Process for epoxidation and catalyst to be used therein

• US 8,119,550 B2
• Filed: 09/16/2003
• Issued: 02/21/2012
• Est. Priority Date: 09/17/2002
• Status: Active Grant

• Current Assignee: BASF AG (BASF SE)
• Original Assignee: BASF AG (BASF SE)
• Inventors: Mueller, Ulrich, Krug, Georg, Bassler, Peter, Goebbel, Hans-Georg, Rudolf, Peter, Teles, Joaquim Henrique
• Primary Examiner(s): WOOD, ELIZABETH D
• Application Number:
  US10/526,939
• Publication Number:
  US 20060167286A1
• Time in Patent Office: 3,080 Days
• Field of Search: 502/214, 502/60, 502/85, 423/713, 423/716, 423/326, 549/529
• US Class Current: 502/60
• 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 also 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. An integrated process for treating a solid material comprising at least one zeolite which comprises Ti and being at least partly crystalline, or a shaped body, obtained from said solid material by shaping said solid material into a shaped body, said process comprising:

bringing said solid material or said shaped body in contact with deionized water at a temperature between 120°

C. and 175°

C. for a duration of 12 to 24 hours after

at least partial crystallization of the solid material containing the at least one zeolite out of a synthesis mixture, resulting in mixture (I) containing the solid material and its mother liquor;

separating the solid material from its mother liquor wherein said separating is a step (II), and calcining the solid material at temperatures higher than 400°

C. wherein said calcining is a step (C);

or after

at least partial crystallization of the solid material containing the at least one zeolite out of a synthesis mixture, resulting in mixture (I) containing the solid material and its mother liquor;

separating the solid material from its mother liquor wherein said separating is a step (II), calcining the solid material at temperatures higher than 400°

C. wherein said calcining is a step (C), shaping the solid material into the shaped body, wherein said shaping is a step (S), and optionally calcining the shaped body wherein said calcining is a step (C).

2. The process according to claim 1, wherein the at least one zeolite containing Ti is selected from the group consisting of materials of the structure classes MFI, MEL, MWW, BEA or any mixed structures thereof.

3. The process according to claim 1, wherein the bringing of the solid material or the shaped body in contact with deionized water at a temperature between 120°

C. and 175°

C. for a duration of 12 to 24 hours 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 the shaped body are used as catalysts in a chemical reaction.

4. An integrated process for the production of a solid material containing at least one zeolite, said process, comprising:

(I) at least partial crystallization of the solid material containing at least one zeolite which comprises Ti out of a synthesis mixture, resulting in mixture (I) containing the solid material and its mother liquor;

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

(C) calcining the solid material at temperatures higher than 400°

C.;

(W) bringing the solid material from step (II) in contact with deionized water at a temperature between 120°

C. and 175°

C. for a duration of 12 to 24 hours;

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

wherein step (III) is optional.

5. The integrated process according to claim 4, wherein, after step (W), a repetition of step (II) is performed wherein the solid material is separated from at least parts of the composition containing water.

6. The integrated process according to claim 4, wherein the method of separating and/or concentrating in step (II) is selected from the group consisting of ultrafiltration, spray-drying, spray granulating, and bringing inert support bodies in contact with the synthesis solution from (I).

7. An integrated process for the production of a shaped body, comprising:

(I) at least partial crystallization of at least one solid material containing at least one zeolite which comprises Ti out of a synthesis mixture, resulting in mixture (I) containing the solid material and its mother liquor;

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

(C) calcining the solid material at temperatures higher than 400°

C.;

(W) bringing the solid material from step (C) in contact with deionized water at a temperature between 120°

C. and 175°

C. for a duration of 12 to 24 hours;

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

wherein step (III) is optional;

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

wherein said shaped body comprises the at least one zeolite.

8. The integrated process according to claim 7, wherein the at least one step of shaping the solid material is selected from the group consisting of pelletizing, pressing, extruding, sintering, roasting, briquetting.

9. The integrated process according to 7, wherein the step (W) is performed after the step (S) is performed,

wherein said step (W) either replaces the step (W) performed after step (C) or is performed in addition to the step (W) performed after step (C).

10. The integrated process according to claim 7, wherein after at least one of the steps (W) or (III), a step (C) of calcining the shaped body is performed.

11. A solid material, obtained by an integrated process, comprising:

treating a solid material comprising at least one zeolite which comprises Ti and being at least partly crystalline by bringing said solid material in contact with deionized water at a temperature between 120°

C. and 175°

C. for a duration of 12 to 24 hours after

at least partial crystallization of the solid material containing the at least one zeolite out of a synthesis mixture, resulting in mixture (I) containing the solid material and its mother liquor;

separating the solid material from its mother liquor wherein said separating is a step (II), and calcining the solid material at temperatures higher than 400°

C. wherein said calcining is a step (C).

12. The solid material according to claim 11, which displays an increased UV/VIS absorption over materials that have not been brought in contact with deionized water, in the region from 250 to 350 nm.

13. The solid material according to claim 11, which is shaped into a shaped body in a step (S);

and

wherein in addition to the step of bringing the solid material in contact with water or instead of said step, the shaped body is brought in contact with 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, wherein said bringing into contact with water is performed with deionized water at a temperature between 120°

C. and 175°

C. for a duration of 12 to 24 hours.

14. The solid material according to claim 11, which is shaped into a shaped body in a step (S);

and

wherein in addition to the step of bringing the solid material in contact with water or instead of said step, the shaped body is brought. in contact with 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, wherein said bringing into contact with water is performed with deionized water at a temperature between 120°

C. and 175°

C. for a duration of 12 to 24 hours.

15. A method of obtaining a reaction product of the reaction of at least one C-C-double bond with at least one hydroperoxide, said method comprising:

reacting at least one compound with at least one C-C-double bond with at least one hydroperoxide in the presence of the solid material according to claim 11.

16. The method of claim 15, wherein said solid material is a catalyst.

17. The method of claim 15, wherein said solid material is a co-catalyst.