CN112410793A - Alkaline etching solution extraction electrolysis regeneration and copper recovery method - Google Patents
Alkaline etching solution extraction electrolysis regeneration and copper recovery method Download PDFInfo
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- CN112410793A CN112410793A CN202011224207.9A CN202011224207A CN112410793A CN 112410793 A CN112410793 A CN 112410793A CN 202011224207 A CN202011224207 A CN 202011224207A CN 112410793 A CN112410793 A CN 112410793A
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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
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- 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
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- 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
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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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- 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 discloses an alkaline etching solution extraction electrolysis regeneration and copper recovery method, which comprises the following steps: the method comprises the following steps of guiding alkaline etching solution on a production line into an extraction tank, simultaneously quantitatively adding a copper extractant added with a catalyst into the extraction tank, arranging a condensation pipe in the extraction tank, dividing the extraction tank into two cavities with a partition plate in a volume ratio of 1:3, wherein a stirrer is arranged in a small cavity, and along with the continuous addition of the etching solution and the extractant from the bottom of the extraction tank, an oil-water mixture in the small cavity overflows into a large cavity to form a copper-containing oil phase and a copper-removing stock solution water phase. The invention leads the oil phase at the top in the big cavity of the extraction tank to slowly overflow from the overflow port to the back extraction tank beside the extraction tank, and the liquid phase formed by back extraction with sulfuric acid solution is copper sulfate solution which directly enters the electrolytic tank for electrolytic deposition of copper, and the temperature of the extraction tank is controlled by design, and the efficiency of extracting and electrolytically recovering copper is improved by the design of the two cavities of the extraction tank.
Description
Technical Field
The invention relates to the technical field of etching solution recovery, in particular to an alkaline etching solution extraction electrolysis regeneration and copper recovery method.
Background
At present, PCB production forms a large-scale industry in China, the annual output reaches 2 hundred million m2, the PCB production generates a large amount of etching solution, the PCB etching solution mainly comprises alkaline etching solution and acidic etching solution, the total copper content of the etching waste solution is about 5 million tons every year, the etching solution has the characteristics of multiple types, high toxicity, strong corrosivity and the like, belongs to a national class of hazardous waste, the alkaline etching waste solution contains copper-ammonia complex, ammonium chloride and ammonia water, the copper content can reach 120 plus 170g/L, if the etching waste solution is directly discharged, serious harm can be brought to the environment, in the production of printed boards, the etching waste solution needs to be recycled, the resources are fully utilized, the cost is reduced, the pollutant discharge is reduced, extremely serious damage can be caused to the ecology, even the life safety of people is seriously threatened, if the large amount of waste solution cannot be effectively recycled, the pollution of a large amount of water resources can be caused, and the main method for recycling the etching solution at present is the method for extracting Etc.;
the prior art has the following defects: in the existing alkaline etching solution recovery method, the reaction rate is low, and the separation speed of different substances generated by the reaction is low, so that the recovery efficiency is low, the recovery and the use of the alkaline etching solution are greatly influenced, and certain limitations are realized.
Disclosure of Invention
The invention aims to provide a method for extracting, electrolyzing and regenerating alkaline etching solution and recovering copper, which aims to overcome the defects in the prior art.
In order to achieve the above purpose, the invention provides the following technical scheme: an alkaline etching solution extraction electrolysis regeneration and copper recovery method comprises the following steps:
firstly, arranging a condensation pipe in an extraction tank, dividing the extraction tank into a large cavity and a small cavity by using a partition plate, arranging a stirrer in the small cavity, quantitatively guiding alkaline etching solution on a production line into the extraction tank from the bottom of the small cavity through a pump, a pipeline and a flowmeter, quantitatively adding a copper extracting agent added with a catalyst into the extraction tank, starting the stirrer to stir at a high speed, starting the condensation pipe to cool liquid in the extraction tank, continuously adding the etching solution and the extracting agent into the small cavity in a stirring state along with the etching solution and the extracting agent from the bottom of the extraction tank, overflowing an oil-water mixture in the small cavity into the large cavity, and carrying out a heavy separation reaction on the oil-water mixture to form a copper-containing oil phase with a clear interface and a copper-removed stock solution water phase;
step two, arranging an oil phase overflow port on one side of the large cavity of the extraction tank, which is far away from the small cavity, arranging a liquid phase outlet at the bottom of the large cavity, slowly injecting water into the large cavity from the bottom of the large cavity, so that the oil phase at the top in the extraction tank slowly overflows to a back extraction tank beside the extraction tank from the oil phase overflow port, stopping injecting the water into the extraction tank after the copper-containing oil phase completely overflows, and leading out the residual copper-removed stock solution water phase in the extraction tank from the liquid phase outlet;
step three, filtering the water phase of the copper-removing stock solution led out from the extraction tank in the step two through a filter vat, adding a small amount of ammonia water and ammonium chloride, returning to an etching line for etching after reaching the standard of an etching sub-solution, thereby realizing a copper-extracting recycling system of the alkaline etching solution;
adding a 15-25% sulfuric acid solution into a stripping tank, standing for 1.5-2h, performing stripping on the copper-containing oil phase to form a new oil phase and a copper-containing electro-deposition liquid, namely a copper sulfate solution, forming an oil phase overflow port on one side of the stripping tank, slowly injecting water from the bottom of the stripping tank, discharging the useless oil phase from the oil phase overflow port into an oil collecting tank for collection, cleaning, returning the oil phase to the extraction tank for extraction, and stopping injecting water after the oil phase in the stripping tank is completely discharged;
and step five, draining the residual copper-containing electrolyte in the stripping tank into an electrolytic tank, carrying out electrolytic deposition on copper, standing for 50-100min, slowly discharging the electrolyte after copper extraction after the solution in the electrolytic tank is completely precipitated, and recovering copper-containing solids after the discharge is finished, and extracting the copper.
Preferably, in the first step, the temperature of the solution in the extraction tank is controlled at 20 ℃ by using a condensation pipe.
Preferably, the volume ratio of the small cavity to the large cavity in the extraction tank is 1: 3.
Preferably, the catalyst added in the extraction reaction in the first step is one or more of solutions of palladium salt, ruthenium salt, nickel salt and cobalt salt.
Preferably, the inside of filter vat is filled with two cotton sandwich layers and an activated carbon layer, and the activated carbon layer is pressed from both sides between two cotton sandwich layers.
Preferably, the electrolyte discharged in the fifth step after copper extraction is filtered by a filter vat, cleaned and recycled from a new stripping tank.
In the technical scheme, the invention provides the following technical effects and advantages:
1. according to the invention, the upper part of one side of the large cavity far away from the small cavity is provided with the oil phase overflow port, the lower part of the side is provided with the liquid phase outlet, so that the copper-containing oil phase at the top in the large cavity of the extraction tank slowly overflows into the back extraction tank from the oil phase overflow port, the oil phase formed after the back extraction work is carried out by cleaning with 15% -25% sulfuric acid solution and then returns to the extraction tank for extraction work, and the liquid phase formed after the back extraction work is copper sulfate solution and directly enters the electrolytic tank for electrolytic deposition of copper.
Drawings
In order to more clearly illustrate the embodiments of the present application or technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings can be obtained by those skilled in the art according to the drawings.
FIG. 1 is a diagram of an apparatus used in the present invention.
Description of reference numerals:
1. an extraction tank; 11. a condenser tube; 12. a stirrer; 2. a stripping tank; 3. an electrolytic cell; 4. an oil collecting tank; 5. and (7) a filter barrel.
Detailed Description
In order to make the technical solutions of the present invention better understood, those skilled in the art will now describe the present invention in further detail with reference to the accompanying drawings.
The invention provides a method for extracting, electrolyzing and regenerating alkaline etching solution and recovering copper, which comprises the following steps:
firstly, arranging a condensation pipe 11 in an extraction tank 1, dividing the extraction tank 1 into a large cavity and a small cavity by using a partition plate, arranging a stirrer 12 in the small cavity, quantitatively draining alkaline etching solution on a production line from the bottom of the small cavity into the extraction tank 1 through a pump, a pipeline and a flowmeter, quantitatively adding a copper extractant added with a catalyst into the extraction tank 1, starting the stirrer 12 to stir at a high speed, starting the condensation pipe 11 to cool liquid in the extraction tank 1, continuously adding the etching solution and the extractant into the small cavity in a stirring state from the bottom of the extraction tank 1, overflowing an oil-water mixture in the small cavity into the large cavity, and carrying out a redistribution reaction on the oil-water mixture to form a copper-containing oil phase and a copper-removed stock solution water phase with clear interfaces;
step two, arranging an oil phase overflow port on one side of the large cavity of the extraction tank 1, which is far away from the small cavity, arranging a liquid phase outlet at the bottom of the large cavity, slowly injecting water into the large cavity from the bottom of the large cavity, so that the oil phase at the top in the extraction tank 1 slowly overflows from the oil phase overflow port to a back extraction tank 2 beside the extraction tank 1, stopping injecting water into the extraction tank 1 after the copper-containing oil phase completely overflows, and leading out the residual copper-removed stock solution water phase in the extraction tank 1 from the liquid phase outlet;
step three, filtering the copper-removed stock solution water phase led out from the extraction tank 1 in the step two through a filter vat 5, adding a small amount of ammonia water and ammonium chloride, returning to an etching line for etching after reaching the standard of an etching sub-solution, thereby realizing a system for recycling the copper extracted from the alkaline etching solution;
adding a 15-25% sulfuric acid solution into the stripping tank 2, standing for 1.5-2h, performing stripping on the copper-containing oil phase to form a new oil phase and a copper-containing electro-deposition liquid, namely a copper sulfate solution, in the solution in the stripping tank 2, arranging an oil phase overflow port on one side of the stripping tank 2, slowly injecting water from the bottom of the stripping tank 2, discharging the useless oil phase from the oil phase overflow port into an oil collecting tank 4 for collection, cleaning, returning to the extraction tank 1 for extraction, and stopping injecting water after the oil phase in the stripping tank 2 is completely discharged;
draining the residual copper-containing electrolyte in the stripping tank 2 into an electrolytic tank 3, performing electrolytic deposition on copper, standing for 50-100min, slowly discharging the electrolyte after copper extraction after the solution in the electrolytic tank 3 is completely precipitated, recovering copper-containing solids after the discharge is finished, and extracting copper;
further, in the above technical scheme, in the first step, the temperature of the solution in the extraction tank 1 is controlled at 20 ℃ by using the condensation pipe 11;
further, in the above technical scheme, the volume ratio of the small cavity to the large cavity in the extraction tank 1 is 1: 3;
further, in the above technical solution, the catalyst added in the extraction reaction in the first step is one or more of solutions of palladium salt, ruthenium salt, nickel salt and cobalt salt;
further, in the above technical scheme, two cotton core layers and an activated carbon layer are filled in the filtering barrel 5, and the activated carbon layer is sandwiched between the two cotton core layers;
further, in the above technical solution, the electrolyte discharged in the step five after copper extraction is filtered in the filter vat 5, cleaned, and then recycled from the newly-placed stripping tank 2;
the implementation mode is specifically as follows: guiding alkaline etching solution on a production line into an extraction tank 1, simultaneously quantitatively adding a copper extractant added with a catalyst into the extraction tank 1, arranging a condensation pipe in the extraction tank 1, dividing the extraction tank into two cavities with a partition plate in a volume ratio of 1:3, wherein a small cavity is provided with a stirrer 12, starting the stirrer 12 and then stirring at a high speed, controlling the temperature of the extraction tank at 20 ℃ by using the condensation pipe 11, continuously adding the etching solution and the extractant into the small cavity under stirring from the bottom of the extraction tank 1, overflowing an oil-water mixture in the small cavity into a large cavity, carrying out a re-separation reaction on the oil-water mixture to form a copper-containing oil phase with a clear interface and a copper-removed raw liquid water phase, arranging an oil phase overflow port at the upper part of one side of the large cavity far away from the small cavity, arranging a liquid phase outlet at the lower part, and slowly overflowing the copper-containing oil phase at the top in the large cavity of the extraction tank 1 from the, the oil phase formed after the back extraction work is carried out by using 15 to 25 percent sulfuric acid solution is cleaned and then returned to the extraction tank 1 for extraction work, the liquid phase formed after the back extraction is copper sulfate solution which directly enters the electrolytic bath 3 for electrolytic deposition of copper, the electrolyte after copper extraction can be returned to the back extraction bath 2 for back extraction, the copper-removed raw water phase reaches the standard of etching liquid after being supplemented with relevant materials for etching and returns to the etching line for etching, thereby realizing a system for recycling the copper extracted from the alkaline etching solution, and by designing the two cavities of the extraction tank 1, the condensing pipe 11 is used for controlling the liquid in the extraction tank 1 at low temperature, so that the oil phase generated by extraction can effectively and quickly float, thereby improving the separation speed, thereby greatly improving the treatment efficiency of extraction electrolysis regeneration and copper recovery and saving a large amount of treatment cost.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are illustrative in nature and should not be construed as limiting the scope of the invention.
Claims (6)
1. The method for extracting, electrolyzing and regenerating the alkaline etching solution and recovering the copper is characterized by comprising the following steps of:
step one, arranging a condensation pipe (11) in an extraction tank (1), dividing the extraction tank (1) into a large cavity and a small cavity by utilizing a partition plate, arranging a stirrer (12) in the small cavity, quantitatively draining alkaline etching solution on a production line from the bottom of the small cavity into the extraction tank (1) through a pump, a pipeline and a flowmeter, simultaneously quantitatively adding a copper extractant added with a catalyst into the extraction tank (1), starting the stirrer (12) to stir at a high speed, starting the condensation pipe (11) to cool liquid in the extraction tank (1), continuously adding the etching solution and the extractant into the small cavity in a stirring state from the bottom of the extraction tank (1), overflowing an oil-water mixture in the small cavity into the large cavity, and carrying out a redistribution reaction through an oil-water mixed solution to form a copper-containing oil phase and a decoppered raw solution water phase with clear interfaces;
step two, arranging an oil phase overflow port on one side of the large cavity of the extraction tank (1), which is far away from the small cavity, arranging a liquid phase outlet at the bottom of the large cavity, slowly injecting water into the large cavity from the bottom of the large cavity, so that the oil phase at the top in the extraction tank (1) slowly overflows into the back extraction tank (2) beside the extraction tank (1) from the oil phase overflow port, stopping injecting water into the extraction tank (1) after the copper-containing oil phase completely overflows, and leading out the residual copper-removed stock solution water phase in the extraction tank (1) from the liquid phase outlet;
step three, filtering the copper-removed stock solution water phase led out from the extraction tank (1) in the step two through a filter barrel (5), adding a small amount of ammonia water and ammonium chloride, returning to an etching line for etching after reaching the standard of an etching sub-solution, thereby realizing a copper-extraction recycling system of the alkaline etching solution;
adding 15% -25% sulfuric acid solution into the back extraction tank (2), standing for 1.5-2h, performing back extraction on the copper-containing oil phase to enable the solution in the back extraction tank (2) to form a new oil phase and copper-containing electro-deposition liquid, namely copper sulfate solution, arranging an oil phase overflow port on one side of the back extraction tank (2), slowly injecting water from the bottom of the back extraction tank (2), discharging useless oil phase from the oil phase overflow port into the oil receiving tank (4) for collection, cleaning, returning the oil phase to the extraction tank (1) for extraction, and stopping water injection after the oil phase in the back extraction tank (2) is completely discharged;
and fifthly, draining the residual copper-containing electro-deposition liquid in the back extraction tank (2) into an electrolytic tank (3), carrying out electrolytic deposition on copper, standing for 50-100min, slowly discharging the electrolyte after copper extraction after the solution in the electrolytic tank (3) is completely precipitated, recovering the copper-containing solid after the discharge is finished, and extracting the copper.
2. The method of claim 1, wherein the alkaline etching solution is extracted, electrolyzed, regenerated and recycled, and the method comprises the following steps: in the first step, the temperature of the solution in the extraction tank (1) is controlled at 20 ℃ by using a condensation pipe (11).
3. The method of claim 1, wherein the alkaline etching solution is extracted, electrolyzed, regenerated and recycled, and the method comprises the following steps: the volume ratio of the small cavity to the large cavity in the extraction tank (1) is 1: 3.
4. The method of claim 1, wherein the alkaline etching solution is extracted, electrolyzed, regenerated and recycled, and the method comprises the following steps: and the catalyst added in the extraction reaction in the first step is one or more of solutions of palladium salt, ruthenium salt, nickel salt and cobalt salt.
5. The method of claim 1, wherein the alkaline etching solution is extracted, electrolyzed, regenerated and recycled, and the method comprises the following steps: two cotton core layers and an activated carbon layer are filled in the filter barrel (5), and the activated carbon layer is sandwiched between the two cotton core layers.
6. The method of claim 1, wherein the alkaline etching solution is extracted, electrolyzed, regenerated and recycled, and the method comprises the following steps: and filtering the electrolyte discharged in the step five after copper extraction in a filter barrel (5), cleaning, and recycling the electrolyte from the newly-thrown stripping tank (2).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011224207.9A CN112410793A (en) | 2020-11-05 | 2020-11-05 | Alkaline etching solution extraction electrolysis regeneration and copper recovery method |
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| CN202011224207.9A CN112410793A (en) | 2020-11-05 | 2020-11-05 | Alkaline etching solution extraction electrolysis regeneration and copper recovery method |
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| CN112410793A true CN112410793A (en) | 2021-02-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113089023A (en) * | 2021-03-22 | 2021-07-09 | 浙江中金格派锂电产业股份有限公司 | Method and device for purifying electrodeposited cobalt solution |
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2020
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113089023A (en) * | 2021-03-22 | 2021-07-09 | 浙江中金格派锂电产业股份有限公司 | Method and device for purifying electrodeposited cobalt solution |
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