IP Library › Granted Patent US 10,160,659
Granted Patent B2
US 10,160,659 · App. 15/853,906 · Granted Dec 25, 2018

Titanium-dioxide-based double-layer hollow material, preparation method thereof, and application thereof in photocatalytic treatment of hydrogen sulfide

Inventors: Jianmei Lu (Suzhou, CN); Dongyun Chen (Suzhou, CN); Jun Jiang (Suzhou, CN)
Assignee: SOOCHOW UNIVERSITY
C01G23/08B01D53/52B01J35/004B05D1/18B05D7/52B29B11/14C01B17/167C01G23/053C08J7/12C08L25/06B05D2201/02B05D2451/00C01P2002/30C01P2004/03C01P2004/04C01P2004/32C01P2004/34C01P2004/64C08K2003/2241
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Quick Facts
Patent No.
US 10,160,659
App. No.
15/853,906
Filed
Dec 25, 2017
Granted
Dec 25, 2018
Kind
B2
Art Unit
1736
USPC
423/230
Abstract

A preparation method of a titanium-dioxide-based double-layer hollow material includes the following steps: (1) using polystyrene nanospheres with particle size of 180 nm as a template, tetrabutyl titanate as a precursor, to prepare hollow titanium dioxide by calcining; (2) subjecting said hollow titanium dioxide to carboxylation modification to prepare carboxylated titanium dioxide; and (3) dispersing said carboxylated titanium dioxide in ethanol, using chromic nitrate nonahydrate as an assembly agent and trimesic acid as a crosslinking agent to carry out layer-by-layer self-assembly so as to prepare the titanium-dioxide-based double-layer hollow material.

Claims (17)

1. A preparation method of a titanium-dioxide-based double-layer hollow material, which comprises following steps:

(1) using polystyrene nanospheres with particle size of 180 nm as a template, tetrabutyl titanate as a precursor, to prepare hollow titanium dioxide by calcining;

(2) subjecting said hollow titanium dioxide to carboxylation modification to prepare carboxylated titanium dioxide;

(3) dispersing said carboxylated titanium dioxide in ethanol, using chromic nitrate nonahydrate as an assembly agent and trimesic acid as a crosslinking agent to carry out layer-by-layer self-assembly so as to prepare the titanium-dioxide-based double-layer hollow material.

2. The preparation method of a titanium-dioxide-based double-layer hollow material according to claim 1 , wherein in step (1), heating styrene aqueous solution to 80 to 90° C. in the presence of a surfactant in nitrogen atmosphere; and adding an aqueous solution of initiator in drops, polymerizing for 10 to 20 hours; and after the polymerization, adding sodium chloride to obtain a precipitate, and then washing the precipitate with deionized water and then drying at 60° C. to prepare a polystyrene nanosphere.

3. The preparation method of a titanium-dioxide-based double-layer hollow material according to claim 1 , wherein in step (1), calcining is carried out at 500 to 700° C. for 2 to 3 hours, and the rate of heating is 1 to 5° C./min.

4. The preparation method of a titanium-dioxide-based double-layer hollow material according to claim 1 , wherein in step (1), adding tetrabutyl titanate into acetonitrile to prepare the tetrabutyl titanate solution by stirring; adding polystyrene nanospheres into a solvent to prepare a polystyrene suspension with ultrasonic dispersion; and then dripping ammonia, deionized water and tetrabutyl titanate solution into the polystyrene suspension, stirring for 1 hour to prepare a mixed liquid; and then washing the mixed liquid and centrifuging to obtain solid, drying and calcining the solid to prepare hollow titanium dioxide particles; the mass ratio of tetrabutyl titanate, polystyrene nanospheres and ammonia is 30:1:20.

5. The preparation method of a titanium-dioxide-based double-layer hollow material according to claim 1 , wherein in step (2), the carboxylation modification is adding the hollow titanium dioxide to an ethanol solution of a silane coupling agent and stirring for 8 to 10 hours to give a solid; and then taking the solid into an the N, N-dimethylformamide solution of succinic anhydride and stirring for 8 to 10 hours to obtain carboxylated titanium dioxide; the mass ratio of titanium dioxide, silane coupling agent and succinic anhydride is 50:1:1.

6. The preparation method of a titanium-dioxide-based double-layer hollow material according to claim 1 , wherein in step (3), each self-assembly step is adding an ethanol solution of chromium nitrate nonahydrate to the carboxylated titanium dioxide ethanol dispersion, stirring and then centrifuging with ethanol and then adding a trimesic acid ethanol solution to continue stirring; then washing and centrifuging to remove the liquid.

7. The preparation method of a titanium-dioxide-based double-layer hollow material according to claim 1 , wherein in step (3), the mass ratio of carboxylated titanium dioxide, chromic nitrate nonahydrate and trimesic acid is 20:1:1, and the number of times of layer-by-layer self-assembly is 10 to 20.

8. Titanium-dioxide-based double-layer hollow material prepared by the preparation method according to claim 1 .

9. A method of photocatalytically treating hydrogen sulfide comprising:

providing the titanium-dioxide-based double-layer hollow material according to claim 8 ; and

treating hydrogen sulfide with the titanium-dioxide-based double-layer hollow material.

10. A method of treating polluted gas comprising:

providing the titanium-dioxide-based double-layer hollow material according to claim 8 ; and

treating polluted gas with the titanium-dioxide-based double-layer hollow material.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 25, 2017
From: LU, JIANMEI; CHEN, DONGYUN; JIANG, JUN
To: SOOCHOW UNIVERSITY
Reel/Frame 044480/0099 →
Priority Claims (1)
CN 2016 1 1239594 · Dec 28, 2016 · national
Continuity (1)
Related Publication 20180179079A1 · Jun 28, 2018