CN110335761B - Carbon-based polyaniline composite material and preparation method and application thereof - Google Patents

Carbon-based polyaniline composite material and preparation method and application thereof Download PDF

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CN110335761B
CN110335761B CN201910480612.8A CN201910480612A CN110335761B CN 110335761 B CN110335761 B CN 110335761B CN 201910480612 A CN201910480612 A CN 201910480612A CN 110335761 B CN110335761 B CN 110335761B
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aniline
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polyaniline composite
batteries
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闵永刚
刘荣涛
王勇
刘屹东
廖松义
张诗洋
庞贻宇
肖天华
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Guangdong University of Technology
Dongguan South China Design and Innovation Institute
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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    • H—ELECTRICITY
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    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
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    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • H—ELECTRICITY
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • 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
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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
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    • H01M4/02—Electrodes composed of, or comprising, active material
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    • 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
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    • Y02E60/10—Energy storage using batteries
    • 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
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Abstract

The invention belongs to the field of new energy device electrodes, and discloses a carbon-based polyaniline composite material and a preparation method and application thereof. The carbon-based polyaniline composite material is prepared by adding a carboxylated carbon-based material and an aniline oligomer into an organic solvent according to a certain proportion under an inert atmosphere, uniformly stirring, adding a catalyst lipase at 30-80 ℃ for reaction, filtering, washing and drying. The carbon-based polyaniline composite material has the characteristics of high specific surface area, large porosity, high energy density, good cycling stability, certain temperature resistance, simple preparation method and the like when being used as a primary battery or super capacitor electrode, and can be applied to the field of super capacitors or secondary batteries.

Description

Carbon-based polyaniline composite material and preparation method and application thereof
Technical Field
The invention belongs to the field of new energy device electrodes, and particularly relates to a carbon-based polyaniline composite material and a preparation method and application thereof.
Background
Secondary battery materials and supercapacitors are two important directions in the field of new energy. The super capacitor can realize a rapid charging and discharging process in a short time, has good cycle stability, but has low energy density to limit development and application; a representative lithium ion battery as a secondary battery has a high energy density and can release a large amount of energy, but its charge and discharge mechanism and process limit its continuity in rapid charge and discharge. Therefore, it is a hot spot of current research to find an electrode that can satisfy both fast charge and discharge and have huge energy density.
The carbon-based material represented by graphene has a large spatial structure and excellent photoelectric properties, and is successfully applied to the electrode of the secondary battery material, so that various properties of the secondary battery material are improved to a certain extent. Polyaniline material is used as a conductive polymer material, and is not popular in application to super capacitor electrodes in recent years. But neither addresses the above-mentioned critical issues. Therefore, the two materials are considered to be combined to exert respective advantages, and the novel electrode formed by more efficiently using has huge application prospect and potential.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention mainly aims to provide a carbon-based polyaniline composite material. The composite material has the advantages of high specific surface area, large porosity, large energy density, good circulation stability and capability of resisting a certain temperature (20-80 ℃), and is a novel energy electrode.
The invention also aims to provide a preparation method of the carbon-based polyaniline composite material.
The invention further aims to provide application of the carbon-based polyaniline composite material.
The purpose of the invention is realized by the following technical scheme:
a carbon-based polyaniline composite material is prepared by adding a carboxylated carbon-based material and an aniline oligomer into an organic solvent, uniformly stirring, and performing ultrasonic oscillation; adding a lipase catalyst at 30-80 ℃ in an inert atmosphere for reaction, and filtering, washing and drying the mixture to obtain the lipase catalyst.
Preferably, the inert atmosphere is nitrogen, argon or helium.
Preferably, the carbon-based material in the carboxylated carbon-based material is more than one of fullerene, graphene oxide, carbon nanotube, carbon nanohorn or graphene quantum dot.
Preferably, the aniline oligomer is aniline trimer, aniline tetramer, aniline pentamer, aniline hexamer, aniline heptamer or aniline octamer.
Preferably, the organic solvent is one or more of ethanol, diethyl ether, acetone, dichloromethane, chloroform, carbon disulfide, toluene, tetrahydrofuran, N-dimethylformamide, benzoic acid, or N-methylpyrrolidone.
Preferably, the mass ratio of the carboxylated carbon-based material to the aniline oligomer is (1-100): 1.
preferably, the lipase catalyst is 0.1-10 wt% of the mass of the aniline oligomer.
The preparation method of the carbon-based polyaniline composite material comprises the following specific steps:
s1, adding a carbon-based material with carboxyl and an aniline oligomer into an organic solvent, uniformly stirring, and performing ultrasonic oscillation to generate an aniline oligomer-carbon-based material mixed solution;
and S2, adding a lipase catalyst at 30-80 ℃ under the condition of inert gas for reaction, stirring, washing with deionized water after the reaction is finished, and performing vacuum drying treatment to obtain the carbon-based polyaniline composite material.
The carbon-based polyaniline composite material is applied to the field of super capacitors or secondary batteries.
Preferably, the secondary battery is a lithium ion battery, a sodium ion battery, a lithium polymer battery, a nickel hydrogen battery, a nickel cadmium battery, or a lead storage battery.
The lipase of the invention is an enzyme with a plurality of catalytic capacities, can exert different activities in different reaction systems, promotes ester hydrolysis at an oil-water interface, and can carry out enzymatic synthesis, ester exchange and amidation in an organic phase. Under the dispersion action of an organic solvent, the carbon-based material with carboxyl and aniline oligomer are subjected to amidation reaction on the surface of lipase, the lipase has specific catalytic activity, amide bonds (-NH-CO-) are formed between layers of the carbon-based material, the distance between the layers of the carbon-based material is increased, metal ions can pass through the carbon-based material quickly, and electrons can be transferred through the amide bonds by the carbon-based material, so that the overall conductivity and volume expansibility of the electrode material are increased. By the chain initiation and chain growth reaction, the reaction conditions in the whole process are mild, and the efficiency is high. The reaction process is shown as formula (1):
Figure BDA0002083719520000021
compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, a lipase catalyst is added into a blending system of a carboxylated carbon-based material and an aniline oligomer to synthesize the new energy electrode which has the advantages of high specific surface area, large porosity, high energy density, good circulation stability and certain temperature resistance.
2. The method adopts lipase for catalysis, has high efficiency, is stable and continuous, and can bond the carboxylated carbon-based material and the aniline oligomer more efficiently through amido bond.
3. The preparation method is simple, and the conductivity and the volume expansibility of the electrode material can be enhanced by increasing the distance between layers of the carbon-based material.
Drawings
Fig. 1 shows the structure of the carbon-based polyaniline composite material of the present invention.
FIG. 2 is a schematic diagram of the reaction process of carboxylated graphene and aniline oligomer under the catalysis of lipase.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention.
Example 1
1. Dissolving 0.8g of carboxylated graphene oxide and 0.8g of aniline trimer in 100ml of DMF, stirring and mixing for 0.5h, and ultrasonically oscillating for 20 min;
2. in N2And adding 0.1g of lipase into the solution at the temperature of 30 ℃ for reaction for 10 hours, washing the solution clean by using deionized water after the reaction is finished, and drying the solution for 24 hours in a vacuum drying oven at the temperature of 50 ℃ to obtain the graphene aniline trimer composite material.
The obtained graphene aniline trimer composite material is prepared into a lithium ion battery cathode material, the cycle stability is improved by 50% compared with that of a common lithium ion battery, and the energy density of 85% can be still maintained after 100 times of charge and discharge.
Example 2
1. Dissolving 1.6g of carboxylated carbon nano tube and 1.0g of aniline pentamer in 150ml of toluene, stirring and mixing for 0.5h, and then carrying out ultrasonic oscillation for 0.5 h;
2. and adding 0.08g of lipase into the solution at the temperature of 30 ℃ for reaction for 8h at Ar, washing the solution clean with deionized water after the reaction is finished, and drying the solution for 24h at the temperature of 60 ℃ in a vacuum drying oven to obtain the carbon nano tube aniline pentamer composite material.
The obtained carbon nano tube aniline pentamer composite material is prepared into a super capacitor electrode, the window voltage is improved by 22.4%, and the specific capacitance is improved by 38.7%.
Example 3
1. Dissolving 2.5g of carboxylated carbon nanohorns and 0.5g of aniline tetramers in 200ml of dichloromethane, stirring and mixing for 0.5h, and then carrying out ultrasonic oscillation for 30 min;
2. in N2And adding 0.5g of lipase into the solution at 50 ℃ for reaction for 10h, washing the solution clean by using deionized water after the reaction is finished, and drying the solution in a vacuum drying oven at 50 ℃ for 24h to obtain the carbon nanohorn aniline tetramer composite material.
The obtained carbon nanohorn aniline tetramer composite material is prepared into a sodium ion battery cathode material, the cycle stability is improved by 30 percent compared with that of a common sodium ion battery, and 80 percent of energy density can be still maintained after 100 times of charge and discharge.
Example 4
1. Dissolving 5g of carboxylated graphene quantum dots and 0.5g of aniline octamer in 350ml of N, N-dimethylformamide, stirring and mixing for 0.5h, and then carrying out ultrasonic oscillation for 0.5 h;
2. and adding 0.08g of lipase into the solution at the temperature of 70 ℃ for reaction for 12h at Ar, washing the solution clean with deionized water after the reaction is finished, and drying the solution for 24h at the temperature of 60 ℃ in a vacuum drying oven to obtain the graphene quantum dot aniline octamer composite material.
The obtained graphene quantum dot aniline octamer composite material is prepared into a nickel-metal hydride battery cathode material, the cycle stability is improved by 28% compared with that of a common nickel-metal hydride battery, and the energy density of 86% can be still maintained after 100 times of charge and discharge.
Fig. 1 is a structural formula of the carbon-based polyaniline composite material of the present invention. FIG. 2 is a schematic diagram of the reaction process of carboxylated graphene and aniline oligomer under the catalysis of lipase. Wherein a is graphene, b is carboxylic acid graphene, c is amino-terminated aniline tetramer, and d is graphene aniline oligomer compound; the process is characterized in that the carboxylation is performed, the reaction condition is that lipase is used as a catalyst, and the temperature is 30-80 ℃ under an organic solvent. As can be seen from fig. 1 and 2, under the catalytic action of lipase, the aniline tetramer terminated by the amino group can increase the distance between graphene layers, and the multilayer graphite is connected with the aniline tetramer through the amide bond, so that the conductivity and specific capacitance of the graphene are increased, and the improvement of the access passage of the metal ions of the secondary battery and the enhancement of the environmental stability of the supercapacitor are facilitated.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.

Claims (6)

1. A carbon-based polyaniline composite material is characterized in that a carboxylated carbon-based material and an aniline oligomer are added into an organic solvent and uniformly stirred, and ultrasonic oscillation is carried out; adding a lipase catalyst at 30-80 ℃ in an inert atmosphere for reaction, and filtering, washing and drying the mixture to obtain the lipase catalyst; the carbon-based material in the carboxylated carbon-based material is more than one of fullerene, graphene oxide, carbon nano tube or carbon nanohorn; the aniline oligomer is aniline tripolymer, aniline tetramer, aniline pentamer, aniline hexamer, aniline heptamer or aniline octamer; the mass ratio of the carboxylated carbon-based material to the aniline oligomer is (1-100): 1; the lipase catalyst is 0.1-10 wt% of the mass of the aniline oligomer; the carbon-based polyaniline composite material is of a layered structure.
2. The carbon-based polyaniline composite material as described in claim 1, wherein the inert atmosphere is nitrogen, argon, or helium.
3. The carbon-based polyaniline composite material as described in claim 1, wherein the organic solvent is one or more of ethanol, diethyl ether, acetone, dichloromethane, chloroform, carbon disulfide, toluene, tetrahydrofuran, N-dimethylformamide, benzoic acid, and N-methylpyrrolidone.
4. The method for preparing a carbon-based polyaniline composite as described in any one of claims 1 to 3, comprising the following specific steps:
s1, adding the carbon-based material with the carboxyl and the aniline oligomer into an organic solvent, uniformly stirring, and performing ultrasonic oscillation to generate an aniline oligomer-carbon-based material mixed solution;
and S2, adding a lipase catalyst at 30-80 ℃ under the inert gas condition for reaction, stirring, washing with deionized water after the reaction is finished, and performing vacuum drying treatment to obtain the carbon-based polyaniline composite material.
5. Use of the carbon-based polyaniline composite as defined in any one of claims 1 to 3 in the field of supercapacitors or secondary batteries.
6. The use of the carbon-based polyaniline composite material as described in claim 5, in the field of supercapacitors or secondary batteries, wherein the secondary batteries are lithium ion batteries, sodium ion batteries, lithium polymer batteries, nickel hydrogen batteries, nickel cadmium batteries, or lead storage batteries.
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