CN216947238U - High-efficient electrodeposition copper recovery system of acid etching solution - Google Patents
High-efficient electrodeposition copper recovery system of acid etching solution Download PDFInfo
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Abstract
The utility model provides a high-efficiency electrodeposited copper recovery system for an acidic etching solution, which belongs to the technical field of acidic waste liquid treatment in PCB (printed circuit board) production, and comprises an etching machine, an etching machine waste liquid discharge pump, a waste liquid collection device, an electrolytic cell waste liquid addition pump, an electrolytic cell component, a circulating pump, a regenerated liquid discharge pump, a regenerated liquid storage barrel, a regenerated liquid recycling pump, an additive storage barrel, an additive metering pump and a specific gravity controller, wherein an inlet of the specific gravity controller is communicated with an outlet of the circulating pump, an outlet of the electrolytic cell waste liquid addition pump and an outlet of the additive metering pump; when the specific gravity is higher than the control point, the electrolyte tank waste liquid adding pump and the additive metering pump are stopped at the same time, and the additive in the electrolyte tank is ensured to be maintained at a certain content.
Description
Technical Field
The utility model belongs to the technical field of treatment of acidic waste liquid in circuit board production in the PCB industry, and particularly relates to a high-efficiency electrodeposited copper recovery system for acidic etching liquid.
Background
The production and manufacturing processes of the circuit board use an acidic etching liquid which can rapidly etch copper foil to generate a designed circuit, the main components of the current mainstream acidic etching liquid comprise copper chloride, hydrochloric acid and ammonium chloride, and redundant copper foil is dissolved in the solution by means of the oxidizability of divalent copper ions. In the process, a certain amount of monovalent copper ions are generated in the solution, the content of the monovalent copper ions is reduced by adding an oxidizing agent (such as hydrogen peroxide, sodium chlorate, chlorine and the like), and redundant etching liquid is discharged, wherein the content of the monovalent copper ions is more than 9%, the content of the hydrochloric acid is more than 3%, and the content of ammonia nitrogen is more than 0.3%.
Such a waste stream has a high economic value and can be recycled either by electrochemical means or by chemical separation. Different reaction devices are designed in Chinese patents CN102730742B, CN102491402B, CN208980341U and CN113233494A, and refined copper oxide is obtained by controlling and adding different chemical reagents and reaction conditions; chinese patent CN112080748A proposes a process for preparing copper oxalate by extraction and back extraction of oxalate-containing ions, and the copper oxalate is roasted at high temperature to obtain copper oxide powder; chinese patent CN105314668B proposes a chemical process for recovering basic copper carbonate from acidic etching waste liquid; chinese patent CN102583819B proposes an integrated treatment method for preparing copper oxide by adding alkali into acidic etching waste liquid, and then removing ammonia nitrogen by sodium hypochlorite and removing metal by PAC and PAM precipitation in turn. The copper in the acid etching solution is made into different types of copper products by adopting more chemical methods, so that higher added values are generated, but a large amount of chemical medicines are consumed, and meanwhile, the process control is more complex, more used equipment is provided, and the occupied area is larger.
By an electrochemical (electrodeposition) method, the high conductivity of the etching waste liquid is utilized, copper ions in the solution are converted into elemental copper through cathode discharge, and chlorine is generated at the anode. The high content (no less than 99%) of copper (product) produced can be obtained with a large yield, and chlorine gas can be used as an oxidizing agent for regenerating etching waste liquid. The etching waste liquid for extracting part of copper can be recycled by supplementing a small amount of effective components, the whole process flow is simple, the consumption of chemical raw materials is low, the occupied area is small, the investment is low, and the method has great advantages compared with a chemical process treatment method.
Disclosure of Invention
The utility model designs an efficient electrodeposited copper recovery system for acidic etching solution, which can realize output maximization and complete automatic operation, and comprises the following contents:
the utility model discloses a high-efficiency acid etching solution electrodeposited copper recovery system, which comprises an etching machine, an etching machine waste liquid discharge pump, a waste liquid collection device, an electrolytic bath waste liquid addition pump, an electrolytic bath component, a circulating pump, a regenerated liquid discharge pump, a regenerated liquid storage barrel, a regenerated liquid reuse pump, an additive storage barrel and an additive metering pump, wherein an outlet of the etching machine is communicated with an inlet of the etching machine waste liquid discharge pump, an outlet of the etching machine waste liquid discharge pump is communicated with an inlet of the waste liquid collection device, an outlet of the waste liquid collection device is communicated with an inlet of the electrolytic bath waste liquid addition pump, an outlet of the electrolytic bath waste liquid addition pump is communicated with an inlet of the electrolytic bath component, an outlet of the electrolytic bath component is communicated with an inlet of the regenerated liquid discharge pump, an outlet of the regenerated liquid discharge pump is communicated with an inlet of the regenerated liquid storage barrel, and an outlet of the regenerated liquid storage barrel is communicated with an inlet of the regenerated liquid reuse pump, the device is characterized by also comprising a specific gravity controller, wherein the inlet of the specific gravity controller is communicated with the outlet of the circulating pump, the outlet of the electrolytic cell waste liquid adding pump and the outlet of the additive metering pump.
Preferably, the electrolytic bath component in the acid etching solution high-efficiency electrodeposited copper recovery system consists of at least one electrolytic bath.
Preferably, the electrolytic tank in the acid etching solution high-efficiency electro-deposited copper recovery system comprises an anode, a cathode, a ballast, a high liquid level meter and a low liquid level meter, wherein the anode is composed of continuously spaced anode materials of the electrolytic tank, the cathode is composed of cathode materials of the electrolytic tank, the anode materials and the cathode materials of the electrolytic tank are connected with the ballast, and the high liquid level meter and the low liquid level meter are communicated with an inlet of the regeneration solution discharge pump.
The utility model relates to a high-efficiency electrodeposited copper recovery system for acidic etching solution, which has the following beneficial effects:
the efficient electrodeposited copper recovery system for the acidic etching solution also comprises a specific gravity controller, wherein an inlet of the specific gravity controller is communicated with an outlet of the circulating pump, an outlet of the electrolytic cell waste solution adding pump and an outlet of the additive metering pump; when the specific gravity is higher than the control point, the electrolyte tank waste liquid adding pump and the additive metering pump are stopped simultaneously, and the additive in the electrolyte tank is ensured to be maintained at a certain content.
Drawings
FIG. 1 is a schematic diagram of the process flow of the electrodeposition process of etching waste liquid with high automatic control designed by the utility model;
FIG. 2 is a schematic plan view of the electrolyzer design;
FIG. 3 is a graph of time versus copper yield.
In the figure: 1-etching machine; 2-a pump for discharging the waste liquid of the etching machine; 3-a waste liquid collecting device; 4-electrolytic cell waste liquid adding pump; 5-additive storage barrel; 6-additive metering pump; 7-cell assembly, 701-cell anode material, 702-cell cathode material; 8-a circulating pump; 9-a specific gravity controller; 10-a ballast; 11-high level gauge; 12-low level gauge; 13-regeneration liquid discharge pump; 14-regenerated liquid storage barrel; 15-regenerated liquid recycling pump.
Detailed Description
As shown in figure 1, the high-efficiency acid etching solution electrodeposited copper recovery system comprises an etching machine 1, an etching machine waste liquid discharge pump 2, a waste liquid collection device 3, an electrolytic bath waste liquid addition pump 4, an electrolytic bath component 7, a circulating pump 8, a regeneration liquid discharge pump 13, a regeneration liquid storage barrel 14, a regeneration liquid recycling pump 15, an additive storage barrel 5 and an additive metering pump 6, wherein an outlet of the etching machine 1 is communicated with an inlet of the etching machine waste liquid discharge pump 2, an outlet of the etching machine waste liquid discharge pump 2 is communicated with an inlet of the waste liquid collection device 3, an outlet of the waste liquid collection device 3 is communicated with an inlet of the electrolytic bath waste liquid addition pump 4, an outlet of the electrolytic bath waste liquid addition pump 4 is communicated with an inlet of the electrolytic bath component 7, an outlet of the electrolytic bath component 7 is communicated with an inlet of the regeneration liquid discharge pump 13, an outlet of the regeneration liquid discharge pump 13 is communicated with an inlet of the regeneration liquid storage barrel 14, the technical points are that the device also comprises a specific gravity controller 9, wherein the inlet of the specific gravity controller 9 is communicated with the outlet of the circulating pump 8, the outlet of the electrolytic cell waste liquid adding pump 4 and the outlet of the additive metering pump 6, the specific gravity controller can continuously detect the specific gravity of the etching waste liquid in the electrolytic cell assembly, and when the specific gravity is lower than a certain control point, the electrolytic cell waste liquid adding pump and the additive metering pump are simultaneously started to control the liquid flow, the local non-uniformity of the concentration of copper ions is avoided; when the specific gravity is higher than the control point, the electrolyte tank waste liquid adding pump and the additive metering pump are stopped at the same time, and the additive in the electrolyte tank is ensured to be maintained at a certain content.
Preferably, the electrolytic bath component 7 in the acid etching solution high-efficiency electrodeposited copper recovery system of the utility model consists of at least one electrolytic bath.
Preferably, the electrolytic cell in the high-efficiency acid etching solution electro-deposited copper recovery system of the utility model comprises an anode, a cathode, a ballast 10, a high liquid level meter 11 and a low liquid level meter 12, wherein the anode is composed of continuously spaced anode material 701 of the electrolytic cell, the cathode is composed of cathode material 702 of the electrolytic cell, the anode material 701 and the cathode material 702 of the electrolytic cell are connected with the ballast 10, and the high liquid level meter 11 and the low liquid level meter 12 are communicated with the inlet of the regeneration solution discharge pump 13. The electrolytic cell is simultaneously provided with a high liquid level meter 11 and a low liquid level meter 12 for control, when the liquid level of the electrolytic cell continuously adds waste liquid to reach a high liquid level, a regenerated liquid discharge pump 13 is started to discharge etching liquid to a regenerated liquid storage barrel 14; when the liquid level of the electrolytic bath is continuously discharged to reach a low liquid level, the regeneration liquid discharge pump 13 is stopped. The discharged electrolyte is returned to the etching machine 1 for recycling by adding effective components.
The method adopts an electrochemical method to treat the acid etching waste liquid, can quickly obtain the metal copper, and simultaneously can recycle the acid etching waste liquid. By continuously detecting the operation parameters, accurately controlling the parameters such as copper ion concentration, liquid flow rate, current, additive content and the like in the electrolysis process, continuously operating for 5-12 days, obtaining a copper product with the purity higher than 98.5 percent, and having high copper yield. All main parameters are measured on line through the instrument, and the equipment is controlled to run through an automatic program, so that the risk of manual operation is reduced, and the labor intensity is low.
During the process of continuously replenishing the etching waste liquid, the content of the additive in the electrolytic bath is preferably maintained between 0.1 and 0.5 percent. The main components of the electrolysis additive are leveling agent and surfactant, wherein the leveling agent is polyethyleneimine alkyl compound, the use concentration range is 3-100mg/L, and the surfactant is sodium dodecyl sulfate polyethyleneimine alkyl compound 50-150 mg/L. Preferably, the leveling agent is a polyethyleneimine alkyl compound, the use concentration range is 20-50mg/L, and the surfactant is a sodium dodecyl sulfate polyethyleneimine alkyl compound of 80-120 mg/L;
preferably, when the current density of each cathode is 200-400A/m2, the copper ion concentration is a certain value in the range of 40-60g/L, the specific gravity is a certain value in the range of 1.16-1.18g/L, and when the specific gravity is lower than a certain control point, the waste liquid adding pump and the additive metering pump are started at the same time, the waste liquid adding flow is controlled, and the local overhigh copper ion concentration is avoided; when the specific gravity is higher than the control point, the waste liquid adding pump and the additive metering pump are stopped at the same time, so that the additive in the electrolytic cell is maintained at a certain content, and high electrolytic efficiency can be realized.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the specific embodiments of the present invention and the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the utility model, and not restrictive of the full scope of the utility model. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The following detailed description of the present invention is provided by 2 examples, 2 comparative examples and the accompanying drawings, the description of the examples only represents one way of the operation of the present invention, and the present invention is protected by using different types and specifications of devices and equipments without changing the basic principle.
Example 1:
the acid etching solution high-efficiency electrodeposited copper recovery system operates as follows:
the etching machine 1 etches redundant copper foil of the circuit board through bivalent copper ions in the acidic etching solution to generate monovalent copper ions, when the concentration of the monovalent copper ions in the etching solution exceeds 5g/L, the etching capacity of the etching solution is rapidly reduced, in order to recover the etching capacity, low-copper etching solution and oxidant are continuously supplemented, redundant etching waste liquid is overflowed and discharged, and the redundant etching waste liquid enters a waste liquid collecting device 3 through an etching machine waste liquid discharge pump 2;
a plurality of continuously spaced cathode and anode materials are arranged in the electrolytic cell component 7, wherein the electrolytic cell anode material 701 adopts titanium as a base material, the surface of the anode material is coated with ruthenium or iridium ruthenium and other coatings, high conductivity is kept, and chloride ions in the etching solution are oxidized to generate chlorine gas after losing electrons; the cathode material 702 of the electrolytic bath is a titanium material, and copper ions in the etching waste liquid are converted into a copper simple substance through electrons; in order to prevent the copper simple substance generated by the cathode material from being oxidized by the chlorine generated by the anode, the anode material of the electrolytic cell is surrounded by the cation membrane material, and the chlorine overflows from the solution and is treated by the gas collecting device.
The electrolysis trough passes through circulating pump 8 with the solution misce bene, for guaranteeing whole electrolysis trough solution copper ion misce bene, the flow control is in 2.2 times of electrolysis trough solution total volume every hour of circulating pump, proportion controller sets for 1.18, copper ion is about 45g/L-55g/L among the electrolysis process, cathode material constantly separates out the elementary substance copper, copper ion concentration constantly reduces in the electrolysis trough etching solution, the proportion reduces gradually, begin to start electrolysis trough waste liquid adding pump 4 and regeneration liquid discharge pump 13, cause copper ion concentration local inhomogeneous for avoiding the waste liquid to add the excess, electrolysis trough waste liquid adding pump is controlled at 4.1% of electrolysis trough solution total volume every hour. When the addition amount of the waste liquid exceeds the control value of the high liquid level meter 11, stopping the waste liquid addition pump; after the waste liquid adding pump is stopped, because the electrolytic cell waste liquid is discharged through the regeneration liquid discharge pump and is continuously reduced, when the volume of the electrolytic cell waste liquid reaches the low liquid level meter 12, the regeneration liquid discharge pump is stopped, and the discharge flow of the regeneration liquid discharge pump is controlled to be 3.5 percent of the total volume of the electrolytic cell solution.
In the process of continuously replenishing the waste liquor, continuously replenishing the electrolytic additive through an additive metering pump 6 according to the proportion of 0.2 percent of the volume of the waste liquor, wherein the additive comprises a polyethyleneimine alkyl compound, the preparation concentration is 20mg/L, and the preparation concentration of the sodium dodecyl sulfate polyethyleneimine alkyl compound is 80 mg/L. The additive is continuously supplemented, so that the content stability in the continuous electrolysis process is ensured;
in the electrolytic process, the concentration of copper ions is controlled to be 45-55 g/L, and the current density of each electrode is controlled to be 350A/m2；
In order to obtain the copper product which accords with the actual industrial production, the electrolytic production is continuously carried out for 5 days.
Comparative example 1:
to further illustrate the advantages of the novel process proposed by the present patent, comparative tests were conducted using the above described electrolysis apparatus using conventional electrolysis processes.
Etching waste liquid enters a waste liquid collecting device through a waste liquid discharge pump, an electrolytic tank uniformly mixes solution through a circulating pump 8, in order to ensure that copper ions in the solution of the whole electrolytic tank are uniformly mixed, the flow of the circulating pump per hour is controlled to be 2.2 times of the total volume of the solution of the electrolytic tank, elemental copper is continuously separated out from a cathode material, the concentration of copper ions in the etching liquid of the electrolytic tank is continuously reduced, when the concentration of the copper ions is reduced to 45g/L, one third of the regeneration liquid is manually controlled to be discharged through a regeneration liquid discharge pump, and then one third of the etching waste liquid is manually added;
when the etching waste liquid is supplemented every time, according to the proportion of 0.2% of the volume of the waste liquid, the electrolytic additive is diluted by tap water by 30 times and then added into an electrolytic tank, wherein the additive component comprises a polyethyleneimine alkyl compound, the preparation concentration is 20mg/L, and the preparation concentration of the sodium dodecyl sulfate polyethyleneimine alkyl compound is 80 mg/L. The current density of each electrode is controlled at 350A/m2；
In order to obtain the copper product which accords with the actual industrial production, the electrolytic production is continuously carried out for 5 days.
Example 2:
etching waste liquid passes through waste liquid discharge pump and gets into waste liquid collection device, the electrolysis trough passes through circulating pump 8 with solution misce bene, for guaranteeing whole electrolysis trough solution copper ion misce bene, the every hour flow control of circulating pump is 2.5 times at electrolysis trough solution total volume, proportion controller sets for 1.17, copper ion is at about 35g/L-45g/L among the electrolysis process, cathode material constantly precipitates elementary substance copper, copper is from the concentration and constantly reduces in the electrolysis trough etching solution, the proportion reduces gradually, begin to start electrolysis trough waste liquid and add pump 4 and regeneration liquid discharge pump 13, it is local inhomogeneous to arouse copper ion concentration for avoiding the waste liquid to add the excess, electrolysis trough waste liquid adds the pump and adds the volume and controls 3.5 at electrolysis trough total volume every hour. When the addition amount of the waste liquid exceeds the control value of the high liquid level meter 11, stopping the waste liquid addition pump; after the waste liquid adding pump is stopped, because the electrolytic cell waste liquid is discharged through the regeneration liquid discharge pump and is continuously reduced, when the volume of the electrolytic cell waste liquid reaches the low liquid level meter 12, the regeneration liquid discharge pump is stopped, and the discharge flow of the regeneration liquid discharge pump is controlled to be 3 percent of the total volume of the electrolytic cell solution.
In the process of continuously replenishing the waste liquor, continuously replenishing the electrolytic additive through an additive metering pump 6 according to the proportion of 0.18 percent of the volume of the waste liquor, wherein the additive comprises a polyethyleneimine alkyl compound, the preparation concentration is 30mg/L, and the preparation concentration of the sodium dodecyl sulfate polyethyleneimine alkyl compound is 100 mg/L. The stable content in the continuous electrolysis process is ensured by continuously adding additives;
in the electrolytic process, the concentration of copper ions is controlled to be 35g/L-45g/L, and the current density of each electrode is controlled to be 300A/m2；
In order to obtain the copper product which accords with the actual industrial production, the electrolytic production is continuously carried out for 5 days.
Comparative example 2:
to further illustrate the advantages of the novel process proposed by the present patent, comparative tests were conducted using the above described electrolysis apparatus using conventional electrolysis processes.
Etching waste liquid passes through waste liquid discharge pump entering waste liquid collection device, the electrolysis trough passes through circulating pump 8 with solution misce bene, for guaranteeing whole electrolysis trough solution copper ion misce bene, the every hour flow control of circulating pump is at 2.5 times of electrolysis trough solution total volume, elemental copper is constantly appeared to cathode material, copper is constantly reduced from concentration in the electrolysis trough etching solution, reduce to 35g/L when copper ion concentration, discharge third regeneration liquid through regeneration liquid discharge pump manual control, manual third etching waste liquid that adds again.
When the etching waste liquid is replenished every time, according to the proportion of 0.18 percent of the volume of the waste liquid, diluting an electrolysis additive by 30 times by using tap water, and adding the diluted electrolysis additive into an electrolytic bath, wherein the additive component comprises a polyethyleneimine alkyl compound, the preparation concentration is 30mg/L, and the preparation concentration of a sodium dodecyl sulfate polyethyleneimine alkyl compound is 100 mg/L;
the current density of each electrode is controlled to be 300A/m2；
In order to obtain the copper product which accords with the actual industrial production, the electrolytic production is continuously carried out for 5 days.
FIG. 3 shows the cumulative copper yield per day after 5 days of electrolytic production in example 1, comparative example 1, example 2 and comparative example 2. it can be seen from the table that the cumulative copper yield of example 1 is increased by 24.6% compared with comparative example 1 and the cumulative copper yield of example 2 is increased by 26.9% compared with comparative example 2 by the patented process of the utility model. The copper yield of all the embodiments is improved by more than 20%, and the operation mode shows that the process provided by the utility model avoids the discharge and addition operation processes of batch electrolysis waste liquid in a continuous electrodeposition mode; meanwhile, the process can avoid the continuous reduction of the proportion of the additive caused by the decomposition of the additive in the electrolytic process by continuously adding the electrolytic additive in a certain proportion in the electrolytic process, and ensure the uniform plating layer in the copper electrodeposition process.
The above description is only an example of the present invention and is not intended to limit the present invention. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (3)
1. An acid etching solution high-efficiency electrodeposited copper recovery system comprises an etching machine (1), an etching machine waste liquid discharge pump (2), a waste liquid collection device (3), an electrolytic bath waste liquid adding pump (4), an electrolytic bath component (7), a circulating pump (8), a regeneration liquid discharge pump (13), a regeneration liquid storage barrel (14), a regeneration liquid recycling pump (15), an additive storage barrel (5) and an additive metering pump (6), wherein an outlet of the etching machine (1) is communicated with an inlet of the etching machine waste liquid discharge pump (2), an outlet of the etching machine waste liquid discharge pump (2) is communicated with an inlet of the waste liquid collection device (3), an outlet of the waste liquid collection device (3) is communicated with an inlet of the electrolytic bath waste liquid adding pump (4), an outlet of the electrolytic bath waste liquid adding pump (4) is communicated with an inlet of the electrolytic bath component (7), an outlet of the electrolytic bath component (7) is communicated with an inlet of the regeneration liquid discharge pump (13), the export of regeneration liquid drainage pump (13) and the entry intercommunication that bucket (14) were stored to the regeneration liquid, the export that bucket (14) were stored to the regeneration liquid communicates with the entry of regeneration liquid retrieval and utilization pump (15), the export of regeneration liquid retrieval and utilization pump (15) with the entry intercommunication of etching machine, the export of electrolysis trough subassembly (7) and the entry intercommunication of circulating pump (8), the export that bucket (5) were stored to the additive communicates with the entry of additive measuring pump (6), the export of additive measuring pump (6) with the entry intercommunication of electrolysis trough subassembly (7), its characterized in that still includes specific gravity controller (9), the entry of specific gravity controller (9) and the export of circulating pump (8), the export of electrolysis trough waste liquid adding pump (4), the export of additive measuring pump (6) all communicate.
2. The acidic etchant high efficiency electrodeposited copper recovery system as claimed in claim 1 wherein said electrolytic cell assembly (7) is comprised of at least one electrolytic cell.
3. The acid etching solution high efficiency electrodeposited copper recovery system as claimed in claim 2 wherein said electrolytic cell comprises an anode comprised of continuously spaced electrolytic cell anode material (701), a cathode comprised of electrolytic cell cathode material (702), a ballast (10), a high level gauge (11) and a low level gauge (12), said electrolytic cell anode material (701) and electrolytic cell cathode material (702) are connected to ballast (10), said high level gauge (11) and low level gauge (12) are in communication with an inlet of said regenerant discharge pump (13).
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