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Preparation method of hollow porous carbon spheres with high specific surface area

A high specific surface area, hollow carbon sphere technology, applied in the field of inorganic materials, can solve the problems of inability to control the surface parameters of spheres, low specific surface area of ​​hollow carbon spheres, cumbersome steps, etc., to achieve controllable particle size and wall thickness, and easy to obtain raw materials , The effect of simple process

Inactive Publication Date: 2016-01-06
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the methods for synthesizing porous hollow carbon spheres are not uncommon, among which the template method is the most common, but most of them have the following shortcomings in the synthesis process: 1. The cost is high and the steps are cumbersome;
Patent CN101993057A uses nano-silicon spheres as templates to prepare carbon nano-hollow spheres by chemical vapor deposition, and controls the specific surface area of ​​the hollow spheres by changing the deposition thickness of the carbon layer. Although this method is simple, the specific surface area of ​​the prepared hollow carbon spheres is relatively small. Low (200-600m 2 / g)

Method used

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  • Preparation method of hollow porous carbon spheres with high specific surface area
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  • Preparation method of hollow porous carbon spheres with high specific surface area

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preparation example Construction

[0033] Such as figure 1 As shown, the present invention discloses a method for preparing porous hollow carbon spheres with a high specific surface area. The method includes:

[0034] S101, SiO 2 Disperse the ball into a mixed solution of absolute ethanol and deionized water, add cetyltrimethylammonium bromide to fully dissolve; the specific steps are:

[0035] SiO with a diameter of 50nm~1000nm 2 Put the ball in the beaker, add absolute ethanol, deionized water, SiO 2 The mass ratio of ball and absolute ethanol is 0.05: 9.875, the volume ratio of absolute ethanol and deionized water is (12.5~15): (30~40), ultrasonic vibration 15min makes SiO 2 The balls are fully dispersed into the mixed solution of absolute ethanol and deionized water, and cetyltrimethylammonium bromide is added. The mass fraction of cetyltrimethylammonium bromide in the reaction system is (0.04~0.18 )% to make it fully dissolved;

[0036] S102, adding resorcinol, silane, formaldehyde solution and ammonia solution, ...

Embodiment 1

[0044] Example 1: The method for preparing porous hollow carbon spheres with high specific surface area described in the embodiment of the present invention is as follows: take 0.0500 g of silica spheres with a diameter of about 180 nm in a small beaker and add no Water ethanol 12.5mL, deionized water 30mL ultrasonic for 15min, pour the solution into the flask, and add 0.0750g cetyltrimethylammonium bromide to the flask, after it is fully dissolved, add 0.0160g resorcinol , Ethyl orthosilicate 17μL, after stirring for 10min, add 61μL formaldehyde, 230μL ammonia water, stirring at room temperature for 24h, centrifuge the resulting product, wash 3 times with absolute ethanol, dry at 70℃ for 12h to prepare phenolic resin ball; Carbonized in a nitrogen atmosphere, heated to 350°C at a rate of 1°C / min, kept for 2h, and then heated to 600°C at a rate of 1°C / min, kept for 4h; put the resulting product in a 10% (mass fraction) hydrofluoric acid solution After stirring for 24h, filter, ...

Embodiment 2

[0045] Example 2: The method for preparing porous hollow carbon spheres with high specific surface area described in the embodiment of the present invention is as follows: take 0.0500 g of silica spheres with a diameter of about 180 nm in a small beaker and add no Water ethanol 12.5mL, deionized water 30mL ultrasonic for 15min, pour the solution into the flask, and add 0.0750g cetyltrimethylammonium bromide to the flask, after it is fully dissolved, add 0.0480g resorcinol , Methyl orthosilicate 17μL, after stirring for 10min, add 183μL formaldehyde, 230μL ammonia water, stirring at room temperature for 24h, centrifuge the resulting product, wash 3 times with absolute ethanol, dry at 70℃ for 12h to prepare phenolic resin ball; Carbonized in a nitrogen atmosphere, heated to 350°C at a rate of 1°C / min, kept for 2h, and then heated to 600°C at a rate of 1°C / min, kept for 4h; put the resulting product in a 10% (mass fraction) hydrofluoric acid solution Stir for 24h, filter, wash and...

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Abstract

The invention discloses a preparation method of hollow porous carbon spheres with high specific surface area. The preparation method comprises the steps of dispersing SiO2 spheres into a mixed solution of absolute ethanol and deionized water, adding cetyltrimethylammonium bromide, and sufficiently dissolving; adding resorcinol, silane, a formaldehyde solution and an ammonia solution, and centrifuging, washing and drying after reacting to obtain phenolic resin spheres; and carbonizing the phenolic resin spheres, removing silicon, filtering, washing and drying to obtain hollow porous carbon spheres with high specific surface area. The hollow carbon spheres are obtained by taking SiO2 spheres as templates, silane as a pore-forming agent as well as formaldehyde and resorcinol as carbon sources through the operation process of carbonizing, removing silicon and the like by using a coating technology. The preparation method is simple in process, easily available in raw materials as well as simple and convenient in operation; and the prepared hollow porous carbon spheres have the characteristics of high specific surface area, high specific volume, controllable particle size and wall thickness and the like.

Description

Technical field [0001] The invention relates to the field of inorganic materials, in particular to a method for preparing porous hollow carbon spheres with high specific surface area. Background technique [0002] In recent years, with the continuous deepening of carbon materials research, the synthesis technology of spherical carbon materials has been gradually improved. Among them, porous hollow carbon spheres have received widespread attention due to their high specific surface area, large pore volume, excellent electrical conductivity, and good thermal stability. They are widely used in drug delivery, catalysis, electrode materials, sensors, adsorbents, fuels, etc. The battery and other fields are widely used. [0003] At present, methods for synthesizing porous hollow carbon spheres have been common, among which template method is the most common, but most of them have the following shortcomings in the synthesis process: 1. High cost and cumbersome steps; 2. Simple and effect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 李雪娜白诗扬孙继红武霞
Owner BEIJING UNIV OF TECH
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