Preparation method of sulfonated two-dimensional titanium carbide nanosheet

Patent metadata

Field	Value
Publication number	US-10508039-B2
Application number	US-201615735238-A
Country	US
Kind code	B2
Filing date	May 6, 2016
Priority date	Jul 3, 2015
Publication date	Dec 17, 2019
Grant date	Dec 17, 2019

Abstract

The present invention discloses a preparation method of a sulfonated two-dimensional titanium carbide nanosheet, which comprises the following steps of preparing two-dimensional titanium carbide by using aluminum atomic layers in hydrofluoric acid chemical stripping layer-shaped titanium aluminum carbide; preparing sulfanilic acid diazosalt; conducting a sulfonation reaction between the two-dimensional titanium carbide and the sulfanilic acid diazosalt to prepare the sulfonated two-dimensional titanium carbide nanosheet. The sulfonated two-dimensional titanium carbide nano material prepared through the present invention has good dispersity in water and common organic solvents, and a single-layer or few-layer sulfonated two-dimensional titanium carbide nanosheet with large size and high quality can be obtained after ultrasonic treatment is performed on a dispersion liquid. The preparation method has the characteristics of low production cost, easiness in obtaining raw materials, and simplicity and controllability during preparation.

First claim

The invention claimed is:

1. A preparation method of a sulfonated two-dimensional titanium carbide nanosheet, comprising:
(1) preparing two-dimensional titanium carbide sediment by using aluminum atomic layers in hydrofluoric acid chemical stripping layer-shaped titanium aluminum carbide;
(2) redispersing the two-dimensional titanium carbide sediment obtained in step (1) into water to obtain a two-dimensional titanium carbide suspension;
(3) dissolving sulfanilic acid and sodium nitrite in a hydrochloric acid solution to react under an ice-bath condition to obtain sulfanilic acid diazosalt solution;
(4) adding the sulfanilic acid diazosalt solution obtained in step (3) into the two-dimensional titanium carbide suspension liquid obtained in step (2), reacting for a certain time by magnetic stirring under the ice-bath condition to make the two-dimensional titanium carbide have a sulfonation reaction with the sulfanilic acid diazosalt, so as to obtain a sulfonated two-dimensional titanium carbide solution; and
(5) centrifugalizing and precipitating the sulfonated two-dimensional titanium carbide solution obtained in step (4), then washing the solution by deionized water until the pH is 5 to 6, then filtering the solution by a millipore filter and redispersing the solution into water to obtain a sulfonated two-dimensional titanium carbide dispersion liquid, then conducting ultrasonic treatment on the dispersion liquid to obtain a single-layer or few-layer sulfonated two-dimensional titanium carbide dispersion liquid, and then freezing and drying the dispersion liquid to obtain sulfonated two-dimensional titanium carbide powder.

2. The preparation method of a sulfonated two-dimensional titanium carbide nanosheet according to claim 1 , wherein, in step (1), the reaction condition of the titanium aluminum carbide and the hydrofluoric acid is that: the concentration of the hydrofluoric acid is 10 to 50 wt %, a stirring reaction is conducted for 2 to 8 h at a stirring speed of 1500 to 2000 rpm under 25 to 60° C., and then the reaction solution is filtered and repeatedly washed till the pH is neutral, and then centrifuged to obtain the two-dimensional titanium carbide sediment.

3. The preparation method of a sulfonated two-dimensional titanium carbide nanosheet according to claim 1 , wherein, in step (2), the concentration of the two-dimensional titanium carbide sediment after being redispersed into the water is 0.01 to 0.05 g/ml.

4. The preparation method of a sulfonated two-dimensional titanium carbide nanosheet according to claim 1 , wherein, in step (3), the mass ratio of the sulfanilic acid to the sodium nitrite and the hydrochloric acid solution is 40 to 50:8 to 12:10 to 15.

5. The preparation method of a sulfonated two-dimensional titanium carbide nanosheet according to claim 1 , wherein, in step (4), the volume ratio of the two-dimensional titanium carbide suspension liquid to the sulfanilic acid diazosalt solution is 1:1 to 5.

6. The preparation method of a sulfonated two-dimensional titanium carbide nanosheet according to claim 1 , wherein, in step (4), the time of the sulfonation reaction between the two-dimensional titanium carbide and the sulfanilic acid diazosalt is 2 to 6 h.

7. The preparation method of a sulfonated two-dimensional titanium carbide nanosheet according to claim 1 , wherein, in step (5), the centrifugal condition of the sulfonated two-dimensional titanium carbide nanosheet is 4000 to 6000 rpm and centrifugation for 5 to 8 min.

8. The preparation method of a sulfonated two-dimensional titanium carbide nanosheet according to claim 1 , wherein, in step (5), the ultrasonic treatment time of the sulfonated two-dimensional titanium carbide dispersion liquid is 1 to 4 h.

Assignees

• Univ Hohai

Inventors

• Zhang Jianfeng
• Wang Hongbing
• Wu Yuping
• Zhang Xin

Classifications

• C01B32/921 Primary

  Titanium carbide · CPC title

• C01B32/907 Primary

  Oxycarbides; Sulfocarbides; Mixture of carbides · CPC title

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title