IP Library Granted Patent US 12,390,771
Granted Patent B2
US 12,390,771 · App. 18/083,155 · Granted Aug 19, 2025

Rigid self-supporting MXene separation membrane and preparation method and use thereof

Inventors: Shuo Chen (Dalian, CN); Chengyu Yuan (Dalian, CN); Qi Zhang (Dalian, CN); Gaoliang Wei (Dalian, CN); Xie Quan (Dalian, CN)
Assignee: DALIAN UNIVERSITY OF TECHNOLOGY
B01D71/0221B01D67/00416B01D67/0058B01D67/006B01D67/0076B01D69/02B01D71/021C01B32/907C01B32/921B01D2323/08B01D2323/10B01D2323/12B01D2323/21815B01D2323/21817B01D2323/28B01D2323/36B01D2323/56B01D2325/26B01D2325/28B01D2325/36
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Quick Facts
Patent No.
US 12,390,771
App. No.
18/083,155
Granted
Aug 19, 2025
Kind
B2
Abstract

The present disclosure provides a rigid self-supporting MXene separation membrane and a preparation method and use thereof, belonging to the technical field of membranes. In the present disclosure, a MXene material is mixed with an aluminum salt powder to conduct one-step membrane formation by hot-pressing. The pressure forms the powder into a membrane and imparts rigidity, enabling a self-supporting structure; the heating breaks an ionic bond of an inorganic metal salt to reach a molten ionic state, and free metal cations react with active oxygen-containing functional groups on the surface of the MXene to form new chemical bonds (such as an Al—O bond); such a chemical bond has higher energy, achieving a desirable anti-swelling effect to improve the membrane stability. The separation membrane further has excellent conductivity and hydrophilicity.

Claims (19)

1. A preparation method of a rigid self-supporting MXene separation membrane, comprising the following steps:

conducting membrane formation on a mixed powder of MXene and an inorganic metal salt by hot-pressing to obtain the rigid self-supporting MXene separation membrane; wherein the membrane formation by hot-pressing is conducted at 150° C. to 300° C. and 5 MPa to 20 MPa for 5 min to 30 min;

the MXene and the inorganic metal salt have a mass ratio of 1:(0.02-0.1); and

the inorganic metal salt comprises an aluminum salt.

2. The preparation method according to claim 1 , wherein the aluminum salt is one or more selected from the group consisting of aluminum chloride, aluminum sulfate, aluminum nitrate, and aluminum silicate.

3. The preparation method according to claim 1 , wherein the MXene is selected from the group consisting of Ti 3 C 2 T x , Ti 2 CT x , Ti 3 CNT x , V 2 CT x , Ti 4 N 3 T x , and Nb 2 CT x .

4. The preparation method according to claim 1 , wherein a preparation method of the MXene comprises the following steps:

mixing a MAX material (corresponding to the MXene), lithium fluoride, and a hydrochloric acid solution and conducting chemical etching on an obtained mixed solution;

conducting solid-liquid separation on an etched product, and mixing an obtained solid precipitate with water; and

subjecting a resulting mixture to ultrasonic exfoliation to obtain the MXene.

5. The preparation method according to claim 4 , wherein the hydrochloric acid solution has a concentration of 8 mol/L to 12 mol/L, the MAX material and the lithium fluoride have a mass ratio of 1:(1.5-2), the MAX material and the hydrochloric acid solution have a dosage ratio of 1 g:(15-30) mL, and the chemical etching is conducted at 45° C. to 80° C. for 24 hours to 48 hours.

6. A rigid self-supporting MXene separation membrane prepared by the preparation method according to claim 1 .

7. The rigid self-supporting MXene separation membrane according to claim 6 , wherein the aluminum salt is one or more selected from the group consisting of aluminum chloride, aluminum sulfate, aluminum nitrate, and aluminum silicate.

8. The rigid self-supporting MXene separation membrane according to claim 6 , wherein the MXene is selected from the group consisting of Ti 3 C 2 T x , Ti 2 CT x , Ti 3 CNT x , V 2 CT x , Ti 4 N 3 T x , and Nb 2 CT x .

9. The rigid self-supporting MXene separation membrane according to claim 6 , wherein a preparation method of the MXene comprises the following steps:

mixing a MAX material (corresponding to the MXene), lithium fluoride, and a hydrochloric acid solution, and conducting chemical etching on an obtained mixed solution;

conducting solid-liquid separation on an etched product, and mixing an obtained solid precipitate with water; and

subjecting a resulting mixture to ultrasonic exfoliation to obtain the MXene.

10. The rigid self-supporting MXene separation membrane according to claim 9 , wherein the hydrochloric acid solution has a concentration of 8 mol/L to 12 mol/L, the MAX material and the lithium fluoride have a mass ratio of 1:(1.5-2), the MAX material and the hydrochloric acid solution have a dosage ratio of 1 g:(15-30) mL, and the chemical etching is conducted at 45° C. to 80° C. for 24 hours to 48 hours.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 16, 2023
From: CHEN, SHUO; YUAN, CHENGYU; ZHANG, QI; WEI, GAOLIANG; QUAN, XIE
To: DALIAN UNIVERSITY OF TECHNOLOGY
Reel/Frame 063003/0928 →
Priority Claims (1)
CN 202111579747.3 · Dec 22, 2021 · national
Continuity (1)
Related Publication 20230191338A1 · Jun 22, 2023
References Cited (2)
CN 112967923A1 · 2021 [cited by examiner]
Long et al., “Self-assembly enabled nano-intercalation for stable high-performance MXene membranes,” Journal of Membrane Science 635 (2021) 119464 (Year: 2021). [cited by examiner]