CN112663065A - Regeneration and recycling method of alkaline etching solution - Google Patents
Regeneration and recycling method of alkaline etching solution Download PDFInfo
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- CN112663065A CN112663065A CN202011332801.XA CN202011332801A CN112663065A CN 112663065 A CN112663065 A CN 112663065A CN 202011332801 A CN202011332801 A CN 202011332801A CN 112663065 A CN112663065 A CN 112663065A
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- alkaline etching
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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 a method for recycling alkaline etching solution, which is characterized by comprising the following steps: step S1, collecting waste alkaline etching solution; step S2, extraction and back extraction treatment; step S3, copper is extracted through electrolysis; step S4, regenerating extraction mother liquor; and step S5, recycling. The regeneration and recycling method of the alkaline etching solution disclosed by the invention has the advantages of simple process, operation control method and less equipment investment, can safely and efficiently realize the recycling of the waste liquid, changes waste into valuable, and realizes the synchronous promotion of economic benefit, social benefit and ecological benefit. The comprehensive performance of the regenerated alkaline etching solution can be effectively enhanced by adding the regenerated additive of the alkaline etching solution; therefore, the production cost of enterprises is effectively reduced, the elemental copper can be obtained while the elemental copper is recycled, the enterprise benefit is increased, in the whole process engineering, the resource is saved due to cyclic utilization, and the environmental problem caused by leakage in the transportation process is avoided.
Description
Technical Field
The invention relates to the technical field of waste liquid recycling treatment and non-ferrous metal recovery, in particular to a method for recycling alkaline etching solution.
Background
With the more and more rapid development of the Printed Circuit Board (PCB) industry, a large amount of etching solution is required in the production and manufacturing process of the PCB, and in the alkaline etching process of the PCB, the etching effect is reduced due to the increase of the concentration of copper ions in the etching solution, and at the moment, the etching solution loses the etching capability and becomes etching waste liquid. The waste liquid has high toxicity and strong corrosivity, and the currently common alkaline etching waste liquid treatment method is that the alkaline etching waste liquid without any treatment is directly sold to qualified waste liquid recovery companies, and PCB (printed Circuit Board) manufacturing plants continuously purchase etching salt and ammonia water to prepare etching sub-liquid for production, so that resource waste is caused, and the risk of leakage of the etching waste liquid is increased.
The regeneration and recycling of the alkaline etching solution can not only solve the influence of the alkaline etching solution on the environment, but also realize the change of waste into valuable, recycle resources and be a treatment mode of the alkaline etching waste liquid with coexisting economic value, social value and ecological value. The existing method for detecting the regeneration and recycling of the etching solution has complex process, the prepared regenerated alkaline etching solution has low etching speed and large influence on comprehensive performance, and secondary pollution is easy to generate.
Chinese patent No. CN 102732887B discloses a method and system for recycling alkaline etching waste liquid and extracting copper. By utilizing the principle of layering and electrolysis, copper ions in the waste liquid are electrolyzed and reduced into elemental copper, and meanwhile, the additive is added into the alkaline etching recovery liquid to form regenerated etching liquid for recycling. By the method, the production cost of enterprises can be greatly reduced, the income of the enterprises is improved through the recovery of copper, resources are saved, the national call for energy conservation and emission reduction is responded, and the environmental pollution caused by the leakage of waste liquid is avoided. However, the method depends on an intelligent storage tank device, so that the equipment investment is large, the process flow is complex, and the recycling efficiency is low.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for recycling alkaline etching solution, which has the advantages of simple process, operation control method, less equipment investment, capability of safely and efficiently recycling waste liquid, waste material recycling and realization of synchronous promotion of economic benefit, social benefit and ecological benefit. The comprehensive performance of the regenerated alkaline etching solution can be effectively enhanced by adding the regenerated additive of the alkaline etching solution; therefore, the production cost of enterprises is effectively reduced, the elemental copper can be obtained while the elemental copper is recycled, the enterprise benefit is increased, in the whole process engineering, the resource is saved due to cyclic utilization, and the environmental problem caused by leakage in the transportation process is avoided.
In order to achieve the purpose, the invention adopts the technical scheme that: a regeneration and recycling method of alkaline etching solution is characterized by comprising the following steps:
step S1, collection of waste alkaline etching solution: conveying the regenerated etching solution in the regenerated solution tank to an alkaline etching line (SES) for etching, and collecting the generated waste alkaline etching solution into an etching waste solution tank;
step S2, extraction and back extraction treatment: conveying the waste alkaline etching solution prepared in the step S1 to an extraction tank, and adding an extracting agent for extraction; then separating the copper-rich extractant and the extraction mother liquor through filtering operation, and placing the copper-rich extractant and the extraction mother liquor into the copper-rich extractant back-extraction agent for back-extraction to obtain electrolyte;
step S3, electrolytic copper extraction: inputting the electrolyte prepared in the step S2 into an electrolytic cell for electrolysis to obtain a copper simple substance;
step S4, regeneration of extraction mother liquor: adding a regenerant into the extraction mother liquor obtained by the treatment of the step S2, and uniformly mixing to realize regeneration;
step S5, recycling: and returning the alkaline etching regeneration liquid subjected to the regeneration treatment in the step S4 to the etching production line for reuse.
Preferably, the extractant in step S2 is at least one of a strong acid styrene cation exchange resin and an AMBERJET 1200H strong acid cation exchange resin.
Preferably, the mass ratio of the waste alkaline etching solution to the extracting agent in the step S2 is (3-5): 1.
Preferably, the stripping agent in step S2 is at least one of a copper sulfate solution and a copper nitrate solution.
Preferably, the mass percentage concentration of the stripping agent in the step S2 is 15-30%.
Preferably, the range of the electrolytic cathode current density in step S3 is 800-1800A/m2The range of the current density of the anode is 100-200A/m2。
Preferably, the amount of the regenerant added in step S3 is 1L (300- & lt 500- & gt) ppm of the extraction mother liquor.
Preferably, the regenerant in step S3 comprises the following components in parts by weight: 3-5 parts of ammonia water, 2-4 parts of first-generation polythiourea dendrimer, 4-8 parts of ammonium bicarbonate, 1-3 parts of bis (2-hydroxyethyl) amino (trihydroxymethyl) methane, 1-3 parts of N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] diethanolamine and 1-2 parts of hydroxyurea.
Another object of the present invention is to provide a regenerated alkaline etching solution prepared by the method for regenerating and recycling the alkaline etching solution.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the invention provides a method for recycling alkaline etching solution, which has the advantages of simple process, operation control method, less equipment investment, capability of safely and efficiently recycling waste liquid, waste material recycling, and realization of synchronous promotion of economic benefit, social benefit and ecological benefit. The comprehensive performance of the regenerated alkaline etching solution can be effectively enhanced by adding the regenerated additive of the alkaline etching solution; therefore, the production cost of enterprises is effectively reduced, the elemental copper can be obtained while the elemental copper is recycled, the enterprise benefit is increased, in the whole process engineering, the resource is saved due to cyclic utilization, and the environmental problem caused by leakage in the transportation process is avoided.
Detailed Description
The following detailed description of preferred embodiments of the invention will be made.
A regeneration and recycling method of alkaline etching solution is characterized by comprising the following steps:
step S1, collection of waste alkaline etching solution: conveying the regenerated etching solution in the regenerated solution tank to an alkaline etching line (SES) for etching, and collecting the generated waste alkaline etching solution into an etching waste solution tank;
step S2, extraction and back extraction treatment: conveying the waste alkaline etching solution prepared in the step S1 to an extraction tank, and adding an extracting agent for extraction; then separating the copper-rich extractant and the extraction mother liquor through filtering operation, and placing the copper-rich extractant and the extraction mother liquor into the copper-rich extractant back-extraction agent for back-extraction to obtain electrolyte;
step S3, electrolytic copper extraction: inputting the electrolyte prepared in the step S2 into an electrolytic cell for electrolysis to obtain a copper simple substance;
step S4, regeneration of extraction mother liquor: adding a regenerant into the extraction mother liquor obtained by the treatment of the step S2, and uniformly mixing to realize regeneration;
step S5, recycling: and returning the alkaline etching regeneration liquid subjected to the regeneration treatment in the step S4 to the etching production line for reuse.
Preferably, the extractant in step S2 is at least one of a strong acid styrene cation exchange resin and an AMBERJET 1200H strong acid cation exchange resin.
Preferably, the mass ratio of the waste alkaline etching solution to the extracting agent in the step S2 is (3-5): 1.
Preferably, the stripping agent in step S2 is at least one of a copper sulfate solution and a copper nitrate solution.
Preferably, the mass percentage concentration of the stripping agent in the step S2 is 15-30%.
Preferably, the range of the electrolytic cathode current density in step S3 is 800-1800A/m2The range of the current density of the anode is 100-200A/m2。
Preferably, the amount of the regenerant added in step S3 is 1L (300- & lt 500- & gt) ppm of the extraction mother liquor.
Preferably, the regenerant in step S3 comprises the following components in parts by weight: 3-5 parts of ammonia water, 2-4 parts of first-generation polythiourea dendrimer, 4-8 parts of ammonium bicarbonate, 1-3 parts of bis (2-hydroxyethyl) amino (trihydroxymethyl) methane, 1-3 parts of N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] diethanolamine and 1-2 parts of hydroxyurea.
Preferably, the preparation method of the first-generation polythiourea dendrimer is referred to CN105524285A example 1.
Another object of the present invention is to provide a regenerated alkaline etching solution prepared by the method for regenerating and recycling the alkaline etching solution.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the invention provides a method for recycling alkaline etching solution, which has the advantages of simple process, operation control method, less equipment investment, capability of safely and efficiently recycling waste liquid, waste material recycling, and realization of synchronous promotion of economic benefit, social benefit and ecological benefit. The comprehensive performance of the regenerated alkaline etching solution can be effectively enhanced by adding the regenerated additive of the alkaline etching solution; therefore, the production cost of enterprises is effectively reduced, the elemental copper can be obtained while the elemental copper is recycled, the enterprise benefit is increased, in the whole process engineering, the resource is saved due to cyclic utilization, and the environmental problem caused by leakage in the transportation process is avoided.
The invention will be further described with reference to specific examples, but the scope of protection of the invention is not limited thereto:
example 1
Embodiment 1 provides a method for recycling an alkaline etching solution, which is characterized by comprising the following steps:
step S1, collection of waste alkaline etching solution: conveying the regenerated etching solution in the regenerated solution tank to an alkaline etching line (SES) for etching, and collecting the generated waste alkaline etching solution into an etching waste solution tank;
step S2, extraction and back extraction treatment: conveying the waste alkaline etching solution prepared in the step S1 to an extraction tank, and adding an extracting agent for extraction; then separating the copper-rich extractant and the extraction mother liquor through filtering operation, and placing the copper-rich extractant and the extraction mother liquor into the copper-rich extractant back-extraction agent for back-extraction to obtain electrolyte;
step S3, electrolytic copper extraction: inputting the electrolyte prepared in the step S2 into an electrolytic cell for electrolysis to obtain a copper simple substance;
step S4, regeneration of extraction mother liquor: adding a regenerant into the extraction mother liquor obtained by the treatment of the step S2, and uniformly mixing to realize regeneration;
step S5, recycling: and returning the alkaline etching regeneration liquid subjected to the regeneration treatment in the step S4 to the etching production line for reuse.
In the step S2, the extractant is strong acid styrene cation exchange resin; the mass ratio of the waste alkaline etching solution to the extracting agent is 3: 1; the back extractant is copper sulfate solution; the mass percentage concentration of the stripping agent is 15%.
The range of the electrolytic cathode current density in the step S3 is 800A/m2The range of the anode current density is 100A/m2(ii) a The addition amount of the regenerant is 1L, and 300ppm of extraction mother liquor.
The regenerant in the step S3 comprises the following components in parts by weight: 3 parts of ammonia water, 2 parts of first-generation polythiourea dendrimer, 4 parts of ammonium bicarbonate, 1 part of bis (2-hydroxyethyl) amino (trihydroxymethyl) methane, 1 part of N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] diethanolamine and 1 part of hydroxyurea.
A regenerated alkaline etching solution prepared according to the method for regenerating and recycling the alkaline etching solution.
Example 2
Embodiment 2 provides a method for recycling an alkaline etching solution, which is substantially the same as embodiment 1, except that the regenerant in step S3 comprises the following components in parts by weight: 3.5 parts of ammonia water, 2.5 parts of first-generation polythiourea dendrimer, 5 parts of ammonium bicarbonate, 1.5 parts of bis (2-hydroxyethyl) amino (trihydroxymethyl) methane, 1.5 parts of N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] diethanolamine and 1.2 parts of hydroxyurea.
Example 3
Embodiment 3 provides a method for recycling an alkaline etching solution, which is substantially the same as embodiment 1, except that the regenerant in step S3 comprises the following components in parts by weight: 4 parts of ammonia water, 3 parts of first-generation polythiourea dendrimer, 6 parts of ammonium bicarbonate, 2 parts of bis (2-hydroxyethyl) amino (trihydroxymethyl) methane, 2 parts of N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] diethanolamine and 1.5 parts of hydroxyurea.
Example 4
Embodiment 4 provides a method for recycling an alkaline etching solution, which is substantially the same as embodiment 1, except that the regenerant in step S3 comprises the following components in parts by weight: 4.5 parts of ammonia water, 3.5 parts of first-generation polythiourea dendrimer, 7 parts of ammonium bicarbonate, 2.5 parts of bis (2-hydroxyethyl) amino (trihydroxymethyl) methane, 2.5 parts of N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] diethanolamine and 1.8 parts of hydroxyurea.
Example 5
Embodiment 5 provides a method for recycling an alkaline etching solution, which is substantially the same as embodiment 1, except that the regenerant in step S3 comprises the following components in parts by weight: 5 parts of ammonia water, 4 parts of first-generation polythiourea dendrimer, 8 parts of ammonium bicarbonate, 3 parts of bis (2-hydroxyethyl) amino (trihydroxymethyl) methane, 3 parts of N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] diethanolamine and 2 parts of hydroxyurea.
Comparative example 1
Comparative example 1 provides a method of recycling an alkaline etching solution, which is substantially the same as in example 1 except that the regenerant of step S3 does not include the first-generation polythiourea dendrimer.
Comparative example 2
Comparative example 2 provides a method of recycling the alkaline etching solution, which is substantially the same as example 1, except that the regenerant described in step S3 does not include bis (2-hydroxyethyl) amino (trimethylol) methane.
Comparative example 3
Comparative example 3 provides a method of recycling the alkaline etching solution, which is substantially the same as in example 1 except that the regenerant described in step S3 does not include N- [ (5-methyl-1H-benzotriazol-1-yl) methyl ] diethanolamine.
Comparative example 4
Comparative example 4 provides a method for recycling the alkaline etching solution, which is substantially the same as example 1, except that the regenerant described in step S3 does not include hydroxyurea.
In order to further illustrate the beneficial technical effects of the embodiments, the regenerated alkaline etching solution obtained by the method of each embodiment is used for etching, and the etching rate is calculated statistically. The test results are shown in Table 1.
TABLE 1
As can be seen from the above table, the regenerated alkaline etching solution obtained by the method for recycling the alkaline etching solution according to the embodiment of the present invention has a better etching effect, which is a result of the synergistic effect of the additives in each step.
The above-mentioned embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (9)
1. A regeneration and recycling method of alkaline etching solution is characterized by comprising the following steps:
step S1, collection of waste alkaline etching solution: conveying the regenerated etching solution in the regenerated solution tank to an alkaline etching line (SES) for etching, and collecting the generated waste alkaline etching solution into an etching waste solution tank;
step S2, extraction and back extraction treatment: conveying the waste alkaline etching solution prepared in the step S1 to an extraction tank, and adding an extracting agent for extraction; then separating the copper-rich extractant and the extraction mother liquor through filtering operation, and placing the copper-rich extractant and the extraction mother liquor into the copper-rich extractant back-extraction agent for back-extraction to obtain electrolyte;
step S3, electrolytic copper extraction: inputting the electrolyte prepared in the step S2 into an electrolytic cell for electrolysis to obtain a copper simple substance;
step S4, regeneration of extraction mother liquor: adding a regenerant into the extraction mother liquor obtained by the treatment of the step S2, and uniformly mixing to realize regeneration;
step S5, recycling: and returning the alkaline etching regeneration liquid subjected to the regeneration treatment in the step S4 to the etching production line for reuse.
2. The method as claimed in claim 1, wherein the extractant in step S2 is at least one of a strong acid styrene cation exchange resin and an AMBERJET 1200H strong acid cation exchange resin.
3. The method as claimed in claim 1, wherein the mass ratio of the waste alkaline etching solution to the extractant in step S2 is (3-5): 1.
4. The method as claimed in claim 1, wherein the stripping agent in step S2 is at least one of copper sulfate solution and copper nitrate solution.
5. The method according to claim 1, wherein the mass percentage concentration of the stripping agent in step S2 is 15-30%.
6. The method as claimed in claim 1, wherein the electrolytic cathodic current density in step S3 is in the range of 800-1800A/m2The range of the current density of the anode is 100-200A/m2。
7. The method as claimed in claim 1, wherein the amount of the regenerant added in step S3 is 1L (300- & 500) ppm of the extraction mother liquor.
8. The method of claim 1, wherein the regenerant of step S3 comprises the following components in parts by weight: 3-5 parts of ammonia water, 2-4 parts of first-generation polythiourea dendrimer, 4-8 parts of ammonium bicarbonate, 1-3 parts of bis (2-hydroxyethyl) amino (trihydroxymethyl) methane, 1-3 parts of N- [ (5-methyl-1H-benzotriazole-1-yl) methyl ] diethanolamine and 1-2 parts of hydroxyurea.
9. A regenerated alkaline etching solution prepared by the method for regenerating and recycling the alkaline etching solution according to any one of claims 1 to 8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114032394A (en) * | 2021-11-08 | 2022-02-11 | 昆山华拓环保科技有限公司 | Regeneration copper extraction method of alkaline etching solution |
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Application publication date: 20210416 |