage tank for working. The corrosion resistant pump 19 serves as the power of the cycle.
Example two:
the anode 13 adopts a boron-doped diamond membrane electrode, and the current density of the anode is 50A/dm2Circularly stirring the solution in the anode chamber, and after electrolyzing for 90 minutes, converting 90 percent of ammonium sulfate into ammonium persulfate and Cu2+And also substantially moved to the cathode chamber 12, and the microetching solution is returned to the microetching solution reservoir after regeneration to operate. The micro corrosion-resistant pump 18 is used as the power of the circulation.
The cathode 14 adopts 35 μm thick copper foil, and the cathode current density is 12A/dm2The cathode chamber 12 and the acidic etching solution reservoir 17 are circulated by the corrosion resistant pump 19 to electrolyze for 160 minutes, and Cu is added+The rest 6 percent of the regenerated etching solution is returned to the acid etching liquid storage tank for working. The corrosion resistant pump 19 serves as the power of the cycle.
Claims (6)
1. A method for simultaneously regenerating acidic etching solution and microetching solution by electrolysis comprises separating an anode chamber (11) and a cathode chamber (12) by a cation exchange membrane in an electrolytic bath made of acid-resistant material; communicating an acidic etching solution reservoir (17) with the cathode chamber (12), the acidic etching solution comprising hydrochloric acid and copper chloride; the method is characterized in that:
communicating a microetching liquid storage tank (16) with the anode chamber (11), wherein the microetching liquid comprises ammonium persulfate and sulfuric acid;
during the electrolytic reaction, ammonium sulfate formed by the microetching reaction is oxidized into ammonium persulfate in the anode chamber (11), and then returns to the microetching liquid storage tank (16), and meanwhile, divalent copper ions pass through the cation exchange membrane and enter the cathode chamber (12); in the cathode chamber (12), monovalent copper ions formed by the etching reaction are preferentially reduced to metallic copper at the cathode (14), while divalent copper ions are returned to the acidic etching solution reservoir (17).
2. The method for simultaneous electrolytic regeneration of acidic etching solutions and microetching solutions according to claim 1, wherein: the cation exchange membrane is made of polytetrafluoroethylene.
3. The method for simultaneous electrolytic regeneration of acidic etching solutions and microetching solutions according to claim 1, wherein: the anode (13) arranged in the anode chamber (11) adopts a boron-doped diamond membrane electrode.
4. The method for simultaneous electrolytic regeneration of acidic etching solutions and microetching solutions according to claim 1, wherein: the anode current density is 50-100A/dm2。
5. The method for simultaneous electrolytic regeneration of acidic etching solutions and microetching solutions according to claim 1, wherein: the cathode current density is 6-15A/dm2。
6. The method for simultaneous electrolytic regeneration of acidic etching solutions and microetching solutions according to claim 1, wherein: the microetching solution also comprises copper sulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100620866A CN100494500C (en) | 2006-08-04 | 2006-08-04 | Method for simultaneous electrolysis and regeneration of acid etching solution and micro-etching solution |
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| CNB2006100620866A CN100494500C (en) | 2006-08-04 | 2006-08-04 | Method for simultaneous electrolysis and regeneration of acid etching solution and micro-etching solution |
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| CN1966773A true CN1966773A (en) | 2007-05-23 |
| CN100494500C CN100494500C (en) | 2009-06-03 |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101988200A (en) * | 2009-08-04 | 2011-03-23 | 章晓冬 | Cyclic regeneration and metal reclamation equipment for acid chloride-containing etchant |
| CN102321908A (en) * | 2011-09-02 | 2012-01-18 | 广州市天承化工有限公司 | Recycling and regenerating process method and metal copper recovery system of acid chloride etching solution |
| CN102502925A (en) * | 2011-11-29 | 2012-06-20 | 浙江大学 | Device capable of generating electric energy and simultaneously removing metal ions and method of device |
| 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 |
| CN102807294A (en) * | 2011-05-31 | 2012-12-05 | 无锡尚德太阳能电力有限公司 | Recirculation system for treating used etching liquid |
| CN104535636A (en) * | 2014-12-16 | 2015-04-22 | 宇宙电路板设备(深圳)有限公司 | Oxidizing agent inductor, oxidizing agent adding control circuit and controller |
| CN104630825A (en) * | 2015-01-20 | 2015-05-20 | 昆山美源达环保科技有限公司 | Device and process for electrolytically extracting copper in acidic etching liquid |
| CN107829111A (en) * | 2017-10-17 | 2018-03-23 | 天津大学 | A kind of acid copper chloride etching liquid in-situ electrolysis regeneration and copper recovery method |
| CN108531914A (en) * | 2018-06-15 | 2018-09-14 | 哈尔滨工业大学深圳研究生院 | A kind of H2SO4/S2O82-The copper of microetch waste liquid recycles and synchronizing regeneration micro etching solution system and method |
| CN108668452A (en) * | 2018-06-12 | 2018-10-16 | 江苏博敏电子有限公司 | A kind of PCB fine-lines electrolytic etching recycles correlation technology with copper |
| CN108796545A (en) * | 2017-05-05 | 2018-11-13 | 深圳市憬泰晖科技有限公司 | The method of circuit board acidic etching liquid electrolytic regeneration hydrochloric acid |
| CN108950563A (en) * | 2018-07-16 | 2018-12-07 | 深圳市祺鑫天正环保科技有限公司 | Acid etching regenerates solution additive and acid etching regenerated liquid |
| 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 |
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2006
- 2006-08-04 CN CNB2006100620866A patent/CN100494500C/en active Active
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101988200A (en) * | 2009-08-04 | 2011-03-23 | 章晓冬 | Cyclic regeneration and metal reclamation equipment for acid chloride-containing etchant |
| CN102807294A (en) * | 2011-05-31 | 2012-12-05 | 无锡尚德太阳能电力有限公司 | Recirculation system for treating used etching liquid |
| CN102321908A (en) * | 2011-09-02 | 2012-01-18 | 广州市天承化工有限公司 | Recycling and regenerating process method and metal copper recovery system of acid chloride etching solution |
| CN102502925A (en) * | 2011-11-29 | 2012-06-20 | 浙江大学 | Device capable of generating electric energy and simultaneously removing metal ions and method of device |
| CN102502925B (en) * | 2011-11-29 | 2013-11-13 | 浙江大学 | Device capable of generating electric energy and simultaneously removing metal ions and method of device |
| 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 |
| CN104535636A (en) * | 2014-12-16 | 2015-04-22 | 宇宙电路板设备(深圳)有限公司 | Oxidizing agent inductor, oxidizing agent adding control circuit and controller |
| CN104630825A (en) * | 2015-01-20 | 2015-05-20 | 昆山美源达环保科技有限公司 | Device and process for electrolytically extracting copper in acidic etching liquid |
| CN108796545A (en) * | 2017-05-05 | 2018-11-13 | 深圳市憬泰晖科技有限公司 | The method of circuit board acidic etching liquid electrolytic regeneration hydrochloric acid |
| CN107829111A (en) * | 2017-10-17 | 2018-03-23 | 天津大学 | A kind of acid copper chloride etching liquid in-situ electrolysis regeneration and copper recovery method |
| CN108668452A (en) * | 2018-06-12 | 2018-10-16 | 江苏博敏电子有限公司 | A kind of PCB fine-lines electrolytic etching recycles correlation technology with copper |
| CN108531914A (en) * | 2018-06-15 | 2018-09-14 | 哈尔滨工业大学深圳研究生院 | A kind of H2SO4/S2O82-The copper of microetch waste liquid recycles and synchronizing regeneration micro etching solution system and method |
| CN108950563A (en) * | 2018-07-16 | 2018-12-07 | 深圳市祺鑫天正环保科技有限公司 | Acid etching regenerates solution additive and acid etching regenerated liquid |
| 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 |
| CN110408936B (en) * | 2019-07-18 | 2021-09-03 | 惠州市臻鼎环保科技有限公司 | Method for electrolyzing acidic etching waste liquid of circuit board |
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| CN100494500C (en) | 2009-06-03 |
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Assignee: Shenzhen Dongjiang Environmental Protection Co., Ltd. Assignor: Liu Jingliang Contract fulfillment period: 2009.5.20 to 2014.5.19 contract change Contract record no.: 2009440000513 Denomination of invention: Method for simultaneous electrolysis and regeneration of acid etching solution and micro-etching solution Granted publication date: 20090603 License type: Exclusive license Record date: 2009.6.18 |
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Owner name: YAN TAT PRINTED CIRCUIT (SHENZHEN) CO., LTD. Free format text: FORMER OWNER: LIU JINGLIANG Effective date: 20140925 |
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Effective date of registration: 20140925 Address after: 518000 Guangdong province Shenzhen Pingshan New District Shenzhen Industrial Zone No. 8 Endalu Patentee after: Yan Tat Circuit (Shenzhen) Co., Ltd. Address before: 108 7H, 518057 village, Futian District, Shenzhen, Guangdong, Yitian Patentee before: Liu Jingliang |