CN111349961B - Method for cleaning waste titanium anode plate for foil forming machine and removing and recycling precious metal - Google Patents
Method for cleaning waste titanium anode plate for foil forming machine and removing and recycling precious metal Download PDFInfo
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- CN111349961B CN111349961B CN202010358396.2A CN202010358396A CN111349961B CN 111349961 B CN111349961 B CN 111349961B CN 202010358396 A CN202010358396 A CN 202010358396A CN 111349961 B CN111349961 B CN 111349961B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
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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
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/106—Other heavy metals refractory metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/04—Wires; Strips; Foils
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
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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 provides a method for cleaning a waste titanium anode plate for a foil forming machine and removing and recovering precious metals, which comprises the following steps: s1, firstly, washing the surface sundries of the waste anode plate to be cleaned with distilled water, and naturally airing the washed surface sundries; s2, placing the washed anode plate into an oxidation furnace for sintering, and naturally cooling to room temperature after discharging; s3, soaking the sintered old anode plate in HCL and H2O2 water; s4, fishing out the soaked anode plate, washing with a high-pressure water gun, and removing lead oxide impurities on the surface; s5, drying the washed anode plate in a drying furnace, and waiting for precious metal removal after drying; s6, preparing 50% potassium hydroxide solution and 30% NaCl. The method for cleaning the waste titanium anode plate and removing and recovering the noble metal for the foil producer does not need external force, does not cause physical damage to the titanium anode plate, has high cleaning efficiency, can complete the recovery of the noble metal, is safe and easy to operate, and has low danger.
Description
Technical Field
The invention relates to precious metal recovery of a waste titanium anode plate of a foil forming machine for electronic copper foil production, in particular to a method for cleaning the waste titanium anode plate of the foil forming machine and removing and recovering the precious metal.
Background
The anode current of the electrolytic copper foil is 6000-10000A/square meter, and a small amount of additives and trace metal impurities are contained in the electrolyte. In the electrolytic process, the surface of the anode is slowly covered by a compact scaling layer, which causes the adverse effects of increased tank pressure, increased power consumption, insufficient uniformity of copper foil, reduced product qualification rate and the like, and leads to the passivation failure of the anode plate coating.
Scale formation composition analysis
| Element(s) | Pb | Mn | Fe | Cu | Mo | Sn | Sb | Ti | Ir | Ta |
| w/％ | 89.015 | 0.064 | 1.224 | 0.645 | 1.775 | 2.484 | 1.101 | 1.41 | 1.424 | 0.892 |
Cause of scale formation
Pb enters through the electrolyte, and although the process requires that the Pb is controlled to be less than 0.1g/L, the electrolyte is continuously circulated in the electrolytic process, Pb2+ is continuously oxidized to be Pb4+ on the surface of the anode, and is slowly accumulated and separated out in the form of PbO2 and attached to the surface of the anode. When power is cut off, because the polarization direction of an electrode system is reversed, PbO2 on the surface of the anode is reduced to PbSO4 which is not conductive, so that the surface of the anode is covered by PbO2 and PbSO4, and a compact scaling layer is formed, the anode conductivity is deteriorated by the scaling layer, the tank pressure is increased, the power consumption is increased, meanwhile, the anode potential is not uniformly distributed by the scaling layer, the uniformity of the electrolyzed copper foil is not enough, and the product percent of pass is reduced. The areas covered by the fouling layer are poor in conduction, so that the current density of the uncovered areas is relatively increased, the anode potential is increased, and the passivation failure of the coating in the areas is accelerated.
Current methods for removing scale deposits and noble metal coatings
1. Mechanical removal means that the scale is directly scraped off by a tool through external force.
2. The acid cooking process-efficiency is too low and the precious metals cannot be recovered.
3. The alkaline boiling method has high operation danger and low recycling rate.
The conventional method adopts a high-temperature melting and alkaline boiling method, namely melting sodium hydroxide at high temperature of 300 ℃ and 400 ℃, and then putting the material into the melting and alkaline boiling method for reaction, wherein the method is easy to cause fire and other hidden troubles.
Therefore, it is necessary to provide a method for cleaning waste titanium anode plates for a new foil machine and removing and recovering precious metals to solve the above problems.
Disclosure of Invention
The invention provides a method for cleaning a waste titanium anode plate for a crude foil machine and removing and recovering precious metals, which solves the technical problems.
In order to solve the technical problem, the invention provides a method for cleaning a waste titanium anode plate for a crude foil machine and removing and recovering precious metals, which comprises the following steps:
s1, firstly, washing the surface sundries of the waste anode plate to be cleaned with distilled water, and naturally airing the washed surface sundries;
s2, placing the washed anode plate into an oxidation furnace for sintering, and naturally cooling to room temperature after discharging;
s3, placing the old anode plate after sintering into HCL and H2O2Soaking in water;
s4, fishing out the soaked anode plate, washing with a high-pressure water gun, and removing the lead oxide and manganese metal oxide on the surface;
s5, drying the washed anode plate in a drying furnace, and waiting for precious metal removal after drying;
s6, preparing 50% potassium hydroxide solution and adding 30% NaCl;
s7, uniformly coating the prepared potassium hydroxide solution on the surface of the waste anode plate by using a brush, then feeding the waste anode plate into an oxidation furnace, and keeping the temperature at 430 ℃ for 10 min.
S8, immediately putting the anode plate into a cooling water tank after discharging, repeating the operation for 2-3 times to remove the precious metals on the surface, and carrying out centralized collection treatment on the cooling water containing the precious metals;
and S9, putting the waste anode plate with the coating removed into a mixed acid solution of hydrofluoric acid, nitric acid and water again for cleaning, removing residual impurities on the surface, and reusing the titanium substrate with the precious metal coating removed.
Preferably, in step S2, the anode plate after washing is placed in an oxidation furnace at 480 ℃ and sintered for 30 min.
Preferably, in step S3, the old anode plate after sintering is placed in 10% HCL and 5% H2O2Soaking in water for 24 hr at about 40 deg.C.
Preferably, in step S5, the anode plate after washing is dried in a drying oven at 120 ℃ for 15-20 min.
Preferably, in step S6, the solution must be prepared with distilled water.
Preferably, in step S9, the ratio of hydrofluoric acid: nitric acid: the proportion of water is 1: 6: 20.
compared with the prior art, the method for cleaning the waste titanium anode plate and removing and recovering the precious metal for the green foil machine does not need external force, does not cause physical damage to the titanium anode plate, is high in cleaning efficiency, can complete the recovery of the precious metal, and is safe, easy to operate and low in danger.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for cleaning a waste titanium anode plate for a foil forming machine and removing and recovering precious metals, which comprises the following steps:
s1, firstly, washing the surface sundries of the waste anode plate to be cleaned with distilled water, and naturally airing the washed surface sundries;
s2, placing the washed anode plate into an oxidation furnace for sintering, and naturally cooling to room temperature after discharging;
s3, placing the old anode plate after sintering into HCL and H2O2Soaking in water;
s4, fishing out the soaked anode plate, washing with a high-pressure water gun, and removing the lead oxide and manganese metal oxide on the surface;
s5, drying the washed anode plate in a drying furnace, and waiting for precious metal removal after drying;
s6, preparing 50% potassium hydroxide solution and adding 30% NaCl;
s7, uniformly coating the prepared potassium hydroxide solution on the surface of the waste anode plate by using a brush, then feeding the waste anode plate into an oxidation furnace, and keeping the temperature at 430 ℃ for 10 min.
S8, immediately putting the anode plate into a cooling water tank after discharging, repeating the operation for 2-3 times to remove the precious metals on the surface, and carrying out centralized collection treatment on the cooling water containing the precious metals;
and concentrating the cooling water containing the precious metals by adopting a rotary evaporator and a negative pressure distillation method according to batches, and separating and refining the precious metals from the treated concentrated solution. Greatly improving the recovery efficiency and the purity.
And S9, putting the waste anode plate with the coating removed into a mixed acid solution of hydrofluoric acid, nitric acid and water again for cleaning, removing residual impurities on the surface, and reusing the titanium substrate with the precious metal coating removed.
In step S2, the anode plate after washing is placed in an oxidation furnace at 480 ℃ and sintered for 30 min.
In step S3, the old anode plate after sintering is placed in 10% HCL and 5% H2O2Soaking in water for 24 hr at about 40 deg.C.
In step S5, the anode plate after washing is dried in a 120 ℃ drying oven for 15-20 min.
In step S6, the solution must be prepared with distilled water.
In step S9, hydrofluoric acid: nitric acid: the proportion of water is 1: 6: 20.
the chemical components of the cleaned anode plate meet the requirements of TA1 materials, and GB/T3620.1-94 can be referred, and the mechanical properties meet GB/T3621-94 standard parameters of titanium and titanium alloy plates, namely, the tensile strength: 370-530N/mm2 specifies a residual elongation stress of > 250N/mm2 and an elongation of 30-40%.
The invention adopts a surface coating process, molten alkali and molten salt are completely reacted with the surface of the material by slow heating, and the purpose of adding sodium chloride can promote the faster crack of the surface coating and the complete separation of the titanium base. The sintered material has no potential safety hazard, and the molten alkali can be prevented from splashing and igniting in the treatment process in the operation process.
Compared with the prior art, the method for cleaning the waste titanium anode plate and removing and recovering the precious metal for the green foil machine does not need external force, does not cause physical damage to the titanium anode plate, is high in cleaning efficiency, can complete the recovery of the precious metal, and is safe, easy to operate and low in danger.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (6)
1. A method for cleaning a waste titanium anode plate for a crude foil machine and removing and recovering precious metals is characterized by comprising the following steps:
s1, firstly, washing the surface sundries of the waste anode plate to be cleaned with distilled water, and naturally airing the washed surface sundries;
s2, placing the washed anode plate into an oxidation furnace for sintering, and naturally cooling to room temperature after discharging;
s3, putting HCl and H into the old anode plate after sintering2O2Soaking in water;
s4, fishing out the soaked anode plate and washing the anode plate by using a high-pressure water gun;
s5, drying the washed anode plate in a drying furnace, and waiting for precious metal removal after drying;
s6, preparing 50% potassium hydroxide solution and adding 30% NaCl;
s7, uniformly coating the prepared solution on the surface of an anode plate by using a brush, then feeding the anode plate into an oxidation furnace, and keeping the temperature at 430 ℃ for 10 min;
s8, immediately putting the anode plate into a cooling water tank after discharging, repeating the operation for 2-3 times to remove the precious metals on the surface, and carrying out centralized collection treatment on the cooling water containing the precious metals;
and S9, cleaning the waste anode plate with the coating removed in a mixed acid solution of hydrofluoric acid, nitric acid and water to remove residual impurities on the surface, wherein the titanium substrate with the precious metal coating removed can be reused.
2. The method for cleaning the waste titanium anode plate and removing and recovering the noble metals for the green foil machine according to claim 1, wherein in step S2, the anode plate after being washed is placed in an oxidation furnace at 480 ℃ and sintered for 30 min.
3. The method for cleaning waste titanium anode plates for green foil machines and removing and recovering precious metals according to claim 1, wherein in step S3, the sintered waste anode plates are placed in 10% HCl and 5% H2O2Soaking in water for 24h at 40 ℃.
4. The method for cleaning the waste titanium anode plate and removing and recovering the noble metals for the green foil machine according to claim 1, wherein in step S5, the anode plate after being washed is dried in a 120 ℃ drying oven for 15-20 min.
5. The method for cleaning waste titanium anode plates for green foil machines and removing and recovering precious metals according to claim 1, wherein in step S6, the solution must be prepared with distilled water.
6. The method for cleaning waste titanium anode plates for green foil machines and removing and recovering precious metals according to claim 1, wherein in step S9, hydrofluoric acid: nitric acid: the proportion of water is 1: 6: 20.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010358396.2A CN111349961B (en) | 2020-04-29 | 2020-04-29 | Method for cleaning waste titanium anode plate for foil forming machine and removing and recycling precious metal |
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| CN202010358396.2A CN111349961B (en) | 2020-04-29 | 2020-04-29 | Method for cleaning waste titanium anode plate for foil forming machine and removing and recycling precious metal |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112795932B (en) * | 2020-12-18 | 2023-03-24 | 西安泰金新能科技股份有限公司 | Method for removing titanium anode surface coating |
| CN114540824B (en) * | 2022-03-08 | 2023-12-15 | 昆明冶金研究院有限公司 | Method for regenerating titanium anode plate by using waste acid solution |
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| CN101818360A (en) * | 2010-03-16 | 2010-09-01 | 西安泰金工业电化学技术有限公司 | Method for removing waste titanium anode coating |
| CN104120460A (en) * | 2014-07-02 | 2014-10-29 | 广州鸿葳科技股份有限公司 | Method for removing scaling of surface of titanium anode for electrolytic copper foil |
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| CN109023399A (en) * | 2018-08-28 | 2018-12-18 | 常州大学 | The regeneration method of regeneration treatment liquid of electrolytic copper foil Ni―Ti anode and preparation method thereof and Ni―Ti anode |
| CN110714205A (en) * | 2019-09-16 | 2020-01-21 | 铜陵市华创新材料有限公司 | Electrolytic copper foil integrated machine anode plate descaling agent for lithium ion battery and preparation and use methods thereof |
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2020
- 2020-04-29 CN CN202010358396.2A patent/CN111349961B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS602684A (en) * | 1983-06-20 | 1985-01-08 | Permelec Electrode Ltd | Reactivating method of insoluble electrode |
| CN101818360A (en) * | 2010-03-16 | 2010-09-01 | 西安泰金工业电化学技术有限公司 | Method for removing waste titanium anode coating |
| CN104120460A (en) * | 2014-07-02 | 2014-10-29 | 广州鸿葳科技股份有限公司 | Method for removing scaling of surface of titanium anode for electrolytic copper foil |
| CN104775036A (en) * | 2015-05-12 | 2015-07-15 | 昆明贵益金属材料有限公司 | Method for recovering noble metal from waste titanium anodes with noble metal coatings |
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| CN110923467A (en) * | 2019-11-28 | 2020-03-27 | 三明学院 | Method for recycling lead from waste lead-acid battery |
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Effective date of registration: 20210207 Address after: Block h, phase I, Baoji high end equipment Industrial Park, No. 95, Shuxiang Road South, Baoji hi tech Development Zone, Shaanxi Province, 721000 Applicant after: Baoji Titanium Prius Titanium Anode Technology Co.,Ltd. Address before: 721000 south section of Gaoxin 18th Road, high tech Development Zone, Baoji City, Shaanxi Province Applicant before: BAOJI CHANGLI SPECIAL METAL Co.,Ltd. |
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Inventor after: Li Qiao Inventor after: Qiao Zhihua Inventor before: Qiao Zhihua Inventor before: Li Qiao |
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Effective date of registration: 20221222 Address after: Block h, phase I, Baoji high end equipment Industrial Park, No. 95, Shuxiang Road South, Baoji hi tech Development Zone, Shaanxi Province, 721000 Patentee after: Baoji Titanium Prius Titanium Anode Technology Co.,Ltd. Patentee after: BAOJI CHANGLI SPECIAL METAL Co.,Ltd. Address before: Block h, phase I, Baoji high end equipment Industrial Park, No. 95, Shuxiang Road South, Baoji hi tech Development Zone, Shaanxi Province, 721000 Patentee before: Baoji Titanium Prius Titanium Anode Technology Co.,Ltd. |