Controllable synthesis method for nitrogen and phosphorus co-doped graphitized carbon ball with hollow structure

A technology of hollow structure and synthesis method, applied in the direction of nano-carbon, carbon preparation/purification, nanotechnology for materials and surface science, etc., to achieve the effect of low price, easy recycling and high product purity

Inactive Publication Date: 2015-02-25
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, 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 40 milliliters of deionized water. After stirring evenly, move them into a 50 milliliter hydrothermal reactor, and react at 160 ° C for 15 After one hour, the reaction product was filtered and washed with deionized water at 25° C. 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 gas flow rate of 30 ml per minute. After natural cooling to room temperature, 14 mol / Soak in L phosphoric acid at 90°C for 6 hours to remove tin and iron, and obtain graphitized carbon spheres co-doped with nitrogen and phosphorus with a hollow structure, the outer diameter is 224 nm, the inner diameter is 140 nm, the ratio of outer diameter / inner diameter is 1.6, and the carbon she...

Embodiment 2

[0039] 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 a mixture of 20 milliliters of deionized water and 20 milliliters of phosphoric acid (phosphoric acid concentration 52%~54%) , stirred evenly, moved into a 50 ml hydrothermal reaction kettle, reacted at 160°C for 3 hours, filtered the reaction product, and washed it with 25°C 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 with a heating rate of 5°C per minute and an ammonia gas flow rate of 30 ml per minute. After natural cooling to room temperature, 5 mol / Soak in L phosphoric acid at 90°C for 6 hours to remove tin and iron, and obtain graphitized carbon spheres co-doped with nitrogen and phosphorus with a hollow structure. The outer diameter is 94 nm, the inner diameter is 71 nm, the ratio...

Embodiment 3

[0040] Embodiment 3: first 4.0 grams of glucose, 0.21 gram of sodium stannate, 0.22 gram of ferric chloride, mol ratio 25:1:1, are dissolved in 10 milliliters of deionized water and 30 milliliters of phosphoric acid (phosphoric acid concentration 52%~54% ) mixture, stirred evenly and transferred to a 50 ml hydrothermal reaction kettle, reacted at 160°C for 9 hours, filtered the reaction product, and washed it with 50°C 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 an ammonia gas flow rate of 30 ml per minute. After natural cooling to room temperature, 2 mol / Soak in L phosphoric acid at 90°C for 6 hours to remove tin and iron, and obtain graphitized carbon spheres co-doped with nitrogen and phosphorus with a hollow structure, the outer diameter is 125 nm, the inner diameter is 104 nm, the ratio of o...

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Abstract

The invention relates to a controllable synthesis method for a nitrogen and phosphorus co-doped graphitized carbon ball with a hollow structure. The method comprises the following preparation steps: (1) a carbon source, soluble metal salt and a catalyst are dissolved in a solvent according to a molar ratio, the mixture is transferred to a hydrothermal reaction kettle for hydrothermal synthesis after stirred to be dissolved completely, and an obtained precipitate is cleaned, filtered and dried to obtain a primary product; (2) the obtained primary product is subjected to high-temperature reduction under the protection of gas in a high-temperature reaction furnace; and (3) the product obtained by high-temperature reduction is placed in an acid solution to be soaked, and then cleaned, filtered and dried to obtain the nitrogen and phosphorus co-doped graphitized carbon ball with the hollow structure. The nitrogen and phosphorus co-doped graphitized carbon ball with the hollow structure prepared with the method has the advantages that the appearance is uniform, a carbon shell has a cellular structure, the interior of the carbon ball has a mesoporous carbon support structure, the graphitization degree is good, and the like; and the carbon ball can be used in various fields of efficient catalytic conversion, energy storage and conversion, medicine release and control, substance adsorption and separation and the like. A template-free hydrothermal synthesis technique is simple and controllable, and can be used for mass production.

Description

technical field [0001] The invention relates to a synthesis method of nitrogen and phosphorus co-doped nano hollow carbon spheres, in particular to a controllable synthesis method of nitrogen and phosphorus co-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 reacti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/02B82Y30/00B82Y40/00C01B32/05C01B32/15
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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