CN106654217A - Composite carbon negative-electrode active material for lead carbon power battery as well as preparation method and application of composite carbon negative-electrode active material - Google Patents
Composite carbon negative-electrode active material for lead carbon power battery as well as preparation method and application of composite carbon negative-electrode active material Download PDFInfo
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- CN106654217A CN106654217A CN201710013020.6A CN201710013020A CN106654217A CN 106654217 A CN106654217 A CN 106654217A CN 201710013020 A CN201710013020 A CN 201710013020A CN 106654217 A CN106654217 A CN 106654217A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
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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
- H01M4/36—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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
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- 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 composite carbon negative-electrode active material for a lead carbon power battery. The material is prepared from the following components in percentage by weight: 0.7%-1.5% of barium sulfate, 0.08%-0.2% of polyester staple fiber, 0.2%-0.5% of humic acid, 0.2%-0.6% of HT-1 type lignin, 0.5%-3% of activated carbon, 0.1%-2% of graphene, 0.1%-2% of carbon nanotube, 0.1%-0.5% of bismuth sulfate, and 0.2%-0.5% of sodium carboxymethyl cellulose, 10%-15% of distilled water, 8%-10% of dilute sulfuric acid and 73%-79% lead powder. The material has the advantages that the composite carbon material comprising the activated carbon, graphene with the multi-layer structure and the carbon nanotube is used, the specific surface area of the negative-electrode active material is further increased, the battery has a better capacitance characteristic, instantaneous large current discharge property of the battery is enhanced, and the problem of sulfation of a negative electrode is effectively solved; at the same time, bismuth sulfate is added to the formula of the negative electrode, so that the hydrogen evolution potential of the battery can be effectively reduced, water loss of the battery is inhibited, and the service life of the battery is prolonged.
Description
Technical field
The present invention relates to a kind of lead carbon electrokinetic cell composite carbon negative electrode active material；The invention further relates to a kind of negative pole
The preparation method and application of active material.
Background technology
In the face of the traditional energy day by day exhausted continuous deterioration with global environment, the utilization of clean energy resource and the need of energy-conserving product
Ask more and more urgent.Electric automobile will be increasingly becoming the inevitable direction of China Automobile Industry as new cleaning fuel automobile, so
And because common lead-acid accumulator is present, resistance to low temperature is poor, cycle life is short, discharge capacity is low, discharge and recharge ability to accept is not strong
The shortcomings of, become and limit its key factor promoted and use in electric automobile field.Therefore, the lower temperature resistance of battery is improved
Can, the dehydration of battery is reduced, the high rate during charging-discharging and service life cycle for improving battery is always batteries of electric automobile
The technology emphasis of research and development.In the case where international advanced lead accumulator federation (ALABC) is supported, the concept of " superbattery " is suggested simultaneously
Researched and developed.Australia Commonwealth Scientific and Industrial Research Organisation first reported the sex work of starting of lead carbon superbattery, and
With Furukawa Electronic's Battery Company cooperation, lead carbon superbattery has been produced.Jing after driving the examination of road, it was demonstrated that it possesses the big of capacitor
Power and the jumbo characteristic of battery, are suitable for electrokinetic cell field and energy storage field.The lead carbon power of market sale at present
Battery can effectively suppress sulfation phenomenon of the battery under deeper cavity use condition, but due to the addition of in lead carbon battery compared with
Many carbon, reduces the liberation of hydrogen potential of battery, and dehydration is serious when causing battery to charge, and thermal runaway phenomenon easily occurs in battery.Therefore,
It is badly in need of a kind of method for solving above variety of problems.
The content of the invention
It is an object of the invention to provide a kind of composite carbon negative electrode active material and preparation method thereof, and using the negative pole
Active material prepares the negative plate of lead carbon electrokinetic cell.
The technical solution used in the present invention is：
A kind of lead carbon electrokinetic cell composite carbon negative electrode active material, its percentage is composed of the following components：Sulphur
Sour barium 0.7～1.5%, polyester staple fiber 0.08～0.2%, humic acid 0.2～0.5%, HT-1 types lignin 0.2～0.6%, activated carbon
0.5～3%, the Graphene 0.1～2% of sandwich construction, CNT 0.1～2%, bismuth sulfate 0.1～0.5%, carboxymethylcellulose calcium
Sodium 0.2～0.5%, distilled water 10～15%, concentration are 1.400g/ml dilute sulfuric acids 8～10%, lead powder 73～79%.
Specifically preparation process is：
The activated carbon of proportional quantity, CNT and Graphene are added in the distilled water of proportional quantity, with rotating speed be 3500～
The high-speed shearing machine of 4000r/min carries out 5～30min of shearing, and reuse frequency is that the ultrasonic wave of 30～40KHz carries out ultrasound and smashes
5～40min, is prepared into the composite carbon aqueous solution；
The barium sulfate of proportional quantity, humic acid, HT-1 lignins, bismuth sulfate and sodium carboxymethylcellulose are mixed by mechanical lapping,
30～100min of grinding, is prepared into premix；
The lead powder of proportional quantity, premix made by terylene short fiber peacekeeping are added in paste mixing machine carries out 3～10min of mixing, will
The composite carbon aqueous solution for preparing is added in paste mixing machine in 1～2min and continues to stir 3～10min, slow uniformly
The dilute sulfuric acid of proportional quantity is added in paste mixing machine, total addition time control of the composite carbon aqueous solution and dilute sulfuric acid 10～
25min, the maximum temperature during control and cream is less than 65 DEG C, continues to stir 5～12min, and cream terminates that lead plaster is obtained（Negative pole
Active material）, test lead plaster apparent gravity is 4.3～4.6g/cm3.
The preparation process of lead carbon electrokinetic cell negative plate is：By 350～370g negative electrode active materials（Lead plaster）By double
Face coating machine is uniformly applied on lead calcium sheet tin grid（The mass percentage content of tin is 0.15～0.35% in lead calcium sheet tin grid,
The mass percentage content of calcium is 0.09～0.14%）, through intermediate temperature setting, remove false lug, frame polishing is fabricated to finished product
Lead Carbon anode plate.
It is an advantage of the invention that：Using activated carbon+sandwich construction Graphene+carbon nano tube composite carbon cellulosic material, using work
Property charcoal itself have micropore characteristic, Graphene and carbon nanotube adsorption are formed into a kind of new composite carbon material in micropore
Material, the specific surface area of the composite carbon element material is much larger than the specific surface area of activated carbon itself.And carbon materials is passed through into Physical
It is distributed in distilled water and is fabricated to the composite carbon aqueous solution, the lead plaster that carbon materials can be uniformly added using this kind of mode
In, while avoiding the caused loss problem because carbon materials kicks the beam.The addition of new composite carbon element material further increases
The big specific surface area of negative electrode active material, makes battery have more preferable capacitance characteristic, strengthens the transient large current discharge of battery
Performance and the effectively problem of suppression negative pole sulfation.Adding bismuth sulfate in cathode formula simultaneously can effectively reduce the analysis of battery
Hydrogen potential, suppresses the dehydration of battery, extends battery.Add HT-1 lignins and humic acid in cathode formula, effectively
The contraction of active material when suppressing battery to discharge under cryogenic, improves the cryogenic property and charge acceptance of battery.
Specific embodiment
Embodiment 1
A kind of lead carbon electrokinetic cell composite carbon negative electrode active material, its percentage is composed of the following components：Sulphur
Sour barium 0.7%, polyester staple fiber 0.08%, humic acid 0.2%, HT-1 types lignin 0.6%, activated carbon 0.5%, sandwich construction Graphene
0.1%th, CNT 2%, bismuth sulfate 0.5%, sodium carboxymethylcellulose 0.5%, distilled water 13.82%, concentration are that 1.400g/ml is dilute
Sulfuric acid 8%, lead powder 73%.
Embodiment 2
A kind of lead carbon electrokinetic cell composite carbon negative electrode active material, its percentage is composed of the following components：Sulphur
Sour barium 1.5%, polyester staple fiber 0.2%, humic acid 0.5%, HT-1 types lignin 0.2%, activated carbon 3%, sandwich construction Graphene 2%,
CNT 0.1%, bismuth sulfate 0.1%, sodium carboxymethylcellulose 0.2%, distilled water 10%, concentration be 1.400g/ml dilute sulfuric acids 9%,
Lead powder 73.2%.
Embodiment 3
A kind of lead carbon electrokinetic cell composite carbon negative electrode active material, its percentage is composed of the following components：Sulphur
Sour barium 1%, polyester staple fiber 0.1%, humic acid 0.3%, HT-1 types lignin 0.4%, activated carbon 1.5%, sandwich construction Graphene 1%,
CNT 1%, bismuth sulfate 0.3%, sodium carboxymethylcellulose 0.4%, distilled water 10%, concentration are 1.400g/ml dilute sulfuric acids 8%, lead
Powder 76%.
Embodiment 4
A kind of lead carbon electrokinetic cell composite carbon negative electrode active material, its percentage is composed of the following components：Sulphur
Sour barium 0.7%, polyester staple fiber 0.08%, humic acid 0.2%, HT-1 types lignin 0.2%, activated carbon 0.5%, sandwich construction Graphene
0.1%th, CNT 0.1%, bismuth sulfate 0.1%, sodium carboxymethylcellulose 0.2%, distilled water 15%, concentration are the dilute sulphur of 1.400g/ml
Acid 8%, lead powder 74.82%.
Embodiment 5
A kind of lead carbon electrokinetic cell composite carbon negative electrode active material, its percentage is composed of the following components：Sulphur
Sour barium 1%, polyester staple fiber 0.1%, humic acid 0.3%, HT-1 types lignin 0.4%, activated carbon 3%, bismuth sulfate 0.3%, carboxymethyl are fine
The plain sodium 0.4% of dimension, distilled water 10%, concentration are 1.400g/ml dilute sulfuric acids 9.5%, lead powder 76%.
Embodiment 6
A kind of lead carbon electrokinetic cell composite carbon negative electrode active material, its percentage is composed of the following components：Sulphur
Sour barium 1%, polyester staple fiber 0.1%, humic acid 0.3%, HT-1 types lignin 0.4%, activated carbon 1.5%, sandwich construction Graphene 1%,
Bismuth sulfate 0.3%, sodium carboxymethylcellulose 0.4%, distilled water 10%, concentration are 1.400g/ml dilute sulfuric acids 8%, lead powder 77%.
Embodiment 7
A kind of lead carbon electrokinetic cell composite carbon negative electrode active material, its percentage is composed of the following components：Sulphur
Sour barium 1%, polyester staple fiber 0.1%, humic acid 0.3%, HT-1 types lignin 0.4%, activated carbon 1.5%, CNT 1%, bismuth sulfate
0.3%th, sodium carboxymethylcellulose 0.4%, distilled water 10%, concentration are 1.400g/ml dilute sulfuric acids 8%, lead powder 77%.
Embodiment 8
Respectively lead plaster is prepared according to each component content in embodiment 1-7, is comprised the following steps that：
By the activated carbon of formula ratio, CNT, Graphene（Without component by " 0 " calculate）It is added to the distilled water of formula ratio
In, shearing 5-30min is carried out with the high-speed shearing machine that rotating speed is 3500-4000r/min, reuse frequency is the ultrasound of 30-40KHz
Ripple carries out ultrasound and smashes 5-40min, is prepared into the carbon aqueous solution.
The barium sulfate of formula ratio, humic acid, HT-1 lignins, bismuth sulfate, sodium carboxymethylcellulose are mixed by mechanical lapping
Close, grind 30-100min, be prepared into premix.
The lead powder of formula ratio, polyester staple fiber, premix are added in paste mixing machine carries out mixing 3-10min, by carbon
The aqueous solution is added in paste mixing machine in 1-2min and continues to stir 3-10min, slow uniform by the 1.400g/ml's of formula ratio
Dilute sulfuric acid is added in paste mixing machine, and maximum temperature of total addition time control during 10-25min, control and cream is less than 65
DEG C, continue to stir 5-12min, and cream terminates that lead plaster is obtained.
7 groups of lead plasters are obtained, for the ease of distinguishing, this 7 groups of lead plasters are numbered respectively, correspondence embodiment 1-7, by embodiment
1-7 gained lead plaster number consecutivelies are 1#, 2#, 3#, 4#, 5#, 6#, 7#.
Here is noted that each condition all same in the preparation process of this 7 groups of lead plasters.
Make lead Carbon anode plate respectively using this 7 groups of lead plasters, i.e., it is respectively that 360g lead plasters is uniform by dual-side coating machine
It is applied to lead calcium sheet tin grid（The mass percentage content of tin is 0.15～0.35% in lead calcium sheet tin grid, and the mass percent of calcium contains
Measure as 0.09～0.14%）On through intermediate temperature setting, remove false lug, frame polishing, making obtain 7 groups of lead Carbon anode plates.
7 groups of lead Carbon anode plates are fabricated into finished product 3-EVF-200 lead carbon batteries according to battery production technology is internalized into, according to
National standard carries out test and obtains following correction data：
Contrasted by test performance, using the lead carbon battery produced of negative electrode active material of the present invention have low temperature performance well,
Charge acceptance is strong, and large current density electrical characteristics are excellent, the characteristics of deeper cavity life-span length.
Claims (6)
1. a kind of lead carbon electrokinetic cell composite carbon negative electrode active material, it is characterised in that：Percentage, by following
Component is constituted：
Barium sulfate 0.7～1.5%,
Polyester staple fiber 0.08～0.2%,
Humic acid 0.2～0.5%,
HT-1 types lignin 0.2～0.6%,
Activated carbon 0.5～3%,
Graphene 0.1～2%,
CNT 0.1～2%,
Bismuth sulfate 0.1～0.5%,
Sodium carboxymethylcellulose 0.2～0.5%,
Distilled water 10～15%,
Dilute sulfuric acid 8～10%,
Lead powder 73～79%.
2. a kind of lead carbon electrokinetic cell composite carbon negative electrode active material according to claim 1, it is characterised in that：Institute
The concentration for stating dilute sulfuric acid is 1.400g/ml.
3. a kind of lead carbon electrokinetic cell composite carbon negative electrode active material according to claim 1, it is characterised in that：Institute
It is sandwich construction Graphene to state Graphene, and the number of plies is less than 10.
4. a kind of lead carbon electrokinetic cell composite carbon negative electrode active material according to claim 1, it is characterised in that：System
It is for step：
The activated carbon of proportional quantity, CNT and Graphene are added in the distilled water of proportional quantity, with rotating speed be 3500～
The high-speed shearing machine of 4000r/min carries out 5～30min of shearing, and reuse frequency is that the ultrasonic wave of 30～40KHz carries out ultrasound and smashes
5～40min, is prepared into the composite carbon aqueous solution；
The barium sulfate of proportional quantity, humic acid, HT-1 lignins, bismuth sulfate and sodium carboxymethylcellulose are mixed by mechanical lapping,
30～100min of grinding, is prepared into premix；
The lead powder of proportional quantity, premix made by terylene short fiber peacekeeping are added in paste mixing machine carries out 3～10min of mixing, will
The composite carbon aqueous solution for preparing is added in paste mixing machine in 1～2min and continues to stir 3～10min, slow uniformly
The dilute sulfuric acid of proportional quantity is added in paste mixing machine, total addition time control of the composite carbon aqueous solution and dilute sulfuric acid 10～
25min, controls to be less than 65 DEG C with the maximum temperature during cream, continues to stir 5～12min, and cream terminates prepared lead plaster and is
Negative electrode active material, test lead plaster apparent gravity is 4.3～4.6g/cm3.
5. a kind of lead carbon electrokinetic cell composite carbon negative electrode active material according to claim 1 or 4, its feature exists
In：With its make lead carbon electrokinetic cell negative plate the step of be：350～370g negative electrode active materials are passed through into dual-side coating machine
Uniformly it is applied on lead calcium sheet tin grid, through intermediate temperature setting, removes false lug, frame polishing is fabricated to finished product lead Carbon anode
Plate.
6. a kind of lead carbon electrokinetic cell composite carbon negative electrode active material according to claim 5, it is characterised in that：Institute
The mass percentage content for stating tin in lead calcium sheet tin grid is 0.15～0.35%, the mass percentage content of calcium is 0.09～
0.14%。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108682851A (en) * | 2018-06-06 | 2018-10-19 | 超威电源有限公司 | A kind of energy storage diachylon of negative electrode of lead carbon battery and preparation method thereof |
| WO2019068186A1 (en) * | 2017-10-02 | 2019-04-11 | Cwze Power Inc. | Method of preparing carbon-graphene-lead composite particles |
| CN110364737A (en) * | 2019-07-22 | 2019-10-22 | 雅迪科技集团有限公司 | A kind of graphene composite conductive slurry and its preparation method and application |
| CN110635136A (en) * | 2019-09-21 | 2019-12-31 | 泉州市凯鹰电源电器有限公司 | Carbon gelatinized lignin for lead storage battery and preparation method thereof |
| CN111082049A (en) * | 2019-12-16 | 2020-04-28 | 浙江绿源电动车有限公司 | Graphene lead-carbon battery cathode lead paste plate and preparation method thereof |
| CN111293310A (en) * | 2019-12-30 | 2020-06-16 | 安徽力普拉斯电源技术有限公司 | Preparation method of lead-carbon energy storage battery |
| CN114005966A (en) * | 2021-09-14 | 2022-02-01 | 江苏海宝电池科技有限公司 | Formula slurry of negative active material of lead-carbon battery and preparation method and application thereof |
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