CN113097443B - Tubular positive plate prepared from tubular positive waste lead paste and preparation method thereof - Google Patents
Tubular positive plate prepared from tubular positive waste lead paste and preparation method thereof Download PDFInfo
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- CN113097443B CN113097443B CN202110336523.3A CN202110336523A CN113097443B CN 113097443 B CN113097443 B CN 113097443B CN 202110336523 A CN202110336523 A CN 202110336523A CN 113097443 B CN113097443 B CN 113097443B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
- H01M10/12—Construction or manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/56—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides 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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a method for preparing a positive active material by utilizing an atom economic method for waste lead paste of a tubular positive electrode of a lead-acid battery and a tubular positive plate of the lead-acid battery, which comprises the steps of mechanically crushing the waste lead-acid battery, sorting out the waste lead paste of the positive electrode, crushing into fine powder with a certain size, removing a carbonaceous additive in the waste lead paste of the positive electrode by a powder dust remover, adding lead powder and a grinding aid according to the content of PbO2 in the waste lead paste of the positive electrode after dust removal, carrying out ball milling reaction to prepare mixed powder taking PbSO4, PbO2 and 4BS as main components, and finally mechanically mixing with a certain amount of acetylene black, filling powder, water leaching and melting to prepare the positive plate of the lead-acid battery. The invention shortens the process route of the traditional 'waste lead paste → lead prepared by fire method or wet method smelting → lead prepared by ball milling or gas phase oxidation method', the prepared active substance replaces the lead-acid battery positive plate prepared by the traditional lead powder, and the initial capacity and the cycle life are equivalent to those of the lead-acid battery positive plate prepared by the traditional lead powder.
Description
Technical Field
The invention relates to the technical field of waste lead-acid battery recycling, in particular to a method for preparing a positive plate by utilizing a tubular positive electrode waste lead plaster atom economic method of a lead-acid battery and a tubular positive plate of the lead-acid battery.
Background
The lead-acid storage battery mainly comprises five parts, namely a positive plate, a negative plate, a diaphragm, electrolyte and a shell. The lead-acid storage battery can realize the mutual conversion between chemical energy and electric energy in the charging and discharging processes, the working principle of the lead-acid storage battery is named as a bipolar sulfate theory, and the electrode reaction equations are shown as (1), (2) and (3):
and (3) positive electrode reaction: PbO2+4H++SO4 2-+2e＝PbSO4+2H2O (1)
And (3) cathode electrode reaction: pb + SO4 2--2e＝PbSO4 (2)
Overall reaction of the cell: PbO2+Pb+2H2SO4＝2PbSO4+2H2O (3)
The active material PbO2 of the positive electrode and Pb of the negative electrode react with the electrolyte sulfuric acid to generate soft PbSO4 crystals which are uniformly dispersed in the electrode plate when the battery is charged, and the PbSO4 crystals on the electrode plate are restored to original PbO2 and spongy Pb when the battery is discharged.
As the battery is repeatedly charged and discharged during use, the soft PbSO4 crystals on the electrode plate are dissolved and recrystallized for multiple times to form a large and poor-conductivity PbSO4 crystals, and the large and poor-conductivity PbSO4 crystals cannot be completely converted into the active material PbO2 and spongy Pb during charging, and the vulcanization phenomenon is called irreversible sulfation. The irreversible PbSO4 crystal blocks micro-pores on the polar plate, prevents the electrolyte from permeating, increases the internal resistance, reduces active substances, reduces the battery capacity and shortens the service life of the lead-acid storage battery until the lead-acid storage battery is scrapped. In addition, during the repeated charge and discharge of the positive plate of the lead-acid battery, the alpha-PbO 2 which plays a skeleton role is continuously consumed, so that the porous structure of the positive plate which plays a supporting role is damaged, the positive electrode is softened, the real electrode area participating in the reaction is reduced, the battery capacity is reduced, and the service life is also stopped.
The waste lead-acid storage battery consists of 11-30% of waste electrolyte, 24-30% of lead alloy grid, 22-30% of organic matter and 30-40% of lead plaster. The electrolyte mainly contains a large amount of sulfuric acid, is relatively easy to recover, can be recycled as the electrolyte of a new lead-acid storage battery after separation and purification, and can also be used as industrial-grade sulfuric acid; the slab lattice is mainly metal lead, and is smelted into new slab lattice or high purity lead, and the organic matter is mainly plastic casing, partition, hard rubber, etc. for battery, and may be regenerated and reused as side product. The lead plaster is a layer of pasty substance which is attached to a polar plate after the active substance on the polar plate gradually exchanges components with electrolyte after the battery is subjected to multiple charging and discharging cycles and is dissolved and separated out for multiple times, and the main components of the lead plaster are 50-60% of lead sulfate, 20-30% of lead dioxide, 5-15% of lead oxide and 1-2% of metallic lead. Lead sulfate in the lead plaster has stable property, high melting point and decomposition temperature, is difficult to recycle, and lead dioxide has strong oxidizing property, is insoluble in oxidizing acid and alkali, and can be converted into a relatively pure product after being reduced in the conversion treatment of the lead plaster, so the conversion treatment of the lead sulfate and the lead dioxide in the lead plaster becomes the difficult point and the key point of the conversion treatment of the lead plaster.
The conventional method for treating the waste lead plaster of the lead-acid battery mainly comprises a pyrometallurgical process, a wet-pyrometallurgical combined smelting process and a wet electrolysis process, wherein the pyrometallurgical regeneration smelting process needs to heat PbSO4 in the lead plaster to the temperature of over 1000 ℃ for complete decomposition, a large amount of SO2 is generated in the process, and meanwhile, a large amount of lead is volatilized and lost at high temperature to form polluting lead dust. The process for recovering and treating the lead plaster by combining the wet method and the fire method is to convert lead sulfate in the lead plaster into a lead salt compound which can be decomposed at low temperature by utilizing a chemical reaction and then recover lead in the lead by a low-temperature smelting method, and generally about 5 percent of PbSO4 remains in the converted lead plaster due to the problem of the conversion efficiency of desulfurization conversion, and the problem of SO2 emission still occurs in the smelting process. The wet process for recovering lead mainly comprises a solid-phase electrolysis method, a direct leaching-electrolytic deposition method, a desulfurization conversion-reduction leaching-electrolytic deposition method and the like, and the lead plaster in a liquid phase is subjected to electrolytic deposition treatment by utilizing a chemical method. The wet process solves the problems of SO2 emission in the pyrometallurgical process and lead volatilization at high temperature. However, the process is large in investment, and the energy consumption for producing 1kg of lead is about 12kWh, which is higher than that of the traditional pyrometallurgical process.
The waste lead paste is subjected to pyrometallurgical or electrowinning hydrometallurgy with high energy consumption to recover metal Pb, the metal Pb is used as a raw material for manufacturing an active substance for producing the lead-acid storage battery plate again, the step of preparing lead powder with PbO as a main component by a ball milling method or a gas phase oxidation method is required, the added positive electrode additive 4BS needs to undergo a reaction step between PbO and H2SO4, and the additive red lead or lead dioxide needs to be prepared by high-temperature oxidation of lead. It seems that the lead-acid battery has the advantages of easy recovery and reuse and realization of battery cycle production, but the cycle production route is long, the cost is high, and the environmental pollution is large.
The method is characterized in that the method comprises the steps of mixing positive lead plaster and negative lead plaster, then uniformly treating the mixed positive lead plaster and negative lead plaster, wherein the components of the positive pole of the tubular lead-acid battery are relatively simple except for carbon materials such as lead sulfate, lead dioxide, carbon black, graphene and the like, and the mixed treatment of the positive pole lead plaster and the negative lead plaster is equivalent to introducing more impurities into the positive waste lead plaster, so that the treatment process is prolonged, and the treatment cost is increased.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for preparing a positive plate by utilizing a tubular positive waste lead paste atom economic method of a lead-acid battery and the tubular positive plate of the lead-acid battery, which avoid the defects of high-temperature high pollution of a pyrometallurgical process and the consumption of a large amount of desulfurizer, reducer and electric energy of a pyrometallurgical-hydrometallurgical combined smelting process and a hydrometallurgical process, simplify the process route of the traditional 'waste lead paste → smelted lead → lead powder preparation → lead powder production → production', directly add a certain amount of lead powder according to the relative contents of main components PbSO4 and PbO2 of the positive waste lead paste, lead powder in the positive plate reacts with PbO2 to generate PbO and PbO reacts with PbSO4 to generate basic lead sulfate 4BS through ball milling reaction, control the proportion of PbO2 in the positive powder after the ball milling reaction through a certain lead powder adding amount, and prepare the positive powder with high-activity PbSO4, 4 and electric energy, The mixed powder of PbO2 and 4BS is used as the raw material for preparing the anode, so that the step of adding red lead and 4BS additionally and the reagent consumption in the traditional anode preparation are saved, the grinding aid additionally introduced in the waste lead paste treatment process is removed through the water immersion step after powder filling, the requirement of the anode preparation on the content limitation of impurities is ensured, and the anode preparation process is simplified due to the change of the raw material for preparing the anode.
(II) technical scheme
The invention provides a method for preparing a positive plate by utilizing a tubular positive waste lead plaster atom economic method of a lead-acid battery, which specifically comprises the following steps:
s1, mechanically crushing the waste lead-acid battery, sorting the positive waste lead paste, and crushing the positive waste lead paste into fine powder with a certain size;
s2, removing the carbonaceous additive in the crushed anode waste lead plaster through a powder dust remover, and detecting the content of each component in the waste lead plaster;
s3, adding lead powder and grinding aid according to the content of PbO2 in the dedusted waste positive lead paste, and performing ball milling reaction to obtain positive mixed powder with 4BS, PbO2 and PbSO4 as main components;
s4, the prepared positive electrode mixed powder replaces the traditional lead powder to be mechanically mixed with acetylene black, and then the mixture is subjected to powder filling and water leaching to form the tubular positive plate for preparing the lead-acid battery.
In the step S1, the waste positive lead paste is washed with pure water and dried, and then is pulverized by a ball mill, wherein the rotation speed of the ball mill is 200-. The lead plaster particles after being crushed are 40-120 mu m.
In step S2, the dust remover may be a cyclone separator or a gravity settling chamber.
In step S3, the lead powder is added with ingredients according to the content of PbO2 in the waste lead paste and the content of PbO2 in the finally prepared anode powder, and then ball milling reaction is performed, wherein the ball milling rotation speed is 300-.
In step S4, after powder filling, soaking, removing grinding aid, and directly carrying out formation operation, wherein the formation current density is 1/3-1/2 of the formation current density of the conventional lead powder as raw material.
The invention also provides a tubular positive plate of the lead-acid battery, which is prepared by the method provided by the invention.
(III) advantageous effects
The invention provides a method for preparing a positive plate by utilizing a lead-acid battery tubular positive electrode waste lead paste atomic economic method and a lead-acid battery tubular positive plate, which have the following beneficial effects:
the method has the advantages that the waste positive lead plaster is treated by a ball milling method, the powder for preparing the positive electrode is directly produced, the resource utilization route of the traditional waste lead plaster for preparing the positive electrode raw material of the lead-acid battery is shortened, additives such as grinding aids are added, and the problems that in the later stage of ball milling, due to the fact that the surfaces of microparticles are in a metastable high-energy state, aggregates which are difficult to disperse again are formed, and the ball milling difficulty is increased are solved; meanwhile, additives such as grinding aids and the like are added, so that the activity of a ball-milled product is improved, the electric energy consumption in the formation process is reduced, and the initial capacity of the anode is improved; due to the water solubility of additives such as grinding aids and the like, the additives can be automatically removed from the anode raw material in the soaking stage after powder filling, and can be recycled; because the product of the waste lead plaster treated by the atom economic method directly comprises the positive active substance PbO2 or PbSO4 which can be converted into the active substance after formation and 4BS which has important influence on the service life of the positive electrode, the extra reagent consumption in the preparation process of the traditional positive plate is saved, and the preparation process of the positive electrode is simplified. Compared with the traditional lead-acid battery waste lead plaster treatment method, the method has the advantages of high-efficiency utilization of resources, environmental protection and simplified preparation process.
Drawings
FIG. 1 is a schematic flow chart of the practice of the present invention.
Detailed Description
FIG. 1 is a schematic flow chart of the present invention for preparing a positive plate of a lead-acid battery by using an economic method of using waste lead paste atoms of a tubular positive electrode of the lead-acid battery. As shown in fig. 1, S1, mechanically crushing the waste lead-acid battery, sorting the positive waste lead paste, and crushing the positive waste lead paste into fine powder with a certain size;
s2, removing the carbonaceous additive in the crushed anode waste lead plaster through a powder dust remover, and detecting the content of each component in the waste lead plaster;
s3, adding a certain amount of lead powder and grinding aid according to the content of PbO2 in the dedusted waste positive lead paste, and carrying out ball milling reaction to obtain positive mixed powder with 4BS, PbO2 and PbSO4 as main components;
s4, the prepared positive electrode mixed powder replaces the traditional lead powder to be mechanically mixed with acetylene black, and then the mixture is subjected to powder filling and water leaching to form and prepare the positive plate of the lead-acid battery.
In S1, the waste positive lead paste is washed and dried by pure water, and then is crushed by a ball mill, wherein the rotation speed of the ball mill is 200-300 r/min, and the ball milling time is 15-20 min. The lead plaster particles after being crushed are 40-120 mu m; in S2, the powder dust collector may use a cyclone separator or a gravity settling chamber; in S3, the lead powder is added according to the content of PbO2 in the waste lead paste and the content of PbO2 in the finally prepared anode powder, and then ball milling reaction is carried out, wherein the reaction conditions are ball milling rotating speed of 300-; s4, in the preparation process of the positive plate, after powder filling, soaking and grinding aid removal, formation operation is directly carried out, and the formation current density is 1/3-1/2 of the formation current density when conventional lead powder is used as a raw material.
The method for preparing the positive active material from the waste lead paste for the tubular positive electrode of the lead-acid battery and the tubular positive plate of the lead-acid battery proposed in the present invention will be further explained with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
(1) Crushing of tubular anode waste lead plaster
And washing the waste lead-acid battery pole plate by pure water, mechanically crushing, and sorting out the positive waste lead paste.
(2) Impurity removal and component analysis of waste positive lead paste
120g of crushed anode waste lead plaster powder is taken to pass through a cyclone separator, carbonaceous additives are separated, the mass is 119.5g, the mass fraction of PbSO4 is analyzed to be 72%, the mass fraction of PbO2 is analyzed to be 28%, and the powder is crushed into 100 mu m.
(3) Ball milling reaction
119.5g of crushed and impurity-removed anode waste lead paste is added with 10g of pure lead powder for ball milling reaction to prepare anode mixed powder with 4BS, PbO2 and PbSO4 as main components.
(4) Positive plate preparation
And adding 0.4g of acetylene black into the prepared positive electrode mixed powder, mixing, filling the powder, soaking in water, and forming into a positive plate with the electric quantity of 10C 10.
(5) Positive plate Performance test
1 positive plate and 2 negative plates with excessive capacity are assembled into a simulated battery, and the battery is discharged at a constant current of I2 until the battery voltage is 1.75V, and the discharge capacity of the positive plate is 4.72 A.h; for comparison, the discharge capacity of the positive electrode plate made of the same equivalent amount of lead powder was measured to be 4.74A · h.
The simulated battery is charged for 42min at a constant current of 2I2 and then discharged for 18min at a constant current of 4I2, the cycle is repeated, the capacity is recovered once after 30 times of charging and discharging in each cycle, when the voltage is continuously lower than 1.75V for 3 times after discharging, the cycle is stopped, and the cycle number is recorded as 196 times. For comparison, the cycle life of the positive plate made of the same equivalent lead powder is measured to be 202 times by the experiment.
Example 2
(1) Crushing of tubular anode waste lead plaster
And washing the waste lead-acid battery pole plate by pure water, mechanically crushing, and sorting out the positive waste lead paste.
(2) Impurity removal and component analysis of waste positive lead paste
120g of crushed anode waste lead plaster powder is taken to pass through a cyclone separator, carbonaceous additives are separated, the mass is 119.4g, the mass fraction of PbSO4 is analyzed to be 72%, the mass fraction of PbO2 is analyzed to be 28%, and the powder is crushed into 50 mu m.
(3) Ball milling reaction
119.4g of crushed and impurity-removed anode waste lead paste is added with 10g of pure lead powder for ball milling reaction to prepare anode mixed powder with 4BS, PbO2 and PbSO4 as main components.
(4) Positive plate preparation
The prepared positive electrode mixed powder was added with 0.4g of acetylene black, and after mixing, powder filling was performed to prepare a positive electrode plate having the same specification as in example 1, which was then immersed in water to obtain a positive electrode plate having an electric quantity of 10C 10.
(5) Positive plate Performance test
According to the same test method as in example 1, the positive electrode plate capacity was 4.735A · h, and the lifetime was 199 times.
Example 3
(1) Crushing of tubular anode waste lead plaster
Washing the waste lead-acid battery pole plate with purified water, mechanically crushing, sorting out positive waste lead paste, analyzing that the mass fraction of PbSO4 is 72% and the mass fraction of PbO2 is 28%, and crushing the positive waste lead paste into 50 mu m.
(2) Impurity removal and component analysis of waste positive lead paste
120g of crushed anode waste lead plaster powder is taken to pass through a cyclone separator, and the mass is 119.4g after carbonaceous additives are separated.
(3) Ball milling reaction
119.4g of crushed and impurity-removed anode waste lead paste is added with 20g of pure lead powder for ball milling reaction to prepare anode mixed powder with 4BS, PbO2 and PbSO4 as main components.
(4) Positive plate preparation
The prepared positive electrode mixed powder was added with 0.4g of acetylene black, and after mixing, powder filling was performed to prepare a positive electrode plate having the same specification as in example 1, which was then immersed in water to obtain a positive electrode plate having an electric quantity of 10C 10.
(5) Positive plate Performance test
According to the same test method as in example 1, the positive electrode plate capacity was 4.755A · h, and the lifetime was 201 times.
Example 4
(1) Tubular anode waste lead plaster crushing
Washing the waste lead-acid battery pole plate with purified water, mechanically crushing, sorting out positive waste lead paste, analyzing that the mass fraction of PbSO4 is 72% and the mass fraction of PbO2 is 28%, and crushing the positive waste lead paste into 50 mu m.
(2) Impurity removal and component analysis of waste positive lead paste
120g of crushed anode waste lead plaster powder is taken to pass through a cyclone separator, and the mass is 119.4g after carbonaceous additives are separated.
(3) Ball milling reaction
119.4g of crushed and impurity-removed anode waste lead plaster is added with 20g of pure lead powder and a certain amount of grinding aid to carry out ball milling reaction to prepare anode mixed powder taking 4BS, PbO2 and PbSO4 as main components.
(4) Preparation of Positive plate
And adding 0.4g of acetylene black into the prepared positive electrode mixed powder, mixing, filling powder to prepare a positive plate with the same specification as that of the embodiment 1, then soaking in water to remove the grinding aid, and forming the positive plate with the formation electric quantity of 10C 10.
(5) Positive plate Performance test
According to the same test method as in example 1, the positive electrode plate capacity was 4.788A · h, and the lifetime was 206 times.
The above embodiments are illustrative of the present invention, and are not intended to limit the present invention, and any simple modifications of the present invention are within the scope of the present invention.
Claims (3)
1. A method for preparing a positive plate of a lead-acid battery by using waste lead paste of a tubular positive electrode of the lead-acid battery is characterized by comprising the following steps:
sl, mechanically crushing the waste lead-acid battery, sorting out the waste positive lead plaster, and crushing into fine powder;
s2, removing the carbonaceous additive in the crushed positive waste lead plaster through a powder dust remover;
s3, adding lead powder and grinding aid according to the content of Pb02 in the dedusted waste positive lead paste, and performing ball milling reaction to obtain positive mixed powder with 4BS, Pb02 and PbS04 as main components:
s4, mechanically mixing the prepared positive electrode mixed powder instead of conventional lead powder with acetylene black, filling the powder, soaking in water, and forming a tubular positive plate for preparing the lead-acid battery;
in the step Sl, the waste positive lead plaster is washed and dried by pure water, and then is crushed by a ball mill, wherein the rotating speed of the ball mill is 200-300 r/min, the ball milling time is 15-20 min, and the particle size of the crushed lead plaster is 40-120 m;
in step S3, the lead powder is added according to the content of Pb02 in the waste lead paste and the content of Pb02 in the finally prepared anode powder, and then ball milling reaction is performed, wherein the ball milling rotation speed is 300-;
in the step S4, after powder filling, soaking, removing grinding aids, and directly carrying out formation operation, wherein the formation current density is 1/3-1/2 of the formation current density of the conventional lead powder serving as a raw material.
2. The method of claim 1, wherein in step S2, the dust collector is a cyclone separator or a gravity settling chamber.
3. A positive plate for a lead-acid battery, characterized in that it is obtained by the method of any one of claims 1 to 2.
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| CN104218270A (en) * | 2014-07-01 | 2014-12-17 | 超威电源有限公司 | Method for preparing tetrabasic lead sulfate by using acid leaching byproduct in production of lead acid storage battery positive electrode plate |
| CN105870527B (en) * | 2016-03-30 | 2019-07-16 | 超威电源有限公司 | The processing method of positive plate lead paste in a kind of waste lead acid battery |
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| CN110649345A (en) * | 2019-10-09 | 2020-01-03 | 巨江电源科技有限公司 | Method for recycling waste lead paste in production process of lead-acid storage battery and application of recycled materials |
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| JP2008098009A (en) * | 2006-10-12 | 2008-04-24 | Furukawa Battery Co Ltd:The | Cathode plate for lead-acid battery |
| CN105390763A (en) * | 2015-11-06 | 2016-03-09 | 天能电池集团（安徽）有限公司 | Method for preparing tetrabasic lead sulfate from waste lead plaster |
| CN106684463A (en) * | 2016-07-14 | 2017-05-17 | 安徽轰达电源有限公司 | Method for preparing 4BS seed crystal of lead-acid battery employing grinding method |
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