CN107732161A - A kind of chloride plate preparation method for reducing polar board surface dry linting rate - Google Patents
A kind of chloride plate preparation method for reducing polar board surface dry linting rate Download PDFInfo
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- CN107732161A CN107732161A CN201710855282.7A CN201710855282A CN107732161A CN 107732161 A CN107732161 A CN 107732161A CN 201710855282 A CN201710855282 A CN 201710855282A CN 107732161 A CN107732161 A CN 107732161A
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- board surface
- polar board
- mixed
- acid
- lead plaster
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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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- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
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Abstract
The invention discloses a kind of chloride plate preparation method for reducing polar board surface dry linting rate, including with cream process, polar board surface coating or spray process, described and cream process includes the addition of addition conductive adhesive and control acid addition rate and temperature changes lead plaster structure;Described polar board surface coating or spray process, polar board surface active material is connected by using polymer sol, polar board surface coating binding force is improved to reduce the floating powder during point brushing piece, this is also beneficial to solve the problems such as relatively low battery capacity caused by floating powder during chemical conversion and follow-up micro-short circuit, when pole plate, which is assembled into battery, fills chemical conversion, be dissolved in as temperature rises polymer sol by polymerisation in electrolyte, can effectively improve the mixed initial stage internal temperature of battery of acid it is too high caused by formation effect it is bad the problem of.
Description
Technical field
The present invention relates to lead-acid battery manufacturing technology field, more particularly to a kind of lead electric power storage for reducing polar board surface dry linting rate
Pond pole plate preparation method.
Background technology
Lead-acid accumulator have it is cheap, it is easy to use, the characteristics of stable performance, be widely applied to always each
Field, as one of main body used in secondary power supply, commercially occupy very big share.But as Environmental is protected
Shield policy is constantly put into effect, it is meant that the formulation of lead-acid storage battery production enterprise production technology should meet environment-friendly requirement.
Using and reclaiming and suffer from strict system regulationses in lead-acid accumulator.And in the process caused waste material or
Raw material can be reduced largely in the process, can effectively be mitigated lead-acid accumulator environmental protection pressure, be improved the protective capability to environment.Lead
Sour battery can produce many lead dust particles in process of production, especially during pole plate point brush, and how reduce it
Surface picking rate turns into existing stage urgent problem.
The content of the invention
The present invention be in order to when overcoming chemical conversion in the prior art micro-short circuit situation caused by floating powder make battery capacity relatively low and
The problem of cycle life decays too early, there is provided a kind of chloride plate preparation method for reducing polar board surface dry linting rate, reduce
The floating powder divided during brushing piece, effectively improves battery capacity and cycle life.During battery acid filling chemical conversion simultaneously, pass through polymerisation
Endothermic dissolution suppresses temperature and risen, and can effectively avoid acid adding stage internal temperature of battery is too high from causing formation effect is bad to ask
Topic.
To achieve these goals, the present invention uses following technical scheme:
1. a kind of chloride plate preparation method for reducing polar board surface dry linting rate, the preparation method comprise the steps of:
(1)And cream:It is 1000 in mass ratio by lead oxide powder and additive:(1~20)After well mixed, add binding agent, go from
Sub- water and dilute sulfuric acid, are prepared into lead plaster, and sulfuric acid progress acid is added into lead plaster and is mixed, 43 ~ 50 DEG C is down to lead plaster temperature, obtains institute
The lead plaster needed, carry out coated plate;
(2)Polar board surface coating or spray process:
A, it is in mass ratio by polymerizable compound presoma, polymeric material and polyvinyl alcohol(1.5~3.5):(5~8):(15~22)
It is well mixed;
B, organic solvent regulation mixing is added in the mixture into step a, mixed solution is obtained by extraction, by the mixed solution
Good pressure distribution is handled, and is stirred 2 ~ 3 hours under normal temperature, and washing is dry must to be mixed to prepare thing;
C, it is 1 in mass ratio that will be mixed to prepare thing, inorganic silicate, aerosil and acid solution:(0 .3~0.5):(15~
34)Mixing, ultrasonic disperse obtain mixed sols, and vacuum stands 10 ~ 15min;The particle diameter of the aerosil be 30 ~
80nm;
D, the mixed sols described in step c is sheared into 3 ~ 10min, obtains mixed gel, then mixed gel is sprayed at pole plate
The solidification of surface drying kiln is crossed behind surface, obtains the chloride plate.Polar board surface coating or spray process, by using polymerization
Thing colloidal sol connects polar board surface active material, and polar board surface coating binding force is improved to reduce the floating powder during point brushing piece,
This is also beneficial to solve the problems such as relatively low battery capacity caused by floating powder during chemical conversion and follow-up micro-short circuit.When pole plate is assembled into electricity
When basin irrigation fills chemical conversion, it is dissolved in as temperature rises polymer sol by polymerisation in electrolyte, can effectively suppresses acid
The problems such as formation effect caused by mixed initial stage internal temperature of battery is too high is bad.
Preferably, step(1)Described in acid is mixed divides four-part form to carry out:
When lead plaster temperature is less than 48 DEG C, the adding rate of sulfuric acid is 0.17 ~ 0.22L/s;
When lead plaster temperature is 48 ~ 57 DEG C, the adding rate of sulfuric acid is adjusted to the 70 ~ 85% of original flow velocity;
When lead plaster temperature is 57 ~ 68 DEG C, the adding rate of sulfuric acid is adjusted to the 50 ~ 60% of original flow velocity;
When lead plaster temperature is more than 68 DEG C, lead plaster temperature is maintained to keep 3 ~ 5min.Binding agent is added with cream process and control adds
Mollic acid and temperature, change lead plaster structure, strengthen pole plate internal bond strength.
Preferably, whole acid adding process control is in 12~15min.
Preferably, step(1)Described in adhesive be poly- diacrylate ethylene glycol fat and polymethyl methacrylate second
One or both of two alcohol esters.Addition is consideration and cream step acid adding stage lead plaster after lead powder is well mixed with additive
Temperature stabilization rises, and lead plaster can be made to be effectively combined and harden with binding agent.
Preferably, it is characterized in that, step(a)Described in polymerizable compound presoma be selected from diethyl triamine and hexamethyl
Diamines, the polymeric material are selected from the one or more in 3,4- methylene dioxies acetophenone, ortho-terphenyl and dibenzofurans.
Preferably, step(b)Described in organic solvent be 1,2- dichloro-benzenes-chloroformic solution and ethers organic solution in
Any one.
Preferably, step(b)Described in the quality of polymerizable compound presoma contained in mixture and polymeric material
The mass ratio of summation and organic solution is 1:(50~85).
Preferably, step(c)Described in inorganic silicate be sodium metasilicate or potassium silicate.
Preferably, step(c)Described in acid solution be sulfuric acid, phosphoric acid, oxalic acid and citric acid solution in it is any one
Kind, wherein the mass fraction of sulfuric acid be 5 ~ 15wt% in the sulfuric acid solution, in the phosphoric acid, oxalic acid and citric acid solution arbitrarily
A kind of sour mass fraction is 0.5 ~ 3wt%.
Preferably, step(b)Described in good pressure distribution processing carried out in good pressure distribution equipment instrument, condition of high voltage is
15000 ~ 18000psi, mixing time are 5 ~ 8h, and speed of agitator is 800 ~ 1100rpm.
Therefore, the present invention has the advantages that:(1)The floating powder during point brush is reduced, when advantageously accounting for chemical conversion
Battery capacity caused by floating powder is relatively low and the problems such as follow-up micro-short circuit;(2)Effectively suppress the mixed initial stage inside battery of acid
The problems such as formation effect caused by temperature is too high is bad;(3)Include the addition of addition conductive adhesive and control acid adding with cream process
Speed and temperature change lead plaster structure, strengthen pole plate internal bond strength.
Brief description of the drawings
Fig. 1 is the discharge time of the present invention with cycle-index change curve.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
The chloride plate preparation method of polar board surface dry linting rate is reduced, is comprised the steps of:
1 and cream process
1000 mass parts lead oxide powder add the acryl resin class of 5 parts by weight in paste mixing machine after being well mixed with additive
The poly- diacrylate ethylene glycol fat of binding agent slowly stirs a period of time, then adds deionized water and sulfuric acid solution, is prepared into
Lead plaster, the sulfuric acid progress acid for being slowly added to get ready material in the positive and negative electrode lead plaster after above-mentioned wet mixing respectively mix, and mixing divides four-part form
Carry out:
A, when lead plaster temperature is in less than 48 DEG C, the adding rate of sulfuric acid is controlled in 0.17%L/s, wherein above-mentioned L tables
Show the volume of sulfuric acid solution,
B, when lead plaster temperature is between 48 ~ 57 DEG C, the adding rate of sulfuric acid is adjusted to the 70% of original flow velocity,
C, when lead plaster temperature is between 57 ~ 68 DEG C, the adding rate of sulfuric acid is adjusted to the 50% of original flow velocity,
D, when lead plaster temperature rises to 68 DEG C, lead plaster temperature is maintained to keep 3min to form the generation of four basic lead sulphates
Stage preserves, and at 12 minutes, acid adding continued stirring 5 minutes after terminating for whole acid adding process control, until lead plaster temperature is down to 43
DEG C, you can required lead plaster is obtained, reusable lead cream carries out coated plate.
2nd, polar board surface coating or spray process
Step 1:By polymerizable compound presoma diethyl triamine, polymeric material 3,4- methylene dioxy acetophenones and neighbour three
Benzol mixture and polyvinyl alcohol in proportion 1.5:5:15 is well mixed;
Step 2:Organic solvent 1 will be added in upper step mixture, 2- dichloro-benzenes-chloroformic solution regulation mixes, before polymerizable compound
The liquid-solid ratio for driving body, polymeric material mixture quality and organic solution is 1g:25mL.Pour into reaction high pressure in autoclave
Dispersing apparatus instrument carries out good pressure distribution and handled 3 times, is 15000psi under condition of high voltage, and mixing time is 5 hours, and speed of agitator is
800rpm.The polymer dispersion liquid handled well stirs 2 hours under conditions of normal temperature, the mixed with polymers liquid stablized;
Step 3, polymeric precipitate is collected by filtration in stable mixed with polymers liquid, after being washed with ethanol or pure water
Dry, thing must be mixed to prepare;
Step 4:Above-mentioned obtained thing, inorganic silicic acid sodium, aerosil, water are 1 in mass ratio:0 .3:0 .05:15 is mixed
Close, obtain mixture, it is scattered then to carry out ultrasonic agitation, during add sulfuric acid, it is molten to be configured to the sulfuric acid that mass concentration is 12%
Liquid, the obtained compositions are mixed with the silica mixed gel, then stand 10min under vacuum.
To silica mixed sols, the particle diameter of the gas phase nano silicon is 50nmnm;
Step 5:The silica mixed sols is sheared into 3min before service stage, obtains silica mixed gel;
Step 6:The solidification of surface drying kiln will be crossed into being sprayed at containing silica mixed sols after polar board surface, and obtain lead accumulator
Pole plate.
Embodiment 2
1 and cream process
1000 mass parts lead oxide powder add the acryl resin of 15 parts by weight in paste mixing machine after being well mixed with additive
The poly- diacrylate ethylene glycol fat of class binding agent slowly stirs a period of time, then adds deionized water and sulfuric acid solution, prepares
Into lead plaster
It is mixed to be slowly added to get ready the sulfuric acid progress acid of material in the positive and negative electrode lead plaster after above-mentioned wet mixing respectively, mixes and divides four-part form
Carry out:
A, when lead plaster temperature is in less than 48 DEG C, the adding rate of sulfuric acid is controlled in 0.22%L/s, wherein above-mentioned L tables
Show the volume of sulfuric acid solution,
B, when lead plaster temperature is between 48 ~ 57 DEG C, the adding rate of sulfuric acid is adjusted to the 85% of original flow velocity,
C, when lead plaster temperature is between 57 ~ 68 DEG C, the adding rate of sulfuric acid is adjusted to the 60% of original flow velocity,
D, when lead plaster temperature rises to 68 DEG C, lead plaster temperature is maintained to keep 5min to form the generation of four basic lead sulphates
Stage preserves, and at 15 minutes, acid adding continued stirring 8 minutes after terminating for whole acid adding process control, until lead plaster temperature is down to 50
DEG C, you can required lead plaster is obtained, reusable lead cream carries out coated plate.
2nd, polar board surface coating or spray process
Step 1:By polymerizable compound presoma hexamethylene diamine, polymeric material dibenzofurans and polyvinyl alcohol in proportion
3.5:8:22 is well mixed;
Step 2:Organic solvent 1 will be added in upper step mixture, 2- dichloro-benzenes-chloroformic solution regulation mixes, before polymerizable compound
The liquid-solid ratio for driving body, polymeric material mixture quality and organic solution is 1g:40mL, pour into reaction high pressure in autoclave
Dispersing apparatus instrument carries out good pressure distribution and handled 5 times, is 18000psi under condition of high voltage, and mixing time is 8 hours, and speed of agitator is
1100rpm.The polymer dispersion liquid handled well stirs 3 hours under conditions of normal temperature, the mixed with polymers liquid stablized;
Step 3, polymeric precipitate is collected by filtration in stable mixed with polymers liquid, after being washed with ethanol or pure water
Dry, thing must be mixed to prepare;
Step 4:Above-mentioned obtained thing, inorganic silicic acid potassium, aerosil, water are 1 in mass ratio:0 .5:0 .05:34 is mixed
Close, obtain mixture, it is scattered then to carry out ultrasonic agitation, during add phosphoric acid, it is molten to be configured to the phosphoric acid that mass concentration is 3%
Liquid, the obtained compositions are mixed with the silica mixed gel, then stand 15min under vacuum.
To silica mixed sols, the particle diameter of the gas phase nano silicon is 80nm;
Step 5:The silica mixed sols is sheared into 5min before service stage, obtains silica mixed gel;
Step 6:The solidification of surface drying kiln will be crossed into being sprayed at containing silica mixed sols after polar board surface, and obtain lead accumulator
Pole plate.
Embodiment 3
1 and cream process
1000 mass parts lead oxide powder add the acryl resin of 20 parts by weight in paste mixing machine after being well mixed with additive
Class binding agent polymethyl methacrylate ethylene glycol fat slowly stirs a period of time, then adds deionized water and sulfuric acid solution,
Lead plaster is prepared into, the sulfuric acid for being slowly added to get ready material in the positive and negative electrode lead plaster after above-mentioned wet mixing respectively carries out sour mixed, mixing point
Four-part form is carried out:
A, when lead plaster temperature is in less than 48 DEG C, by the adding rate control of sulfuric acid in 0.2%L/s, wherein above-mentioned L is represented
The volume of sulfuric acid solution,
B, when lead plaster temperature is between 48 ~ 57 DEG C, the adding rate of sulfuric acid is adjusted to the 80% of original flow velocity,
C, when lead plaster temperature is between 57 ~ 68 DEG C, the adding rate of sulfuric acid is adjusted to the 55% of original flow velocity,
D, when lead plaster temperature rises to 68 DEG C, lead plaster temperature is maintained to keep 5min to form the generation of four basic lead sulphates
Stage preserves, and at 14 minutes, acid adding continued stirring 8 minutes after terminating for whole acid adding process control, until lead plaster temperature is down to 48
DEG C, you can required lead plaster is obtained, reusable lead cream carries out coated plate.
2nd, polar board surface coating or spray process
Step 1:By polymerizable compound presoma hexamethylene diamine, polymeric material dibenzofurans and polyvinyl alcohol in proportion 3:
7:18 is well mixed;
Step 2:The regulation mixing of organic solvent diethyl ether solution, polymerizable compound presoma, polymerization material will be added in upper step mixture
The liquid-solid ratio for expecting mixture quality and organic solution is 1g:35mL, pour into reaction good pressure distribution equipment instrument in autoclave
Carry out good pressure distribution to handle 4 times, be 16000psi under condition of high voltage, mixing time is 7 hours, speed of agitator 900rpm.Place
The polymer dispersion liquid managed stirs 2 hours under conditions of normal temperature, the mixed with polymers liquid stablized;
Step 3:Polymeric precipitate is collected by filtration in stable mixed with polymers liquid, after being washed with ethanol or pure water
Dry, thing must be mixed to prepare;
Step 4:Above-mentioned obtained thing, inorganic silicic acid potassium, aerosil, water are 1 in mass ratio:0 .4:0 .2:30 mixing,
Obtain mixture, it is scattered then to carry out ultrasonic agitation, during add phosphoric acid, it is molten to be configured to the phosphoric acid that mass concentration is 0.5%
Liquid, the obtained compositions are mixed with the silica mixed gel, then stand 12min under vacuum.
To silica mixed sols, the particle diameter of the gas phase nano silicon is 65nm;
Step 5:The silica mixed sols is sheared into 4min before service stage, obtains silica mixed gel;
Step 6:The solidification of surface drying kiln will be crossed into being sprayed at containing silica mixed sols after polar board surface, and obtain lead accumulator
Pole plate.
As shown in figure 1, wherein series 2 is the chloride plate being prepared using method described in the embodiment of the present invention
Test result curve, series 1 are the chloride plate test result curves that common process is prepared, it can be seen that this
Inventing the chloride plate cycle-index that the chloride plate cycle ratio common process being prepared is prepared has
Increased, illustrate that service life is extended, and the impulse discharge time rises appreciably, and illustrates the lead electric power storage that the present invention is prepared
Pond polar plate battery capacity is improved.
Claims (10)
1. a kind of chloride plate preparation method for reducing polar board surface dry linting rate, it is characterized in that, the preparation method includes
Following steps:
(1)And cream:It is 1000 in mass ratio by lead oxide powder and additive:(1~20)After well mixed, add binding agent, go from
Sub- water and dilute sulfuric acid, are prepared into lead plaster, and sulfuric acid progress acid is added into lead plaster and is mixed, 43 ~ 50 DEG C is down to lead plaster temperature, obtains institute
The lead plaster needed, carry out coated plate;
(2)Polar board surface coating or spray process:
A, it is in mass ratio by polymerizable compound presoma, polymeric material and polyvinyl alcohol(1.5~3.5):(5~8):(15~22)
It is well mixed;
B, organic solvent regulation mixing is added in the mixture into step a, mixed solution is obtained by extraction, by the mixed solution
Good pressure distribution is handled, and is stirred 2 ~ 3 hours under normal temperature, and washing is dry must to be mixed to prepare thing;
C, it is 1 in mass ratio that will be mixed to prepare thing, inorganic silicate, aerosil and acid solution:(0 .3~0.5):(15~
34)Mixing, ultrasonic disperse obtain mixed sols, and vacuum stands 10 ~ 15min;The particle diameter of the aerosil be 30 ~
80nm;
D, the mixed sols described in step c is sheared into 3 ~ 10min, obtains mixed gel, then mixed gel is sprayed at pole plate
The solidification of surface drying kiln is crossed behind surface, obtains the chloride plate.
2. a kind of chloride plate preparation method for reducing polar board surface dry linting rate according to claim 1, its feature
It is step(1)Described in acid is mixed divides four-part form to carry out:
When lead plaster temperature is less than 48 DEG C, the adding rate of sulfuric acid is 0.17 ~ 0.22L/s;
When lead plaster temperature is 48 ~ 57 DEG C, the adding rate of sulfuric acid is adjusted to the 70 ~ 85% of original flow velocity;
When lead plaster temperature is 57 ~ 68 DEG C, the adding rate of sulfuric acid is adjusted to the 50 ~ 60% of original flow velocity;
When lead plaster temperature is more than 68 DEG C, lead plaster temperature is maintained to keep 3 ~ 5min.
3. a kind of chloride plate preparation method for reducing polar board surface dry linting rate according to claim 2, its feature
It is that whole acid adding process control is in 12~15min.
4. a kind of chloride plate preparation method for reducing polar board surface dry linting rate according to claim 1, its feature
It is step(1)Described in adhesive be poly- diacrylate ethylene glycol fat and polymethyl methacrylate ethylene glycol fat in one kind
Or two kinds.
5. a kind of chloride plate preparation method for reducing polar board surface dry linting rate according to claim 1, its feature
It is step(a)Described in polymerizable compound presoma be selected from diethyl triamine and hexamethylene diamine, the polymeric material is selected from 3,
One or more in 4- methylene dioxies acetophenone, ortho-terphenyl and dibenzofurans.
6. a kind of chloride plate preparation method for reducing polar board surface dry linting rate according to claim 1, its feature
It is step(b)Described in organic solvent be 1,2- dichloro-benzenes-chloroformic solution and ethers organic solution in any one.
7. a kind of chloride plate preparation method for reducing polar board surface dry linting rate according to claim 1, its feature
It is step(b)Described in the quality summation and organic solution of polymerizable compound presoma contained in mixture and polymeric material
Mass ratio be 1:(50~85).
8. a kind of chloride plate preparation method for reducing polar board surface dry linting rate according to claim 1, its feature
It is step(c)Described in inorganic silicate be sodium metasilicate or potassium silicate.
9. a kind of chloride plate preparation method for reducing polar board surface dry linting rate according to claim 1, its feature
It is step(c)Described in acid solution be sulfuric acid, phosphoric acid, oxalic acid and citric acid solution in any one, wherein the sulfuric acid
The mass fraction of sulfuric acid is 5 ~ 15wt% in solution, any one sour mass fraction in the phosphoric acid, oxalic acid and citric acid solution
For 0.5 ~ 3wt%.
10. a kind of chloride plate of reduction polar board surface dry linting rate according to claim 1 to 9 any one makes
Method, it is characterized in that, step(b)Described in good pressure distribution processing carried out in good pressure distribution equipment instrument, condition of high voltage is
15000 ~ 18000psi, mixing time are 5 ~ 8h, and speed of agitator is 800 ~ 1100rpm.
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CN111668456A (en) * | 2020-05-12 | 2020-09-15 | 吉林省凯禹电化学储能技术发展有限公司 | External application type lead-carbon start-stop battery negative plate and preparation method thereof and battery |
CN112768641A (en) * | 2021-01-20 | 2021-05-07 | 天能电池集团股份有限公司 | Preparation method of lead storage battery polar plate and lead storage battery polar plate |
CN114551815A (en) * | 2022-02-16 | 2022-05-27 | 天能电池集团(马鞍山)新能源科技有限公司 | Lead storage battery pole plate curing method |
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CN106910872A (en) * | 2017-01-22 | 2017-06-30 | 天能电池集团有限公司 | A kind of positive plate of lead storage battery and preparation method thereof |
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CN111668456A (en) * | 2020-05-12 | 2020-09-15 | 吉林省凯禹电化学储能技术发展有限公司 | External application type lead-carbon start-stop battery negative plate and preparation method thereof and battery |
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CN112768641A (en) * | 2021-01-20 | 2021-05-07 | 天能电池集团股份有限公司 | Preparation method of lead storage battery polar plate and lead storage battery polar plate |
CN114551815A (en) * | 2022-02-16 | 2022-05-27 | 天能电池集团(马鞍山)新能源科技有限公司 | Lead storage battery pole plate curing method |
CN114551815B (en) * | 2022-02-16 | 2023-09-22 | 天能电池集团(马鞍山)新能源科技有限公司 | Lead storage battery polar plate curing method |
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