CN111933947A - Polypyrrole battery conductive additive and preparation method thereof - Google Patents
Polypyrrole battery conductive additive and preparation method thereof Download PDFInfo
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- CN111933947A CN111933947A CN202010821832.5A CN202010821832A CN111933947A CN 111933947 A CN111933947 A CN 111933947A CN 202010821832 A CN202010821832 A CN 202010821832A CN 111933947 A CN111933947 A CN 111933947A
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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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
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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
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- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a polypyrrole battery conductive additive, which is prepared from the following raw materials in parts by weight: pyrrole 130, dicumyl peroxide 5, 2-mercaptobenzimidazole 1, hydroxy ethylidene diphosphonic acid 2, pentaerythritol 3, acetylene carbon black 1, ethoxylated ammonium alkyl phenol sulfate 0.8, sucrose acetate isobutyrate 1, zinc stearate 0.1 and stannous octoate 0.1.
Description
The application is a divisional application of a patent with the application date of 2018, 5 and 4, the application number of 201810417880.0 and the invention name of polypyrrole battery conductive additive and a preparation method thereof.
Technical Field
The invention belongs to the field of conductive materials, and particularly relates to a polypyrrole battery conductive additive and a preparation method thereof.
Background
The conductive additive is one of indispensable key materials of the lithium ion battery, and particularly has very important function in the large-current charging and discharging process of the power lithium ion battery. Different conductive agents have respective characteristics and forms of different conductive agents are different; the conductive agents widely used by the current battery can be divided into three main types of conductive carbon black, conductive graphite, novel conductive agents and the like, the novel conductive agents mainly refer to carbon nano tubes, graphene and the like, and polypyrrole is used as a conductive polymer and has good conductive stability, but the application of the polypyrrole in the field of the battery is low, so that the purpose of the invention is to provide a novel battery additive which is strong in conductivity, good in mechanical property and high in conductive stability.
Disclosure of Invention
The invention aims to provide a polypyrrole battery conductive additive and a preparation method thereof, aiming at the defects and shortcomings of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a polypyrrole battery conductive additive is composed of the following raw materials in parts by weight:
pyrrole 130, dicumyl peroxide 5, 2-mercaptobenzimidazole 1, hydroxyethylidene diphosphonic acid 2, pentaerythritol 3, acetylene black 1, ethoxylated ammonium alkyl phenol sulfate 0.8, sucrose acetate isobutyrate 1, zinc stearate 0.1 and stannous octoate 0.1.
A preparation method of a polypyrrole battery conductive additive comprises the following steps:
(1) mixing acetylene black and ethoxylated ammonium alkylphenol sulfate, adding the mixture into deionized water with the weight of 25 times of that of the mixture, carrying out ultrasonic treatment for 10 minutes, raising the temperature to 60 ℃, adding zinc stearate, and carrying out heat preservation and stirring for 1 hour to obtain an activated carbon black dispersion liquid;
(2) adding 2-mercaptobenzimidazole into absolute ethyl alcohol with the weight 7-9 times of that of the 2-mercaptobenzimidazole, uniformly stirring, mixing with pentaerythritol, and uniformly stirring to obtain a composite alcohol solution;
(3) mixing the activated carbon black dispersion and the composite alcohol solution, uniformly stirring, adding hydroxyethylidene diphosphonic acid, raising the temperature to 90 ℃, keeping the temperature and stirring for 1 hour, adding sucrose acetate isobutyrate, and stirring to normal temperature to obtain an ester dispersion;
(4) adding dicumyl peroxide into 10 times of absolute ethyl alcohol by weight, and uniformly stirring to obtain an initiator solution;
(5) adding pyrrole into the ester dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 65 ℃, adding the initiator solution, keeping the temperature and stirring for 4 hours, discharging and cooling to obtain carbon black modified polypyrrole dispersion liquid;
(6) adding stannous octoate into the carbon black modified polypyrrole dispersion liquid, uniformly stirring, raising the temperature to 80 ℃, keeping the temperature and stirring for 20 minutes, filtering, washing the precipitate with water, drying for 1 hour at 55 ℃ in vacuum, and cooling to normal temperature to obtain the polypyrrole battery conductive additive.
The invention has the advantages that:
the acetylene black is used as a conductive raw material, treated by stearate, dispersed into an aqueous solution of ethoxylated ammonium alkylphenol sulfate, taken as a solvent, added with hydroxy ethylidene diphosphonic acid and alcohol for blending esterification, and then taken as a monomer, dispersed in the esterified solution and polymerized under the action of an initiator, so that the dispersion compatibility of the carbon black among polypyrrole is effectively improved, and the mechanical stability and the conductive stability of a finished material are improved.
Detailed Description
Example 1
A polypyrrole battery conductive additive is composed of the following raw materials in parts by weight:
pyrrole 130, dicumyl peroxide 5, 2-mercaptobenzimidazole 1, hydroxyethylidene diphosphonic acid 2, pentaerythritol 3, acetylene black 1, ethoxylated ammonium alkyl phenol sulfate 0.8, sucrose acetate isobutyrate 1, zinc stearate 0.1 and stannous octoate 0.1.
A preparation method of a polypyrrole battery conductive additive comprises the following steps:
(1) mixing acetylene black and ethoxylated ammonium alkylphenol sulfate, adding the mixture into deionized water with the weight of 25 times of that of the mixture, carrying out ultrasonic treatment for 10 minutes, raising the temperature to 60 ℃, adding zinc stearate, and carrying out heat preservation and stirring for 1 hour to obtain an activated carbon black dispersion liquid;
(2) adding 2-mercaptobenzimidazole into absolute ethyl alcohol with the weight 7-9 times of that of the 2-mercaptobenzimidazole, uniformly stirring, mixing with pentaerythritol, and uniformly stirring to obtain a composite alcohol solution;
(3) mixing the activated carbon black dispersion and the composite alcohol solution, uniformly stirring, adding hydroxyethylidene diphosphonic acid, raising the temperature to 90 ℃, keeping the temperature and stirring for 1 hour, adding sucrose acetate isobutyrate, and stirring to normal temperature to obtain an ester dispersion;
(4) adding dicumyl peroxide into 10 times of absolute ethyl alcohol by weight, and uniformly stirring to obtain an initiator solution;
(5) adding pyrrole into the ester dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 65 ℃, adding the initiator solution, keeping the temperature and stirring for 4 hours, discharging and cooling to obtain carbon black modified polypyrrole dispersion liquid;
(6) adding stannous octoate into the carbon black modified polypyrrole dispersion liquid, uniformly stirring, raising the temperature to 80 ℃, keeping the temperature and stirring for 20 minutes, filtering, washing the precipitate with water, drying for 1 hour at 55 ℃ in vacuum, and cooling to normal temperature to obtain the polypyrrole battery conductive additive.
Example 2
A polypyrrole battery conductive additive is composed of the following raw materials in parts by weight:
pyrrole 110, dicumyl peroxide 3, 2-mercaptobenzimidazole 0.6, hydroxyethylidene diphosphonic acid 2, pentaerythritol 3, acetylene black 1, ethoxylated ammonium alkyl phenol sulfate 0.8, sucrose acetate isobutyrate 1, zinc stearate 0.1 and stannous octoate 0.1.
A preparation method of a polypyrrole battery conductive additive comprises the following steps:
(1) mixing acetylene black and ethoxylated ammonium alkylphenol sulfate, adding the mixture into deionized water with the weight of 25 times of that of the mixture, carrying out ultrasonic treatment for 10 minutes, raising the temperature to 60 ℃, adding zinc stearate, and carrying out heat preservation and stirring for 1 hour to obtain an activated carbon black dispersion liquid;
(2) adding 2-mercaptobenzimidazole into absolute ethyl alcohol with the weight 7 times of that of the 2-mercaptobenzimidazole, uniformly stirring, mixing with pentaerythritol, and uniformly stirring to obtain a composite alcohol solution;
(3) mixing the activated carbon black dispersion and the composite alcohol solution, uniformly stirring, adding hydroxyethylidene diphosphonic acid, raising the temperature to 90 ℃, keeping the temperature and stirring for 1 hour, adding sucrose acetate isobutyrate, and stirring to normal temperature to obtain an ester dispersion;
(4) adding dicumyl peroxide into 10 times of absolute ethyl alcohol by weight, and uniformly stirring to obtain an initiator solution;
(5) adding pyrrole into the ester dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 65 ℃, adding the initiator solution, keeping the temperature and stirring for 4 hours, discharging and cooling to obtain carbon black modified polypyrrole dispersion liquid;
(6) adding stannous octoate into the carbon black modified polypyrrole dispersion liquid, uniformly stirring, raising the temperature to 80 ℃, keeping the temperature and stirring for 20 minutes, filtering, washing the precipitate with water, drying for 1 hour at 55 ℃ in vacuum, and cooling to normal temperature to obtain the polypyrrole battery conductive additive.
And (3) performance testing:
the polypyrrole battery conductive additive is subjected to charge and discharge tests, and the specific capacitance under the charge and discharge condition of 0.2A/g is 195.5-199.2F/g; the tensile strength is 163.3-172.7 MPa.
Claims (1)
1. The polypyrrole battery conductive additive is characterized by being composed of the following raw materials in parts by weight:
pyrrole 130, dicumyl peroxide 5, 2-mercaptobenzimidazole 1, hydroxyethylidene diphosphonic acid 2, pentaerythritol 3, acetylene black 1, ethoxylated ammonium alkyl phenol sulfate 0.8, sucrose acetate isobutyrate 1, zinc stearate 0.1 and stannous octoate 0.1.
A preparation method of a polypyrrole battery conductive additive comprises the following steps:
(1) mixing acetylene black and ethoxylated ammonium alkylphenol sulfate, adding the mixture into deionized water with the weight of 25 times of that of the mixture, carrying out ultrasonic treatment for 10 minutes, raising the temperature to 60 ℃, adding zinc stearate, and carrying out heat preservation and stirring for 1 hour to obtain an activated carbon black dispersion liquid;
(2) adding 2-mercaptobenzimidazole into absolute ethyl alcohol with the weight 7-9 times of that of the 2-mercaptobenzimidazole, uniformly stirring, mixing with pentaerythritol, and uniformly stirring to obtain a composite alcohol solution;
(3) mixing the activated carbon black dispersion and the composite alcohol solution, uniformly stirring, adding hydroxyethylidene diphosphonic acid, raising the temperature to 90 ℃, keeping the temperature and stirring for 1 hour, adding sucrose acetate isobutyrate, and stirring to normal temperature to obtain an ester dispersion;
(4) adding dicumyl peroxide into 10 times of absolute ethyl alcohol by weight, and uniformly stirring to obtain an initiator solution;
(5) adding pyrrole into the ester dispersion liquid, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 65 ℃, adding the initiator solution, keeping the temperature and stirring for 4 hours, discharging and cooling to obtain carbon black modified polypyrrole dispersion liquid;
(6) adding stannous octoate into the carbon black modified polypyrrole dispersion liquid, uniformly stirring, raising the temperature to 80 ℃, keeping the temperature and stirring for 20 minutes, filtering, washing the precipitate with water, drying for 1 hour at 55 ℃ in vacuum, and cooling to normal temperature to obtain the polypyrrole battery conductive additive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010821832.5A CN111933947A (en) | 2018-05-04 | 2018-05-04 | Polypyrrole battery conductive additive and preparation method thereof |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810417880.0A CN108598485B (en) | 2018-05-04 | 2018-05-04 | Polypyrrole battery conductive additive and preparation method thereof |
| CN202010821832.5A CN111933947A (en) | 2018-05-04 | 2018-05-04 | Polypyrrole battery conductive additive and preparation method thereof |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810417880.0A Division CN108598485B (en) | 2018-05-04 | 2018-05-04 | Polypyrrole battery conductive additive and preparation method thereof |
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| CN111933947A true CN111933947A (en) | 2020-11-13 |
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| CN202010821832.5A Withdrawn CN111933947A (en) | 2018-05-04 | 2018-05-04 | Polypyrrole battery conductive additive and preparation method thereof |
| CN201810417880.0A Active CN108598485B (en) | 2018-05-04 | 2018-05-04 | Polypyrrole battery conductive additive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109537098A (en) * | 2018-10-26 | 2019-03-29 | 董荣志 | A kind of polythiophene conductive fiber and preparation method thereof |
| CN110783537A (en) * | 2019-09-19 | 2020-02-11 | 安徽清泉新能源科技集团有限责任公司 | Polypyrrole lithium-sulfur battery material |
| CN110676445B (en) * | 2019-09-19 | 2022-11-08 | 安徽清泉新能源科技集团有限责任公司 | Lithium battery material and preparation method thereof |
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| CN102358778B (en) * | 2011-07-29 | 2014-06-18 | 上海载和实业投资有限公司 | Novel biodegradable master batch and preparation method thereof |
| CN107459944A (en) * | 2017-07-14 | 2017-12-12 | 泰州市溪龙包装有限公司 | A kind of environment-friendly water-based packaging glue and preparation method thereof |
| CN107603218A (en) * | 2017-10-18 | 2018-01-19 | 温州市赢创新材料技术有限公司 | A kind of graphene conductive material and preparation method thereof |
| CN107629453A (en) * | 2017-10-18 | 2018-01-26 | 温州市赢创新材料技术有限公司 | A kind of polypyrrole conductive sol film and preparation method thereof |
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- 2018-05-04 CN CN202010821832.5A patent/CN111933947A/en not_active Withdrawn
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| CN108598485A (en) | 2018-09-28 |
| CN108598485B (en) | 2021-02-02 |
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