CN116004990A - Method for recycling copper and gold from waste mobile phone circuit board - Google Patents
Method for recycling copper and gold from waste mobile phone circuit board Download PDFInfo
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- CN116004990A CN116004990A CN202310133734.6A CN202310133734A CN116004990A CN 116004990 A CN116004990 A CN 116004990A CN 202310133734 A CN202310133734 A CN 202310133734A CN 116004990 A CN116004990 A CN 116004990A
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- 229910052737 gold Inorganic materials 0.000 title claims abstract description 128
- 239000010931 gold Substances 0.000 title claims abstract description 128
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 116
- 239000010949 copper Substances 0.000 title claims abstract description 88
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 87
- 239000002699 waste material Substances 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 62
- 238000004064 recycling Methods 0.000 title claims abstract description 19
- 238000002386 leaching Methods 0.000 claims abstract description 105
- 239000000843 powder Substances 0.000 claims abstract description 47
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims abstract description 40
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 40
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims abstract description 40
- 238000000498 ball milling Methods 0.000 claims abstract description 32
- 239000007787 solid Substances 0.000 claims abstract description 28
- 239000011780 sodium chloride Substances 0.000 claims abstract description 20
- 239000000654 additive Substances 0.000 claims abstract description 18
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- -1 gold ions Chemical class 0.000 claims abstract description 12
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001431 copper ion Inorganic materials 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 52
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 30
- 235000006408 oxalic acid Nutrition 0.000 claims description 10
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 9
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000012074 organic phase Substances 0.000 claims description 6
- 238000005868 electrolysis reaction Methods 0.000 claims description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 description 24
- 238000000227 grinding Methods 0.000 description 17
- 229910052751 metal Inorganic materials 0.000 description 16
- 239000002184 metal Substances 0.000 description 16
- 230000008569 process Effects 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 230000035484 reaction time Effects 0.000 description 15
- 239000010439 graphite Substances 0.000 description 13
- 229910002804 graphite Inorganic materials 0.000 description 13
- 238000012360 testing method Methods 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 10
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- 238000002474 experimental method Methods 0.000 description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 6
- 238000005192 partition Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000003828 vacuum filtration Methods 0.000 description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 238000004070 electrodeposition Methods 0.000 description 5
- 239000010793 electronic waste Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000002608 ionic liquid Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000005749 Copper compound Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001880 copper compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
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- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000009853 pyrometallurgy Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
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- 238000002848 electrochemical method Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003353 gold alloy Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 239000012433 hydrogen halide Substances 0.000 description 1
- 229910000039 hydrogen halide Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
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- 229920005989 resin Polymers 0.000 description 1
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- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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Images
Classifications
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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
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Abstract
The invention discloses a method for recovering copper and gold from a waste mobile phone circuit board, which is characterized by comprising the following steps: crushing the waste mobile phone circuit board to obtain waste mobile phone circuit board powder; mechanically ball milling sodium persulfate, an additive I and waste mobile phone circuit board powder to obtain solid powder; reacting the solid powder with water to obtain a copper-containing leaching solution and gold-containing filter residues; extracting copper ions in the copper-containing leaching solution to obtain copper; reacting the gold-containing filter residues with a liquid containing sodium persulfate and sodium chloride to obtain a gold-containing leaching solution; extracting gold ions in the gold-containing leaching solution to obtain gold; wherein the additive I is one or more of iron powder, zinc powder and aluminum powder. The method is environment-friendly, clean and efficient, and is beneficial to further reducing the risk of environmental pollution and efficiently recycling copper and gold in the waste mobile phone circuit board powder.
Description
Technical Field
The invention belongs to the technical field of electronic waste treatment and recycling, and particularly relates to a method for recycling copper and gold from a waste mobile phone circuit board.
Background
With the occurrence of problems such as shortage of natural mineral resources, environmental pollution, ecological destruction, etc., recycling of urban mineral resources has gradually attracted widespread attention worldwide. Electronic waste, which is one of the main sources of urban mineral products, has important resource value and contains a large amount of recyclable metals (such as gold, silver, copper, etc.). Currently, electronic waste has become one of the fastest growing waste species worldwide. Among all kinds, discarding mobile phones has become the most common electronic waste. The production of waste mobile phones is increasing dramatically due to the short life of the product and the large yield. In 2015 and 2017, the number of abandoned mobile phones in China reaches 7.8 and 8 hundred million parts respectively. It was estimated that by 2025, the number of chinese obsolete handsets would increase to 9.37 billion parts, respectively.
The circuit board is an important component of the abandoned mobile phone, and complex, valuable and harmful components of the circuit board have very remarkable environmental attributes and resource attributes, and are attracting wide attention. Copper usage amounts vary from 6 grams to 23 grams per cell phone circuit board, while gold usage amounts to about 0.03 grams. Taking gold as an example, the grade of gold in the waste mobile phone circuit board is more than 4 times of that of common gold concentrate, and the waste mobile phone circuit board has high recovery value. The research shows that the circuit board of the 1 ton abandoned mobile phone contains 0.86-1.6 kg of gold, 0.14-5.8 kg of silver and 259-550 kg of copper, and the gold recovered from the abandoned mobile phone can meet the gold requirement of nearly 10% of the global electronic manufacturing industry. Meanwhile, when gold, silver and copper of the same quality are produced, the original mining cost is almost 7 times that of the recovery cost of the abandoned mobile phone circuit board. In addition, in the aspect of energy conservation and emission reduction, the recovery and reuse of the metal resources in the waste mobile phone circuit board can save energy and resource consumption in the primary metal production process, and simultaneously can reduce the emission of waste water, waste gas and waste residues in metal ore exploitation. However, waste cell phone circuit boards also contain nickel, cadmium, lead, brominated flame retardants and other hazardous materials. Therefore, if the waste mobile phone circuit board is handled and disposed of in a non-environmentally friendly manner, environmental pollution and health risks may be caused. Therefore, from the multiple viewpoints of resource recovery, environmental protection, economy, health, and the like, it is necessary to realize resource recovery of the waste mobile phone circuit board.
At present, the recovery method of the waste mobile phone circuit board metal (especially noble metal) mainly comprises the following steps: pyrometallurgy, hydrometallurgy, biometallurgy, and mechanochysical methods. Currently, in china, most normal recycling enterprises use mechanical physical sorting processes to process circuit boards of large-sized waste home appliances (televisions, refrigerators and air conditioners). However, this method is not suitable for the waste mobile phone circuit board with complex structural components, various kinds, small volume and high noble metal content. Pyrometallurgical processes are a technique for the large-scale recovery of circuit boards, which processes have been operated essentially in many global recovery enterprises (such as the Umicore in Belgium). However, the waste circuit boards are relatively large non-metallic materials, and contain toxic and harmful substances such as brominated flame retardants, thermosetting resins, reinforcing agents and the like, and the substances easily generate a large amount of harmful gases such as dioxin, hydrogen halide and the like in the high-temperature combustion process, so that serious environmental and health problems are caused. The leaching process of the biological metallurgy process has the advantages of environmental protection and high cost effectiveness, however, the process has high leaching environment requirement and low leaching efficiency, and still needs to be studied intensively. Among these methods, hydrometallurgical processes have the advantages of good stability, low cost, high leaching efficiency, less environmental pollution, and the like. The wet metallurgy recovery process principle of the waste mobile phone circuit board is that a leaching agent is adopted to dissolve metal in the waste mobile phone circuit board, and then metal ions in the solution are separated and recovered. The acid leaching process is currently the most common chemical method. However, the acid leaching process has the defects of slow leaching process speed, long production period, large consumption of chemical reagents and larger potential safety hazard, and simultaneously, a large amount of waste water and waste gas are easy to generate in the process operation process, so that secondary pollution is caused.
Therefore, a green process for recycling copper and gold in a waste mobile phone circuit board is still needed urgently, the environment load is reduced to the minimum extent while metal resources are recovered to the maximum extent, and a new idea is provided for efficient and sustainable recycling of copper and gold in electronic wastes.
Disclosure of Invention
The invention aims to solve at least one of the technical problems existing in the prior art to a certain extent, and therefore, the invention provides a method for recycling copper and gold from a waste mobile phone circuit board.
The method is characterized in that sodium persulfate is adopted to recover copper and gold in the waste mobile phone circuit board step by step. The first step of the method is to mechanically ball mill the waste mobile phone circuit board powder, sodium persulfate and additive I, oxidize metal zero-valent copper into bivalent copper compound, separate the bivalent copper compound from the waste mobile phone circuit board by water immersion, and obtain the copper simple substance product by electrochemical method. And the second step is to add the rest of waste mobile phone circuit board powder (gold-containing filter residues) into ionic liquid containing sodium persulfate and sodium chloride for reaction, and the leaching rate of gold in the waste mobile phone circuit board powder is improved due to the fact that the solid powder sample is activated by the previous mechanical ball milling. Finally, obtaining a gold simple substance product through extraction and reduction processes. The method is suitable for recycling copper and gold in the waste mobile phone circuit board, and can achieve the purpose of recycling resources.
According to one aspect of the present invention, there is provided a method for recovering copper and gold from a waste mobile phone circuit board, comprising the steps of: crushing the waste mobile phone circuit board to obtain waste mobile phone circuit board powder; mechanically ball milling sodium persulfate, an additive I and the waste mobile phone circuit board powder to obtain solid powder; reacting the solid powder with water to obtain a copper-containing leaching solution and gold-containing filter residues; extracting copper ions in the copper-containing leaching solution to obtain copper; reacting the gold-containing filter residue with a liquid containing sodium persulfate and sodium chloride to obtain a gold-containing leaching solution, wherein the concentration of the sodium persulfate is 0.5-1.5mol/L, the concentration of the sodium chloride is 0.5-3.0mol/L, the reaction time of the gold-containing filter residue and the liquid containing the sodium persulfate and the sodium chloride is 1.0-2.5h, and the reaction temperature is 50-75 ℃; extracting gold ions in the gold-containing leaching solution to obtain gold; wherein the additive I is one or more of iron powder, zinc powder and aluminum powder.
Preferably, the waste mobile phone circuit board is crushed to a particle size of 0.1-0.5mm.
Preferably, the ball milling time is 2-6h, the ball-material ratio is 40:1-80:1, and the ball milling rotating speed is 350-550 rpm.
Preferably, the solid powder is reacted with water for 1-15min with a solid-to-liquid ratio of 1:100kg/L.
Preferably, the copper-containing leachate is electrolyzed to deposit the copper at a cathode electrode.
Preferably, the electrolysis voltage is 5-7V and the electrolysis time is 15-60min.
Preferably, extracting gold ions in the gold-containing leaching solution to obtain gold, comprising the following steps: reacting the gold-containing leaching solution with methyl isobutyl ketone to obtain a gold-carrying organic phase; and (3) reacting the gold-carrying organic phase with oxalic acid to obtain the gold.
The invention provides a method for recycling copper and gold from a waste mobile phone circuit board. The method comprises the steps of taking sodium persulfate and an additive I as grinding aids, effectively recycling copper in waste mobile phone circuit board powder through a mechanical ball milling method, and effectively recycling gold in waste mobile phone circuit board powder through an ionic liquid system of sodium sulfate and sodium chloride. Compared with the prior art, the method avoids the use of corrosive leaches such as strong acid, strong alkali and the like, has low equipment requirements, is safe in recovery process and has no secondary pollution. Meanwhile, the sodium persulfate and the additive adopted by the invention have low price, and are very convenient for popularization and industrialized application. In addition, by improving the recovery process flow and the operation parameter conditions, the invention greatly shortens the reaction time, reduces the energy consumption and reduces the carbon emission. In general, the method is environment-friendly, clean and efficient, and is beneficial to further reducing the risk of environmental pollution and efficiently recycling copper and gold in the waste mobile phone circuit board powder.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiments of the invention and together with the description serve to explain the invention and do not constitute a limitation on the invention. In the drawings:
FIG. 1 is a flow chart of a method for recovering copper and gold from a waste cell phone circuit board according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of mechanical ball milling of sodium persulfate, additive I and waste cell phone circuit board powder according to an embodiment of the invention;
FIG. 3 is a schematic illustration of copper leaching and recovery from a solid powder according to an embodiment of the present invention;
FIG. 4 is a schematic illustration of gold leaching from a gold-containing filter residue according to an embodiment of the present invention;
FIG. 5 is a graph showing the variation of solid powder samples before and after the reaction according to an embodiment of the present invention; and
fig. 6 is a state diagram of copper and gold recovered from a discarded phone circuit board according to an embodiment of the invention.
Detailed Description
The examples set forth below are presented to provide those skilled in the art with a more clear understanding of the present invention. The following examples are not intended to limit the scope of the invention, but are merely illustrative examples. The starting materials, reagents or apparatus mentioned in the examples below are all available commercially, or are obtained by known existing means, unless otherwise specified.
The embodiment of the invention provides a method for recycling copper and gold from a waste mobile phone circuit board. FIG. 1 is a flowchart of a method for recovering copper and gold from a waste cell phone circuit board according to an embodiment of the present invention, and the method for recovering copper and gold from a waste cell phone circuit board is described in detail with reference to FIG. 1, and includes the steps of: crushing the waste mobile phone circuit board to obtain waste mobile phone circuit board powder, and putting the crushed circuit board with the particle size of 0.1-0.5mm into a ball milling tank for mechanical ball milling; mechanically ball-milling sodium persulfate, an additive I and waste mobile phone circuit board powder to obtain solid powder, wherein zirconia is used as a mechanically ball-milled grinding ball, the ball-to-material ratio is 40:1-80:1, the mass ratio of the waste mobile phone circuit board to grinding aid (sodium persulfate and additive I) is 1:2-1:5, the additive I is one or more of iron powder, zinc powder and aluminum powder, and in addition, the mechanical ball milling is carried out at a rotating speed of 350rpm-550rpm. Adding a proper amount of pure water into the ground solid powder (reaction product) to carry out leaching reaction, wherein the time of the leaching reaction is 5-15min, the solid-liquid ratio of the solid powder to the pure water is 1:100kg/L, and after the reaction is finished, obtaining copper-containing leaching liquid and gold-containing filter residues.
Adding gold-containing filter residues into ionic liquid containing sodium persulfate and sodium chloride for leaching reaction, wherein the concentration of the sodium persulfate is 0.5-1.5mol/L, the concentration of the sodium chloride is 0.5-3mol/L, the reaction time is 1.0h-2.5h, the reaction temperature is 50-75 ℃, and after the reaction is finished, filtering, collecting filtrate and washing the filter residues to obtain the gold-containing leaching solution.
Reducing gold ions in the gold-containing leaching solution into solid gold by an extraction and reduction method, specifically, reacting the gold-containing leaching solution with methyl isobutyl ketone to obtain a gold-carrying organic phase; the gold-carrying organic phase is further reacted with oxalic acid to obtain gold, wherein the concentration of the oxalic acid is 15%.
The method comprises the steps of placing an electrode into a copper-containing leaching solution, externally connecting direct current, carrying out electrodeposition reaction of copper at room temperature, recovering copper precipitated from a cathode after the electrodeposition reaction is finished, collecting electrolyte, and continuously carrying out electrodeposition reaction on the copper-containing leaching solution and the collected electrolyte, so that efficient recovery of copper in a waste mobile phone circuit board is realized, wherein the voltage of the electrodeposition reaction of copper is 5-7V, the electrodeposition time of copper is 15-60min, and the electrodeposited electrode is a platinum electrode (anode) and a graphite electrode (cathode).
Compared with the prior art, the invention has the following advantages:
(1) Gold and copper are the two elements with highest recovery value in the waste mobile phone circuit board. However, the development of the prior art has focused more on how to recover a single metal. According to the invention, sodium persulfate and the additive I are used as grinding aids, sodium persulfate and sodium chloride are used as ion reaction systems, and a process for recovering copper and gold of the waste mobile phone circuit board step by step is developed, so that copper and gold in the waste mobile phone circuit board powder can be effectively recovered at the same time.
(2) The invention avoids the use of corrosive reagents such as strong acid or strong alkali, does not generate toxic substances in the leaching process, and has safe recovery process and no secondary pollution. In addition, the method has the advantages of simple process flow and low requirement on equipment, and the leaching and recovery of copper can be synchronously carried out, thereby being beneficial to improving the recovery efficiency.
(3) The sodium persulfate and the additive adopted by the invention have low price and stable chemical properties, and are very suitable for popularization and industrialized application.
(4) By controlling the recovery process flow and the operation parameter conditions, the invention takes sodium persulfate and the additive I as grinding aids, and the copper in the waste mobile phone circuit board powder is recovered cleanly and efficiently through mechanochemical reaction and water immersion reaction. Meanwhile, the mechanochemical reaction can also provide mechanical activating force for the subsequent leaching of gold in the waste mobile phone circuit board powder, greatly shortens the reaction time of gold in a sodium persulfate and sodium chloride ion system, is beneficial to reducing the energy consumption of the whole process and finally realizes carbon emission reduction.
Example 1
And (3) putting the waste mobile phone circuit board into a Chinese manufacturing DFT-200 crusher for crushing, selecting waste mobile phone circuit board powder with the particle size of 0.1-0.5mm as an experimental object, taking three groups of parallel samples for digestion, and performing ICP detection to obtain the table 1.
TABLE 1 Metal content of waste Mobile phone circuit board powder (unit: kg/t)
| Category(s) | Gold alloy | Copper (Cu) | Iron (Fe) | Nickel (Ni) | Tin (Sn) | Lead |
| 1 | 0.10 | 310.81 | 1.98 | 5.30 | 6.61 | 5.60 |
| 2 | 0.12 | 291.24 | 2.51 | 5.45 | 7.04 | 5.26 |
| 3 | 0.08 | 282.98 | 2.33 | 5.69 | 6.57 | 6.90 |
| Average value of | 0.10 | 295.01 | 2.27 | 5.48 | 6.74 | 5.92 |
Recovering copper: the crushed waste mobile phone circuit board powder and grinding aid (only sodium persulfate and no additive I) are put into a ball milling tank according to the mass ratio of 1:3 for mechanochemical reaction, zirconium oxide is used as a grinding ball for mechanical ball milling, the ball-material ratio is 80:1, the rotating speed of the ball mill is 550rpm, and the reaction time is 4 hours. After the ball milling reaction is finished, the reaction product is filled into a filter bag and is put into a leaching zone of a self-made double-layer reaction tank with a baffle plate, and 100ml of pure water is added for leaching reaction. And after the leaching reaction is finished, taking the filter bag away to obtain gold-containing filter residues, and opening the partition plate to enable the copper-containing leaching solution to flow into the recovery area of the double-layer reaction tank completely to obtain the copper-containing leaching solution. The test shows that the leaching rate of copper is 88.45%, and meanwhile, the leaching rate of gold is about 0.02%. Then, copper ions in the leaching solution are precipitated at the cathode graphite electrode through electrochemical reaction. And after the experiment is finished, recovering the metal copper precipitated by the graphite electrode.
Recovering gold: the gold-containing filter residue is placed in 1mol/L sodium persulfate solution according to a liquid-solid ratio of 20L/kg, 0.5mol/L sodium chloride is added, the stirring speed is 500rpm, the constant temperature is kept at 60 ℃, and the reaction time is 2 hours. After the reaction is finished, obtaining leaching liquid containing gold through vacuum filtration. Through testing, the leaching rate of gold reaches 84.17 percent. Subsequently, methyl isobutyl ketone is used as an extracting agent, oxalic acid is used as a reducing agent, and gold ions in the leaching solution are reduced into solid metallic gold through extraction and reduction methods.
Example 2
And (3) putting the waste mobile phone circuit board into a Chinese manufacturing DFT-200 crusher for crushing, selecting waste mobile phone circuit board powder with the particle size of 0.1-0.5mm as an experimental object, taking three groups of parallel samples for digestion, and performing ICP detection to obtain the table 1.
Recovering copper: the crushed waste mobile phone circuit board powder and grinding aid (sodium persulfate only, additive I-small amount of iron powder) are put into a ball milling tank according to the mass ratio of 1:3 for mechanochemical reaction, zirconium oxide is used as grinding balls for mechanical ball milling, the ball-material ratio is 80:1, the rotating speed of the ball mill is 550rpm, and the reaction time is 4 hours. After the ball milling reaction is finished, the reaction product is filled into a filter bag and is put into a leaching zone of a self-made double-layer reaction tank with a baffle plate, and 100ml of pure water is added for leaching reaction. And after the leaching reaction is finished, taking the filter bag away to obtain gold-containing filter residues, and opening the partition plate to enable the copper-containing leaching solution to flow into the recovery area of the double-layer reaction tank completely to obtain the copper-containing leaching solution. The copper leaching rate was 98.60% and the gold leaching rate was about 0.02% by testing. Then, copper ions in the leaching solution are precipitated at the cathode graphite electrode through electrochemical reaction. And after the experiment is finished, recovering the metal copper precipitated by the graphite electrode.
Recovering gold: the gold-containing filter residue is placed in 1mol/L sodium persulfate solution according to a liquid-solid ratio of 20L/kg, the stirring speed is 500rpm, the constant temperature is kept at 60 ℃, and the reaction time is 2 hours. After the reaction is finished, obtaining leaching liquid containing gold through vacuum filtration. Through tests, the leaching rate of gold can only reach about 5%. Subsequently, methyl isobutyl ketone is used as an extracting agent, oxalic acid is used as a reducing agent, and gold ions in the leaching solution are reduced into solid metallic gold through extraction and reduction methods.
Example 3
And (3) putting the waste mobile phone circuit board into a Chinese manufacturing DFT-200 crusher for crushing, selecting waste mobile phone circuit board powder with the particle size of 0.1-0.5mm as an experimental object, taking three groups of parallel samples for digestion, and performing ICP detection to obtain the table 1.
Recovering copper: the crushed waste mobile phone circuit board powder and grinding aid (sodium persulfate and a small amount of iron powder) are put into a ball milling tank according to the mass ratio of 1:5 to carry out mechanochemical reaction, zirconium oxide is used as a grinding ball for mechanical ball milling, the ball-material ratio is 40:1, the rotating speed of the ball mill is 350rpm, and the reaction time is 2 hours. After the ball milling reaction is finished, the reaction product is filled into a filter bag and is put into a leaching zone of a self-made double-layer reaction tank with a baffle plate, and 100ml of pure water is added for leaching reaction. And after the leaching reaction is finished, taking the filter bag away to obtain gold-containing filter residues, and opening the partition plate to enable the copper-containing leaching solution to flow into the recovery area of the double-layer reaction tank completely to obtain the copper-containing leaching solution. The test shows that the leaching rate of copper is 98.89%, and meanwhile, the leaching rate of gold is about 0.02%. Then, copper ions in the leaching solution are precipitated at the cathode graphite electrode through electrochemical reaction. And after the experiment is finished, recovering the metal copper precipitated by the graphite electrode.
Recovering gold: the gold-containing filter residue is placed in 1.5mol/L sodium persulfate solution according to a liquid-solid ratio of 50L/kg, 2.5mol/L sodium chloride is added, the stirring speed is 300rpm, the constant temperature is kept at 75 ℃, and the reaction time is 1h. After the reaction is finished, obtaining leaching liquid containing gold through vacuum filtration. Through testing, the leaching rate of gold reaches 96.21 percent. Subsequently, methyl isobutyl ketone is used as an extracting agent, oxalic acid is used as a reducing agent, and gold ions in the leaching solution are reduced into solid metallic gold through extraction and reduction methods.
Example 4
And (3) putting the waste mobile phone circuit board into a Chinese manufacturing DFT-200 crusher for crushing, selecting waste mobile phone circuit board powder with the particle size of 0.1-0.5mm as an experimental object, taking three groups of parallel samples for digestion, and performing ICP detection to obtain the table 1.
Recovering copper: the crushed waste mobile phone circuit board powder and grinding aid (sodium persulfate and a small amount of zinc powder) are put into a ball milling tank according to the mass ratio of 1:4 to carry out mechanochemical reaction, zirconium oxide is used as grinding balls for mechanical ball milling, the ball material ratio is 60:1, the rotating speed of the ball mill is 450rpm, and the reaction time is 6 hours. After the ball milling reaction is finished, the reaction product is filled into a filter bag and is put into a leaching zone of a self-made double-layer reaction tank with a baffle plate, and 100ml of pure water is added for leaching reaction. And after the leaching reaction is finished, taking the filter bag away to obtain gold-containing filter residues, and opening the partition plate to enable the copper-containing leaching solution to flow into the recovery area of the double-layer reaction tank completely to obtain the copper-containing leaching solution. The test shows that the leaching rate of copper is 98.54%, and meanwhile, the leaching rate of gold is about 0.02%. Then, copper ions in the leaching solution are precipitated at the cathode graphite electrode through electrochemical reaction. And after the experiment is finished, recovering the metal copper precipitated by the graphite electrode.
Recovering gold: the gold-containing filter residue is placed into 0.5mol/L sodium persulfate solution according to 25L/kg of liquid solid, 1mol/L sodium chloride is added, the stirring speed is 400rpm, the constant temperature is kept at 50 ℃, and the reaction time is 1.5h. After the reaction is finished, obtaining leaching liquid containing gold through vacuum filtration. Through testing, the leaching rate of gold reaches 79.76%. Subsequently, methyl isobutyl ketone is used as an extracting agent, oxalic acid is used as a reducing agent, and gold ions in the leaching solution are reduced into solid metallic gold through extraction and reduction methods.
Example 5
And (3) putting the waste mobile phone circuit board into a Chinese manufacturing DFT-200 crusher for crushing, selecting waste mobile phone circuit board powder with the particle size of 0.1-0.5mm as an experimental object, taking three groups of parallel samples for digestion, and performing ICP detection to obtain the table 1.
Recovering copper: the crushed waste mobile phone circuit board powder and grinding aid (sodium persulfate and a small amount of aluminum powder) are put into a ball milling tank according to the mass ratio of 1:2 to carry out mechanochemical reaction, zirconium oxide is used as a grinding ball for mechanical ball milling, the ball-material ratio is 80:1, the rotating speed of the ball mill is 550rpm, and the reaction time is 5 hours. After the ball milling reaction is finished, the reaction product is filled into a filter bag and is put into a leaching zone of a self-made double-layer reaction tank with a baffle plate, and 100ml of pure water is added for leaching reaction. And after the leaching reaction is finished, taking the filter bag away to obtain gold-containing filter residues, and opening the partition plate to enable the copper-containing leaching solution to flow into the recovery area of the double-layer reaction tank completely to obtain the copper-containing leaching solution. The copper leaching rate was 97.04% and the gold leaching rate was about 0.02% by testing. Then, copper ions in the leaching solution are precipitated at the cathode graphite electrode through electrochemical reaction. And after the experiment is finished, recovering the metal copper precipitated by the graphite electrode.
Recovering gold: the gold-containing filter residue is placed in 0.5mol/L sodium persulfate solution according to a liquid-solid ratio of 20L/kg, sodium chloride of 2mol/L is added, the stirring speed is 700rpm, the constant temperature is kept at 70 ℃, and the reaction time is 2 hours. After the reaction is finished, obtaining leaching liquid containing gold through vacuum filtration. Through testing, the leaching rate of gold reaches 95.45 percent. Subsequently, methyl isobutyl ketone is used as an extracting agent, oxalic acid is used as a reducing agent, and gold ions in the leaching solution are reduced into solid metallic gold through extraction and reduction methods.
Example 6
And (3) putting the waste mobile phone circuit board into a Chinese manufacturing DFT-200 crusher for crushing, selecting waste mobile phone circuit board powder with the particle size of 0.1-0.5mm as an experimental object, taking three groups of parallel samples for digestion, and performing ICP detection to obtain the table 1.
Recovering copper: the crushed waste mobile phone circuit board powder and grinding aid (sodium persulfate, iron powder and zinc powder) are put into a ball milling tank according to the mass ratio of 1:3 to carry out mechanochemical reaction, zirconium oxide is used as grinding balls for mechanical ball milling, the ball material ratio is 80:1, the rotating speed of the ball mill is 550rpm, and the reaction time is 4 hours. After the ball milling reaction is finished, the reaction product is filled into a filter bag and is put into a leaching zone of a self-made double-layer reaction tank with a baffle plate, and 100ml of pure water is added for leaching reaction. And after the leaching reaction is finished, taking the filter bag away to obtain gold-containing filter residues, and opening the partition plate to enable the copper-containing leaching solution to flow into the recovery area of the double-layer reaction tank completely to obtain the copper-containing leaching solution. The test shows that the leaching rate of copper is 99.98%, and meanwhile, the leaching rate of gold is about 0.02%. Then, copper ions in the leaching solution are precipitated at the cathode graphite electrode through electrochemical reaction. And after the experiment is finished, recovering the metal copper precipitated by the graphite electrode.
Recovering gold: and (3) placing 50L/kg of the gold-containing filter residue in the step (2) into 1.5mol/L of sodium persulfate solution according to the liquid-solid state, adding 3mol/L of sodium chloride, stirring at the speed of 700rpm, and keeping the constant temperature of 65 ℃ for 2.5 hours. After the reaction is finished, obtaining leaching liquid containing gold through vacuum filtration. Through testing, the leaching rate of gold reaches 99.05 percent. Subsequently, methyl isobutyl ketone is used as an extracting agent, oxalic acid is used as a reducing agent, and gold ions in the leaching solution are reduced into solid metallic gold through extraction and reduction methods.
In summary, the method for recycling copper and gold in the waste mobile phone circuit board powder by steps through sodium persulfate can efficiently recycle copper and gold in the waste mobile phone circuit board, the highest leaching rates of the copper and gold in the waste mobile phone circuit board can reach 99.98% and 99.05% respectively, and the method is efficient in process, environment-friendly, simple in flow, convenient to operate, high in cost efficiency and very suitable for industrial popularization and large-scale use.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by 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 protection scope of the present invention.
Claims (10)
1. The method for recycling copper and gold from the waste mobile phone circuit board is characterized by comprising the following steps:
crushing the waste mobile phone circuit board to obtain waste mobile phone circuit board powder;
mechanically ball milling sodium persulfate, an additive I and the waste mobile phone circuit board powder to obtain solid powder;
reacting the solid powder with water to obtain a copper-containing leaching solution and gold-containing filter residues;
extracting copper ions in the copper-containing leaching solution to obtain copper;
reacting the gold-containing filter residues with a liquid containing sodium persulfate and sodium chloride to obtain a gold-containing leaching solution;
extracting gold ions in the gold-containing leaching solution to obtain gold;
wherein the additive I is one or more of iron powder, zinc powder and aluminum powder.
2. The method of claim 1, wherein the waste cell phone circuit board is crushed to a particle size of 0.1-0.5mm.
3. The method according to claim 1, wherein the ball milling time is 2-6 hours, the ball-to-material ratio is 40:1-80:1, and the ball milling rotation speed is 350rpm-550rpm.
4. The method according to claim 1, wherein the solid powder is reacted with water for a period of 1-15min with a solid to liquid ratio of 1:100kg/L.
5. The method according to claim 1, wherein extracting gold ions from the gold-containing leach solution to obtain gold comprises the steps of:
reacting the gold-containing leaching solution with methyl isobutyl ketone to obtain a gold-carrying organic phase;
and (3) reacting the gold-carrying organic phase with oxalic acid to obtain the gold.
6. The method of claim 1, wherein the copper-containing leachate is electrolyzed to deposit the copper at a cathode electrode.
7. The method according to claim 6, wherein the electrolysis voltage is 5-7V and the electrolysis time is 15-60min.
8. The method according to any one of claims 1 to 7, wherein the concentration of sodium persulfate in the liquid system containing sodium persulfate and sodium chloride is 0.5-1.5mol/L.
9. The method according to any one of claims 1 to 7, wherein the concentration of sodium chloride in the liquid system containing sodium persulfate and sodium chloride is 0.5-3.0mol/L.
10. The method according to any one of claims 1 to 7, wherein the gold-containing filter residue is reacted with the liquid containing sodium persulfate and sodium chloride for a time of 1.0-2.5 hours at a reaction temperature of 50-75 ℃.
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