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WO2017041472A1 - Procédé et système à émission zéro de récupération et de réutilisation de solution résiduaire de gravure à l'acide - Google Patents

Procédé et système à émission zéro de récupération et de réutilisation de solution résiduaire de gravure à l'acide Download PDF

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Publication number
WO2017041472A1
WO2017041472A1 PCT/CN2016/077066 CN2016077066W WO2017041472A1 WO 2017041472 A1 WO2017041472 A1 WO 2017041472A1 CN 2016077066 W CN2016077066 W CN 2016077066W WO 2017041472 A1 WO2017041472 A1 WO 2017041472A1
Authority
WO
WIPO (PCT)
Prior art keywords
etching
liquid
tank
zero
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2016/077066
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English (en)
Chinese (zh)
Inventor
韦建敏
吴梅
赵兴文
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chengdu Honghua Environmental Protection Technology Co Ltd
Original Assignee
Chengdu Honghua Environmental Protection Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from CN201520694083.9U external-priority patent/CN204982052U/zh
Priority claimed from CN201510569200.3A external-priority patent/CN105177583B/zh
Application filed by Chengdu Honghua Environmental Protection Technology Co Ltd filed Critical Chengdu Honghua Environmental Protection Technology Co Ltd
Publication of WO2017041472A1 publication Critical patent/WO2017041472A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C25B1/26—Chlorine; Compounds thereof
    • 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
    • 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

Definitions

  • the present invention relates to a waste liquid processing system, and more particularly to a zero-emission acid etching waste liquid recycling method and system.
  • the acidic etching solution is an etching liquid for fine circuit fabrication of a printed circuit board and fabrication of an inner layer of a multilayer board.
  • the regeneration of acid etching old liquid is mainly converted into an acidic solution of suitable specific gravity, transparency and high oxidation-reduction potential by chemical and electrochemical methods to maintain stable and rapid etching of the printed circuit board.
  • Chemical regeneration is the main method for the regeneration of acidic copper chloride etching solution. The principle is to discharge a certain proportion of the old liquid (high specific gravity), add a certain amount of liquid (low specific gravity), or add a certain amount of water. , to adjust the specific gravity of the etching solution.
  • the oxidizing agent in the same sputum liquid oxidizes the monovalent copper ion to the divalent copper ion, or the oxidizing agent is separately added to increase the oxidation-reduction potential of the etching liquid, thereby restoring the original performance of the etching liquid.
  • Common oxidants are air, oxygen, chlorine, ozone, sodium hypochlorite, sodium chlorate, hydrogen peroxide, and the like.
  • electrochemical regeneration method is an online regeneration method.
  • Metallic copper with commercial value can be produced by electrolysis, but chlorine gas is generated at the same time to form a polluted exhaust gas, which not only pollutes the environment but also causes waste.
  • Chinese Patent Application No. 201020567155.0 discloses a copper ion acid etching solution regeneration system, which is used for online processing of an acidic etching solution, which is limited by the etching line production, and can only be etched with Simultaneous production, and the exhaust gas treatment device inside the system consumes the chlorine inside the system. Although it is environmentally friendly, it causes waste of resources, causing the loss of chlorine inside the system, and additional acid solution is needed to ensure the efficiency of the etching solution. technical problem
  • An object of the present invention is to overcome the disadvantages of the prior art and to provide an acid etching waste liquid recycling system for recycling resources and a method for recycling etching liquid.
  • a zero-emission acid etching waste liquid recycling method comprising electrolyzing metal copper in an etching waste liquid in an electrolytic cell and generating exhaust gas at the same time, after electrolysis
  • the etching waste liquid is recycled as a regenerating liquid, and the regenerating liquid is separated into a high acidity solution and a low acidity solution by an acid concentration technique, and the high acidity solution is directly returned to the etching line for recycling, and the low acidity solution is formulated into an oxidizing agent.
  • the exhaust gas is processed to produce a valuable product containing chlorine. No waste liquid is generated during the whole cycle to achieve true zero emissions.
  • Electrolytic treatment is used to electrolyze the acid etching waste liquid, and the cathode tank in the electrolytic tank is electrochemically reduced to obtain electrolytic copper, and the anode tank in the electrolytic tank is electrochemically oxidized to regenerate the etching liquid to be regenerated. Liquid, and some chlorine is produced;
  • etching production is not running online, the chlorine gas generated in the anode tank is processed to form a chlorine-containing product;
  • etching production online operation ⁇ chlorine gas and etching waste liquid to generate a new etching liquid, direct circulation application To the etching line;
  • regeneration liquid treatment the regeneration liquid enters the regeneration liquid circulation system, is concentrated to separate the high acidity liquid and the low acidity liquid, the high acidity liquid enters the etching production line as the etching liquid, and the low acidity liquid is used to prepare the oxidant .
  • a zero-emission acid etching waste liquid circulation device system comprising an etching liquid processing system, a regeneration liquid circulation system, a liquid distribution system, and a chlorine gas recovery system, wherein the etching liquid processing system includes an etching production line, a mother liquid storage tank, an electrolytic tank, and a dissolution
  • the electrolytic cell comprises a cathode tank, a membrane and an anode tank, the mother liquor storage tank, the cathode tank, the anode tank, and the dissolution absorption system are sequentially connected, and the etching production line is respectively connected with the mother liquid storage tank and the dissolution absorption system, and the dissolution absorption system is connected with the etching production line.
  • the regenerating liquid circulation system includes a regenerating liquid storage tank and a regenerating liquid processing system, and the anode tank, the regenerating liquid storage tank, the regenerating liquid processing system, and the etching production line are sequentially connected;
  • the dosing system includes a regenerating liquid processing system and a dosing device, and the rehydrating liquid treatment System, with The liquid device and the etching production line are sequentially connected;
  • the chlorine gas recovery system includes a gas scrubbing system and an exhaust gas treatment system, and the anode tank, the scrubbing system, and the exhaust gas treatment system are sequentially connected.
  • the membrane is a membrane, a cationic membrane or an anionic membrane.
  • the cathode tank is connected to a copper washing device.
  • An ion concentration detecting device is disposed in the electrolytic cell.
  • the apparatus and piping within the system are all made of an acid, alkali, and corrosion resistant material.
  • the regenerative liquid processing system is provided with an acidity detecting device, and an acidity detecting device is disposed in the liquid dispensing device.
  • the present invention has the following advantages:
  • the system is used for processing acidic etching waste liquid, and the etching liquid can be recycled and recycled in the same manner as the metal copper is extracted, so that the etching liquid processing can be performed offline, the processing efficiency is improved, and the reasonable distribution is facilitated.
  • Resources enable dynamic balancing of etching and etching solutions, avoiding waste of resources and achieving sustainable production
  • the electrolytic chlorine gas can be recovered, and the chlorine gas is dissolved in the production line to react with the cuprous ions to form divalent copper ions, and the regenerated etching liquid is directly returned to the production line for recycling, if not and etching.
  • the electrolyzed chlorine gas can be washed and further processed to produce a valuable product containing chlorine, which can be used in the dosing system to prepare acid or as a commodity, thereby avoiding environmental pollution, wasting resources, and realizing chlorine.
  • the circulation of water in the system reducing the addition of additives or oxidants, reducing production costs and saving resources.
  • FIG. 1 is a schematic structural view of an acid etching waste liquid recycling system for recycling resources
  • a zero-emission acid etching waste liquid circulation device system includes an etching liquid processing system, a regenerating liquid circulation system, a dosing system, and a chlorine gas recovery system, and the etching liquid processing system includes an etching production line 1 and a mother liquid.
  • the storage tank 2, the electrolysis tank and the dissolution absorption system 6, the electrolysis tank comprises a cathode tank 3, a membrane 4 and an anode tank 5, the mother liquor storage tank 2, the cathode tank 3, the anode tank 5, the dissolution absorption system 6 are sequentially connected, and the etching production line 1 respectively Interconnected with the mother liquor storage tank 2 and the dissolution absorption system 6, and the dissolution absorption system 6 is in communication with the etching line 1;
  • the regeneration liquid circulation system includes a regeneration liquid storage tank 10 and a regeneration liquid treatment system 11, and the anode tank 5, the regeneration liquid storage tank 10, the regeneration liquid treatment system 11 and the etching production line 1 are sequentially connected;
  • the dosing system includes a regenerant treatment system 11 and a dosing device 12, and the reconditioning solution processing system 11, the dosing device 12, and the etching line 1 are sequentially connected;
  • the chlorine gas recovery system includes a scrubbing system 7 and an exhaust gas treatment system 8, and the anode tank 5, the scrubbing system 7, and the exhaust gas treatment system 8 are sequentially connected.
  • the membrane 4 is a membrane, a cation membrane or an anion membrane, and different membranes can be used to control the flow rate of ions according to production needs.
  • the cathode tank 3 is connected to the copper washing device 9, and the electrolytic copper obtained by electrolysis in the cathode tank 3 is treated by the copper washing device 9, whereby copper metal having commercial value can be obtained.
  • an ion concentration detecting device is disposed in the electrolytic cell, so that the concentration of each ion in the electrolytic cell can be detected, thereby controlling the flow rate of the liquid, thereby facilitating rational utilization and resource allocation.
  • the device and the pipeline in the system are made of acid-proof, alkali-resistant and corrosion-resistant materials, thereby prolonging the service life of the system.
  • the regeneration liquid processing system 11 is provided with an acidity detecting device, and the liquid adjusting device 12 is provided with an acidity detecting device, so that the detection of the acidity can be performed, thereby controlling the flow rate of the liquid. It is conducive to rational use and allocation of resources to achieve sustainable production.
  • a zero-emission acid etching waste liquid recycling method comprises: electrolytically recovering metallic copper in an etching waste liquid in a cathode tank 3 of an electrolytic cell and generating exhaust gas in the anode tank 5, and etching waste liquid after electrolysis
  • the regeneration liquid is recycled, the regeneration liquid is separated into a high acidity solution and a low acidity solution in the regeneration liquid treatment system 11 by acid concentration technology, and the high acidity solution is directly returned to the etching line for recycling, and the low acidity solution is used. It can be added into the etchant in the liquid-dispensing device 12 and then added back to the etching line.
  • the exhaust gas is washed by the scrubbing system 7 and then enters the exhaust gas treatment system 8 to produce a valuable product containing chlorine. There is no waste liquid increase during the whole cycle. Produce and achieve true zero emissions.
  • a zero-emission acid etching waste liquid recycling method comprises the following steps:
  • etching production is not online operation ⁇ , the chlorine gas generated in the anode tank 5 is washed by the scrubbing system 7 and then enters the tail gas treatment system 8 to produce a valuable product containing chlorine; etching production online operation ⁇ , chlorine gas Entering the dissolution absorption system 6 and the acidic etching waste liquid to regenerate a new etching liquid, and directly applying it to the etching production line 1;
  • the regeneration liquid can be stored in the regeneration liquid storage tank 10, and the regeneration liquid enters the regeneration liquid circulation system 11 and is concentrated to separate a high acidity liquid and a low acidity liquid, and the high acidity liquid is used as an etching.
  • the liquid enters the etching line 1, and the low acidity liquid enters the dosing device 12 for preparing the oxidant;
  • the working process of the present invention is as follows:
  • the etching liquid flowing out of the etching production line 1 is partially stored in the dissolution absorption system 6 for storage, and the other portion is stored in the mother liquid storage tank 2, and the flow rate is controlled by the mother liquid storage tank 2 to make the mother liquid storage tank 2
  • the etching solution enters the cathode tank 3.
  • cuprous ions are reduced to divalent copper ions, and the divalent copper ions are reduced to electrolytic copper.
  • the remaining unreduced copper ions and other ions enter the anode tank 5 through the membrane 4.
  • Chloride ions are oxidized under the action of electrolysis in the anode tank 5 to form chlorine gas.
  • chlorine gas enters the solvent absorption system 6, and undergoes redox reaction with cuprous ions to obtain copper ions and an acidic liquid.
  • the liquid can be used as an etchant to enter the etching line 1 to complete the production; when the etching line 1 is not produced ⁇ , the chlorine gas enters the scrubbing system 7 to obtain pure chlorine gas after the impurity removal, and the pure chlorine gas enters the exhaust gas treatment system 8 and is reacted to form a valuable chlorine-containing product.
  • the liquid remaining after the electrolysis contains ions such as copper ions, chloride ions, and hydrogen ions as the regenerating liquid, and the regenerating liquid has weak acidity, and the regenerating liquid enters the regenerating liquid storage tank 10 to be stored, and is regenerated.
  • the storage tank 10 controls the flow rate to be delivered to the regenerating liquid processing system 11, and the regenerating liquid is concentrated in the regenerating liquid processing system 11 to separate the high acidity liquid and the low acidity liquid, and the high acidity liquid is stored as the etching liquid and the low acidity liquid separately.
  • the high acidity liquid can be transported to the etching line 1 for production, and the low acidity liquid is transported into the dosing system 12, and is formulated into a new liquid together with the oxidant, the additive, etc., and is slowly added back to the etching line to control the etching liquid.
  • ORP value Dynamic balancing can be achieved by controlling the degree of electrolysis and the flow of liquid, facilitating automated production and off-line processing of acid etching waste.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • ing And Chemical Polishing (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

Cette invention concerne un procédé et un système à émission zéro de récupération et de réutilisation de solution résiduaire de gravure à l'acide. Ledit procédé comprend un certain nombre d'étapes, comprenant : l'exécution d'une opération d'électrolyse ; l'exécution d'un traitement au gaz de chlore ; et l'exécution d'un traitement en solution. Une technique de concentration d'acide et une technique de recyclage et de réutilisation de gaz résiduaire sont utilisées pour éliminer efficacement le cuivre métallique à partir d'une solution résiduaire de gravure et permettre la récupération et la réutilisation de la solution de gravure, de sorte à empêcher la génération d'une quelconque solution résiduaire, et à atteindre une émission zéro. Ledit système à émission zéro de récupération et de réutilisation de solution résiduaire de gravure à l'acide comprend : un système de traitement de solution de gravure ; un système de réutilisation de solution récupérée ; un système de distribution de solution ; et un système de recyclage de gaz de chlore. Ledit système de traitement de solution de gravure comprend : une ligne de production de gravure (1) ; un réservoir de stockage de liqueur mère (2) ; une cellule électrolytique ; et un système d'absorption et de dissolution (6). Ladite cellule électrolytique comprend un compartiment de cathode (3) et un compartiment d'anode (5). Ledit système de réutilisation de solution récupérée comprend un réservoir de stockage de solution récupérée (10) et un système de traitement de solution récupérée (11). Ledit système à émission zéro de récupération et de réutilisation de solution résiduaire de gravure à l'acide est configuré pour traiter une solution résiduaire de gravure acide, et il peut extraire le cuivre métallique, effectuer une opération de production hors ligne, économiser les coûts et les ressources, et éviter la pollution environnementale.
PCT/CN2016/077066 2015-09-09 2016-03-23 Procédé et système à émission zéro de récupération et de réutilisation de solution résiduaire de gravure à l'acide Ceased WO2017041472A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN201510569200.3 2015-09-09
CN201520694083.9U CN204982052U (zh) 2015-09-09 2015-09-09 一种零排放酸性蚀刻废液循环再生系统
CN201510569200.3A CN105177583B (zh) 2015-09-09 2015-09-09 一种零排放酸性蚀刻废液循环再生方法及系统
CN201520694083.9 2015-09-09

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WO2017041472A1 true WO2017041472A1 (fr) 2017-03-16

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CN105177581A (zh) * 2015-09-09 2015-12-23 成都虹华环保科技股份有限公司 一种具有尾气处理功能的酸性蚀刻废液循环再生系统
CN204898084U (zh) * 2015-09-09 2015-12-23 成都虹华环保科技股份有限公司 一种可节约资源的酸性蚀刻废液循环再生系统
CN204982052U (zh) * 2015-09-09 2016-01-20 成都虹华环保科技股份有限公司 一种零排放酸性蚀刻废液循环再生系统
CN204982053U (zh) * 2015-09-09 2016-01-20 成都虹华环保科技股份有限公司 一种具有尾气处理功能的酸性蚀刻废液循环再生系统

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008139021A1 (fr) * 2007-05-16 2008-11-20 Pp Recycling Ltd. Procédé de régénération de produit d'attaque chimique usagé à base de chlorure de cuivre (ii) acide
CN101805083A (zh) * 2010-03-26 2010-08-18 南通市申海特种镀饰有限责任公司 一种从电镀废水中回收贵金属的工艺方法
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CN104630825A (zh) * 2015-01-20 2015-05-20 昆山美源达环保科技有限公司 一种酸性蚀刻液电解提铜装置及其工艺
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CN105177583A (zh) * 2015-09-09 2015-12-23 成都虹华环保科技股份有限公司 一种零排放酸性蚀刻废液循环再生方法及系统
CN105177581A (zh) * 2015-09-09 2015-12-23 成都虹华环保科技股份有限公司 一种具有尾气处理功能的酸性蚀刻废液循环再生系统
CN204898084U (zh) * 2015-09-09 2015-12-23 成都虹华环保科技股份有限公司 一种可节约资源的酸性蚀刻废液循环再生系统
CN204982052U (zh) * 2015-09-09 2016-01-20 成都虹华环保科技股份有限公司 一种零排放酸性蚀刻废液循环再生系统
CN204982053U (zh) * 2015-09-09 2016-01-20 成都虹华环保科技股份有限公司 一种具有尾气处理功能的酸性蚀刻废液循环再生系统

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