CN109301172B - Method for curing, heat-treating and drying anode wet green plate - Google Patents
Method for curing, heat-treating and drying anode wet green plate Download PDFInfo
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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
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- 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
- H01M4/21—Drying of pasted electrodes
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Abstract
A method for solidifying, heat-treating and drying a wet positive plate belongs to the technical field of lead-acid storage batteries. The method for curing, heat treating and drying the anode wet green plate is characterized by comprising the following steps: curing the anode wet green plate for 18-40h at the temperature of 40-70 ℃ and the relative humidity of 80% -100%; then setting the temperature to be 150-; preserving the heat for 1.5-5h after the set temperature is reached; after the heat preservation is finished, regulating the pressure release valve to be reduced to a normal pressure state; and finally drying for 3-8h under normal pressure. The invention can realize the heat treatment of the positive grid of the wet green plate in the curing and drying process of the wet green plate, improve the corrosion resistance of the positive grid, effectively shorten the total time of curing and heat treatment drying, and avoid the adverse effects of newly added production procedures, increased transfer workload, prolonged production period and the like caused by independently carrying out heat treatment on the positive lead belt or the grid.
Description
Technical Field
The invention belongs to the technical field of lead-acid storage batteries, and particularly relates to a method for curing, heat-treating and drying a wet positive plate.
Background
The lead belt formed by rolling and the grid prepared by the rolled lead belt are subjected to proper heat treatment, so that the internal residual stress and internal energy of the positive grid alloy of the lead-acid storage battery can be reduced, the grain boundary reconstruction and recrystallization of the grid alloy are promoted, the chemical instability of the grid alloy is reduced, and the corrosion resistance of the positive grid of the lead-acid storage battery is enhanced. The U.S. patent US 6802917B and chinese patents CN 106435421B, CN102925834A and CN1775962A both show beneficial improvement in corrosion resistance of positive grids after heat treatment. But the published heat treatment mode adds a production process, increases the transportation workload, prolongs the production period of the polar plate and brings certain inconvenience to the production.
On the other hand, the curing and drying temperature of the positive plate of the conventional lead-acid storage battery is basically within 90 ℃, the drying time of the wet green plate after the curing stage is as long as 15-30h, and especially when the loading capacity of the wet green plate in a curing chamber is large and the number of stacked wet green plates is large, the time for completely drying the wet green plate is long. Chinese patent CN 1330024C discloses a method for curing by increasing pressure and temperature: the temperature is 115-125 ℃ in the pressure range of 170-230 KPa; or the curing time can be shortened from dozens of hours to 1.5-2 hours under the conditions of the pressure range of 250KPa-360KPa and the temperature of 126-140 ℃, but the drying time is still more than 18 hours. And the curing time disclosed by the patent is too short, and experimental verification shows that the stable transformation of the crystal form of the positive lead plaster substance is difficult to complete within 1.5-2 hours.
Disclosure of Invention
In order to overcome the defects in the background technology, the invention provides a method for curing, heat-treating and drying a wet green plate of a positive electrode, which can realize the heat treatment of the positive plate grid of the wet green plate in the curing and drying process of the wet green plate, improve the corrosion resistance of the positive plate grid, effectively shorten the total time of curing, heat-treating and drying, avoid the adverse effects of newly added production procedures, increased transfer workload, prolonged production period and the like caused by independently heat-treating a positive lead belt or the plate grid, and is more suitable for industrial production and application.
The invention is realized by the following technical scheme: the method comprises the following steps: (1) and (3) curing: curing the positive electrode wet green plate for 18-40h at the temperature of 40-70 ℃ and the relative humidity of 80-100%, wherein the pressure in a curing chamber is in a normal pressure state (1 atm), a circulating fan and atomized water are turned on for humidification, and air doors at an inlet and an outlet are in a timing control state; (2) and (3) a heat treatment temperature rise and pressure rise stage: setting the temperature to be 150-180 ℃, setting the opening pressure of the pressure release valve to be 0.4-0.8Mpa, heating for 1-3 hours, keeping the circulating fan in an open state in the process, closing the air doors of the inlet and the outlet and humidifying atomized water, and introducing compressed air into the curing chamber at regular time; (3) and (3) heat treatment and heat preservation: keeping the temperature for 1.5-5h after the indoor temperature reaches a set value, setting the opening pressure of a pressure release valve to be 0.4-0.8Mpa, keeping the circulating fan in an open state in the heat preservation process, and introducing compressed air into the curing chamber at regular time; (4) a pressure relief stage: after the heat preservation time is up, stopping heating, closing the circulating fan and the compressed air, and regulating the opening degree of the pressure relief valve to reduce the pressure in the curing chamber to the normal pressure state (1 atm) within 20-90 min; (5) and (3) a drying stage: the temperature is 70-100 ℃, the indoor relative humidity is set to be lower than 20%, a circulating fan and an inlet and outlet air door are opened, and drying is carried out for 3-8 h. And after drying is finished, opening the sealing door and moving out the raw plate.
In the step (2) of heat treatment for temperature and pressure rise, the set value of the opening pressure of the pressure release valve is 0.05-0.3 MPa lower than the saturated steam pressure of the water steam at the set temperature.
The set value of the opening pressure of the pressure release valve in the heat treatment and heat preservation stage of the step (3) is 0.05-0.3 MPa lower than the saturated steam pressure of water steam at the set temperature.
The pressure in the curing chamber in the step (3) is not lower than 0.4 Mpa;
the temperature in the curing chamber in the step (3) is not lower than 150 ℃;
the pressure range of the compressed air in the step (2) is 0.6-1.0 MPa;
the pressure range of the compressed air in the step (3) is 0.6-1.0 MPa;
the pressure of the compressed air in the step (2) is not lower than the actual pressure in the curing chamber;
the pressure of the compressed air in the step (3) is not lower than the actual pressure in the curing chamber, so that the compressed air can be smoothly supplemented into the chamber.
In the step (1) of the invention, the curing time is preferably 20 h-25 h;
the heating time in the step (2) is controlled to be 1-2.5 h;
in the step (3), the heat preservation time is preferably 2-3 h;
in the step (4) of the invention, the pressure relief time is preferably 0.5-1 h.
The total time of curing and heat treatment drying of the invention is 24-55 h, preferably 28-38 h.
The timing control state of the inlet and outlet air doors is to set the time interval between the closing and opening of the air doors through PLC programming.
The opening and closing of the pressure relief valve are controlled by monitoring the pressure in the curing chamber, and the pressure relief valve is automatically opened to release the pressure when the pressure in the chamber is higher than a set value; and when the pressure in the chamber is lower than a set value, the pressure release valve is automatically closed. The pressure release valve is used for keeping the pressure in the chamber stable, so that the water vapor in the chamber is in a state close to saturation in the heating and heat preservation processes, and the phenomenon that the water of the polar plate is dissipated too fast is avoided while the thermal motion of water molecules is accelerated. If the heat treatment process only heats and raises the temperature without increasing the internal pressure of the curing chamber, the moisture of the wet green plate is quickly evaporated and dissipated, and the curing effect of the polar plate is influenced.
The curing stage in the step (1) of the invention can be divided into two substeps, wherein the relative humidity of the positive electrode wet-growing plate in the first step is 92-100%, and the relative humidity of the positive electrode wet-growing plate in the second step is 80-90%.
After the positive wet green sheet undergoes the curing stage, the metallic lead content in the lead paste should be not higher than 5%, and if this requirement cannot be met, the curing time needs to be increased appropriately.
The pressure release speed in the pressure release stage can not be too fast, and the total pressure release time is controlled by adjusting the opening of the pressure release valve, so that the pressure is slowly released, and cracks on the surface of the polar plate caused by too fast moisture loss are avoided.
In addition, the rotating speed of the circulating fan can be adjusted, so that the optimal rotating speed of the fan can be selected according to the size of the curing chamber and the curing amount of the wet green plate. The circulating fan has the function of enabling indoor air and moisture to flow and exchange fully, and the uniformity of the air, the moisture and the temperature is guaranteed.
The invention integrates the heat treatment of the positive lead belt or the grid into the curing and drying process of the wet green plate, realizes the heat treatment of the positive wet green plate grid and the rapid curing and drying of the positive wet green plate in one technological process, improves the corrosion resistance of the positive grid and avoids the heat treatment process of independently and newly adding a lead belt or a grid.
The invention has the following beneficial effects: (1) and the corrosion resistance of the positive plate grid is improved. In chinese patent CN 106435421B, published research results show that heat treatment is performed at 150-250 ℃, and the corrosion resistance of the positive grid can be improved by performing obvious grain boundary recombination and recrystallization processes on the positive grid alloy. But when the temperature is higher than 180 ℃, the recrystallization speed of the alloy of the positive plate grid is obviously accelerated, the consistency of crystal grains is difficult to control, and the requirements on temperature resistance and pressure resistance of a curing chamber are higher, so the temperature setting range of the invention is selected from 150 ℃ to 180 ℃, and the corrosion resistance of the positive plate grid is improved under the condition of convenient production control. (2) The strength of the polar plate is enhanced. Under the high-temperature and high-pressure state, the wet green plate is in a steam atmosphere, the thermal motion of water molecules is more violent, the pore-forming of positive lead paste is facilitated, meanwhile, the solubility of oxygen in a lead paste water film is increased, compressed air is supplemented in a time-interval mode, the corrosion of the surface of the grid and the oxidation of metal lead in the positive lead paste are facilitated, and the bonding strength of the grid and active substances is enhanced. (3) The total time of curing, drying and heat treatment is shortened, the time of the drying stage can be shortened to be within 8h, the total time of curing, heat treatment and drying is controlled to be 28h-38h, and the production efficiency is improved. The heat treatment temperature rise and pressure rise and heat preservation stage has the curing effect and the drying effect, and the pressure release stage can quickly reduce the moisture of the wet green plate. Drying for 3-8h at 70-100 ℃ after pressure relief, namely reducing the water content of the positive plate lead paste to be within 0.5%, and reducing the content of metallic lead in the positive plate lead paste to be within 3%.
Drawings
FIG. 1 is a schematic view of the process of curing, heat treating and drying a wet green plate of a positive electrode.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings of the specification, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work based on the embodiments of the present invention belong to the protection scope of the present invention.
Example 1
The main flow of the curing and heat treatment drying of the cathode wet green sheet is shown in fig. 1, and the specific technical parameters of this example are shown in table 1:
TABLE 1
Step 1, curing stage: the temperature was set at 55 deg.C, the relative humidity at 98% and the time at 28 h. The pressure release valve and the compressed air are in a closed state, the circulating fan and the atomized water are opened for humidification, the indoor pressure is in a normal pressure state (1 atm), and the air doors of the inlet and the outlet are in a timing control state.
Compressed air can also be started in the curing stage to ensure that the oxygen in the curing chamber is sufficient. However, because the atomized water contains compressed air, the atomization and humidification process has the function of supplementing air; and when the inlet and outlet air doors are opened at regular time, moisture is discharged from the outlet air door, air enters from the inlet air door, and the function of supplementing air is also provided.
Step 2, a heat treatment temperature rise and pressure rise stage: the temperature is set to 170 ℃, the opening pressure of the pressure release valve is set to 0.5 Mpa, and the temperature rise time is set to 2.5 h. And closing the air doors of the inlet and the outlet and humidifying the atomized water, keeping the circulating fan in an open state, and introducing compressed air into the solid chamber at regular time.
In the stage of heat treatment and temperature rise, the evaporation of water in the wet green plate is accelerated along with the rise of temperature, the curing chamber is in a closed state, the water is not dissipated outwards, and the pressure in the chamber is gradually increased. The saturated vapor pressure corresponding to 170 ℃ is about 0.8Mpa, the pressure value kept in the chamber is lower than 0.8Mpa, and the opening pressure of the pressure relief valve is set to 0.5 Mpa in the embodiment. At this stage, the inlet and outlet dampers must be closed in order to ensure high temperature and high pressure. The relative humidity does not need to be set in the process, and the atomized water is not needed to be humidified.
Step 3, heat treatment and heat preservation: keeping the temperature at 170 ℃ for 2h, setting the opening pressure of the pressure release valve to be 0.5 Mpa, keeping the circulating fan in an operating state in the heat preservation process, and introducing compressed air into the solid chamber at regular time.
The set value of the opening pressure of the pressure release valve is 0.05-0.3 MPa lower than the saturated steam pressure of water steam at the set temperature. If the opening pressure of the pressure relief valve is set to be too low, the water loss of the wet green sheet is accelerated in the process, and the curing effect of the green sheet is influenced.
Step 4, pressure relief stage: stopping heating after the heat preservation is finished, closing the circulating fan and the compressed air, and regulating the opening degree of the pressure relief valve to reduce the indoor pressure to the normal pressure state (1 atm) within 1.5 h;
step 5, a drying stage: the relative humidity is set to be 10%, a circulating fan and an inlet and outlet air door are opened, and drying is carried out for 6 hours at the temperature of 70 ℃.
And finally, opening the sealing door and moving out the raw plate.
Example 2:
the main flow of the curing and heat treatment drying of the cathode wet green sheet is shown in fig. 1, and the specific technical parameters of this example are shown in table 2:
TABLE 2
Step 1, curing stage: the method comprises two substeps, wherein the temperature of the first step is set to be 45 ℃, the relative humidity is set to be 95%, and the time is set to be 18 h; the temperature of the second step was set to 65 ℃, the relative humidity to 80% and the time to 6 h. And closing the pressure release valve and the compressed air, opening the circulating fan and humidifying the atomized water, wherein the indoor pressure is in a normal pressure state (1 atm), and the air doors at the inlet and the outlet are in a timing control state.
Step 2, a heat treatment temperature rise and pressure rise stage: the temperature is set to 150 ℃, the opening pressure of the pressure release valve is set to 0.4Mpa, and the temperature rise time is set to 2 hours. In the process, the air doors of the inlet and the outlet and the atomized water are closed for humidification, the circulating fan keeps an open state, and compressed air is introduced into the solid chamber at regular time.
Step 3, heat treatment and heat preservation: keeping the temperature at 150 ℃ for 3h, setting the opening pressure of the pressure relief valve to be 0.4Mpa, keeping the circulating fan in an operating state in the heat preservation process, and introducing compressed air into the solid chamber at regular time.
Step 4, pressure relief stage: after the heat treatment heat preservation time is up, stopping heating, closing the circulating fan and the compressed air, and regulating the opening degree of the pressure relief valve to reduce the indoor pressure to the normal pressure state (1 atm) within 0.5 h;
step 5, a drying stage: the method comprises two substeps, wherein the temperature of the first step is set to be 90 ℃, the relative humidity is set to be 10%, the time is set to be 4h, and a circulating fan and an inlet and outlet air door are opened; in the second step, the temperature is set to be 45 ℃, the relative humidity is set to be 20%, the time is set to be 0.5h, and the circulating fan and the inlet and outlet air doors are kept in an open state.
When the set temperature in the drying stage is higher (such as 80-100 ℃) or the ambient temperature is lower (such as-10 ℃), a transitional cooling step can be added in the drying stage, so as to avoid directly moving the dried green plate with higher temperature out to be placed in the environment with lower temperature.
And finally, opening the sealing door and moving out the raw plate.
The method for curing, heat treating and drying the wet green sheet of the positive electrode provided by the embodiment of the invention is described in detail above, and the principle and the embodiment of the invention are explained in the present document by applying specific examples, and the description of the above embodiment is only used to help understanding the method and the core concept of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (8)
1. A method for curing, heat-treating and drying a wet anode green sheet is characterized by comprising the following steps: (1) and (3) curing: curing the anode wet green plate for 18-40h at the temperature of 40-70 ℃ and the relative humidity of 80-100%, wherein the pressure in a curing chamber is in a normal pressure state, a circulating fan and atomized water are turned on for humidification, and an inlet air door and an outlet air door are in a timing control state; (2) and (3) a heat treatment temperature rise and pressure rise stage: setting the temperature to be 150-180 ℃, setting the opening pressure of the pressure release valve to be 0.4-0.8Mpa, heating for 1-3 hours, keeping the circulating fan in an open state in the process, closing the air doors of the inlet and the outlet and humidifying atomized water, and introducing compressed air into the curing chamber at regular time; (3) and (3) heat treatment and heat preservation: keeping the temperature for 1.5-5h after the indoor temperature reaches a set value, setting the opening pressure of a pressure release valve to be 0.4-0.8Mpa, keeping the circulating fan in an open state in the heat preservation process, and introducing compressed air into the curing chamber at regular time; (4) a pressure relief stage: after the heat preservation time is up, stopping heating, closing the circulating fan and the compressed air, and regulating the opening degree of the pressure relief valve to reduce the pressure in the curing chamber to the normal pressure state within 20-90 min; (5) and (3) a drying stage: the temperature is 70-100 ℃, the indoor relative humidity is set to be lower than 20%, a circulating fan and an inlet and outlet air door are opened, and drying is carried out for 3-8 hours; and after drying is finished, opening the sealing door and moving out the raw plate.
2. The method for curing, heat-treating and drying the cathode wet green sheet according to claim 1, wherein: and (3) in the step (2), in the stage of heat treatment temperature rise and pressure rise, the opening pressure set value of the pressure relief valve is 0.05-0.3 Mpa lower than the saturated steam pressure of the steam at the set temperature.
3. The method for curing, heat-treating and drying the cathode wet green sheet according to claim 1, wherein: and (3) the set value of the opening pressure of the pressure release valve in the heat treatment and heat preservation stage is 0.05-0.3 MPa lower than the saturated steam pressure of the steam at the set temperature.
4. The method for curing, heat-treating and drying the cathode wet green sheet according to claim 1, wherein: the pressure in the curing chamber in the step (3) is not lower than 0.4 Mpa;
the temperature in the curing chamber in the step (3) is not lower than 150 ℃;
the pressure range of the compressed air in the step (2) is 0.6-1.0 MPa;
the pressure range of the compressed air in the step (3) is 0.6-1.0 MPa;
the pressure of the compressed air in the step (2) is not lower than the actual pressure in the curing chamber;
and (3) the pressure of the compressed air in the step (3) is not lower than the actual pressure in the curing chamber.
5. The method for curing, heat-treating and drying the cathode wet green sheet according to claim 1, wherein: in the step (1), the curing time is 20-25 h;
the heating and temperature rising time in the step (2) is controlled to be 1h-2.5 h;
in the step (3), the heat preservation time is 2-3 h;
in the step (4), the pressure relief time is 0.5-1 h.
6. The method for curing, heat-treating and drying the cathode wet green sheet according to claim 1, wherein: the total time of curing and heat treatment drying is 24-55 h.
7. The method for curing, heat-treating and drying the cathode wet green sheet according to claim 6, wherein: the total time of curing and heat treatment drying is 28-38 h.
8. The method for curing, heat-treating and drying the cathode wet green sheet according to claim 1, wherein: the timing control state of the inlet and outlet air doors is to set the closing and opening time intervals of the air doors through PLC programming.
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| CN110474022B (en) * | 2019-08-05 | 2020-10-13 | 天能电池集团股份有限公司 | Solidifying and drying method for lead storage battery pole plate |
| CN112467090B (en) * | 2020-11-06 | 2021-12-14 | 浙江天能汽车电池有限公司 | Curing and drying process for positive plate of start-stop storage battery and storage battery plate group |
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| JPH0765824A (en) * | 1993-08-30 | 1995-03-10 | Shin Kobe Electric Mach Co Ltd | Manufacture of electrode for lead acid battery |
| CN101345305B (en) * | 2008-08-25 | 2010-10-06 | 风帆股份有限公司 | Growth plate curing and dying process of lead-acid accumulator |
| US10522883B2 (en) * | 2010-05-10 | 2019-12-31 | Rsr Technologies, Inc. | Recycling electrochemical cells and batteries |
| CN104362301A (en) * | 2014-10-14 | 2015-02-18 | 浙江南都电源动力股份有限公司 | Carbon coated titanium-based lead dioxide positive plate for lead-acid storage battery |
| CN106207193B (en) * | 2015-05-08 | 2019-04-09 | 曾碚凯 | The high-tension battery group and packaging method of a kind of bipolar plate-shaped unit high-energy lead-acid battery and its composition |
| CN105428606B (en) * | 2015-11-12 | 2016-11-09 | 骆驼集团蓄电池研究院有限公司 | A kind of battery curing process |
| WO2017138038A1 (en) * | 2016-02-09 | 2017-08-17 | Hitachi Chemical Company, Ltd. | Negative electrode for lead-acid battery, lead-acid battery, and method for manufacturing a negative electrode for lead-acid battery |
| CN106058162B (en) * | 2016-08-23 | 2018-05-11 | 安徽永恒动力科技有限公司 | A kind of method of energy battery positive plate rapid curing drying |
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