IP Library Granted Patent US 10,464,811
Granted Patent B2
US 10,464,811 · App. 12/754,519 · Granted Nov 5, 2019

Method of forming a particulate porous metal oxide or metalloid oxide

Inventors: Yanhui Yang (Singapore, SG); Siu-Choon Ng (Singapore, SG); Xianbin Liu (Singapore, SG); Laisheng Li (Singapore, SG); Yu Du (Singapore, SG)
Assignee: NANYANG TECHNOLOGICAL UNIVERSITY
C01B13/36B01J20/103B01J20/283B01J20/28004B01J20/28019B01J20/28047B01J20/28064B01J20/28066B01J20/28069B01J20/28083B01J20/3204B01J20/3219B01J29/0308B01J29/0325B01J31/1633C01B13/363C01B37/02B01J2531/18C01P2002/01C01P2002/72C01P2002/86C01P2004/03C01P2006/12C01P2006/14C01P2006/16
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Quick Facts
Patent No.
US 10,464,811
App. No.
12/754,519
Granted
Nov 5, 2019
Kind
B2
Abstract

The present invention relates to a method of forming a particulate porous metal oxide or metalloid oxide, as well as uses of the obtained a particulate porous metal oxide or metalloid oxide. A solution of a non-ionic surfactant and either an ionic surfactant or an inorganic salt is formed in an acidic aqueous solution. A metal oxide precursor or a metalloid oxide precursor is added. The formed reaction mixture is heated under reflux upon agitation for a period sufficient to obtain a particulate porous metal oxide or metalloid oxide.

Claims (24)

1. A method of forming a particulate porous metal oxide or metalloid oxide, the method comprising:

forming an acidic aqueous solution of a non-ionic surfactant and an ionic surfactant, wherein the non-ionic surfactant and the ionic surfactant self-assemble in the acidic aqueous solution to form a micelle and the ionic surfactant forms a core of the micelle;

adding to the solution a metal oxide precursor or a metalloid oxide precursor, thereby forming a reaction mixture, the reaction mixture comprising the micelle and the metal oxide precursor or the metalloid oxide precursor;

agitating the reaction mixture; and

heating the reaction mixture under reflux following agitation for a period of time sufficient to obtain a particulate porous metal oxide or metalloid oxide.

2. The method of claim 1 , wherein agitating the reaction mixture is carried out at an elevated temperature below the boiling point thereof for a period of time sufficient to allow a gel to form.

3. The method of claim 1 , wherein heating the reaction mixture under reflux following agitation is carried out in the presence of an alcohol.

4. The method of claims 1 , wherein the acidic aqueous solution further comprises an alcohol.

5. The method of claim 1 , wherein the metal oxide precursor or metalloid oxide precursor is an alkoxide.

6. The method of claim 1 , further comprising removing the surfactant from the product obtained by heating the reaction mixture for a sufficient period of time.

7. The method of claim 6 , wherein removing the surfactant is carried out by one of (i) calcining the product obtained by heating the reaction mixture under reflux for a sufficient period of time and (ii) extracting the surfactant from the product obtained by heating the reaction mixture under reflux for a sufficient period of time with a suitable solvent.

8. The method of claim 7 , wherein the solvent is ethanol.

9. The method of claim 1 , wherein the non-ionic surfactant is a polyether.

10. The method of claim 1 , wherein the ionic surfactant is one of an ionic liquid and an alkyl ammonium salt.

11. The method of claim 1 , wherein pH of the acidic aqueous solution is selected in the range from about pH 1 to about pH 6.

12. The method of claim 1 , wherein forming the acidic aqueous solution further comprises adding an alcohol.

13. The method of claim 1 , wherein the non-ionic surfactant is used in a ratio between about 0.001 and about 0.007 to the metal oxide precursor or the metalloid oxide precursor.

14. The method of claim 1 , wherein the ionic surfactant is used in a ratio between about 0.01 and about 0.04 to the metal oxide precursor or the metalloid oxide precursor.

15. The method of claim 2 , wherein the elevated temperature below the boiling point of the reaction mixture at which a gel is allowed to form is selected in the range from about 35 to about 65° C.

16. The method of claim 1 , wherein the method is a method of forming a UPLC matrix.

17. The method of claim 1 , wherein the acidic aqueous solution further comprises an inorganic salt.

18. The method of claim 1 , wherein the particulate porous metal oxide or metalloid oxide has one or more mesopores having a pore diameter ranging from about 2 nm to about 50 nm.

19. The method of claim 1 , wherein the metal oxide precursor or the metalloid precursor are nanoparticles.

20. The method of claim 1 , further comprising immobilizing a molecule or moiety onto or into the particulate porous metal oxide or metalloid oxide.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 25, 2011
From: YANG, YANHUI; NG, SIU-CHOON; LIU, XIANBIN; LI, LAISHENG; DU, YU
To: NANYANG TECHNOLOGICAL UNIVERSITY
Reel/Frame 026807/0594 →
Continuity (2)
Provisional Application 61166802 · Apr 6, 2009
Related Publication 20100254890A1 · Oct 7, 2010