CN111048777A - High-porosity EVF series lead storage battery positive electrode lead plaster and plaster mixing method thereof - Google Patents
High-porosity EVF series lead storage battery positive electrode lead plaster and plaster mixing method thereof Download PDFInfo
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- CN111048777A CN111048777A CN201911289754.2A CN201911289754A CN111048777A CN 111048777 A CN111048777 A CN 111048777A CN 201911289754 A CN201911289754 A CN 201911289754A CN 111048777 A CN111048777 A CN 111048777A
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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
- H01M4/57—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead of "grey lead", i.e. powders containing lead and lead oxide
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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
- H01M4/14—Electrodes for lead-acid accumulators
- H01M4/16—Processes of manufacture
- H01M4/20—Processes of manufacture of pasted electrodes
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses an EVF series lead storage battery anode lead plaster with high porosity, which consists of lead powder, sulfuric acid solution and an additive, wherein the additive consists of the following raw materials in parts by weight according to 1000 parts by weight of the lead powder: 0.4-0.6 part of graphite, 0.5-0.7 part of stannous sulfate, 0.7-0.9 part of antimony oxide, 0.9-1.1 part of magnesium carbonate and 1.4-1.6 parts of short fibers. The invention also provides a paste mixing method of the EVF series lead storage battery anode lead paste with high porosity, which comprises the steps of premixing all raw materials except the sulfuric acid solution, adding the sulfuric acid solution, uniformly mixing, controlling the highest temperature to be 82-85 ℃ in the paste mixing process and controlling the paste outlet temperature to be not higher than 45 ℃. The lead plaster has uniform overall particle size and high porosity, and can improve the low-temperature performance and the battery cycle performance of the lead storage battery.
Description
Technical Field
The invention relates to the technical field of lead storage batteries, in particular to EVF series lead storage battery positive electrode lead plaster with high porosity and a plaster mixing method thereof.
Background
The EVF series lead storage battery refers to a lead acid storage battery for an electric road vehicle. The formula of the green plate and the paste mixing process are very important processes in the production process of the lead-acid storage battery. In the paste mixing process of the green plate, the metal lead is further oxidized to generate lead oxide, tribasic lead sulfate and tetrabasic lead sulfate in a certain proportion are also formed, different porosities are formed by the lead paste prepared by the paste mixing process, and the binding capacity and the skeleton structure of the active substance are enhanced, so that the formula additive and the paste mixing process are particularly critical.
Since the paste is a process of mixing various substances, there are both physical and chemical changes in the process, and a skeleton of different structure is formed as the transfer process proceeds. Meanwhile, the lead plaster colloid must be ensured to well complete the oxidation of metallic lead and the recrystallization process of various basic lead sulfates.
The patent specification with the publication number of CN 109273712A discloses a lead storage battery anode lead plaster and a preparation method thereof, wherein the anode lead plaster comprises lead powder, an additive, water and a sulfuric acid solution, and the additive comprises 3-7 parts of lead dioxide, (iso) nicotinamide 0.001-0.1 part, 0.01-0.5 part of polyester fiber, 0.02-0.5 part of antimony trioxide, 0.02-0.5 part of stannous sulfate and 0.02-0.2 part of a carbon material based on 100 parts of the lead powder by weight. The oxidation degree of the lead powder is 75-80%, and the density of the sulfuric acid solution is 1.40g/cm3。
Patent specification with publication number CN 107887591 a discloses lead paste and paste for improving the binding force between the positive grid and the lead paste of a lead-acid storage battery and a preparation method thereof. Adding lead powder accounting for 80-90% of the total mass into a paste mixer, then adding 8-10% of sulfuric acid, 0.1-0.3% of stannous sulfate, 0.08-010% of conductive fiber, 0.3-0.5% of colloidal graphite, 0.05-0.15% of sodium borate and 1.0-1.2% of antimony oxide, mixing for 8-10 min in a dry mode, adding deionized water, mixing for 2min in a wet mode, adding the rest paste, and mixing for 8-10 min in a wet mode; dropwise adding sulfuric acid accounting for 8-10% of the total mass, and stirring after dropwise addingStirring for 10-12 min to obtain the product with apparent density of 4.4 +/-0.02 g/cm3The lead paste of (1). The mass percentage concentration of the sulfuric acid is 50%.
Disclosure of Invention
Aiming at the defects in the field, the invention provides the EVF series lead storage battery anode lead plaster with high porosity, the overall grain size of the lead plaster is uniform, the porosity is high, and the low-temperature performance and the battery cycle performance of the lead storage battery can be improved.
The EVF series lead storage battery positive lead plaster with high porosity comprises lead powder, sulfuric acid solution and an additive, wherein the additive comprises the following raw materials in parts by weight according to 1000 parts by weight of the lead powder:
in the formula of the EVF series lead storage battery positive lead plaster with high porosity, on one hand, the addition of red lead powder is cancelled, the contents of stannous sulfate and antimony oxide are reduced, the cost is reduced, and the negative antimony effect (such as influence on self-discharge performance) possibly brought by the antimony oxide is avoided; on the other hand, the components which are not used in the field of positive lead plaster of EVF series lead storage batteries, namely magnesium carbonate, are added for the first time, and the addition of the magnesium carbonate can reduce the addition of stannous sulfate and antimony oxide, thereby being beneficial to the formation of pores in the lead plaster. In addition, the lead plaster formula of the invention increases the content of short fiber, and can obviously improve the pole plate adhesive force.
Preferably, the degree of oxidation of the lead powder is 62% to 68%. The oxidation degree of the lead powder in the lead plaster formula is obviously lower than that of the conventional formula (the oxidation degree of the lead powder is generally 72-80%). According to the invention, the oxidation degree of the lead powder is reduced, the red lead powder is not added, the proportion of the metallic lead is obviously improved, the capacity of the lead powder is favorably improved, the energy efficiency is improved, and the generation of basic lead sulfate crystals is promoted by further oxidizing the metallic lead in the paste mixing process, so that the low-temperature performance and the battery cycle performance of the lead storage battery are improved.
Preferably, the sulfuric acid solution is 225-235 parts by weight, the density of the sulfuric acid solution is 1.15-1.17 g/mL, the low-density (low-concentration) sulfuric acid solution is adopted in the lead paste formula to replace a conventional high-density (high-concentration) sulfuric acid solution (the density of the sulfuric acid solution is generally 1.40g/mL) and additional water needs to be added, so that a water adding step can be omitted in the process of the lead paste and the paste, the acid adding time is prolonged, the lead paste is dispersed more uniformly, and the porosity and the α -PbO content of the obtained lead paste are improved.
In a preferred example, the positive electrode lead paste of the EVF series lead storage battery with high porosity comprises the following raw materials in parts by weight:
the density of the sulfuric acid solution was 1.16 g/mL.
The positive lead plaster of the EVF series lead storage battery obtained by the components and the mixture ratio has the best porosity and the best basic lead sulfate crystal content, and has the best low-temperature performance and battery cycle performance.
The invention also provides a paste mixing method of the EVF series lead storage battery anode lead paste with high porosity, which comprises the steps of premixing all raw materials except the sulfuric acid solution, adding the sulfuric acid solution, and uniformly mixing.
The method and the paste method of the invention omit the step of adding water, simplify the working procedure, thus can prolong the acid adding time under the condition of ensuring the time of the total process to be unchanged, lead paste is dispersed more uniformly, and the porosity and α -PbO content of the obtained lead paste are improved.
Preferably, the highest temperature in the paste mixing process is controlled to be 82-85 ℃, the paste outlet temperature is not higher than 45 ℃, the highest temperature of the conventional paste mixing process is usually controlled to be not higher than 80 ℃, such as 70-75 ℃, while the highest temperature in the paste mixing process controlled by the paste mixing method is 82-85 ℃, and the higher paste mixing temperature is favorable for forming a better loose skeleton structure, improving the porosity of the lead paste, improving the content of α -PbO and improving the strength of the polar plate.
The duration of adding the sulfuric acid solution is 18-22 min, and the time for adding the sulfuric acid solution is prolonged, so that the oxidation of metallic lead and the generation of basic lead sulfate crystals are facilitated.
Preferably, the apparent density of the prepared EVF series lead storage battery positive electrode lead paste with high porosity is 4.30-4.40 g/cm3Reflecting the high porosity of the resulting lead paste.
The paste mixing method is matched with the lead paste formula, and the positive lead paste with more excellent performance can be prepared.
Compared with the prior art, the invention has the main advantages that:
1. the invention improves the proportion of metallic lead by reducing the oxidation degree of lead powder and eliminating the addition of red lead powder, is beneficial to improving the productivity of the lead powder and improving the energy efficiency, and promotes the generation of basic lead sulfate crystals by further oxidizing the metallic lead in the paste mixing process, thereby improving the low-temperature performance and the battery cycle performance of the lead storage battery.
2. Magnesium carbonate is adopted to replace part of stannous sulfate and antimony oxide, so that the cost is reduced, the negative antimony effect (such as influence on self-discharge performance) possibly brought by the antimony oxide is avoided, pores are formed in the lead paste, and the low-temperature performance and the battery cycle performance of the lead storage battery are improved.
3. The lead plaster formula of the invention increases the content of short fiber, and can obviously improve the pole plate adhesive force.
Drawings
FIG. 1 is an SEM photograph of a lead paste obtained by an EVF series lead storage battery positive electrode lead paste formulation and paste method according to a comparative example;
fig. 2 is an SEM photograph of a lead paste obtained by the EVF series lead storage battery positive electrode lead paste formulation and paste method according to the example.
Detailed Description
The invention is further described with reference to the following drawings and specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are conducted under conditions not specified, usually according to conventional conditions, or according to conditions recommended by the manufacturer.
Formulations of positive electrode lead pastes for EVF series lead storage batteries of examples and comparative examples are shown in table 1 below, and commercially available products are used unless otherwise specified.
TABLE 1 EVF SERIES LEAD ACCUMULATOR POSITIVE ELECTRODE LEAD PASTE FORMULATION (in 1000kg LEAD POWDER)
| Name of Material | Unit of | Comparative example | Examples |
| Degree of oxidation of lead powder | ％ | 72～78％ | 62～68％ |
| Red lead | kg | 100±2 | / |
| Graphite (II) | g | 500±0.2 | 500±0.2 |
| Stannous sulfate | g | 1000±0.2 | 600±0.2 |
| Antimony oxide | g | 1500±0.2 | 800±0.2 |
| Magnesium carbonate | g | / | 1000±0.2 |
| 1.40. + -. 0.002g/mL sulfuric acid solution (25 ℃ C.) | kg | 99±1 | / |
| 1.16. + -. 0.002g/mL sulfuric acid solution (25 ℃ C.) | kg | / | 2305±2 |
| Short fiber | g | 950±5 | 1500±5 |
| Pure water | kg | 115±10 | / |
The positive electrode lead paste mixing method of EVF series lead storage batteries of examples and comparative examples is shown in table 2 below.
TABLE 2 EVF-SERIES LEAD BATTERY POSITIVE ELECTRODE LEAD PASTE MIXING METHOD
The shapes of the lead pastes obtained by the positive electrode lead paste formula and the paste method of the EVF series lead storage batteries according to the comparative example and the example are respectively shown in figures 1 and 2. As can be seen from FIG. 1, the lead pastes of the comparative examples had large differences in the sizes of the respective particles, small overall voids, and many particles were in the form of blocks or flakes, and it was judged from the characteristics of the tetrabasic lead sulfate and tribasic lead sulfate crystals that the tetrabasic lead sulfate crystals accounted for a very small proportion. As can be seen from fig. 2, the overall lead paste particle size of the example is relatively uniform, with a majority of the particles being acicular crystals and uniformly distributed, with little agglomeration, high porosity, and a distinct skeletal structure being seen. Obviously, the lead paste morphology of the examples meets the conditions for preparing high capacity, high and low temperature performance, long life batteries.
The positive electrode plate of E16A was prepared using the positive electrode pastes for EVF series lead storage batteries of examples and comparative examples, respectively, and the positive electrode plate strength, free lead content by mass and moisture content by mass were measured, and the results are shown in table 3 below. Wherein, the strength test adopts the ratio of the weight lost after the positive plate respectively falls off from the positive plate for 6 times and the negative plate for 6 times.
TABLE 3
As can be seen from Table 3, the content of free lead and moisture in the positive plate obtained by using the lead paste of the embodiment meets the industrial requirements of lead storage batteries, the strength of the positive plate is obviously improved compared with that of the positive plate obtained by using the conventional process, and the absolute value of the loss mass of the No. 6 positive plate is less than half of that of the loss mass of the No. 1 positive plate.
XRD was used to test the above E16A positive plate lead pastes, and the contents of α -PbO and β -PbO are shown in Table 4 below.
TABLE 4
It is generally recognized in the art that α -PbO contributes significantly to the cycle life of the battery, it can be seen from Table 4 that the α -PbO content of the example lead paste is significantly higher than that of the comparative example, so that the positive electrode obtained using the example lead paste should have better cycle life capacity and cycle number than the positive electrode plate obtained using the comparative example lead paste.
Assembled 6-EVF-80 batteries (E16A plate 5 positive/6 negative) were prepared using the EVF series lead storage battery positive electrode pastes of examples and comparative examples, respectively, and tested for low temperature performance and cycle life according to GB/T32620.1-2016, with the results shown in Table 5 below.
TABLE 5
Therefore, the proportion of metallic lead is improved by reducing the oxidation degree of the lead powder and eliminating the addition of the red lead powder, and the magnesium carbonate is adopted to replace part of stannous sulfate and antimony oxide, so that the cost is reduced, the negative antimony effect (such as influence on self-discharge performance) possibly brought by the antimony oxide is avoided, the formation of pores in lead paste is facilitated, the content of α -PbO is increased, and the low-temperature performance and the battery cycle performance of the lead storage battery are improved.
Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the above description of the present invention, and equivalents also fall within the scope of the invention as defined by the appended claims.
Claims (8)
1. The EVF series lead storage battery positive lead plaster with high porosity consists of lead powder, sulfuric acid solution and an additive, and is characterized in that the additive consists of the following raw materials in parts by weight, wherein the weight of the lead powder is 1000 parts:
2. the high porosity EVF series lead storage battery positive lead paste according to claim 1, wherein the degree of oxidation of the lead powder is 62% to 68%.
3. The high-porosity positive lead paste for EVF-series lead storage batteries according to claim 1, wherein the sulfuric acid solution is 225 to 235 parts by weight and has a density of 1.15 to 1.17 g/mL.
4. The EVF series lead storage battery positive electrode lead paste with high porosity according to any one of claims 1 to 3, which is characterized by comprising the following raw materials in parts by weight:
the density of the sulfuric acid solution was 1.16 g/mL.
5. The method for mixing positive electrode lead plaster of EVF series lead storage batteries with high porosity according to any one of claims 1 to 4, wherein all raw materials except sulfuric acid solution are premixed, and then sulfuric acid solution is added to be uniformly mixed.
6. The method for pasting the positive electrode lead paste for the EVF series lead storage battery with high porosity according to claim 5, wherein the maximum temperature in the pasting process is controlled to be 82-85 ℃, and the paste outlet temperature is not higher than 45 ℃.
7. The method for pasting a positive electrode lead paste for a high-porosity EVF series lead storage battery according to claim 5, wherein the duration of the sulfuric acid solution addition is 18-22 min.
8. The paste mixing method for the positive electrode lead paste of the high-porosity EVF-series lead storage battery according to claim 5, wherein the apparent density of the prepared positive electrode lead paste of the high-porosity lead storage battery is 4.30-4.40 g/cm3。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112151776A (en) * | 2020-08-21 | 2020-12-29 | 安徽理士电源技术有限公司 | Long-life silicon-based bipolar lead storage battery anode lead paste and preparation method thereof |
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