Amine-supported mesoporous carbon and preparation method and use thereof

Patent metadata

Field	Value
Publication number	US-12285737-B1
Application number	US-202418963457-A
Country	US
Kind code	B1
Filing date	Nov 27, 2024
Priority date	Dec 1, 2023
Publication date	Apr 29, 2025
Grant date	Apr 29, 2025

Abstract

Amine-supported mesoporous carbon and a preparation method and use thereof are provided. The preparation method includes: dissolving glucosamine hydrochloride completely in deionized water; adding aqueous colloidal silica dropwise under stirring for full dispersion; heating, stirring, and conducting evaporation to dryness; grinding to obtain a powder, adding the powder to a crucible, and conducting a hydrothermal reaction to obtain a black powder; oven-drying the black powder, and conducting carbonization in a muffle furnace in a protective gas environment to obtain a carbonized solid; adding the carbonized solid to an ammonium hydrogen fluoride solution to remove silica; repeatedly washing with deionized water, and drying in an oven to obtain nitrogen-doped mesoporous carbon (NC); adding the NC to an amine solution prepared with absolute ethanol, and stirring for full dispersion; and stirring a mixed solution in an oil bath until the absolute ethanol is completely evaporated to obtain the amine-supported mesoporous carbon.

First claim

What is claimed is:

1. A method of preparing amine-supported mesoporous carbon for CO 2 adsorption, comprising the following steps:
S1, dissolving glucosamine hydrochloride completely in deionized water to obtain a solution;
S2, adding aqueous colloidal silica dropwise to the solution obtained in the S1 under stirring, and allowing full dispersion to obtain a first mixed solution; and heating and stirring the first mixed solution, and conducting evaporation to dryness to obtain a brown solid;
S3, grinding the brown solid into a powder, adding the powder to a crucible, placing the crucible in a hydrothermal reactor, and conducting a hydrothermal reaction;
S4, oven-drying a black powder produced after the hydrothermal reaction, and conducting carbonization in a muffle furnace in a protective gas environment to obtain a carbonized solid;
S5, adding the carbonized solid obtained in the S4 to an ammonium hydrogen fluoride solution, and continuously stirring to remove silica; and repeatedly washing with deionized water until a resulting washing solution is neutral, and drying in an oven to obtain nitrogen-doped mesoporous carbon (NC);
S6, adding the NC obtained in the S5 to an amine solution prepared with absolute ethanol, and continuously stirring to allow full dispersion to obtain a second mixed solution; and
S7, stirring the second mixed solution in an oil bath until the absolute ethanol is completely evaporated to obtain the amine-supported mesoporous carbon,
wherein an amine in the S6 is tetraethylenepentamine (TEPA), and an amine load is 50%; and
before the S6, the NC obtained in the S5 is pre-oxidized as follows: stirring in nitric acid with a concentration of 8 mol/L to 12 mol/L at room temperature for 10 h to 20 h, conducting washing and suction filtration until neutral, and oven-drying.

2. The method according to claim 1 , wherein the hydrothermal reaction in the S3 is conducted at 150° C. to 200° C. for 20 h to 30 h.

3. The method according to claim 1 , wherein the protective gas environment in the S4 is as follows: a protective gas is nitrogen, a flow rate is 80 mL/min to 120 mL/min, and a heating rate is 8° C./min to 15° C./min.

4. The method according to claim 1 , wherein the carbonization in the S4 is conducted under the following conditions: a temperature of 800° C. to 1,200° C., and a heat preservation time of 45 min to 90 min.

5. The method according to claim 1 , wherein a concentration of the ammonium hydrogen fluoride solution in the S5 is 0.2 g/mL to 0.5 g/mL.

6. A use of the amine-supported mesoporous carbon for CO 2 adsorption prepared according to claim 1 , comprising: introducing a feed gas comprising a CO 2 gas into a fixed bed carrying the amine-supported mesoporous carbon, and conducting adsorption at 60° C. to 90° C.

7. The use according to claim 6 , further comprising the following regeneration treatment: heating spent amine-supported mesoporous carbon generated after the adsorption in a pure nitrogen environment for regeneration, wherein the regeneration is conducted at 105° C. to 125° C.

Assignees

• Univ Zhejiang

Inventors

• Tang Minghui
• Li Hongxian
• Lu Shengyong
• Liu Qi
• Gong Zhiyuan
• Yan Jianhua

Classifications

• B01J20/3204

  Inorganic carriers, supports or substrates · CPC title

• B01J20/3085

  Chemical treatments not covered by groups B01J20/3007 - B01J20/3078 · CPC title

• B01D53/02

  by adsorption, e.g. preparative gas chromatography {(solid sorbent compositions B01J20/00, preparation of inorganic compounds or elements C01)} · CPC title

• B01J20/3078

  Thermal treatment, e.g. calcining or pyrolizing · CPC title

• B01J20/3071

  Washing or leaching · CPC title