CN103618089A - Modified activated carbon as well as preparation method thereof and method for manufacturing carbon negative plate of super lead-acid battery by using modified activated carbon - Google Patents
Modified activated carbon as well as preparation method thereof and method for manufacturing carbon negative plate of super lead-acid battery by using modified activated carbon Download PDFInfo
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- CN103618089A CN103618089A CN201310686364.5A CN201310686364A CN103618089A CN 103618089 A CN103618089 A CN 103618089A CN 201310686364 A CN201310686364 A CN 201310686364A CN 103618089 A CN103618089 A CN 103618089A
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
-
- 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
-
- 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 relates to modified activated carbon as well as a preparation method thereof and a method for manufacturing a carbon negative plate of a super lead-acid battery by using the modified activated carbon. The modified activated carbon is formed by processing a modifier and activated carbon, wherein the modifier is one or more combinations of Pb, BaSO4 and ZnO or one or more combinations of Pb(NO3)2, Ba(CH3COO)2 and Bi(NO3)3. The method for preparing the modified activated carbon comprises a mechanical mixing method and a chemical depositing method; the method for manufacturing the carbon negative plate of the super lead-acid battery comprises the following steps: preparing the modified activated carbon into negative carbon cream; coating the negative carbon cream on an aluminum alloy board gate, and drying so as to obtain the carbon negative plate. The modified activated carbon disclosed by the invention has the advantages that hydrogen evolution velocity of the modified activated carbon is lowered, specific capacitance of the modified activated carbon is increased, problems that working electric potentials of a carbon electrode and a lead electrode in the super lead-acid battery are not matched and hydrogen evolution is severe at a charging later stage are solved, and service life of the super lead-acid battery is prolonged; the used materials and the battery operation are beneficial to environmental protection.
Description
Technical field
The present invention relates to modified activated carbon and preparation method thereof and for making the method for lead-acid ultra-battery charcoal negative plate, belong to lead-acid battery technical field.
Background technology
Lead-acid battery is the most ripe battery of technology in all chemical power sources, it has, and cheap, safe, heavy-current discharge performance is good, battery recycling rate advantages of higher, and oneself is widely used in the fields such as traction battery of electric bicycle, battery-operated motor cycle, the communications industry, power industry back-up source, beeliner.Yet lead-acid battery is because the shortcomings such as specific energy low (35-40Wh/kg), volume is large, useful life is short (300-800 times), quick charge difficulty have limited its application greatly.Many lead-acid battery new technologies had been developed in recent years, as corrosion-resistant lead alloy anode plate grid, Lead Foam grid, Carbon foam grid, novel cathode additive agent, superbattery etc.Wherein, superbattery is one of technology at present of greatest concern.
Superbattery, is also lead-acid ultra-battery, is a kind of hybrid novel energy-storing power supply, by Asymmetric Supercapacitor and lead-acid battery, is combined, and has the feature of electric capacity and the difunctional energy storage of battery concurrently.It has realized electric double layer energy storage and these two kinds of energy storage mode loong shunts evolution of electrochemical reaction energy storage are the great-leap-forward development of interior parallel connection.The positive plate of lead-acid battery just very, two property negative plates that the carbon resistance rod that negative pole is ultracapacitor and the lead electrode of lead-acid battery combine.When keeping electrokinetic cell high-energy-density, and do not increase in the situation of complicated circuit, also there is high power density, high current charge-discharge, the overlength cycle life characteristics of ultracapacitor.Superbattery is acknowledged as the outstanding representative of " advanced battery of future generation ", and it is leading the technological development direction of lead-acid battery.
Yet the operation interval of carbon electrode of super capacitor and lead-acid battery lead electrode does not mate.If simply by two electrode parallel connections, when electric discharge, electrode current mainly comes from the plumbous negative pole of lead-acid battery, and capacitor carbon resistance rod does not provide electric current substantially; And when charging, the plumbous negative pole of lead-acid battery does not provide electric current substantially, electrode current mainly comes from capacitor carbon resistance rod.In addition, charging latter stage, capacitor carbon resistance rod produces a large amount of hydrogen, causes electrolyte dry-out, greatly reduces the cycle life of battery.Therefore, must carry out modification to absorbent charcoal material, make it possess the operation interval similar to plumbous negative pole and very low liberation of hydrogen speed.
Summary of the invention
The object of the invention is, provide a kind of modified activated carbon and preparation method thereof and for making the method for lead-acid ultra-battery charcoal negative plate.By absorbent charcoal material is carried out to modification, the activated carbon electrodes liberation of hydrogen speed after modification is obviously reduced, and its operation interval and lead electrode match, extended the cycle life of lead-acid battery.And manufacturing process is simple, cost is low, material therefor and battery operation are conducive to environmental protection.
Technical scheme of the present invention is:
A kind of modified activated carbon of the present invention, comprises active carbon and trim; It is trim to be incorporated into mixing, attrition process in activated carbon powder form; Described trim comprises Pb, BaSO
4and ZnO, be one or more combinations wherein.
The compounding method of described modified activated carbon, step is mainly: first take in proportion active carbon and trim, then described active carbon and trim are dropped in ball mill, using ethanol as ball-milling medium mixing, attrition process, finally the material processing is placed in to baking oven dry, makes modified activated carbon.
A kind of modified activated carbon of the present invention, comprises active carbon and trim; It is active carbon is immersed in trim salting liquid stir, vibration processes; Described trim comprises Pb (NO
3)
2, Ba (CH
3cOO)
2and Bi(NO
3)
3, be one or more combinations wherein.
The preparation method of described modified activated carbon, step is mainly: first take in proportion active carbon and trim, then described trim is mixed with to trim salting liquid, again active carbon is immersed in trim salting liquid with magnetic agitation, sonic oscillation, filtering and washing again, after this, then by filter cake be dispersed in excessive precipitant solution with magnetic agitation, sonic oscillation; Filtering and washing to filtrate Ph value is pH6～8 again, finally the material processing is placed in to baking oven dry, makes modified activated carbon.
The preparation method of described modified activated carbon, is characterized in that, precipitant solution is H
2sO
4, or KOH.
Described modified activated carbon, the mass ratio of its trim and active carbon is 0.01～0.3: 1.
The method that use modified activated carbon of the present invention is made lead-acid ultra-battery charcoal negative plate, its charcoal negative plate comprises that lead alloy grid and Tu negative pole carbon paste thereon forms through solidifying last oven dry; The constituent of described negative plate carbon paste comprises: modified activated carbon, acetylene black, sodium cellulose glycolate (CMC) and butadiene-styrene rubber (SBR); Making step is mainly: first take in proportion modified activated carbon, acetylene black, CMC and SBR, then mix form slurry, and regulate the viscosity of slurry, again the slurry mixing is coated on lead alloy grid, finally be placed in baking oven vacuumize, become lead-acid ultra-battery charcoal negative plate.
The method that described use modified activated carbon of the present invention is made lead-acid ultra-battery charcoal negative plate, the constituent content ratio of its negative plate carbon paste is by negative plate carbon paste weighing scale: modified activated carbon is 75～85%, acetylene black is that 6～12%, CMC is that 2～3%, SBR is 6～8%.
The method that described use modified activated carbon of the present invention is made lead-acid ultra-battery charcoal negative plate, it regulates the viscosity of slurry is 3.5～5.5g/cm
3.
The method that described use modified activated carbon of the present invention is made lead-acid ultra-battery charcoal negative plate, the thickness that the slurry mixing is coated on lead alloy grid is 1.2～3mm.
The technology of the present invention effect is remarkable: compared with prior art, the present invention, by active carbon is carried out to modification, can improve the ratio electric capacity of active carbon greatly, obviously reduces the liberation of hydrogen speed of active carbon.In effective solution lead-acid ultra-battery, due to carbon resistance rod and the inconsistent serious problem of carbon resistance rod liberation of hydrogen in latter stage that causes charging of lead electrode operating potential, improved the charge efficiency of lead-acid ultra-battery, the cycle life that has extended lead-acid ultra-battery.The preparation method of this modified activated carbon is simple, is easy to large-scale production.
Accompanying drawing explanation
Accompanying drawing 1 is the cyclic voltammetry curve figure of the invention process example 7.The cyclic voltammetry curve figure that in figure, "-" solid line is unmodified active carbon; The cyclic voltammetry curve figure that "-----" dotted line is modified activated carbon.
Accompanying drawing 2 is liberation of hydrogen rate profile of the invention process example 9.In figure, " mouth " square frame is labeled as the liberation of hydrogen rate profile of unmodified active carbon; "
" the triangular marker liberation of hydrogen rate profile that is modified activated carbon.
Embodiment
It is as follows that the invention will be further described in conjunction with the accompanying drawings and embodiments:
embodiment 1:a basic embodiment of modified activated carbon of the present invention.This modified activated carbon comprises active carbon and trim; It is trim to be incorporated into mixing, attrition process in activated carbon powder form; Described trim comprises Pb, BaSO
4and ZnO, be one or more combinations wherein.
embodiment 2:the compounding method embodiment of embodiment 1 modified activated carbon.The method step is mainly: first take in proportion active carbon and trim, then described active carbon and trim are dropped in ball mill, using ethanol as ball-milling medium mixing, attrition process, finally the material processing is placed in to baking oven dry, make modified activated carbon.The mass ratio of described trim and active carbon is 0.01～0.3: 1.
embodiment 3:another basic embodiment of modified activated carbon of the present invention.This modified activated carbon comprises active carbon and trim; It is active carbon is immersed in trim salting liquid stir, vibration processes; Described trim comprises Pb (NO
3)
2, Ba (CH
3cOO)
2and Bi(NO
3)
3, be one or more combinations wherein.
embodiment 4:the compounding method embodiment of embodiment 3 modified activated carbons.The method step is mainly: first take in proportion active carbon and trim, then described trim is mixed with to trim salting liquid, again active carbon is immersed in trim salting liquid with magnetic agitation, sonic oscillation, filtering and washing again, after this, then by filter cake be dispersed in excessive precipitant solution with magnetic agitation, sonic oscillation; Filtering and washing to filtrate Ph value is pH6～8 again, finally the material processing is placed in to baking oven dry, makes modified activated carbon.The mass ratio of trim and active carbon is 0.01～0.3: 1.Described precipitant solution is H
2sO
4, or KOH.
embodiment 5:the basic embodiment of method that a kind of use modified activated carbon of the present invention is made lead-acid ultra-battery charcoal negative plate.This charcoal negative plate comprises that lead alloy grid and Tu negative pole carbon paste thereon forms through solidifying last oven dry; The constituent of described negative plate carbon paste comprises: modified activated carbon, acetylene black, sodium cellulose glycolate (CMC) and butadiene-styrene rubber (SBR); Making step is mainly: first take in proportion modified activated carbon, acetylene black, CMC and SBR, then mix form slurry, and regulate the viscosity of slurry, again the slurry mixing is coated on lead alloy grid, finally be placed in baking oven vacuumize, become lead-acid ultra-battery charcoal negative plate.
embodiment 6:the further embodiment of embodiment 5.As different from Example 5: the constituent content ratio of negative plate carbon paste is by negative plate carbon paste weighing scale: modified activated carbon is 75～85%, and acetylene black is that 6～12%, CMC is that 2～3%, SBR is 6～8%.Regulating the viscosity of slurry is 3.5～5.5g/cm
3.The thickness that the slurry mixing is coated on lead alloy grid is 1.2～3mm.
Below 4 further comprehensive embodiment:
embodiment 7:10wt.% lead powder, 90wt.% active carbon are mixed, add appropriate ethanol as dispersant, mechanical mixture in ball mill, drum's speed of rotation is 300r/min, stirs 7 hours.Then, mixture is placed in to 120 ℃ of true drying boxes, more than dry 10h.Make the modified activated carbon of doping Pb powder.
The modified activated carbon, the 10 wt.% acetylene blacks that take 80 wt.% doping Pb powder are evenly mixed, and 2.5 wt.% CMC, 7.5 wt.% SBR are added in mixture, add appropriate ethanol and deionized water to regulate the viscosity of mixture simultaneously.Carry out mechanical mixture, rotating speed is 600r/min, stirs 3 hours.Then by the slurry dual coating mixing on latticed lead alloy grid, be placed in 80
oin C baking oven, vacuumize is more than 10 hours, the charcoal negative plate for lead-acid ultra-battery that obtains being made by modified activated carbon.
embodiment 8:8wt.%ZnO, 92wt.% active carbon are mixed, add appropriate ethanol as dispersant, mechanical mixture in ball mill, drum's speed of rotation is 300r/min, stirs 7 hours.Then, mixture is placed in to 120 ℃ of true drying boxes, more than dry 10h.Make the modified activated carbon of doping ZnO.
The modified activated carbon, the 10 wt.% acetylene blacks that take 80 wt.% doping ZnOs are evenly mixed, and 2.5 wt.% CMC, 7.5 wt.% SBR are added in mixture, add appropriate ethanol and deionized water to regulate the viscosity of mixture simultaneously.Carry out mechanical mixture, rotating speed is 600r/min, stirs 3 hours.Then by the slurry dual coating mixing on latticed lead alloy grid, be placed in 80
oin C baking oven, vacuumize is more than 10 hours, the charcoal negative plate for lead-acid ultra-battery that obtains being made by modified activated carbon.
embodiment 9:take 10wt.%Pb (NO
3)
2with 90wt.% active carbon.By Pb (NO
3)
2be dissolved in deionized water, make Pb (NO
3)
2solution.Active carbon is immersed in to Pb (NO
3)
2in solution, magnetic agitation 2 hours; Said mixture is placed in to ultrasonic washing instrument ultrasonic 2 hours; With vacuum pump, mixture is carried out to suction filtration, and with deionized water washing for several times; Filter cake is dispersed in to the H of 2mol/L
2sO
4in solution, magnetic agitation 2 hours, ultrasonic 2 hours; With vacuum pump, mixture is carried out to suction filtration, and wash to filtrate PH ≈ 7 with deionized water; Filter cake is placed in to 120 ℃ of baking ovens, dry more than 10 hours.Make chemical modification PbSO
4active carbon.
Take 80 wt.% doping chemical modification PbSO
4active carbon, 10 wt.% acetylene blacks evenly mix, 2.5 wt.% CMC, 7.5 wt.% SBR are added in mixture, add appropriate ethanol and deionized water to regulate the viscosity of mixture simultaneously.Carry out mechanical mixture, rotating speed is 600r/min, stirs 3 hours.Then by the slurry dual coating mixing on latticed lead alloy grid, be placed in 80
oin C baking oven, vacuumize is more than 10 hours, the charcoal negative plate for lead-acid ultra-battery that obtains being made by modified activated carbon.。
embodiment 10:take 8wt.%Bi
2o
3with 92wt.% active carbon.By Pb (NO
3)
2be dissolved in deionized water, make Bi (NO
3)
3solution.Active carbon is immersed in to Bi (NO
3)
3in solution, magnetic agitation 2 hours; Said mixture is placed in to ultrasonic washing instrument ultrasonic 2 hours; With vacuum pump, mixture is carried out to suction filtration, and with deionized water washing for several times; Filter cake is dispersed in the KOH solution of 2mol/L to magnetic agitation 2 hours, ultrasonic 2 hours; With vacuum pump, mixture is carried out to suction filtration, and wash to filtrate PH ≈ 7 with deionized water; Filter cake is placed in to 120 ℃ of baking ovens, dry more than 10 hours.Make chemical modification Bi (OH)
3active carbon.
Take 80 wt.% doping chemical modification Bi (OH)
3active carbon, 10 wt.% acetylene blacks evenly mix, 2.5 wt.% CMC, 7.5 wt.% SBR are added in mixture, add appropriate ethanol and deionized water to regulate the viscosity of mixture simultaneously.Carry out mechanical mixture, rotating speed is 600r/min, stirs 3 hours.Then by the slurry dual coating mixing on latticed lead alloy grid, be placed in 80
oin C baking oven, vacuumize is more than 10 hours, the charcoal negative plate for lead-acid ultra-battery that obtains being made by modified activated carbon.
To technique effect of the present invention, be described further as follows:
The negative plate electrode that the modified activated carbon making for embodiment 7 makes as electrode material carries out cyclic voltammetry scan, sweeps speed for 5mV/s, and sweep limits is-0.7V～0V; Carry out timing testing current, step potential is-0.55V～-1.1V.Result shows, after modification, the ratio electric capacity of active carbon increases 40%, liberation of hydrogen rate reduction 5～40%.Visible employing this method modified activated carbon capacitance characteristic is obvious, and liberation of hydrogen rate reduction, reaches the object of mating with Pb electrode potential.
The negative plate electrode making as electrode material for the modified activated carbon with embodiment 9 makes carries out cyclic voltammetry scan, sweeps speed for 5mV/s, and sweep limits is-0.7V～0V; Carry out timing testing current, step potential is-0.55V～-1.1V.Result shows, after modification, the ratio electric capacity of active carbon increases 75%; Liberation of hydrogen rate reduction 20～74%.The active carbon capacitance characteristic preparing after the modification of visible employing this method obviously strengthens, and liberation of hydrogen speed obviously reduces, and reaches the object of mating with Pb electrode potential.
The claims in the present invention protection range is not limited to above-described embodiment.
Claims (10)
1. a modified activated carbon, is characterized in that, comprises active carbon and trim; It is trim to be incorporated into mixing, attrition process in activated carbon powder form; Described trim comprises Pb, BaSO
4and ZnO, be one or more combinations wherein.
2. the compounding method of modified activated carbon claimed in claim 1, it is characterized in that, step is mainly: first take in proportion active carbon and trim, then described active carbon and trim are dropped in ball mill, using ethanol as ball-milling medium mixing, attrition process, finally the material processing is placed in to baking oven dry, makes modified activated carbon.
3. a modified activated carbon, is characterized in that, comprises active carbon and trim; It is active carbon is immersed in trim salting liquid stir, vibration processes; Described trim comprises Pb (NO
3)
2, Ba (CH
3cOO)
2and Bi(NO
3)
3, be one or more combinations wherein.
4. the preparation method of modified activated carbon claimed in claim 3, it is characterized in that, step is mainly: first take in proportion active carbon and trim, then described trim is mixed with to trim salting liquid, again active carbon is immersed in trim salting liquid with magnetic agitation, sonic oscillation, filtering and washing, after this, then is dispersed in excessive precipitant solution filter cake with magnetic agitation, sonic oscillation again; Filtering and washing to filtrate Ph value is pH6～8 again, finally the material processing is placed in to baking oven dry, makes modified activated carbon.
5. the preparation method of modified activated carbon according to claim 4, is characterized in that, precipitant solution is H
2sO
4, or KOH.
6. according to the modified activated carbon described in claim 1 or 3, it is characterized in that, the mass ratio of trim and active carbon is 0.01～0.3: 1.
7. of modified activated carbon of the present invention, make a method for lead-acid ultra-battery charcoal negative plate, it is characterized in that, charcoal negative plate comprises that lead alloy grid and Tu negative pole carbon paste thereon forms through solidifying last oven dry; The constituent of described negative plate carbon paste comprises: modified activated carbon, acetylene black, sodium cellulose glycolate (CMC) and butadiene-styrene rubber (SBR); Making step is mainly: first take in proportion modified activated carbon, acetylene black, CMC and SBR, then mix form slurry, and regulate the viscosity of slurry, again the slurry mixing is coated on lead alloy grid, finally be placed in baking oven vacuumize, become lead-acid ultra-battery charcoal negative plate.
8. the method that use according to claim 7 modified activated carbon of the present invention is made lead-acid ultra-battery charcoal negative plate, it is characterized in that, the constituent content ratio of negative plate carbon paste is by negative plate carbon paste weighing scale: modified activated carbon is 75～85%, acetylene black is 6～12%, CMC is that 2～3%, SBR is 6～8%.
9. the method that use according to claim 7 modified activated carbon of the present invention is made lead-acid ultra-battery charcoal negative plate, is characterized in that, regulating the viscosity of slurry is 3.5～5.5g/cm
3.
10. the method that use according to claim 7 modified activated carbon of the present invention is made lead-acid ultra-battery charcoal negative plate, is characterized in that, the thickness that the slurry mixing is coated on lead alloy grid is 1.2～3mm.
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Cited By (1)
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| CN103887505A (en) * | 2014-04-14 | 2014-06-25 | 中南大学 | Application of functional carbon material and high-hydrogen-evolution substance doped functional carbon material |
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Application publication date: 20140305 |