Process for the production of a titanium silicalite shaped body

• US 6,849,570 B2
• Filed: 03/21/2001
• Issued: 02/01/2005
• Est. Priority Date: 03/29/2000
• Status: Expired due to Term

• Current Assignee: Evonik Degussa GmbH
• Original Assignee: Degussa AG (Rag-Stiftung)
• Inventors: Hasenzahl, Steffen, Jantke, Ralf
• Primary Examiner(s): Bell, Mark L.
• Assistant Examiner(s): Hailey, Patricia L.
• Application Number:
  US10/204,305
• Publication Number:
  US 20030078160A1
• Time in Patent Office: 1,413 Days
• Field of Search: 502/202, 502/208, 502/214, 502/242, 264/628, 264/636, 264/638, 549/523, 549/524, 549/531, 564/253, 564265-268
• US Class Current: 502/242
• CPC Class Codes: B01J 29/89 Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium B01J29/005 takes precedence
• CPC Class Codes: B01J 37/0009 Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
• CPC Class Codes: B01J 37/0018 Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
• CPC Class Codes: C07C 249/04 of oximes
• CPC Class Codes: C07D 301/12 with hydrogen peroxide or inorganic peroxides or peracids

Abstract

The present invention relates to a process for the production of a titanium silicalite shaped body by: (a) forming a formable composition containing titanium silicalite, a binder and a pasting agent, so that the Curd curve of the formable composition has a plateau value in the range from 20 to 90 mm; (b) shaping the composition of step (a) to form a green body; (c) optionally drying and (d) calcining the green body, to a titanium silicalite shaped body obtainable by that process, and to the use of such titanium silicalite shaped bodies in the epoxidation of olefins or the ammoximation of ketones.

Claims

1. Process for the production of a titanium silicalite shaped body by

(a) forming a formable composition containing titanium silicalite, a binder and a pasting agent, so that the Curd curve of the formable composition has a plateau value in the range from 20 to 90 mm,

(b) shaping the composition of step a) to form a green body,

(c) optionally drying and

(d) calcining the green body.

2. Process according to claim 1, wherein

the Curd curve of the formable composition has a plateau value in the range from 25 to 70 mm.

3. Process according to any one of the preceding claim 1, wherein

compounds of silicon, aluminum, boron, phosphorus, zirconium and/or titanium are used as binder.

4. Process according to claim 3, wherein

the binder is selected from aluminum oxide, silicon dioxide, hydrolyzable silicon compounds and partial or complete hydrolysates thereof, boron compounds, phosphorus compounds, clay minerals and mixtures thereof.

5. Process according to claim 4, wherein

the binder contains aluminium oxide.

6. Process according to claim 4, wherein

the binder contains a clay mineral.

7. Process according to claim 4, wherein

the binder contains a combination of silica sol and a boron compound.

8. Process according to claim 7, wherein

the boron compound is boric acid.

9. Process according to claim 7, wherein

silica sol is present in the mixture of silica sol and a boron compound in an amount of from 50 to 99.99 wt. %.

10. Process according to claim 1, wherein

the pasting agent used is an aqueous medium optionally containing a water-miscible organic solvent.

11. Process according to claim 1, wherein

the green body is calcined at a temperature of from 400°

C. to 1000°

C.

12. Process according to claim 11, wherein

the green body is calcined at a temperature from 500°

C. to 750°

C.

13. A titanium silicalite shaped body resulting from a process according to claim 1.

14. Process for the epoxidation of olefins, comprising:

reacting an olefin with aqueous hydrogen peroxide in the presence of titanium silicalite shaped bodies according to claim 13.

15. Process for the ammoximation of ketones, comprising:

reacting a ketone aqueous hydrogen peroxide and ammonia in the presence of titanium silicalite shaped bodies according to claim 13.