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Chitosan-based porous carbon sphere and preparation method thereof

A chitosan and porous carbon technology, applied in chemical instruments and methods, carbon compounds, other chemical processes, etc., can solve the problems that limit the efficient utilization of chitosan-based carbon materials, the low efficiency of hydrothermal carbonization into spheres, and the shape of carbon materials. irregular appearance and other problems, to achieve the effects of low cost, strong physical and chemical stability, and improved porosity and specific surface area

Active Publication Date: 2019-03-26
SOUTH CHINA NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The current research mainly uses acetic acid as a solvent to dissolve chitosan, but the hydrothermal carbonization efficiency of chitosan in acetic acid system is low, and the obtained carbon material has irregular morphology and low specific surface area, which limits the ability of chitosan-based Efficient utilization of carbon materials

Method used

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  • Chitosan-based porous carbon sphere and preparation method thereof
  • Chitosan-based porous carbon sphere and preparation method thereof
  • Chitosan-based porous carbon sphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A preparation method of chitosan-based porous carbon spheres, the specific steps are as follows:

[0037] (1) Add 0.5 g of chitosan with a molecular weight of 50,000 Da to 500 mL of dilute hydrochloric acid solution with a concentration of 0.1 mol / L to dissolve it at a stirring rate of 600 rpm, and obtain the mass fraction (g / mL ) is 0.1% chitosan solution;

[0038] (2) Transfer the chitosan solution prepared in step (1) to a hydrothermal reaction kettle, heat it to 180 °C, and conduct hydrothermal carbonization at a constant temperature for 8 hours. Press and dry at 30°C to obtain black powder, which is chitosan-based carbon spheres;

[0039] (3) According to the mass ratio of chitosan-based carbon spheres and KOH particles of 1:0.1, weigh 0.25 g of chitosan-based carbon spheres and 0.025 g of KOH particles obtained in step (2) respectively, place them in an agate mortar, grind and mix Finally, in a nitrogen atmosphere, the temperature was raised to 600 °C in a tube ...

Embodiment 2

[0042] A preparation method of chitosan-based porous carbon spheres, the specific steps are as follows:

[0043] (1) Under the condition of stirring rate of 700 rpm, 5 g of chitosan with a molecular weight of 200,000 Da was added to 500 mL of dilute hydrochloric acid solution system with a concentration of 1 mol / L to dissolve it, and the mass fraction (g / mL) is 1% chitosan solution;

[0044] (2) Transfer the chitosan solution prepared in step (1) to a hydrothermal reaction kettle, heat it to 200 °C, and conduct hydrothermal carbonization at a constant temperature for 12 h. After the reaction, cool to room temperature and dialyze with a 3000 D dialysis bag. Vacuum drying at 50 °C to obtain black powder, which is chitosan-based carbon spheres;

[0045](3) According to the mass ratio of chitosan-based carbon spheres and KOH particles of 1:0.5, weigh 0.5 g of chitosan-based carbon spheres and 0.25 g of KOH particles obtained in step (2) respectively, place them in an agate morta...

Embodiment 3

[0048] A preparation method of chitosan-based porous carbon spheres, the specific steps are as follows:

[0049] (1) Add 20 g of chitosan with a molecular weight of 200,000 Da to 500 mL of dilute hydrochloric acid solution with a concentration of 2 mol / L at a stirring rate of 1000 rpm to obtain the mass fraction (g / mL ) is 4% chitosan solution;

[0050] (2) Transfer the chitosan solution prepared in step (1) to a hydrothermal reactor, heat it to 250 °C, and conduct constant temperature hydrothermal carbonization for 24 h. After the reaction, cool to room temperature and dialyze with a 3000 D dialysis bag. Freeze drying to obtain a black powder, which is chitosan-based carbon spheres;

[0051] (3) According to the mass ratio of chitosan-based carbon spheres and KOH particles of 1:3, weigh 0.5 g of chitosan-based carbon spheres and 1.5 g of KOH particles obtained in step (2), place them in an agate mortar, and grind them thoroughly After mixing, in a nitrogen atmosphere, the t...

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Abstract

The invention discloses a chitosan-based porous carbon sphere and a preparation method thereof. The preparation method disclosed by the invention comprises the following steps: taking chitosan as a carbon precursor and a diluted hydrochloric acid solution as a solvent; carrying out low-temperature hydrothermal carbonization to obtain a chitosan-based carbon sphere; then taking alkaline melted saltKOH as a pore-forming agent and carrying out high-temperature carbonization activation under a nitrogen gas atmosphere; carrying out acid washing; washing with water until a product is neutral; carrying out freeze drying to obtain the chitosan-based porous carbon sphere. According to the chitosan-based porous carbon sphere, an adopted carbonization raw material is wide and low in cost, is safe and has no toxicity and can be regenerated; the preparation method has the advantages of relatively low reaction temperature, simplicity in operation, energy saving and environment protection; the prepared chitosan-based porous carbon sphere has a relatively high specific surface area (the specific surface area is 2400 to 3500 m<2> / g), abundant three-dimensional porous structures (a pore channel comprises a micro-pore and a mesopore and the pore diameter is 0.5 to 2.5 nm), good stability and high adsorption performance, can be used as an efficient adsorbent and an electrode material and is applied to the fields of sewage treatment and super-capacitors.

Description

technical field [0001] The invention relates to the technical field of industrial wastewater treatment and energy chemical industry, in particular to a chitosan-based porous carbon sphere and a preparation method thereof. Background technique [0002] Porous carbon material is a carbon material with a pore structure, mainly using carbon as the basic skeleton. The pore structure of porous carbon materials is determined by its material type, and its pore shape is generally divided into spherical, cylindrical, and conical. The raw materials of porous carbon materials are widely available and easy to obtain. According to practical applications, porous carbon materials with various shapes and controllable channels can be prepared, such as porous carbon spheres, carbon films, carbon rods, and carbon fibers. Porous carbon materials have the characteristics of light weight, high special surface area (SSA), large porosity, good chemical stability, high mechanical strength, high temp...

Claims

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Application Information

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IPC IPC(8): C01B32/318C01B32/348B01J20/20B01J20/30C02F1/28H01G11/34H01G11/44H01G11/24H01G11/86
CPCB01J20/20C02F1/283C01B32/318C01B32/348H01G11/24H01G11/34H01G11/44H01G11/86Y02E60/13
Inventor 罗继文吴正国邓伟杰吴泽琪黄曼妥顾孟媛
Owner SOUTH CHINA NORMAL UNIVERSITY
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