CN111762772A - Preparation method of solvent-free micron carbon sphere material - Google Patents

Preparation method of solvent-free micron carbon sphere material Download PDF

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CN111762772A
CN111762772A CN202010737615.8A CN202010737615A CN111762772A CN 111762772 A CN111762772 A CN 111762772A CN 202010737615 A CN202010737615 A CN 202010737615A CN 111762772 A CN111762772 A CN 111762772A
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solvent
micron carbon
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sphere material
carbon sphere
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CN111762772B (en
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周亮
杜寰
冯世豪
麦立强
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Wuhan University of Technology WUT
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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
    • H01G11/22—Electrodes
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • 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
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
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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
    • 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
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • 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
    • 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
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H—ELECTRICITY
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    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract

The invention provides a preparation method of a solvent-free micron carbon sphere material, which comprises the following steps: weighing m-phenylenediamine, hexamethylenetetramine and polyoxyethylene polyoxypropylene ether block copolymer; putting the weighed substances into a grinding body, adding deionized water, and grinding to obtain a white jelly sample; and putting the white colloid sample into a container, putting the container into a reaction kettle, sintering at high temperature, and cooling to obtain the micron carbon sphere material. According to the invention, the micron carbon spheres are obtained by combining a solid hydrothermal method with a reaction kettle for sintering, and after later carbonization and activation, the micron carbon spheres with high specific surface area can be obtained, so that molecular dispersion and assembly among solid materials are realized, the process is simple, no solvent is used, and the method has the advantages of small pollution, easiness in operation, high safety, high selectivity, high reaction efficiency and the like.

Description

Preparation method of solvent-free micron carbon sphere material
Technical Field
The invention relates to the technical field of nano materials and electrochemical devices, in particular to a preparation method of a solvent-free micron carbon sphere material.
Background
Environmental pollution and energy problems are one of the hot spots of social attention at present, and the development of high-efficiency energy storage equipment is an effective way for improving the problems of environmental pollution and energy shortage at present. Super capacitors are energy storage devices which are developed rapidly in recent years, and store energy by electrostatic adsorption of electrolyte ions without electrochemical reaction in the middle, so that the super capacitors have the remarkable advantages of high power density, long cycle life and the like. The properties of the electrode material of a supercapacitor have a crucial role for its electrochemical performance.
The electrode material is one of the important factors determining the performance of the supercapacitor, and the carbon material has the characteristics of high specific surface area, uniform and adjustable pore structure, good electrical conductivity, excellent chemical stability and the like, and the unique chemical and physical characteristics are the most ideal electrode material of the supercapacitor. At present, in commercial supercapacitor preparation, a carbon material is used as an electrode material in 80 percent, and nanocrystallization research and production are focused, but the problem of material agglomeration caused by a nanometer effect is particularly serious, the problem that specific capacity is influenced by the violent reduction of tap density caused by size reduction is directly limited, and the application of the carbon material in the supercapacitor is directly limited. Therefore, the researchers have great interest in solving the problems so as to explore a brand-new preparation method of the carbon microsphere with the hierarchical porous structure and simple process.
Disclosure of Invention
The invention aims to provide a preparation method of a solvent-free micron carbon sphere material, which is characterized in that micron carbon spheres are obtained by combining a solid hydrothermal method with a reaction kettle for sintering, and after later carbonization and activation, micron carbon spheres with high specific surface area can be obtained, so that molecular dispersion and assembly among solid materials are realized, the process is simple, no solvent is used, and the preparation method has the advantages of small pollution, simplicity and easiness in operation, high safety, high selectivity, high reaction efficiency and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a solvent-free micron carbon sphere material comprises the following steps:
1) weighing m-phenylenediamine, hexamethylenetetramine and polyoxyethylene polyoxypropylene ether block copolymer F-127 (pluronic F-127);
2) putting the weighed substances into a grinding body, adding deionized water, and grinding to obtain a white jelly sample;
3) and putting the white colloid sample into a container, putting the container into a reaction kettle, sintering at high temperature, and cooling to obtain the micron carbon sphere material.
According to the scheme, the mass ratio of the m-phenylenediamine to the hexamethylenetetramine to the polyoxyethylene polyoxypropylene block copolymer is 3.3: 1-1.5: 8.3-12.5.
According to the scheme, the mass ratio of the addition amount of the deionized water to the m-phenylenediamine is 0.38-1.54: 3.3.
According to the scheme, the grinding time is 8-10 min.
According to the scheme, the high-temperature sintering temperature is 150-200 ℃, and the sintering time is 24 h.
According to the scheme, the temperature of the high-temperature sintering is 160 ℃.
The solvent-free method belongs to typical solid-solid reaction, no reaction solvent is added in the whole process, the direct contact reaction between solid materials can effectively avoid the troublesome problem existing in a hydrothermal system, and the method is a novel method for synthesizing the supercapacitor electrode material with a green chemical concept at present. The material prepared by the invention can be used as an electrode material of lithium ion and sodium ion batteries.
The action mechanism of the invention is as follows: hexamethylenetetramine and added trace water are subjected to hydrolysis reversible reaction at high temperature to generate ammonia gas and formaldehyde, amino of m-phenylenediamine and aldehyde group of the formaldehyde are subjected to aldehyde-amine condensation reaction to form small balls, the m-phenylenediamine has an amino group and has a catalytic acceleration effect, the reaction can be quickly completed, nitrogen atoms are introduced into the raw materials, the nitrogen atoms have strong electron affinity, so that the polarity of the porous carbon material can be changed, and meanwhile, the lone pair of electrons of the nitrogen atoms can be conjugated with the carbon material to obtain a large pi bond to form conjugation, so that the electrochemical and catalytic performances of the porous carbon material are improved.
The invention has the beneficial effects that:
1) the invention has little pollution: because no solvent is involved, the volatilization of the solvent and the discharge of waste liquid are avoided, and the green chemical concept of chemical reaction under the non-toxic and harmless condition is met;
2) the invention has simple operation: the solvent-free method only needs to mechanically mix and grind the solid raw materials, seal the solid raw materials in a reaction kettle and sinter the solid raw materials;
3) the invention has high safety: no reaction solvent is added, so that the problem of over-high autogenous pressure generated in the reaction process is avoided, and the green chemical principle that the potential safety hazard is minimum in the chemical production process is met;
4) the invention has high selectivity: the solvent-free method provides a novel molecular environment for the synthesis reaction, solid molecules are bound by crystal lattices, the conformation of the molecules is frozen, the reaction molecules are orderly arranged, the directional reaction can be realized, and the effective collision probability among the solid molecules is larger, so that the product selectivity is favorably improved;
5) the invention has high reaction efficiency: under the solvent-free system, the intervention of solvent molecules is avoided, so that a local high-concentration micro chemical environment is formed under the reaction system, and the reaction efficiency is improved.
Drawings
FIG. 1 is an SEM image of micron carbon spheres of inventive example 1;
FIG. 2 is an SEM image of micron carbon spheres of inventive example 2;
FIG. 3 is an SEM image of micron carbon spheres of inventive example 3;
FIG. 4 is an SEM image of micron carbon spheres of inventive example 4;
FIG. 5 is an SEM image of micron carbon spheres of inventive example 5;
FIG. 6 is an SEM image of micron carbon spheres of inventive example 6;
fig. 7 is an SEM image of micro carbon spheres of inventive example 7;
fig. 8 is an SEM image of micron carbon spheres of inventive example 8.
Detailed Description
The technical solution of the present invention will be described with reference to the following examples.
Example 1:
the invention provides a preparation method of a solvent-free micron carbon sphere material, which comprises the following steps:
(1) weighing 0.33g of m-phenylenediamine, 0.1g of hexamethylenetetramine and 0.83g of pluronic F-127;
(2) putting the three samples obtained in the step (1) into a grinding body, adding 38mg of deionized water, and grinding to obtain a white jelly sample;
(3) and (3) putting the white colloid sample obtained in the step (2) into a small beaker, putting the beaker into a reaction kettle, sintering the mixture at the high temperature of 160 ℃ for 24 hours, and cooling the mixture to obtain the micron carbon sphere material.
The SEM image of the sample prepared in this example is shown in FIG. 1, which shows that the dispersibility and uniformity are good, and the diameter is 300-400nm micron carbon spheres.
Example 2:
the invention provides a method for preparing a solvent-free micron carbon sphere material, which is basically the same as the embodiment and is characterized in that: deionized water was added at 58 mg.
SEM images of samples prepared in this example are shown in FIG. 2, and micron carbon spheres with a diameter of about 200nm are visible.
Example 3:
the invention provides a method for preparing a solvent-free micron carbon sphere material, which is basically the same as the embodiment and is characterized in that: the amount of deionized water added was 77 mg.
The SEM image of the sample prepared in this example is shown in fig. 3, and the thin and long micron carbon rods and carbon spheres with good dispersibility can be seen.
Example 4:
the invention provides a method for preparing a solvent-free micron carbon sphere material, which is basically the same as the embodiment and is characterized in that: the amount of deionized water added was 154 mg.
The SEM image of the sample prepared in this example is shown in FIG. 4, which shows that the more uniform micron carbon rods with a length of about 1 μm are obtained.
Example 5:
the invention provides a method for preparing a solvent-free micron carbon sphere material, which is basically the same as the embodiment and is characterized in that: 0.15g of hexamethylenetetramine, 115mg of deionized water and 200 ℃ of high-temperature sintering temperature.
The SEM image of the sample prepared in this example is shown in FIG. 5, and it can be seen that the micron carbon rods having a diameter of about 2 μm and the micron carbon spheres having good uniformity coexist.
Example 6:
the invention provides a method for preparing a solvent-free micron carbon sphere material, which is basically the same as the embodiment and is characterized in that: 0.15g of hexamethylenetetramine and 115mg of deionized water were added.
The SEM image of the sample prepared in this example is shown in FIG. 6, which shows that the shape is not uniform, and the diameter is about 400-500 nm.
Example 7:
the invention provides a method for preparing a solvent-free micron carbon sphere material, which is basically the same as the embodiment and is characterized in that: 0.15g of hexamethylenetetramine, 1.25g of pluronic F-127, 115mg of deionized water and 200 ℃ of high-temperature sintering temperature.
The SEM image of the sample prepared in this example is shown in FIG. 7, which shows that the dispersion is good, and the diameter of the micron carbon spheres is about 200-500nm and has non-uniform size.
Example 8:
the invention provides a method for preparing a solvent-free micron carbon sphere material, which is basically the same as the embodiment and is characterized in that: 0.15g of hexamethylenetetramine, 1.25g of Pluronic F-127 and 115mg of deionized water were added.
The SEM image of the sample prepared in this example is shown in FIG. 8, and it can be seen that the dispersibility and uniformity are good, and the diameter of the micron carbon sphere is about 250 nm.
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the above embodiments describe the present invention in detail, those skilled in the art should understand that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and any modifications and equivalents may fall within the scope of the claims.

Claims (6)

1. A method for preparing a solvent-free micron carbon sphere material is characterized by comprising the following steps:
1) weighing m-phenylenediamine, hexamethylenetetramine and polyoxyethylene polyoxypropylene ether block copolymer;
2) putting the weighed substances into a grinding body, adding deionized water, and grinding to obtain a white jelly sample;
3) and putting the white colloid sample into a container, putting the container into a reaction kettle, sintering at high temperature, and cooling to obtain the micron carbon sphere material.
2. The method for preparing the solvent-free micron carbon sphere material according to claim 1, wherein the mass ratio of the m-phenylenediamine to the hexamethylenetetramine to the polyoxyethylene polyoxypropylene ether block copolymer is 3.3: 1-1.5: 8.3-12.5.
3. The method for preparing the solvent-free micron carbon sphere material according to claim 1, wherein the mass ratio of the added deionized water to the m-phenylenediamine is 0.38-1.54: 3.3.
4. The method for preparing solvent-free micron carbon sphere material according to claim 1, wherein the grinding time is 8-10 min.
5. The method for preparing the solvent-free micron carbon sphere material according to claim 1, wherein the high-temperature sintering temperature is 150-200 ℃, and the sintering time is 24 h.
6. The method for preparing solvent-free micron carbon sphere material according to claim 1, wherein the temperature of the high temperature sintering is 160 ℃.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113649011A (en) * 2021-07-29 2021-11-16 武汉理工大学 Non-noble metal carbon-based catalyst and preparation method and application thereof
CN114906838A (en) * 2022-04-08 2022-08-16 武汉理工大学 Preparation method of solvent-free tadpole-shaped asymmetric carbon-based nano material
CN116477605A (en) * 2023-06-15 2023-07-25 武汉理工大学三亚科教创新园 Preparation method of in-situ nitrogen-doped micron carbon sphere material and sodium ion battery pack
CN116479546A (en) * 2023-06-19 2023-07-25 武汉理工大学三亚科教创新园 Method for preparing carbon fiber material without solvent and sodium ion battery pack

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107572523A (en) * 2017-09-11 2018-01-12 桂林电子科技大学 A kind of classifying porous carbosphere of N doping and its preparation method and application
CN108569697A (en) * 2018-06-21 2018-09-25 夏辉 A kind of nitrogen doped micropore carbon ball and preparation method thereof for electrode material for super capacitor
CN108899557A (en) * 2018-06-07 2018-11-27 上海交通大学 It is a kind of with through mesoporous N doping flower pattern carbon nanomaterial and preparation method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107572523A (en) * 2017-09-11 2018-01-12 桂林电子科技大学 A kind of classifying porous carbosphere of N doping and its preparation method and application
CN108899557A (en) * 2018-06-07 2018-11-27 上海交通大学 It is a kind of with through mesoporous N doping flower pattern carbon nanomaterial and preparation method
CN108569697A (en) * 2018-06-21 2018-09-25 夏辉 A kind of nitrogen doped micropore carbon ball and preparation method thereof for electrode material for super capacitor

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113649011A (en) * 2021-07-29 2021-11-16 武汉理工大学 Non-noble metal carbon-based catalyst and preparation method and application thereof
CN114906838A (en) * 2022-04-08 2022-08-16 武汉理工大学 Preparation method of solvent-free tadpole-shaped asymmetric carbon-based nano material
CN114906838B (en) * 2022-04-08 2023-06-27 武汉理工大学 Preparation method of solvent-free tadpole-shaped asymmetric carbon-based nanomaterial
CN116477605A (en) * 2023-06-15 2023-07-25 武汉理工大学三亚科教创新园 Preparation method of in-situ nitrogen-doped micron carbon sphere material and sodium ion battery pack
CN116477605B (en) * 2023-06-15 2023-09-15 武汉理工大学三亚科教创新园 Preparation method of in-situ nitrogen-doped micron carbon sphere material and sodium ion battery pack
CN116479546A (en) * 2023-06-19 2023-07-25 武汉理工大学三亚科教创新园 Method for preparing carbon fiber material without solvent and sodium ion battery pack
CN116479546B (en) * 2023-06-19 2023-08-22 武汉理工大学三亚科教创新园 Method for preparing carbon fiber material without solvent and sodium ion battery pack

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