CN112877543A - Method for recovering lead from lead slag - Google Patents
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- CN112877543A CN112877543A CN202110049526.9A CN202110049526A CN112877543A CN 112877543 A CN112877543 A CN 112877543A CN 202110049526 A CN202110049526 A CN 202110049526A CN 112877543 A CN112877543 A CN 112877543A
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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
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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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
- C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
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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
本发明提供了一种铅渣回收铅的方法，包括以下步骤：S1、将铅渣置于浸出剂中浸出，搅拌后得到浆料；其中，所述浸出剂为甲基磺酸溶液；S2、将所述浆料过滤后得到浸出液；S3、以浸出液作为阴极电解液，利用电解装置电解后回收得到铅。本发明的铅渣回收铅的方法，使用甲基磺酸溶液回收铅，是一种环境友好的铅回收方法，在铅回收过程中零污染，既能实现含铅废渣中铅的选择性浸出，同时可直接作为电解液进行电解，直接快速获得精铅；回收过程中各部分都能被回收利用，实现了含铅废渣回收的原子经济性，对环境不产生污染，产物具高附加值。
The invention provides a method for reclaiming lead from lead slag, comprising the following steps: S1, placing lead slag in a leaching agent for leaching, and stirring to obtain a slurry; wherein, the leaching agent is a methanesulfonic acid solution; S2, After filtering the slurry to obtain a leachate; S3, using the leachate as the catholyte, and recovering lead after electrolysis with an electrolysis device. The method for recovering lead from lead slag of the present invention uses a methanesulfonic acid solution to recover lead, which is an environment-friendly lead recovery method, has zero pollution in the lead recovery process, and can realize selective leaching of lead in lead-containing waste residues. At the same time, it can be directly used as an electrolyte for electrolysis to obtain refined lead directly and quickly; all parts in the recovery process can be recycled, realizing the atomic economy of lead-containing waste slag recovery, without causing pollution to the environment, and the product with high added value.
Description
Technical Field
The invention relates to the technical field of waste residue treatment, in particular to a method for recovering lead from lead slag.
Background
The lead-containing waste residue is toxic and harmful industrial solid waste, has complex components, large difficulty in harmless treatment and higher treatment cost. Along with the crisis of human resource shortage, the lead-containing waste residue is used as a secondary lead resource to realize the resource-regeneration cycle of lead.
At present, the method for recycling the lead slag mainly comprises the step of manufacturing building materials, valuable metal elements such as lead and the like in the waste slag cannot be recycled, potential environmental hazards exist, and the problem of waste slag treatment cannot be fundamentally solved. The method for extracting the valuable metal elements from the lead slag comprises pyrogenic treatment and wet treatment. The production enterprises of secondary lead mainly adopt a pyrogenic process treatment method, but the method needs to be carried out at a higher temperature, has higher energy consumption, can generate a large amount of harmful lead-containing smoke dust and sulfur dioxide gas at a high temperature, and has serious hidden danger of environmental pollution in the production process. Compared with the fire method, the wet method processed slag does not produce smoke dust, and reduces the damage to the environment.
The prior reports utilize hydrogen peroxide, sulfuric acid or nitric acid to leach and treat the waste residue, and lead-containing waste residue is treated by taking a lead compound as a recovery form. But has the problems of complex process flow, high energy consumption, possible generation of wastewater and waste residues in each link and the like. And the leaching agent is expensive, difficult to recycle and has high requirement on leaching equipment.
Based on the problems of complex process, more waste water and waste residue, sulfur dioxide gas generation and the like in the conventional lead-containing waste residue treatment, the conventional lead-containing waste residue needs to be improved.
Disclosure of Invention
In view of the above, the invention provides a method for recovering lead from lead slag, so as to solve the technical problem in the prior art that the usage amount of lithium resources is too large.
In a first aspect, the invention provides a method for recovering lead from lead slag, which comprises the following steps:
s1, putting the lead slag into a leaching agent for leaching, and stirring to obtain slurry; wherein the leaching agent is a methanesulfonic acid solution;
s2, filtering the slurry to obtain a leaching solution;
and S3, electrolyzing the leachate serving as a catholyte by using an electrolyzer, and recovering the lead.
Optionally, in the method for recovering lead from lead slag, the electrolysis device in S3 includes a cathode, an anode and a diaphragm, the cathode is a stainless steel or titanium plate, the anode is one of a titanium-based iridium oxide electrode, graphite or a lead plate, the diaphragm is an anion exchange membrane, and the anolyte is a methanesulfonic acid solution.
Optionally, in the method for recovering lead from lead slag, the leaching temperature in S1 is 20-150 ℃, and the leaching time is 30-180 min.
Optionally, in the method for recovering lead from lead slag, in the step S1, the lead slag is placed in a leaching agent so that the solid-liquid mass-volume ratio is 1g: 5-20 mL.
Optionally, the method for recovering lead from lead slag further comprises the steps of placing the lead slag in a ball mill for ball milling before leaching in a leaching agent, drying after crushing, and then removing iron.
Optionally, in the method for recovering lead from lead slag, the ball milling rotation speed is 200-400 r/min, and the ball milling time is 20-40 min.
Optionally, the method for recovering lead from lead slag comprises a magnetic separation iron removal method.
Optionally, in the method for recovering lead from lead slag, the anion exchange membrane comprises a homogeneous anion exchange membrane or a heterogeneous anion exchange membrane.
Optionally, the method for recovering lead from lead slag further includes collecting the solution on the anode side after electrolysis and returning the solution to the leaching agent.
Optionally, in the method for recovering lead from lead slag, an additive is added into a cathode electrolyte in the electrolysis process in S3, wherein the additive is one or more of butyl acetate, sodium lignosulphonate and arginine.
Compared with the prior art, the method for recovering lead from lead slag has the following beneficial effects:
(1) the method for recovering lead from lead slag uses a methanesulfonic acid solution to recover lead, the methanesulfonic acid is strong non-oxidative organic acid, and has the advantages of high solubility of metal salts (Pb, Sn, Zn, Bi and the like), low toxicity, high conductivity and the like, the methanesulfonic acid is biodegradable, the recycling rate can reach 80%, and the methanesulfonic acid has great advantages in the aspect of environmental protection; all parts can be recycled in the recycling process, the atom economy of recycling the lead-containing waste residues is realized, no pollution is caused to the environment, and the product has high added value;
(2) according to the method for recovering lead from lead slag, the methanesulfonic acid solution collected in the anode chamber can be reused in the leaching process, so that closed cycle of the process is realized;
(3) the method for recovering lead from lead slag can be applied to laboratories and engineering practices, is carried out in the laboratories, is convenient for the inspection and test of products, and can be applied to mass production and sale in the engineering practices.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is a schematic view of an electrolytic apparatus according to an embodiment of the present application;
FIG. 2 is a schematic drawing of an electron microscope showing the refined lead recovered in example 1 of the present application;
FIG. 3 is an energy spectrum of the refined lead recovered in example 1 of the present application.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with 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 obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The application provides a method for recovering lead from lead slag, which comprises the following steps:
s1, putting the lead slag into a leaching agent for leaching, and stirring to obtain slurry; wherein the leaching agent is a methanesulfonic acid solution;
s2, filtering the slurry to obtain a leaching solution;
and S3, electrolyzing the leachate serving as a catholyte by using an electrolyzer, and recovering the lead.
The lead slag in the application is from various lead-containing waste slag generated in waste lead-acid battery treatment, or waste slag generated in non-ferrous metal smelting processes such as copper smelting, zinc smelting, lead smelting and the like.
The leaching agent used in the method is a methanesulfonic acid solution, methanesulfonic acid (MSA) is strong non-oxidative organic acid, and has the advantages of high solubility of metal salts (Pb, Sn, Zn, Bi and the like), low toxicity, high conductivity and the like, the methanesulfonic acid is biodegradable, the recycling rate reaches 80%, and the methanesulfonic acid has great advantages in the aspect of environmental protection.
Specifically, in the embodiment of the present application, the electrolysis apparatus in S3, as shown in fig. 1, includes a cathode 1, an anode 2, a diaphragm 3, and an electrolysis bath 4, where the cathode 1, the anode 2, and the diaphragm 3 are all disposed in the electrolysis bath 4, the diaphragm 3 divides the electrolysis bath 4 into an anode chamber and a cathode chamber, the anode 2 is located in the anode chamber, the cathode 1 is located in the cathode chamber, a catholyte is located in the cathode chamber, an anolyte is located in the anode chamber, the cathode 1 is stainless steel or a titanium plate, and the anode 2 is a titanium-based iridium oxide electrode (Ti/IrO) electrode2) Graphite or lead plate, the diaphragm 3 is an anion exchange membrane,the anolyte is a methanesulfonic acid solution; when the device is used, the anode 2 is connected with the positive pole of a power supply, the cathode 1 is connected with the negative pole of the power supply, and electrochemical reaction is carried out, wherein the specific reaction is as follows:
and (3) anode reaction: 2H2O-4e-→4H++O2
And (3) cathode reaction: pb2++4e-→2Pb
And (3) total reaction: pb (CH)3SO3)2+2H2O＝4Pb+O2+4CH3SO3H
After electrochemical reaction, lead can be obtained at the cathode, and the lead obtained by stripping is collected after being washed and dried.
Specifically, in some embodiments, the electrolysis device further comprises a water bath 5, the electrolysis bath 4 is placed in the water bath 5, and the electrolysis bath 4 is subjected to water bath heating through the water bath 5.
Specifically, in some embodiments, the leaching temperature in the S1 is 20-150 ℃, and the leaching time is 30-180 min.
Specifically, in some embodiments, the lead slag is placed in the leaching agent in S1, so that the solid-liquid mass-volume ratio is 1g: 5-20 mL. By controlling the adding amount of the lead slag, the solid-liquid mass-volume ratio in the leaching agent is 1g: 5-20 mL.
Specifically, in some embodiments, before the lead slag is placed in the leaching agent for leaching, the method further comprises placing the lead slag in a ball mill for ball milling, drying after crushing, and then removing iron. Specifically, the ball milling is dry milling, wet milling or wet milling with a leaching aid; the drying may be done in a vacuum oven.
Specifically, in some embodiments, the ball milling speed is 200 to 400r/min, and the ball milling time is 20 to 40 min.
Specifically, in some embodiments, the iron removal method is magnetic iron removal.
In particular, in some embodiments, the anion exchange membrane comprises a homogeneous anion exchange membrane or a heterogeneous anion exchange membrane; the concentration of the methanesulfonic acid liquid in the anode chamber can be achieved by using an anion exchange membrane.
Specifically, in some embodiments, the method further comprises collecting the solution on the anode side after electrolysis and returning the solution to the leaching agent. That is, in the embodiment of the present application, the methanesulfonic acid solution enriched in the anode chamber after electrolysis is recycled for the leaching stage in S1, so as to realize the closed cycle of the process.
Specifically, in some embodiments, the electrolysis process in S3 may include adding an additive to the catholyte, wherein the additive is one or more of butyl acetate, sodium lignosulfonate, and arginine. The additive can improve the overpotential of cathode lead deposition, and can also improve the appearance of an electric deposition layer by adding a small amount of the additive.
Specifically, in some embodiments, the slurry filtration in S2 includes one of vacuum filtration, plate and frame filter press, belt filter press, etc., and the solution residue can be rapidly separated by filtration.
The method for recovering lead from lead slag uses the methanesulfonic acid solution to recover lead, is an environment-friendly lead recovery method, has zero pollution in the lead recovery process, can realize selective leaching of lead in lead-containing waste slag, and can be directly used as an electrolyte for electrolysis to directly and quickly obtain refined lead; all parts can be recycled in the recycling process, the atomic economy of recycling the lead-containing waste residues is realized, the environment is not polluted, the product has high added value, and the methanesulfonic acid solution collected in the anode chamber can be reused in the leaching process, so that the closed cycle of the process is realized; the method for recovering lead from lead slag can be applied to laboratories and engineering practices, is carried out in the laboratories, is convenient for the inspection and test of products, and can be applied to mass production and sale in the engineering practices.
The method for recovering lead from the lead dross of the present application will be described in further detail below with reference to specific examples.
Example 1
The embodiment of the application provides a method for recovering lead from side-blown lead slag in waste lead-acid battery recovery, which comprises the following steps:
s1, taking lead side-blown slag, and testing the slag by XRF (X-ray diffraction) to obtain the following specific mass percentages: pb: 8.92%, Fe: 29.93%, Si: 25.74%, S: 1.35%, Al: 8.02 percent;
the short-term stability of the lead slag is evaluated, and the toxic leaching result of the lead slag is 357.36mg/L which is far higher than the value of 5mg/L of the national solid waste toxic leaching standard by adopting a solid toxic leaching method of the environmental protection industry standard (HJ/T300-2007) of the people's republic of China.
S2, carrying out dry milling on a certain amount of lead slag with the composition in a ball mill at the ball milling speed of 300rpm for 40 min; s3, carrying out magnetic separation on the ball-milled lead slag, placing the lead slag into a 3mol/L methanesulfonic acid solution after the magnetic separation, controlling the solid-liquid mass-volume ratio to be 1g:20mL, and leaching for 5 hours at the leaching temperature of 30 ℃; after leaching, vacuum filtering to obtain filter residue and filtrate; washing the filter residue to be neutral by water, drying the obtained sample by a vacuum oven for 8 hours, wherein the residue rate is 2%, and the main component of the leaching residue is Si; the filtrate is the leaching solution;
s3, placing the leachate into a cathode chamber of an electrolyzer, taking a titanium-based iridium oxide electrode as an anode, a mirror-surface stainless steel plate as a cathode, a homogeneous-phase anion exchange membrane as a diaphragm, 3mol/L methanesulfonic acid solution as anolyte, and performing electrolysis at a current density of 30mA/cm2And obtaining refined lead at the cathode after electrolysis, wherein the mass fraction of lead in the obtained refined lead is 95%.
Example 2
The embodiment of the application provides a method for recovering lead from short-kiln lead slag in a smelting plant, which comprises the following steps:
s1, taking short-kiln lead slag of a smelting plant, and testing the slag by XRF, wherein the slag comprises the following components in percentage by mass: 3.21%, Fe: 37.41%, Ca: 11.05%, Si: 29.21%, Al: 8.57%, S: 1.67 percent;
the short-term stability of the lead slag is evaluated, and the toxic leaching result of the lead slag is 10.87mg/L which is far higher than the value of 5mg/L of the national solid waste toxic leaching standard by adopting a solid toxic leaching method of the environmental protection industry standard (HJ/T300-2007) of the people's republic of China.
S2, carrying out dry milling on a certain amount of lead slag with the composition in a ball mill at the ball milling speed of 300rpm for 40 min; carrying out magnetic separation on the ball-milled lead slag, placing the lead slag into a 2mol/L methanesulfonic acid solution after the magnetic separation, controlling the solid-liquid mass-volume ratio to be 1g:20mL, and leaching for 5h at the leaching temperature of 30 ℃; after leaching, vacuum filtering to obtain filter residue and filtrate; washing the filter residue to be neutral by water, drying the obtained sample by a vacuum oven for 8 hours, wherein the residue rate is 5%, the main component of the leaching residue is Si, the toxic leaching result of the residue is lower than 5mg/L and reaches the standard, and the filter residue can be used for building materials; the filtrate is the leaching solution;
s3, placing the leachate into a cathode chamber of an electrolyzer, taking a titanium-based iridium oxide electrode as an anode, a mirror-surface stainless steel plate as a cathode, an anion exchange membrane as a diaphragm, and 2mol/L methanesulfonic acid solution as anolyte, wherein the current density is 20mA/cm2Then obtaining spongy lead at the cathode after electrolysis; by the recovery method, the lead recovery rate is more than 85 percent.
The electron microscope and the energy spectrum of the refined lead obtained by cathode recovery in example 1 are shown in FIGS. 2 to 3, respectively. As can be seen from FIGS. 2 to 3, the obtained sample was lead.
The invention is not to be considered as limited to the particular embodiments shown and described, but is to be accorded the widest scope consistent with the principles and novel features herein disclosed.
Claims (10)
1. The method for recovering lead from lead slag is characterized by comprising the following steps:
s1, putting the lead slag into a leaching agent for leaching, and stirring to obtain slurry; wherein the leaching agent is a methanesulfonic acid solution;
s2, filtering the slurry to obtain a leaching solution;
and S3, electrolyzing the leachate serving as a catholyte by using an electrolyzer, and recovering the lead.
2. The method for recovering lead from lead slag according to claim 1, wherein the electrolysis device in S3 comprises a cathode, an anode and a diaphragm, wherein the cathode is a stainless steel or titanium plate, the anode is one of a titanium-based iridium oxide electrode, graphite or a lead plate, the diaphragm is an anion exchange membrane, and the anolyte is a methanesulfonic acid solution.
3. The method for recovering lead from lead slag according to claim 1, wherein the leaching temperature in S1 is 20-150 ℃, and the leaching time is 30-180 min.
4. The method for recovering lead from lead slag according to claim 1, wherein the lead slag is placed in a leaching agent in S1 so that the solid-liquid mass-volume ratio is 1g: 5-20 mL.
5. The method for recovering lead from lead slag as recited in claim 1, wherein before the lead slag is leached in the leaching agent, the method further comprises the steps of ball milling the lead slag in a ball mill, crushing, drying and removing iron.
6. The method for recovering lead from lead slag according to claim 5, wherein the ball milling rotation speed is 200-400 r/min, and the ball milling time is 20-40 min.
7. The method for recovering lead from lead slag as recited in claim 5, wherein the iron removal method is magnetic iron removal.
8. The method for recovering lead from lead slag according to claim 2, wherein the anion exchange membrane comprises a homogeneous anion exchange membrane or a heterogeneous anion exchange membrane.
9. The method for recovering lead from lead slag as recited in claim 2, further comprising collecting the solution on the anode side after electrolysis and returning the solution to the leaching agent.
10. The method for recovering lead from lead slag as claimed in claim 2, wherein an additive is further added to the catholyte in the electrolysis process in S3, wherein the additive is one or more of butyl acetate, sodium lignosulphonate and arginine.
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| CN114180692A (en) * | 2021-12-02 | 2022-03-15 | 武汉鸿劲金属铝业有限公司 | Compound coagulant, preparation method and application thereof |
| CN114480862A (en) * | 2022-01-25 | 2022-05-13 | 长沙有色冶金设计研究院有限公司 | Method for recovering valuable elements from copper dross |
| CN114990327A (en) * | 2022-05-18 | 2022-09-02 | 济源豫光有色冶金设计研究院有限公司 | Method for resource utilization of waste lead storage battery electrolyte |
| WO2025228545A1 (en) * | 2023-05-05 | 2025-11-06 | Bluecap Resources | Extraction method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114480862A (en) * | 2022-01-25 | 2022-05-13 | 长沙有色冶金设计研究院有限公司 | Method for recovering valuable elements from copper dross |
| CN114480862B (en) * | 2022-01-25 | 2024-01-30 | 长沙有色冶金设计研究院有限公司 | Method for recovering valuable elements from copper dross |
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| WO2025228545A1 (en) * | 2023-05-05 | 2025-11-06 | Bluecap Resources | Extraction method |
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Application publication date: 20210601 |