Method of forming a particulate porous metal oxide or metalloid oxide

Patent metadata

Field	Value
Publication number	US-10464811-B2
Application number	US-75451910-A
Country	US
Kind code	B2
Filing date	Apr 5, 2010
Priority date	Apr 6, 2009
Publication date	Nov 5, 2019
Grant date	Nov 5, 2019

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.

First claim

What is claimed is:

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.

Assignees

• Yang Yanhui
• Ng Siu Choon
• Liu Xianbin
• Li Laisheng
• Du Yu
• Univ Nanyang Tech

Inventors

• Yang Yanhui
• Ng Siu-Choon
• Liu Xianbin
• Li Laisheng
• Du Yu

Classifications

• B01J31/1633

  covalent linkages via silicon containing groups · CPC title

• B01J29/0325

  Noble metals · CPC title

• C01P2006/14

  Pore volume · CPC title

• B01J20/28066

  being more than 1000 m2/g · CPC title

• B01J20/28069

  Pore volume, e.g. total pore volume, mesopore volume, micropore volume · CPC title