Process for epoxidation and catalyst to be used therein

• US 20050085646A1
• Filed: 10/12/2004
• Published: 04/21/2005
• Est. Priority Date: 09/17/2002
• Status: Abandoned Application

• Current Assignee: BASF AG (BASF SE)
• Original Assignee: BASF AG (BASF SE)
• Inventors: Teles, Joaquim Henrique, Rudolf, Peter, Muller, Ulrich, Krug, Georg, Bassler, Peter, Gobbel, Hans-Georg
• Application Number:
  US10/960,989
• Publication Number:
  US 20050085646A1
• Time in Patent Office: Days
• US Class Current: 549/523
• CPC Class Codes: B01J 2229/36 Steaming
• CPC Class Codes: B01J 2229/40 Special temperature treatment, i.e. other than just for template removal
• CPC Class Codes: B01J 29/89 Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium B01J29/005 takes precedence
• CPC Class Codes: B01J 37/10 in the presence of water, e.g. steam
• CPC Class Codes: C07D 301/12 with hydrogen peroxide or inorganic peroxides or peracids
• CPC Class Codes: C07D 301/19 with organic hydroperoxides
• CPC Class Codes: Y02P 20/10 Process efficiency

Abstract

The present invention relates to a process for treating a solid material containing at least one zeolite and being at least partly crystalline or treating a shaped body obtained from said solid material wherein said solid material or shaped body is brought in contact with a composition containing water after at least one of the following steps of an integrated process for producing a solid material or a shaped body containing at least one zeolite: (i) after step (II) of separating the at least partly crystalline solid material from its mother liquor or (ii) after step (S) of shaping said solid material into a shaped body or (iii) after a step (C) of calcining said solid material or said shaped body. The present invention furthermore relates to the solid material obtainable by the inventive process and the shaped body obtainable by the inventive process. The present invention finally relates to the use of the solid material or the shaped body as mentioned above as a catalyst in chemical reactions, in particular in reactions of compounds containing at least one C—C double bond with at least one hydroperoxide.

Claims

1. A process for treating a solid material or a shaped body comprising at least one zeolite, and being at least partly crystalline, wherein said solid material or the shaped body is brought in contact with a composition comprising waters after at least one of the following steps of an integrated process for producing a solid material or a shaped body:

(i) after step (II) of separating the at least partly crystalline solid material from its mother liquors or (ii) after step (S) of shaping said solid material into a shaped body, or (iii) after a step (C) of calcining said solid material or said shaped body.

2. The process according to claim 1, wherein the solid material is brought in contact with a composition comprising water at elevated temperatures with respect to room temperature.

3. The process according to claim 1, wherein the composition comprising water is selected from:

deionized water, water vapor, steam, steam at elevated pressures relative to ambient pressure, supercritical water, aqueous solutions, or ammonia water.

4. The process according to claim 1, wherein the at least one zeolite comprises Ti.

5. The process according to claim 4, wherein the at least one zeolite comprising Ti is selected from materials of the structure classes MFI, MEL, MWW, BEA or combinations thereof.

6. The process according to claim 1, wherein the step of bringing the solid material or the shaped body in contact with a composition comprising water, is performed in a reactor that is used for the synthesis or treatment of the solid material, or in a reactor in which the solid material, or one or more shaped bodies made form the solid material, are used as catalysts in a chemical reaction.

25. The process according to claim 2, wherein the at least one zeolite comprises Ti.

26. The process according to claim 3, wherein the at least one zeolite contains comprises Ti.

7. An integrated process for the production of a solid material, comprising at least one zeolite, said process comprising at least the following steps:

(I) crystallizing, at least partially, at least one solid material comprising at least one zeolite, out of a synthesis mixture, resulting in mixture (I) comprising at least said solid material and a mother liquor;

(II) separating and/or concentrating the solid material in mixture (I);

(W) contacting the solid material from step (II) with a composition comprising water;

(III) agglomerating or granulating or agglomerating and granulating the solid material from step (W);

wherein step (III) is optional.

8. The integrated process according to claim 7, further comprising, after step (W), separating the solid material from at least a part of the composition comprising water.

9. The integrated process according to claim 7, wherein the method of separating and/or concentrating in step (II), is selected from the group consisting of:

ultrafiltration, spray-drying, spray granulating, contacting inert support bodies with the synthesis solution from (I).

13. The integrated process according to claim 7, further comprising, after at least one of the steps (II), (W) or (III), a step (C) of calcining the solid material and/or a shaped body comprising said solid material.

14. The integrated process according to claim 13, wherein said step of calcining is performed at temperatures higher than 400°

C.

27. The integrated process according to claim 8, further comprising, after at least one of the steps (II), (W) or (III), a step (C) of calcining the solid material and/or a shaped body comprising said solid material.

28. The integrated process according to claim 9, further comprising, after at least one of the steps (II), (W) or (III), a step (C) of calcining the solid material and/or a shaped body comprising said solid material.

10. The integrated process for the production of a shaped body comprising at least one zeolite, said process comprising at least the following steps:

(I) crystallizing at least partially, at least one solid material comprising at least one zeolite, out of a synthesis mixture, resulting in mixture (I) comprising at least said solid material and a mother liquor;

(II) separating and/or concentrating the solid material in mixture (I);

(W) contacting the solid material from step (II) with a composition comprising water,

(III) agglomerating or granulating or agglomerating and granulating the solid material from step (W);

wherein step (III) is optional, and wherein, after step (W), or after step (III), at least one step (S) of shaping the solid material into a shaped body is performed.

11. The integrated process according to claim 10, wherein the at least one step of shaping the solid material is selected from:

pelletizing, pressing, extruding, sintering, roasting, or briquetting.

12. The integrated process according to claim 10, wherein the step (W) is performed after the step (S) of shaping the solid material is performed, and wherein said step (W), either replaces the step (W) performed after step (II), or is performed in addition to the step (W) performed after step (II).

29. The integrated process according to claim 10, further comprising, after at least one of the steps (II), (W) or (III), a step (C) of calcining the solid material and/or the shaped body.

30. The integrated process according to claim 11, further comprising, after at least one of the steps (II), (W) or (III), a step (C) of calcining the solid material and/or the shaped body.

31. The integrated process according to claim 12, further comprising, after at least one of the steps (II), (W) or (III), a step (C) of calcining the solid material and/or the shaped body.

15. A solid material obtained by a process of treating a solid material comprising at least one zeolite, and being at least partly crystalline, wherein said solid material is brought in contact with a composition comprising water, after at least one of the following steps of an integrated process for producing said solid material:

(i) after step (II) of separating the at least partly crystalline material from its mother liquor, or (ii) after a step (C) of calcining said solid material or a shaped body comprising said solid material.

16. The solid material according to claim 15, wherein the solid material comprises Ti.

17. The solid material according to claim 15, wherein the solid material displays an increased UV/VIS absorption, over materials that have not been brought in contact with a composition comprising water, in the region from 250 to 350 nm.

18. The solid material according to claim 15, characterized in that it wherein the solid material is shaped into a shaped body in a step (S), and that in addition to the step of bringing the solid material in contact with a composition comprising water, or instead of said step, the shaped body is brought in contact with a composition comprising water, either directly after the step (S) of shaping the solid material into a shaped body, or after a subsequent step (C) of calcining said shaped body.

19. A method of catalyzing a reaction, comprising contacting the solid material according to claim 15, or a shaped body comprising said solid material, with a mixture comprising at least one compound with at least one C—

C-double bond and at least one hydroperoxide.

20. A method of catalyzing a reaction, comprising contacting the solid material according to claim 17, or a shaped body comprising said solid material, with a mixture comprising at least one compound with at least one C—

C-double bond and at least one hydroperoxide.

21. A catalyst or co-catalyst comprising the solid material according to claim 15, or a shaped body comprising said solid material, and one or more additives.

22. A catalyst or co-catalyst comprising the solid material body according to claim 16, or a shaped body comprising said solid material, and one or more additives.

23. A catalyst or co-catalyst comprising the solid material according to claim 17, or a shaped body comprising said solid material, and one or more additives.

24. A catalyst or co-catalyst comprising the solid material according to claim 18, or a shaped body comprising said solid material, and one or more additives.

32. The solid material according to claim 16, wherein the solid material is shaped into a shaped body in a step (S), and that in addition to the step of bringing the solid material in contact with a composition comprising water, or instead of said step, the shaped body is brought in contact with a composition comprising water, either directly after the step (S) of shaping the solid material into a shaped body, or after a subsequent step (C) of calcining said shaped body.

33. The solid material according to claim 17, wherein the solid material is shaped into a shaped body in a step (S), and that in addition to the step of bringing the solid material in contact with a composition comprising water, or instead of said step, the shaped body is brought in contact with a composition comprising water, either directly after the step (S) of shaping the solid material into a shaped body, or after a subsequent step (C) of calcining said shaped body.

39. The solid material according to claim 16, wherein the solid material comprises at least one zeolite comprising Ti, selected from materials of the structure classes MFI, MEL, MWW, BEA or combinations thereof.

40. The solid material according to claim 39, wherein the at least one zeolite further comprises a member selected from vanadium, zirconium, niobium or combinations thereof.

34. A shaped body comprising a solid material comprising at least one zeolite, and being at least partly crystalline, obtained by a process comprising the steps of:

(I) crystallizing, at least partially, the at least one solid material comprising at least one zeolite, out of a synthesis mixture, to form a mixture (I) comprising at least the solid material and a mother liquor;

(II) separating and/or concentrating the solid material in mixture (I);

(S) shaping the solid material into a shaped body;

(C) calcining the shaped body at temperatures higher than 400°

C., to form a calcined shape body;

(W) contacting the calcined shaped body with a composition comprising water; and

wherein the separation and/or concentration in step (II) is carried out by a method selected from the group consisting of;

filtration, ultrafiltration, diafiltration, centrifuge methods, spray drying and spray granulating; and

wherein the shaping of the solid material in step (S) is carried out by a method selected from the group consisting of;

pelletizing, pressing, extruding, sintering, roasting and briquetting.

35. The shaped body according to claim 34, wherein the at least one zeolite comprises Ti.

36. The shaped body according to claim 35, wherein the at least one zeolite comprising Ti is selected from materials of the structure classes MFI, MEL, MWW, BEA or combinations thereof.

37. The shaped body according to claim 34, wherein the solid material displays an increased UV/VIS absorption, over materials that have not been brought in contact with a composition comprising water, in the region from 250 to 350 nm.

38. The shaped body according to claim 34, wherein step (S) is carried out by extruding the solid material into an extrudate with a diameter ranging from about 1 mm to about 10 mm.