Method for manufacture of mesoporous silica in the presence of water-soluble ODSO

Patent metadata

Field	Value
Publication number	US-11685663-B2
Application number	US-202117347125-A
Country	US
Kind code	B2
Filing date	Jun 14, 2021
Priority date	Jun 14, 2021
Publication date	Jun 27, 2023
Grant date	Jun 27, 2023

Abstract

Methods of synthesis of mesoporous silica are disclosed. The mesoporous silica synthesized herein, like SBA-15, possesses a two-dimensional, hexagonal, through-hole structure with a space group p6mm. An effective quantity of one or more water-soluble oxidized disulfide oil (ODSO) compounds are used during synthesis to impart distinct characteristics.

First claim

The invention claimed is:

1. A method for the sol-gel synthesis of mesoporous silica having hexagonal p6mm symmetry, the method comprising:
mixing in an aqueous medium under conditions conducive to promote hydrolysis reactions effective quantities of
a surfactant as a soft template material to influence a silica mesoporous structure,
one or more water-soluble oxidized disulfide oil (ODSO) compounds as an acidity modifier, and
a silica source;

heating the mixture under conditions and for a time effective conducive to promote condensation reactions and to form mesoporous silica as a precipitate suspended in a supernatant as an intermediate suspension; and
recovering the mesoporous silica from the intermediate suspension.

2. A method for the sol-gel synthesis of mesoporous silica having hexagonal p6mm symmetry, the method comprising:
mixing in an aqueous medium effective quantities of one or more water-soluble oxidized disulfide oil (ODSO) compounds as an acidity modifier and a surfactant as a soft template material to influence a silica mesoporous structure to form a first mixture;
mixing an effective quantity of a silica source with the first mixture under conditions conducive to promote hydrolysis reactions and form a second mixture;
heating the second mixture under conditions and for a time effective conducive to promote condensation reactions and to form mesoporous silica as a precipitate suspended in a supernatant as an intermediate suspension, and
recovering the mesoporous silica from the intermediate suspension.

3. The method of claim 1 , wherein the aqueous medium is an acidic aqueous medium comprising an acid component as an additional acidity modifier.

4. The method of claim 1 , further comprising treating the mesoporous silica to remove surfactant, wherein treating comprises solvent extraction or thermal treatment.

5. The method as in claim 1 , wherein the hydrolysis reactions occur at a temperature in the range of about 20-65° C., condensation reactions occur at a temperature in the range of about 80-120° C., and wherein removing surfactant is by thermal treatment at a temperature in the range of about 215-600° C.

6. The method of claim 1 , wherein the ODSO compounds include 3 or more oxygen atoms.

7. The method of claim 1 , wherein the ODSO compounds having 1 to 20 carbon atoms.

8. The method of claim 1 , wherein the ODSO compounds have an average density greater than about 1.0 g/cc.

9. The method of claim 1 , wherein the ODSO compounds have an average boiling point greater than about 80° C.

10. The method of claim 1 , wherein the ODSO compounds are selected from the group consisting of (R—SOO—SO—R′), (R—SOO—SOO—R′), (R—SO—SOO—OH), (R—SOO—SOO—OH), (R—SO—SO—OH), (R—SOO—SO—OH), and mixtures thereof, where R and R′ can be the same or different and are alkyl groups comprising 1-10 carbon atoms.

11. The method as in claim 1 , wherein the silica source is selected from the group consisting of tetraethyl orthosilicate (TEOS), tetramethyl orthosilicate (TMOS), tetrapropyl orthosilicate (TPOS), tetrabutyl orthosilicate (TBOS) or sodium (meta)silicate.

12. The method as in claim 1 , wherein the surfactant is a non-ionic surfactant.

13. The method as in claim 1 , wherein the surfactant is a triblock copolymer of ethylene oxide/propylene oxide/ethylene oxide.

14. The method of claim 2 , wherein the aqueous medium is an acidic aqueous medium comprising an acid component as an additional acidity modifier.

15. The method of claim 2 , further comprising treating the mesoporous silica to remove surfactant, wherein treating comprises solvent extraction or thermal treatment.

16. The method as in claim 2 , wherein the hydrolysis reactions occur at a temperature in the range of about 20-65° C., condensation reactions occur at a temperature in the range of about 80-120° C., and wherein removing surfactant is by thermal treatment at a temperature in the range of about 215-600° C.

17. The method of claim 2 , wherein the ODSO compounds include 3 or more oxygen atoms and 1 to 20 carbon atoms.

18. The method of claim 2 , wherein the ODSO compounds have an average density greater than about 1.0 g/cc and an average boiling point greater than about 80° C.

19. The method of claim 2 , wherein the ODSO compounds are selected from the group consisting of (R—SOO—SO—R′), (R—SOO—SOO—R′), (R—SO—SOO—OH), (R—SOO—SOO—OH), (R—SO—SO—OH), (R—SOO—SO—OH), and mixtures thereof, where R and R′ can be the same or different and are alkyl groups comprising 1-10 carbon atoms.

20. The method as in claim 2 ,
wherein the silica source is selected from the group consisting of tetraethyl orthosilicate (TEOS), tetramethyl orthosilicate (TMOS), tetrapropyl orthosilicate (TPOS), tetrabutyl orthosilicate (TBOS) or sodium (meta)silicate, and
wherein the surfactant is a triblock copolymer of ethylene oxide/propylene oxide/ethylene oxide.

Assignees

• Saudi Arabian Oil Co

Inventors

• Hodgkins Robert Peter
• Koseoglu Omer Refa

Classifications

• C01B33/128 Primary

  by acidic treatment of aqueous silicate solutions · CPC title

• C01B33/143

  of aqueous solutions of silicates · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2002/88

  by thermal analysis data, e.g. TGA, DTA, DSC · CPC title

• C01P2004/03

  obtained by SEM · CPC title