CN113235132A - Additive for regenerating electrolytic copper from etching waste liquid, preparation method thereof and electrolyte - Google Patents
Additive for regenerating electrolytic copper from etching waste liquid, preparation method thereof and electrolyte Download PDFInfo
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- CN113235132A CN113235132A CN202110537189.8A CN202110537189A CN113235132A CN 113235132 A CN113235132 A CN 113235132A CN 202110537189 A CN202110537189 A CN 202110537189A CN 113235132 A CN113235132 A CN 113235132A
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- additive
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- waste liquid
- electrolytic copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/46—Regeneration of etching compositions
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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
Abstract
The invention discloses an additive for regenerating electrolytic copper from etching waste liquid, a preparation method thereof and electrolyte. Wherein the additive for the etching waste liquid regenerated electrolytic copper comprises the following components in parts by mass: 500 portions of copper brightener; 300 portions of conductive agent and 500 portions of conductive agent; 1000-1500 parts of stabilizer; wetting agent, 2000-; and 20-100 parts of a complexing agent. The technical scheme of the invention can improve the electrolytic density in the electrolytic process, thereby enhancing the hardness of the obtained copper plate, saving the electrolytic time and reducing the electrolytic power consumption.
Description
Technical Field
The invention relates to the technical field of etching waste liquid regeneration, in particular to an additive for regenerating electrolytic copper from etching waste liquid, a preparation method thereof and electrolyte.
Background
The etching treatment is an important step in the PCB manufacturing process, and both acid etching and alkaline etching generate a large amount of waste etching solution containing a large amount of copper ions, and the waste etching solution is usually subjected to an electrolysis operation to recover the metals therein. In the existing copper electrolysis process, the current density is often low, so that the hardness of the obtained copper plate is low, the electrolysis operation time is long, and the electrolysis power consumption is large.
Disclosure of Invention
The invention mainly aims to provide an additive for regenerating electrolytic copper from etching waste liquid, a preparation method thereof and electrolyte, aiming at improving the electrolytic density in the electrolytic process, thereby enhancing the hardness of the obtained copper plate, saving the electrolytic time and reducing the electrolytic power consumption.
In order to achieve the purpose, the additive for the waste etching solution regenerated electrolytic copper provided by the invention comprises the following components in parts by mass: 500 portions of copper brightener; 300 portions of conductive agent and 500 portions of conductive agent; 1000-1500 parts of stabilizer; wetting agent, 2000-; and 20-100 parts of a complexing agent.
In an optional embodiment, the copper brightener is N, N-dimethyl dithio-carbon propane sodium sulfonate; and/or the conductive agent is sodium polydithio-dipropyl sulfonate.
In an optional embodiment, the stabilizer is isothiourea propyl sulfonate; and/or, the wetting agent is selected from polyethylene glycol with the molecular weight of 10000.
In an optional embodiment, the complexing agent is a sulfuric acid solution with a mass concentration of 98%.
In an optional embodiment, the additive for regenerating electrolytic copper from etching waste liquid further comprises 300-500 parts of leveling agent by mass.
In an alternative embodiment, the leveling agent is prepared by the following steps:
adding 0.5g-1g of wine red dye into 500mL of polyethylene glycol with molecular weight of 200, and stirring and mixing.
The invention also provides a preparation method of the additive for regenerating electrolytic copper from etching waste liquid, which comprises the following steps:
adding an acidic reagent into 15kg of water, and adjusting the pH value to be 2-3;
sequentially adding 500-1000 parts of copper brightening agent, 300-500 parts of conductive agent, 1000-1500 parts of stabilizing agent and 2000-2500 parts of wetting agent, and stirring to dissolve;
adding an acidic reagent, slowly adding 20-100 parts of complexing agent while stirring, adjusting the pH value to 1, and continuously stirring and mixing to obtain the additive for the etching waste liquid regenerated electrolytic copper.
In an optional embodiment, the method further includes the steps of adding an acidic reagent, slowly adding 20 to 100 parts of a complexing agent while stirring, and adjusting the pH to 1:
adding 300-500 parts of leveling agent, stirring and mixing, wherein the leveling agent is prepared by the following steps:
adding 0.5g-1g of wine red dye into 500mL of polyethylene glycol with molecular weight of 200, and stirring and mixing.
The invention also provides an electrolyte for regenerating electrolytic copper from etching waste liquid, which comprises the additive for regenerating electrolytic copper from etching waste liquid.
In an alternative embodiment, the additive is added in an amount ranging from 200mL to 300mL per ton of the electrolyte.
The technical scheme of the invention can at least obtain the following beneficial effects: the additive provided by the invention is used for carrying out regeneration electrolytic copper operation on the etching waste liquid, so that an electrolytic copper plate with higher purity and higher hardness can be obtained, the current density in the electrolytic process can be improved, the adsorption speed of electrolytic cathode copper is improved, the electrolytic time is saved, the power consumption is saved, and the cost is saved. The additive is energy-saving and environment-friendly, is convenient to use and is harmless to human bodies. In addition, the additive has no adverse side effect on the electrolyzed etching waste liquid, the electrolyzed regenerated etching liquid can be recycled all the time without replacement, the etching speed of the additive is not different from that of a brand new etching sub-liquid, and the additive is even faster and more stable. In addition, the additive is a multipurpose multifunctional electrolytic copper additive, and is suitable for regenerating electrolytic copper by alkaline, acidic and micro-etching solution.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
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.
The invention provides an additive for regenerating electrolytic copper from etching waste liquid, wherein the etching waste liquid can be acidic etching waste liquid, alkaline etching waste liquid or micro etching waste liquid.
The additive for regenerating electrolytic copper from etching waste liquid comprises the following components in parts by mass: 500 portions of copper brightener; 300 portions of conductive agent and 500 portions of conductive agent; 1000-1500 parts of stabilizer; wetting agent, 2000-; and 20-100 parts of a complexing agent.
After the copper brightening agent is added, a plating layer with better bright ductility can be obtained in the copper electrolysis process, and due to the addition of the conductive agent, the plating layer can be crystallized and refined, the current density of electrolysis operation is improved, the adsorption speed of electrolytic cathode copper is improved, the hardness of the copper plating layer is enhanced, the electrolysis time is saved, the power consumption is saved, and the cost is saved. The stability of the anion activity of the surface layer of the plating layer can be improved by adding the stabilizer. The addition of the wetting agent has the effects of eliminating pinhole and pockmark on the surface of the plating layer and reducing stress, so that the copper at the bottom of the plating layer is not easy to burn black and change color and keeps bright. The addition of the complexing agent mainly plays a role in complexing and adjusting the pH.
It should be noted that when the additive of the invention is used for carrying out regeneration electrolytic copper operation on etching waste liquid, 2500-. And the regenerated etching solution after electrolysis etches the lines 2mi to 3mi finest.
When the additive for the electrolytic copper regenerated from the etching waste liquid is prepared, the dosage of each component is reasonably controlled, so that the additive can fully play the role of the component, and the additive with better performance is obtained. In alternative embodiments, the amount of the copper brightener is 500 parts, 600 parts, 700 parts, 800 parts, 900 parts, or 1000 parts by mass; the amount of the conductive agent is 300 parts, 400 parts or 500 parts; the amount of the stabilizer is 1000 parts, 1100 parts, 1200 parts, 1300 parts, 1400 parts or 1500 parts; the amount of wetting agent is 2000 parts, 2100 parts, 2200 parts, 2300 parts, 2400 parts or 2500 parts; and the amount of the complexing agent is 20 parts, 40 parts, 60 parts, 80 parts or 100 parts.
The technical scheme of the invention can at least obtain the following beneficial effects: the additive provided by the invention is used for carrying out regeneration electrolytic copper operation on the etching waste liquid, so that an electrolytic copper plate with higher purity and higher hardness can be obtained, the current density in the electrolytic process can be improved, the adsorption speed of electrolytic cathode copper is improved, the electrolytic time is saved, the power consumption is saved, and the cost is saved. The additive is energy-saving and environment-friendly, is convenient to use and is harmless to human bodies. In addition, the additive has no adverse side effect on the electrolyzed etching waste liquid, the electrolyzed regenerated etching liquid can be recycled all the time without replacement, the etching speed of the additive is not different from that of a brand new etching sub-liquid, and the additive is even faster and more stable. In addition, the additive is a multipurpose multifunctional electrolytic copper additive, and is suitable for regenerating electrolytic copper by alkaline, acidic and micro-etching solution.
In an alternative embodiment, the copper brightener is sodium N, N-dimethyldithiocarbylpropane sulfonate. The N, N-dimethyl dithio carbon propane sodium sulfonate is DPS for short, can be directly purchased from the market, and can obtain a metal copper plating layer with better brightness and ductility after being added.
In an alternative embodiment, the conductive agent is sodium polydithio dipropyl sulfonate. The sodium polydithio-dipropyl sulfonate (SPS) is a conductive agent with good performance, and can be added to make the coating be crystallized and refined, raise current density of electrolytic operation, raise adsorption speed of electrolytic cathode copper, raise purity of copper coating, raise hardness, at the same time can save electrolytic time, save power consumption and save cost.
In an alternative embodiment, the stabilizer is isothiourea propyl sulfonate. The isothiourea propyl sulfonate inner salt is called UPS for short, is a stabilizer with better performance, and can effectively improve the stability of the anion activity of the surface layer of the plating layer after being added.
In an alternative embodiment, the humectant is polyethylene glycol having a molecular weight of 10000. Polyethylene glycol with molecular weight of 10000 is called PEG-10000 for short, is a wetting agent with good performance, can effectively eliminate pinhole pocks on the surface of a plating layer after being added, reduces stress, and ensures that copper at the bottom of the plating layer is not easy to burn black and change color and keeps bright.
In an alternative embodiment, the complexing agent is a sulfuric acid solution with a mass concentration of 98%.
Further, the additive for regenerating electrolytic copper from etching waste liquid also comprises 300-500 parts of leveling agent by mass. The leveling agent is added, so that the brightness of the surface of the plating layer can be further improved, and the metal copper plating layer with smooth and uniform surface can be obtained.
In an alternative embodiment, the leveling agent is prepared by the following steps:
adding 0.5g-1g of wine red dye into 500mL of polyethylene glycol with molecular weight of 200, and stirring and mixing.
The wine red dye can adjust the color of the liquid to be consistent and uniform, so that the metal copper plating layer with better surface uniformity and consistency is obtained.
The invention also provides a preparation method of the additive for regenerating electrolytic copper from etching waste liquid, which comprises the following steps:
adding an acidic reagent into 15kg of water, and adjusting the pH value to be 2-3;
sequentially adding 500-1000 parts of copper brightening agent, 300-500 parts of conductive agent, 1000-1500 parts of stabilizing agent and 2000-2500 parts of wetting agent, and stirring to dissolve;
adding an acidic reagent, slowly adding 20-100 parts of complexing agent while stirring, adjusting the pH value to 1, and continuously stirring and mixing to obtain the additive for the etching waste liquid regenerated electrolytic copper.
Specifically, the acidic reagent may be a 49% by mass sulfuric acid purity reagent, and 100g of the 49% by mass sulfuric acid purity reagent is added to 15kg of water to adjust the pH to 2 to 3. Then adding copper brightening agent, conductive agent, stabilizing agent and wetting agent into the mixture in turn, stirring to make them fully dissolved, here, slowly adding while stirring to make them fully dissolved to obtain liquid with better uniformity, and further beneficial to obtain copper coating with more compact surface uniformity. And then adding 100g of sulfuric acid with the mass concentration of 49% for analytical purification, slowly adding a complexing agent while stirring, adjusting the pH value to 1, and continuously stirring and uniformly mixing to obtain the additive for the etching waste liquid regenerated electrolytic copper.
Further, adding an acidic reagent, slowly adding 20-100 parts of a complexing agent while stirring, and after the step of adjusting the pH value to 1, the method also comprises the following steps:
adding 500 parts of 300-one leveling agent, stirring and mixing, wherein the leveling agent is prepared by the following steps:
adding 0.5g-1g of wine red dye into 500mL of polyethylene glycol with molecular weight of 200, and stirring and mixing.
The leveling agent is prepared in advance, the complexing agent is added, then the leveling agent is added, and the mixture is stirred and mixed uniformly, so that the additive for the etching waste liquid regenerated electrolytic copper can be obtained.
The invention also provides an electrolyte for regenerating electrolytic copper from etching waste liquid, which comprises the additive for regenerating electrolytic copper from etching waste liquid.
The additive provided by the invention is used for carrying out regeneration electrolytic copper operation on the etching waste liquid, so that an electrolytic copper plate with higher purity and higher hardness can be obtained, the current density in the electrolytic process can be improved, the adsorption speed of electrolytic cathode copper is improved, the electrolytic time is saved, the power consumption is saved, and the cost is saved. The additive is energy-saving and environment-friendly, is convenient to use and is harmless to human bodies. In addition, the additive has no adverse side effect on the electrolyzed etching waste liquid, the electrolyzed regenerated etching liquid can be recycled all the time without replacement, the etching speed of the additive is not different from that of a brand new etching sub-liquid, and the additive is even faster and more stable. In addition, the additive is a multipurpose multifunctional electrolytic copper additive, and is suitable for regenerating electrolytic copper by alkaline, acidic and micro-etching solution.
In an alternative embodiment, the additive is added in an amount ranging from 200mL to 300mL per ton of electrolyte. The additive is convenient to use and has lasting efficacy, only 200mL of the additive is needed to be added into each ton of electrolyte to continuously electrolyze for less than 48 hours, and 500-600 kg of electrolytic copper plate with 99% copper-containing purity can be produced.
The additive for regenerating electrolytic copper from etching waste liquid, the preparation method thereof, and the electrolyte of the present invention will be described in detail below with reference to specific examples.
Example 1
The additive of this example can be prepared by the following steps:
(1) adding 100g of sulfuric acid with the mass concentration of 49% into 15kg of water for analytical purification, and adjusting the pH value to be 2-3;
(2) adding 1000g of copper brightening agent, 500g of conductive agent, 1000g of stabilizing agent and 2500 parts of wetting agent in sequence, and stirring to dissolve the copper brightening agent, the conductive agent and the stabilizing agent;
(3) adding 100g of sulfuric acid with the mass concentration of 49% for analytical purification, slowly adding 100g of complexing agent while stirring, and adjusting the pH value to 1;
(4) and adding 500g of leveling agent prepared in advance, stirring and mixing to obtain the additive for the etching waste liquid regenerated electrolytic copper. Wherein, the leveling agent is prepared by the following steps: to 500mL of polyethylene glycol having a molecular weight of 200 was added 0.5g of a wine red dye, and mixed with stirring.
Example 2
The additive of this example can be prepared by the following steps:
(1) adding 100g of sulfuric acid with the mass concentration of 49% into 15kg of water for analytical purification, and adjusting the pH value to be 2-3;
(2) sequentially adding 800g of copper brightening agent, 450g of conductive agent, 1200g of stabilizing agent and 2400 parts of wetting agent, and stirring to dissolve the copper brightening agent, the conductive agent and the stabilizing agent;
(3) adding 100g of sulfuric acid with the mass concentration of 49% for analytical purification, slowly adding 80g of complexing agent while stirring, and adjusting the pH value to 1;
(4) and adding 400g of leveling agent prepared in advance, stirring and mixing to obtain the additive for the etching waste liquid regenerated electrolytic copper. Wherein, the leveling agent is prepared by the following steps: to 500mL of polyethylene glycol having a molecular weight of 200 was added 0.8g of a wine red dye, and mixed with stirring.
Example 3
The additive of this example can be prepared by the following steps:
(1) adding 100g of sulfuric acid with the mass concentration of 49% into 15kg of water for analytical purification, and adjusting the pH value to be 2-3;
(2) adding 500g of copper brightening agent, 300g of conductive agent, 1000g of stabilizing agent and 2000 parts of wetting agent in sequence, and stirring to dissolve the copper brightening agent, the conductive agent and the stabilizing agent;
(3) adding 100g of sulfuric acid with the mass concentration of 49% for analytical purification, slowly adding 50g of complexing agent while stirring, and adjusting the pH value to 1;
(4) and adding 350g of leveling agent which is prepared in advance, stirring and mixing to obtain the additive for the etching waste liquid regenerated electrolytic copper. Wherein, the leveling agent is prepared by the following steps: to 500mL of polyethylene glycol having a molecular weight of 200 was added 1g of a wine red dye, and the mixture was stirred and mixed.
It should be noted that in examples 1 to 3, the copper brightener is sodium N, N-dimethyldithiocarbylpropane sulfonate, the conductive agent is sodium polydithio-dipropyl sulfonate, the stabilizer is isothio-propanesulfonate, the wetting agent is polyethylene glycol with a molecular weight of 10000, and the complexing agent is 98% sulfuric acid solution.
The additive prepared in the embodiments 1 to 3 is added into the electrolyte, and the etching waste liquid is subjected to regeneration electrolytic copper operation, and only 200mL of the additive is required to be added into each ton of the electrolyte to continuously electrolyze for less than 48 hours, which shows that the additive has lasting efficacy. And 500-600 kg of electrolytic copper plate with the copper purity of 99 percent can be produced, and the hardness of the electrolytic copper plate is higher. Meanwhile, when the additive prepared in the embodiments 1 to 3 is used for carrying out the operation of regenerating electrolytic copper on the etching waste liquid, 2500-. In addition, the additives prepared in the embodiments 1 to 3 have no adverse side effect on the electrolyzed etching waste liquid, are environment-friendly, and the electrolyzed regenerated etching liquid can be recycled all the time without replacement, and has no difference with a brand-new etching sub-liquid in etching speed, and is even faster and more stable.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. The additive for the etching waste liquid regenerated electrolytic copper is characterized by comprising the following components in parts by mass:
500 portions of copper brightener;
300 portions of conductive agent and 500 portions of conductive agent;
1000-1500 parts of stabilizer;
wetting agent, 2000-; and
20-100 parts of a complexing agent.
2. The additive for regenerating electrolytic copper from etching waste liquid as claimed in claim 1, wherein said copper brightener is N, N-dimethyldithiocarbo propane sodium sulfonate; and/or the presence of a gas in the gas,
the conductive agent is sodium polydithio-dipropyl sulfonate.
3. The additive for regenerating electrolytic copper from etching waste liquid according to claim 1, wherein said stabilizer is isothiourea propanesulfonate; and/or the presence of a gas in the gas,
the humectant is polyethylene glycol with molecular weight of 10000.
4. The additive for regenerating electrolytic copper from etching waste liquid according to claim 1, wherein the complexing agent is a sulfuric acid solution having a mass concentration of 98%.
5. The additive for regenerating electrolytic copper from etching waste liquid as claimed in any one of claims 1 to 4, wherein the additive for regenerating electrolytic copper from etching waste liquid further comprises 300-500 parts by mass of leveling agent.
6. The additive for regenerating electrolytic copper from etching waste liquid according to claim 5, wherein said leveler is prepared by the steps of:
adding 0.5g-1g of wine red dye into 500mL of polyethylene glycol with molecular weight of 200, and stirring and mixing.
7. The preparation method of the additive for regenerating electrolytic copper from etching waste liquid is characterized by comprising the following steps:
adding an acidic reagent into 15kg of water, and adjusting the pH value to be 2-3;
sequentially adding 500-1000 parts of copper brightening agent, 300-500 parts of conductive agent, 1000-1500 parts of stabilizing agent and 2000-2500 parts of wetting agent, and stirring to dissolve;
adding an acidic reagent, slowly adding 20-100 parts of complexing agent while stirring, adjusting the pH value to 1, and continuously stirring and mixing to obtain the additive for the etching waste liquid regenerated electrolytic copper.
8. The method for preparing the additive for regenerating electrolytic copper from etching waste liquid according to claim 7, wherein the step of adding the acidic reagent, slowly adding 20 to 100 parts of the complexing agent while stirring, and adjusting the pH value to 1 further comprises:
adding 300-500 parts of leveling agent, stirring and mixing, wherein the leveling agent is prepared by the following steps:
adding 0.5g-1g of wine red dye into 500mL of polyethylene glycol with molecular weight of 200, and stirring and mixing.
9. An electrolyte for regenerating electrolytic copper from spent etching solution, characterized in that the electrolyte comprises the additive for regenerating electrolytic copper from spent etching solution according to any one of claims 1 to 6.
10. The electrolyte for copper electrolysis from spent etching solution according to claim 9, wherein the additive is added in an amount ranging from 200mL to 300mL per ton of the electrolyte.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110537189.8A CN113235132A (en) | 2021-05-17 | 2021-05-17 | Additive for regenerating electrolytic copper from etching waste liquid, preparation method thereof and electrolyte |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110537189.8A CN113235132A (en) | 2021-05-17 | 2021-05-17 | Additive for regenerating electrolytic copper from etching waste liquid, preparation method thereof and electrolyte |
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| CN113235132A true CN113235132A (en) | 2021-08-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114395789A (en) * | 2021-12-31 | 2022-04-26 | 广东鑫菱环境科技有限公司 | Method for recycling copper in PCB electroplating process |
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2021
- 2021-05-17 CN CN202110537189.8A patent/CN113235132A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114395789A (en) * | 2021-12-31 | 2022-04-26 | 广东鑫菱环境科技有限公司 | Method for recycling copper in PCB electroplating process |
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