Method for manufacture of mesoporous silica in the presence of thermally expandable microcells

Patent metadata

Field	Value
Publication number	US-12312244-B2
Application number	US-202117347081-A
Country	US
Kind code	B2
Filing date	Jun 14, 2021
Priority date	Jun 14, 2021
Publication date	May 27, 2025
Grant date	May 27, 2025

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 thermally expandable microcells 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 acid 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,
thermally expandable microcells, 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. The method of claim 1 , wherein the aqueous medium is an acidic aqueous medium comprising hydrochloric acid as an acid component.

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

4. 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.

5. The method of claim 1 , wherein the thermally expandable microcells comprise a core containing low-boiling-point liquid hydrocarbon or oxygen-containing hydrocarbon within a thermoplastic shell, wherein the volumes the microcells increase about 5-60 fold under conditions of the condensation reactions.

6. The method of claim 5 , wherein the thermoplastic shell comprises a polymer of acrylonitrile, vinylidene chloride, methyl methacrylate or combinations thereof.

7. The method of claim 5 , wherein the core comprises paraffins with a carbon number between 4 and 8.

8. The method of claim 7 , wherein the core comprises isobutane, isopentane, 2,2,4-trimethylpentane (C 8 H 18 ) or combinations thereof.

9. The method of claim 5 , wherein the core comprises an ether.

10. 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.

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

12. The method as in claim 1 , 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

• C01P2002/72

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

• C01P2002/86

  by NMR- or ESR-data · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• C01P2002/88

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

• C01P2002/76

  by a space-group or by other symmetry indications · CPC title