CN106450293B - A kind of high active substance utilization rate battery cathode lead paste formula and preparation method thereof - Google Patents
A kind of high active substance utilization rate battery cathode lead paste formula and preparation method thereof Download PDFInfo
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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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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- 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
- 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 present invention relates to a kind of high active substance utilization rate battery cathode lead paste formulas and preparation method thereof, belong to Lead-acid Battery Technology field, and the high active substance utilization rate battery cathode lead plaster includes following components：Density is dilute sulfuric acid, deionized water, lignin Vanisperse AT, polyaniline potassium sulfonate PAN K, nano-hollow barium sulfate, acetylene black, lotion carbon nanotube Sus CNT, the lead powder of 1.38g/ml.The present invention substitutes conventional polyester staple fiber completely on the basis of traditional cathode lead plaster formula using water-soluble polyaniline potassium sulfonate PAN K；Traditional blanc fixe is substituted using nano-hollow barium sulfate completely；Cream deionized water is closed using the substitution of lotion carbon nanotube Sus CNT parts.The cathode produced with the formula can be under the premise of cycle life not be reduced, conspicuousness promotes negative electrode active material utilization rate and charge acceptance, and huge application and promotion prospect will be had in negative electrode active material lightweight, reduction lead-acid accumulator manufacture cost development field.
Description
Technical field
The invention belongs to Lead-acid Battery Technology field, born specifically, being related to a kind of high active substance utilization rate battery
Pole lead paste formula and preparation method thereof.
Background technology
With lead-acid accumulator industry encourage competition situation, major accumulator manufacturer continuously improve production technology and
Technology manufactures cost and material cost to lead-acid accumulator and optimizes, wherein for the light of grid and its active material
Quantization is almost the focus technology research tendency of all battery manufacturers in the whole world.At present, orthodox car starts with SLI plumbic acids
Storage battery negative extremely 20h rates active material utilization be 55%-65%, take into account battery cycle life not conspicuousness reduce and
Under the premise of not changing battery structure, cathode 20h rates active material utilization can not almost break through 70%.Therefore, lead acid storage battery
Cathode too low active material utilization in pond seriously hinders the development and application of negative electrode active material lightweight cost declining technology.
It is main due to being directed to Pb-Ca-Sn-Al grid alloys and its negative electrode active material lightweight cost declining in industry
Technical solution concentrates on the following aspects：
Grid alloy lightweight improves.Traditional Pb-Ca- is replaced using Lead Foam grid or plastics plating Pb grids
Sn-Al alloy grids, since still Lead Foam grid or plastics plate the defects of Pb grids are due to technology and manufacturing process, machine
Tool intensity and the anticorrosive ability of growing up are far away from traditional Pb-Ca-Sn-Al alloys, it is difficult to industrialization promotion.
The apparent density of cathode lead plaster is greatly lowered, increases lead plaster acid content.Orthodox car is started with SLI cathode lead plasters
Apparent density by 4.2g/cm2It is reduced to 4.0g/cm2Even lower, this behave can obviously improve the active material utilization of cathode,
But the conspicuousness reduction of cathode lead plaster apparent density can seriously affect the cycle life of negative electrode active material, and contain by increasing lead plaster
Acid is measured to reduce cathode lead plaster apparent density, and the conspicuousness reduction of apparent density can cause lead plaster hardness excessive, when filling, grid deformation
Seriously, while to technique and equipment there is higher requirement.
Invention content
In order to overcome the shortcomings of in above-mentioned background technology, the present invention provides a kind of high active substance utilization rate battery cathode lead
Paste formulation and preparation method thereof, the cathode produced with the formula can be under the premise of cycle life do not reduced, and conspicuousness is promoted negative
Pole active material utilization and charge acceptance.
To achieve these goals, the present invention is implemented according to following technical scheme：
A kind of high active substance utilization rate battery cathode lead paste formula, the high active substance utilization rate battery cathode lead
Cream includes following components：Density is dilute sulfuric acid, deionized water, lignin VanisperseAT, the polyaniline sulfonic acid of 1.38g/mL
Potassium PAN-K, nano-hollow barium sulfate, acetylene black, lotion carbon nanotube Sus-CNT, lead powder.
Further, the dosage of the high active substance utilization rate battery cathode lead plaster each component is：Density is
The dilute sulfuric acid of 1.38g/mL is the 9%~11% of lead powder weight, deionized water is the 6%~8% of lead powder weight, lignin
Vanisperse AT are the 0.2%~0.4% of lead powder weight, polyaniline potassium sulfonate PAN-K is lead powder weight 0.1%~
0.2%th, nano-hollow barium sulfate is the 0.8%~1.0% of lead powder weight, acetylene black is lead powder weight 0.2%~0.25%,
Lotion carbon nanotube Sus-CNT is the 2%~4% of lead powder weight.
Preferably, the degree of oxidation of lead powder is 70%~80%, impurity iron, manganese, copper, chlorinity are less than 5ppm.
A kind of preparation method of high active substance utilization rate battery cathode lead paste formula, the specific steps are：
1) lignin Vanisperse AT of formula ratio, nano-hollow barium sulfate, acetylene black are subjected to mechanical premix；
2) uniform material will be premixed integrally to be scattered in lead powder, carries out dry stirring, be uniformly mixed for use；
3) polyaniline potassium sulfonate PAN-K is added in 6%~7.5% (the 6%~7.5% of lead powder weight) deionized water
It is sufficiently stirred, is configured to suspension；
4) suspension, lotion carbon nanotube obtained by step 3) are rapidly joined together in the mixing lead powder obtained by step 2),
Carry out wet stirring；
5) dilute sulfuric acid that density is 1.38g/mL is slowly added in the lead plaster obtained by step 4), continues stirring and close cream, most
It is afterwards 4.3~4.4g/cm with remaining deionized water tune apparent density of lead paste3, needle penetration is 18~20 ㎜.
Preferably, in step 5), the control of cream temperature is closed between 45 DEG C~55 DEG C.
Polyaniline potassium sulfonate PAN-K is that one kind is chemically modified in traditional polyaniline molecule structure, in polyaniline point
Sulfonic water-soluble conducting polymer sylvite is introduced in subchain, sulfonic group is located at the ortho position of phenyl ring-NH- substituent groups, and oxygen is born
Ion can form intramolecular hydrogen bond with the hydrogen atom on-NH-, greatly improve the stability of PAN-K molecular structures.Its effective content
95% should be not less than, the impurity contents such as Fe, Mn, Cu, Cl are not higher than 5ppm.
The nano-hollow barium sulfate is that a kind of chemical inertness is strong, and the ellipticity nanometer of high-crystallinity and high rheological variation energy is empty
Core material, have higher BET specific surface area, with lead plaster matrix compatibility it is good, be tightly combined the features such as.Its barium sulfate effectively contains
Amount should be not less than 99.9%, and the impurity contents such as Fe, Mn, Cu, Cl are not higher than 5ppm.
The lotion carbon nanotube Sus-CNT is that one kind purifies traditional multi-walled carbon nanotube and chemical modification is grown up
The carbon nanotube of uniform, three-dimensional netted intertexture is spent, then its ultrasound is dispersed in particular polarity protonic solvent DMSO and is gone
A kind of suspension in Ar ion mixing solvent.The impurity contents such as its Fe, Mn, Cu, Cl are not higher than 50ppm.
Beneficial effects of the present invention：
The present invention substitutes conventional polyester staple fiber completely using water-soluble polyaniline potassium sulfonate PAN-K, can effectively improve
Compatibility of the active material between material enhances the binding force between active material and grid, reduces charge and discharge polarization resistance,
Improve the initial capacitance and charge acceptance of lead-acid battery；Traditional blanc fixe is substituted using nano-hollow barium sulfate,
Can barium sulfate itself reunion probability be reduced with conspicuousness, improve lead sulfate nucleus quantity when discharging and reduce the effective ruler of lead sulfate
It is very little, cathode sulfation and crystal is effectively delayed to grow up, improves discharge capacity；Lotion carbon nanotube Sus-CNT is added in, can be increased
Cathode is practical to participate in reactivity real table area, reduces the current density in discharge process and electrode polarization, makes carbon nanotube
It is uniformly distributed between active material and forms effectively three-dimensional conductive network, reduce the internal resistance of cell, increase the hole of active material
Rate improves active material utilization and charge acceptance.
While improving cycle life in part using the lead-acid accumulator of the cathode formula, negative electrode active material profit is promoted
With rate to 74% (promotion amplitude is up to more than 15%)；Charge acceptance promotes amplitude and is up to 75%；Partial state of charge is high
The circulation service life, (HRPSoC) can promote 5%.Under the premise of ensureing that cycle life does not reduce, lead acid storage battery is significantly promoted
Pond performance early period has great application value in negative electrode active material lightweight field.
Description of the drawings
Fig. 1 is the discharge voltage time curve of battery testing one；
Fig. 2 is charging/discharging voltage-cycle-index curve of battery testing three.
Specific embodiment
Embodiment 1
1) first by lignin Vanisperse AT 0.25Kg, nano-hollow barium sulfate 0.92Kg, acetylene black 0.225Kg into
Row machinery premix, after premixing uniformly it is whole be scattered in 100Kg lead powder carry out it is dry be uniformly mixed, dry mixing time control exists
In 10~15min；
In a certain range, extend mixing time, be conducive to improve Vanisperse AT, nano-hollow barium sulfate, acetylene
The black dispersion degree in lead powder, makes additive be dispersed in lead powder powder, but the time is too long that be easy to cause production efficiency low.
2) 0.125Kg polyaniline potassium sulfonates PAN-K in 7Kg deionized waters is sufficiently stirred in advance and is configured to suspension,
Itself and 3Kg lotions carbon nanotube are rapidly joined simultaneously again, wet stirring is carried out in above-mentioned mixing lead powder, wet mixing time control is 3
In~5min；
3) the 10.2Kg aqueous sulfuric acids that density is 1.38g/mL are slowly added to the lead plaster after wet stir evenly, continue to stir
Control is mixed in 18~20min, during entire cathode lead plaster closes cream, cream temperature is closed and must be strictly controlled at 45 DEG C~55 DEG C
Between, it is finally 4.3~4.4g/cm with 0.25Kg deionized waters fine tuning apparent density of lead paste3, needle penetration is 18~20mm.
4) negative plate is prepared as stated above, is carried out dry curing according to normal production technology, encapsulating, assembling, is changed
Into etc. processes, the battery for manufacturing respective model tested.
Embodiment 2
1) first by lignin Vanisperse AT 0.25Kg, nano-hollow barium sulfate 0.98Kg, acetylene black 0.21Kg into
Row machinery premix, after premixing uniformly it is whole be scattered in 100Kg lead powder carry out it is dry be uniformly mixed, dry mixing time control exists
In 10~15min；
2) 0.145Kg polyaniline potassium sulfonates PAN-K in 6.82Kg deionized waters is sufficiently stirred in advance and is configured to suspend
Liquid, then it with 3.2Kg lotions carbon nanotube is rapidly joined simultaneously, wet stirring is carried out in above-mentioned mixing lead powder, wet mixing time control
System is in 3~5min；
3) the 9.9Kg aqueous sulfuric acids that density is 1.38g/mL are slowly added to the lead plaster after wet stir evenly, continue to stir
Control is mixed in 18~20min, during entire cathode lead plaster closes cream, cream temperature is closed and must be strictly controlled at 45 DEG C -55 DEG C
Between, it is finally 4.3~4.4g/cm with 0.35Kg deionized waters fine tuning apparent density of lead paste3, needle penetration is 18~20mm；
4) negative plate is prepared as stated above, is carried out dry curing according to normal production technology, encapsulating, assembling, is changed
Into etc. processes, the battery for manufacturing respective model tested.
Experimental analysis：
Battery testing one：
2V/3Ah AGM start and stop lead-acid accumulators, the tool of 20h active material utilizations are prepared using inventive formulation
Body examination method for testing：
Under 25 DEG C of water bath conditions, after accumulator full charge, with I20=0.15A is discharged to 1.75V, records discharge time
T (h), and integral and calculating 20h rate discharge capacities C is carried out according to current versus time curve20And 20h rate active material utilizations.Its
Middle η20hRate=C20/ 6*100%.Following table is 20h negative electrode active material utilization rate statistical forms, and Fig. 1 is discharge voltage time curve.
| 20h negative electrode active materials utilization rate (%) | |
| Inventive formulation | 74% |
| Regular convention formula | 64% |
Battery testing two：
2V/3Ah AGM start and stop lead-acid accumulators, charge acceptance test method ginseng are prepared using inventive formulation
It is performed according to GB/T 5008.1-2013, it is specific as follows：
With I in 1~3h after accumulator is fully charged10Then constant-current discharge 5h stands for 24 hours at a temperature of 0 DEG C, takes out battery,
With constant-voltage charge 10min under the conditions of 2.4V in 2min, the charging current I of 10min is recordedca(A), and according to current-vs-time
Change curve carries out actually being filled with electricity Q in integral and calculating 10minca, and calculate Ica/I10Ratio and Qca/C20Ratio.Herein
I10=C20/ 10, I20To test 20h rate capacity Cs20When corresponding discharge current.
| Ica(A) | Ica/I10 | Qca/C20(%) | |
| Inventive formulation | 3.82 | 8.51 | 18.87% |
| Regular convention formula | 1.83 | 4.77 | 9.74% |
Battery testing three：
2V/3Ah AGM start and stop lead-acid accumulators are prepared using inventive formulation, in partial state of charge (50%
SOC the high power charging-discharging cycle life test method under) is：
Under (1) 25 DEG C of water-bath test environment, with I=2*I in 1~2h after accumulator is fully charged20Constant-current discharge 5h to 50%
Then state-of-charge, end condition 1.75V do following cycle：
A) with I=3C constant-current charges 1min；
B) 1min is stood；
C) with I=3C constant-current discharges 1min；
D) 1min is stood；
(2) wherein in cyclic process, charging voltage reaches end-of-life higher than 2.83V or discharge voltage less than 1.73V
Condition.C herein is 20h rate capacity Cs20, I20To test 20h rate capacity Cs20When corresponding discharge current.Following table is global cycle time
Number test statistics are as a result, Fig. 2 is this test charging/discharging voltage-cycle-index curve.
| Global cycle number | |
| Inventive formulation | 3080 |
| Regular convention formula | 2500 |
Above-mentioned detection experiment is carried out by examination criteria, and the performance test results show：20h negative electrode active materials utilization rate compared with
Existing regular convention formula improves 10%；The more existing regular convention formula of charge acceptance improves more than 75%；Under partial state of charge
The more existing regular convention formula of high power charging-discharging cycle life (HRPSoC) improves 5%.
In conclusion using the AGM start and stop lead-acid accumulators of the cathode formula, before can not being reduced ensureing cycle life
It puts, lead-acid battery negative pole active substance utilization rate and charge acceptance is significantly promoted, in negative electrode active material light weight
Change field has great application value.
Finally, above example and attached drawing are merely illustrative of the technical solution of the present invention and unrestricted, although by above-mentioned
Embodiment is described in detail the present invention, however, those skilled in the art should understand that, can in form and carefully
Various changes are made to it on section, without departing from claims of the present invention limited range.
Claims (5)
1. a kind of high active substance utilization rate battery cathode lead plaster, it is characterised in that：The high active substance utilization rate battery
Cathode lead plaster includes following components：Density is dilute sulfuric acid, deionized water, lignin Vanisperse AT, the polyphenyl of 1.38g/mL
Amine potassium sulfonate PAN-K, nano-hollow barium sulfate, acetylene black, lotion carbon nanotube Sus-CNT, lead powder.
2. high active substance utilization rate battery cathode lead plaster according to claim 1, it is characterised in that：The high activity
The dosage of material utilization battery cathode lead plaster each component is：The dilute sulfuric acid that density is 1.38g/mL be lead powder weight 9%~
11%th, deionized water is the 6%~8% of lead powder weight, lignin Vanisperse AT are the 0.2%~0.4% of lead powder weight, polyphenyl
Amine potassium sulfonate PAN-K is the 0.1%~0.2% of lead powder weight, nano-hollow barium sulfate is the 0.8%~1.0% of lead powder weight, acetylene
It is black be lead powder weight 0.2%~0.25%, lotion carbon nanotube Sus-CNT be the 2%~4% of lead powder weight.
3. high active substance utilization rate battery cathode lead plaster according to claim 1, it is characterised in that：The lead powder oxygen
Change degree is 70%~80%, and impurity iron, manganese, copper, chlorinity are less than 5ppm.
4. the preparation method of high active substance utilization rate battery cathode lead plaster according to claim 1, it is characterised in that：Tool
Body step is：
1）Lignin Vanisperse AT, nano-hollow barium sulfate, acetylene black of formula ratio are subjected to mechanical premix；
2）Uniform material will be premixed integrally to be scattered in lead powder, carry out dry stirring, be uniformly mixed for use；
3）Polyaniline potassium sulfonate PAN-K is added in the deionized water that weight is lead powder 6%~7.5% and is sufficiently stirred, is configured to
Suspension；
4）By step 3）Gained suspension, lotion carbon nanotube rapidly join step 2 together）In the mixing lead powder of gained, carry out
Wet stirring；
5）The dilute sulfuric acid that density is 1.38g/mL is slowly added to step 4）In the lead plaster of gained, continue stirring and close cream, finally use
Remaining deionized water tune apparent density of lead paste is 4.3~4.4g/cm3, needle penetration is 18~20 ㎜.
5. the preparation method of high active substance utilization rate battery cathode lead plaster according to claim 4, it is characterised in that：Step
Rapid 5）In, the control of cream temperature is closed between 45 °C~55 °C.
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| CN111224097B (en) * | 2020-01-16 | 2021-09-21 | 中国科学院福建物质结构研究所 | Lead paste, battery plate and preparation method and application thereof |
| CN111403827B (en) * | 2020-03-19 | 2023-09-15 | 风帆有限责任公司 | Air cooling formation method and air cooling formation system for lead-acid storage battery |
| CN112242524B (en) * | 2020-09-15 | 2022-07-15 | 骆驼集团蓄电池研究院有限公司 | Formula and preparation method of negative lead plaster for improving high and low temperature performance of lead-acid storage battery |
| CN114639802B (en) * | 2022-03-02 | 2023-09-29 | 中国科学院福建物质结构研究所 | Barium sulfate-conductive polymer composite material and preparation method and application thereof |
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| JP2003142104A (en) * | 2001-10-31 | 2003-05-16 | Masaru Sugita | Battery constituting material |
| CN104900851A (en) * | 2015-06-24 | 2015-09-09 | 湖北骆驼蓄电池研究院有限公司 | Cathode for lead-carbon batteries, production method of cathode and battery made with cathode |
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| CN105702953A (en) * | 2016-04-27 | 2016-06-22 | 骆驼集团蓄电池研究院有限公司 | High-temperature heavy-load negative lead paste for start-stop battery and preparation method of negative lead paste |
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| JP2003142104A (en) * | 2001-10-31 | 2003-05-16 | Masaru Sugita | Battery constituting material |
| CN104900851A (en) * | 2015-06-24 | 2015-09-09 | 湖北骆驼蓄电池研究院有限公司 | Cathode for lead-carbon batteries, production method of cathode and battery made with cathode |
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| CN105702953A (en) * | 2016-04-27 | 2016-06-22 | 骆驼集团蓄电池研究院有限公司 | High-temperature heavy-load negative lead paste for start-stop battery and preparation method of negative lead paste |
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Effective date of registration: 20190222 Address after: No. 16 Gushui Road, Gucheng Economic Development Zone, Xiangyang City, Hubei Province Patentee after: Camel Group Huazhong Battery Company Address before: 441000 No. 65 Hanjiang North Road, Xiangyang High-tech Zone, Xiangfan City, Hubei Province Patentee before: CAMEL GROUP STORAGE BATTERY RESEARCH INSTITUTE CO., LTD. |