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Method for preparing high-performance porous carbon material from organic solid wastes through nitrogen-doping hydrothermal operation and activation

A technology of porous carbon materials and organic solids, applied in the field of porous carbon materials, can solve the problems of cumbersome and time-consuming process, cumbersome and time-consuming nitrogen doping process, and inconspicuous micropore characteristics, and achieve the effect of enhancing adsorption performance and improving pores.

Active Publication Date: 2019-10-18
HUAZHONG UNIV OF SCI & TECH
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Problems solved by technology

Among them: Chinese patent document CN107697915A discloses a method for preparing nitrogen-doped porous carbon materials using silk fibroin and amino-terminated hyperbranched polymers as nitrogen sources, but it involves pre-carbonization of biomass raw materials, nitrogen source solution impregnation, and nitrogen doping Heat treatment, activator impregnation and high-temperature activation are multiple steps, and the nitrogen doping process is cumbersome and time-consuming, so it is difficult to popularize and apply in practice
Chinese patent document CN109251031A discloses the use of microwave-assisted hydrothermal mixing of ammonium pentaborate tetrahydrate, followed by high-temperature pyrolysis to obtain porous carbon with a boron content of 10.19~13.05wt.% and a nitrogen content of 15.13~19.5wt.% for supercapacitor applications , but because no activator is used for activation, its specific surface area is lower than 1000m 2 / g, the pore structure needs to be further improved
Chinese patent document CN109354006A discloses the technical scheme of using hydrothermal nitrogen-doped precursors and molecular sieve templates to prepare porous carbon at high temperature. However, under the influence of molecular sieve structure, the porous carbon pore structure is dominated by mesopores, and the specific surface area is up to 910.82m 2 / g, at the same time, the micropore characteristics that play a leading role in gas adsorption are not obvious
[0005] In the above-mentioned existing technical solutions, it involves the use of traditional immersion heat treatment for nitrogen doping, and the process is cumbersome and time-consuming; in addition, the nitrogen-doped intermediate product obtained by using the method of synchronous doping of nitrogen source in the hydrothermal process can be obtained after high-temperature treatment The pore structure of porous carbon materials is mostly in the 1000 m 2 / g or less, lower than the porous carbon material obtained by general activation treatment

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  • Method for preparing high-performance porous carbon material from organic solid wastes through nitrogen-doping hydrothermal operation and activation

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Experimental program
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Embodiment 1

[0033] Step 1. Select wood chips, orange peels and other mass-mixed mixtures as organic solid waste raw materials for preparing nitrogen-doped hydrothermal charcoal, crush and sieve them into powders with a particle size of 50-300 μm, and then follow the organic solid waste and nitrogen-doping agent Add melamine at a mass ratio of 1:2, and then add water at a solid-liquid mass ratio of 1:8 to form a solid-liquid mixture;

[0034] Step 2. Put the solid-liquid mixture in the reactor for hydrothermal carbonization reaction. The hydrothermal temperature is 190°C, the reaction time is 100min, and the reaction pressure is 3.4Mpa. Dry for 12 hours to obtain a solid, i.e. nitrogen-doped hydrothermal charcoal;

[0035] Step 3. Add KHCO according to the mass ratio of nitrogen doping agent and activator 1:0.8 3 Activator, mixed evenly with nitrogen-doped hydrothermal carbon for high-temperature activation, the activation atmosphere is argon, the heating rate is 8°C / min, the activation t...

Embodiment 2

[0038] Compared with embodiment 1, the present embodiment is mainly different in that:

[0039] In step 1, select coconut shells, cigarette butts and other mass-mixed mixtures as organic solid waste raw materials for preparing nitrogen-doped hydrothermal charcoal, and add urea and dicyandiamide according to the mass ratio of organic solid waste and nitrogen-doping agent 1:4 The nitrogen doping agent formed by mixing is added with water at a solid-liquid mass ratio of 1:3 to form a solid-liquid mixture.

[0040] In step 2, 170 ℃ of hydrothermal temperatures, reaction times 10min, reaction pressure 2.2MPa.

[0041] In step 3, add K according to the mass ratio of nitrogen doping agent and activator 1:1 2 CO 3 The activator is mixed evenly with nitrogen-doped hydrothermal charcoal for high-temperature activation, the heating rate is 5°C / min, the activation temperature is 700°C, and the activation time is 1h. The prepared nitrogen-doped porous carbon and nitrogen content is 5.1w...

Embodiment 3

[0044] Compared with embodiment 2, the present embodiment is mainly different in that:

[0045] In step 1, the mixed mixture of sawdust and coconut shell is selected as the organic solid waste raw material for preparing nitrogen-doped hydrothermal charcoal, and the mass ratio of melamine and dicyandiamide is added according to the mass ratio of organic solid waste and nitrogen-doping agent 1:1. The nitrogen doping agent formed by mixing is added with water at a solid-liquid mass ratio of 1:10 to form a solid-liquid mixture.

[0046] In step 2, 200 DEG C of hydrothermal temperature, reaction times 60min, reaction pressure 4.3MPa.

[0047] In step 3, add KOH activator according to the mass ratio of nitrogen-doping agent and activator 1:0.1, mix with nitrogen-doped hydrothermal charcoal and carry out high-temperature activation, heating rate 3 ℃ / min, activation temperature 900 ℃, activation time 2h. The prepared nitrogen-doped porous carbon and nitrogen content is 0.9wt.%, and ...

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Abstract

The embodiment of the invention provides a method for preparing a high-performance porous carbon material from organic solid wastes through nitrogen-doping hydrothermal operation and activation. The method comprises the following steps: by taking coconut shells, orange peel, cigarette ends and saw dust as organic solid wastes, organic nitrogen sources such as melamine, urea and dicyandiamide as hydrothermal nitrogen doping agents, preparing nitrogen-doping hydrothermal charcoal by using an organic solid waste hydrothermal process nitrogen source synchronous doping method; further by taking thenitrogen-doping hydrothermal charcoal as a precursor, performing solid-phase mixing on the precursor with an activator of potassium carbonate, potassium bicarbonate or potassium hydroxide, further performing activation treatment so as to obtain a porous carbon material which is rich in micropore and mesoporous structure and has a specific surface area as high as 1526-3365m<2> / g. Meanwhile, the carbon material has an excellent methylbenzene adsorption and iodine adsorption capability. The method is simple in process, easy in condition control and good in practicability, has considerable application prospects in the field of pollutant adsorption treatment and has good economic benefits and social benefits.

Description

technical field [0001] The invention belongs to the field of porous carbon materials, and in particular relates to a method for preparing high-performance porous carbon materials by doping organic solid waste with nitrogen and activating them through hydrothermal treatment, which can be used to apply high-value organic solid waste to the field of pollutant adsorption. Background technique [0002] Porous carbon materials are widely used in adsorption fields such as air pollution control, gas separation, and energy storage due to their excellent properties such as developed pore structure, good chemical stability, and recyclability. In the pre-carbonization process of porous carbon materials, hydrothermal carbonization treatment has become an ideal pre-carbonization method due to the characteristics of no need for dehydration, high surface activity of solid product hydrothermal carbon, and considerable activation potential. As an ideal porous carbon precursor, hydrothermal ca...

Claims

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Application Information

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IPC IPC(8): C01B32/348C01B32/324
CPCC01B32/324C01B32/348
Inventor 刘欢肖康鑫李杨汪家兴姚洪
Owner HUAZHONG UNIV OF SCI & TECH
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