Method for manufacture of amorphous silica-alumina composition in the presence of ODSO

Patent metadata

Field	Value
Publication number	US-11649169-B2
Application number	US-202117493201-A
Country	US
Kind code	B2
Filing date	Oct 4, 2021
Priority date	Oct 4, 2021
Publication date	May 16, 2023
Grant date	May 16, 2023

Abstract

A method for the preparation of an amorphous silica-alumina composition is provided that advantageously utilizes as a component oxidized disulfide oil, for example derived from a waste refinery stream of disulfide oil. The amorphous silica-alumina is formed from an aqueous mixture of an aluminum source, a silica source, oxidized disulfide oil, an alkali metal source and optionally a structure directing agent, which is heating under conditions and for a time effective to form the amorphous silica-alumina.

First claim

The invention claimed is:

1. A method for the preparation of an amorphous silica-alumina composition comprising:
forming a homogeneous aqueous mixture of water soluble oxidized disulfide oil (ODSO), a silica source, an aluminum source, an alkali metal source and optionally a structure directing agent;
heating the homogeneous aqueous mixture under conditions and for a time effective to form amorphous silica-alumina as a precipitate suspended in a supernatant as an intermediate suspension; and
recovering the amorphous silica-alumina composition from the intermediate suspension.

2. The method of claim 1 , further comprising calcining the recovered amorphous silica-alumina composition.

3. The method of claim 1 , wherein the intermediate suspension has a pH of less than about 9.

4. The method of claim 1 , wherein the alkali metal source is sodium and the mass ratio of ODSO to sodium is greater than about 9.

5. The method of claim 1 , wherein the recovered amorphous silica-alumina composition has a silica-to-alumina ratio in the range of about 20-1500.

6. The method as in claim 1 , wherein the aluminum source comprises aluminates, alumina, other zeolites, aluminum colloids, boehmites, pseudo-boehmites, aluminum hydroxides, aluminum salts, aluminum alkoxides or alumina gels.

7. The method as in claim 1 , wherein the silica source comprises sodium silicate (water glass), fumed silica, precipitated silica, colloidal silica, silica gels, zeolites, dealuminated zeolites, silicon hydroxides or silicon alkoxides.

8. The method as in claim 1 , wherein a structure directing agent is used, and wherein the structure directing agent comprises quaternary ammonium cation compounds, bifunctional dicationic molecules containing a long aliphatic chain, dual-porogenic surfactants, silylated polyethylenimine polymers, amphiphilic organosilanes, or hydrophilic cationic polyelectroyltes/polymers.

9. The method as in claim 8 , wherein the structure directing agent comprises quaternary ammonium cation compounds selected from the group consisting of tetramethylammonium (TMA) cation compounds, tetraethylammonium (TEA) cation compounds, tetrapropylammonium (TPA) cation compounds, tetrabutylammonium (TBA) cation compounds, cetyltrimethylammonium (CTA) cation compounds and combinations thereof.

10. The method as in claim 8 , wherein the structure directing agent comprises bifunctional dicationic molecules selected from the group consisting of C 22-6-6 , C 22-6-3 , and poly(ethylene glycol).

11. The method of claim 1 , wherein the ODSO comprises ODSO compounds having 3 or more oxygen atoms.

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

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

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

15. The method of claim 1 , wherein the ODSO comprises ODSO compounds 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.

16. The method of claim 1 , wherein the homogeneous aqueous mixture is formed by:
providing the silica source; and
combining with the silica source
the aluminum oxide source, the alkali metal source, and optionally the structure directing agent; and
the water soluble ODSO;

wherein the water soluble ODSO is added after the aluminum oxide source, the alkali metal source, and optionally the structure directing agent; or wherein the water soluble ODSO is first combined with the aluminum oxide source, the alkali metal source and optionally the structure directing agent, and then combined with the silica source; and
wherein an effective quantity of water for the homogeneous aqueous mixture is provided by using a water-containing silica source, and/or by using an aqueous mixture of the aluminum oxide source, the alkali metal source and optionally the structure directing agent.

17. The method of claim 1 , wherein the homogeneous aqueous mixture is formed by:
providing the aluminum oxide source, the alkali metal source and optionally the structure directing agent as a first mixture; and
combining the first mixture with the silica source and the water soluble ODSO;
wherein the water soluble ODSO is added after the silica source; or wherein the water soluble ODSO is first combined with the silica source, and then combined with the first mixture,
wherein an effective quantity of water for the homogeneous aqueous mixture is provided by using a water-containing silica source, and/or by using an aqueous mixture of the aluminum oxide source, the alkali metal source and optionally the structure directing agent.

18. The method of claim 1 , wherein the homogeneous aqueous mixture is formed by:
combining the water soluble ODSO with the silica source to form a first mixture; and
combining the first mixture with the aluminum oxide source, alkali metal source and optionally the structure directing agent;
wherein an effective quantity of water for the homogeneous aqueous mixture is provided by using a water-containing silica source, and/or by using an aqueous mixture of the aluminum oxide source, the alkali metal source and optionally the structure directing agent.

19. The method of claim 1 , wherein the homogeneous aqueous mixture is formed by:
combining the water soluble ODSO with the aluminum oxide source, the alkali metal source and optionally the structure directing agent to form a first mixture; and
combining the first mixture with the silica source;
wherein an effective quantity of water for the homogeneous aqueous mixture is provided by using a water-containing silica source, and/or by using an aqueous mixture of the aluminum oxide source, the alkali metal source and optionally the structure directing agent.

20. The method of claim 1 , wherein an effective quantity of water for the homogeneous aqueous mixture is provided by using a water-containing silica source, and/or by using an aqueous mixture of the aluminum oxide source, the alkali metal source and optionally the structure directing agent.

Assignees

• Saudi Arabian Oil Co

Inventors

• Koseoglu Omer Refa
• Hodgkins Robert Peter

Classifications

• C01P2002/02

  Amorphous compounds · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• C01B33/18 Primary

  Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof (preparation of aerogels by dehydrating gels C01B33/158; treatment to enhance the pigmenting or filling properties C09C) · CPC title

• C01P2002/88

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

• C01F7/14

  Aluminium oxide or hydroxide from alkali metal aluminates · CPC title