Preparation method of carbon material for adsorbing hydrophilic ionic liquid

An ionic liquid and carbon material technology, applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., can solve the problems of small adsorption capacity and low adsorption efficiency, and achieve easy operation, energy saving, huge specific surface area and pore volume. Effect

Inactive Publication Date: 2014-07-30
AGRO ENVIRONMENTAL PROTECTION INST OF MIN OF AGRI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the problems of small adsorption capacity and low adsorption efficiency of traditional activated carbon for hydrophilic ionic liquids, the present invention provides a method for

Method used

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  • Preparation method of carbon material for adsorbing hydrophilic ionic liquid
  • Preparation method of carbon material for adsorbing hydrophilic ionic liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Add 20 g of microcrystalline cellulose and 60 mL of distilled water successively under magnetic stirring, and continue stirring for 30 minutes;

[0021] (2) Transfer the mixed solution prepared in step (1) into a stainless steel autoclave lined with polytetrafluoroethylene, seal and heat to 250 o C constant temperature for 10 h, stirring at 1000 rpm;

[0022] (3) Cool to room temperature after the reaction, and wash the resulting black powder alternately with distilled water and ethanol, and dry at 80°C for 12 hours to remove all the water, and obtain carbon microspheres with a particle size of 3 to 5 microns;

[0023] (4) After mixing the carbon microsphere material obtained in step (3) and KOH powder at a mass ratio of 1:4, put it into a muffle furnace, pass in nitrogen gas, and set the temperature at 600 °C under a nitrogen atmosphere. o Heat treatment at C for 2 hours;

[0024] (5) The solid obtained in step (4) was alternately washed with 1 mol / L HCl solution...

Embodiment 2

[0029] (1) Add 10 g of microcrystalline cellulose and 60 mL of distilled water successively under magnetic stirring, and continue stirring for 30 minutes;

[0030] (2) Transfer the mixed solution prepared in step (1) into a stainless steel autoclave lined with polytetrafluoroethylene, seal and heat to 260 o C constant temperature for 8 h, stirring at 1000 rpm;

[0031] (3) Cool to room temperature after the reaction, and wash the resulting black powder alternately with distilled water and ethanol, and dry at 80°C for 12 hours to remove all the water, and obtain carbon microspheres with a particle size of 3 to 5 microns;

[0032] (4) After mixing the carbon microsphere material obtained in step (3) and KOH powder at a mass ratio of 1:2, put it into a muffle furnace, pass in nitrogen gas, and in a nitrogen atmosphere at 600 o Heat treatment at C for 4 hours;

[0033] (5) The solid obtained in step (4) was alternately washed with 1 mol / L HCl solution and distilled water until t...

Embodiment 3

[0037] (1) Add 20 g of microcrystalline cellulose and 50 mL of distilled water successively under magnetic stirring, and continue stirring for 30 minutes;

[0038] (2) Transfer the mixed solution prepared in step (1) into a stainless steel autoclave lined with polytetrafluoroethylene, seal and heat to 250 o C constant temperature for 12 h, stirring at 1000 rpm;

[0039] (3) Cool to room temperature after the reaction, and wash the resulting black powder alternately with distilled water and ethanol, and dry at 80°C for 12 hours to remove all the water, and obtain carbon microspheres with a particle size of 3 to 5 microns;

[0040](4) After mixing the carbon microsphere material obtained in step (3) and KOH powder at a mass ratio of 1:4, put it into a muffle furnace, pass in nitrogen gas, and set the temperature at 600 °C under a nitrogen atmosphere. o Heat treatment at C for 2 hours;

[0041] (5) The solid obtained in step (4) was alternately washed with 1 mol / L HCl solution ...

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Abstract

The invention provides a preparation method of a carbon material for adsorbing hydrophilic ionic liquid. The method comprises the following steps: performing hydrothermal reaction on cellulose which serves as a raw material in a high-pressure hydrothermal reaction kettle to obtain carbon microspheres rich in oxygen-containing groups such as hydroxyl and carboxyl; and activating the carbon microspheres in a muffle furnace by using KOH under the protection of nitrogen atmosphere to obtain a spongy carbon material with the large specific surface area and the surface rich in the oxygen-containing groups. The carbon microspheres with the surface rich in the oxygen-containing groups can be obtained by incomplete hydrothermal carbonization of the cellulose, the specific surface area of the carbon material can be greatly improved by KOH activation under the condition of retaining oxygen-containing chemical groups on the surface, a pore channel structure is improved, a carbon material adsorbent with unique hydrophilic ionic liquid adsorption performance is finally obtained, and the adsorption efficiency and the adsorption capacity are greatly improved. The needed raw materials are common and easily available, the preparation method is simple, and the obtained carbon material adsorbent has good effects on adsorption and recycling of the hydrophilic ionic liquid in wastewater.

Description

technical field [0001] The invention belongs to the field of preparation of biomass adsorbent and its environment and chemical application, in particular, it relates to the incomplete hydrothermal carbonization of cellulose biomass and its KOH activation, thereby obtaining high specific surface area and pore volume and simultaneously surface A method for adsorbents of carbon materials enriched with oxygen-containing functional groups. Background technique [0002] Ionic liquids refer to salts that are in a liquid state at or near normal temperature, usually composed of organic cations and inorganic anions. Due to their good thermal stability and undetectable vapor pressure, ionic liquids have been considered as a green solvent and have been widely used in material preparation, energy storage, biomass utilization, chemical industry, catalysis, and environmental analysis, etc. field. However, recent research results show that ionic liquids have certain toxicity to fleas, alg...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/30C01B31/12C01B32/318C01B32/348
Inventor 漆新华李陆杨
Owner AGRO ENVIRONMENTAL PROTECTION INST OF MIN OF AGRI
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