Method for preparing graphitization nano carbon

A nano-carbon and graphitization technology, which is applied in the field of nano-carbon preparation, can solve the problems of low purity, uncontrollable shape, and low yield of graphitized nano-carbon, and achieve the effect of easy operation and simple method

Inactive Publication Date: 2009-06-17
HEILONGJIANG UNIV
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AI-Extracted Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problems of low yield, low purity and uncontrollable appearan...
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Abstract

The invention relates to a method for preparing graphitized nano carbon, which relates to a method for preparing the nano carbon. The method solves the problems of low yield, low purity and uncontrollable shape in the prior art for preparing the graphitized nano carbon. The method comprises: coordination of carbon sources and metallic ions; complex curing; heat treatment; and activation treatment, so as to obtain the graphitized nano carbon. The graphitized nano carbon prepared by the method has high yield, high purity and controllable shape. The method is simple, easy to operate, and suitable for industrial production.

Technology Topic

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  • Method for preparing graphitization nano carbon
  • Method for preparing graphitization nano carbon
  • Method for preparing graphitization nano carbon

Examples

  • Experimental program(59)

Example Embodiment

[0008] Specific embodiment 1: The graphitized nanocarbon of this embodiment is prepared according to the following steps: 1. Coordination of carbon source and metal ions: mix the carbon source with the metal catalyst solution, stir for 12-24h, and then ultrasonically treat the mixture for 30-120min. Add the surfactant solution to it, and continue to stir for 1~3h; 2. Solidification of the complex: The mixed solution prepared in step 1 is vacuum dried at 20~100℃ for 2~24h, and then cooled to room temperature; 3. Heat treatment: 5 The temperature is increased to 400~1100℃ at a rate of ~20℃/min, and the product of step 2 is heat-treated for 0.5~6h under the conditions of air flow rate of 60~250ml/min and temperature of 600~1100℃; 4. Activation treatment: Yes The product of step 3 is physically activated or chemically activated to obtain graphitized nanocarbon; wherein the weight ratio of the solute in the metal catalyst solution to the carbon source in step 1 is 0.025~0.05:2.5, and the carbon source and the surfactant solution The weight ratio of the solute is 10-50:1, the molar concentration of the metal catalyst solution is 0.025-0.3 mol/L, and the molar concentration of the surfactant solution is 0.0015-0045 mol/L.
[0009] The Raman spectrum of the graphitized nanocarbon prepared in this embodiment is as follows figure 1 Shown from figure 1 It can be seen that the samples treated at 600°C to 1100°C have obvious Raman vibration peaks of graphite.
[0010] The graphitized nanocarbon Raman peak area and area ratio obtained in this example are shown in Table 1.
[0011] Table 1
[0012] Carbonization temperature S D (D peak area) S G (G peak area) S G /S D (G peak area and 600℃ / / / 700℃ 147961 178166 1.204 800℃ 526634 690326 1.311 900℃ 568377 764282 1.345 1000℃ 508958 703140 1.382 1100℃ 615559 971908 1.579
[0013] From the data in Table 1, it can be seen that as the processing temperature increases, S G /S D Gradually increase, indicating that the graphitization degree of the sample gradually increases with the increase of temperature.
[0014] The yield of graphitized nanocarbon prepared in this embodiment is 93.5% and the purity is 97.4%; the graphitized carbon prepared in this embodiment is graphitized carbon nanocapsules, graphitized carbon nanosheets, graphitized carbon nanorolls, and graphite Carbon nanowall, graphitized carbon nanowire, graphitized carbon nanorod, graphitized carbon nanobelt, and graphitized carbon nanotree.

Example Embodiment

[0015] Specific embodiment 2: The graphitized nanocarbon of this embodiment is prepared according to the following steps: 1. The carbon source is coordinated with the metal ion: the carbon source is mixed with the metal catalyst solution, stirred for 12 to 24 hours, and then ultrasonically treated for 30 to 120 minutes. Add the surfactant solution to it and continue to stir for 1~3h; 2. Solidification of the complex: dry the mixed solution prepared in step 1 at 20~80℃ for 2~24h in vacuum, and then cool to room temperature; 3. Heat treatment: Raise the temperature to 600~1100℃ at a rate of ~20℃/min, and then heat the product of step 2 for 0.5~6h under the conditions of air flow of 60~250ml/min and temperature of 400~1100℃; 4. Activation treatment: Yes The product of step 3 is subjected to physical activation or chemical activation treatment; 5. Add 50ml of concentrated hydrochloric acid with a concentration of 12mol/L to the product prepared in step 4, and react at 90-100°C for 5-12h to obtain graphitized nanocarbon; In step 1, the weight ratio of the solute in the metal catalyst solution to the carbon source is 0.025~0.05:2.5, the weight ratio of the carbon source to the solute in the surfactant solution is 10~50:1, and the molar concentration of the metal catalyst solution is 0.025 ~0.3mol/L, the molar concentration of the surfactant solution is 0.0015~0045mol/L.
[0016] The yield of graphitized nanocarbon prepared in this embodiment is 95.3%, and the purity is 94.9%; the graphitized carbon prepared in this embodiment is graphitized carbon nanocapsules, graphitized carbon nanosheets, graphitized carbon nanorolls, and graphite Carbon nanowall, graphitized carbon nanowire, graphitized carbon nanorod, graphitized carbon nanobelt, and graphitized carbon nanotree.

Example Embodiment

[0017] Specific embodiment three: This embodiment is different from specific embodiment one or two in that the carbon source in step one is a polymer with polar groups, agricultural and forestry crop extracts or agricultural and forestry wastes; those with polar groups The polymer is one of polymethacrylic acid, polystyrene, polyfurfuryl alcohol, polyacrylamide, polyimine, polyurethane, polyglucosamine, polyethylene glycol, anion and cation exchange resin, polyvinyl alcohol, polyaniline or A mixture of several, the extracts of agricultural and forestry crops are glucose, sucrose, fructose or starch, and the agricultural and forestry wastes are beet residue, bagasse, corn stalks, reeds, cattail or wormwood. Others are the same as the first or second embodiment.
[0018] When there are two or more polymers with polar groups in this embodiment, the components are mixed in any ratio.
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