CN107579240A - A kind of preparation method of C-base composte material for lead carbon battery negative pole - Google Patents
A kind of preparation method of C-base composte material for lead carbon battery negative pole Download PDFInfo
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- CN107579240A CN107579240A CN201710849941.6A CN201710849941A CN107579240A CN 107579240 A CN107579240 A CN 107579240A CN 201710849941 A CN201710849941 A CN 201710849941A CN 107579240 A CN107579240 A CN 107579240A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The present invention relates to a kind of preparation method of the C-base composte material for lead carbon battery negative pole, can prepare the controllable carbon-based lead compound composite of ratio, and wherein lead compound is uniformly distributed in carbon material surface and keeps the architectural feature of carbon material script.Preparation method is as follows：Carbon material and lead ion solution are well mixed in reaction vessels, precipitating reagent is slowly added dropwise, lead ion is completely deposited at carbon material surface, filtering, washing, which is dried, obtains presoma, then obtains composite by high-temperature process, and lead compound mass ratio is between 1 90%.The particles of lead oxide on surface, which can make to have between composite and lead-acid battery cathode active material, preferably to be combined, the cathode specific capacity of the GND prepared simultaneously using the composite additives has obvious increase, reduce negative pole hydrogen-separating quantity, negative electrode active material utilization rate is set also to have a distinct increment, the cycle life of the high power charging-discharging of its partial state of charge is significantly increased.
Description
Technical field
The present invention relates to a kind of method that carbon-based oxidation lead composite material is prepared by chemical deposition, it is related to electrochmical power source
Field
Background technology
As the consumption to fossil fuel and the pay attention to day by day of environmental problem, the development of sustainable clean energy resource are standby
It is concerned.Secondary cell has further been sent out as a ring indispensable in energy storage and output transfer process
Exhibition, but higher challenge is also faced with simultaneously.The important a member of VRLA battery (VRLA) as secondary cell because its into
Ripe manufacturing process, low production cost and high safety performance is by one of important candidate as electrokinetic cell and energy-storage battery.But
It is that battery is often in charge less electricity condition, in partial state of charge (PSoC-- under whether power application or stored energy application
Partial State of Charge).Easily there is negative pole in the charge and discharge process under PSoC states in traditional lead-acid battery
The problem of sulfation of plate, while the charging current ability to accept of battery is relatively low, can reduce current efficiency and the circulation of battery
In the life-span, cause the premature failure of battery.
Modified of the lead carbon battery as lead-acid battery, by regarding carbon material as cathode additive agent, can effectively it carry
The performance of high battery.P.T.Moseley once summarized the possible mechanism of action of carbon material：Carbon material has good conductive energy
Power, conductive network can be formed in plumbic acid negative plate；High-specific surface area can provide more places for reaction, while can be with
Promote the reduction of lead sulfate, suppress the generation of negative plate sulfation；Carbon material can also be used as a solution in negative plate
Holder；The electric capacity carbon material of high-specific surface area simultaneously, the electric capacity of carbon material can be provided in the discharge process that battery fills
Effect, improve the charge acceptance of negative plate.
But the material that carbon material is relatively low as a kind of hydrogen-evolution overpotential, the aggravation that can cause pole plate hydrogen evolution phenomenon is added, together
When due to interface problem existing for carbon material and negative electrode active material, both combinations in pole plate are not close, follow-up
Carbon material is easily separated with active material in charge and discharge process, influences the property of lead charcoal negative pole.
Therefore suppress or slow down the sulfation process of negative plate, improve the knot between carbon material and negative electrode active material
Conjunction property is particularly important, while it is to improve negative pole in partial state of charge to improve the overall electric current ability to accept of negative pole and current efficiency
The importance of cycle life under state.
Patent in terms of the improvement of plumbic acid negative pole is more, in the B of its Patent CN 102074702 by by carbon material and
The material mixings such as carbon black, adhesive are supported on conductive motherboard, with the method for electro-deposition by lead deposit to carbon material particles, then from
Material is scraped on motherboard；But this method operation is more troublesome, and be easily destroyed surface texture, at the same prepare the amount of material by
Load and limit to early stage, be not easy to mass produce.Patent CN201310077914, by by conductive carbon material and containing lead solution,
Composite is obtained by spray drying process, then by drying process, this method forms lead oxide shell by carbon material surface, and one
Determine to reduce the liberation of hydrogen problem of carbon material in degree, but this method, in preparation process, the lead oxide on surface is to pass through carbon materials
After expecting surface and lead ion combination, just formed by drying, its distribution is relevant with carbon surface and uneven.Other patent
The method that CN201210493085 is modified by wet ball grinding and surface is prepared to carbon material, and passes through vacuum lead plating
Method prepares composite, improves the lead content on surface and the caking property of active material, but material prepared by this method loses
The structural property of original carbon material, it is also relatively complicated.And CN201210070245 and CN201210070245 is by by carbon source
The composite of carbon material cladding lead is prepared for by the method for hydro-thermal and microwave with lead powder mixing, the machinery for improving pole plate is strong
Degree, but the exposed of carbon material can cause more serious liberation of hydrogen problem.
The present invention prepares carbon-based oxidation lead composite material, carbon material surface by simple controllable chemical deposition
Uniform particles of lead oxide is evenly distributed, material can be made preferably to be mixed with negative active core-shell material, improves pole plate
Internal caking property, conductive network is formed between active material, promote the mutual conversion of lead and lead sulfate in course of reaction, from
And improve the utilization rate of positive and negative pole active matter.The composite prepared simultaneously maintains the multistage pore canal knot of original carbon material
Structure.
The content of the invention
The invention provides a kind of preparation method of the C-base composte material for lead carbon battery negative pole, method simply may be used
OK, the material surface of preparation be evenly distributed, size it is homogeneous, while improve being well mixed for composite and negative electrode active material
Property, the utilization rate of positive and negative pole active matter can be improved during applied to plumbic acid negative pole, and possess good charge-discharge performance and follow
Ring performance.
For achieving the above object, this programme takes following technical scheme：
A kind of preparation method of C-base composte material for lead carbon battery negative pole, in reaction vessels add carbon material and
Lead ion solution is uniformly mixed, and described carbon material is in 1mol L-1H2SO4In electrolyte solution, its quality specific capacitance
In 20-250F g-1Between；The lead ion solution concentration is in 0.005-0.1mol L-1Between, between pH=3-7；It is described mixed
The ratio of the quality of lead ion and the quality of carbon material is between 0.0094-8.354 in conjunction solution；The mixing time of material
Between 15-45min, after being uniformly mixed, precipitant solution is slowly added dropwise, precipitant solution concentration is 0.001-
0.05mol L-1Between, rate of addition is 0.5-5 drops s-1, lead-containing compounds is deposited on carbon material surface, it is complete to precipitating,
Filtering, dry by organic solvent and deionized water washing and obtain presoma, high-temperature process obtains under a shielding gas by presoma
Obtain carbon-based oxidation lead composite material.
Selected carbon material is derived from the electric capacity carbon material of organic matter, and organic matter includes petroleum coke, polymer or life
Material etc..
Described carbon material has multi-stage artery structure, and its specific surface area is in 1500-3000m2g-1Between, particle diameter is less than
1000 mesh.
Used lead ion solution is the one or more in lead chloride, plumbi nitras, lead acetate, pyrovinic acid lead.
Added precipitating reagent is the one or more in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
The filtering, which uses, to be filtered under diminished pressure, and is washed 1-5 times repeatedly with deionized water and absolute ethyl alcohol.
The drying is that 5-12h is dried at 50-100 DEG C using air dry oven.
High-temperature process is at the tube furnace high temperature under nitrogen or argon gas protection to the presoma under a shielding gas
Reason, temperature is at 300-800 DEG C, time 0.5-5h.
Prepared composite material surface lead oxide is evenly distributed, size uniformity, while lead oxide and carbon material in material
Ratio it is controllable, the content of lead oxide is between 1% to 90%.
Beneficial effect：The composite prepared using such scheme improves original proportion, and it is equal to obtain surface distributed
Even, uniform carbon-based oxidation lead composite material, and negative electrode active material mixing, after tested, the capacity and active matter of negative pole
The utilization rate of matter is significantly improved.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the composite prepared by embodiment 1；
Fig. 2 is the XRD diffraction patterns of the composite prepared by embodiment 1；
Fig. 3 is the cathode specific capacity and voltage relationship figure of composite prepared by addition embodiment 1；
Fig. 4 is the scanning electron microscope (SEM) photograph of the composite prepared by embodiment 2；
Fig. 5 is the cathode specific capacity and voltage relationship figure of composite prepared by addition embodiment 2；
Fig. 6 is the scanning electron microscope (SEM) photograph of the composite prepared by embodiment 3；
Fig. 7 is the cathode specific capacity and voltage relationship figure of composite prepared by addition embodiment 3；
The high magnification operation number of turns under the partial status of each embodiments of Fig. 8.
Embodiment
Below in conjunction with example, the invention will be further described.
Embodiment 1：
(1) 10.0g rice husks base electric capacity carbon material and 860ml 0.1mol L are added in beaker-1Lead nitrate solution, stir
Mix 20min it is well mixed after, obtain finely dispersed mixed solution；
(2) 0.05mol L are slowly added dropwise into (1) described mixed solution-1Sodium hydroxide solution, make lead in carbon material surface
Precipitation is complete, is filtered under diminished pressure, is washed repeatedly 3 times by absolute ethyl alcohol and deionized water, and 8h is dried in 60 DEG C of air dry oven,
Obtain persursor material；
(3) persursor material described in (2) is placed on N in 380 DEG C of tube furnaces2The lower processing 5h of protection, obtains black finally
Composite.
(4) composite obtained by above-mentioned (3) is used to prepare GND and and PbO as additive2Positive plate assembling electricity
Pond, 5mol L are used as barrier film, electrolyte using AGM dividing plates-1Sulfuric acid solution.
(5) through 5mA g-1Current density is discharged, the mass-energy density of the cell negative plate and the utilization rate of negative electrode active material
Amount compares improves 16% than plumbic acid negative plate.The high magnification test life-span of partial state of charge improves a lot simultaneously, and the life-span carries
It is high 1.87 times.
Embodiment 2
(1) 10g rice husks base electric capacity carbon material and 860ml 0.025mol L are added in beaker-1Lead nitrate solution, stir
Mix 30min it is well mixed after, obtain finely dispersed mixed solution；
(2) 0.025mol L are slowly added dropwise into (1) described mixed solution-1Sodium hydroxide solution, lead-containing compounds are made to sink
Product is complete in carbon material surface precipitation, is filtered under diminished pressure, is washed repeatedly 3 times by absolute ethyl alcohol and deionized water, 60 DEG C of air blast
8h is dried in drying box, obtains persursor material；
(3) persursor material described in (2) is placed on processing 5h in 380 DEG C of tube furnaces, obtains black composite finally.
(4) composite obtained by above-mentioned (3) is used to prepare GND and and PbO as additive2Positive plate assembling electricity
Pond, 5mol L are used as barrier film, electrolyte using AGM dividing plates-1Sulfuric acid solution.
(5) through 5mA g-1Current density is discharged, the mass-energy density of the cell negative plate and the utilization rate of negative electrode active material
Amount compares improves 20% than plumbic acid negative plate.The high magnification test life-span of partial state of charge improves a lot simultaneously, and the life-span carries
It is high 2.48 times.
Embodiment 3
(1) 10g rice husks base electric capacity carbon material and 860ml 0.005mol L are added in beaker-1Lead nitrate solution, stir
Mix 30min it is well mixed after, obtain finely dispersed mixed solution；
(2) 0.001mol L are slowly added dropwise into (1) described mixed solution-1Sodium hydroxide solution, lead-containing compounds are made to sink
Product is complete in carbon material surface precipitation, is filtered under diminished pressure, is washed repeatedly 3 times by absolute ethyl alcohol and deionized water, 60 DEG C of air blast
8h is dried in drying box, obtains persursor material；
(3) persursor material described in (2) is placed on processing 5h in 380 DEG C of tube furnaces, obtains black composite finally.
(4) composite obtained by above-mentioned (3) is used to prepare GND and and PbO as additive2Positive plate assembling electricity
Pond, 5mol L are used as barrier film, electrolyte using AGM dividing plates-1Sulfuric acid solution.
(5) through 5mA g-1Current density is discharged, the mass-energy density of the cell negative plate and the utilization rate of negative electrode active material
Amount compares improves 23.4% than plumbic acid negative plate.The high magnification test life-span of partial state of charge improves a lot simultaneously, the life-span
Improve 4.45 times.
Claims (9)
- A kind of 1. preparation method of C-base composte material for lead carbon battery negative pole, it is characterised in that：Add in reaction vessels Enter carbon material and lead ion solution is uniformly mixed, described carbon material is in 1mol L-1H2SO4In electrolyte solution, its Quality specific capacitance is in 20-250F g-1Between；The lead ion solution concentration is in 0.005-0.1mol L-1Between, pH=3-7 it Between；The ratio of the quality of lead ion and the quality of carbon material is between 0.0094-8.354 in the mixed solution；Material mixes Mixing time is closed between 15-45min, after being uniformly mixed, precipitant solution is slowly added dropwise, precipitant solution concentration is 0.001-0.05mol L-1Between, rate of addition is 0.5-5 drops s-1, lead-containing compounds is deposited on carbon material surface, to precipitation Completely, filter, dry by organic solvent and deionized water washing and obtain presoma, by presoma under a shielding gas at high temperature Reason obtains carbon-based oxidation lead composite material.
- 2. a kind of preparation method of C-base composte material for lead carbon battery negative pole according to claim 1, its feature It is, the carbon material of selection is derived from the electric capacity carbon material of organic matter, and organic matter includes petroleum coke, polymer or biomass Deng.
- 3. a kind of preparation method of C-base composte material for lead carbon battery negative pole according to claim 1 or 2, it is special Sign is：Described carbon material has multi-stage artery structure, and its specific surface area is in 1500-3000m2g-1Between, particle diameter is less than 1000 mesh.
- 4. a kind of preparation method of C-base composte material for lead carbon battery negative pole according to claim 1, its feature It is, the lead ion solution used is the one or more in lead chloride, plumbi nitras, lead acetate, pyrovinic acid lead.
- 5. a kind of preparation method of C-base composte material for lead carbon battery negative pole according to claim 1, its feature It is, added precipitating reagent is the one or more in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
- 6. a kind of preparation method of C-base composte material for lead carbon battery negative pole according to claim 1, its feature It is, using being filtered under diminished pressure, and is washed 1-5 times repeatedly with deionized water and absolute ethyl alcohol.
- 7. a kind of preparation method of C-base composte material for lead carbon battery negative pole according to claim 1, its feature It is, the drying is that 5-12h is dried at 50-100 DEG C using air dry oven.
- 8. a kind of preparation method of C-base composte material for lead carbon battery negative pole according to claim 1, its feature It is, high-temperature process is to be carried out in the tube furnace under nitrogen or argon gas protection at high temperature to the presoma under a shielding gas Reason, temperature is at 300-800 DEG C, time 0.5-5h.
- 9. a kind of preparation method of C-base composte material for lead carbon battery negative pole according to claim 1, its feature It is, prepared composite material surface lead oxide is evenly distributed, size uniformity, while the ratio of lead oxide and carbon material in material Example is controllable, and the content of lead oxide is between 1% to 90%.
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Cited By (7)
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| CN109119606A (en) * | 2018-08-02 | 2019-01-01 | 天能电池集团有限公司 | A kind of preparation method and application of nanometer of lead deposit hierarchical porous structure carbon composite |
| CN109860531A (en) * | 2018-12-16 | 2019-06-07 | 浙江工业大学 | A kind of nanometer of lead/carbon composite preparation method and application |
| CN110010899A (en) * | 2019-05-09 | 2019-07-12 | 淮南市通霸蓄电池有限公司 | A kind of nanometer of basic lead carbonate-carbon composite and its preparation method and application |
| CN110137452A (en) * | 2019-04-26 | 2019-08-16 | 浙江工业大学 | A kind of preparation method and application of Nanometer sized lead oxide/carbon composite |
| CN111082001A (en) * | 2019-11-29 | 2020-04-28 | 吉林省凯禹电化学储能技术发展有限公司 | Porous lead oxide-carbon composite material for negative electrode of lead-carbon battery and preparation method thereof |
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| CN113871599A (en) * | 2021-09-28 | 2021-12-31 | 广西超威鑫锋能源有限公司 | Lead-coated nitrogen-doped carbon composite material, preparation thereof and application thereof in lead-carbon battery |
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| CN109860531A (en) * | 2018-12-16 | 2019-06-07 | 浙江工业大学 | A kind of nanometer of lead/carbon composite preparation method and application |
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| CN112133914A (en) * | 2020-04-09 | 2020-12-25 | 吉林省凯禹电化学储能技术发展有限公司 | Porous carbon-loaded ultra-small PbSO4Nano particle composite material, preparation thereof and application thereof in lead carbon battery anode |
| CN113871599A (en) * | 2021-09-28 | 2021-12-31 | 广西超威鑫锋能源有限公司 | Lead-coated nitrogen-doped carbon composite material, preparation thereof and application thereof in lead-carbon battery |
| CN113871599B (en) * | 2021-09-28 | 2024-04-12 | 广西超威鑫锋能源有限公司 | Lead-coated nitrogen-doped carbon composite material, preparation method thereof and application thereof in lead-carbon battery |
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Application publication date: 20180112 |