CN115961331A - Method for recycling cathode copper from acidic etching waste liquid to replace phosphor copper balls - Google Patents
Method for recycling cathode copper from acidic etching waste liquid to replace phosphor copper balls Download PDFInfo
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- CN115961331A CN115961331A CN202211604912.0A CN202211604912A CN115961331A CN 115961331 A CN115961331 A CN 115961331A CN 202211604912 A CN202211604912 A CN 202211604912A CN 115961331 A CN115961331 A CN 115961331A
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Abstract
The invention discloses a method for recovering cathode copper from acidic etching waste liquid to replace phosphor copper balls, which comprises the following steps: electrolyzing the acidic etching waste liquid to obtain recovered cathode copper; the recovered cathode copper is sequentially subjected to alkali washing, acid washing, pure water washing and drying to obtain pretreated recovered cathode copper; putting the pretreated and recovered cathode copper into an electrolytic cell for electrochemical dissolution to obtain copper-rich electrolyte; and recycling the copper-rich electrolyte to an electroplating production line. This application retrieves negative pole copper through etching waste liquid electrolysis and purifies the preliminary treatment after, adopts the mode preparation rich copper electrolyte that the electrolysis trough electrochemistry dissolved, and rich copper electrolyte retrieval and utilization PCB electroplating production line to let retrieve negative pole copper and replace the phosphorus copper ball as the copper electroplating, prevent the inhomogeneous problem of current distribution, the loss of circuit board enterprise copper value that has significantly reduced simultaneously has reduced circuit board enterprise cost on the metal copper by a wide margin, has good economy.
Description
Technical Field
The invention relates to the technical field of recycling of acidic etching waste liquid, in particular to a method for recycling cathode copper from acidic etching waste liquid to replace phosphor copper balls.
Background
The PCB (printed circuit board) is a support body of electronic product components, is the most basic hardware carrier of the current information society, and the PCB industry is the pillar industry of the Chinese electronic information industry, and the growth rate of the PCB is the same as that of the electronic information industry. However, the production process for manufacturing the circuit pattern on the circuit board is still a reduction process, namely, the copper-clad plate is manufactured into the circuit pattern through the working procedures of cutting, film pasting, pattern transfer, developing, etching, film stripping and the like, and then the circuit board production is completed through the working procedures of pressing, drilling, copper electroplating, outer layer manufacturing and the like. The inner layer etching adopts an acid etching method, the oxidation-reduction potential and the copper ion concentration in the etching solution are kept in a certain area to maintain the etching rate, an oxidant and hydrochloric acid are continuously added in the etching process, meanwhile, the overflowing etching solution becomes etching waste liquid, the main components of the acid etching waste liquid are copper chloride and hydrochloric acid, the copper content is about 10%, according to statistics, the annual generation amount of the national PCB copper-containing waste liquid is more than million tons, namely the waste liquid contains more than 10 ten thousand tons, and on the other hand, the annual demand of the domestic PCB industry for copper electroplating on phosphor copper balls, copper oxide and copper sulfate is more than 10 ten thousand tons.
The graphic copper electroplating is one of the main processing technologies in the PCB manufacturing process, the copper is thickened to a certain degree through electroplating so as to meet the rated current load of each circuit, the copper electroplating mainly adopts a copper sulfate liquid medicine system at present, the copper ion source in the liquid medicine is the dissolution of a phosphorus copper ball anode or the supplement of copper oxide powder, the phosphorus copper ball and the copper oxide are deep-processed products of metal copper, the energy consumption is high in the production process, the environmental pollution is large, the product selling price is high, and the cost of copper-containing raw materials of circuit board enterprises is also high correspondingly. The demand of the PCB industry for the phosphor copper balls is large, according to statistics, the annual demand is more than 4 ten thousand tons, but the phosphor copper balls have more positive residues, and the problem of uneven current distribution is easy to occur along with the consumption of the phosphor copper balls.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for recovering cathode copper from acidic etching waste liquid to replace phosphor copper balls.
The invention discloses a method for recovering cathode copper from acidic etching waste liquid to replace phosphor copper balls, which comprises the following steps:
electrolyzing the acidic etching waste liquid to obtain recovered cathode copper;
the recovered cathode copper is sequentially subjected to alkali washing, acid washing, pure water washing and drying to obtain pretreated recovered cathode copper;
putting the pretreated and recovered cathode copper into an electrolytic cell for electrochemical dissolution to obtain copper-rich electrolyte;
and recycling the copper-rich electrolyte to an electroplating production line.
According to one embodiment of the invention, the method for pretreating and recovering cathode copper and placing the cathode copper into an anode chamber of an electrolytic cell for electrochemical dissolution to obtain a copper-rich electrolyte comprises the following substeps:
the pretreated and recovered cathode copper is put into an anode chamber of an electrolytic cell for electrochemical dissolution;
the overflow solution of the anode chamber is a copper-rich electrolyte.
According to one embodiment of the invention, the electrolytic cell further comprises a diaphragm and a cathode chamber, the diaphragm is arranged between the anode chamber and the cathode chamber, and the diaphragm is an anion heterogeneous ion exchange membrane.
According to one embodiment of the invention, a copper sulfate solution is provided in the anode compartment and a sulfuric acid solution is provided in the cathode compartment.
According to one embodiment of the invention, the recycling of the copper-rich electrolyte to the electroplating line comprises the following substeps:
recycling the copper-rich electrolyte to an electroplating production line;
the overflow solution of the electroplating production line is a copper-poor electrolyte;
the poor copper electrolyte is recycled to the anode chamber.
According to one embodiment of the present invention, the copper ion concentration of the solution in the plating line is 15 to 50g/L.
According to one embodiment of the invention, the electrolysis of the acidic etching waste liquid to obtain the recovered cathode copper comprises the following substeps:
adding quaternary ammonium salt electrolysis additive into the acidic etching waste liquid for electrolysis;
and stripping the recovered cathode copper from the cathode to obtain the recovered cathode copper.
According to one embodiment of the present invention, the polymeric quaternary ammonium salt electrolytic additive is polydienedimethylammonium chloride.
According to one embodiment of the present invention, the amount of the electrolytic additive of the polymeric quaternary ammonium salt is 0.01 to 0.05Kg/1000L.
According to an embodiment of the present invention, before the acidic etching waste liquid is electrolyzed to obtain the recovered cathode copper, the method further comprises the following steps:
and filtering the acidic etching waste liquid.
The beneficial effect of this application lies in: after the cathode copper is recovered by electrolyzing the etching waste liquid and subjected to purification pretreatment, the copper-rich electrolyte is prepared in a mode of electrochemical dissolution of an electrolytic bath, and the copper-rich electrolyte is recycled on a PCB (printed Circuit Board) electroplating production line, so that the recovered cathode copper replaces a phosphor copper ball as electroplated copper, the problem of uneven current distribution is prevented, the loss of copper value of a circuit board enterprise is greatly reduced, the cost of the circuit board enterprise on metal copper is greatly reduced, and the method has good economy.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a flow chart of the method for recovering cathode copper instead of phosphor copper balls from acidic waste etching solution in the example.
Detailed Description
In the following description, for purposes of explanation, numerous implementation details are set forth in order to provide a thorough understanding of the various embodiments of the present invention. It should be understood, however, that these implementation details are not to be interpreted as limiting the invention. That is, in some embodiments of the invention, such implementation details are not necessary. In addition, some conventional structures and components are shown in simplified schematic form in the drawings for the sake of simplicity.
It should be noted that all the directional indicators in the embodiments of the present invention, such as up, down, left, right, front, and back, 8230, are only used to explain the relative position relationship between the components, the motion situation, etc. in a specific posture as shown in the drawings, and if the specific posture is changed, the directional indicator is changed accordingly.
In addition, the descriptions related to the first, the second, etc. in the present invention are only used for description purposes, do not particularly refer to an order or sequence, and do not limit the present invention, but only distinguish components or operations described in the same technical terms, and are not understood to indicate or imply relative importance or implicitly indicate the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Referring to fig. 1, fig. 1 is a flow chart of a method for recovering cathode copper instead of phosphor copper balls from acidic waste etching solution in an embodiment. In this embodiment, a method for recovering cathode copper from acidic etching waste liquid to replace phosphor copper balls includes the following steps:
s1: filtering the acidic etching waste liquid.
S2: and electrolyzing the acidic etching waste liquid to obtain the recovered cathode copper.
S3: and (4) sequentially carrying out alkali washing, acid washing, pure water washing and drying on the recovered cathode copper to obtain the pretreated recovered cathode copper.
S4: and (4) putting the pretreated and recovered cathode copper into an electrolytic cell for electrochemical dissolution to obtain the copper-rich electrolyte.
S5: and recycling the copper-rich electrolyte to an electroplating production line.
Specifically, in step S1, the waste etching solution obtained by overflowing the etching line of the circuit board is collected, and is subjected to a filtering pretreatment, so as to filter out solid impurities carried in the etching solution, such as film residues and ink residues introduced by the circuit board. The copper content in the acidic etching waste liquid is 110-140g/L. By continuously adding the etching waste liquid into the electrolytic circulating tank and linking the current density of the electrolytic circulating tank, the copper ions in the electrolytic circulating tank are kept stable in a certain concentration range, so that the current density is relatively stable, the quality of the recovered electrolytic copper is stable, and a foundation is laid for the subsequent recovery of cathode copper to return to a circuit board electrolytic copper plating production line through a copper-rich electrolyte.
Specifically, step S2 includes the following substeps:
s21: adding quaternary ammonium salt electrolytic additive into the acidic etching waste liquid for electrolysis.
S22: and stripping the recovered cathode copper from the cathode to obtain the recovered cathode copper.
Preferably, in step S21, the acidic waste etching solution is continuously added into the electrolytic circulating tank, so that the copper ions of the solution in the electrolytic circulating tank are maintained at 40-60g/L; the overflow solution in the electrolytic circulation tank is a regenerated etching solution which can be recycled to a circuit board etching production line. In order to ensure that the surface of the recovered cathode copper required by the step S3 is smooth, the recovered cathode copper in the step S4 can be smoothly electrochemically dissolved, the current density of the electrolytic circulating tank is controlled to be 150A/square meter-200A/square meter, the anode of the electrolytic circulating tank is a titanium ruthenium-plated insoluble anode, and the cathode is a titanium cathode which is not corroded in a hydrochloric acid solution. The polymeric quaternary ammonium salt electrolytic additive is polydiene dimethyl ammonium chloride, the addition amount of the polymeric quaternary ammonium salt electrolytic additive is 0.01-0.05Kg/1000L, namely 0.01-0.05Kg of quaternary ammonium salt electrolytic additive is added into every 1000L of etching waste liquid, and the electrolysis efficiency is improved by adding the quaternary ammonium salt electrolytic additive. During electrolysis, copper ions are reduced into copper and deposited on the surface of the cathode to form recovered cathode copper. In step S22, when the thickness of the recovered cathode copper reaches 5-10 mm, the recovered cathode copper is stripped from the cathode.
Specifically, the alkali used in the step S3 for recovering the copper alkali washing process is 5-10% of sodium hydroxide solution with mass concentration, the washing temperature is 60-80 ℃, and the soaking and washing time is 30-60 minutes; the acid used in the acid washing process is sulfuric acid, and the pH value of acid washing liquid is 4-6 by adding the sulfuric acid; a pure water washing step for controlling the pH of the washing water after washing with pure water to 6-9; the content of chloride ions, sulfate radical anions and sodium ions in the washing water is less than 10ppm; the hot air drying temperature is 80-120 ℃. And conveying the washing water to a comprehensive sewage treatment station for treatment.
Specifically, step S4 includes the following substeps:
s41: the pretreated and recovered cathode copper is put into an anode chamber of an electrolytic cell for electrochemical dissolution;
s42: the overflow solution of the anode chamber is copper-rich electrolyte.
The electrolytic cell also comprises a diaphragm and a cathode chamber, wherein the diaphragm is arranged between the anode chamber and the cathode chamber, and the diaphragm is an anion heterogeneous ion exchange membrane so that copper ions cannot flow to the cathode chamber. Copper sulfate solution with copper ion concentration of 50-80g/L is arranged in the anode chamber, and sulfuric acid solution with mass concentration of 20-30% is arranged in the cathode chamber. The cathode of the electrolytic cell adopts a cathode copper starting sheet with the thickness of 2-4 mm, the current density is adjusted by the copper ion concentration of the anode area, the high current density is adjusted when the copper ion concentration is low, and the low current density is adjusted when the copper ion concentration is high. The addition mode of recovering cathode copper is continuous addition.
Specifically, step S5 includes the following substeps:
s51: and recycling the copper-rich electrolyte to an electroplating production line.
S52: the overflow solution of the electroplating production line is copper-poor electrolyte.
S53: the poor copper electrolyte is recycled to the anode chamber.
Preferably, the anode of the electroplating production line is an insoluble anode, the copper-rich electrolyte replaces a phosphorus copper ball to be reused in the electroplating production line, and the phosphorus copper ball is added into the electroplating production line at a certain speed, so that the concentration of copper ions in an electroplating solution tank is maintained at 15-50g/L, the electroplating solution overflowing from the electroplating tank is a copper-poor electrolyte, and the electroplating solution returns to the anode chamber of the step S41, and the copper-poor electrolyte is continuously added.
In order to further understand the contents, features and effects of the present invention, the following examples are illustrated:
example 1
Filtering the overflowing acidic etching waste liquid of the acidic etching line of a certain A circuit board factory, adding an electrolytic additive according to the proportion of 0.01Kg/1000L, and then adding an electrolytic circulating tank with the current density of 200A/square meter at a certain speed to ensure that the concentration of copper ions in the electrolytic circulating tank is maintained at 60g/L; taking out the cathode plate when the thickness of copper on the cathode plate is 5 mm, sequentially washing the cathode plate by tap water, soaking the cathode plate in liquid alkali with the mass concentration of 8% at the temperature of 60 ℃ for 60 minutes, washing the cathode plate by sulfuric acid and washing the cathode plate by pure water, and drying the cathode plate by hot air at the temperature of 120 ℃ when the pH of the last washing water is 7 and the chloride ions, the sodium ions and the sulfate ions are all less than 10ppm; then, the air-dried recovered copper is placed into an anode chamber of an electrolytic cell, copper sulfate solution with the copper ion concentration of 80g/L is injected into the anode chamber, sulfuric acid solution with the mass concentration of 15% is injected into a cathode chamber, a cathode consists of a copper sheet with the thickness of 2 mm, the anode copper is electrified and electrochemically dissolved, due to the obstruction of an ionic membrane, copper ions in the anode chamber cannot enter the cathode chamber, hydrogen gas emerges from the cathode copper sheet, copper-rich electrolyte in the anode chamber is added into an electrolytic copper plating production line at a certain speed, so that the copper ion concentration of the electrolytic copper plating production line is maintained at 50g/L, and the electrolyte overflowing from the electrolytic copper plating production line is copper-poor electrolyte and returns to the anode chamber of the electrolytic cell in the copper-rich electrolyte preparation process.
Example 2
Filtering the overflow acidic etching waste liquid of an acidic etching line of a certain B circuit board factory, adding an electrolytic additive according to the proportion of 0.03Kg/1000L, and adding an electrolytic circulation tank with the current density of 160A/square meter at a certain speed to keep the concentration of copper ions in the electrolytic circulation tank at 45g/L; taking out the electrolytic circulation tank when the thickness of copper on a cathode plate of the electrolytic circulation tank is 10 mm, sequentially washing by tap water, soaking by liquid alkali with the mass concentration of 10% at 50 ℃ for 50 minutes for cleaning, washing by sulfuric acid and cleaning by pure water, and drying by hot air at 100 ℃ when the pH of the last washing water is 7 and the content of chloride ions, sodium ions and sulfate ions is less than 10ppm; then, the air-dried recovered copper is placed into an anode chamber of an electrolytic cell, copper sulfate solution with copper ion concentration of 70g/L is injected into the anode chamber, sulfuric acid solution with mass concentration of 20% is injected into a cathode chamber, a cathode consists of a copper sheet with the thickness of 2 mm, the anode is electrified, anode copper is subjected to electrochemical dissolution, due to the blocking of an ionic membrane, copper ions in the anode chamber cannot enter a cathode area, hydrogen gas emerges from the cathode copper sheet, copper-rich electrolyte in the anode chamber is added into an electrolytic copper plating production line at a certain speed, the copper ion concentration of the electrolytic copper plating production line is maintained at 30g/L, the electrolyte overflowing from the electrolytic copper plating production line is copper-poor electrolyte, and the electrolyte returns to the anode chamber of the electrolytic cell in the copper-rich electrolyte preparation process.
Example 3
Filtering the overflowing acidic etching waste liquid of an acidic etching line of a certain C circuit board factory, adding an electrolytic additive according to the proportion of 0.05Kg/1000L, and adding an electrolytic circulating tank with the current density of 200A/square meter at a certain speed to keep the concentration of copper ions in the electrolytic circulating tank at 40g/L; taking out the cathode plate when the copper thickness is 8 mm, sequentially washing the cathode plate by tap water, soaking the cathode plate in liquid alkali with the mass concentration of 5% for 30 minutes at 70 ℃, washing the cathode plate by sulfuric acid and washing the cathode plate by pure water, and drying the cathode plate by hot air at 90 ℃ after the pH of the last washing water is 7 and the chloride ions, the sodium ions and the sulfate ions are all less than 10ppm; then, the air-dried recovered copper is placed into an anode chamber of an electrolytic cell, copper sulfate solution with copper ion concentration of 60g/L is injected into the anode chamber, sulfuric acid solution with mass concentration of 20% is injected into a cathode chamber, a cathode consists of a copper sheet with the thickness of 2 mm, the anode copper is electrified, electrochemical dissolution is carried out on the anode copper, copper ions in the anode chamber cannot enter the cathode chamber due to the obstruction of an ionic membrane, hydrogen gas is emitted from the cathode copper sheet, copper-rich electrolyte in the anode chamber is added into an electrolytic copper plating production line at a certain speed, the copper ion concentration of the electrolytic copper plating production line is maintained at 25g/L, the electrolyte overflowing from the electrolytic copper plating production line is copper-poor electrolyte, and the copper-poor electrolyte returns to an electrolytic cell polar chamber of a copper-rich electrolyte preparation process.
To sum up: the method for recovering cathode copper from acidic waste etching solution to replace phosphorus copper balls in the application comprises the steps of after the cathode copper is recovered from the waste etching solution through electrolysis, preparing copper-rich electrolyte in a mode of electrochemical dissolution of an electrolytic cell, and recycling the copper-rich electrolyte to a PCB (printed Circuit Board) electroplating production line, so that the recovered cathode copper replaces the phosphorus copper balls to serve as the electroplated copper, the problem of uneven current distribution is prevented, the loss of copper value of circuit board enterprises is greatly reduced, the cost of the circuit board enterprises on the metal copper is greatly reduced, and the method has good economy.
The above is merely an embodiment 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 (10)
1. A method for recovering cathode copper from acidic etching waste liquid to replace phosphor copper balls is characterized by comprising the following steps:
electrolyzing the acidic etching waste liquid to obtain recovered cathode copper;
sequentially carrying out alkali washing, acid washing, pure water washing and drying on the recovered cathode copper to obtain pretreated recovered cathode copper;
putting the pretreated and recovered cathode copper into an electrolytic cell for electrochemical dissolution to obtain copper-rich electrolyte;
and the copper-rich electrolyte is recycled to the electroplating production line.
2. The method for recovering cathode copper from acidic waste etching solution to replace phosphor copper balls as claimed in claim 1, wherein the pretreatment of the recovered cathode copper is put into an anode chamber of an electrolytic cell for electrochemical dissolution to obtain copper-rich electrolyte, comprising the following substeps:
the pretreated and recovered cathode copper is put into an anode chamber of an electrolytic cell for electrochemical dissolution;
and the overflow solution of the anode chamber is copper-rich electrolyte.
3. The method for recovering cathode copper from the acidic etching waste liquid to replace phosphorus copper balls as claimed in claim 2, wherein the electrolytic cell further comprises a diaphragm and a cathode chamber, the diaphragm is arranged between the anode chamber and the cathode chamber, and the diaphragm is an anion heterogeneous ion exchange membrane.
4. The method for recovering cathode copper instead of phosphorus copper balls according to claim 3, characterized in that a copper sulfate solution is provided in the anode chamber and a sulfuric acid solution is provided in the cathode chamber.
5. The method for recovering cathode copper to replace phosphor copper balls according to claim 2, wherein the copper-rich electrolyte is recycled to an electroplating production line, and the method comprises the following substeps:
the copper-rich electrolyte is recycled to the electroplating production line;
the overflow solution of the electroplating production line is a copper-poor electrolyte;
and the copper-poor electrolyte is recycled to the anode chamber.
6. The method for recovering cathode copper to replace phosphor copper balls according to claim 1, wherein the copper ion concentration of the solution in the electroplating production line is 15-50g/L.
7. The method for recovering cathode copper from acidic waste etching solution to replace phosphor copper balls as claimed in claim 1, wherein the acidic waste etching solution is electrolyzed to obtain recovered cathode copper, and the method comprises the following substeps:
adding quaternary ammonium salt electrolytic additive into the acidic etching waste liquid for electrolysis;
and stripping the recovered cathode copper from the cathode to obtain the recovered cathode copper.
8. The method for recovering cathode copper from acidic etching waste liquid to replace phosphor copper balls as claimed in claim 7, wherein the polymeric quaternary ammonium salt electrolytic additive is polydiene dimethyl ammonium chloride.
9. The method for recovering cathode copper from acidic waste etching solution to replace phosphorus copper balls as claimed in claim 7, wherein the addition amount of the polymeric quaternary ammonium salt electrolytic additive is 0.01-0.05Kg/1000L.
10. The method for recovering cathode copper from acidic etching waste liquid to replace phosphor copper balls according to claim 1, wherein before the acidic etching waste liquid is electrolyzed to obtain the recovered cathode copper, the method further comprises the following steps: filtering the acidic etching waste liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211604912.0A CN115961331A (en) | 2022-12-14 | 2022-12-14 | Method for recycling cathode copper from acidic etching waste liquid to replace phosphor copper balls |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211604912.0A CN115961331A (en) | 2022-12-14 | 2022-12-14 | Method for recycling cathode copper from acidic etching waste liquid to replace phosphor copper balls |
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| CN115961331A true CN115961331A (en) | 2023-04-14 |
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| CN202211604912.0A Pending CN115961331A (en) | 2022-12-14 | 2022-12-14 | Method for recycling cathode copper from acidic etching waste liquid to replace phosphor copper balls |
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- 2022-12-14 CN CN202211604912.0A patent/CN115961331A/en active Pending
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