Method to co-synthesize amorphous and crystalline materials in the presence of ODSO

Patent metadata

Field	Value
Publication number	US-12522509-B2
Application number	US-202218057910-A
Country	US
Kind code	B2
Filing date	Nov 22, 2022
Priority date	Nov 22, 2022
Publication date	Jan 13, 2026
Grant date	Jan 13, 2026

Abstract

The present disclosure is directed to a method to co-synthesize amorphous and crystalline porous materials, including a phase of crystalline solids possessing well-defined structures and uniform pore sizes, and an amorphous phase. A sol-gel formulation which includes a water-soluble fraction of ODSO as an additional component is provided that precipitates multiple solid phases.

First claim

What is claimed is:

1 . A method to co-synthesize amorphous material and crystalline material comprising:
forming a homogeneous aqueous mixture of precursors and reagents effective for a crystalline material and/or an amorphous material, water and an effective amount of water-soluble oxidized disulfide oil (ODSO); and heating the homogeneous aqueous mixture under conditions and for a time effective to form a precipitate suspended in a supernatant as an intermediate suspension, wherein the precipitate comprises crystalline material and amorphous material.

2 . The method of claim 1 , wherein the crystalline material comprises about 0.1-99.9 percent by mass of the precipitate and wherein at least a portion of remaining precipitate comprises amorphous material.

3 . The method of claim 1 , wherein the amorphous material comprises one or more of silica, alumina or silica-alumina.

4 . The method as in claim 1 , wherein the crystalline material comprises a crystalline aluminosilicate zeolite, and wherein the precursors and reagents comprise a silica source, an aluminum source, an alkali metal source, an optional structure directing agent and an optional seed material.

5 . The method as in as in claim 4 , wherein the alkali metal source is sodium, and wherein:
the crystalline aluminosilicate comprises zeolite Y and a mass ratio of ODSO to sodium from the alkali metal source is in the range of about 1.9-2.4; or the crystalline aluminosilicate comprises MFI zeolite and a mass ratio of ODSO to sodium from the alkali metal source is in the range of about 7.9-8.9; and wherein increased mass ratio of ODSO to sodium within the ranges increases a relative amount of amorphous material in the precipitate.

6 . The method as in claim 4 , wherein the structure directing agent is used to stabilize the structure of the crystalline aluminosilicate.

7 . The method as in claim 6 , wherein the structure directing agent includes one or more of quaternary ammonium ions, trialkylamines, dialkylamines, monoalkylamines, cyclic amines, alkylethanol amines, cyclic diamines, alkyl diamines, alkyl polyamines, and other templates including alcohols, ketones, morpholine and glycerol.

8 . The method as in claim 4 , wherein the optional seed material is included and wherein the seed material comprises zeolite structures of the same or similar crystalline framework structure as the crystalline aluminosilicate:
wherein the crystalline aluminosilicate comprises MFI zeolites and seed materials comprise or more of include ZSM-5 (MFI), ZSM-8 (MFI), ZSM-11 (MEL) and Silicalite-1 (MFI); or wherein the crystalline aluminosilicate comprises beta zeolites and, seed materials comprise beta zeolites; or wherein the crystalline aluminosilicate comprises mordenite zeolites, seed materials comprise other mordenite zeolites; or wherein the crystalline aluminosilicate comprises FAU zeolites, seed comprise zeolite Y, zeolite X, USY zeolite, faujasite zeolite or small protozeolitic species (gels).

9 . The method as in claim 1 , wherein the precursors and reagents are effective for a crystalline material comprising a crystalline aluminosilicate, and wherein the precursors and reagents comprise a silica source, an aluminum source, an optional structure directing agent and an optional seed material, and wherein an alkali metal source is provided from a pH modified ODSO composition comprising an aqueous mixture of one or more water-soluble ODSO compounds and an effective amount of an alkaline agent, and wherein the alkaline agent includes an alkali metal component as the alkali metal source.

10 . The method as in claim 1 , wherein the crystalline material comprises pure silica zeolite, and wherein the precursors and reagents comprise a silica source, and one or both of a structure directing agent and a seed material.

11 . The method as in claim 1 , wherein the crystalline material comprises aluminophosphate, and wherein the precursors and reagents comprise an aluminum source, a phosphorus source, an acid medium, an optional structure directing agent and an optional seed material.

12 . The method as in claim 1 , wherein the crystalline material comprises silicoaluminophosphate, and wherein the precursors and reagents comprise an aluminum source, a silica source, a phosphorus source, an acid medium, an optional structure directing agent and an optional seed material.

13 . The method as in claim 1 , wherein the crystalline material comprises metal aluminophosphate, and wherein the precursors and reagents comprise an aluminum source, a metal source, a phosphorus source, an acid medium, an optional structure directing agent and an optional seed material.

14 . The method as in claim 1 , wherein the mixture of precursors and reagents includes an aluminum source is selected from the group consisting of aluminates, alumina, other zeolites, aluminum colloids, boehmites, pseudo-boehmites, aluminum hydroxides, aluminum salts, aluminum alkoxides, aluminum wire and alumina gels.

15 . The method as in claim 1 , wherein the mixture of precursors and reagents includes a silica source is selected from the group consisting of sodium silicate (water glass), rice husk, fumed silica, precipitated silica, colloidal silica, silica gels, zeolites, dealuminated zeolites, silicon hydroxides and silicon alkoxides.

16 . The method as in claim 1 , wherein:
the homogeneous aqueous mixture is (optionally) aged before being subjected to heating for a period of about 0-48 hours; the homogeneous aqueous mixture is heated at a temperature in the range of about 90-200° C.; the homogeneous aqueous mixture is heated at autogenous pressure or a pressure in the range of atmospheric to 17 bar; and the homogeneous aqueous mixture is heated for a crystallization time period within the range of about 0.1-8 days.

17 . The method as in claim 1 , wherein the ODSO is derived from oxidation of disulfide oil compounds present in an effluent refinery hydrocarbon stream recovered following catalytic oxidation of mercaptans present in a mercaptan-containing hydrocarbon stream.

18 . The method as in claim 1 , wherein the one or more ODSO compounds comprise ODSO compounds having 3 or more oxygen atoms and 1 to 20 carbon atoms, and are contained in a mixture having an average density greater than about 1.0 g/cc and an average boiling point greater than about 80° C.

19 . The method as in any claim 1 , wherein the ODSO compounds have 3 or more oxygen atoms and include:
one or more compounds selected from the group consisting of (R—SOO—SO—R′), (R—SOO—SOO—R′), (R—SO—SOO—OH), (R—SOO—SOO—OH), (R—SOO—SO—OH), (R′—SO—SO—OR), (R′—SOO—SO—OR), (R′—SO—SOO—OR) and (R′—SOO—SOO—OR), two or more compounds selected from the group consisting of (R—SOO—SO—R′), (R—SOO—SOO—R′), (R—SO—SOO—OH), (R—SOO—SOO—OH), (R—SOO—SO—OH), (R′—SO—SO—OR), (R′—SOO—SO—OR), (R′—SO—SOO—OR) and (R′—SOO—SOO—OR); one or more 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); or two or more 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); wherein R and R′ are C1-C10 alkyl or C6-C10 aryl groups.

20 . A method of producing support particles for catalyst comprising:
providing amorphous material and crystalline material co-synthesized as in claim 1 ; mixing and kneading the co-synthesized amorphous material and crystalline material with an effective amount

Assignees

• Saudi Arabian Oil Co

Inventors

• Hodgkins Robert Peter
• Koseoglu Omer Refa

Classifications

• C01B39/24

  Type Y {(C01B39/205 takes precedence)} · CPC title

• C01B39/265

  using at least one organic template directing agent · CPC title

• C01B39/46

  Other types characterised by their X-ray diffraction pattern and their defined composition {(C01B39/023, C01B39/026, C01B39/06 take precedence)} · CPC title

• C01B39/026

  After-treatment · CPC title

• C01B39/04 Primary

  using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound · CPC title