Composite loaded with nano-magnesium hydride and preparation method thereof

Patent metadata

Field	Value
Publication number	US-12227413-B2
Application number	US-202218557452-A
Country	US
Kind code	B2
Filing date	Oct 24, 2022
Priority date	Oct 25, 2021
Publication date	Feb 18, 2025
Grant date	Feb 18, 2025

Abstract

Disclosed is a method for preparing a composite loaded with nano-magnesium hydride, including: adding a cationic surfactant into an aqueous dispersion of a two-dimensional transition metal carbide such that a nanosheet of the two-dimensional transition metal carbide wrinkles, to avoid re-stacking, and then washing and drying; placing a dried product into a sealed container, vacuuming the sealed container, heating to a high temperature, and holding at the high temperature for a period of time; filling the sealed container with high-pressure hydrogen and holding for a period of time to obtain a heated product; adding the heated product and dibutyl magnesium into an organic solvent, conducting ultrasonic dispersion, then heating under stirring at a hydrogen pressure of 3 MPa to 6 MPa and a temperature of 180° C. to 220° C. for 12 h to 48 h, and centrifuging and drying to obtain the composite loaded with nano-magnesium hydride.

First claim

What is claimed is:

1. A method for preparing a composite loaded with nano-magnesium hydride, comprising:
step (1):
adding a cationic surfactant into an aqueous dispersion of a two-dimensional transition metal carbide such that a nanosheet of the two-dimensional transition metal carbide wrinkles, to obtain a wrinkled two-dimensional transition metal carbide, and
washing and drying the wrinkled two-dimensional transition metal carbide to obtain a dried product;
step (2):
placing the dried product obtained from step (1) into a sealed container, vacuuming the sealed container, heating the dried product to a temperature of 600° C. to 1,000° C., and holding the dried product at the temperature for 2 h to 5 h to obtain a heated product, and
filling the sealed container with 1 MPa to 10 MPa of hydrogen and holding the heated product for 2 h to 5 h to obtain a product; and
step (3):
adding the product obtained from step (2) and dibutyl magnesium into an organic solvent to obtain a mixture,
subjecting the mixture to ultrasonic dispersion to obtain a dispersion mixture,
heating the dispersion mixture under stirring at a hydrogen pressure of 3 MPa to 6 MPa and a temperature of 180° C. to 220° C. for 12 h to 48 h to obtain a heated dispersion mixture, and
centrifuging and drying the heated dispersion mixture to obtain the composite loaded with nano-magnesium hydride.

2. The method for preparing a composite loaded with nano-magnesium hydride of claim 1 , wherein the cationic surfactant is a nitrogen-containing organic amine derivative.

3. The method for preparing a composite loaded with nano-magnesium hydride of claim 2 , wherein the nitrogen-containing organic amine derivative is cetyltrimethylammonium bromide (CTAB).

4. The method for preparing a composite loaded with nano-magnesium hydride of claim 1 , wherein in step (1), the cationic surfactant is dissolved in deionized water, and a resulting solution is then added into the aqueous dispersion of the two-dimensional transition metal carbide under stirring.

5. The method for preparing a composite loaded with nano-magnesium hydride of claim 1 , wherein heating the dried product to a temperature of 600° C. to 1,000° C. in step (2) is conducted at a rate of 5° C./min to 10° C./min.

6. The method for preparing a composite loaded with nano-magnesium hydride of claim 1 , wherein the organic solvent in step (3) comprises one or more selected from the group consisting of cyclohexane, hexane, and heptane.

7. A method for preparing a composite loaded with nano-magnesium hydride, comprising:
step (1):
adding acidified melamine into an aqueous dispersion of a two-dimensional transition metal carbide such that a nanosheet of the two-dimensional transition metal carbide wrinkles, to obtain a wrinkled two-dimensional transition metal carbide, and
washing and drying the wrinkled two-dimensional transition metal carbide to obtain a dried product;
step (2):
placing the dried product obtained from step (1) into a sealed container, vacuuming the sealed container, heating the dried product to a temperature of 600° C. to 1,000° C. and holding the dried product at the temperature for 2 h to 5 h to obtain a heated product, and
filling the sealed container with 1 MPa to 10 MPa of hydrogen and holding the heated product for 2 h to 5 h to obtain a product; and
step (3):
adding the product obtained from step (2) and dibutyl magnesium into an organic solvent to obtain a mixture,
subjecting the mixture to ultrasonic dispersion to obtain a dispersion mixture,
heating the dispersion mixture under stirring at a hydrogen pressure of 3 MPa to 6 MPa and a temperature of 180° C. to 220° C. for 12 h to 48 h to obtain a heated dispersion mixture, and
centrifuging and drying the heated dispersion mixture to obtain the composite loaded with nano-magnesium hydride.

Assignees

• Univ Shanghai Jiaotong

Inventors

• Zou Jianxin
• Zhu Wen
• Ren Li

Classifications

• Y02E60/32

  Hydrogen storage · CPC title

• C01B3/0078 Primary

  Composite solid storage media, e.g. mixtures of polymers and metal hydrides, coated solid compounds or structurally heterogeneous solid compounds · CPC title