CN112876844A - Polyaniline battery film and preparation method thereof - Google Patents

Polyaniline battery film and preparation method thereof Download PDF

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Publication number
CN112876844A
CN112876844A CN202110203634.7A CN202110203634A CN112876844A CN 112876844 A CN112876844 A CN 112876844A CN 202110203634 A CN202110203634 A CN 202110203634A CN 112876844 A CN112876844 A CN 112876844A
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parts
temperature
stirring
emulsion
dispersion liquid
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王凯
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
    • H01M4/602—Polymers
    • H01M4/606—Polymers containing aromatic main chain polymers
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/08—Cellulose derivatives
    • C08J2401/26—Cellulose ethers
    • C08J2401/28—Alkyl ethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
    • C08J2491/06—Waxes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02—Organic and inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a polyaniline battery film, which is composed of the following raw materials in parts by weight: 60-80 parts of aniline, 2-3 parts of ammonium persulfate, 40-50 parts of graphene nanosheets, 3-5 parts of hydroxyethylidene diphosphonic acid, 2-4 parts of dimethylaminopropylamine and 30-50 parts of compatilizer emulsion. Compared with the traditional method of directly mixing polyaniline and graphene sheets, the method has the advantages of better bonding strength, higher specific capacitance and better conductivity.

Description

Polyaniline battery film and preparation method thereof
Technical Field
The invention belongs to the field of thin film materials, and particularly relates to a polyaniline battery thin film.
Background
The electric activity of the polyaniline is derived from a P electron conjugated structure in a molecular chain, wherein a valence band and a conduction band are respectively formed in a P bonding state and a P-reversed bonding state along with the enlargement of a P electron system in the molecular chain, and the non-localized P electron conjugated structure can be doped to form a P type and an N type conduction state. Unlike other conducting polymer doping mechanism to produce cationic vacancy under the action of oxidant, the electron number of polyaniline is not changed during doping, but rather the doped protonic acid is decomposed to produce H + and anions, such as Cl-, sulfate radical, phosphate radical, etc. to enter the main chain and combine with N atom in amine and imine radical to form polar and bipolar ion delocalized in the P bond of the whole molecular chain, so that polyaniline has relatively high conductivity. The unique doping mechanism enables the doping and de-doping of the polyaniline to be completely reversible, the doping degree is influenced by factors such as pH value, potential and the like, and is expressed as corresponding change of appearance color, and the polyaniline also has electrochemical activity and electrochromic property;
at present, a battery thin film product compounded by polyaniline and graphene sheets exists, but the electric performance is weak due to poor compatibility of polyaniline and graphene and low stability of a finished product.
Disclosure of Invention
The invention aims to provide a polyaniline battery film and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a polyaniline battery film is composed of the following raw materials in parts by weight:
60-80 parts of aniline, 2-3 parts of ammonium persulfate, 40-50 parts of graphene nanosheets, 3-5 parts of hydroxyethylidene diphosphonic acid, 2-4 parts of dimethylaminopropylamine and 30-50 parts of compatilizer emulsion.
The compatilizer emulsion is composed of the following raw materials in parts by weight:
5-7 parts of palm wax, 2-3 parts of trimethylolpropane, 1-4 parts of stearic acid, 0.1-0.2 part of p-methylbenzenesulfonic acid, 1-2 parts of alkanolamide, 5-7 parts of hydroxyethyl cellulose and sp-800.1-0.3 part of the mixture.
The preparation method of the compatilizer emulsion comprises the following steps:
(1) adding carnauba wax into absolute ethyl alcohol with the weight 15-20 times of the carnauba wax, raising the temperature to 70-76 ℃, and keeping the temperature and stirring for 30-40 minutes to obtain alcohol emulsion;
(2) adding hydroxyethyl cellulose into deionized water with the weight of 80-100 times of that of the hydroxyethyl cellulose, and uniformly stirring to obtain a fiber dispersion liquid;
(3) mixing the alcohol emulsion and the fiber dispersion liquid, stirring uniformly, adding alkanolamide, and performing ultrasonic treatment for 3-10 minutes to obtain a mixed dispersion liquid;
(4) and adding trimethylolpropane into the mixed dispersion liquid, uniformly stirring, feeding into a reaction kettle, adding stearic acid and p-toluenesulfonic acid, adjusting the temperature of the reaction kettle to 95-98 ℃, keeping the temperature and stirring for 2-3 hours, discharging, cooling, adding sp-80, and uniformly stirring to obtain the compatilizer emulsion.
A preparation method of a polyaniline battery film comprises the following steps:
(1) mixing hydroxyethylidene diphosphonic acid and aniline, adding the mixture into deionized water with the weight being 20-30 times of that of the mixture, and uniformly stirring to obtain aniline dispersion liquid;
(2) adding graphene nanosheets into the compatilizer emulsion, adding aniline dispersion liquid, introducing nitrogen, adding ammonium persulfate, stirring and reacting for 10-17 hours at the temperature of 5-20 ℃, adding dimethylaminopropylamine, raising the temperature to 70-75 ℃, keeping the temperature and stirring for 40-50 minutes, performing suction filtration, washing filter cakes with water, and performing vacuum drying to obtain the graphene nano-sheets.
The temperature of the vacuum drying is 80-85 ℃.
The invention has the advantages that:
the graphene nano-sheet is used as a base material, then the base material is added into an aniline monomer solution, polymerization is carried out under the action of an initiator, polymerized polyaniline can be well deposited on the surface of a graphene sheet through a compatilizer, and a stable battery film is formed.
Detailed Description
Example 1
A polyaniline battery film is composed of the following raw materials in parts by weight:
aniline 60, ammonium persulfate 2, graphene nanosheets 40, hydroxyethylidene diphosphonic acid 3, dimethylaminopropylamine 2 and a compatilizer emulsion 30.
The compatilizer emulsion is composed of the following raw materials in parts by weight:
5 parts of palm wax, 2 parts of trimethylolpropane, 1 part of stearic acid, 0.1 part of p-methylbenzenesulfonic acid, 1 part of alkanolamide, 5 parts of hydroxyethyl cellulose and sp-800.1 parts of the raw materials.
The preparation method of the compatilizer emulsion comprises the following steps:
(1) adding carnauba wax into absolute ethyl alcohol 15 times of the carnauba wax, raising the temperature to 70 ℃, and stirring for 30 minutes under the condition of heat preservation to obtain alcohol emulsion;
(2) adding hydroxyethyl cellulose into deionized water with the weight being 80 times of that of the hydroxyethyl cellulose, and uniformly stirring to obtain a fiber dispersion liquid;
(3) mixing the alcohol emulsion and the fiber dispersion liquid, stirring uniformly, adding alkanolamide, and performing ultrasonic treatment for 3 minutes to obtain a mixed dispersion liquid;
(4) and adding trimethylolpropane into the mixed dispersion liquid, uniformly stirring, feeding into a reaction kettle, adding stearic acid and p-toluenesulfonic acid, adjusting the temperature of the reaction kettle to 95 ℃, keeping the temperature, stirring for 2 hours, discharging, cooling, adding sp-80, and uniformly stirring to obtain the compatilizer emulsion.
A preparation method of a polyaniline battery film comprises the following steps:
(1) mixing hydroxyethylidene diphosphonic acid and aniline, adding the mixture into deionized water with the weight being 20 times of that of the mixture, and uniformly stirring to obtain aniline dispersion liquid;
(2) adding graphene nanosheets into the compatilizer emulsion, adding aniline dispersion liquid, introducing nitrogen, adding ammonium persulfate, stirring and reacting for 10 hours at the temperature of 5 ℃, adding dimethylaminopropylamine, raising the temperature to 70 ℃, keeping the temperature and stirring for 40 minutes, performing suction filtration, washing filter cakes with water, and performing vacuum drying to obtain the graphene nano-particles.
The temperature of the vacuum drying was 80 ℃.
Example 2
A polyaniline battery film is composed of the following raw materials in parts by weight:
80 parts of aniline, 3 parts of ammonium persulfate, 50 parts of graphene nanosheets, 5 parts of hydroxyethylidene diphosphonic acid, 4 parts of dimethylaminopropylamine and 50 parts of compatilizer emulsion.
The compatilizer emulsion is composed of the following raw materials in parts by weight:
palm wax 7, trimethylolpropane 3, stearic acid 4, p-toluenesulfonic acid 0.2, alkanolamide 2, hydroxyethyl cellulose 7, sp-800.3.
The preparation method of the compatilizer emulsion comprises the following steps:
(1) adding carnauba wax into absolute ethyl alcohol with the weight 20 times of that of the carnauba wax, raising the temperature to 70-76 ℃, and keeping the temperature and stirring for 40 minutes to obtain alcohol emulsion;
(2) adding hydroxyethyl cellulose into deionized water with the weight of 100 times of that of the hydroxyethyl cellulose, and uniformly stirring to obtain a fiber dispersion liquid;
(3) mixing the alcohol emulsion and the fiber dispersion liquid, stirring uniformly, adding alkanolamide, and performing ultrasonic treatment for 10 minutes to obtain a mixed dispersion liquid;
(4) and adding trimethylolpropane into the mixed dispersion liquid, uniformly stirring, feeding into a reaction kettle, adding stearic acid and p-toluenesulfonic acid, adjusting the temperature of the reaction kettle to 98 ℃, keeping the temperature, stirring for 3 hours, discharging, cooling, adding sp-80, and uniformly stirring to obtain the compatilizer emulsion.
A preparation method of a polyaniline battery film comprises the following steps:
(1) mixing hydroxyethylidene diphosphonic acid and aniline, adding the mixture into deionized water with the weight 30 times that of the mixture, and uniformly stirring to obtain aniline dispersion liquid;
(2) adding graphene nanosheets into the compatilizer emulsion, adding aniline dispersion liquid, introducing nitrogen, adding ammonium persulfate, stirring and reacting for 17 hours at the temperature of 20 ℃, adding dimethylaminopropylamine, raising the temperature to 75 ℃, keeping the temperature and stirring for 50 minutes, performing suction filtration, washing filter cakes with water, and performing vacuum drying to obtain the graphene nano-particles.
The temperature of the vacuum drying was 85 ℃.
Comparative example 1
A polyaniline battery film is composed of the following raw materials in parts by weight:
60 parts of aniline, 2 parts of ammonium persulfate, 40 parts of graphene nanosheets, 3 parts of hydroxyethylidene diphosphonic acid and 2 parts of dimethylaminopropylamine.
A preparation method of a polyaniline battery film comprises the following steps:
(1) mixing hydroxyethylidene diphosphonic acid and aniline, adding the mixture into deionized water with the weight being 20 times of that of the mixture, and uniformly stirring to obtain aniline dispersion liquid;
(2) adding aniline dispersion into graphene nanosheets, introducing nitrogen, adding ammonium persulfate, stirring and reacting for 10 hours at 5 ℃, adding dimethylaminopropylamine, raising the temperature to 70 ℃, keeping the temperature and stirring for 40 minutes, performing suction filtration, washing filter cakes with water, and performing vacuum drying to obtain the graphene nanosheets.
The temperature of the vacuum drying was 80 ℃.
And (3) performance testing:
the specific capacitance of the composite material is tested at normal temperature by adopting a cyclic voltammetry method, wherein a working electrode is a film modified electrode, a spreading auxiliary electrode is a platinum wire, a reference electrode is a saturated calomel electrode, an electrolyte is a 1mol/L nitric acid solution, and the test results are as follows:
item Specific capacitance (F/g)
Film of example 1 of the invention 399
Film of example 2 of the invention 407
Film of comparative example 1 211
Pure graphene 183

Claims (5)

1. A polyaniline battery film is characterized by comprising the following raw materials in parts by weight:
60-80 parts of aniline, 2-3 parts of ammonium persulfate, 40-50 parts of graphene nanosheets, 3-5 parts of hydroxyethylidene diphosphonic acid, 2-4 parts of dimethylaminopropylamine and 30-50 parts of compatilizer emulsion.
2. The polyaniline cell film as claimed in claim 1, wherein the compatibilizer emulsion is composed of the following raw materials in parts by weight:
5-7 parts of palm wax, 2-3 parts of trimethylolpropane, 1-4 parts of stearic acid, 0.1-0.2 part of p-methylbenzenesulfonic acid, 1-2 parts of alkanolamide, 5-7 parts of hydroxyethyl cellulose and sp-800.1-0.3 part of the mixture.
3. The polyaniline cell membrane as claimed in claim 2, wherein the method for preparing the compatibilizer emulsion comprises the following steps:
(1) adding carnauba wax into absolute ethyl alcohol with the weight 15-20 times of the carnauba wax, raising the temperature to 70-76 ℃, and keeping the temperature and stirring for 30-40 minutes to obtain alcohol emulsion;
(2) adding hydroxyethyl cellulose into deionized water with the weight of 80-100 times of that of the hydroxyethyl cellulose, and uniformly stirring to obtain a fiber dispersion liquid;
(3) mixing the alcohol emulsion and the fiber dispersion liquid, stirring uniformly, adding alkanolamide, and performing ultrasonic treatment for 3-10 minutes to obtain a mixed dispersion liquid;
(4) and adding trimethylolpropane into the mixed dispersion liquid, uniformly stirring, feeding into a reaction kettle, adding stearic acid and p-toluenesulfonic acid, adjusting the temperature of the reaction kettle to 95-98 ℃, keeping the temperature and stirring for 2-3 hours, discharging, cooling, adding sp-80, and uniformly stirring to obtain the compatilizer emulsion.
4. The method for preparing the polyaniline cell film as described in claim 1, comprising the steps of:
(1) mixing hydroxyethylidene diphosphonic acid and aniline, adding the mixture into deionized water with the weight being 20-30 times of that of the mixture, and uniformly stirring to obtain aniline dispersion liquid;
(2) adding graphene nanosheets into the compatilizer emulsion, adding aniline dispersion liquid, introducing nitrogen, adding ammonium persulfate, stirring and reacting for 10-17 hours at the temperature of 5-20 ℃, adding dimethylaminopropylamine, raising the temperature to 70-75 ℃, keeping the temperature and stirring for 40-50 minutes, performing suction filtration, washing filter cakes with water, and performing vacuum drying to obtain the graphene nano-sheets.
5. The method for preparing the polyaniline cell film as claimed in claim 4, wherein the temperature of the vacuum drying is 80-85 ℃.
CN202110203634.7A 2021-02-24 2021-02-24 Polyaniline battery film and preparation method thereof Withdrawn CN112876844A (en)

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Application Number Priority Date Filing Date Title
CN202110203634.7A CN112876844A (en) 2021-02-24 2021-02-24 Polyaniline battery film and preparation method thereof

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