CN106450212A - Method for preparing lead-carbon battery cathode composite material - Google Patents
Method for preparing lead-carbon battery cathode composite material Download PDFInfo
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- CN106450212A CN106450212A CN201610969195.XA CN201610969195A CN106450212A CN 106450212 A CN106450212 A CN 106450212A CN 201610969195 A CN201610969195 A CN 201610969195A CN 106450212 A CN106450212 A CN 106450212A
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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
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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
-
- 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
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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
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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)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method of an in-situ-synthesized carbon material which can be used as a lead-carbon battery cathode composite material. The raw materials comprise chitosan, conductive agent acetylene black, binder PTFR emulsion, expanding agent barium sulfate, hydrogen evolution inhibitor indium oxide and gallium oxide, anode active material lead oxide, lead powder and the like. Through the method of in-situ synthesis, the lead-carbon battery cathode composite material is prepared. The adoption of the in-situ-synthesized carbon material effectively improves compatibility of the carbon material and an active material interface, constructs an ideal conductive network, improves use ratio of the an active material and high dispersibility of the biomass carbon material, and inhibits generation of irreversible PbSO4.
Description
Technical field
The present invention relates to a kind of method for preparing lead carbon battery anode material.
Background technology
The non-renewable natural calculus-dissolving energy is used as power source, automobile has become as causes city haze and air dirt
The one of the main reasons of dye.Greatly developing new-energy automobile such as electric automobile becomes the optimal path for solving this problem.Lead carbon
Battery has the high-energy of lead-acid accumulator as a kind of novel battery for growing up on the basis of lead-acid accumulator, lead carbon battery
Density and the high power density of ultracapacitor, equivalent to both mixture, can be widely applied to need fast energy to reclaim,
The field that the conventional batteries such as long-term charge less electricity cannot be applied.Meanwhile, lead carbon battery production technology is non-with the making of existing lead-acid battery
Very close to industrialization is relatively easy to, perfect further with technology, becomes the features such as lead carbon battery is with its higher cost performance
One of power source (battery) of hybrid vehicle first-selection, lead carbon battery will be played a significant role in power and energy storage field.But
There is following point in lead carbon battery negative material, still annoying the development of lead carbon battery：In most cases, people be by carbon
The main active substances such as additive such as lead oxide powder, liberation of hydrogen inhibitor, binding agent in material and negative material is a certain amount of molten
Carry out mechanical mixture in agent (water and sulphuric acid), lead plaster is obtained, is then coated with metal grid, cured, dry, be melted into
To negative plate.But such a preparation process, in lead plaster mixture system, between active substance and Carbon Materials there is one kind in interface
Incompatibility, this incompatibility can increase interface ohmic resistance, so as to cause to be transported under (HRPSoC) working condition for a long time
During row, the battery operated electric conductivity for being possible to interruption, finally affecting negative electrode active material (NAM).Charcoal has flourishing
Pore structure, high specific surface area and abundant surface functional group.This patent is proposed in active substance, with biomass as carbon
Source, by fabricated in situ Carbon Materials, adds it in lead plaster, improves the compatibility at interface therebetween, using well dispersed
Carbon Materials, construct a preferable conductive network, improve the utilization rate of active substance, suppress irreversible PbSO4Generation.
Shitosan (CS) is unique a large amount of a kind of alkaline polysaccharides for existing in nature, belongs to the deacetylated product of chitin N-
Thing, has a wide range of applications field as natural macromolecular material shitosan.Iwona seminar is miscellaneous in Hydrogen Energy
The absorbent charcoal material for having made high porosity using the method for activation of potassium hydroxide with shitosan as raw material is reported in will.This is special
Profit is raw material using shitosan, conductive agent, binding agent, extender, liberation of hydrogen inhibitor etc., using the method for fabricated in situ, prepares
Fabricated in situ shitosan Carbon Materials are gone out, and have been applied in lead carbon battery.
Content of the invention
It is an object of the invention to provide a kind of method for preparing lead carbon battery anode material.
Concretely comprise the following steps：
1st, a kind of method for preparing lead carbon battery anode material, it is characterised in that concretely comprise the following steps：
(1) 2 grams of shitosans are weighed, is that 2% acetum impregnates 1 hour with concentration, then takes out as 85 DEG C in baking oven
Dry 5 hours, clayed into power after taking out cooling again.
(2) mass ratio in PbO and PbO and shitosan sum is that 76% ratio weighs PbO, step and processed in (1)
Shitosan, be fully ground mix homogeneously, prepare sample, be put into crucible, insert in Muffle furnace, heat under nitrogen protection, rise
5 DEG C/min of warm speed is heated to 800 DEG C, is incubated 2 hours, naturally cools to room temperature, that is, obtain chitosan in situ synthesis Carbon Materials.
(3) the chitosan in situ synthesis Carbon Materials for obtaining in step (2) are mixed with negative electrode active material, negative electrode active material
Matter is by 50 grams of Hydrocerussitum (Ceruse), 10 grams of PbO, 10 grams of extender BaSO4, 0.5 gram of conductive agent acetylene black, liberation of hydrogen inhibitor Indium sesquioxide. and oxidation
The each 0.5 gram of composition of gallium, adds 20mL ptfe emulsion and 10mL secondary water after mixing, mechanical agitation extremely generates cream in 12 hours
Shape material, that is, obtain lead carbon battery anode material.
4) lead plaster is coated onto on plate railings of anode and cathode, smears uniformly, then this battery lead plate is put in 50 DEG C of baking oven and dries
12h, then 60 DEG C dry 8h, obtains lead carbon battery positive/negative plate.
The lead carbon battery anode material for preparing as stated above is have rated by electrochemical method, as a result shows electrification
Learn functional.This is because passing through fabricated in situ Carbon Materials, Carbon Materials are effectively improved compatible with reactive species interface
Property, construct preferable conductive network, improve the utilization rate of active substance, the polymolecularity of biomass carbon material, suppression can not
Inverse PbSO4Generation.
Description of the drawings
Fig. 1 is the cyclic voltammetry curve of shitosan anode material in the embodiment of the present invention.
Fig. 2 is the electrochemical alternate impedance spectrum figure of shitosan anode material in the embodiment of the present invention.
Fig. 3 is that in the embodiment of the present invention, shitosan is the first charge-discharge figure of the anode material of carbon source.
Fig. 4 is that in the embodiment of the present invention, shitosan is the cycle life curve of the anode material of carbon source.
Specific embodiment
Embodiment:
Concretely comprise the following steps：
1st, a kind of method for preparing lead carbon battery anode material, it is characterised in that concretely comprise the following steps：
(1) 2 grams of shitosans are weighed, is that 2% acetum impregnates 1 hour with concentration, then takes out as 85 DEG C in baking oven
Dry 5 hours, clayed into power after taking out cooling again.
(2) mass ratio in PbO and PbO and shitosan sum is that 76% ratio weighs PbO, step and processed in (1)
Shitosan, be fully ground mix homogeneously, prepare sample, be put into crucible, insert in Muffle furnace, heat under nitrogen protection, rise
5 DEG C/min of warm speed is heated to 800 DEG C, is incubated 2 hours, naturally cools to room temperature, that is, obtain chitosan in situ synthesis Carbon Materials.
(3) the chitosan in situ synthesis Carbon Materials for obtaining in step (2) are mixed with negative electrode active material, negative electrode active material
Matter is by 50 grams of Hydrocerussitum (Ceruse), 10 grams of PbO, 10 grams of extender BaSO4, 0.5 gram of conductive agent acetylene black, liberation of hydrogen inhibitor Indium sesquioxide. and oxidation
The each 0.5 gram of composition of gallium, adds 20mL ptfe emulsion and 10mL secondary water after mixing, mechanical agitation extremely generates cream in 12 hours
Shape material, that is, obtain lead carbon battery anode material.
4) lead plaster is coated onto on plate railings of anode and cathode, smears uniformly, then this battery lead plate is put in 50 DEG C of baking oven and dries
12h, then 60 DEG C dry 8h, obtains lead carbon battery positive/negative plate.
5) 150mL, 1.28g/cm are added in the beaker of 250mL3Sulphuric acid, positive/negative plate insert beaker both sides, in
Between separated with industrial battery AGM dividing plate, you can obtain simulation lead carbon battery, which is connected with LAND5.8 battery test system, is entered
Row drenches acid, solidification, dry, chemical conversion, obtains qualified plate railings of anode and cathode, can carry out electrochemical property test as follows.
A adopts three-electrode system, using 5) in obtain qualified grid as working electrode, Hg/Hg2SO4As reference electrode,
Platinum electrode is that sulphuric acid is circulated volt-ampere curve test as electrolyte, and sweep limitss are -1.2-0.8V, as a result to see to electrode
Fig. 1.The rectangular area for sweeping speed for the cyclic voltammetry curve under 0.1mV/s is read by Fig. 1, according to than capacitance calculation Cs=A/ (2s ×
Δ V × m), the ratio electric capacity of Carbon Materials can be calculated, so as to sweeping under speed in 0.1mV/s, anode material than electric capacity is
162.9F/g.
B adopts three-electrode system, using 5) in obtain qualified grid as working electrode, Hg/Hg2SO4As reference electrode,
Platinum electrode is that sulphuric acid carries out the test of electrochemical alternate impedance spectrum figure as electrolyte, as a result sees Fig. 2, test temperature to electrode
For room temperature, test parameter is set to 0.01Hz～100000Hz, amplitude be.As shown in Figure 2, shitosan anode material
It is 1.872 that Rs is 0.015892, Rp.
C assemble simulation lead carbon battery, fully charged after, control 750mA under the conditions of, carry out first discharge curve test.Cut
Only voltage be 1.75V, as a result as shown in figure 3, from the figure 3, it may be seen that with shitosan as carbon source anode material assembling battery
Discharge curve have longer discharge platform, termination capacity reaches 108.72mAh/g, this is because the addition of shitosan Carbon Materials
Define the second surface for being mutually enclosed in sulphuric acid leading crystal in media as well, limit growing up for sulphuric acid leading crystal longer so as to have
Discharge platform.
D assemble simulation lead carbon battery, fully charged after, carry out battery cycle life test, as a result see Fig. 4, can by Fig. 4
Know, anode material is different in the percentage ratio for circulating theoretical capacity shared by capacity after 10000 times, and shitosan is carbon source
Anode material when specific capacity account for the 98% of theoretical specific capacity, this is the lead sulfate of negative pole as battery is in discharge and recharge
When being converted into lead, as sulphuric acid leading crystal is less, and a lot of active substance is deposited on the surface of Carbon Materials and causes the work of negative pole
Property material lead keep higher activity.So that shitosan is for having higher specific capacity, and 10000 circles during carbon source after
Almost it is not lost.
Claims (1)
1. a kind of method for preparing lead carbon battery anode material, it is characterised in that concretely comprise the following steps：
(1) 2 grams of shitosans are weighed, is that 2% acetum impregnates 1 hour with concentration, then takes out as 85 DEG C of dryings 5 in baking oven
Hour, clayed into power after taking out cooling again；
(2) mass ratio in PbO and PbO and shitosan sum is that 76% ratio weighs PbO, the shell for processing in step (1)
Polysaccharide, is fully ground mix homogeneously, prepares sample, is put into crucible, inserts in Muffle furnace, heat under nitrogen protection, and heat up speed
5 DEG C/min of rate is heated to 800 DEG C, is incubated 2 hours, naturally cools to room temperature, that is, obtain chitosan in situ synthesis Carbon Materials；
(3) the chitosan in situ synthesis Carbon Materials for obtaining in step (2) are mixed with negative electrode active material, negative electrode active material by
50 grams of Hydrocerussitum (Ceruse), 10 grams of PbO, 10 grams of extender BaSO4, 0.5 gram of conductive agent acetylene black, liberation of hydrogen inhibitor Indium sesquioxide. and gallium oxide each
0.5 gram of composition, adds 20mL ptfe emulsion and 10mL secondary water after mixing, mechanical agitation extremely generates paste in 12 hours
Matter, that is, obtain lead carbon battery anode material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610969195.XA CN106450212A (en) | 2016-11-06 | 2016-11-06 | Method for preparing lead-carbon battery cathode composite material |
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| CN201610969195.XA CN106450212A (en) | 2016-11-06 | 2016-11-06 | Method for preparing lead-carbon battery cathode composite material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108336351A (en) * | 2018-04-03 | 2018-07-27 | 肇庆益晟商贸有限公司 | A kind of high energy lead-acid battery anode material and preparation method thereof |
| CN112340814A (en) * | 2019-08-09 | 2021-02-09 | 宁波方太厨具有限公司 | Electrode plate, electrode plate module, preparation method of electrode plate module and sterilization and desalination treatment method |
| CN114335537A (en) * | 2021-12-23 | 2022-04-12 | 中国科学院福建物质结构研究所 | Polypyrrole-coated conductive carbon black/indium oxide composite material and preparation method and application thereof |
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| US20030235760A1 (en) * | 2002-06-19 | 2003-12-25 | Hitachi, Ltd. | Lead-acid storage battery, carbon material and process of manufacturing the carbon material |
| CN101667637A (en) * | 2009-09-22 | 2010-03-10 | 南京双登科技发展研究院有限公司 | Method for manufacturing negative electrode of lead-carbon super-capacitor battery |
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| CN105024046A (en) * | 2015-07-31 | 2015-11-04 | 湘潭大学 | Preparation method of lead-carbon battery cathode |
| CN105226290A (en) * | 2015-10-22 | 2016-01-06 | 桂林理工大学 | The method of the plumbous carbon battery anode material of a kind of fabricated in situ |
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Patent Citations (5)
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| US20030235760A1 (en) * | 2002-06-19 | 2003-12-25 | Hitachi, Ltd. | Lead-acid storage battery, carbon material and process of manufacturing the carbon material |
| CN101667637A (en) * | 2009-09-22 | 2010-03-10 | 南京双登科技发展研究院有限公司 | Method for manufacturing negative electrode of lead-carbon super-capacitor battery |
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| CN105226290A (en) * | 2015-10-22 | 2016-01-06 | 桂林理工大学 | The method of the plumbous carbon battery anode material of a kind of fabricated in situ |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108336351A (en) * | 2018-04-03 | 2018-07-27 | 肇庆益晟商贸有限公司 | A kind of high energy lead-acid battery anode material and preparation method thereof |
| CN108336351B (en) * | 2018-04-03 | 2020-06-12 | 福建省顺昌县威仕达电源科技有限公司 | Negative electrode material for high-energy lead storage battery and preparation method thereof |
| CN112340814A (en) * | 2019-08-09 | 2021-02-09 | 宁波方太厨具有限公司 | Electrode plate, electrode plate module, preparation method of electrode plate module and sterilization and desalination treatment method |
| CN112340814B (en) * | 2019-08-09 | 2021-11-26 | 宁波方太厨具有限公司 | Electrode plate, electrode plate module, preparation method of electrode plate module and sterilization and desalination treatment method |
| CN114335537A (en) * | 2021-12-23 | 2022-04-12 | 中国科学院福建物质结构研究所 | Polypyrrole-coated conductive carbon black/indium oxide composite material and preparation method and application thereof |
| CN114335537B (en) * | 2021-12-23 | 2023-09-29 | 中国科学院福建物质结构研究所 | Polypyrrole coated conductive carbon black/indium oxide composite material and preparation method and application thereof |
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