Preparation of a crystalline, zeolitic solid

• US 7,081,237 B2
• Filed: 08/30/2004
• Issued: 07/25/2006
• Est. Priority Date: 08/20/1999
• Status: Expired due to Term

• Current Assignee: BASF AG (BASF SE)
• Original Assignee: BASF AG (BASF SE)
• Inventors: Mueller, Ulrich, Hill, Friedrich, Rieber, Norbert
• Primary Examiner(s): SAMPLE, DAVID R
• Application Number:
  US10/928,104
• Publication Number:
  US 20050031535A1
• Time in Patent Office: 694 Days
• Field of Search: 423/705, 423/716, 423/717, 423/326, 502/60, 502/242, 549/531
• US Class Current: 423/705
• CPC Class Codes: B01J 20/18 Synthetic zeolitic molecular sieves
• CPC Class Codes: B01J 29/7049 containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
• CPC Class Codes: B01J 29/89 Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium B01J29/005 takes precedence
• CPC Class Codes: C01B 37/00 Compounds having molecular sieve properties but not having base-exchange properties
• CPC Class Codes: C01B 37/005 Silicates, i.e. so-called metallosilicalites or metallozeosilites
• CPC Class Codes: C01B 39/026 After-treatment
• CPC Class Codes: C01B 39/04 using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
• CPC Class Codes: C01B 39/36 Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
• CPC Class Codes: C01G 23/04 Oxides; Hydroxides
• CPC Class Codes: Y02P 20/10 Process efficiency
• CPC Class Codes: Y10S 423/22 MFI, e.g. ZSM-5. silicalite, LZ-241

Abstract

Process for the preparation of a crystalline solid comprising at least one zeolitic material, in which the solid is crystallized from at least one precursor compound and the reaction discharge of the crystallization is fed directly to a drying stage.

Claims

1. A crystalline solid comprising at least one zeolitic material preparable by a process in which the solid is crystallized from at least one precursor compound and the reaction discharge of the crystallization is fed without removing any components and without any additional intermediate steps directly to a drying stage where it is spray dried, and wherein the drying is carried out in an atmosphere comprising oxygen and at least one inert gas, and wherein the zeolitic material is a Ti zeolite of the structure type wherein the drying is carried out in an atmosphere comprising less than 10% but greater than 0% by volume of oxygen, and at least one inert gas.

2. A method of preparing propylene oxide comprising reacting propene with H₂O₂ using the crystalline solid of claim 1 as catalyst.

3. The crystalline solid of claim 1, wherein the drying is carried out in an atmosphere comprising less than 5% by volume of oxygen, and at least one inert gas.

4. The crystalline solid of claim 1, wherein the at least one inert gas is nitrogen.

5. The crystalline solid of claim 1, wherein the drying is carried out while maintaining the temperature in the range of from 100 to 350°

C.

6. The crystalline solid of claim 1, wherein the drying is carried out while maintaining the temperature in the range of from 100 to 250°

C.

7. The crystalline solid of claim 3, wherein the at least one inert gas is nitrogen.

8. The crystalline solid of claim 3, wherein the drying is carried out while maintaining the temperature in the range of from 100 to 350°

C.

9. The crystalline solid of claim 3, wherein the drying is carried out while maintaining the temperature in the range of from 100 to 250°

C.

10. A crystalline solid comprising at least one zeolitic material preparable by a process in which the solid is crystallized from at least one precursor compound and the reaction discharge of the crystallization is fed without removing any components and without any additional intermediate steps directly to a drying stage where it is spray dried, and wherein the drying is carried out in an atmosphere comprising oxygen and at least one inert gas, and wherein the zeolitic material is a Ti zeolite of the structure type MFI, wherein the drying is carried out in an atmosphere comprising less than 5% but greater than 0% by volume of oxygen, and nitrogen, and wherein the drying is carried out while maintaining the temperature in the range of from 100 to 250°

C.

11. A method of preparing propylene oxide comprising reacting propene with H₂O₂ using the crystalline solid of claim 10 as catalyst.