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Controllable synthesis method of N-doped graphitized carbon ball with hollow structures

A hollow structure and synthesis method technology, applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., to achieve the effects of low price, easy recycling and high product purity

Inactive Publication Date: 2013-07-03
CHINA UNIV OF MINING & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the carbon spheres obtained by this synthesis method do not have graphitic carbon

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1: First, 4.0 grams of glucose, 0.21 grams of sodium stannate, and 0.22 grams of ferric chloride, in a molar ratio of 25:1:1, were dissolved in 40 milliliters of deionized water, stirred evenly, and moved into a 50 milliliter hydrothermal reaction kettle. After reacting at 160° C. for 15 hours, the reaction product was filtered, and washed with 25° C. deionized water to remove impurities. After the reaction product was vacuum-dried at 70°C for 12 hours, it was placed in a high-temperature tube furnace and heated at 1000°C for 2 hours, with a heating rate of 5°C per minute and an ammonia flow rate of 30 milliliters per minute. After naturally cooling to room temperature, pass 12mol / L hydrochloric acid soaked at 25°C for 12 hours to remove tin and iron, and obtained nitrogen-doped graphitized carbon spheres with a hollow structure. The pore size (0.7nm, 1.1nm), the carbon core mesopore size is 4.7nm, the specific surface area is about 420 square meters per gram, t...

Embodiment 2

[0038] Example 2: First, dissolve 4.0 grams of glucose, 0.21 grams of sodium stannate, and 0.22 grams of ferric chloride at a molar ratio of 25:1:1 in 20 milliliters of deionized water and 20 milliliters of ammonia water (ammonia content 27-30%) The mixed solution was stirred evenly and then moved into a 50 ml hydrothermal reaction kettle. After 3 hours of reaction at 160° C., the reaction product was filtered, and cleaned with 25° C. of deionized water to remove impurities. After the reaction product was vacuum-dried at 100°C for 4 hours, it was placed in a high-temperature tube furnace and heated at 1000°C for 2 hours at a heating rate of 5°C per minute, with a nitrogen flow rate of 30 milliliters per minute. After naturally cooling to room temperature, pass through 12mol / L hydrochloric acid soaked at 25°C for 12 hours to remove tin and iron to obtain nitrogen-doped graphitized carbon spheres with a hollow structure, with an outer diameter of 94 nanometers, an inner diameter...

Embodiment 3

[0039] Example 3: First, dissolve 4.0 grams of glucose, 0.21 grams of sodium stannate, and 0.22 grams of ferric chloride in a molar ratio of 25:1:1 in 40 milliliters of ammonia water (ammonia content 27-30%). Milliliter of hydrothermal reaction kettle, 160 DEG C reacts for 9 hours and the reaction product is filtered, washes with 50 DEG C of deionized water and removes impurity. After the reaction product was vacuum-dried at 100°C for 4 hours, it was placed in a high-temperature tube furnace and heated at 1000°C for 2 hours at a heating rate of 5°C per minute, with a nitrogen flow rate of 30 milliliters per minute. After naturally cooling to room temperature, pass through 12mol / L hydrochloric acid soaked at 25°C for 12 hours to remove tin and iron to obtain nitrogen-doped graphitized carbon spheres with a hollow structure. Size (0.7 nanometers, 1.1 nanometers), the carbon core mesopore size is 4.7 nanometers, the specific surface area is about 530 square meters per gram, the ...

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Abstract

The invention discloses a controllable synthesizing method of an N-doped graphitized carbon ball with hollow structures. The method comprises the following steps: (1) dissolving silicon source, soluble metal salt and a catalyst to the solvent according to the molar ratio, transferring the solvent to the thermal water kettle to conduct hydro-thermal synthesis after being stirred until being thoroughly dissolved, and cleaning, filtering and drying the sediment to obtain a primary commodity; (2) reducing the primary commodity at high temperature under the protection of gas in a high-temperature reaction furnace; and (3) soaking the product obtained by high-temperature reducing in acidic solution, and obtaining the graphitized carbon ball nitrogen doping with the hollow structure after cleaning, filtering and drying. The graphitized carbon ball with the hollow structures provided by the invention has the advantages that the carbon sphere has a uniform appearance, the carbon shell has millipore structures, a mesoporous carbon support structure is formed inside the carbon sphere and a better graphitize degree is provided, and can be used in the field of high-efficient catalyzing and transforming, energy storage and transforming, medicine releasing, substance adsorptive separation and the like. The non-template hydrothermal synthesis technique provided by the invention is simple and controllable, and can be used in large scale production.

Description

technical field [0001] The invention relates to a synthesis method of nitrogen-doped nanometer hollow carbon spheres, in particular to a controllable synthesis method of nitrogen-doped graphitized carbon spheres with a hollow structure. Background technique [0002] Nano hollow carbon sphere is a special carbon material with high chemical stability, low density, good thermal stability and biocompatibility, not only can be used as electrode material, catalyst carrier, gas storage medium, lubrication It is also used as dyes, rubber reinforcement materials, lightweight structural materials and many other fields, attracting more and more attention. [0003] At present, hollow carbon spheres are mainly prepared by pyrolysis of organic matter, chemical vapor deposition, dielectric reduction, laser distillation, arc discharge, template self-assembly and other methods. These methods are usually carried out under high temperature conditions, the reaction time is long, the energy con...

Claims

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Application Information

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IPC IPC(8): C01B31/04B82Y30/00B82Y40/00C01B32/205
Inventor 尹诗斌罗林荆胜羽朱强强卫怡杨力祥贾优黄飞张绍良强颖怀
Owner CHINA UNIV OF MINING & TECH
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