CN104993128A - Lead-carbon battery negative electrode and preparation method thereof - Google Patents
Lead-carbon battery negative electrode and preparation method thereof Download PDFInfo
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- CN104993128A CN104993128A CN201510484014.XA CN201510484014A CN104993128A CN 104993128 A CN104993128 A CN 104993128A CN 201510484014 A CN201510484014 A CN 201510484014A CN 104993128 A CN104993128 A CN 104993128A
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- lead
- battery negative
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- carbon battery
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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
- H01M4/14—Electrodes for 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
-
- 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
- H01M4/62—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
Abstract
The invention belongs to the technical field of lead storage batteries, and particularly relates to a lead-carbon battery negative electrode and a preparation method thereof. The lead-carbon battery negative electrode comprises the raw materials including, by weight, 0.2-2% of flocculent carbon materials, 0.1-0.3% of humic acid, 0.05-0.1% of conductive graphite, 0.01-0.05% of indium oxide, 0.1-0.5% of barium sulfate, 0.5-1.5% of a binding agent, 0.5-2.5% of thionyl chloride and the balance lead powder. According to the flocculent carbon materials, highly oriented pyrolytic graphite is used as the positive pole, a lead plate is used as an auxiliary electrode, electrolysis is performed in an electrolyte, the current density ranges from 10 mA/cm<2> to 20 mA/cm<2>, then dispersion is performed, the dispersion speed ranges from 2000 r/min to 3000 r/min, and the time is 2-5 h. The hydrogen evolution potential of a negative plate can be improved, the large-current charging and discharging performance is excellent, the preparation method of the lead-carbon battery negative electrode and the paste mixing technology are simple, and the consistency is good.
Description
Technical field
The invention belongs to lead accumulator technical field, be specifically related to a kind of lead carbon battery negative pole and preparation method thereof.
Background technology
Plumbous charcoal superbattery is the international advanced cutting edge technology of current battery industry, is the breakthrough in battery technology aspect.But at home, because the screening of Carbon Materials, Carbon Materials dispersion and the technical bottleneck such as liberation of hydrogen do not obtain substantive breakthroughs, cause the research and development of this technology and commercialization to be made slow progress.
Carbon Materials is the key component of such technology, and the effective dispersion of Carbon Materials in active material has important impact equally.Due to the kind of Carbon Materials internal functionality and the impact of quantity on battery performance and operating procedure comparatively large, is therefore mostly by modification at present, thus obtains the Carbon Materials of excellent performance and good hydrophilic property.By the pre-dispersed mode of powder or utilize continuously and cream equipment carry out the preparation of active material, complex operation, investment is large, and different processing methods and pre-dispersed effect are larger with expection difference, this all will have a strong impact on battery performance and lot stability, thus delay the commercialization process of this type product.
For this problem, by special item, carry out a large amount of comparative study and test from aspects such as the preparations of active matter formula and required Carbon Materials, finally determined solution.
Summary of the invention
The object of this invention is to provide a kind of lead carbon battery negative pole, can improve the hydrogen-evolution overpotential of negative plate, big current charging-discharging performances is excellent, and the present invention also provides its preparation method, and cream technique is simple, and consistency is good.
A kind of lead carbon battery negative pole of the present invention, comprises the raw material of following percetage by weight:
Cotton-shaped Carbon Materials 0.2 ~ 2%, pyrotomalenic acid 0.1 ~ 0.3%, electrically conductive graphite 0.05 ~ 0.1%, indium oxide 0.01 ~ 0.05%, barium sulfate 0.1 ~ 0.5%, binding agent 0.5 ~ 1.5%, thionyl chloride 0.5 ~ 2.5%, lead powder surplus.
Binding agent is polytetrafluoroethylene, and polytetrafluoroethylene is emulsus.
The preparation method of pyrotomalenic acid is: be dissolved in by humic acid in absolute ethyl alcohol, filters, spread out by filter residue and ventilate under ventilating kitchen after fully stirring, and is then placed in 50 ~ 85 DEG C of baking ovens and dries 1 ~ 3h, then in 105 ~ 125 DEG C of oven dry, be pyrotomalenic acid.
The preparation method of described cotton-shaped Carbon Materials is: using highly oriented pyrolytic graphite plate as positive pole, using stereotype as auxiliary electrode, and electrolysis in containing the electrolyte of sulfate, current density is 10 ~ 20mA/cm
2, then disperse, rate of dispersion is 2000 ~ 3000r/min, time 2 ~ 5h.In electrolytic process, adopt highly oriented pyrolytic graphite plate as positive pole, using stereotype as auxiliary electrode, in the aqueous solution containing sodium sulphate and/or potassium sulfate, carry out electrolysis, conduction time can adjust as required flexibly.
Pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate all cross 20 mesh sieves.
The preparation method of described lead carbon battery negative pole, comprises the following steps:
(1) first lead powder is added in vacuum paste mixing machine, then pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate are added in paste mixing machine, then add polytetrafluoroethylene binding agent and thionyl chloride;
(2) cotton-shaped Carbon Materials and water mixing are disperseed, the solution after dispersion is added in vacuum paste mixing machine, stirs;
(3) again sulfuric acid solution is evenly drenched in paste mixing machine, continue to stir, after shutdown, obtain lotion;
(4) lotion is filled on lead alloy grid, through solidification and drying, obtain lead carbon battery negative pole.
Wherein: in step (1), pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate are added in paste mixing machine and be: pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate are sieved in paste mixing machine with 20.
The weight ratio of lead powder, sulfuric acid and water is 1000:30 ~ 45:100 ~ 150, and wherein the amount of sulfuric acid is in the concentrated sulfuric acid, is evenly to drench diluting concentrated sulfuric acid in paste mixing machine after sulfuric acid solution.
In step (2), mixing time is 10 ~ 15 minutes.
In step (3), mixing time is 5 ~ 10 minutes.
Solidification and drying stage solidification used and drying process are prior art.
As a kind of preferred version, the preparation method of described lead carbon battery negative pole is as follows:
First lead powder is added in vacuum paste mixing machine; then raw material pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate are sieved in paste mixing machine with 20; if there have caking to rub with the hands to be broken after sieve; add emulsus polytetrafluoroethylene binding agent and thionyl chloride again; cotton-shaped Carbon Materials and water mixing are disperseed; solution after dispersion is added in vacuum paste mixing machine; stir 10 ~ 15 minutes; again the sulfuric acid solution of formula ratio was evenly drenched in paste mixing machine with 10 ~ 20min time, shut down after continuing stirring 5 ~ 10min.Fill on lead alloy grid after obtaining lotion, through solidification and drying, obtain lead carbon battery negative pole.
The lead carbon battery negative pole that the present invention prepares carries out acid circulation through assembled battery and is internalized into and prepares battery.
The present invention compared with prior art, has following beneficial effect:
(1) the cotton-shaped Carbon Materials that obtains of the present invention is as cathode additive agent, pre-dispersed without the need to powder, lead carbon battery can be met to technical requirements such as the technical matters of charcoal performance and dispersion, this is mainly because Carbon Materials in this way joins in lotion, the structure that Carbon Materials particle has owing to having hydrophily and particulate, simultaneously due to charcoal particle with electric charge, effectively can penetrate into particle space in lotion inner.
(2) the present invention is uniformly dispersed in active material without the need to the pre-dispersed Carbon Materials that just can make of powder, and the hydrogen-evolution overpotential of negative plate can be improved, use lead carbon battery prepared by this formula, simple with cream technique, consistency is good, and plate strength is large, and big current charging-discharging performances is excellent, do not need additionally to increase equipment and special process simultaneously, traditional lead acid batteries production equipment can be used completely, easily realize the mass production of product.
(3) the present invention waits operation bidirectional without the need to powder is pre-dispersed, is effectively added in active material by the Carbon Materials of excellent electrical property, good hydrophilic property, improves the possibility of this battery batch production, and improve mechanics and the electrical property of lead carbon battery.
Accompanying drawing explanation
Fig. 1 is the Electronic Speculum figure of cotton-shaped Carbon Materials;
Fig. 2 is the Sample Cell that obtains of embodiment 1 and common batteries C
5electric discharge figure;
Fig. 3 be embodiment 2 obtain the different current discharge figure of Sample Cell.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
A kind of lead carbon battery negative pole, formula following (mass fraction): cotton-shaped Carbon Materials 0.2%, pyrotomalenic acid 0.1%, electrically conductive graphite 0.06%, indium oxide 0.015%, barium sulfate 0.2%, polyfluortetraethylene of binding element 0.6%, thionyl chloride 0.5%, lead powder surplus.
Wherein: pyrotomalenic acid is: humic acid is dissolved in absolute ethyl alcohol, filter after fully stirring, filter residue is spread out and ventilates under ventilating kitchen, be then placed in 60 DEG C of baking ovens and dry 2h, then in 110 DEG C of oven dry, be pyrotomalenic acid.The preparation method of cotton-shaped Carbon Materials is: using highly oriented pyrolytic graphite plate as positive pole, using stereotype as auxiliary electrode, and electrolysis in containing the electrolyte of sulfate, current density is 10mA/cm
2, then disperse, rate of dispersion is 3000r/min, time 4h.
Preparation method is as follows: first added by lead powder in vacuum paste mixing machine; then raw material pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate are sieved in paste mixing machine with 20; if there have caking to rub with the hands to be broken after sieve; add emulsus polytetrafluoroethylene binding agent and thionyl chloride again; cotton-shaped Carbon Materials and water mixing are disperseed; solution after dispersion is added in vacuum paste mixing machine; stir 10 minutes; again the sulfuric acid solution 10min time of formula ratio is evenly drenched in paste mixing machine, shut down after continuing to stir 10min.Fill on lead alloy grid after obtaining lotion, through solidification and dry, obtain lead carbon battery negative pole, then carry out acid through assembled battery and circulate to be internalized into and prepare battery, wherein: the weight ratio of lead powder, sulfuric acid and water is 1000:30:100, and wherein the amount of sulfuric acid is in the concentrated sulfuric acid.
Battery performance detection is carried out to above-mentioned battery, reduces 0.2m Ω with the static internal resistance of battery of the same type, and carry out C
5electric discharge, concrete condition is shown in Fig. 2.
Embodiment 2
A kind of lead carbon battery negative pole, formula following (mass fraction): wherein cotton-shaped Carbon Materials 2%, pyrotomalenic acid 0.2%, electrically conductive graphite 0.065%, indium oxide 0.01%, barium sulfate 0.25%, polyfluortetraethylene of binding element 0.6%, thionyl chloride 1.5%, lead powder surplus.
Wherein: the preparation method of pyrotomalenic acid is: be dissolved in by humic acid in absolute ethyl alcohol, filter after fully stirring, filter residue is spread out and ventilates under ventilating kitchen, be then placed in 85 DEG C of baking ovens and dry 1h, then in 125 DEG C of oven dry, be pyrotomalenic acid.The preparation method of cotton-shaped Carbon Materials is: using highly oriented pyrolytic graphite plate as positive pole, using stereotype as auxiliary electrode, and electrolysis in containing the electrolyte of sulfate, current density is 20mA/cm
2, then disperse, rate of dispersion is 2000r/min, time 3h.
Preparation method is as follows: first added by lead powder in vacuum paste mixing machine; then raw material pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate are sieved in paste mixing machine with 20; if there have caking to rub with the hands to be broken after sieve; add emulsus polytetrafluoroethylene binding agent and thionyl chloride again; cotton-shaped Carbon Materials and water mixing are disperseed; solution after dispersion is added in vacuum paste mixing machine; stir 15 minutes; again the sulfuric acid solution 20min time of formula ratio is evenly drenched in paste mixing machine, shut down after continuing to stir 5min.Fill on lead alloy grid after obtaining lotion, through solidification and dry, obtain lead carbon battery negative pole, then carry out acid through assembled battery and circulate to be internalized into and prepare battery, wherein: the weight ratio of lead powder, sulfuric acid and water is 1000:45:150, and wherein the amount of sulfuric acid is in the concentrated sulfuric acid.
Carry out battery performance detection to above-mentioned battery, reduce 0.4m Ω with the static internal resistance of battery of the same type, and carry out electric discharge and the charge test of different multiplying to Sample Cell, discharge scenario is shown in Fig. 3, and charge condition is in table 1.
The charge condition of table 1 embodiment 2 battery different multiplying
In table 1 data be embodiment 2 battery with different current charges to electricity during 2.4V, time and the percentage accounting for rated capacity.Can find the increase along with charging current, the charge efficiency of battery declines gradually.When with 2C current charges, the electricity higher than 80% can be charged within half an hour; When with 4C current charges, 60% electricity can be filled with in 10 minutes.This mainly because the existence of cotton-shaped Carbon Materials strengthens the conductivity between lead sulfate crystal, and reduces the current potential of hydrogen precipitation, improves pole plate charge acceptance.
Claims (10)
1. a lead carbon battery negative pole, is characterized in that: the raw material comprising following percetage by weight:
Cotton-shaped Carbon Materials 0.2 ~ 2%, pyrotomalenic acid 0.1 ~ 0.3%, electrically conductive graphite 0.05 ~ 0.1%, indium oxide 0.01 ~ 0.05%, barium sulfate 0.1 ~ 0.5%, binding agent 0.5 ~ 1.5%, thionyl chloride 0.5 ~ 2.5%, lead powder surplus.
2. lead carbon battery negative pole according to claim 1, is characterized in that: binding agent is polytetrafluoroethylene.
3. lead carbon battery negative pole according to claim 1, it is characterized in that: the preparation method of pyrotomalenic acid is: be dissolved in by humic acid in absolute ethyl alcohol, filter after abundant stirring, filter residue is spread out and ventilates under ventilating kitchen, then be placed in 50 ~ 85 DEG C of baking ovens and dry 1 ~ 3h, again in 105 ~ 125 DEG C of oven dry, be pyrotomalenic acid.
4. lead carbon battery negative pole according to claim 1, is characterized in that: the preparation method of cotton-shaped Carbon Materials is: using highly oriented pyrolytic graphite plate as positive pole, using stereotype as auxiliary electrode, electrolysis in the electrolytic solution, and current density is 10 ~ 20mA/cm
2, then disperse, rate of dispersion is 2000 ~ 3000r/min, time 2 ~ 5h.
5. lead carbon battery negative pole according to claim 1, is characterized in that: pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate all cross 20 mesh sieves.
6. a preparation method for the arbitrary described lead carbon battery negative pole of claim 1-5, is characterized in that: comprise the following steps:
(1) first lead powder is added in vacuum paste mixing machine, then pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate are added in paste mixing machine, then add polytetrafluoroethylene binding agent and thionyl chloride;
(2) cotton-shaped Carbon Materials and water mixing are disperseed, the solution after dispersion is added in vacuum paste mixing machine, stirs;
(3) again sulfuric acid solution is evenly drenched in paste mixing machine, continue to stir, after shutdown, obtain lotion;
(4) lotion is filled on lead alloy grid, through solidification and drying, obtain lead carbon battery negative pole.
7. the preparation method of lead carbon battery negative pole according to claim 6, is characterized in that: pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate are added in paste mixing machine in step (1) and be: pyrotomalenic acid, electrically conductive graphite, indium oxide and barium sulfate are sieved in paste mixing machine with 20.
8. the preparation method of lead carbon battery negative pole according to claim 6, is characterized in that: the weight ratio of lead powder, sulfuric acid and water is 1000:30 ~ 45:100 ~ 150, and wherein the amount of sulfuric acid is in the concentrated sulfuric acid.
9. the preparation method of lead carbon battery negative pole according to claim 6, is characterized in that: in step (2), mixing time is 10 ~ 15 minutes.
10. the preparation method of lead carbon battery negative pole according to claim 6, is characterized in that: in step (3), mixing time is 5 ~ 10 minutes.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114068915A (en) * | 2021-11-04 | 2022-02-18 | 惠州锂威新能源科技有限公司 | Preparation method and application of positive electrode slurry |
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