CN114606538A - Waste lead paste recovery treatment method - Google Patents

Waste lead paste recovery treatment method Download PDF

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CN114606538A
CN114606538A CN202210077660.4A CN202210077660A CN114606538A CN 114606538 A CN114606538 A CN 114606538A CN 202210077660 A CN202210077660 A CN 202210077660A CN 114606538 A CN114606538 A CN 114606538A
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waste lead
solution
recycling
lead
lead paste
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CN114606538B (en
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曹靖
于佳佳
李江敏
张俊丰
周圣权
吴磊
黄妍
付辅彬
饶炎钊
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Xiangtan University
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    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes

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Abstract

The invention discloses a waste lead paste recovery treatment method, which comprises the following steps: 1) pretreatment: mixing waste lead paste with a transforming agent to obtain a solution A and a material B; (2) microwave treatment: mixing the material B with a carbon material and carrying out microwave heating treatment to obtain a material C; (3) preparing slurry: mixing the material C with an auxiliary material to obtain slurry; (4) recovering metal lead: and (3) uniformly coating the obtained slurry on a cathode plate, and carrying out electrolytic reaction in an inert atmosphere by using the solution A as an electrolyte to obtain metallic lead and a solution D, wherein the solution D contains a conversion agent required in the step (1). The invention aims to improve the recycling rate of the waste lead plaster.

Description

Waste lead paste recovery treatment method
Technical Field
The invention relates to the technical field of waste lead paste recovery, in particular to a waste lead paste recovery processing method.
Background
At present, lead-acid batteries are widely applied to the fields of automobiles, electric automobiles, motorcycles, navigation, communication, electric power and the like. China is the largest lead-acid battery producing country in the world and is also the largest lead-acid battery consuming country. The large-scale use of lead-acid batteries inevitably leads to the scrapping of a large number of lead-acid batteries. The lead-acid battery contains more than 60% of lead and also contains heavy metal elements such as Sb and Ba. If the lead-acid battery is directly discarded without being treated, the lead-acid battery not only pollutes the natural environment, but also has harm to the health of human beings. 86% of lead in the world is used for producing lead-acid batteries, so that the recovery of metallic lead from waste lead-acid batteries is the key point of sustainable development of lead resources and is an important measure for effectively utilizing the resources and reducing environmental pollution.
The lead-acid battery mainly comprises lead paste, electrolyte, a lead alloy grid and other parts. Wherein the waste lead plaster contains a large amount of PbSO4And also a part of PbO2PbO and a small amount of Pb. Therefore, the recovery of metallic lead from waste lead paste has been the focus of research. Up to now, there are two main methods for recovering lead from waste lead paste, pyrometallurgical process and hydrometallurgical process. The pyrometallurgical process has high cost, while the wet process is to convert the insoluble lead sulfate into lead carbonate by pretreating the waste lead plaster and the carbonate, and the treated lead plaster is dissolved into lead ion solution by acid and then electrolyzed to prepare refined lead. The method consumes carbonate resources and discharges a large amount of greenhouse gas CO2. The reaction principle is as follows:
PbSO4+MCO3＝MSO4+PbCO3；
PbCO3+H+＝Pb2++H2O+CO2↑。
disclosure of Invention
The invention mainly aims to provide a waste lead paste recovery processing method, and aims to solve the problem that the cost performance of the existing waste lead paste recovery processing is not high.
In order to achieve the aim, the invention provides a waste lead paste recovery and treatment method, which comprises the following steps:
(1) pretreatment: mixing waste lead paste with a transforming agent to obtain a solution A and a material B;
(2) microwave treatment: mixing the material B with a carbon material and carrying out microwave heating treatment to obtain a material C;
(3) preparing slurry: mixing the material C with an auxiliary material to obtain slurry;
(4) recovering metal lead: and (2) uniformly coating the obtained slurry on a cathode plate, and carrying out electrolytic reaction in an inert atmosphere by taking the solution A as an electrolyte to obtain metallic lead and a solution D, wherein the solution D contains a conversion agent required in the step (1).
Optionally, the step (1) specifically includes: and mixing a certain amount of ammonium bicarbonate or ammonium carbonate solution with the waste lead paste to obtain PbCO3 precipitate and (NH4)2SO4 solution.
Optionally, the ratio of the amount of sulfate radicals to the amount of ammonium bicarbonate or ammonium carbonate in the waste lead paste is 1: 2.0-2.4 and 1: 1.0 to 1.2.
Optionally, the carbon material includes one or more of activated carbon, acetylene black, carbon nanotubes, and graphene.
Optionally, the auxiliary material is uniformly dispersed PVDF-polyvinylidene fluoride in NMP-N-methyl pyrrole.
Optionally, the carbon material is acetylene black, and the mass ratio of the PbCO3 to the PVDF to the acetylene black is 1: 0.001 to 0.003: 0.1 to 0.5.
Optionally, the microwave power of the microwave heating treatment in the step (2) is 500-1000W, and the heating time is 0.5-3 min.
Optionally, the inert atmosphere in the step (4) is CO2, nitrogen and helium, and the pressure ranges from 100kPa to 110 kPa.
Optionally, the pH value of the electrolysis reaction in the step (4) is 8.5-10.5, the concentration of (NH4)2SO4 in the electrolyte is 100-400 g/L, and the electrolysis temperature is 0-60 ℃.
Optionally, the solution D is subjected to a recycling pretreatment so that the ratio of the amount of carbonate in the solution to the amount of sulfate in the waste lead plaster to be treated is 1.0-2.2: 1.
the method for recycling the waste lead paste provided by the invention comprises the steps of carrying out desulfurization, microwave heating and size mixing treatment on the waste lead paste, then uniformly coating the waste lead paste on a cathode plate, and carrying out electrolytic reaction in an inert atmosphere to further obtain metal lead and a conversion agent for desulfurization treatment, wherein an electrolyte of the electrolytic reaction can directly adopt a solution obtained by desulfurization treatment, and further the recycling of the solution in the waste lead paste recycling treatment is realized while the metal lead is recycled. And when the conversion agent adopts ammonium bicarbonate or ammonium carbonate solution, the closed cycle of carbonate is realized, the waste of carbonate resources and the emission of greenhouse gases are avoided, and the economic effect is improved and the environment is protected.
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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 present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a characteristic diffraction peak diagram of the lead paste processed in the embodiment of the waste lead paste recycling method according to the present invention, which is detected by X-ray diffraction.
Detailed Description
It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a waste lead paste recovery processing method, which comprises the following steps:
(1) pretreatment: mixing waste lead paste with a transforming agent to obtain a solution A and a material B; wherein the main component in the waste lead plaster contains a large amount of PbSO4And also a part of PbO2The waste lead plaster treatment mainly comprises the desulfurization treatment of the waste lead plaster, and the conversion agent adopted in the invention is ammonium bicarbonate or ammonium carbonate, so that the conversion of lead sulfate in the lead plaster into lead carbonate is realized, and (NH) is generated at the same time4)2SO4The solution, the main reaction principle is as follows:
PbSO4+NH4HCO3/(NH4)2CO3＝(NH4)2SO4+PbCO3；
wherein the mass ratio of sulfate radicals to ammonium bicarbonate or ammonium carbonate in the waste lead plaster is respectively 1: 2.0-2.4 and 1: 1.0-1.2, and the processing of the waste lead paste mainly removes unnecessary impurities in the waste batteries.
(2) Microwave treatment: the main component obtained in the step (1) is PbCO3The material B is mixed with a carbon material and subjected to microwave heating treatment to obtain a certain amount of lead-containing nuclei and PbCO3And a mixture C of the carbon material and the carbon material, wherein the carbon material comprises one or more of activated carbon, acetylene black, carbon nano tubes and graphene, the microwave power of the microwave heating treatment is 500-1000W, and the heating time is 0.5-3 min.
(3) Preparing slurry: mixing the mixed product subjected to microwave treatment in the step (2) with an auxiliary material for size mixing, wherein the auxiliary material is uniformly dispersed PVDF-polyvinylidene fluoride in NMP-N-methylpyrrole; when the carbon material is acetylene black, the PbCO is3And the mass ratio of PVDF to acetylene black is 1: 0.001 to 0.003: 0.1 to 0.5.
(4) Recovering metal lead: uniformly coating the slurry obtained in the step (3) on a cathode plate, drying, curing, and reacting with (NH) obtained in the step (1) in an inert atmosphere4)2SO4The solution is used as electrolyte to carry out electrolytic reactionAnd obtaining a solution of metal lead and ammonium bicarbonate and/or ammonium carbonate, and further realizing the regeneration of the ammonium bicarbonate and/or ammonium carbonate, wherein the drying and curing temperature is 60-140 ℃.
Further, the inert atmosphere in the step (4) is CO2, nitrogen and helium, and the pressure range is 100 kPa-110 kPa.
Further, the pH value range of the electrolytic reaction in the step (4) is 8.5-10.5, and (NH) in the electrolyte4)2SO4The concentration is 100-400 g/L, and the electrolysis temperature is 0-60 ℃.
Further, the ammonium bicarbonate and/or ammonium carbonate solution obtained in the step (4) is subjected to recycling pretreatment, so that the ratio of the amount of carbonate in the solution to the amount of sulfate in the waste lead plaster to be treated is kept between 1.0 and 2.2: 1 range.
In order to better verify the implementation steps of the method for recycling and treating the waste lead paste, the following embodiments are provided:
detailed description of the preferred embodiment 1
The processed 100g of waste lead paste was treated with 35g of ammonium bicarbonate to obtain mainly PbCO3Precipitation and (NH)4)2SO4Solution, filtering and drying the treated precipitate, weighing 5g of precipitate and 0.016g of acetylene black, mixing, heating for 1 minute under the power of 600W of microwave, adding 0.012g of polyvinylidene fluoride (PVDF) mixed solvent uniformly dispersed in N-methyl pyrrole (NMP), and uniformly stirring to prepare corresponding slurry;
uniformly coating the prepared slurry on a cathode, drying and curing at 100 ℃, and adding CO under the pressure of 100kPa2Carrying out an electrolytic reaction in an atmosphere in which the electrolyte used is (NH) generated after the above-mentioned treatment of the lead paste4)2SO4Solution, maintaining pH value of 9.0 and current density of 200Am in electrochemical reduction-2The concentration of the electrolyte is 200g/L, the electrolysis temperature is 25 ℃, and the metal lead is obtained by electrochemical reduction. The conversion of the finally obtained lead recovery was 83.60%.
Comparative example 1:
the processed 100g of waste lead paste was treated with 35g of ammonium bicarbonate to obtain mainly PbCO3Precipitation and (NH)4)2SO4Solution, filtering and drying the treated precipitate, weighing 5g of precipitate and 0.016g of acetylene black, mixing, adding 0.012g of polyvinylidene fluoride (PVDF) mixed solvent which is uniformly dispersed in N-methyl pyrrole (NMP), and uniformly stirring to prepare corresponding slurry;
uniformly coating the prepared slurry on a cathode, drying and curing at 100 ℃, and adding CO under the pressure of 100kPa2Carrying out an electrolytic reaction in an atmosphere in which the electrolyte used is (NH) generated after the above-mentioned treatment of the lead paste4)2SO4Solution, maintaining pH value of 9.0 and current density of 200Am in electrochemical reduction-2The concentration of the electrolyte is 200g/L, the electrolysis temperature is 25 ℃, and the metal lead is obtained by electrochemical reduction. The conversion of the finally obtained lead recovery was 81.20%.
Specific example 2
The processed 100g of waste lead paste was treated with 35g of ammonium bicarbonate to obtain mainly PbCO3Precipitation and (NH)4)2SO4Solution, filtering and drying the treated precipitate, weighing 5g of precipitate and 0.016g of acetylene black, mixing, heating for 2 minutes under the power of 500W of microwave, adding 0.012g of polyvinylidene fluoride (PVDF) mixed solvent uniformly dispersed in N-methyl pyrrole (NMP), and uniformly stirring to prepare corresponding slurry;
uniformly coating the prepared slurry on a cathode, drying and curing at 100 ℃, and adding CO under the pressure of 100kPa2Carrying out an electrolytic reaction in an atmosphere in which the electrolyte used is (NH) generated after the above-mentioned treatment of the lead paste4)2SO4Solution, maintaining pH value of 9.0 and current density of 200Am in electrochemical reduction-2The concentration of the electrolyte is 200g/L, the electrolysis temperature is 25 ℃, and the metal lead is obtained by electrochemical reduction. The conversion of the finally obtained lead recovery was 88.60%.
Specific example 3
The processed 100g of waste lead paste is treated with 35g of ammonium bicarbonate to obtain mainly PbCO3Precipitation and (NH)4)2SO4Solution, filtering and drying the treated precipitate, weighing 7g of precipitate, mixing with 0.022g of acetylene black, heating for 1 minute under the power of 600W of microwave, adding into 0.0162g of polyvinylidene fluoride (PVDF) mixed solvent uniformly dispersed in N-methyl pyrrole (NMP), and uniformly stirring to prepare corresponding slurry;
uniformly coating the prepared slurry on a cathode, drying at 120 deg.C, curing, and adding CO under 100kPa2Carrying out an electrolytic reaction in an atmosphere in which the electrolyte used is (NH) generated after the above-mentioned treatment of the lead paste4)2SO4The solution maintains the pH value of 9.5 and the current density in electrochemical reduction is 320Am-2The concentration of the electrolyte is 250g/L, the electrolysis temperature is 25 ℃, and the metal lead is obtained by electrochemical reduction. The conversion of the finally obtained lead recovery was 92.90%.
Specific example 4
The processed 100g of waste lead paste was treated with 35g of ammonium bicarbonate to obtain mainly PbCO3Precipitation of and (NH)4)2SO4Solution, filtering and drying the treated precipitate, weighing 7g of precipitate, mixing with 0.022g of acetylene black, heating for 1 minute under the power of 600W of microwave, adding into 0.0162g of polyvinylidene fluoride (PVDF) mixed solvent uniformly dispersed in N-methyl pyrrole (NMP), and uniformly stirring to prepare corresponding slurry;
uniformly coating the prepared slurry on a cathode, drying and curing at 100 ℃, and adding CO under the pressure of 100kPa2Carrying out an electrolytic reaction in an atmosphere in which the electrolyte used is (NH) generated after the above-mentioned treatment of the lead paste4)2SO4Solution, maintaining pH value of 10 and current density of 200Am in electrochemical reduction-2The concentration of the electrolyte is 250g/L, the electrolysis temperature is 50 ℃, and the metal lead is obtained by electrochemical reduction. The conversion of the finally obtained lead recovery was 95.41%.
Comparative example 2:
the processed 100g of waste lead paste was treated with 35g of ammonium bicarbonate to obtain mainly PbCO3Precipitation and (NH)4)2SO4Solution, filtering and drying the treated precipitate, weighing 7g of precipitate, mixing with 0.022g of acetylene black, adding into 0.0162g of polyvinylidene fluoride (PVDF) mixed solvent which is uniformly dispersed in N-methyl pyrrole (NMP), and uniformly stirring to prepare corresponding slurry;
uniformly coating the prepared slurry on a cathode, drying and curing at 100 ℃, and adding CO under the pressure of 100kPa2Carrying out an electrolytic reaction in an atmosphere in which the electrolyte used is (NH) generated after the above-mentioned treatment of the lead paste4)2SO4Solution, maintaining pH value of 10 and current density of 200Am in electrochemical reduction-2The concentration of the electrolyte is 250g/L, the electrolysis temperature is 50 ℃, and the metal lead is obtained by electrochemical reduction. The conversion of the finally obtained lead recovery was 67.32%.
The parameter information of the above examples and comparative examples are as follows:
Figure BDA0003484691340000061
Figure BDA0003484691340000071
from the above table, it can be seen that,
(1) the conversion rate of lead recovery obtained after the microwave treatment step is higher than that obtained after the microwave treatment step is not carried out.
(2) By comparing the conversion in example 2 with that in example 1, the conversion of lead recovery is improved in the end in the case of slightly reducing the microwave power and increasing the time of the microwave treatment.
(3) By comparing the conversion rates of example 3 with example 1, the electrolyte solubility, current density, and PH during the electrolysis reaction are increased, and the conversion rate of lead recovery is significantly increased.
(4) By comparing the conversion rates of example 4 and example 1, the conversion rate of the finally obtained lead recovery is obviously improved by increasing the pH value in the electrolytic reaction process, increasing the electrolytic reaction temperature and increasing the electrolyte solubility.
Therefore, based on the above conclusions, the setting of different parameters under different conditions in the lead recovery process has a great influence on the finally obtained lead recovery conversion rate, and the method can realize the rapid improvement of the lead recovery conversion rate by adopting a microwave treatment mode and has a good effect.
Further, based on (NH) generated in the process of lead recovery as described above4)2SO4The solution and the desulfurization transforming agent can be recycled and further determined by further detection, the details are as the following example 5:
example 5
(NH) after completion of the electrolysis in example 34)2SO4The electrolyte is reused for treating the waste lead plaster, and the ratio of the amount of carbonate in the electrolyte to the amount of sulfate in the waste lead plaster is set to be 1.5: the results of the X-ray diffraction detection of the treated lead paste are shown in FIG. 1. As can be seen from the figure, (PbCO)3)Pb(OH)2The characteristic diffraction peak of (a) is very distinct. Therefore, it was confirmed that the carbonate or bicarbonate contained in the electrolytic solution after electrolysis can be reused for the conversion treatment of the waste lead paste.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or system. Without further limitation, an element described by the phrase "comprising" does not exclude the presence of other identical elements in a process, method, article, or system that comprises the element. The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments.
The above description is only a preferred 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 (10)

1. The method for recycling and treating the waste lead paste is characterized by comprising the following steps of:
(1) pretreatment: mixing the waste lead plaster with a transforming agent to obtain a solution A and a material B;
(2) microwave treatment: mixing the material B with a carbon material and carrying out microwave heating treatment to obtain a mixture C;
(3) preparing slurry: mixing the mixture C with auxiliary materials to obtain slurry;
(4) recovering metal lead: and (3) uniformly coating the obtained slurry on a cathode plate, and carrying out electrolytic reaction in an inert atmosphere by using the solution A as an electrolyte to obtain metallic lead and a solution D, wherein the solution D contains a conversion agent required in the step (1).
2. The method for recycling and processing waste lead paste according to claim 1, wherein the step (1) specifically comprises: mixing a certain amount of ammonium bicarbonate or ammonium carbonate solution with the waste lead paste to obtain PbCO3Precipitation and (NH)4)2SO4And (3) solution.
3. The method for recycling waste lead paste according to claim 2, wherein the ratio of the amount of sulfate radicals to the amount of ammonium bicarbonate or ammonium carbonate in the waste lead paste is 1: 2.0-2.4 and 1: 1.0 to 1.2.
4. The method for recycling and treating waste lead paste according to claim 2 or 3, wherein the carbon material comprises one or more of activated carbon, acetylene black, carbon nanotubes and graphene.
5. The method for recycling and treating waste lead plaster according to claim 4, wherein the auxiliary material is uniformly dispersed PVDF-polyvinylidene fluoride in NMP-N-methyl pyrrole.
6. The method according to claim 5, wherein the carbon material is acetylene black, and the PbCO is used as the material3And the mass ratio of PVDF to acetylene black is 1: 0.001 to 0.003: 0.1 to 0.5.
7. The method for recycling waste lead paste according to claim 5 or 6, wherein the microwave heating treatment in the step (2) has a microwave power of 500-1000W and a heating time of 0.5-3 min.
8. The method for recycling waste lead paste as claimed in claim 7, wherein the inert atmosphere in the step (4) is CO2Nitrogen and helium, and the pressure range is 100 kPa-110 kPa.
9. The method for recycling waste lead paste as claimed in claim 7, wherein the pH value of the electrolysis reaction in the step (4) is 8.5-10.5, and (NH) in the electrolyte4)2SO4The concentration is 100-400 g/L, and the electrolysis temperature is 0-60 ℃.
10. The waste lead plaster recycling method according to claim 8 or 9, wherein the solution D is subjected to a recycling pretreatment so that the ratio of the amount of carbonate in the solution to the amount of sulfate in the waste lead plaster to be treated is 1.0-2.2: 1.
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