CN113471560B - Formation method of horizontal lead-acid storage battery - Google Patents
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Abstract
The invention belongs to the technical field of lead-acid storage battery manufacturing, and particularly relates to a horizontal lead-acid storage battery formation method, which comprises the following steps: step 1, passing through a liquid adding holeInjecting an electrolyte into the storage battery; step 2, the formation is carried out according to the following method: charging and discharging once are a stage, the charging current is calculated according to the battery capacity multiplying power, charging is carried out at 0.1C for the initial stage of the formation stage, then increasing is carried out at 0.05C, when the charging current reaches 0.3C, decreasing is carried out at 0.05C until the last charging current is 0.05C, and the charging time is decreased by 1h at intervals of one stage; the discharge current was 50% of the charge current at the stage where it was, and the discharge time was 0.5h per stage. The invention uses in-situ electrode plate Pb, PbO, 3PbO, PbSO4、4PbO·PbSO4Conversion of isoactive substances into positive plate PbO2And the current is controlled at the optimal current in the spongy Pb process of the negative plate, the discharge is reasonably and timely arranged, and the conversion of active substances in the formation process is facilitated.
Description
Technical Field
The invention belongs to the technical field of lead-acid storage battery manufacturing, and particularly relates to a horizontal lead-acid storage battery formation method.
Background
In the manufacturing process of the horizontal storage battery, positive and negative electrode substances in a polar plate need to be activated in a certain charging and discharging mode to be converted into a charge state, and a chemical reaction process for improving the charging and discharging performance and the comprehensive performance of self-discharging, storage and the like of the battery is called as a formation process.
For a bipolar horizontal starting lead-acid battery, the applicant can refer to table 1 for the currently used formation process, and the formation method has the defects of long formation time, low utilization rate of active materials after formation and the like. During actual production, in a formation project, how to design proper current can not only enable the lead plaster to react, but also avoid the electrolysis of redundant current electrolyte, so that the charging efficiency is improved, the charged amount is completely used for converting active substances, and the waste of the electrolyte electrolysis to electric energy is avoided; moreover, the polar plate of the horizontal storage battery is horizontally arranged, and electrolyte is not easy to permeate into each corner of the polar plate, so that the electrolyte is difficult to permeate.
In addition, the density of the electrolyte normally used by the finished storage battery is 1.31-1.33g/cm3Therefore, the existing chemical synthesis process generally adopts secondary acid addition, namely, the primary acid addition density is 1.05-1.06g/cm3Pouring out the electrolyte in the accumulator after the formation is finished, and replacing the electrolyte with the density of 1.31-1.33g/cm3The secondary acid adding process is completed, so that the density of the formed storage battery electrolyte meets the delivery requirements; for a horizontal lead-acid storage battery, the method has the technical problem of difficult acid pouring, and the electrolyte density cannot be easily confirmed by secondary acid addition.
Alternatively, the prior chemical synthesis technology can also adopt one-time acid addition, namely adding 1.245-1.255g/cm3The electrolyte loses water along with charging, and the density of the electrolyte just meets 1.31-1.33g/cm after charging3However, in the formation process, the electrolyte density is high during charging formation, the formation efficiency is low, and the formation time is long.
TABLE 1 formation Charge/discharge procedure of conventional bipolar horizontal starting lead-acid storage battery
Disclosure of Invention
The invention aims to provide a horizontal lead-acid storage battery formation method to solve at least one of the problems in the prior art.
According to one aspect of the invention, a horizontal lead-acid battery formation method is provided, which comprises the following steps:
step 1, injecting electrolyte into a storage battery through a liquid adding hole;
Thus, the invention uses the raw electrode plate of Pb, PbO, 3 PbO. PbSO4、4PbO·PbSO4Conversion of isoactive substances into positive plate PbO2Controlling the current to be the optimal current in the spongy Pb process of the negative plate so as to improve the charging efficiency; and discharge is reasonably and timely arranged to improve the charging acceptance of the polar plate, thereby being beneficial to the conversion of active substances in the formation process.
In some embodiments, the step 2, the formation stage comprises:
in the first stage, after charging for 5h with 0.1C charging current, discharging for 0.5h with 0.05C discharging current;
in the second stage, after charging for 5h with 0.15C charging current, discharging for 0.5h with 0.075C discharging current;
in the third stage, after charging for 4h with 0.2C charging current, discharging for 0.5h with 0.1C discharging current;
in the fourth stage, after charging for 4h with 0.25C charging current, discharging for 0.5h with 0.125C discharging current;
in the fifth stage, after charging for 3h with 0.3C charging current, discharging for 0.5h with 0.15C discharging current;
a sixth stage, after charging for 3h with a charging current of 0.25C, discharging for 0.5h with a discharging current of 0.125C;
a seventh stage, after charging for 2h with 0.2C charging current, discharging for 0.5h with 0.1C discharging current;
in the eighth stage, after charging for 2 hours with 0.15C charging current, discharging for 0.5 hours with 0.075C discharging current;
a ninth stage, after charging for 1h with 0.1C charging current, discharging for 0.5h with 0.05C discharging current;
in the tenth stage, after charging for 1h with a charging current of 0.05C, discharging for 0.5h with a discharging current of 0.025C.
The invention has the following conception in the formation stage in the charging and discharging process:
in the early stage of charging, the charging acceptance of the battery in each stage of formation is different, and at the beginning of formation, the active substances in the polar plate are mostly lead sulfate which is a poor conductor and has larger contact resistance with the plate gate, so that the conductivity of the positive plate is poorer for a long time in the early stage, and the battery is charged by smaller current in the early stage;
a proper reverse charging period (namely a discharging procedure) is added in the charging process, so that a conductive network can be generated between the positive plate grid and the active material, the conductivity of the positive plate is increased, and the charging acceptance of the plate is enhanced;
in the middle stage of charging, along with the progress of charging, the gassing point of the storage battery is reached, the charging acceptance of the storage battery is reduced, the terminal voltage of the storage battery is gradually increased, the charging side reaction is increased, the temperature rise is increased, and the charging efficiency is reduced; at the moment, moderate current is adopted for charging, so that the waste of electric energy is reduced;
in the later charging period, the battery charging acceptance is poorer, and the current requirement is smaller.
In some embodiments, the electrolyte added in step 1 has a density of 1.09 to 1.1g/cm3The temperature of the electrolyte is 5-10 ℃. The reason why the low-temperature electrolyte is initially added is that H is added after the initial acid addition of the secondary battery2SO4Reacting with PbO, 1BS, 3BS and 4BS in the active substance of the polar plate to produce PbSO4、H2And O, the reactions belong to exothermic reactions, the reaction heat aggravates the reaction speed, the temperature rises quickly after acid is added, when the temperature is higher than 70 ℃, the AGM separator is not completely immersed in acid, namely, the AGM separator is etched at high temperature, the aperture and the porosity of the separator are damaged, and the normal charge and discharge of the storage battery are influenced. Meanwhile, the positive plate is passivated at high temperature, the quantity of active substances is reduced, and the capacity of the storage battery is reduced. Further, the density is 1.09-1.10g/cm3The electrolyte is the optimal electrolyte density for formation, the internal resistance of the electrolyte is small under the density, and the formation efficiency is high.
In some embodiments, the electrolyte temperature is maintained between 5 ℃ and 45 ℃ during the step 2 formation stage. Therefore, the negative lead plaster can fall off at the temperature lower than 5 ℃, and the positive lead plaster can peel off and rise; the grid erosion is aggravated at the temperature higher than 45 ℃, the adhesive force of the active substance is reduced, and the life is influenced by easy falling.
In some embodiments, during the formation stage, the high-temperature electrolyte flows out from the lower reserved hole of the storage battery (the outflow temperature is less than 60 ℃) and is pumped into a cooling system, and the cooled electrolyte is circularly injected into the storage battery for formation. Thus, the temperature of the electrolyte entering the storage battery each time can be maintained between 5 ℃ and 45 ℃ by the cooling system. At the moment, the density of the electrolyte is 1.09-1.10g/cm in the formation process3。
In the formation of the battery, the influence of temperature on the charging efficiency is very obvious, the efficiency of the formation of the temperature is low, but the influence of the over-high temperature can have adverse effect on other aspects. The formation is better at the temperature of 5-45 ℃, particularly at the temperature of 25-45 ℃, and not only can the formation efficiency be ensured, but also no negative effect can be caused. The invention ensures that the temperature of the electrolyte formed by the storage battery is kept at the optimal temperature by designing the flowing and circulating electrolyte cooling system, and simultaneously ensures that the formation process can be normally carried out after the charging current is increased, thereby improving the charging efficiency.
In some embodiments, the cooling system includes an electrolyte circulation system connected to the preformed hole and the filling hole, respectively, and an electrolyte cooling system connected to the electrolyte circulation system. Therefore, the high-temperature electrolyte flows out of the reserved hole and is pumped into an electrolyte circulating system, and the high-temperature electrolyte is cooled in the electrolyte circulating system through an electrolyte cooling system and then is pumped into the storage battery through the liquid adding hole, so that formation is continued.
In some embodiments, the electrolyte circulation system comprises a high-temperature tank communicated with the preformed hole through a first pipeline, a low-temperature tank connected with the high-temperature tank through a second pipeline, and a low-temperature tank communicated with the liquid feeding hole through a third pipeline; a first pump body is arranged between the preformed hole and the high-temperature tank, a second pump body is arranged between the high-temperature tank and the low-temperature tank, and a third pump body is arranged between the low-temperature tank and the liquid feeding hole. From this, the first pump body will follow the high temperature electrolyte pump that flows out in the preformed hole and go into the high temperature jar, and the second pump body is with the electrolyte pump in the high temperature jar low temperature jar, and the third pump body is in the battery with the electrolyte pump by the filling hole reentry in the low temperature jar, so formation electrolyte circulation system.
In some embodiments, the electrolyte cooling system comprises a spray cooling tower and a plate heat exchanger connected with the spray cooling tower through a fourth pipeline, and a fourth pump body is arranged between the spray cooling tower and the plate heat exchanger; the second pipeline passes through the plate heat exchanger, and the second pump body is arranged between the plate heat exchanger and the low-temperature tank. From this, go into the low temperature jar in-process at the second pump body with the electrolyte pump in the high temperature jar, high temperature electrolyte takes place the heat exchange with the cold water in the heat exchanger when flowing through plate heat exchanger, and the electrolyte after the cooling is gone into the low temperature jar by the second pump body pump, and cold water temperature risees, flows to the spray cooling tower through the fourth pump body, through spraying, but the storage water tank of outflow spray cooling tower bottom after the air-cooler cooling, circulated use.
Meanwhile, the bipolar horizontal storage battery is difficult to permeate electrolyte because the polar plate is horizontally placed in parallel with the bottom surface and is tightly laminated, and the electrolyte pumped into the bipolar horizontal storage battery is favorable for permeating the electrolyte into the polar plate, so that the electrolyte is uniformly distributed.
According to another aspect of the invention, a horizontal lead-acid storage battery is provided, and the horizontal lead-acid storage battery is obtained after the formation of the horizontal lead-acid storage battery by the formation method.
Compared with the existing storage battery, the storage battery obtained by the formation method has improved battery capacity, low-temperature starting capability, charging acceptance capability and 50% DOD cycle endurance capability, and has better performance.
Drawings
FIG. 1 is a schematic view of a cooling system according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the connection between the battery and the cooling system according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of a positive plate of a battery after formation according to the formation method of the invention;
fig. 4 is a schematic diagram of a negative plate of the storage battery after being formed according to the formation method of the invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
A horizontal lead-acid storage battery formation method comprises the following steps:
step 1, injecting the electrolyte into a storage battery through a liquid adding hole with the density of 1.1g/cm3The dilute sulfuric acid is used as electrolyte, and the temperature of the electrolyte is 10 ℃;
in the first stage, after charging for 5h with 0.1C charging current, discharging for 0.5h with 0.05C discharging current; the first stage is 0.5CAh for charging and 0.025CAh for discharging;
in the second stage, after charging for 5h with 0.15C charging current, discharging for 0.5h with 0.075C discharging current; the charging amount of the second stage is 0.75CAh, and the discharging amount is 0.0375 CAh;
a third stage, after charging for 4h with a charging current of 0.2C, discharging for 0.5h with a discharging current of 0.1C; the third stage has a charge-discharge capacity of 0.005CAh and a charge-discharge capacity of 0.8 CAh;
in the fourth stage, after charging for 4h with 0.25C charging current, discharging for 0.5h with 0.125C discharging current; the quantity of the charging and discharging of the fourth stage is 1CAh, and the quantity of the discharging is 0.0625 CAh;
in the fifth stage, after charging for 3h with 0.3C charging current, discharging for 0.5h with 0.15C discharging current; the charging time of the fifth stage is 0.9CAh, and the discharging amount is 0.075 CAh;
a sixth stage, after charging for 3h with a charging current of 0.25C, discharging for 0.5h with a discharging current of 0.125C; the charging amount of the sixth stage is 0.75CAh, and the discharging amount is 0.0625 CAh;
a seventh stage, after charging for 2h with 0.2C charging current, discharging for 0.5h with 0.1C discharging current; the charging amount of the seventh stage is 0.4CAh, and the discharging amount is 0.05 CAh;
in the eighth stage, after charging for 2h with 0.15C charging current, discharging for 0.5h with 0.075C discharging current; the charging amount of the eighth stage is 0.3CAh, and the discharging amount is 0.0375 CAh;
a ninth stage, after charging for 1h with 0.1C charging current, discharging for 0.5h with 0.05C discharging current; the charging amount of the ninth stage is 0.1CAh, and the discharging amount is 0.025 CAh;
a tenth stage, after charging for 1h with a charging current of 0.05C, discharging for 0.5h with a discharging current of 0.025C; the charging amount in the tenth stage is 0.05CAh, and the discharging amount is 0.0125 CAh.
The integrated charge amount in the formation process of the present embodiment is the charge amount 5.55c (ah); the discharge amount was 0.4375C (Ah). The actual charging amount 5.1125c (ah) and the total formation time length are 35 h.
In the formation process, in order to maintain the temperature of the electrolyte within a specific temperature range, the temperature of the electrolyte needs to be reduced, and the cooling system is adopted to reduce the temperature of the electrolyte in the embodiment.
Fig. 1 shows a schematic structural view of a cooling system of the present embodiment, and as shown in fig. 1, the cooling system includes an electrolyte circulation system, and an electrolyte cooling system, specifically,
the electrolyte circulating system comprises a high-temperature tank 2 communicated with a preformed hole at the bottom of the storage battery through a first pipeline 11, and a low-temperature tank 3 connected with the high-temperature tank 2 through a second pipeline 12, wherein the low-temperature tank 3 is communicated with a liquid adding hole through a third pipeline 13; a first pump body 41 is arranged between the preformed hole and the high-temperature tank 2 and used for pumping high-temperature electrolyte into the high-temperature tank 2 from the storage battery; a second pump body 42 is arranged between the high-temperature tank 2 and the low-temperature tank 3 and is used for pumping the electrolyte in the high-temperature tank 2 into the low-temperature tank 3; and a third pump body 43 is arranged between the low-temperature tank 3 and the liquid adding hole and used for pumping the electrolyte in the low-temperature tank 3 back to the storage battery through the liquid adding hole and continuously forming the electrolyte.
The electrolyte cooling system comprises a spray cooling tower 5, a plate heat exchanger 6 connected with the spray cooling tower 5 through a fourth pipeline 14, and a water storage tank 7 arranged at the bottom of the spray cooling tower 5; a fourth pump body 44 is arranged between the water storage tank 7 at the bottom of the spray cooling tower 5 and the plate heat exchanger 6, and cold water in the water storage tank 7 can be pumped to the top end of the spray cooling tower 5 through the fourth pump body 44 for spray cooling and then returns to the water storage tank 7 for recycling;
wherein, second pipeline 12 passes plate heat exchanger 6, and the in-process that flows into low temperature tank 3 from high temperature tank 2 through second pipeline 12 as high temperature electrolyte takes place the heat exchange with the cold water in the heat exchanger when passing through plate heat exchanger 6, and the electrolyte after the cooling is gone into low temperature tank 3 at the second pump body 42 effect down, and cold water temperature risees, flows to spray cooling tower 5 top under the effect of fourth pump body 44, flows to storage water tank 7 after spraying, air-cooler cooling, recycles.
Performing a formation program by using a storage battery with the model number of 6-QW-100, wherein the height, width and thickness of a positive plate of the storage battery are 100 × 142 × 1.8(mm), and the size of a negative plate is 100 × 142 × 1.5 (mm); the assembly form is as follows: 7 positive plates and 8 negative plates.
When the storage battery with the model number of 6-QW-100 is manufactured according to the forming method of the application in the manufacturing process, the specific procedures are shown in the table 2; when the composition is prepared by a conventional method, the specific procedures are shown in Table 3.
TABLE 2 model number 6-QW-100 accumulator charging and discharging program according to the formation method of the present application
TABLE 3 charging and discharging procedure of storage battery with type 6-QW-100 according to existing formation method
Compared with the conventional formation method and the formation method of the application, the current of the conventional formation method is controlled below 15A, the formation time is 67h, and the formation electric quantity is 667 Ah; the current of the formation method is controlled below 30A, the formation time is 35h, and the formation electric quantity is 445 Ah; therefore, compared with the existing formation method, the formation time of the method is shortened by nearly half;
the formation method increases the charging current, is based on the control consideration of electrolyte circulation, electrolyte cooling and storage battery temperature, and compared with the prior art, the formation method can charge with large current mainly due to the cooperation of an electrolyte cooling system, so that the electrolyte maintains a proper temperature range in the formation process while the current is increased; based on reasonable arrangement of discharge time and duration, the charge acceptance of the storage battery is improved.
After the formation is finished, the chemical conversion is carried out,the storage battery prepared by the existing formation method and the polar plate of the storage battery prepared by the formation method are analyzed and tested according to the method recorded in GB/T23636-; the results in Table 4 show that the formation method of the invention is more beneficial to the formation of the positive electrode PbO2And conversion of the negative spongy lead.
TABLE 4 test results for different plates
Type of test | Content of lead dioxide in positive plate | Spongy lead content of negative plate |
Existing formation method | 83.57% | 85.21% |
The formation method of the application | 91.65% | 91.22% |
Meanwhile, the polar plates obtained by the two formation methods are dissected, no obvious white flower is generated on the surface of the positive plate obtained by the two formation methods, and the formation effect is good; the surface of the negative electrode is soft and has metallic luster, and the formation effect of the storage battery meets the process requirement; the positive and negative electrode plates after the formation of the electrode plate can be shown in figures 3-4. The content of lead dioxide of the positive plate and the spongy lead of the negative plate obtained after the formation are higher than those of the existing formation method, the formation active matter is high in quality, and the storage battery is high in capacity.
This is because the initial capacity of the battery is mainly determined by PbO in the positive electrode plate2The content of (b) is determined. PbO in positive plate2alpha-PbO2And beta-PbO2And amorphous PbO2And the ratio of the three influences the initial capacity of the storage battery.
ɑ-PbO2The crystal has an orthorhombic crystal form, large crystal grain size, small real surface area and small storage battery capacity, and plays a role of a network framework in active substances; beta-PbO2The battery has a tetragonal crystal form, fine crystal grains, large real surface area and large storage battery capacity. During formation charging process, alpha-PbO2Generated in neutral or weakly alkaline environment, beta-PbO2Is generated in a strong acid environment.
In the initial stage of formation, chemical reaction and electrochemical reaction are simultaneously carried out in the pores of the positive plate, and H is consumed by the chemical reaction2SO4Generation of PbSO4To make the environment neutral or alkalescent; electrochemical reaction to form H2SO4。
In the initial stage of formation, the chemical reaction is stronger than the electrochemical reaction, i.e. H2SO4Is greater than the rate of formation, and therefore, the pores of the positive electrode plate are filled with H2SO4Continuously consumed, the pH value in the small holes of the polar plate is higher, more PbO and Pb exist in the polar plate, the pores are neutral or weakly alkaline, and the product formed by the positive polar plate is all alpha-PbO2。
Increasing the concentration of the formed electrolyte (for example, the density of the electrolyte is 1.05-1.06g/cm in the prior art)3Increased to 1.09-1.10g/cm of the present application3) Mainly when H in the pores of the positive plate2SO4When consumed, H in solution2SO4Continuously and rapidly diffuse into pores to shorten the duration of neutral or weak alkaline environment in the pores, and change the neutral or weak alkaline environment into acid environment as soon as possible to generate beta-PbO2Creates conditions and improves beta-PbO2The amount of production of (c).
The density adopted by the invention is 1.09-1.10g/cm3The electrolyte is formed, and after the formation is finished, the electrolyte circulates in the electrolyteThe circulating system is always in a circulating state, and the density of the dilute sulfuric acid in the electrolyte circulating system is only required to be increased to 1.31-1.33g/cm3And then the requirement of the storage battery for leaving factory on the density of the electrolyte can be met after continuous circulation for 15-30min, and the electrolyte in the horizontal storage battery does not need to be poured out and then subjected to secondary acid addition.
The two formation methods were subjected to battery performance tests, and the test methods and results are shown in table 5.
TABLE 5 comparative testing of cell Performance
As can be seen from the table 5, the two formation processes both meet the main index requirements, but the storage battery obtained by the formation method has improved battery capacity, low-temperature starting capability, charging acceptance capability and 50% DOD cycle durability, and has better performance.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. The formation method of the horizontal lead-acid storage battery is characterized by comprising the following steps:
step 1, injecting electrolyte into a storage battery through a liquid adding hole;
step 2, the formation is carried out according to the following method:
the first stage, after charging for 5h with 0.1C charging current, discharging for 0.5h with 0.05C discharging current;
in the second stage, after charging for 5h with 0.15C charging current, discharging for 0.5h with 0.075C discharging current;
in the third stage, after charging for 4h with 0.2C charging current, discharging for 0.5h with 0.1C discharging current;
a fourth stage, after charging for 4 hours with a charging current of 0.25C, discharging for 0.5 hours with a discharging current of 0.125C;
a fifth stage, after charging for 3h with 0.3C charging current, discharging for 0.5h with 0.15C discharging current;
a sixth stage, after charging for 3h with a charging current of 0.25C, discharging for 0.5h with a discharging current of 0.125C;
a seventh stage, after charging for 2h with 0.2C charging current, discharging for 0.5h with 0.1C discharging current;
in the eighth stage, after charging for 2 hours with 0.15C charging current, discharging for 0.5 hours with 0.075C discharging current;
a ninth stage, after charging for 1h with 0.1C charging current, discharging for 0.5h with 0.05C discharging current;
in the tenth stage, after charging for 1h with a charging current of 0.05C, discharging for 0.5h with a discharging current of 0.025C.
2. The method for forming a horizontal lead-acid battery according to claim 1, wherein the density of the electrolyte added in step 1 is 1.09-1.1g/cm3The temperature of the electrolyte is 5-10 ℃.
3. The method for forming a horizontal lead-acid battery according to claim 2, wherein the temperature of the electrolyte is maintained at 5 ℃ to 45 ℃ during the formation stage in step 2.
4. The method for forming the horizontal lead-acid storage battery according to claim 3, wherein in the forming stage, the high-temperature electrolyte flows out of a preformed hole in the lower part of the storage battery and is pumped into a cooling system, and the cooled electrolyte is circularly injected into the storage battery for forming.
5. The method for forming a horizontal lead-acid storage battery according to claim 4, wherein the cooling system comprises an electrolyte circulation system connected with the preformed hole and the charging hole respectively, and an electrolyte cooling system connected with the electrolyte circulation system.
6. The method for forming a horizontal lead-acid storage battery according to claim 5, wherein the electrolyte circulating system comprises a high-temperature tank communicated with the prepared hole through a first pipeline, a low-temperature tank connected with the high-temperature tank through a second pipeline, and the low-temperature tank is communicated with the liquid adding hole through a third pipeline; a first pump body is arranged between the preformed hole and the high-temperature tank, a second pump body is arranged between the high-temperature tank and the low-temperature tank, and a third pump body is arranged between the low-temperature tank and the liquid feeding hole.
7. The formation method of the horizontal lead-acid storage battery according to claim 6, wherein the electrolyte cooling system comprises a spray cooling tower and a plate heat exchanger connected with the spray cooling tower through a fourth pipeline, and a fourth pump body is arranged between the spray cooling tower and the plate heat exchanger; the second pipeline penetrates through the plate heat exchanger, and the second pump body is arranged between the plate heat exchanger and the low-temperature tank.
8. A horizontal lead-acid battery, characterized in that it is obtained by the formation method of any one of claims 1 to 7.
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