CN106207277B - A kind of preparation method of compound carbon polymer lead-acid battery - Google Patents
A kind of preparation method of compound carbon polymer lead-acid battery Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of compound carbon polymer lead-acid battery, the preparation including complex carbon material, the preparation method with the compound method of conducting polymer and battery.Complex carbon material obtained and conducting polymer are subjected to physical mixed, obtain composite carbon polymer composites, the composite carbon polymer composites that will be obtained.The anode that composite carbon conducting polymer composite material is added to lead-acid battery can effectively improve the electric conductivity of anode, increase the voidage of positive being, while can prevent the reunion of graphene and carbon material can be made to form space conductive network structure.Conducting polymer can play the conducting matrix grain that can also become in positive active material, inhibit the too early argillization of anode, to improve cycle life.Composite carbon conducting polymer lead-acid battery prepared by the present invention has the chemical conversion time short, and battery cycle life is long, the high feature of capacity.
Description
Technical field
The invention belongs to lead-acid battery manufacturing technology fields, in particular to a kind of effectively to improve battery positive electrode active object
The electric conductivity and porosity of matter improve the capacity of battery, the composite carbon of discharge performance and service life so as to improve the performance of battery
The preparation method of polymer lead-acid battery.
Background technique
An important factor for the porosity and its electric conductivity of lead-acid battery anode being, which are, influences positive plate performance.High hole
The initial capacity and the capacity under the conditions of high-multiplying power discharge that rate can improve battery, good electric conductivity shorten the chemical conversion of positive plate
Process cycle reduces positive argillization, improves the utilization rate of being.
Graphene has the characteristics that performance is stable as novel two-dimentional carbon material, excellent electric conductivity, thermal conductivity, machine
Tool intensity, its electron mobility is more than 15000cm under room temperature2/ Vs, and resistivity about 10-6Ω cm, specific surface area reach
2630m2The characteristics of/g, has received widespread attention it.The graphene of high quality chemical stabilization under high potential has than it
Its common higher antioxygenic property of carbon material.But the two-dimensional layered structure of graphene, interlayer van der Waals interaction is strong, makes
It is easily stacked in, material property is caused to decline.There is easy reunions in mixed process for graphene, in graphene edge graphite
The problems such as overlap resistance between alkene is larger.
Carbon nanotube is as monodimension nanometer material, and light-weight, hexagonal structure connection is perfect, has many abnormal power
, electricity and chemical property.
Select graphene and the composite carbon of carbon nanotube preparation that largely carbon nanotube adsorption can be made in graphite
Alkene surface avoids the stacking of graphene, improves the multidimensional electric conductivity of carbon material.The satisfactory electrical conductivity and mechanical property of carbon fiber can
On the one hand to realize the electric conductivity of line-surface structure, the mechanical performance of positive being on the other hand can be enhanced.Conducting polymer can
Keep the conductive network in active material more complete to become the conducting matrix grain in positive active material.The good of graphene is led
Hot property can also reduce the appearance of thermal runaway phenomenon to a certain extent.
Summary of the invention
The present invention provides a kind of preparation methods of compound carbon polymer lead-acid battery, and it is living effectively to improve anode
The electric conductivity and porosity of property substance improve the capacity, discharge performance and service life of battery so as to improve the performance of battery.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of compound carbon polymer lead-acid battery, conductive agent when prepared by lead-acid battery in anode diachylon are
Compound carbon polymer, the compound carbon polymer include the raw material of following parts by weight: 480-650 parts of graphene, carbon nanotubes
350-520 parts.In the technical scheme, select graphene and the composite carbon of carbon nanotube preparation that can largely make carbon
Nanotube adsorbs on the surface of graphene, avoids the stacking of graphene, improves the multidimensional electric conductivity of carbon material.Carbon nanotubes it is good
On the one hand electric conductivity and mechanical property can realize the electric conductivity of line-surface structure, the machinery of positive being on the other hand can be enhanced
Performance.
Preferably, compound carbon polymer further includes 30-50 parts of auxiliary agent, 600-900 parts of conducting polymer and acetylacetone,2,4-pentanedione
15-20 parts of iridium, wherein the auxiliary agent is made of the raw material of following parts by weight: 5-10 parts of hydroxyethyl cellulose, modified Nano zirconium English
10-15 parts of powder, 5-10 parts and silane coupling agent 15-25 parts of turpentine alcohol.In the technical scheme, conducting polymer can become just
Conducting matrix grain in the active material of pole keeps the conductive network in active material more complete, the good heating conduction of graphene
The appearance of thermal runaway phenomenon can be reduced to a certain extent.The addition of acetylacetone,2,4-pentanedione iridium is primarily to improve the stabilization of battery
Property, to improve the security performance of battery.
Preferably, modified Nano zirconium English powder the preparation method comprises the following steps: zirconium English powder is ground into 2-3cm after be put into mass fraction
In the hydrogenperoxide steam generator of 72-78%, ultrasonic vibration 10-12h calcines 2-3h after taking out drying, then at 450-500 DEG C
It is ground into nanometer powder and obtains modified Nano zirconium English powder, ultrasonic power 85-90kw.
Preferably, the graphene with a thickness of 1-30 layers, specific surface area 100-2600m2/ g, preparation method are oxygen
Change reduction, mechanical stripping, solvent removing in one or more mixed methods prepare.
Preferably, the carbon nanotubes is single-wall carbon nanotubes, double-wall carbon nano-tube, one of multiple-wall carbon nanotube
Or it is a variety of.
Preferably, conducting polymer be polyacetylene, polythiophene, polypyrrole, polyaniline, polyhenylene, polyphenylene ethylene and
One of poly bis alkynes or a variety of mixing.
Preferably, compound carbon polymer the preparation method comprises the following steps:
A) carbon nanotubes is added in graphene powder, the ethylene glycol of 4.5-6 times of graphene quality is added while stirring, adds
The angle of incidence is 5-10min, and acetylacetone,2,4-pentanedione iridium is then added, and good pressure distribution processing is carried out at pressure 21000PSI, is then heated up
To 150-220 DEG C, high-speed stirred is carried out, gained powder is added under the conditions of gas shield after filtering and is warming up to 300-650 DEG C, is obtained
To composite carbon；
B) conducting polymer and auxiliary agent are added to the ethylene glycol of 3 times of quality of conducting polymer, stirred at 78-90 DEG C
30-60min obtains premixed liquid A；
C) graphene carbon is obtained after addition premixed liquid A, ultrasonic high-speed stirred 0.2-5h in the composite carbon obtained to step a)
The compound slurry of material；
D) it the compound slurry for the graphene carbon material that step c) is obtained is filtered drying and crushing obtains composite carbon and lead
Electric polymer powder.
Preferably, high-speed stirred is ball-milling method or high-speed mixer paddling process, the time of high-speed stirred is 0.2-20h,
Revolving speed is 5000-8000rpm.
Preferably, protective gas is that nitrogen, helium, neon, argon gas, xenon one of are worked as in step a).
The beneficial effects of the present invention are:
1) addition of graphene improves the electric conductivity of active material, is conducive to the charging performance for improving battery；
2) addition of carbon nanotubes can reduce the reunion of graphene, form point face, line face with graphene, point-line-surface connects
Touching improves the electric conductivity of composite material；
3) graphene and the composite carbon of carbon nanotube preparation largely can make carbon nanotube adsorption in graphene
Surface avoids the stacking of graphene, improves the multidimensional electric conductivity of carbon material.The satisfactory electrical conductivity and mechanical property of carbon fiber can be with
On the one hand the electric conductivity for realizing line-surface structure, on the other hand can be enhanced the mechanical performance of positive being.Conducting polymer can be with
Keep the conductive network in active material more complete as the conducting matrix grain in positive active material.Graphene it is good thermally conductive
Performance can also reduce the appearance of thermal runaway phenomenon to a certain extent；
4) conducting matrix grain of the addition of conducting polymer in positive active material improves the binding force between being.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention will be further explained in detail.It should be appreciated that this hair
Bright implementation is not limited by the following examples, and the accommodation in any form made to the present invention and/or changed will all be fallen
Enter the scope of the present invention.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments is unless otherwise instructed the normal of this field
Rule method.
The graphene with a thickness of 1-30 layers, specific surface area 100-2600m2/ g, preparation method are redox, machine
One or more mixed methods preparation in tool removing, solvent removing.Carbon nanotubes is single-wall carbon nanotubes, double-walled nano-sized carbon
Pipe, one of multiple-wall carbon nanotube or a variety of.
Embodiment 1
A kind of preparation method of compound carbon polymer lead-acid battery, conductive agent when prepared by lead-acid battery in anode diachylon are
Compound carbon polymer, the compound carbon polymer include the raw material of following parts by weight: 500 parts of graphene, 500 parts of carbon nanotubes.
500g graphene is taken, surface modifier is added into graphene powder, is stirred while adding, is soaked completely to graphene
It is after profit that graphene powder is soluble in water, 500g carbon nanotube is added in graphene solution, water-bath is super at a temperature of 45 DEG C
After sound 2h, it is changed to high-speed mixer stirring 3h, resulting mixed serum is filtered, obtained powder, which is put into closed container, to be passed through
Temperature is risen to 550 DEG C, maintains 1.5h, obtain composite carbon by nitrogen.600g polyaniline is dissolved in specific solvent stir it is to be polymerized
300g mixing carbon is slowly added into solvent by object after being completely dissolved, and is slowly stirred, after graphene complete wetting, at 50 DEG C
It is carried out in water water bath sonicator 1.5 hours, obtains mixed solution with high-speed mixer stirring 1h later, mixed solution is freezed
Drying to obtain composite carbon polymer powder.The additive that the compound carbon polymer of 1000g is added to removal conductive additive is matched
Fang Zhong is produced according to positive plate production process, is assembled to obtain composite carbon conducting polymer battery.
Embodiment 2
A kind of preparation method of compound carbon polymer lead-acid battery, conductive agent when prepared by lead-acid battery in anode diachylon are
Compound carbon polymer, the compound carbon polymer are made of the raw material of following parts by weight: 480 parts of graphene, carbon nanotubes 520
Part, 30 parts of auxiliary agent, 900 parts and 15 parts of acetylacetone,2,4-pentanedione iridium of conducting polymer.Auxiliary agent is made of the raw material of following parts by weight: ethoxy
5 parts of cellulose, 10 parts of modified Nano zirconium English powder, 5 parts and 15 parts of silane coupling agent of turpentine alcohol.The preparation side of modified Nano zirconium English powder
Method are as follows: zirconium English powder is ground into the hydrogenperoxide steam generator for being put into mass fraction 72% after 2-3cm, ultrasonic vibration 10h, is taken out
2h is calcined after drying at 450 DEG C, nanometer powder is then ground into and obtains modified Nano zirconium English powder, ultrasonic power 85kw.
Compound carbon polymer the preparation method comprises the following steps:
A) 520g carbon nanotubes is added in 480g graphene powder, 4.5 times of graphene quality of second is added while stirring
Glycol, addition time are 5min, and acetylacetone,2,4-pentanedione iridium is then added, good pressure distribution processing is carried out at pressure 21000PSI, then
150 DEG C are warming up to, high-speed stirred is carried out, gained powder is added under nitrogen protection after filtering and is warming up to 300 DEG C, is obtained compound
Carbon；
B) 500g polyhenylene and 400g polyphenylene ethylene and 30g auxiliary agent are added to the second two of 3 times of quality of conducting polymer
Alcohol stirs 30min at 78 DEG C, obtains premixed liquid A；
C) graphene carbon materials are obtained after addition premixed liquid A, ultrasonic high-speed stirred 0.2h in the composite carbon obtained to step a)
The compound slurry of material；
D) by the compound slurry for the graphene carbon material that step c) is obtained be filtered freeze-drying crush obtain it is compound
Carbonaceous conductive polymer powder.Wherein, high-speed stirred is ball-milling method, and the time of high-speed stirred is 0.2h, revolving speed 5000rpm.It will
The compound carbon polymer of 1000g is added in the additive formulations of removal conductive additive, is given birth to according to positive plate production process
It produces, is assembled to obtain composite carbon conducting polymer battery.
Embodiment 3
A kind of preparation method of compound carbon polymer lead-acid battery, conductive agent when prepared by lead-acid battery in anode diachylon are
Compound carbon polymer, the compound carbon polymer are made of the raw material of following parts by weight: 500 parts of graphene, carbon nanotubes 500
Part, 40 parts of auxiliary agent, 600 parts and 18 parts of acetylacetone,2,4-pentanedione iridium of conducting polymer.Auxiliary agent is made of the raw material of following parts by weight: ethoxy
8 parts of cellulose, 12 parts of modified Nano zirconium English powder, 7 parts and 20 parts of silane coupling agent of turpentine alcohol.The preparation side of modified Nano zirconium English powder
Method are as follows: zirconium English powder is ground into the hydrogenperoxide steam generator for being put into mass fraction 76% after 2-3cm, ultrasonic vibration 11h, is taken out
2.5h is calcined after drying at 480 DEG C, nanometer powder is then ground into and obtains modified Nano zirconium English powder, ultrasonic power 88kw.
Compound carbon polymer the preparation method comprises the following steps:
A) 500g carbon nanotubes is added in 500g graphene powder, 5 times of graphene quality of second two is added while stirring
Alcohol, addition time are 9min, and 18g acetylacetone,2,4-pentanedione iridium is then added, good pressure distribution processing is carried out at pressure 21000PSI, then
180 DEG C are warming up to, high-speed stirred is carried out, gained powder under xenon protection plus is warming up to 400 DEG C after filtering, is obtained compound
Carbon；
B) 600g polyaniline and 40g auxiliary agent are added to the ethylene glycol of 3 times of quality of conducting polymer, stirred at 80 DEG C
40min obtains premixed liquid A；
C) graphene carbon material is obtained after addition premixed liquid A, ultrasonic high-speed stirred 3h in the composite carbon obtained to step a)
Compound slurry；
D) by the compound slurry for the graphene carbon material that step c) is obtained be filtered freeze-drying crush obtain it is compound
Carbonaceous conductive polymer powder.Wherein, high-speed stirred is ball-milling method or high-speed mixer paddling process, and the time of high-speed stirred is 10h,
Revolving speed is 7000rpm.The compound carbon polymer of 1000g is added in the additive formulations of removal conductive additive, according to anode
Plate production process is produced, and is assembled to obtain composite carbon conducting polymer battery.
Embodiment 4
A kind of preparation method of compound carbon polymer lead-acid battery, conductive agent when prepared by lead-acid battery in anode diachylon are
Compound carbon polymer, the compound carbon polymer are made of the raw material of following parts by weight: 650 parts of graphene, carbon nanotubes 350
Part, 50 parts of auxiliary agent, 800 parts and 20 parts of acetylacetone,2,4-pentanedione iridium of conducting polymer.Auxiliary agent is made of the raw material of following parts by weight: ethoxy
10 parts of cellulose, 15 parts of modified Nano zirconium English powder, 10 parts and 25 parts of silane coupling agent of turpentine alcohol.The preparation of modified Nano zirconium English powder
Method are as follows: zirconium English powder is ground into the hydrogenperoxide steam generator for being put into mass fraction 78% after 2-3cm, ultrasonic vibration 12h takes
3h is calcined at 500 DEG C after drying out, is then ground into nanometer powder and is obtained modified Nano zirconium English powder, ultrasonic power 90kw.
Compound carbon polymer the preparation method comprises the following steps:
A) 350g carbon nanotubes is added in 650g graphene powder, 6 times of graphene quality of second two is added while stirring
Alcohol, addition time are 10min, and 20g acetylacetone,2,4-pentanedione iridium is then added, good pressure distribution processing is carried out at pressure 21000PSI, so
After be warming up to 220 DEG C, carry out high-speed stirred, gained powder under helium protection plus be warming up to 650 DEG C after filtering, is obtained compound
Carbon；
B) 400g polythiophene and 400g polyaniline and 50g auxiliary agent are added to the ethylene glycol of 3 times of quality of conducting polymer,
60min is stirred at 80 DEG C, obtains premixed liquid A；
C) graphene carbon material is obtained after addition premixed liquid A, ultrasonic high-speed stirred 5h in the composite carbon obtained to step a)
Compound slurry；
D) it the compound slurry for the graphene carbon material that step c) is obtained is filtered drying and crushing obtains composite carbon and lead
Electric polymer powder.Wherein, high-speed stirred is ball-milling method or high-speed mixer paddling process, and the time of high-speed stirred is 20h, revolving speed
For 8000rpm.The compound carbon polymer of 1000g is added in the additive formulations of removal conductive additive, it is raw according to positive plate
It produces process to be produced, is assembled to obtain composite carbon conducting polymer battery.
Using manufactured 12V 12Ah composite carbon conducting polymer lead-acid battery of the invention, the chemical conversion time reduces
20%, 100%DOD cycle life are up to 550 times or more.By after chemical conversion battery carry out specific surface detection, specific surface with it is existing
Battery is compared and improves 15%.Capacity through detecting battery improves 10%, takes 5 groups of batteries to be dissected after circulation 350 times,
Positive being is harder, and argillization phenomenon is substantially not present.To illustrate composite carbon conducting polymer lead-acid battery energy of the invention
Electric conductivity, porosity and the battery capacity for improving positive being, extend the service life of battery.
It should be understood that those skilled in the art, can be improved or be become according to the above description
It changes, and all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (8)
1. a kind of preparation method of compound carbon polymer lead-acid battery, which is characterized in that when prepared by lead-acid battery in anode diachylon
Conductive agent be compound carbon polymer, the compound carbon polymer includes the raw material of following parts by weight: graphene 480-650
Part, 350-520 parts of carbon nanotubes；Compound carbon polymer further includes 30-50 parts of auxiliary agent, 600-900 parts of conducting polymer
With 15-20 parts of acetylacetone,2,4-pentanedione iridium, wherein the auxiliary agent is made of the raw material of following parts by weight: hydroxyethyl cellulose 5-10
Part, 10-15 parts of modified Nano zirconium English powder, 5-10 parts and silane coupling agent 15-25 parts of turpentine alcohol.
2. the preparation method of a kind of compound carbon polymer lead-acid battery according to claim 1, which is characterized in that modified
Nanometer zirconium English powder the preparation method comprises the following steps: zirconium English powder to be ground into the hydrogen peroxide for being put into mass fraction 72-78% after 2-3cm
In solution, ultrasonic vibration 10-12h calcines 2-3h after taking out drying at 450-500 DEG C, is then ground into nanometer powder and obtains
To modified Nano zirconium English powder, ultrasonic power 85-90kw.
3. the preparation method of a kind of compound carbon polymer lead-acid battery according to claim 1, which is characterized in that described
Graphene with a thickness of 1-30 layers, specific surface area 100-2600m2/ g, preparation method is redox, mechanical stripping, molten
One or more mixed methods preparation in agent removing.
4. according to claim 1 or a kind of preparation method of compound carbon polymer lead-acid battery, feature described in 2 exist
In the carbon nanotubes is single-wall carbon nanotubes, double-wall carbon nano-tube, one of multiple-wall carbon nanotube or a variety of.
5. according to claim 1 or a kind of preparation method of compound carbon polymer lead-acid battery, feature described in 2 exist
In conducting polymer is one of polyacetylene, polythiophene, polypyrrole, polyaniline, polyhenylene, polyphenylene ethylene and poly bis alkynes
Or a variety of mixing.
6. according to claim 1 or a kind of preparation method of compound carbon polymer lead-acid battery, feature described in 2 exist
In, compound carbon polymer the preparation method comprises the following steps:
A) carbon nanotubes is added in graphene powder, the ethylene glycol of 4.5-6 times of graphene quality is added while stirring, be added
Time is 5-10min, and acetylacetone,2,4-pentanedione iridium is then added, and good pressure distribution processing is carried out at pressure 21000PSI, is then heated up
To 150-220 DEG C, high-speed stirred is carried out, gained powder is added under the conditions of gas shield after filtering and is warming up to 300-650 DEG C,
Obtain composite carbon；
B) conducting polymer and auxiliary agent are added to the ethylene glycol of 3 times of quality of conducting polymer, stirred at 78-90 DEG C
30-60min obtains premixed liquid A；
C) graphene carbon is obtained after addition premixed liquid A, ultrasonic high-speed stirred 0.2-5h into the composite carbon that step a) obtains
The compound slurry of material；
D) it the compound slurry for the graphene carbon material that step c) obtains is filtered drying and crushing obtains compound carbonaceous conductive and gather
Close object powder.
7. a kind of preparation method of compound carbon polymer lead-acid battery according to claim 6, which is characterized in that high speed
Stirring is ball-milling method or high-speed mixer paddling process, and the time of high-speed stirred is 0.2-20h, revolving speed 5000-8000rpm.
8. a kind of preparation method of compound carbon polymer lead-acid battery according to claim 6, which is characterized in that step
A) protective gas is that nitrogen, helium, neon, argon gas, xenon one of are worked as in.
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| CN107068998A (en) * | 2017-03-21 | 2017-08-18 | 中国科学院福建物质结构研究所 | Battery electrode containing conducting polymer/graphene and its preparation method and application |
| CN107863521A (en) * | 2017-11-13 | 2018-03-30 | 河南超威电源有限公司 | High-activity carbon material lead-acid accumulator negative pole lead paste and preparation method thereof |
| CN108736004A (en) * | 2018-05-31 | 2018-11-02 | 深圳市瑞达电源有限公司 | A kind of anode diachylon for lead-acid accumulator |
| CN109888409A (en) * | 2019-04-03 | 2019-06-14 | 山东星火科学技术研究院 | The high-capacity lead-acid battery and its synthesis technology of a kind of graphene as additive |
| CN110061232B (en) * | 2019-05-22 | 2020-10-27 | 江西丰日电源有限公司 | Lead-acid storage battery positive electrode material and preparation method thereof |
| CN116525177B (en) * | 2023-05-29 | 2024-03-19 | 盐城工学院 | Graphene conductive agent for lithium ion battery and preparation method thereof |
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