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Method for preparing monodisperse nano hollow carbon sphere with controllable size and shape

A monodisperse and hollow technology, which is applied in the field of preparation of monodisperse nano hollow carbon spheres, can solve the problems of difficulty in obtaining target hollow carbon spheres with uniform size, difficulty in controlling template uniformity, and inability to convert hollow carbon spheres. Controllable morphology, high product yield and high purity

Inactive Publication Date: 2010-12-29
DALIAN UNIV OF TECH
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Problems solved by technology

[0004] However, the existing methods for preparing hollow carbon spheres by the soft template method have great limitations. Because the uniformity of the template is difficult to control and the size distribution is wide (50nm-3μm), it is difficult to obtain the target hollow carbon spheres with uniform size. Carbon spheres; and most soft template methods can only prepare hollow polymer spheres, because the polymer used has no carbon residue in the pyrolysis process and cannot be converted into hollow carbon spheres [J.Am.Chem.Soc.2009, 131, 13594]
Therefore, how to find a method for preparing monodisperse hollow carbon spheres with simple process, high yield, high purity, and controllable size and shape is still a big challenge.

Method used

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  • Method for preparing monodisperse nano hollow carbon sphere with controllable size and shape
  • Method for preparing monodisperse nano hollow carbon sphere with controllable size and shape
  • Method for preparing monodisperse nano hollow carbon sphere with controllable size and shape

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Embodiment 1

[0026] Weigh 2.5mmol dihydroxybenzoic acid and 7.5mmol formaldehyde, then they are dissolved in 95ml deionized water to form solution A, and then 0.18mmol carboxylic acid surfactant octadecenoic acid is dissolved in 5ml concentration of 1wt% dilute A solution B was obtained in ammonia water, and then the two solutions A and B were mixed, stirred slowly for 30 minutes, transferred to a reaction kettle, and reacted hydrothermally at 100° C. for 4 hours. Then cool to room temperature naturally. The product was centrifuged, washed twice with water and once with ethanol, and then dried in an oven at 50°C for 6 hours to obtain hollow polymer spheres. Then the obtained hollow polymer spheres were subjected to SiO 2 Embedding, the embedding thickness is 40nm, carbonization at 800°C for 4h, and removal of SiO 2 layer to obtain hollow carbon spheres. figure 1 (a) The TEM image of the hollow polymer sphere prepared in this example, it can be seen from the figure that the sample has a ...

Embodiment 2

[0028] Hydrothermal reaction temperature is 120 ℃, and other conditions are with embodiment 1, figure 1 (b) is a TEM picture of the hollow polymer sphere prepared in this example, the outer diameter of the hollow polymer sphere is 210±10 nm, and the cavity size is 50±5 nm.

[0029] image 3 Middle (a) is the hollow polymer sphere SiO prepared in this embodiment 2 Embedded TEM picture, (b) is the TEM picture of the hollow carbon sphere obtained in this embodiment. It can be seen from (b) that the size of the carbon spheres shrinks to 180±10nm after carbonization, and then the cavity expands slightly to 60±5nm.

[0030] The nitrogen adsorption isotherm of the hollow carbon spheres that present embodiment makes is as follows Figure 4 , where the curve (a) is the adsorption isotherm of the sample after carbonization at 800℃, and its S BET =558m 2 / g,V total =0.44cm 3 / g, (b) and (c) correspond to the adsorption isotherms after activation for 2h and 3h, respectively, and th...

Embodiment 3

[0032] The hydrothermal reaction temperature is 140°C, and other conditions are the same as in Example 1. The TEM image of the resulting hollow polymer sphere is as follows figure 1As shown in (c), the outer diameter is still 210±10nm, and the inner diameter increases to 70±5nm.

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Abstract

The invention relates to a method for preparing a nano hollow carbon sphere, in particular relating to a method for preparing a monodisperse nano hollow carbon sphere with controllable size and shape, comprising the following steps: adopting a surfactant as a mechanism guiding agent, further synthesizing hollow polymer spheres by a hydrothermal process firstly, embedding a layer of inert materialSiO2 on the hollow polymer spheres as an isolating layer for preventing the polymer spheres from mutually crosslinking in the carbonization process, and finally removing the isolating layer to obtainthe dispersible hollow carbon spheres. The invention has the beneficial effects that the size of the hollow carbon sphere and the cavity structure can be controlled by changing the test conditions, namely the method has the advantages of controllable size and shape, simple process, high product yield and high purity, and the hollow carbon sphere can form even colloid in a solvent such as water, ethanol, acetone and the like.

Description

technical field [0001] The invention relates to a preparation method of nanometer hollow carbon spheres, in particular to a preparation method of monodisperse nanometer hollow carbon spheres with controllable size and shape. Background technique [0002] Hollow carbon spheres have unique physical and chemical properties due to their special hollow structure. They have attracted attention in many fields and can be used in adsorption and separation, catalyst carriers, energy storage materials, optical components, drug sustained release, microreactors and other fields. At present, the research on hollow carbon spheres has become one of the frontiers in the research field of porous carbon materials. [0003] In recent years, the template method to prepare hollow carbon spheres is considered to be the most mature synthesis method. The template method can be divided into hard template method and soft template method according to its material properties. Most of the hard template...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 陆安慧王光辉孙蔷
Owner DALIAN UNIV OF TECH