CN112626561A - Method for recovering copper ions in alkaline etching solution - Google Patents
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- CN112626561A CN112626561A CN202011346363.2A CN202011346363A CN112626561A CN 112626561 A CN112626561 A CN 112626561A CN 202011346363 A CN202011346363 A CN 202011346363A CN 112626561 A CN112626561 A CN 112626561A
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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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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Abstract
The invention discloses a method for recovering copper ions in alkaline etching solution, which is characterized by comprising the following steps: step S1, extracting for multiple times; step S2, back extraction treatment; step S3, replenishing electrolytic additives; step S4, electrolysis; the electrolytic additive comprises the following components in parts by weight: 3-5 parts of poly N-methyl pyrrolidone, 1-4 parts of urea, 0.5-1.5 parts of beta-nicotinamide adenine dinucleotide and 201-3 parts of tween. The method for recovering the copper ions in the alkaline etching solution disclosed by the invention can quickly, efficiently and safely realize the recovery of the copper ions in the alkaline etching waste solution, has the advantages of simple recovery process, convenient process operation control, no need of special equipment, low recovery cost, good recovery efficiency and effect and no secondary pollution, and ensures that the recovered copper product has good form and quality through the electrolysis process and the use of additives. Can effectively realize the good combination of economic value, social value and ecological value.
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 recovering copper ions in alkaline etching solution.
Background
In recent years, printed circuit boards are the foundation of the electronic information industry, and advanced technology products are not separated from printed circuit boards. Since the printed circuit board generates a large amount of waste etching solution during the etching process, the waste etching solution contains a large amount of environmentally harmful components such as copper ions and the like. Therefore, the treatment of the waste etching solution is always a problem for enterprises.
The etching solution can be classified into an acidic etching solution and an alkaline etching solution according to its PH. In the alkaline etching solution, the etching effect is generally lowered by the increase of the copper ion concentration, and at this time, the etching solution also loses the etching ability, and the etching solution becomes a waste solution. The etching waste liquid contains a large amount of copper, and if the copper is directly discharged, the resource waste is caused. The current treatment method of the etching waste liquid mainly comprises an acidification method, an alkalization method and a mixing method, wherein the acidification method is to add industrial hydrochloric acid into the etching waste liquid to generate copper hydroxide precipitate, and after filtration and washing, the product is dissolved by sulfuric acid to prepare copper sulfate; the alkalization method is that sodium hydroxide solution is added into the waste liquid, copper is converted into copper oxide precipitate, and copper sulfate is obtained after the copper oxide precipitate is dissolved by sulfuric acid; the mixing method is that acid etching solution is used to neutralize alkaline etching solution to generate basic copper chloride precipitate, the basic copper chloride precipitate is dissolved by concentrated sulfuric acid after separation and washing to obtain copper sulfate, and the copper sulfate crystal can be obtained after cooling and crystallization. The three methods adopt a precipitation method to separate copper, a large amount of reagents are consumed, a large amount of washing wastewater is generated, and the purity of the product cannot be guaranteed.
Patent CN 107354315 a discloses a method for recovering copper from AMOLED alkaline etching waste liquid, comprising the following steps: (1) adding the alkaline etching waste liquid and ammonium diethyldithiocarbamate into a first stirring tank, adding a hydrazine hydrate reducing agent, adding a catalyst, adding an extracting agent into the first stirring tank, uniformly stirring, and standing the solution in the first stirring tank for a period of time after stirring to ensure that the solution in the first stirring tank is automatically layered; (2) adding the layered extractant containing copper ions on the upper layer in the first stirring tank into a second stirring tank, adding a sulfuric acid solution into the second stirring tank for back extraction, stirring the solution in the second stirring tank, and standing the solution in the second stirring tank for a period of time after stirring to automatically layer the solution; (3) and reacting the lower layer solution in the second stirring tank for 20-40min at the reaction temperature of 50-100 ℃, adding into an electrolytic bath for direct current electrolysis to obtain elemental copper, and separating to obtain precipitated copper powder and filtrate. However, the catalyst in step (1) is a composite salt solution formed by mixing a palladium salt solution or a ruthenium salt solution and a nickel salt solution or a cobalt salt solution, which is expensive and brings secondary heavy metal pollution.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for recovering copper ions in alkaline etching liquid, the method can quickly, efficiently and safely recover the copper ions in the alkaline etching waste liquid, the recovery process is simple, the process operation is convenient to control, special equipment is not needed, the recovery cost is low, the recovery efficiency and the recovery effect are good, secondary pollution is avoided, and the form and the quality of the recovered copper product are good through the electrolysis process and the use of additives. Can effectively realize the good combination of economic value, social value and ecological value.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for recovering copper ions in alkaline etching solution is characterized by comprising the following steps:
step S1, multiple extraction processing: adding the alkaline etching waste liquid to be treated into a first extraction tank, and adding a first extraction liquid for primary extraction; then, introducing the mother liquor obtained after the first extraction into a second extraction tank, and adding a second extraction liquid to perform second extraction; finally, the mother liquor after the second extraction is introduced into a third extraction tank, and a third extractant is added for the third extraction;
step S2, stripping treatment: intensively adding the copper-rich extractant obtained through the multiple extraction treatments of S1 into a back extraction tank, and adding a back extractant for back extraction;
step S3, replenishing electrolytic additives: adding an electrolytic additive into the copper-rich liquid obtained by the back extraction treatment in the step S2, and uniformly mixing;
step S4, electrolysis: and (4) inputting the electrolyte obtained in the step (S3) into an electrolytic cell for electrolytic copper extraction.
Preferably, the first extraction liquid is at least one of tributyl phosphate, trioctyl tertiary amine and triisopropyl phosphite.
Preferably, the second extraction liquid is diisooctyl phosphate, 2-ethylhexyl phosphate and guanosine-3 ',5' -cyclic phosphate according to the mass ratio of 1:3 (2-5).
Preferably, the second extractant is any one of a phenolic strongly acidic cation exchange resin, an epoxy strongly acidic cation exchange resin, and a vinylpyridine strongly acidic cation exchange resin.
Preferably, the addition amount of the first extraction liquid in step S1 is 20-30% of the mass of the alkaline waste etching solution.
Preferably, the mass ratio of the mother liquor after the first extraction and the second extraction liquid in the step S1 is (3-5): 1.
Preferably, the mass ratio of the mother liquor after the second extraction to the third extraction agent in the step S1 is (1-2): 1.
Preferably, the stripping agent in step S2 is copper sulfate or sulfuric acid solution with a mass percentage concentration of 10-20%.
Preferably, the mass ratio of the copper-rich extractant to the stripping agent in the step S2 is (2-4): 1.
Preferably, the electrolytic additive in step S3 is prepared from the following components in parts by weight: 3-5 parts of poly N-methyl pyrrolidone, 1-4 parts of urea, 0.5-1.5 parts of beta-nicotinamide adenine dinucleotide and 201-3 parts of tween.
Preferably, the addition amount of the electrolytic additive in the step S3 is 100-200ppm/1L of the copper-rich liquid.
Preferably, the electrolysis current in the step S4 is 30-40A, the temperature is 40-48 ℃, and the time is 15-22 h.
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 recovering copper ions in alkaline etching solution, which can quickly, efficiently and safely recover the copper ions in the alkaline etching waste solution, has simple recovery process, convenient process operation control, no need of special equipment, low recovery cost, good recovery efficiency and effect and no secondary pollution, and ensures that the recovered copper product has good shape and quality through the electrolysis process and the use of additives. Can effectively realize the good combination of economic value, social value and ecological value.
Detailed Description
The following detailed description of preferred embodiments of the invention will be made.
A method for recovering copper ions in alkaline etching solution is characterized by comprising the following steps:
step S1, multiple extraction processing: adding the alkaline etching waste liquid to be treated into a first extraction tank, and adding a first extraction liquid for primary extraction; then, introducing the mother liquor obtained after the first extraction into a second extraction tank, and adding a second extraction liquid to perform second extraction; finally, the mother liquor after the second extraction is introduced into a third extraction tank, and a third extractant is added for the third extraction;
step S2, stripping treatment: intensively adding the copper-rich extractant obtained through the multiple extraction treatments of S1 into a back extraction tank, and adding a back extractant for back extraction;
step S3, replenishing electrolytic additives: adding an electrolytic additive into the copper-rich liquid obtained by the back extraction treatment in the step S2, and uniformly mixing;
step S4, electrolysis: and (4) inputting the electrolyte obtained in the step (S3) into an electrolytic cell for electrolytic copper extraction.
Preferably, the first extraction liquid is at least one of tributyl phosphate, trioctyl tertiary amine and triisopropyl phosphite.
Preferably, the second extraction liquid is diisooctyl phosphate, 2-ethylhexyl phosphate and guanosine-3 ',5' -cyclic phosphate according to the mass ratio of 1:3 (2-5).
Preferably, the second extractant is any one of a phenolic strongly acidic cation exchange resin, an epoxy strongly acidic cation exchange resin, and a vinylpyridine strongly acidic cation exchange resin.
Preferably, the addition amount of the first extraction liquid in step S1 is 20-30% of the mass of the alkaline waste etching solution.
Preferably, the mass ratio of the mother liquor after the first extraction and the second extraction liquid in the step S1 is (3-5): 1.
Preferably, the mass ratio of the mother liquor after the second extraction to the third extraction agent in the step S1 is (1-2): 1.
Preferably, the stripping agent in step S2 is copper sulfate or sulfuric acid solution with a mass percentage concentration of 10-20%.
Preferably, the mass ratio of the copper-rich extractant to the stripping agent in the step S2 is (2-4): 1.
Preferably, the electrolytic additive in step S3 is prepared from the following components in parts by weight: 3-5 parts of poly N-methyl pyrrolidone, 1-4 parts of urea, 0.5-1.5 parts of beta-nicotinamide adenine dinucleotide and 201-3 parts of tween.
Preferably, the addition amount of the electrolytic additive in the step S3 is 100-200ppm/1L of the copper-rich liquid.
Preferably, the electrolysis current in the step S4 is 30-40A, the temperature is 40-48 ℃, and the time is 15-22 h.
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 recovering copper ions in alkaline etching solution, which can quickly, efficiently and safely recover the copper ions in the alkaline etching waste solution, has simple recovery process, convenient process operation control, no need of special equipment, low recovery cost, good recovery efficiency and effect and no secondary pollution, and ensures that the recovered copper product has good shape and quality through the electrolysis process and the use of additives. Can effectively realize the good combination of economic value, social value and ecological value.
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 recovering copper ions in an alkaline etching solution, which is characterized by comprising the following steps:
step S1, multiple extraction processing: adding the alkaline etching waste liquid to be treated into a first extraction tank, and adding a first extraction liquid for primary extraction; then, introducing the mother liquor obtained after the first extraction into a second extraction tank, and adding a second extraction liquid to perform second extraction; finally, the mother liquor after the second extraction is introduced into a third extraction tank, and a third extractant is added for the third extraction;
step S2, stripping treatment: intensively adding the copper-rich extractant obtained through the multiple extraction treatments of S1 into a back extraction tank, and adding a back extractant for back extraction;
step S3, replenishing electrolytic additives: adding an electrolytic additive into the copper-rich liquid obtained by the back extraction treatment in the step S2, and uniformly mixing;
step S4, electrolysis: and (4) inputting the electrolyte obtained in the step (S3) into an electrolytic cell for electrolytic copper extraction.
The first extraction liquid is tributyl phosphate; the second extract liquid is diisooctyl phosphate, 2-ethylhexyl 2-ethyl hexyl phosphate and guanosine-3 ',5' -cyclic phosphate according to the mass ratio of 1:3: 2; the second extractant is phenolic aldehyde strong-acid cation exchange resin.
In the step S1, the addition amount of the first extraction liquid is 20% of the mass of the alkaline etching waste liquid; the mass ratio of the mother liquor after the first extraction to the second extraction liquid in the step S1 is 3: 1; the mass ratio of the mother liquor after the second extraction to the third extracting agent in the step S1 is 1: 1.
In the step S2, the stripping agent is copper sulfate or sulfuric acid solution with the mass percentage concentration of 10%; the mass ratio of the copper-rich extractant to the stripping agent in the step S2 is 2: 1.
The electrolytic additive in the step S3 is prepared from the following components in parts by weight: 3 parts of poly-N-methyl pyrrolidone, 1 part of urea, 0.5 part of beta-nicotinamide adenine dinucleotide and 201 parts of tween.
In the step S3, the additive amount of the electrolytic additive is 100ppm/1L of the copper-rich liquid.
In step S4, the electrolysis current is 30A, the temperature is 40 ℃, and the time is 15 h.
Example 2
Embodiment 2 provides a method for recovering copper ions from an alkaline etching solution, which is substantially the same as embodiment 1, except that the first extraction solution in step S1 is trioctyl tertiary amine; the second extract is 2-ethylhexyl phosphate 2-ethylhexyl ester; the second extractant is epoxy strong-acid cation exchange resin; the electrolytic additive in the step S3 is prepared from the following components in parts by weight: 3.5 parts of poly-N-methyl pyrrolidone, 2 parts of urea, 0.7 part of beta-nicotinamide adenine dinucleotide and 201.5 parts of tween.
Example 3
Example 3 provides a method for recovering copper ions from an alkaline etching solution, which is substantially the same as example 1, except that the first extract in step S1 is triisopropyl phosphite; the second extract liquid is diisooctyl phosphate, 2-ethylhexyl 2-ethyl hexyl phosphate and guanosine-3 ',5' -cyclic phosphate according to the mass ratio of 1:3: 3; the second extractant is vinylpyridine strong-acid cation exchange resin; the electrolytic additive in the step S3 is prepared from the following components in parts by weight: 4 parts of poly-N-methyl pyrrolidone, 2.5 parts of urea, 1 part of beta-nicotinamide adenine dinucleotide and 202 parts of tween.
Example 4
Example 4 provides a method for recovering copper ions from an alkaline etching solution, which is substantially the same as example 1, except that the first extraction solution in step S1 is prepared by mixing tributyl phosphate, trioctyl tertiary amine, and triisopropyl phosphite in a mass ratio of 1:2: 3; the second extract liquid is diisooctyl phosphate, 2-ethylhexyl 2-ethyl hexyl phosphate and guanosine-3 ',5' -cyclic phosphate according to the mass ratio of 1:3: 4.5; the second extractant is phenolic aldehyde strong-acid cation exchange resin; the electrolytic additive in the step S3 is prepared from the following components in parts by weight: 4.5 parts of poly-N-methyl pyrrolidone, 3.5 parts of urea, 1.4 parts of beta-nicotinamide adenine dinucleotide and 202.5 parts of tween.
Example 5
Embodiment 5 provides a method for recovering copper ions from an alkaline etching solution, which is substantially the same as embodiment 1, except that the first extraction solution in step S1 is trioctyl tertiary amine; the second extract liquid is diisooctyl phosphate, 2-ethylhexyl 2-ethyl hexyl phosphate and guanosine-3 ',5' -cyclic phosphate according to the mass ratio of 1:3: 5; the second extractant is phenolic aldehyde strong-acid cation exchange resin; the electrolytic additive in the step S3 is prepared from the following components in parts by weight: 5 parts of poly-N-methyl pyrrolidone, 4 parts of urea, 1.5 parts of beta-nicotinamide adenine dinucleotide and 203 parts of tween.
Comparative example 1
Comparative example 1 provides a method for recovering copper ions in an alkaline etching solution, which is substantially the same as example 1 except that only the first extraction operation is performed in step S1.
Comparative example 2
Comparative example 2 provides a method for recovering copper ions from an alkaline etching solution, which is substantially the same as example 1, except that only the first extraction and the second extraction are performed in step S1.
Comparative example 3
Comparative example 3 provides a method for recovering copper ions in an alkaline etching solution, which is substantially the same as example 1 except that poly-N-methylpyrrolidone is not included in the electrolytic additive.
Comparative example 4
Comparative example 4 provides a method for recovering copper ions in an alkaline etching solution, which is substantially the same as in example 1 except that β -nicotinamide adenine dinucleotide is not included in the electrolytic additive.
Comparative example 5
Comparative example 5 provides a method for recovering copper ions in an alkaline etching solution, which is substantially the same as example 1 except that urea is not included in the electrolytic additive.
To further illustrate the beneficial technical effects of the embodiments, the copper ions in the same alkaline etching solution (copper concentration of 7000mg/L) were recovered according to the method of each example, and the copper ion removal rate was measured and calculated. The test results are shown in Table 1.
TABLE 1
As can be seen from the above table, the method for recovering copper ions in alkaline etching solution according to the embodiment of the present invention has better recovery effect, which is the result of the synergistic effect of each additive 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 (10)
1. A method for recovering copper ions in alkaline etching solution is characterized by comprising the following steps:
step S1, multiple extraction processing: adding the alkaline etching waste liquid to be treated into a first extraction tank, and adding a first extraction liquid for primary extraction; then, introducing the mother liquor obtained after the first extraction into a second extraction tank, and adding a second extraction liquid to perform second extraction; finally, the mother liquor after the second extraction is introduced into a third extraction tank, and a third extractant is added for the third extraction;
step S2, stripping treatment: intensively adding the copper-rich extractant obtained through the multiple extraction treatments of S1 into a back extraction tank, and adding a back extractant for back extraction;
step S3, replenishing electrolytic additives: adding an electrolytic additive into the copper-rich liquid obtained by the back extraction treatment in the step S2, and uniformly mixing;
step S4, electrolysis: and (4) inputting the electrolyte obtained in the step (S3) into an electrolytic cell for electrolytic copper extraction.
2. The method as claimed in claim 1, wherein the first extraction liquid is at least one of tributyl phosphate, trioctyl tertiary amine, and triisopropyl phosphite.
3. The method as claimed in claim 1, wherein the second extraction liquid is diisooctyl phosphate, 2-ethylhexyl phosphate, and guanosine-3 ',5' -cyclic phosphate at a mass ratio of 1:3 (2-5).
4. The method according to claim 1, wherein the second extractant is any one of a phenolic strongly acidic cation exchange resin, an epoxy strongly acidic cation exchange resin, and a vinylpyridine strongly acidic cation exchange resin.
5. The method for recovering copper ions in alkaline etching solution according to claim 1, wherein the addition amount of the first extraction liquid in step S1 is 20-30% of the mass of the alkaline etching waste solution; the mass ratio of the mother liquor after the first extraction to the second extraction liquid in the step S1 is (3-5) to 1; the mass ratio of the mother liquor after the second extraction to the third extracting agent in the step S1 is (1-2): 1.
6. The method as claimed in claim 1, wherein the stripping agent in step S2 is copper sulfate or sulfuric acid solution with a concentration of 10-20% by weight.
7. The method according to claim 1, wherein the mass ratio of the copper-rich extractant to the stripping agent in step S2 is (2-4): 1.
8. The method as claimed in claim 1, wherein the electrolytic additive in step S3 comprises the following components in parts by weight: 3-5 parts of poly N-methyl pyrrolidone, 1-4 parts of urea, 0.5-1.5 parts of beta-nicotinamide adenine dinucleotide and 201-3 parts of tween.
9. The method as claimed in claim 1, wherein the amount of the electrolytic additive added in step S3 is 100-200ppm/1L copper-rich solution.
10. The method according to any one of claims 1 to 9, wherein the electrolysis current in step S4 is 30-40A, 40-48 ℃ and 15-22 h.
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| CN117945451A (en) * | 2024-03-26 | 2024-04-30 | 江苏泰禾金属工业有限公司 | Method for preparing cuprous oxide from copper-containing acidic etching solution |
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Application publication date: 20210409 |