CN109273712A - A kind of positive electode of lead battery lead plaster and preparation method thereof - Google Patents
A kind of positive electode of lead battery lead plaster and preparation method thereof Download PDFInfo
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- CN109273712A CN109273712A CN201811250312.2A CN201811250312A CN109273712A CN 109273712 A CN109273712 A CN 109273712A CN 201811250312 A CN201811250312 A CN 201811250312A CN 109273712 A CN109273712 A CN 109273712A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/56—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead
- H01M4/57—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of lead of "grey lead", i.e. powders containing lead and lead oxide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of positive electode of lead battery lead plasters and preparation method thereof, belong to battery technology field, the anode diachylon includes lead powder, additive, water and sulfuric acid solution, it is in terms of 100 parts by lead powder parts by weight, the additive includes 3~7 parts of brown lead oxide, 0.001~0.1 part of (different) niacinamide, 0.01~0.5 part of polyester fiber, 0.02~0.5 part of antimony oxide, 0.02~0.5 part of stannous sulfate, 0.02~0.2 part of carbon material.The present invention utilizes α-PbO2Have the function of that good electric conductivity plays conducting matrix grain structure in Battery formation and improves formation efficiency, shortens the chemical conversion time；In addition, α-PbO2With good electrochemical stability, good skeleton structure is kept in battery use, (different) niacinamide can be effectively adsorbed in PbO simultaneously2And the surface modification pole plate performance of lead sulfate crystal structure, and then promote battery cycle life.
Description
Technical field
The present invention relates to battery technology fields, and in particular to a kind of positive electode of lead battery lead plaster and preparation method thereof.
Background technique
The a member of lead-acid battery as electrochmical power source, in the role that energy storage field performer holds the balance.Plumbic acid stores
Battery because its heavy-current discharge performance, good safety and lower cost electric car, hybrid electric vehicle, it is electronic from
Large-scale application has been obtained in driving, wind-power electricity generation, solar battery and communication base station facility.
Constitute lead storage battery the basic element of character and material include: positive plate, negative plate, electrolyte or be commonly called as electro-hydraulic, partition,
Cell jar etc..Wherein anode becomes apparent battery performance influence, and positive plate active material is in the form of brown lead oxide again
In the presence of.Brown lead oxide can be divided into α type and β type again, and the brown lead oxide of two kinds of crystal forms plays a different role in pole plate,
In, α-PbO2With relatively stable electrochemical properties, skeleton function is played to maintain the good electric conductivity of pole plate, ensures battery
Service life；β-PbO2Electro-chemical activity with higher is the energy-structure of battery, ensures cell discharge performance.
Currently, the sulfation of positive material(PAM) softening and battery pole plates is the dominant failure mode of battery, prevent
There are two types of the modes of positive material(PAM) softening relative efficiency, and one, improve mixing paste and cured temperature in production process, it improves just
The ratio of four basic lead sulphates in the active material of pole, two, four basic lead sulphates are directly added in mixing paste.
Application publication number is that the patent document of 107742724 A of CN discloses a kind of lead-acid accumulator anode diachylon, by matter
Measure percentages, raw material composition are as follows: lead powder 78%-84%, red lead 1%-3%, staple fiber 0.06%-0.12%, graphite
0.2%-0.4%, sulfuric acid 6.8%-8.2% and water 7.8%-10.8%.Red lead can promote pole plate to be melted into, and it is difficult to reduce chemical conversion
Degree improves battery initial capacity；Staple fibre can be improved the intensity of lead plaster, and then increase the toughness of accumulator plate, prevent
Lead plaster falls off；Graphite additive is not only remarkably improved positive electrode active material utilization, but also can effectively inhibit positive-active
The decaying of material utilization improves the service life of battery to increase the capacity of battery.
The patent document that application notification number is 108428890 A of CN discloses a kind of lead-acid accumulator anode diachylon, with
Weight percentage indicates that raw material forms are as follows: lead powder 75~85%, sulfuric acid 8~15%, stannous sulfate 0.1~0.3% are conductive
Fiber 0.05~0.15%, aquadag 0.2~0.5%, gallic oxide 0.8~1.5%, sodium pyrophosphate 0.05%~
0.15%, surplus is deionized water；The sum of each raw material weight percentage composition is 100%.It through the above technical solution can be effective
The binding force of grid and anode diachylon, prevents active material from falling off, while improving anode during raising lead-acid storage battery production
The electric conductivity and utilization rate of active material and the uniformity of current distribution are finally reached the effect for extending battery life.
Summary of the invention
The purpose of the present invention is to provide a kind of positive electode of lead battery lead plasters, to improve sulfation existing for positive plate,
Improve the active substance particle size (inhibiting lead sulfate particle growth) in battery pole plates charge and discharge process.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of positive electode of lead battery lead plaster, including lead powder, additive, water and sulfuric acid solution, with lead powder parts by weight for 100 parts
Meter, the additive include 3~7 parts of brown lead oxide, 0.001~0.1 part of (different) niacinamide, 0.01~0.5 part of polyester fiber,
0.02~0.5 part of antimony oxide, 0.02~0.5 part of stannous sulfate, 0.02~0.2 part of carbon material.
The additive amount of water is 9~12 parts, and the sulfuric acid solution is that density is 1.40g/cm3Dilute sulfuric acid, additive amount 6
~10 parts.
Preferably, the degree of oxidation of lead powder is 75%~80%, partial size D50It is 2.5~3.5 μm.
The brown lead oxide is α-PbO2。
The molecular formula of described (different) niacinamide is C6H6N2O, molecular weight: 122.13.
6~12 μm of the diameter of the polyester fiber, 2~5mm of length.
The carbon material is aquadag, facilitates the electric conductivity for improving positive green plate.
Preferably, the additive includes: 5 parts of brown lead oxide, 0.05 part of (different) niacinamide, polyester fiber 0.05
Part, 0.1 part of antimony oxide, 0.1 part of stannous sulfate, 0.2 part of carbon material.
The present invention also provides the methods of the preparation positive electode of lead battery lead plaster, comprising the following steps:
(1) brown lead oxide, polyester fiber, antimony oxide, stannous sulfate and carbon material are premixed, adds lead powder stirring
It mixes, obtains mixed powder；
(2) (different) niacinamide solution is made by (different) niacinamide is soluble in water, then (different) niacinamide solution is added
Enter into mixed powder, stirs；Then sulfuric acid solution is added, adds 45~65 DEG C of temperature of control during sulfuric acid solution, continues to stir
Mixing is mixed, the positive electode of lead battery lead plaster is made in cream out.
Sulfuric acid and lead powder, which react, after acid adding discharges heat, and control temperature can be to avoid " the heat mistake inside paste mixing machine
Control " phenomenon controls mixing paste temperature using the cooling system of paste mixing machine, keeps the growth of temperature control 3BS, sulfuric acid leading crystal, keep away
Exempt from the formation (chemical conversion of 4BS lead plaster pole plate difficulty) of larger-size 4BS crystal.
Preferably, (different) niacinamide solution is added to mixing with the speed of 50~150mL/min and does in step (2)
In powder, stir 5~15 minutes；Sulfuric acid solution is added in 10~15min in a manner of spraying, and continues stirring 10~20 minutes.
Preferably, temperature when cream is not higher than 45 DEG C out in step (2).After control paste outer temperature can be to avoid cream out
The variation of lead plaster apparent gravity caused by the moisture that lead plaster is taken away by heat dissipation, and also to avoid when coated plate lead plaster due to higher temperature
Degree influences to apply cream quality (tightness degree of the lead plaster in conjunction with grid) when contacting with cold plate grid, and further influences plate in solidification
The formation of grid lead plaster interfacial corrosion layer.
It is that the present invention has the utility model has the advantages that
Compounding ingredients lead plaster provided by the invention, due to α-PbO2It plays and leads in Battery formation with good electric conductivity
The effect of electric skeleton structure improves formation efficiency, shortens the chemical conversion time；In addition, α-PbO2With good electrochemical stability,
Good skeleton structure is kept in battery use, promotes battery cycle life, (different) niacinamide can effectively be inhaled simultaneously
It is attached to PbO2And the surface modification pole plate performance of lead sulfate crystal structure, and then promote battery cycle life.
Detailed description of the invention
Fig. 1 is that pole plate SEM appearance structure after Battery formation is made in embodiment 1.
Fig. 2 is that pole plate SEM appearance structure after Battery formation is made in embodiment 2.
Fig. 3 is that pole plate SEM appearance structure after Battery formation is made in comparative example 1.
Specific embodiment
In order to better understand and explain the present invention, the present invention is illustrated combined with specific embodiments below.
Embodiment 1
1, according to the following preparation anode diachylon material that requires: 100 parts of lead powder, 5 parts of brown lead oxide, (different) niacinamide 0.05
Part, 12 parts of deionized water, density 1.40g/cm310 parts of sulfuric acid solution, 0.05 part of polyester fiber, 0.1 part of antimony oxide,
0.1 part of stannous sulfate, 0.2 part of carbon material.
2, by α-PbO2, polyester fiber, antimony oxide, stannous sulfate, carbon material after sufficiently premixing, together with lead powder
It is added in paste mixing machine, booting stirring 5 minutes；It is slowly uniformly added into the dissolution pure water of (different) niacinamide, continues 6 points of stirring
Clock；It is uniformly added into sulfuric acid solution according to the ratio in a manner of shape spray in 15min, paste mixing machine is opened while dilute sulfuric acid is added
Air inlet fan and recirculated cooling water control temperature 60 C, after sulfuric acid is added, then continuously stirs 10min and go out cream, paste outer temperature is not
Higher than 45 DEG C, lead battery anode diachylon is obtained.
Then coated plate, solidification, drying, fragment, assembly are carried out, performance is carried out to battery pole plates and battery after container formation
Detection, as a result as shown in figure 1 and table 1.
Fig. 1 is the niacinamide and α-PbO for adding certain content2The microstructure of battery positive plate afterwards.As shown in Figure 1,
Active material is made of the lesser focusing particles body of size, compared to the active material pattern in Fig. 3 (comparative example 1), pole plate
Active material primary particle size fall to approximately 0.3 μm by 0.5 μm.
Embodiment 2
1, require material needed for preparing according to following: 100 parts of lead powder, 5 parts of brown lead oxide, 0.1 part of (different) niacinamide is gone
12 parts of ionized water, 10 parts of sulfuric acid solution, 0.05 part of polyester fiber, 0.1 part of antimony oxide, 0.1 part of stannous sulfate, carbon material
0.2 part.
2, after sufficiently premixing α-PbO2, polyester fiber, antimony oxide, stannous sulfate, carbon material, add together with lead powder
Enter in paste mixing machine, booting stirring 5~10 minutes；Slowly be uniformly added into the dissolution pure water of (different) niacinamide, continue stirring 5~
10 minutes；It is uniformly added into sulfuric acid solution according to the ratio in a manner of shape spray in 15min, opens mixing paste while dilute sulfuric acid is added
The air inlet fan and recirculated cooling water of machine control temperature 60 C, after sulfuric acid is added, then continuously stirs 10min and go out cream, out cream temperature
Degree is not higher than 45 DEG C, obtains lead battery anode diachylon.
Then coated plate, solidification, drying, fragment, assembly are carried out, performance is carried out to battery pole plates and battery after container formation
Detection, as a result as shown in Figure 2 and Table 1.
Fig. 2 is to be added to niacinamide and α-PbO2The microstructure of battery positive plate afterwards.As shown in Fig. 2, working as Buddhist nun gram acyl
It is mostly that corynebacterium structure is then further assembled that amine additive amount, which further increases rear active material pattern, simultaneously containing certain
Particulate matter aggregation.
Comparative example 1
1, according to the following required material of preparation that requires: 100 parts of lead powder, 5 parts of red lead, 12 parts of deionized water, sulfuric acid solution 10
Part, 0.05 part of polyester fiber, 0.1 part of antimony oxide, 0.1 part of stannous sulfate, 0.2 part of carbon material.
2, after red lead, fiber, antimony oxide, stannous sulfate, carbon material being sufficiently pre-mixed, together with lead powder be added and
In cream machine, booting stirring (dry-mixed) 5 minutes；It is slowly uniformly added into pure water and continues stirring 6 minutes；With shape spray in 15min
Mode is uniformly added into sulfuric acid solution (ρ=1.4g/cm according to the ratio3), the air inlet fan of paste mixing machine is opened while dilute sulfuric acid is added
And recirculated cooling water, temperature 60 C is controlled, goes out cream after sulfuric acid is added, then after persistently stirring 10min, control paste outer temperature is not
Higher than 45 DEG C.
Then coated plate, solidification, drying, fragment, assembly are carried out, uses internal formation process to battery after semi-finished product battery acid adding
It is melted into, performance detection then is carried out to battery pole plates and battery, as a result as shown in Figure 3 and Table 1.
Fig. 3 is to be not added with α-PbO2And the microcosmic structure appearance of the battery positive plate prepared when niacinamide.As shown in Figure 3
It is found that active substance particle size is larger, include the particulate matter taken measurements greatly greater than 0.5 μm.
Table 1
Table 1 is the phase structure and circulating battery number of the lead-acid battery positive plate of embodiment preparation.As seen from table, when adding
Add α-PbO2α-PbO in gained positive plate after being melted into afterwards2Content is promoted to 41% or so by 30.5% (comparative example 1), and corresponding
Cycle performance of battery has also obtained certain improvement, and battery cycle life 1.0C (352 times) extends 30%.
Claims (8)
1. a kind of positive electode of lead battery lead plaster, including lead powder, additive, water and sulfuric acid solution, which is characterized in that with lead powder weight
Part is 100 parts of meters, and the additive includes 3~7 parts of brown lead oxide, 0.001~0.1 part of (different) niacinamide, polyester fiber
0.01~0.5 part, 0.02~0.5 part of antimony oxide, 0.02~0.5 part of stannous sulfate, 0.01~0.5 part of carbon material.
2. positive electode of lead battery lead plaster as described in claim 1, which is characterized in that the degree of oxidation of lead powder be 75%~
80%, partial size D50It is 3.0 ± 0.5 μm.
3. positive electode of lead battery lead plaster as described in claim 1, which is characterized in that the brown lead oxide is α-PbO2。
4. positive electode of lead battery lead plaster as described in claim 1, which is characterized in that the carbon material is aquadag.
5. positive electode of lead battery lead plaster according to any one of claims 1-4, which is characterized in that the additive includes:
5 parts of brown lead oxide, 0.05 part of (different) niacinamide, 0.05 part of polyester fiber, 0.1 part of antimony oxide, 0.1 part of stannous sulfate,
0.2 part of carbon material.
6. the preparation method of positive electode of lead battery lead plaster as described in any one in claim 1-5, comprising the following steps:
(1) brown lead oxide, polyester fiber, antimony oxide, stannous sulfate and carbon material are premixed, it is mixed adds lead powder stirring
It is even, obtain mixed powder；
(2) (different) niacinamide solution is made by (different) niacinamide is soluble in water, then (different) niacinamide solution is added to
In mixed powder, stirring；Then sulfuric acid solution is added, adds 45~65 DEG C of temperature of control during sulfuric acid solution, it is mixed to continue stirring
Even, the positive electode of lead battery lead plaster is made in cream out.
7. preparation method as claimed in claim 6, which is characterized in that in step (2), (different) niacinamide solution with 50~
The speed of 150mL/min is added in mixed powder, is stirred 5~15 minutes；Sulfuric acid solution is in a manner of spraying in 10~15min
It inside adds, continues stirring 10~20 minutes.
8. preparation method as claimed in claim 6, which is characterized in that in step (2), temperature when cream is not higher than 45 DEG C out.
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| CN201811250312.2A CN109273712B (en) | 2018-10-25 | 2018-10-25 | Positive lead plaster of lead storage battery and preparation method thereof |
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| CN201811250312.2A CN109273712B (en) | 2018-10-25 | 2018-10-25 | Positive lead plaster of lead storage battery and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110265662A (en) * | 2019-06-24 | 2019-09-20 | 天能电池(芜湖)有限公司 | A kind of additive improving the anti-softening ability of lead-acid battery anode and battery life |
| CN110350163A (en) * | 2019-06-21 | 2019-10-18 | 天能电池集团股份有限公司 | A kind of production method of lead storage battery |
| CN110556515A (en) * | 2019-08-19 | 2019-12-10 | 天能电池集团股份有限公司 | preparation method and application of positive plate of lead storage battery |
| CN111430717A (en) * | 2020-04-01 | 2020-07-17 | 超威电源集团有限公司 | Positive plate of lead-acid storage battery, preparation method of positive plate and storage battery |
| CN111640942A (en) * | 2020-06-03 | 2020-09-08 | 超威电源集团有限公司 | Enhanced antioxidant conductive auxiliary agent, lead-acid storage battery positive lead paste and preparation method |
| CN111799463A (en) * | 2020-07-13 | 2020-10-20 | 天能电池(芜湖)有限公司 | High-capacity long-life battery |
| CN112768640A (en) * | 2020-12-30 | 2021-05-07 | 蚌埠睿德新能源科技有限公司 | Positive active material of lead-acid storage battery electrode and product thereof |
| CN113394408A (en) * | 2021-06-17 | 2021-09-14 | 昆明高聚科技有限公司 | Long-life light composite positive grid and preparation method thereof, and positive electrode plate and preparation method thereof |
| CN114530600A (en) * | 2021-10-28 | 2022-05-24 | 安徽力普拉斯电源技术有限公司 | Formula and preparation method of positive lead paste of energy storage battery |
| CN114597354A (en) * | 2022-02-25 | 2022-06-07 | 天能电池集团股份有限公司 | Lead storage battery positive electrode lead paste and preparation method thereof, and lead storage battery |
| CN117219768A (en) * | 2023-08-21 | 2023-12-12 | 广州埃登达化工有限公司 | Battery anode lead paste, preparation method thereof and storage battery |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110350163A (en) * | 2019-06-21 | 2019-10-18 | 天能电池集团股份有限公司 | A kind of production method of lead storage battery |
| CN110350163B (en) * | 2019-06-21 | 2020-10-13 | 天能电池集团股份有限公司 | Production method of lead storage battery |
| CN110265662A (en) * | 2019-06-24 | 2019-09-20 | 天能电池(芜湖)有限公司 | A kind of additive improving the anti-softening ability of lead-acid battery anode and battery life |
| CN110556515B (en) * | 2019-08-19 | 2020-12-11 | 天能电池集团股份有限公司 | Preparation method and application of positive plate of lead storage battery |
| CN110556515A (en) * | 2019-08-19 | 2019-12-10 | 天能电池集团股份有限公司 | preparation method and application of positive plate of lead storage battery |
| CN111430717A (en) * | 2020-04-01 | 2020-07-17 | 超威电源集团有限公司 | Positive plate of lead-acid storage battery, preparation method of positive plate and storage battery |
| CN111640942B (en) * | 2020-06-03 | 2021-08-10 | 超威电源集团有限公司 | Enhanced antioxidant conductive auxiliary agent, lead-acid storage battery positive lead paste and preparation method |
| CN111640942A (en) * | 2020-06-03 | 2020-09-08 | 超威电源集团有限公司 | Enhanced antioxidant conductive auxiliary agent, lead-acid storage battery positive lead paste and preparation method |
| CN111799463A (en) * | 2020-07-13 | 2020-10-20 | 天能电池(芜湖)有限公司 | High-capacity long-life battery |
| CN112768640A (en) * | 2020-12-30 | 2021-05-07 | 蚌埠睿德新能源科技有限公司 | Positive active material of lead-acid storage battery electrode and product thereof |
| CN113394408A (en) * | 2021-06-17 | 2021-09-14 | 昆明高聚科技有限公司 | Long-life light composite positive grid and preparation method thereof, and positive electrode plate and preparation method thereof |
| CN114530600A (en) * | 2021-10-28 | 2022-05-24 | 安徽力普拉斯电源技术有限公司 | Formula and preparation method of positive lead paste of energy storage battery |
| CN114597354A (en) * | 2022-02-25 | 2022-06-07 | 天能电池集团股份有限公司 | Lead storage battery positive electrode lead paste and preparation method thereof, and lead storage battery |
| CN114597354B (en) * | 2022-02-25 | 2024-08-30 | 天能电池集团股份有限公司 | Positive electrode lead paste of lead storage battery, preparation method of positive electrode lead paste and lead storage battery |
| CN117219768A (en) * | 2023-08-21 | 2023-12-12 | 广州埃登达化工有限公司 | Battery anode lead paste, preparation method thereof and storage battery |
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