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Preparation method of shape-controllable hollow carbon microsphere

A carbon microsphere and hollow technology, which is applied in the field of preparation of hollow carbon microspheres with controllable morphology, can solve problems such as extended production cycle, high requirements for centrifugal equipment, and difficult separation process, and achieve the effect of reducing complexity

Inactive Publication Date: 2011-08-31
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, with this method, after the carbon / inorganic particle composite spheres are formed, the template must be removed through a subsequent step, thereby prolonging the production cycle
[0005] But at present, the preparation of hollow carbon microspheres by the template method also has the following problems: 1) modification treatment of polystyrene microspheres, mainly utilizes concentrated sulfuric acid to carry out acidification treatment to self-prepared polystyrene microspheres in the present invention, so that There are sulfonate groups on its surface to achieve the purpose of modification. It has been proved by experiments that after the modification treatment of small-sized polystyrene microspheres (<300nm), due to the hydrophilic sulfonate groups on the surface , its dispersion in water is very good, which makes the separation process more difficult and requires higher centrifugal equipment
2) The effect of carbonization rate and temperature on the morphology and structure of hollow carbon microspheres. Excessive heating rate during carbonization will cause damage to hollow carbon microspheres, making it difficult to maintain a hollow structure, and the degree of graphitization depends on carbonization temperature, which must be controlled according to the application requirements

Method used

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  • Preparation method of shape-controllable hollow carbon microsphere

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Preparation of core-shell structure phenolic resin / sulfonated polystyrene microspheres (PF / SPS) composite microspheres: add prepared SPS (8.33g / L) to 60ml of absolute ethanol, and heat in a water bath to After 40°C, 20ml of ethanol solution of resole phenolic resin was added dropwise, the mass ratio of resole phenolic resin to sulfonated polystyrene microspheres was 1.5:1, the dropwise addition was completed within 1 hour, reacted for 6h under mechanical stirring conditions, and separated And drying, the obtained particle size is 465nm and shows monodisperse PF / SPS composite microsphere;

[0024] 2) Preparation of hollow carbon microspheres: Under the protection of argon or nitrogen, the PF / SPS composite microspheres were carbonized at 900°C, and the heating rate was 5K / min to obtain hemispherical hollow carbon microspheres.

[0025] Its scanning electron microscope pictures and transmission electron microscope pictures are shown in figure 1 In (a) and (b), it can be ...

Embodiment 2

[0027] 1) Preparation of core-shell structure phenolic resin / sulfonated polystyrene microspheres (PF / SPS) composite microspheres: add prepared SPS (8.33g / L) to 60ml of absolute ethanol, and heat in a water bath to After 40°C, 20ml of ethanol solution of resole phenolic resin was added dropwise, the mass ratio of resole phenolic resin to sulfonated polystyrene microspheres was 2.5:1, the dropwise addition was completed within 1 hour, reacted for 6h under mechanical stirring conditions, and separated And drying, the obtained particle size is 480nm and shows monodisperse PF / SPS composite microsphere;

[0028] 2) Preparation of hollow carbon microspheres: Under the protection of argon or nitrogen, the PF / SPS composite microspheres were carbonized at 900 °C, and the heating rate was 5K / min to obtain hemispherical hollow carbon microspheres and complete Spherical hollow carbon microsphere mixture.

[0029] Its scanning electron microscope photograph is shown in figure 2 , the hol...

Embodiment 3

[0031] 1) Preparation of core-shell structure phenolic resin / polystyrene microspheres (PF / SPS) composite microspheres: add the prepared SPS (8.33g / L) to 60ml of absolute ethanol, and heat to 40°C in a water bath Finally, 20ml of ethanol solution of resole phenolic resin was added dropwise, the mass ratio of resole phenolic resin to modified polystyrene microspheres was 4:1, the dropwise addition was completed within 1 hour, reacted for 6h under mechanical stirring conditions, separated and dried , the obtained particle diameter is 515nm and shows monodisperse PF / SPS composite microsphere;

[0032] 2) Preparation of hollow carbon microspheres: Under the protection of argon or nitrogen, the PF / SPS composite microspheres were carbonized at 900°C, and the heating rate was 5K / min to obtain complete spherical hollow carbon microspheres

[0033] Its scanning electron microscope pictures and transmission electron microscope pictures are shown in image 3 In (a) and (b), the spherical...

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Abstract

The invention discloses a preparation method of a shape-controllable hollow carbon microsphere, belonging to the technical field of energy materials. The preparation method comprises the following steps of: firstly, preparing a polystyrene microsphere with monodispersity by adopting a soap-free emulsion polymerization method; modifying the surface of the polystyrene microsphere by acidizing treatment of concentrated sulfuric acid to enable the surface to have a sulfonic acid group (-SO3H-) with initiation activity to resol; then, dropping a resol ethanol solution into anhydrous ethanol in which the modified polystyrene microsphere is dispersed to enable the solution to carry out cross-linking reaction on the surface of the microsphere to prepare a compound microsphere in a core-shell structure; and finally, putting the compound microsphere in the inert gas protecting environment for carbonizing. The invention can effectively control the particle size of the hollow microsphere by changing the particle size of the microsphere, avoids an operating process of removing a template, effectively reduces the preparation processes, and can realize the purpose of controlling the shape of the hollow carbon microsphere only by changing one variable in the same system.

Description

technical field [0001] The invention belongs to the technical field of energy materials, and relates to a method for preparing a novel carbon carrier used as a direct methanol fuel cell, in particular to a method for preparing hollow carbon microspheres with controllable morphology. Background technique [0002] In recent years, direct methanol fuel cells have attracted more and more attention due to their excellent performance in many aspects, such as high energy density, simple operation, low reaction temperature, and broad application prospects in transportation and portable electronic devices. Whether it has high activity catalytic performance is the criterion for judging the performance of direct methanol fuel cells. Precious metals such as Pt and Pt-Ru alloys are often used to prepare anode catalysts for methanol oxidation, but due to their high prices, they are not used as anode catalysts in practical applications. Very restrictive. Therefore, people hope to develop ...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 王峰周学高刘景军王建军覃事永张良虎
Owner BEIJING UNIV OF CHEM TECH
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