CN108866550B - Process flow for manufacturing electrolytic copper foil by using internal circulation etching solution - Google Patents
Process flow for manufacturing electrolytic copper foil by using internal circulation etching solution Download PDFInfo
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- 238000005530 etching Methods 0.000 title claims abstract description 72
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000011889 copper foil Substances 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 106
- 238000005406 washing Methods 0.000 claims abstract description 68
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 53
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000000605 extraction Methods 0.000 claims abstract description 43
- 239000011888 foil Substances 0.000 claims abstract description 31
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 30
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 28
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 28
- 239000002699 waste material Substances 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 238000004064 recycling Methods 0.000 claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000011084 recovery Methods 0.000 claims description 61
- 239000007788 liquid Substances 0.000 claims description 46
- 239000002912 waste gas Substances 0.000 claims description 16
- 239000000654 additive Substances 0.000 claims description 9
- 230000000996 additive effect Effects 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000003595 mist Substances 0.000 claims description 8
- 238000001471 micro-filtration Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 230000032798 delamination Effects 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000005018 casein Substances 0.000 claims description 3
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 claims description 3
- 235000021240 caseins Nutrition 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 239000003350 kerosene Substances 0.000 claims description 3
- 238000005868 electrolysis reaction Methods 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/30—Oximes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Electrolytic Production Of Metals (AREA)
- ing And Chemical Polishing (AREA)
- Manufacturing Of Printed Circuit Boards (AREA)
Abstract
The invention discloses a process flow for manufacturing electrolytic copper foil by using an internal circulation etching solution, which comprises the steps of extracting copper ions in an etching waste solution by using an extracting agent, conveying the extracting agent containing the copper ions to a washing tank to wash out chloride ions in the extracting agent, conveying the extracting agent containing the copper ions to a back-extraction tank to react with a sulfuric acid solution to obtain a copper sulfate solution, and finally conveying the copper sulfate solution to a foil-producing tank to produce the copper foil; the etching solution, the extracting agent, the ammonia washing water and the sulfuric acid which are used in the process can be recycled and reused without damage, so that the waste of resources is not caused, the waste etching solution is not required to be delivered to a recycling company to produce copper foil, the production link is reduced, the etching solution can be recycled and put into use, the copper foil can be produced independently to be sold, and the economic benefit is greatly improved.
Description
Technical Field
The invention relates to the field of etching solution regenerated copper foil, in particular to a process flow for manufacturing electrolytic copper foil by using internal circulation etching solution.
Background
Since 2002, the production value of the printed circuit board in China has been discharged to the third position of the world, and the printed circuit board is used as a substrate material of a PCB (printed Circuit Board) -a copper-clad plate, so that China also becomes the third country of production for producing the copper-clad plate in the world, and the electrolytic copper foil industry in China has been developed rapidly in recent years. For producing circuit boards, the production of etching solution is an indispensable part, and during the production of circuit boards, a large amount of etching solution containing copper components is generated, and the copper content is about 120-140 g/L. The traditional treatment method of the etching solution by using the ammonia water and the ammonium chloride is that circuit board production enterprises sell the etching solution as waste liquid to a recovery company, and then the recovery company produces copper sulfate products by using the waste liquid as raw materials, so that not only is the resource waste caused by the fact that a large amount of ammonia-containing liquid cannot be effectively utilized and has certain influence on the environment, but also other raw materials such as extract liquor and ammonia washing water cannot be effectively recycled and cannot produce sufficient economic benefit.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a process flow for manufacturing the electrolytic copper foil by using the internal circulation etching solution, which not only does not cause resource waste, but also can recycle various raw materials without loss, thereby greatly improving the economic benefit.
The technical scheme adopted by the invention for solving the problems is as follows:
the process flow for manufacturing the electrolytic copper foil by using the internal circulation etching solution is characterized by comprising the following steps of:
etching waste liquid stored in a T10 tank, extractant stored in a T20 tank, ammonia washing water stored in a T32 tank, sulfuric acid stored in a green foil tank;
conveying the etching waste liquid in the T10 cylinder to an extraction cylinder, conveying an extracting agent in the T20 cylinder to the extraction cylinder, uniformly stirring, standing and layering;
conveying the lower layer solution, namely the etching recovery solution, which is layered in the extraction cylinder to a T13 cylinder, adding an ammonia additive into the T13 cylinder to adjust the pH value of the etching recovery solution, and conveying the etching recovery solution to a T14 cylinder for production after the etching recovery solution is analyzed to be qualified;
conveying the upper-layer solution after layering in the extraction cylinder, namely the extractant containing copper ions, to a water washing cylinder, conveying ammonia washing water in a T32 cylinder to the water washing cylinder, uniformly stirring, and standing for layering;
conveying the lower layer solution, namely ammonia washing water recovery liquid, which is layered in the water washing cylinder to a T31 cylinder, adding a regulator into the T31 cylinder to adjust the pH value of the ammonia washing water recovery liquid, and conveying the ammonia washing water recovery liquid to a T32 cylinder for recycling after the ammonia washing water recovery liquid is analyzed to be qualified;
conveying the upper-layer solution which is layered in the water washing cylinder and contains copper ions but no chloride ions into a back extraction cylinder, conveying sulfuric acid in the raw foil tank into the back extraction cylinder, uniformly stirring, and standing for layering;
the lower layer solution which is the copper sulfate solution after being layered in the stripping cylinder is precisely filtered and then is conveyed into a foil generating tank, and a copper foil is electrolyzed through the foil generating tank;
and (4) conveying the upper solution which is layered in the stripping cylinder, namely the extractant without copper ions, to a T20 cylinder for recycling.
Further, the method also comprises the following steps: and (3) treating waste gas generated in the copper foil electrolysis of the green foil tank by an acid mist tower and then discharging the waste gas.
Further, the method also comprises the following steps: and (3) treating waste gas generated when the ammonia additive is added into the T13 cylinder by an acid mist tower and then discharging the waste gas.
Further, before the lower layer solution after the delamination in the extraction cylinder, namely the etching recovery solution, is conveyed to the T13 cylinder, the method also comprises the following steps: and the lower layer solution, namely the etching recovery solution after the delamination in the extraction cylinder automatically flows to a T11 cylinder, the etching recovery solution in the T11 cylinder is pumped to a T12 cylinder for storage, and the etching recovery solution stored in the T12 cylinder is conveyed to a T13 cylinder.
Further, before the lower layer solution after layering in the water washing tank, namely the ammonia washing water recovery liquid, is conveyed to the T31 tank, the method further comprises the following steps: and (3) enabling the lower layer solution after the layering in the water washing cylinder, namely the ammonia washing water recovery solution to flow to a T30 cylinder, and pumping the ammonia washing water recovery solution in the T30 cylinder to a T31 cylinder.
Further, before the lower layer solution, namely the copper sulfate solution, which is separated in the stripping cylinder is subjected to microfiltration, the method also comprises the following steps: and (3) automatically flowing the lower layer solution, namely the copper sulfate solution, which is layered in the stripping tank to a T40 tank for storage, and then carrying out precise filtration on the copper sulfate solution in the T40 tank.
Further, after the copper sulfate solution in the T40 cylinder is subjected to microfiltration, the method also comprises the following steps: and conveying the copper sulfate solution subjected to microfiltration in the T40 cylinder to a head tank, and automatically flowing into a crude foil tank from the head tank.
Further, the extractant stored in the T20 cylinder is AB oil of N510N910 series compounds, the AB oil comprises A oil and B oil, the A oil comprises N510 compounds and N910 compounds, the B oil comprises kerosene, and the volume ratio of the A oil to the B oil is 1: 3; the ammonia washing water stored in the T32 cylinder is dilute sulfuric acid with the concentration of 0.2 percent; the sulfuric acid stored in the crude foil tank is concentrated sulfuric acid with the concentration of 20-30%, and animal glue, thiourea, casein and hydrochloric acid are also added into the concentrated sulfuric acid.
Further, the extraction jar is tertiary extraction jar.
Further, the stripping cylinder is a secondary stripping cylinder.
The invention has the beneficial effects that: the invention adopts a process flow for manufacturing electrolytic copper foil by using an internal circulation etching solution, which comprises the steps of extracting copper ions in etching waste liquid by using an extracting agent, conveying the extracting agent containing the copper ions to a washing tank to wash out chloride ions in the extracting agent, conveying the extracting agent containing the copper ions to a back extraction tank to react with a sulfuric acid solution to obtain a copper sulfate solution, and finally conveying the copper sulfate solution to a foil generation tank to generate the copper foil; the etching solution, the extracting agent, the ammonia washing water and the sulfuric acid which are used in the process can be recycled and reused without damage, so that the waste of resources is not caused, the waste etching solution is not required to be delivered to a recycling company to produce copper foil, the production link is reduced, the etching solution can be recycled and put into use, the copper foil can be produced independently to be sold, and the economic benefit is greatly improved.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic view of a process flow for manufacturing an electrolytic copper foil by using an internal circulation etching solution according to the present invention.
Detailed Description
Referring to fig. 1, the process flow for manufacturing the electrolytic copper foil by using the internal circulation etching solution comprises the following steps:
etching waste liquid stored in a T10 tank, extractant stored in a T20 tank, ammonia washing water stored in a T32 tank, sulfuric acid stored in a green foil tank; some etching waste liquid is generated in the process of producing the PCB, and in order to store and extract copper from the etching waste liquid, the etching waste liquid is stored in a T10 tank. In addition, the extractant, ammonia wash water and sulfuric acid were also stored in a T20 tank, a T32 tank and a green foil tank, respectively.
Conveying the etching waste liquid in the T10 cylinder to an extraction cylinder, conveying an extracting agent in the T20 cylinder to the extraction cylinder, uniformly stirring, standing and layering; because the etching waste liquid contains a large amount of copper ions, in order to extract the copper ions in the etching waste liquid, an extracting agent is adopted to extract the copper ions in the etching waste liquid, after standing and layering, the lower layer of the solution in the extraction cylinder is etching recovery liquid with extremely low copper ion content, and the upper layer of the solution is the extracting agent rich in copper ions.
Conveying the lower layer solution, namely the etching recovery solution, which is layered in the extraction cylinder to a T13 cylinder, adding an ammonia additive into the T13 cylinder to adjust the pH value of the etching recovery solution, and conveying the etching recovery solution to a T14 cylinder for production after the etching recovery solution is analyzed to be qualified; in order to realize the recycling of the etching recovery liquid, the lower layer solution which is the layered lower layer solution in the extraction cylinder, namely the etching recovery liquid, is extracted, the pH value of the etching recovery liquid is adjusted by adding an ammonia additive, and the etching recovery liquid meets the pH value condition of recycling, is conveyed to a T14 cylinder for storage and is used for etching treatment of copper-clad plates in the future.
Conveying the upper-layer solution after layering in the extraction cylinder, namely the extractant containing copper ions, to a water washing cylinder, conveying ammonia washing water in a T32 cylinder to the water washing cylinder, uniformly stirring, and standing for layering; because the extractant also contains chloride ions which have certain influence on the subsequent electrolytic copper foil, in order to remove the chloride ions in the extractant, the extractant containing the copper ions is conveyed into a water washing tank, and the extractant is washed by ammonia washing water so as to wash out the chloride ions in the extractant. And after standing and layering, the lower layer of the solution in the water washing tank is ammonia washing water recovery liquid, and the upper layer of the solution is an extractant containing copper ions but not containing chloride ions.
Conveying the lower layer solution, namely ammonia washing water recovery liquid, which is layered in the water washing cylinder to a T31 cylinder, adding a regulator into the T31 cylinder to adjust the pH value of the ammonia washing water recovery liquid, and conveying the ammonia washing water recovery liquid to a T32 cylinder for recycling after the ammonia washing water recovery liquid is analyzed to be qualified; in order to realize the recycling of the ammonia washing water recovery liquid, the layered lower layer solution in the washing cylinder, namely the ammonia washing water recovery liquid, is extracted, the pH value of the ammonia washing water recovery liquid is adjusted by adding a regulator, and the ammonia washing water recovery liquid meets the pH value condition of recycling and is conveyed to a T32 cylinder for recycling.
Conveying the upper-layer solution which is layered in the water washing cylinder and contains copper ions but no chloride ions into a back extraction cylinder, conveying sulfuric acid in the raw foil tank into the back extraction cylinder, uniformly stirring, and standing for layering; in order to realize the electrolysis of the copper foil, the extractant is firstly subjected to back extraction to extract copper ions in the extractant, the extractant containing the copper ions but not containing chloride ions is conveyed into a back extraction cylinder, sulfuric acid in a raw foil tank is injected into the back extraction cylinder, and a copper sulfate solution is generated through reaction, so that the copper ions are extracted from the extractant. And after standing and layering, the lower layer of the solution in the back extraction cylinder is a copper sulfate solution, and the upper layer of the solution is an extracting agent without copper ions.
The lower layer solution which is the copper sulfate solution after being layered in the stripping cylinder is precisely filtered and then is conveyed into a foil generating tank, and a copper foil is electrolyzed through the foil generating tank; in order to realize the recycling of copper foil produced by electrolysis and sulfuric acid, the layered lower layer solution in the stripping cylinder, namely copper sulfate solution, is precisely filtered and then conveyed into a raw foil tank, and a cathode roller is used for electrolysis in the raw foil tank, so that the copper foil is electrolyzed at the same time, and the sulfuric acid generated by reaction returns to the raw foil tank to realize the recycling.
And (4) conveying the upper solution which is layered in the stripping cylinder, namely the extractant without copper ions, to a T20 cylinder for recycling. In order to realize the recycling of the extractant, the upper-layer solution after layering in the stripping tank, namely the extractant without copper ions, is conveyed to the T20 tank for recycling.
The process flow for manufacturing the electrolytic copper foil by the internally circulating etching solution comprises the steps of extracting copper ions in the etching waste liquid by using an extracting agent, conveying the extracting agent containing the copper ions to a washing tank to wash out chloride ions in the extracting agent, conveying the extracting agent containing the copper ions to a back-extraction tank to react with a sulfuric acid solution to obtain a copper sulfate solution, and finally conveying the copper sulfate solution to a foil-producing tank to produce the copper foil; the etching solution, the extracting agent, the ammonia washing water and the sulfuric acid which are used in the process can be recycled and reused without damage, so that the waste of resources is not caused, the waste etching solution is not required to be delivered to a recycling company to produce copper foil, the production link is reduced, the etching solution can be recycled and put into use, the copper foil can be produced independently to be sold, and the economic benefit is greatly improved.
Further, the method also comprises the following steps: and (3) treating waste gas generated in the copper foil electrolysis of the green foil tank by an acid mist tower and then discharging the waste gas. Because waste gas is generated when the raw foil tank electrolyzes the copper foil, in order to not pollute the air environment, the waste gas generated when the raw foil tank electrolyzes the copper foil is discharged after being treated by the acid mist tower, and the method is green and environment-friendly.
Further, the method also comprises the following steps: and (3) treating waste gas generated when the ammonia additive is added into the T13 cylinder by an acid mist tower and then discharging the waste gas. Because waste gas is generated when the ammonia additive is added into the T13 cylinder, in order to prevent pollution to the air environment, the waste gas generated when the ammonia additive is added into the T13 cylinder is treated by the acid mist tower and then discharged, and the method is green and environment-friendly.
Further, before the lower layer solution after the delamination in the extraction cylinder, namely the etching recovery solution, is conveyed to the T13 cylinder, the method also comprises the following steps: and the lower layer solution, namely the etching recovery solution after the delamination in the extraction cylinder automatically flows to a T11 cylinder, the etching recovery solution in the T11 cylinder is pumped to a T12 cylinder for storage, and the etching recovery solution stored in the T12 cylinder is conveyed to a T13 cylinder. In order to avoid disturbance to the solution in the extraction cylinder when the etching recovery liquid is conveyed, the lower layer solution in the extraction cylinder, namely the etching recovery liquid, is obtained in a self-flowing mode correspondingly.
Further, before the lower layer solution after layering in the water washing tank, namely the ammonia washing water recovery liquid, is conveyed to the T31 tank, the method further comprises the following steps: and (3) enabling the lower layer solution after the layering in the water washing cylinder, namely the ammonia washing water recovery solution to flow to a T30 cylinder, and pumping the ammonia washing water recovery solution in the T30 cylinder to a T31 cylinder. In order to avoid disturbance to the solution in the washing cylinder when the ammonia washing water recovery liquid is conveyed, the lower layer solution in the washing cylinder, namely the ammonia washing water recovery liquid, is obtained in a self-flowing mode correspondingly.
Further, before the lower layer solution, namely the copper sulfate solution, which is separated in the stripping cylinder is subjected to microfiltration, the method also comprises the following steps: and (3) automatically flowing the lower layer solution, namely the copper sulfate solution, which is layered in the stripping tank to a T40 tank for storage, and then carrying out precise filtration on the copper sulfate solution in the T40 tank.
Further, after the copper sulfate solution in the T40 cylinder is subjected to microfiltration, the method also comprises the following steps: and conveying the copper sulfate solution subjected to microfiltration in the T40 cylinder to a head tank, and automatically flowing into a crude foil tank from the head tank.
Further, the extractant stored in the T20 cylinder is AB oil of N510N910 series compounds, the AB oil comprises A oil and B oil, the A oil comprises N510 compounds and N910 compounds, the B oil comprises kerosene, and the volume ratio of the A oil to the B oil is 1: 3; the ammonia washing water stored in the T32 cylinder is dilute sulfuric acid with the concentration of 0.2 percent; the sulfuric acid stored in the crude foil tank is concentrated sulfuric acid with the concentration of 20-30%, and animal glue, thiourea, casein and hydrochloric acid are also added into the concentrated sulfuric acid.
Further, the extraction jar is tertiary extraction jar.
Further, the stripping cylinder is a secondary stripping cylinder.
The above description is only a preferred embodiment of the present invention, and the present invention is not limited to the above embodiment, and the present invention shall fall within the protection scope of the present invention as long as the technical effects of the present invention are achieved by the same means.
Claims (1)
1. The process flow for manufacturing the electrolytic copper foil by using the internal circulation etching solution is characterized by comprising the following steps of:
etching waste liquid stored in a T10 tank, extractant stored in a T20 tank, ammonia washing water stored in a T32 tank, sulfuric acid stored in a green foil tank;
conveying the etching waste liquid in the T10 cylinder to an extraction cylinder, conveying an extracting agent in the T20 cylinder to the extraction cylinder, uniformly stirring, standing and layering;
conveying the lower layer solution, namely the etching recovery solution, which is layered in the extraction cylinder to a T13 cylinder, adding an ammonia additive into the T13 cylinder to adjust the pH value of the etching recovery solution, and conveying the etching recovery solution to a T14 cylinder for production after the etching recovery solution is analyzed to be qualified;
conveying the upper-layer solution after layering in the extraction cylinder, namely the extractant containing copper ions, to a water washing cylinder, conveying ammonia washing water in a T32 cylinder to the water washing cylinder, uniformly stirring, and standing for layering;
conveying the lower layer solution, namely ammonia washing water recovery liquid, which is layered in the water washing cylinder to a T31 cylinder, adding a regulator into the T31 cylinder to adjust the pH value of the ammonia washing water recovery liquid, and conveying the ammonia washing water recovery liquid to a T32 cylinder for recycling after the ammonia washing water recovery liquid is analyzed to be qualified;
conveying the upper-layer solution which is layered in the water washing cylinder and contains copper ions but no chloride ions into a back extraction cylinder, conveying sulfuric acid in the raw foil tank into the back extraction cylinder, uniformly stirring, and standing for layering;
the lower layer solution which is the copper sulfate solution after being layered in the stripping cylinder is precisely filtered and then is conveyed into a foil generating tank, and a copper foil is electrolyzed through the foil generating tank;
conveying the upper-layer solution which is layered in the stripping cylinder and is the extractant without copper ions to a T20 cylinder for recycling;
further comprising the steps of: treating waste gas generated in the process of electrolyzing copper foil in the foil generating tank by an acid mist tower and then discharging the waste gas;
further comprising the steps of: treating waste gas generated when the ammonia additive is added into the T13 cylinder by an acid mist tower and then discharging the waste gas;
before the lower layer solution, namely the etching recovery solution, which is layered in the extraction cylinder is conveyed to a T13 cylinder, the method further comprises the following steps: the lower layer solution, namely the etching recovery solution after the delamination in the extraction cylinder automatically flows to a T11 cylinder, the etching recovery solution in the T11 cylinder is pumped to a T12 cylinder for storage, and the etching recovery solution stored in the T12 cylinder is conveyed to a T13 cylinder;
before the lower layer solution after layering in the water washing cylinder, namely the ammonia washing water recovery liquid, is conveyed to a T31 cylinder, the method further comprises the following steps: the lower layer solution after being layered in the water washing cylinder, namely the ammonia washing water recovery solution, automatically flows to a T30 cylinder, and then the ammonia washing water recovery solution in the T30 cylinder is pumped to a T31 cylinder;
before the lower layer solution, namely the copper sulfate solution after the delamination in the stripping cylinder is subjected to the precise filtration, the method also comprises the following steps: the lower layer solution after being layered in the stripping tank, namely the copper sulfate solution, automatically flows to a T40 tank for storage, and then the copper sulfate solution in the T40 tank is subjected to precise filtration;
after the copper sulfate solution in the T40 cylinder is subjected to microfiltration, the method also comprises the following steps: conveying the copper sulfate solution subjected to precision filtration in the T40 cylinder to a head tank, and automatically flowing into a crude foil tank from the head tank;
the extractant stored in the T20 cylinder is AB oil, the AB oil comprises A oil and B oil, the A oil comprises N510 compounds and N910 compounds, the B oil comprises kerosene, and the volume ratio of the A oil to the B oil is 1: 3; the ammonia washing water stored in the T32 cylinder is dilute sulfuric acid with the concentration of 0.2 percent; the sulfuric acid stored in the crude foil tank is concentrated sulfuric acid with the concentration of 20-30%, and animal glue, thiourea, casein and hydrochloric acid are also added into the concentrated sulfuric acid;
the extraction cylinder is a three-stage extraction cylinder;
the back extraction cylinder is a secondary back extraction cylinder.
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| CN105018724A (en) * | 2014-04-30 | 2015-11-04 | 天津开发区均诚纸业有限公司 | Copper ore processing technology |
| CN205062198U (en) * | 2015-09-16 | 2016-03-02 | 灵宝金源矿业股份有限公司 | Be arranged in electrolysis plumbe skill acid mist processing apparatus |
| CN106282567A (en) * | 2015-05-29 | 2017-01-04 | 陕西瑞凯环保科技有限公司 | A kind of method reclaiming metal from useless acidic etching liquid |
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| JP5215111B2 (en) * | 2008-08-25 | 2013-06-19 | 水ｉｎｇ株式会社 | Method and apparatus for recovering copper from acidic waste liquid containing copper |
| CN102912142B (en) * | 2012-11-06 | 2013-12-04 | 赣州聚环科技有限公司 | Method for recycling copper from etching solution through combination of multistage cross current and counter current |
| CN107385470A (en) * | 2016-05-17 | 2017-11-24 | 陕西安信显像管循环处理应用有限公司 | Cupric spent etching solution recovery method |
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| CN105018724A (en) * | 2014-04-30 | 2015-11-04 | 天津开发区均诚纸业有限公司 | Copper ore processing technology |
| CN106282567A (en) * | 2015-05-29 | 2017-01-04 | 陕西瑞凯环保科技有限公司 | A kind of method reclaiming metal from useless acidic etching liquid |
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