CN113373479A - Process for treating acid liquor and recovering copper by using acidic etching liquid - Google Patents
Process for treating acid liquor and recovering copper by using acidic etching liquid Download PDFInfo
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- CN113373479A CN113373479A CN202110645134.9A CN202110645134A CN113373479A CN 113373479 A CN113373479 A CN 113373479A CN 202110645134 A CN202110645134 A CN 202110645134A CN 113373479 A CN113373479 A CN 113373479A
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- copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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- 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
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/18—Acidic compositions for etching copper or alloys thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention belongs to the technical field of copper recovery, in particular to a process for treating acid liquor and recovering copper by using acidic etching liquid, aiming at the problems that the existing copper recovery process is complex, the acid liquor is not directly discharged after treatment, and the environment is seriously damaged, the following scheme is proposed, and the process comprises the following process steps: s1: filtering the waste acidic etching liquid treatment acid liquor; s2: heating the acid liquor treated by the acidic etching liquid to remove oil; s3: filtering waste gas; s4: acid-base neutralization of acid etching liquid treatment acid liquor; s5: evaporating the excess water; s6: recovering copper by flowing electrolysis; s7: copper collection, purification and smelting; s8: and (6) treating waste liquid. The copper recovery process is simple to operate, can extract, neutralize and concentrate acid liquor, and can improve the electrolysis efficiency; the acid liquor adopts flowing water type electrolysis, so that copper ions are activated, the moving range of the copper ions is increased, the electrolysis efficiency is improved, and the circular flow can be used for multiple times of electrolysis.
Description
Technical Field
The invention relates to the technical field of copper recovery, in particular to a process for treating acid liquor and recovering copper by using acidic etching liquid.
Background
With the continuous improvement of the living standard of people, the quantity of waste household appliances is increased, the cleaning of the internal circuit board generally adopts acid liquid, the waste household appliances are generally recovered by a crushing method, and copper and other metal mixtures are obtained by separation after crushing.
Acid liquor in the surface treatment of circuit boards or metals contains a large amount of copper, the existing copper recovery process is complex, and the acid liquor is not directly discharged in the treatment process, so that the environmental pollution is caused.
Disclosure of Invention
The invention aims to solve the defects that the existing copper recovery process is complex, acid liquor treatment is not directly discharged, and serious harm is caused to the environment.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process for recovering copper comprising the process steps of:
s1: filtering the waste acidic etching liquid treatment acid liquor;
s2: heating the acid liquor treated by the acidic etching liquid to remove oil;
s3: filtering waste gas;
s4: acid-base neutralization of acid etching liquid treatment acid liquor;
s5: evaporating the excess water;
s6: recovering copper by flowing electrolysis;
s7: copper collection, purification and smelting;
s8: and (6) treating waste liquid.
Preferably, in S1, the waste acidic etching liquid treatment acid liquid is filtered by the coarse mesh and the fine mesh in sequence, so as to remove the block particles and the scum.
Preferably, in S2, the acidic etching liquid treatment acid solution is heated at 45-55 ℃ so that the grease in the liquid is melted and floats on the surface, and the grease on the surface is adsorbed by using oily paper for a plurality of times until the grease is removed.
Preferably, in S3, when the acidic etching liquid treatment acid solution is heated, acidic water vapor floats, and the acidic water vapor is filtered by introducing steam into the alkaline tank and using the principle of acid-base neutralization.
Preferably, in S4, a PH test paper is used to detect the acidity of the acidic etching liquid treatment acid solution, and an alkaline solution is used to mix the acidic etching liquid treatment acid solution with stirring until the PH reaches 6-8.
Preferably, the S5 is characterized in that the neutralized liquid is evaporated by an evaporator to purify and concentrate the liquid to 1/2 as it is, and the evaporation heating temperature is 80 to 90 ℃.
Preferably, in S6, two electrode plates are used to electrolyze the liquid, wherein one electrode plate is an anode and one electrode plate is a cathode, the liquid is contacted with the two electrode plates in a circulating manner, and the liquid level is kept constant, so that both electrode plates are immersed in the liquid, and electrolysis is performed electrically.
Preferably, the electrolysis temperature is controlled to be 60-70 ℃ in S6, a large amount of electrolytic copper is attached to the cathode plate during electrolysis, meanwhile, an external exhaust fan is adopted to extract harmful gas in the electrolytic cell during electrolysis, the harmful gas is collected and treated, and external fresh air is brought into the electrolytic cell by an external blower to form air circulation.
Preferably, after the electrolysis in S7 is completed, the cathode plate is moved to an oxidation resistance tank, an antioxidant solution is added into the oxidation resistance tank, the antioxidant solution performs oxidation resistance treatment on the surface of the cathode copper plate, an oxidation resistance layer is attached to the surface of the cathode copper plate, the cathode copper plate attached with the oxidation resistance layer is finally removed, copper is detached from the cathode plate, electrolytic copper can be collected, the barrel is cleaned by alkaline liquid, the residual acidic impurities are cleaned, the barrel is smelted and collected, and further purification can be performed.
Preferably, the waste liquid is treated after the electrolysis in S9, the electrolyte in the electrolytic cell is pumped away and treated, the remaining fine impurities in the sewage are further purified by using quartz sand, the purified water enters an activated carbon filter, the activated carbon filter can remove the toxic and harmful substances such as chroma and peculiar smell in the sewage, and the subsequent reverse osmosis treatment is pretreated.
The invention further provides an acidic etching liquid treatment acid liquid, which comprises copper chloride, hydrochloric acid, sodium chloride and ammonium chloride, and the acidic etching liquid treatment acid liquid is any one of the acidic etching liquid treatment acid liquids.
Compared with the prior art, the invention has the advantages that:
the copper recovery process is simple to operate, can extract, neutralize and concentrate acid liquor, and can improve the electrolysis efficiency; the acid liquor adopts flowing water type electrolysis, so that copper ions are activated, the moving range of the copper ions is increased, the electrolysis efficiency is improved, and the circular flow can be used for multiple times of electrolysis; the acid liquor is discharged after being treated, so that the harm to the environment is avoided.
Drawings
FIG. 1 is a schematic structural diagram of a process for treating acid solution and recovering copper with an acidic etching liquid according to the present invention
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example one
Referring to fig. 1, a process for recovering copper includes the following process steps:
s1: filtering the waste acidic etching liquid treatment acid liquor;
s2: heating the acid liquor treated by the acidic etching liquid to remove oil;
s3: filtering waste gas;
s4: acid-base neutralization of acid etching liquid treatment acid liquor;
s5: evaporating the excess water;
s6: recovering copper by flowing electrolysis;
s7: copper collection, purification and smelting;
s8: and (6) treating waste liquid.
In this embodiment, in S1, the coarse mesh and the fine mesh are sequentially used to filter the waste acidic etching liquid treatment acid solution, so as to remove the bulk particles and scum.
In this embodiment, in S2, the acidic etching liquid treatment acid solution is heated at 45 to 55 ℃ so that the grease in the liquid is melted and floats on the surface, and the grease on the surface is adsorbed by the oily paper for a plurality of times until the grease is removed.
In this embodiment, in S3, when the acidic etching liquid treatment acid solution is heated, acidic water vapor floats, and the acidic water vapor is filtered by introducing steam into the alkaline tank and utilizing the principle of acid-base neutralization.
In this embodiment, in S4, PH paper is used to detect the acidity of the acidic etching liquid treatment acid solution, and an alkaline solution is used to mix the acidic etching liquid treatment acid solution and the alkaline solution is continuously stirred until the PH reaches 6 to 8.
In this example, S5 evaporates the neutralized liquid using an evaporator to purify and concentrate the liquid to 1/2 as it is, and the evaporation heating temperature is 80 to 90 ℃.
In this embodiment, in S6, two electrode plates are used to electrolyze the liquid, one of the electrode plates is an anode and the other is a cathode, the liquid is in contact with the two electrode plates in a circulating flow manner, and the liquid level is kept constant, so that both the electrode plates are immersed in the liquid, and the electrolysis is performed by applying electricity.
In the embodiment, the electrolysis temperature is controlled to be 60-70 ℃ in S6, a large amount of electrolytic copper is attached to the cathode plate during electrolysis, meanwhile, an external exhaust fan is adopted to extract harmful gas in the electrolytic cell in the electrolysis process, the harmful gas is collected and treated, and external fresh air is brought into the electrolytic cell by an external blower to form air circulation.
In this embodiment, move the negative plate to the anti oxidation groove after the electrolysis is accomplished in S7, add antioxidant solution in the anti oxidation groove, antioxidant solution carries out anti oxidation treatment to the cathode copper surface, an oxidation resisting layer is attached to the cathode copper surface, the cathode copper that will adhere to the oxidation resisting layer at last shifts out to pull down copper from the negative plate, can collect electrolytic copper, use alkaline liquid to wash a section of thick bamboo, will remain acid impurity sanitization, smelt the collection to a section of thick bamboo, can further purify.
In this embodiment, the waste liquid is treated after the electrolysis in S9, the electrolyte in the electrolytic cell is pumped away and treated, the remaining fine impurities in the sewage are further purified by using quartz sand, the purified water enters an activated carbon filter, and the activated carbon filter can remove the chroma and the peculiar smell of the sewage, and pretreats the subsequent reverse osmosis treatment.
The invention also provides an acidic etching liquid treatment acid liquor, which comprises copper chloride, hydrochloric acid, sodium chloride and ammonium chloride.
Example two
Referring to fig. 1, a process for recovering copper includes the following process steps:
s1: filtering the waste acidic etching liquid treatment acid liquor;
s2: heating the acid liquor treated by the acidic etching liquid to remove oil;
s3: filtering waste gas;
s4: acid-base neutralization of acid etching liquid treatment acid liquor;
s5: evaporating the excess water;
s6: recovering copper by flowing electrolysis;
s7: copper collection, purification and smelting;
s8: and (6) treating waste liquid.
In this embodiment, in S1, the waste acidic etching liquid treatment acid liquid is filtered through a coarse mesh and a fine mesh in sequence, and the coarse mesh is selected as 100 mesh, and the fine mesh is selected as 300 mesh.
In this embodiment, in S2, the acidic etching liquid treatment acid solution is heated at 45 to 55 ℃ so that the grease in the liquid is melted and floats on the surface, and the grease on the surface is adsorbed by the oily paper for a plurality of times until the grease is removed.
In this embodiment, in S3, when the acidic etching liquid treatment acid solution is heated, acidic water vapor floats, and the acidic water vapor is filtered by introducing steam into the alkaline tank and utilizing the principle of acid-base neutralization.
In this embodiment, in S4, PH paper is used to detect the acidity of the acidic etching liquid treatment acid solution, and an alkaline solution is used to mix the acidic etching liquid treatment acid solution and the alkaline solution is continuously stirred until the PH reaches 6 to 8.
In this example, S5 evaporates the neutralized liquid using an evaporator to purify and concentrate the liquid to 1/2 as it is, and the evaporation heating temperature is 80 to 90 ℃.
In this embodiment, in S6, two electrode plates are used to electrolyze the liquid, one of the electrode plates is an anode and the other is a cathode, the liquid is contacted with the two electrode plates in a circulating flow manner, and the liquid level is kept constant, so that the two electrode plates are immersed in the liquid, and the liquid is electrolyzed by energization and circulated by a circulation pump.
In the embodiment, the electrolysis temperature is controlled to be 60-70 ℃ in S6, a large amount of electrolytic copper is attached to the cathode plate during electrolysis, meanwhile, an external exhaust fan is adopted to extract harmful gas in the electrolytic cell in the electrolysis process, the harmful gas is collected and treated, and external fresh air is brought into the electrolytic cell by an external blower to form air circulation.
In this embodiment, move the negative plate to the anti oxidation groove after the electrolysis is accomplished in S7, add antioxidant solution in the anti oxidation groove, antioxidant solution carries out anti oxidation treatment to the cathode copper surface, an oxidation resisting layer is attached to the cathode copper surface, the cathode copper that will adhere to the oxidation resisting layer at last shifts out to pull down copper from the negative plate, can collect electrolytic copper, use alkaline liquid to wash a section of thick bamboo, will remain acid impurity sanitization, smelt the collection to a section of thick bamboo, can further purify.
In this example, soda lime solution was added to clean the copper, and then the copper was rinsed clean with clear water.
In this embodiment, the waste liquid is treated after the electrolysis in S9, the electrolyte in the electrolytic cell is pumped away and treated, the remaining fine impurities in the sewage are further purified by using quartz sand, the purified water enters an activated carbon filter, and the activated carbon filter can remove the chroma and the peculiar smell of the sewage, and pretreats the subsequent reverse osmosis treatment.
The invention also provides an acidic etching liquid treatment acid liquor, which comprises copper chloride, hydrochloric acid, sodium chloride and ammonium chloride, and is mainly applied to cleaning circuit boards, copper ions are remained in waste liquor after the circuit boards are cleaned, and then a cylinder is recovered, wherein the mechanism of the acidic etching liquid treatment acid liquor is as follows: the acid etching solution has the characteristics that the etching rate is easy to control, and the etching solution can achieve high etching quality in a stable state; meanwhile, the copper dissolving amount of the copper alloy is large; the acid etching solution is easy to regenerate and recycle, thereby reducing pollution.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A process for recovering copper, characterized by comprising the process steps of:
s1: filtering the waste acidic etching liquid treatment acid liquor;
s2: heating the acid liquor treated by the acidic etching liquid to remove oil;
s3: filtering waste gas;
s4: acid-base neutralization of acid etching liquid treatment acid liquor;
s5: evaporating the excess water;
s6: recovering copper by flowing electrolysis;
s7: copper collection, purification and smelting;
s8: and (6) treating waste liquid.
2. The process of claim 1, wherein the filtering of the spent acid etching liquid treatment acid solution with coarse and fine mesh in sequence at S1 removes bulk particles and dross.
3. The process for recovering copper according to claim 1, wherein the acidic etching liquid treatment acid solution is heated at 45-55 ℃ in S2, so that the grease in the liquid is melted and floats on the surface, and the grease on the surface is adsorbed by using oily paper for a plurality of times until the grease is removed.
4. The process for recovering copper according to claim 1, wherein in the step S3, when the acidic etching liquid treatment acid solution is heated, acidic water vapor floats, the vapor is introduced into the alkaline tank, and the acidic water vapor is filtered by utilizing the principle of acid-base neutralization.
5. The process for recovering copper as claimed in claim 1, wherein the acidic etching liquid treatment acid solution is tested for acidity using PH paper in S4, and mixed with alkaline solution without stirring until PH reaches 6-8.
6. The process of claim 1, wherein the S5 is obtained by evaporating the neutralized liquid by an evaporator to purify and concentrate the liquid to 1/2, and the heating temperature for evaporation is 80-90 ℃.
7. The process of claim 1, wherein in step S6, two electrode plates are used to electrolyze the liquid, one of the electrode plates is an anode and the other is a cathode, the liquid is contacted with the two electrode plates in a circulating flow manner, and the liquid level is kept constant, so that the two electrode plates are immersed in the liquid, the electrolysis temperature is 60-70 ℃, during electrolysis, a large amount of electrolytic copper is attached to the cathode plate, meanwhile, an external exhaust fan is used to extract the harmful gases in the electrolytic cell during electrolysis, collect and process the harmful gases, and an external blower is used to bring fresh air into the electrolytic cell to form air circulation.
8. The process of claim 1, wherein the cathode plate is moved to an oxidation resistant tank after the electrolysis in S7 is completed, an antioxidant solution is added into the oxidation resistant tank, the antioxidant solution performs oxidation resistant treatment on the surface of the cathode copper plate, an oxidation resistant layer is attached to the surface of the cathode copper plate, the cathode copper plate with the oxidation resistant layer is removed, the copper is detached from the cathode plate, the electrolytic copper can be collected, the barrel is cleaned by alkaline liquid, the residual acidic impurities are cleaned, the barrel is smelted and collected, and further purification can be performed.
9. The process of claim 1, wherein the waste liquid is treated after the electrolysis in S9, the electrolyte in the electrolytic cell is pumped out and treated, the fine impurities in the sewage are further purified by quartz sand, the purified water enters an activated carbon filter, and the activated carbon filter can remove the toxic and harmful substances such as chroma and peculiar smell in the sewage and pretreat the subsequent reverse osmosis treatment.
10. An acidic etching liquid treatment acid comprising copper chloride, hydrochloric acid, sodium chloride and ammonium chloride, wherein the acidic etching liquid treatment acid is the acidic etching liquid treatment acid according to any one of claims 1 to 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110645134.9A CN113373479A (en) | 2021-06-09 | 2021-06-09 | Process for treating acid liquor and recovering copper by using acidic etching liquid |
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| CN202110645134.9A CN113373479A (en) | 2021-06-09 | 2021-06-09 | Process for treating acid liquor and recovering copper by using acidic etching liquid |
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Citations (5)
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|---|---|---|---|---|
| CN101693997A (en) * | 2009-09-30 | 2010-04-14 | 深圳市洁驰科技有限公司 | Method for processing acidic etching waste solution of printed circuit board |
| CN103966607A (en) * | 2013-01-31 | 2014-08-06 | 西安瑞凯电力科技有限公司 | Method for recovering copper and hydrochloric acid from acid etching solution |
| CN106119852A (en) * | 2015-08-31 | 2016-11-16 | 叶旖婷 | The electrolytic recovery of a kind of acid copper chloride etching liquid and regeneration technology |
| CN108249670A (en) * | 2018-01-16 | 2018-07-06 | 张家港市佰坤物资有限公司 | A kind of acid etching liquid treatment acid solution and the technique for recycling copper |
| CN109881200A (en) * | 2019-04-10 | 2019-06-14 | 深圳市铿东科技有限公司 | A kind of regenerating alkaline etching liquid and its copper recovery method |
-
2021
- 2021-06-09 CN CN202110645134.9A patent/CN113373479A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101693997A (en) * | 2009-09-30 | 2010-04-14 | 深圳市洁驰科技有限公司 | Method for processing acidic etching waste solution of printed circuit board |
| CN103966607A (en) * | 2013-01-31 | 2014-08-06 | 西安瑞凯电力科技有限公司 | Method for recovering copper and hydrochloric acid from acid etching solution |
| CN106119852A (en) * | 2015-08-31 | 2016-11-16 | 叶旖婷 | The electrolytic recovery of a kind of acid copper chloride etching liquid and regeneration technology |
| CN108249670A (en) * | 2018-01-16 | 2018-07-06 | 张家港市佰坤物资有限公司 | A kind of acid etching liquid treatment acid solution and the technique for recycling copper |
| CN109881200A (en) * | 2019-04-10 | 2019-06-14 | 深圳市铿东科技有限公司 | A kind of regenerating alkaline etching liquid and its copper recovery method |
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