CN109065846B - Process for curing positive electrode plate of lead-acid storage battery - Google Patents
Process for curing positive electrode plate of lead-acid storage battery Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 62
- 239000002253 acid Substances 0.000 title claims abstract description 21
- 238000003860 storage Methods 0.000 title claims abstract description 19
- 230000003647 oxidation Effects 0.000 claims abstract description 152
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 152
- 238000001035 drying Methods 0.000 claims abstract description 96
- 230000003020 moisturizing effect Effects 0.000 claims abstract description 44
- 238000009692 water atomization Methods 0.000 claims description 38
- 238000000889 atomisation Methods 0.000 claims description 32
- 230000001590 oxidative effect Effects 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000007711 solidification Methods 0.000 description 9
- 230000008023 solidification Effects 0.000 description 9
- 238000001514 detection method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 4
- 239000013543 active substance Substances 0.000 description 3
- 238000005755 formation reaction Methods 0.000 description 3
- 229910000464 lead oxide Inorganic materials 0.000 description 3
- OCWMFVJKFWXKNZ-UHFFFAOYSA-L lead(2+);oxygen(2-);sulfate Chemical compound [O-2].[O-2].[O-2].[Pb+2].[Pb+2].[Pb+2].[Pb+2].[O-]S([O-])(=O)=O OCWMFVJKFWXKNZ-UHFFFAOYSA-L 0.000 description 3
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 206010027146 Melanoderma Diseases 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
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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
- H01M4/14—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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- 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
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Abstract
The invention discloses a lead-acid storage battery anode plate curing process which comprises a moisturizing stage, an oxidation stage and a drying stage, wherein the oxidation stage comprises an oxidation curing stage and an oxidation drying stage, and the oxidation curing stage comprises a first stage of oxidation curing, a second stage of oxidation curing and a third stage of oxidation curing. The invention has good curing effect on the anode plate by controlling the curing process of the anode plate, almost no black spots and holes exist in grid corrosion and section faults, the surface of the plate is regular without cracks, and the plate has higher strength.
Description
Technical Field
The invention belongs to the technical field of electrochemistry. In particular to a process for curing a positive electrode plate of a lead-acid storage battery.
Technical Field
In the production process of lead-acid storage batteries, pole plate curing is a very important link. As a main component of the lead-acid storage battery, the pole plate has a critical effect on the quality of the battery, and the solidification quality of the pole plate has a remarkable influence on the physical and chemical parameters of the pole plate of the lead-acid storage battery and the performance of the battery.
In the process of the pole plate curing process, the process control has great influence on the capacity, service life and formation difficulty of the pole plate, how to control reasonable curing process conditions in actual production to ensure that the phase content of the lead plaster is appropriate and a firm frame structure is kept, and the subsequent formation process is facilitated, so that the technical problem needs to be continuously and deeply researched.
Disclosure of Invention
In order to solve the technical problems, the invention provides a process for curing the positive plate of the lead-acid storage battery, and the process obtains the positive plate with excellent performances and obviously improved battery performances by controlling the curing process and the curing process conditions. The invention is realized by the following technical scheme
A lead-acid storage battery positive pole plate curing process comprises a moisturizing stage, an oxidation stage and a drying stage;
in the moisturizing stage, the moisturizing temperature is 43-50 ℃, the moisturizing humidity is 99.6-100%, the moisturizing time is 18-25 h, and the rotating speed of the circulating fan in the curing chamber in the moisturizing stage is 20% of the maximum rotating speed of the circulating fan in the curing chamber in the moisturizing stage; simultaneously carrying out water atomization and steam atomization in the curing chamber;
the oxidation stage comprises an oxidation curing stage and an oxidation drying stage, and the time of the oxidation stage is 23-27 hours;
the oxidation curing stage comprises: in a sealed environment in a curing chamber, the temperature during oxidation curing is 50-65 ℃, the humidity during oxidation curing is 90-100%, the time of oxidation curing is 20-23 hours, the rotating speed of a circulating fan in the curing chamber at the oxidation curing stage is 30-65% of the maximum rotating speed of the circulating fan, and water atomization and/or steam atomization are carried out in the curing chamber;
the oxidation drying stage: in a sealed environment in a curing chamber, the temperature during oxidation drying is 45-54 ℃, the humidity during oxidation drying is 80%, the time during oxidation drying is 3-4 hours, and the rotating speed of a circulating fan in the curing chamber in an oxidation drying stage is 80% of the maximum rotating speed of the circulating fan;
in the drying stage, the temperature during drying is 45-65 ℃, the humidity during drying is 10-20%, the drying time is 18-21 hours, and the rotating speed of a circulating fan in the curing chamber in the drying stage is 100% of the maximum rotating speed of the circulating fan.
Further, the moisturizing stage is as follows: simultaneously carrying out water atomization and steam atomization in a curing chamber, setting the temperature of the curing chamber to be 43 +/-3 ℃, the humidity to be 99.6-100% and the rotating speed of a circulating fan to be 20% of the maximum rotating speed of the circulating fan, and preheating for 1h in the curing chamber under the condition; after preheating, slowly putting the positive electrode plate to be solidified into a solidifying chamber; after the positive electrode plate completely enters the curing chamber, moisturizing for 1h under the conditions that the temperature is 43 +/-3 ℃, the humidity is 99.6-100% and the rotating speed of the circulating fan is 20% of the maximum rotating speed of the circulating fan; after the moisture preservation is finished, the temperature in the curing chamber is increased from 43 +/-3 ℃ to 50 +/-5 ℃ (the humidity is still 99.6-100%, and the rotating speed of the circulating fan is still 20% of the maximum rotating speed of the circulating fan), the positive pole plate is moisturized for 16 +/-1 h under the condition, and the moisturizing stage of the positive pole plate is finished after the moisturizing is finished.
Furthermore, the time required from the beginning of the positive pole plate entering the curing chamber to the complete entering of the positive pole plate into the curing chamber is less than or equal to 5 hours; the time for raising the temperature in the curing chamber from 43 +/-3 ℃ to 50 +/-5 ℃ is 0.5-1 hour.
Further, the oxidation curing stage comprises a first oxidation curing stage, a second oxidation curing stage and a third oxidation curing stage, and the oxidation curing stage and the oxidation drying stage comprise the following steps:
a. first-stage oxidation curing: the anode plate after the moisture preservation stage enters a curing chamber of an oxidation stage, water atomization and steam atomization are simultaneously carried out in the curing chamber, the temperature in the curing chamber is set to be 60 +/-5 ℃, the humidity is set to be 99.6-100%, the rotating speed of a circulating fan is set to be 30% of the maximum rotating speed of the circulating fan, the anode plate is preheated for 1 hour under the condition, and after the preheating is finished, the oxidation curing is carried out for 15 +/-1 hours under the condition, so that the first-stage oxidation curing is finished;
b. second-stage oxidation curing: after the anode plate is oxidized and cured for the first stage, stopping steam atomization (only carrying out water atomization) in the curing chamber, reducing the temperature in the curing chamber from 60 +/-5 ℃ to 50-54 ℃, reducing the humidity from 99.6-100% to 93-95%, wherein the rotating speed of the circulating fan is 60-65% of the maximum rotating speed of the circulating fan, and oxidizing and curing the anode plate for 1 hour under the condition to finish the second stage of oxidizing and curing;
c. third-stage oxidation curing: after the second stage of oxidation curing is finished, the anode plate is oxidized and cured for 3 hours in a curing chamber under the conditions of water atomization, the temperature of 50-54 ℃, the humidity of reduced from 93-95% to 90-92% and the rotating speed of the circulating fan of 60-65% of the maximum rotating speed of the circulating fan, and then the third stage of oxidation curing is finished.
d. An oxidation drying stage: after the third stage of oxidation curing is finished, stopping water atomization in the curing chamber (namely, neither steam atomization nor water atomization is carried out in the curing chamber), then cooling the temperature in the curing chamber from 50-54 ℃ to 45 ℃, reducing the humidity from 90-92% to 80%, setting the rotating speed of the circulating fan to be 80% of the maximum rotating speed of the circulating fan, and carrying out oxidation drying on the positive electrode plate for 3 hours under the condition; and after the oxidation drying is finished, the oxidation stage of the positive electrode plate is finished.
Further, the temperature in the curing chamber in the step b is reduced from 60 +/-5 ℃ to 50-54 ℃, and the time for reducing the humidity from 99.6-100% to 93-95% is 0.5-1 hour; c, the time for reducing the humidity in the curing chamber from 93-95% to 90-92% is 0.5-1 hour; and d, cooling the temperature in the curing chamber from 50-54 ℃ to 45 ℃, and simultaneously cooling the humidity from 90-92% to 80% for 0.5-1 hour.
Further, the drying stage comprises a first stage of drying and a second stage of drying, and comprises the following specific steps:
e. first-stage drying: placing the anode plate after the oxidation stage in a curing chamber of a drying stage, setting the temperature and the humidity in the curing chamber of the drying stage to be 45 +/-5 ℃ and 20%, setting the rotating speed of a circulating fan to be 100% of the maximum rotating speed of the circulating fan, stopping water atomization and steam atomization, preheating the anode plate for 1 hour under the conditions, and drying the anode plate for 3 hours under the conditions (the temperature and the humidity are 45 +/-5 ℃ and 20%, and the rotating speed of the circulating fan is set to be 100% of the maximum rotating speed of the circulating fan) after the preheating is finished, thus finishing the first-stage drying;
f. and (3) second-stage drying: after the first stage of drying is finished, the temperature in the curing chamber is increased from 45 +/-5 ℃ to 65 +/-5 ℃, the humidity is reduced from 20% to 10%, the rotating speed of the circulating fan is set to be 100% of the maximum rotating speed of the circulating fan, water atomization and steam atomization are still not carried out, the positive pole plate is dried for 15 +/-1 hours under the condition, and the drying stage of the positive pole plate is finished after the drying is finished.
Furthermore, the temperature in the curing chamber in the step f is increased from 45 +/-5 ℃ to 65 +/-5 ℃, and the time for reducing the humidity from 20% to 10% is 0.5-1 hour.
Further, the maximum rotating speed of the circulating fan in the curing chamber is 2500 r/min.
The curing chambers adopted by the invention are all common curing chambers, and the control of the conditions in the curing chambers such as temperature, humidity and the like is controlled by an electric control cabinet program.
Compared with the prior art, the invention has the following positive beneficial effects
The moisturizing stage, the oxidizing stage and the drying stage are respectively completed in different curing chambers, and are not influenced, and the polar plate is not greatly influenced by insufficient temperature and humidity changes, so that the performance of the cured polar plate is influenced;
the pole plate corrosion layer obtained by the invention through the control of the curing process has good effect, no black spot and no crack, and the fault of the pole plate section is full.
The positive plate prepared by the curing process further improves the performance of the grid, falls for three times at a height of 1 meter, and has a falling strength of less than 0.9 percent; the water content of the obtained polar plate is less than or equal to 0.16%, and the surface of the grid corrosion layer is almost free of black spots;
the battery prepared by the polar plate is charged and discharged for 3 times under the conditions of 10A and 10.5V, the charging and discharging time reaches 130min, the high cycle capacity is still realized under the condition of low temperature (-18 ℃), and the battery has high consistency; therefore, the positive pole plate obtained by the curing process not only ensures the performance of the battery, but also ensures the consistency and stability of the quality of the battery.
Drawings
FIG. 1 is one of the front views of the positive plate after curing;
FIG. 2 is a second front view of the cured positive plate;
FIG. 3 is a third front view of the cured positive plate;
FIG. 4 is a fourth view of the front side of the positive plate after curing;
FIG. 5 is a cross-sectional view of the cured positive plate;
Detailed Description
The present invention will be described in more detail with reference to the following embodiments, but the present invention is not limited to the embodiments.
The curing chamber and the electric control cabinet program (Jiangsu three-ring, the electric control cabinet program can control the temperature and humidity, the rotating speed of the fan, the temperature rise and temperature reduction time) adopted in the following embodiment, wherein the maximum rotating speed of the circulating fan is 2500 r/min.
Example 1
A lead-acid storage battery positive pole plate curing process comprises a moisturizing stage, an oxidation stage and a drying stage; the specific process is as follows:
(1) and (3) a moisturizing stage:
firstly, setting the temperature in a curing chamber to be 43 +/-3 ℃, the humidity to be 99.6-100 percent and the rotating speed of a circulating fan to be 20 percent of the maximum rotating speed of the circulating fan, and simultaneously carrying out water atomization and steam atomization in the curing chamber; after setting, the curing chamber was preheated for 1 hour under these conditions; after preheating is finished, placing an anode plate to be solidified on an anode plate frame, slowly feeding the anode plate frame with the anode plate into a solidification chamber, wherein the time from the beginning of feeding the anode plate frame into the solidification chamber to the complete feeding of the anode plate frame into the solidification chamber is not more than 5 hours, closing the solidification chamber after the anode plate and the anode plate frame are completely fed into the solidification chamber, and keeping the humidity for 1 hour under the conditions that the temperature is 43 +/-3 ℃, the humidity is 99.6-100%, the rotating speed of a circulating fan is 20% of the maximum rotating speed of the circulating fan, and simultaneously carrying out water atomization and steam atomization in the solidification chamber;
after the positive pole plate is moisturized for 1 hour, the temperature in the curing chamber is increased from 43 +/-3 ℃ to 50 +/-5 ℃, other conditions are not changed, under the conditions, the positive pole plate is moisturized for 16 +/-1 hours, and after the moisturizing time is up, the moisturizing stage of the positive pole plate curing process is completed;
in the process, the time for heating the temperature in the curing chamber from 43 +/-3 ℃ to 50 +/-5 ℃ is 0.5-1 hour, namely, the temperature in the curing chamber is slowly increased, so that the polar plate is not influenced by the sudden environmental change of the outside;
(2) and (3) an oxidation stage:
the oxidation stage comprises an oxidation curing stage and an oxidation drying stage; the oxidation curing stage comprises a first stage oxidation curing, a second stage oxidation curing and a third stage oxidation curing;
first-stage oxidation curing: setting the temperature in a curing chamber in an oxidation stage to be 60 +/-5 ℃, the humidity to be 99.6-100% and the rotating speed of a circulating fan to be 30% of the maximum rotating speed of the circulating fan, and simultaneously carrying out water atomization and steam atomization in the curing chamber; preheating a curing chamber in an oxidation stage for 1 hour under the set condition, after preheating is finished, rapidly moving an anode plate in a moisturizing stage from the curing chamber in the moisturizing stage into the curing chamber in the oxidation stage, wherein the anode plate is subjected to water atomization and steam atomization in the curing chamber at the temperature of 60 +/-5 ℃, the humidity of 99.6-100% and the rotating speed of a circulating fan of 30% of the maximum rotating speed of the circulating fan, and oxidizing and curing for 15 +/-1 hours under the condition, so that the first stage of oxidizing and curing is finished; most of lead is converted into lead oxide in the stage to form active substances with a certain structure, so that the oxidation of the grid and the adhesion of the active substances are promoted to form an interface structure, namely a grid corrosion layer;
second-stage oxidation curing: after the anode plate is oxidized and cured for the first period, stopping steam atomization (only water atomization) in the curing chamber, setting the temperature in the curing chamber to be 50-54 ℃, the humidity to be 93-95% and the rotating speed of the circulating fan to be 60-65% of the maximum rotating speed of the circulating fan, and oxidizing and curing the anode plate for 1 hour under the conditions to finish the second period of oxidation and curing; in the stage, most of lead is reacted into lead oxide, the temperature, humidity and wind speed in the process ensure that the oxidation of the lead is carried out slowly, and the plate of the whole curing chamber can fully oxidize the lead into the lead oxide;
in the process, the temperature in the curing chamber is reduced from 60 +/-5 ℃ to 50-54 ℃, and the time for reducing the humidity from 99.6-100% to 93-95% is 0.5-1 hour, namely, the temperature and the humidity are slowly changed;
third-stage oxidation curing: after the anode plate is subjected to the second stage of oxidation curing, setting the humidity in the curing chamber to be 90% -92%, wherein other conditions are the same as those of the second stage of oxidation curing; oxidizing and curing the positive electrode plate for 3 hours under the condition to finish the third section of oxidizing and curing; the stage further ensures the complete oxidation of lead;
in the process, the time for reducing the humidity in the curing chamber from 93-95% to 90-92% is 0.5-1 hour, namely, the change of the humidity is slowly carried out;
an oxidation drying stage: after the third stage of oxidation curing is finished, stopping water atomization in the curing chamber (namely, stopping steam atomization and water atomization in the curing chamber), setting the temperature in the curing chamber to be 45 ℃, the humidity to be 80% and the rotating speed of the circulating fan to be 80% of the maximum rotating speed of the circulating fan, and after the setting is finished, oxidizing and drying the positive electrode plate for 3 hours under the condition; namely, the oxidation stage of the anode plate is completed; in the stage, the polar plate is completely oxidized and effectively combined with the grid without high-temperature heating, the corresponding air humidity is correspondingly reduced, and the wind speed of the circulating fan ensures the consistency of the polar plate in the whole curing chamber;
in the process, the temperature in the curing chamber is reduced from 50-54 ℃ to 45 ℃, and the time for reducing the humidity from 90-92% to 80% is 0.5-1 hour, namely, the temperature and the humidity in the curing chamber are slowly changed;
(3) drying stage
Setting the temperature in the curing chamber in the drying stage to be 45 +/-5 ℃, the humidity to be 20% and the rotating speed of the circulating fan to be 100% of the maximum rotating speed of the circulating fan (completely stopping water atomization and steam atomization), and preheating the curing chamber in the drying stage for 1 hour under the conditions; after preheating is finished, the anode plate which is finished with the oxidation stage is quickly transferred into a curing chamber of a drying stage from the curing chamber of the oxidation stage, and the anode plate is dried for 3 hours under the conditions that the temperature is 45 +/-5 ℃, the humidity is 20 percent and the rotating speed of a circulating fan is 100 percent; and after drying, setting the temperature in the curing chamber to be 65 +/-5 ℃, the humidity to be 10% and the rotating speed of the circulating fan to be 100%, drying the positive electrode plate for 15 +/-1 hours under the conditions, and finishing the drying stage of the positive electrode plate after drying. The curing process of the positive pole plate is completed after the drying stage of the positive pole plate is completed; the polar plate solidified at the stage loses water, the water content of the polar plate is reduced, and the reaction of free lead can be completed;
in the process, the temperature in the curing chamber is increased from 45 +/-5 ℃ to 65 +/-5 ℃, and the time for reducing the humidity from 20% to 10% is 0.5-1 hour, namely, the temperature and the humidity in the curing chamber in the drying stage are slowly changed.
Example 2
A lead-acid storage battery positive pole plate curing process comprises a moisturizing stage, an oxidation stage and a drying stage; the specific process is as follows:
(1) and (3) a moisturizing stage:
firstly, setting the temperature in a curing chamber to be 43 +/-3 ℃, the humidity to be 100 percent and the rotating speed of a circulating fan to be 20 percent of the maximum rotating speed of the circulating fan, and simultaneously carrying out water atomization and steam atomization in the curing chamber; after setting, the curing chamber was preheated for 1 hour under these conditions; after preheating is finished, placing an anode plate to be cured on an anode plate frame (1200 anode plates are placed on the anode plate frame for curing), slowly entering the anode plate frame with the anode plate into a curing chamber, wherein the time taken for the anode plate frame with the anode plate to completely enter the curing chamber from the beginning is 3 hours, and after the anode plate and the anode plate frame completely enter the curing chamber, keeping moisture for 1 hour under the conditions that the temperature is 43 ℃, the humidity is 100%, the rotating speed of a circulating fan is 20% of the maximum rotating speed, and simultaneously water atomization and steam atomization are carried out in the curing chamber;
after the positive pole plate is moisturized for 1 hour, the temperature in the curing chamber is increased from 43 +/-3 ℃ to 50 ℃, other conditions are not changed, under the conditions, the positive pole plate is moisturized for 16 hours, and after the moisturizing time is up, the moisturizing stage of the positive pole plate curing process is completed;
in the process, the time for heating the temperature in the curing chamber from 43 +/-3 ℃ to 50 ℃ is 1 hour, namely, the temperature of the curing chamber is slowly increased;
after the section is finished, detecting the water content and the free lead content of the anode plate, wherein the results are shown in table 1;
(2) and (3) an oxidation stage:
the oxidation stage comprises an oxidation curing stage and an oxidation drying stage; the oxidation curing stage comprises a first stage oxidation curing, a second stage oxidation curing and a third stage oxidation curing;
first-stage oxidation curing: setting the temperature in a curing chamber in an oxidation stage to be 60 ℃, the humidity to be 100% and the rotating speed of a circulating fan to be 30% of the maximum rotating speed of the curing chamber, and simultaneously carrying out water atomization and steam atomization in the curing chamber; preheating a curing chamber in an oxidation stage for 1 hour under the set condition, after preheating is finished, rapidly moving an anode plate in a moisturizing stage from the curing chamber in the moisturizing stage into the curing chamber in the oxidation stage, wherein the anode plate is subjected to water atomization and steam atomization in the curing chamber at the temperature of 60 ℃, the humidity of 100% and the rotating speed of a circulating fan of 30% of the maximum rotating speed of the anode plate, and oxidizing and curing for 15 hours under the condition to finish the first stage of oxidizing and curing;
second-stage oxidation curing: after the anode plate is subjected to the first stage of oxidation curing, stopping steam atomization (only water atomization) in the curing chamber, setting the temperature in the curing chamber to be 54 ℃, the humidity to be 95% and the rotating speed of the circulating fan to be 60% of the maximum rotating speed, and carrying out oxidation curing on the anode plate for 1 hour under the conditions to finish the second stage of oxidation curing;
in the process, the temperature in the curing chamber is reduced from 60 ℃ to 54 ℃, and the time for reducing the humidity from 100% to 95% is 1 hour, namely, the temperature and the humidity are slowly changed;
third-stage oxidation curing: after the anode plate is subjected to second-stage oxidation curing, setting the humidity in the curing chamber to be 92%, wherein other conditions are the same as those of the second-stage oxidation curing; oxidizing and curing the positive electrode plate for 3 hours under the condition to finish the third section of oxidizing and curing;
in the process, the time for reducing the humidity in the curing chamber from 95% to 92% is 1 hour, namely, the change of the humidity is slowly carried out;
an oxidation drying stage: after the third stage of oxidation curing is finished, stopping water atomization in the curing chamber (namely, stopping steam atomization and water atomization in the curing chamber), setting the temperature in the curing chamber to be 45 ℃, the humidity to be 80% and the rotating speed of the circulating fan to be 80% of the maximum rotating speed, and after the setting is finished, oxidizing and drying the positive electrode plate for 3 hours under the condition; namely, the oxidation stage of the anode plate is completed;
in the process, the temperature in the curing chamber is reduced from 54 ℃ to 45 ℃, and the time for reducing the humidity from 92% to 80% is 1 hour, namely, the temperature and the humidity in the curing chamber are slowly changed;
after the section is finished, detecting the water content and the free lead content of the anode plate, wherein the results are shown in table 1;
(3) drying stage
Setting the temperature in a curing chamber in the drying stage to be 45 ℃, the humidity to be 20% and the rotating speed of a circulating fan to be 100%, and preheating the curing chamber for 1 hour under the conditions; after preheating is finished, the anode plate which is finished with the oxidation stage is quickly transferred into a curing chamber of a drying stage from the curing chamber of the oxidation stage, and the anode plate is dried for 3 hours under the conditions that the temperature is 45 ℃, the humidity is 20% and the rotating speed of a circulating fan is 100%; and after drying, setting the temperature in the curing chamber to 65 ℃, the humidity to 10% and the rotating speed of the circulating fan to 100%, drying the positive electrode plate for 15 hours under the conditions, and finishing the drying stage of the positive electrode plate after drying. The curing process of the positive pole plate is completed after the drying stage of the positive pole plate is completed;
in the process, the temperature in the curing chamber is increased from 45 ℃ to 65 ℃, and the time for reducing the humidity from 20% to 10% is 1 hour, namely, the temperature and the humidity in the curing chamber in the drying stage are slowly changed.
After the section is finished, detecting the water content and the free lead content of the anode plate, wherein the results are shown in table 1;
the following performance tests were performed on the cured positive plate:
(1) the drop strength of the positive pole plate cured by the curing process is detected, 20 cured positive pole plates are randomly selected, the plates freely drop from a height of 1 m, the mass of each plate to be detected before dropping is recorded, then the plates drop three times, the average value of the three-time mass after dropping is recorded, and the test result is shown in table 3;
the drop strength (mass before falling of the plate-mass after falling of the plate)/mass before falling of the plate) is 100 percent
(2) Taking different areas of the positive electrode plate after being cured in the embodiment, carrying out XRD detection, testing the content of each component, and carrying out three tests in each area to obtain an average value, wherein the results are shown in Table 4;
(3) selecting four groups of batteries from the batteries prepared by the positive electrode plate cured by the curing process for performance detection, wherein the four groups of batteries are shown in tables 5-8;
(4) the surface and the section of the positive plate after curing are shown in fig. 1-5, and it can be seen from fig. 1-4 that the surface of the positive plate after curing by the process of the invention has no black spots; as can be seen from FIG. 5, the cured positive plate of the present invention has a full cross-section and no holes; namely, the curing process of the invention obviously improves the quality and the performance of the anode plate.
Example 3
A lead-acid storage battery positive pole plate curing process comprises a moisturizing stage, an oxidation stage and a drying stage; the specific process is as follows:
(1) and (3) a moisturizing stage:
firstly, setting the temperature in a curing chamber to be 45 ℃, the humidity to be 99.8% and the rotating speed of a circulating fan to be 20% of the maximum rotating speed of the circulating fan, and simultaneously carrying out water atomization and steam atomization in the curing chamber; after setting, the curing chamber was preheated for 1 hour under these conditions; after preheating is finished, placing an anode plate to be cured on an anode plate frame (1200 anode plates are placed on the anode plate frame), slowly entering the anode plate frame with the anode plate into a curing chamber, wherein the time taken for the anode plate frame with the anode plate to completely enter the curing chamber from the beginning is 2 hours, and after the anode plate and the anode plate frame completely enter the curing chamber, keeping the humidity for 1 hour under the conditions that the temperature is 45 ℃, the humidity is 99.8%, the rotating speed of a circulating fan is 20% of the maximum rotating speed of the circulating fan, and simultaneously carrying out water atomization and steam atomization in the curing chamber;
after the positive pole plate is moisturized for 1 hour, raising the temperature in the curing chamber from 45 ℃ to 55 ℃, and keeping other conditions unchanged, wherein under the condition, the positive pole plate is moisturized for 15 hours, and after the moisturizing time is up, the moisturizing stage of the positive pole plate curing process is completed;
in the process, the time for heating the temperature in the curing chamber from 45 ℃ to 55 ℃ is 0.6 hour, namely, the temperature of the curing chamber is slowly increased;
after the end of the period, the water content and the free lead content of the positive electrode plate are detected, and the results are shown in table 2;
(2) and (3) an oxidation stage:
the oxidation stage comprises an oxidation curing stage and an oxidation drying stage; the oxidation curing stage comprises a first stage oxidation curing, a second stage oxidation curing and a third stage oxidation curing;
first-stage oxidation curing: setting the temperature in the curing chamber in the oxidation stage to be 65 ℃, the humidity to be 99.6% and the rotating speed of the circulating fan to be 30% of the maximum rotating speed of the circulating fan, and simultaneously carrying out water atomization and steam atomization in the curing chamber; preheating the curing chamber in the oxidation stage for 1 hour under the set condition, after preheating is finished, rapidly moving the anode plate in the moisturizing stage from the curing chamber in the moisturizing stage into the curing chamber in the oxidation stage, wherein the anode plate is subjected to water atomization and steam atomization in the curing chamber at the temperature of 65 ℃, the humidity of 99.6% and the rotating speed of a circulating fan of 30% of the maximum rotating speed, and oxidizing and curing for 14 hours under the condition, so that the first stage of oxidizing and curing is finished;
second-stage oxidation curing: after the anode plate is subjected to the first stage of oxidation curing, stopping steam atomization (only water atomization) in the curing chamber, setting the temperature in the curing chamber to be 50 ℃, the humidity to be 93% and the rotating speed of the circulating fan to be 65% of the maximum rotating speed, and carrying out oxidation curing on the anode plate for 1 hour under the conditions to finish the second stage of oxidation curing;
in the process, the temperature in the curing chamber is reduced from 65 ℃ to 50 ℃, and the time for reducing the humidity from 99.6% to 93% is 0.6 hour, namely, the temperature and the humidity are slowly changed;
third-stage oxidation curing: after the second stage of oxidation curing of the anode plate is completed, setting the humidity in the curing chamber to be 90%, wherein other conditions are the same as those of the second stage of oxidation curing; oxidizing and curing the positive electrode plate for 3 hours under the condition to finish the third section of oxidizing and curing;
in the process, the time for reducing the humidity in the curing chamber from 93% to 90% is 0.5 hour, namely, the change of the humidity is slowly carried out;
an oxidation drying stage: after the third stage of oxidation curing is finished, stopping water atomization in the curing chamber (namely, stopping steam atomization and water atomization in the curing chamber), setting the temperature in the curing chamber to be 45 ℃, the humidity to be 80% and the rotating speed of the circulating fan to be 80% of the maximum rotating speed, and after the setting is finished, oxidizing and drying the positive electrode plate for 3 hours under the condition; namely, the oxidation stage of the anode plate is completed;
in the process, the temperature in the curing chamber is reduced from 50 ℃ to 45 ℃ and the time for reducing the humidity from 90% to 80% is 0.8 hour, namely, the temperature and the humidity in the curing chamber are slowly changed;
after the end of the period, the water content and the free lead content of the positive electrode plate are detected, and the results are shown in table 2;
(3) drying stage
Setting the temperature in a curing chamber in the drying stage to be 45 ℃, the humidity to be 20% and the rotating speed of a circulating fan to be 100% of the maximum rotating speed, and preheating the curing chamber for 1 hour under the conditions; after preheating is finished, the anode plate which is finished with the oxidation stage is quickly transferred into a curing chamber of a drying stage from the curing chamber of the oxidation stage, and the anode plate is dried for 3 hours under the conditions that the temperature is 45 ℃, the humidity is 20% and the rotating speed of a circulating fan is 100%; and after drying, setting the temperature in the curing chamber to 65 ℃, the humidity to 10% and the rotating speed of the circulating fan to 100%, drying the positive electrode plate for 16 hours under the conditions, and completing the drying stage of the positive electrode plate after drying. The curing process of the positive pole plate is completed after the drying stage of the positive pole plate is completed;
in the process, the temperature in the curing chamber is increased from 45 ℃ to 65 ℃, and the time for reducing the humidity from 20% to 10% is 0.8 hour, namely, the temperature and the humidity in the curing chamber in the drying stage are slowly changed.
After the end of the period, the water content and the free lead content of the positive electrode plate are detected, and the results are shown in table 2;
table 1 example 2 detection results of moisture content and free lead content after each stage in the plate curing process
Table 2 example 3 detection results of moisture content and free lead content after each stage in the plate curing process
From the test data in tables 1 and 2, it can be seen that: the average value of the free lead content in the pole plate after the solidification by the solidification process is less than 4 percent, and the water content in the pole plate is less than 0.16 percent; (the water content of the pole plate is less than or equal to 0.3 percent, and the free lead is less than or equal to 4.5 percent, the pole plate is qualified), namely, the water content in the solidified pole plate of the invention far exceeds the standard requirement, the free lead content meets the requirement, and the performance of the obtained solidified pole plate is improved.
Table 3 falling strength test results of the cured positive electrode plate
As can be seen from Table 3, the dropping rate of the positive electrode plate after being cured by the curing process of the present invention is less than 0.9%, i.e., the positive electrode plate after being cured by the curing process of the present invention has a good curing effect.
Table 4 detection results of components of the positive electrode plate after curing
The tetrabasic lead sulfate generates stronger and longer needle crystals than tribasic lead sulfate, and the needle crystals are mutually staggered to form a framework structure of an active substance, so that the strength of a polar plate can be increased, and the cycle service life of the storage battery can be prolonged; the tetrabasic lead sulfate and the tribasic lead sulfate are formed according to a certain proportion, so that the early capacity loss caused by lead calcium and low antimony can be overcome. The formation reaction of the tetrabasic lead sulfate has a memory effect, namely, the electrochemical reaction process only generates the replacement among substances, so that the formed positive active material keeps the three-dimensional network structure of the solidified precursor, the macroscopic framework structure is not changed, the strength of the polar plate is enhanced, and the cycle life of the lead-acid battery is prolonged.
The positive pole plate after being solidified overcomes the early capacity loss, enhances the strength of the pole plate and prolongs the cycle life of the lead-acid battery in the presence of tetrabasic lead sulfate and tribasic lead sulfate.
TABLE 5 results of cell performance test
TABLE 6 results of cell performance measurements
TABLE 7 results of measurements of the performance of the batteries
TABLE 8 results of testing the performance of the batteries
From the above detection results, it can be seen that: the battery prepared by the solidified positive pole plate has good consistency, good performance and strong stability; and under the condition of low temperature, the charge-discharge capacity reaches 98 min.
Claims (7)
1. A lead-acid storage battery positive pole plate curing process comprises a moisturizing stage, an oxidation stage and a drying stage; it is characterized in that the preparation method is characterized in that,
in the moisturizing stage, the moisturizing temperature is 43-50 ℃, the moisturizing humidity is 99.6-100%, the moisturizing time is 18-25 h, and the rotating speed of a circulating fan in a curing chamber in the moisturizing stage is 20% of the maximum rotating speed of the circulating fan in the moisturizing stage;
the oxidation stage comprises an oxidation curing stage and an oxidation drying stage, and the total time of the oxidation stage is 23-27 h;
the oxidation curing stage comprises: in a sealed environment in a curing chamber, the temperature during oxidation curing is 50-65 ℃, the humidity is 90-100%, the time is 20-23 h, the rotating speed of a circulating fan in the curing chamber at the oxidation curing stage is 30-65% of the maximum rotating speed of the circulating fan, and water atomization and/or steam atomization are carried out in the curing chamber;
in the oxidation drying stage, under a sealed environment in a curing chamber, the temperature and the humidity during oxidation drying are 45-54 ℃, the humidity is 80% and the time is 3-4 hours, and the rotating speed of a circulating fan in the curing chamber in the oxidation drying stage is 80% of the maximum rotating speed of the circulating fan;
in the drying stage, under a sealed environment in a curing chamber, the temperature during drying is 45-65 ℃, the humidity is 10-20%, the drying time is 18-21 hours, and the rotating speed of a circulating fan in the curing chamber in the drying stage is 100%;
wherein the oxidation curing stage comprises a first stage oxidation curing, a second stage oxidation curing and a third stage oxidation curing; the oxidation curing stage and the oxidation drying stage comprise the following steps:
a. first-stage oxidation curing: simultaneously carrying out water atomization and steam atomization in a curing chamber in an oxidation stage, wherein the temperature in the curing chamber is 60 +/-5 ℃, the humidity in the curing chamber is 99.6-100%, and the rotating speed of a circulating fan is 30% of the maximum rotating speed of the circulating fan, and preheating the curing chamber in the oxidation stage for 1 hour under the condition; after preheating, transferring the positive electrode plate which is subjected to the moisturizing stage into the preheated curing chamber, and oxidizing and curing the positive electrode plate in the curing chamber for 15 +/-1 hours to finish the first-stage oxidizing and curing;
b. second-stage oxidation curing: after the first stage of oxidation curing of the positive electrode plate is completed, stopping steam atomization in the curing chamber, reducing the temperature in the curing chamber from 60 +/-5 ℃ to 50-54 ℃, reducing the humidity from 99.6-100% to 93-95%, wherein the rotating speed of the circulating fan is 60-65% of the maximum rotating speed of the circulating fan, and carrying out oxidation curing on the positive electrode plate for 1 hour under the condition, namely completing the second stage of oxidation curing;
c. third-stage oxidation curing: after the second stage of oxidation curing is finished, setting the indoor conditions of the curing chamber to be water atomization, the temperature of 50-54 ℃, the humidity of 90-92% from 95-93%, the rotating speed of a circulating fan of 60-65% of the maximum rotating speed of the circulating fan, and carrying out oxidation curing on the positive electrode plate for 3 hours under the conditions, thus finishing the third stage of oxidation curing;
d. an oxidation drying stage: after the third-stage oxidation curing is completed, stopping water atomization in the curing chamber, then reducing the temperature in the curing chamber from 50-54 ℃ to 45 ℃, reducing the humidity from 90-92% to 80%, setting the rotating speed of the circulating fan to be 80% of the maximum rotating speed of the circulating fan, and oxidizing and drying the positive electrode plate for 3 hours under the condition; and after the oxidation drying is finished, the oxidation stage of the positive electrode plate is finished.
2. The process for curing the positive plate of the lead-acid storage battery according to claim 1, wherein the moisture retention stage is as follows: simultaneously carrying out water atomization and steam atomization in a curing chamber, setting the temperature of the curing chamber to be 43 +/-3 ℃, the humidity to be 99.6-100% and the rotating speed of a circulating fan to be 20% of the maximum rotating speed of the circulating fan, and preheating for 1h under the condition; after preheating, slowly putting the positive electrode plate to be solidified into a solidifying chamber; after the positive electrode plate completely enters the curing chamber, moisturizing for 1h under the conditions that the temperature is 43 +/-3 ℃, the humidity is 99.6-100% and the rotating speed of the circulating fan is 20% of the maximum rotating speed of the circulating fan; and after moisturizing, heating the temperature in the curing chamber from 43 +/-3 ℃ to 50 +/-5 ℃, keeping the humidity and the rotating speed of the circulating fan unchanged, moisturizing the positive pole plate for 16 +/-1 h under the condition, and moisturizing the positive pole plate after moisturizing.
3. The process for curing the positive plate of the lead-acid storage battery according to claim 2, wherein the time required for the positive plate to completely enter the curing chamber is less than or equal to 5 hours; the time for raising the temperature in the curing chamber from 43 +/-3 ℃ to 50 +/-5 ℃ is 0.5-1 hour.
4. The process of curing a positive plate of a lead-acid battery according to claim 1,
b, cooling the temperature in the curing chamber from 60 +/-5 ℃ to 50-54 ℃, and simultaneously cooling the humidity from 99.6-100% to 93-95% for 0.5-1 hour;
c, the time for reducing the humidity in the curing chamber from 93-95% to 90-92% is 0.5-1 hour;
and d, cooling the temperature in the curing chamber from 50-54 ℃ to 45 ℃, and simultaneously cooling the humidity from 90-92% to 80% for 0.5-1 hour.
5. The process for curing the positive plate of the lead-acid storage battery according to claim 1, wherein the drying stage comprises a first stage of drying and a second stage of drying, and comprises the following steps:
e. first-stage drying: setting the temperature in the curing chamber in the drying stage to be 45 +/-5 ℃, the humidity to be 20 percent and the rotating speed of a circulating fan to be 100 percent, wherein water atomization and steam atomization do not exist, and the curing chamber in the drying stage is preheated for 1 hour under the conditions; after preheating, placing the anode plate which is subjected to the oxidation stage in a curing chamber after preheating, and drying for 3 hours in the curing chamber to finish first-stage drying;
f. and (3) second-stage drying: after the first stage of drying is finished, the temperature in the curing chamber is increased from 45 +/-5 ℃ to 65 +/-5 ℃, the humidity is reduced from 20% to 10%, the rotating speed of the circulating fan is 100%, the positive pole plate is dried for 15 +/-1 hours under the condition, and the drying stage of the positive pole plate is finished after the drying is finished.
6. The process for curing the positive plate of the lead-acid storage battery according to claim 5, wherein the temperature in the curing chamber in the step f is increased from 45 +/-5 ℃ to 65 +/-5 ℃, and the time for reducing the humidity from 20% to 10% is 0.5-1 hour.
7. The process for curing the positive plate of the lead-acid storage battery according to any one of claims 1 to 6, wherein the maximum rotating speed of the circulating fan is 2500 r/min.
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| CN109873124A (en) * | 2019-01-31 | 2019-06-11 | 安徽超威电源有限公司 | A kind of power lead-acid storage battery high temperature curing process |
| CN109742330B (en) * | 2019-01-31 | 2021-09-10 | 安徽超威电源有限公司 | Two-day high-temperature curing process for power lead-acid storage battery |
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