Preparation of a crystalline, zeolitic solid

• US 20050031535A1
• Filed: 08/30/2004
• Published: 02/10/2005
• Est. Priority Date: 08/20/1999
• Status: Active Grant

• Current Assignee: BASF Coatings GmbH (BASF SE)
• Original Assignee: BASF Coatings GmbH (BASF SE)
• Inventors: Mueller, Ulrich, Hill, Friedrich, Rieber, Norbert
• Granted Patent: US 7,081,237 B2
• Time in Patent Office: Days
• US Class Current: 423/716
• 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

1-10. -10. (Canceled).

11. 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 directly to a drying stage, wherein the zeolitic material is a Ti, Ge, Te, Ta, V, Cr, Nb or Zr zeolite of the structure type ABW, ACO, AEI, AEL, AEN, AET, AFG, AFI, AFN, AFO, AFR, AFS, AFT, AFX, AFY, AHT, ANA, APC, APD, AST, ATN, ATO, ATS, ATT, ATV, AWO, AWW, BEA, BIK, BOG, BPH, BRE, CAN, CAS, CFI, CGF, CGS, CHA, CHI, CLO, CON, CZP, DAC, DDR, DFO, DFT, DOH, DON, EAB, EDI, EMT, EPI, ERI, ESV, EUO, FAU, FER, GIS, GME, GOO, HEU, IFR, ISV, ITE, JBW, KFI, LAU, LEV, LIO, LOS, LOV, LTA, LTL, LTN, MAZ, MET, MEL, MEP, MER, MFI, MFS, MON, MOR, MSO, MTF, MTN, MTT, MTW, MWW, NAT, NES, NON, OFF, OSI, PAR, PAU, PHI, RHO, RON, RSN, RTE, RTH, RUT, SAO, SAT, SBE, SBS, SBT, SFF, SGT, SOD, STF, STI, STT, TER, THO, TON, TSC, VET, VFI, VNI, VSW, WEI, WEN, YUG, ZON or ITQ-4, or of a mixed structure comprising two or more of these structures or a mixture of two or more of these zeolites:

12. The solid of claim 11, wherein the zeolitic material comprises at least one element selected from the group consisting of aluminum, titanium, boron, iron, gallium, vanadium, zirconium, zinc, tin, tellurium, germanium, and rare earth metals, and/or at least one element selected from the group consisting of sodium, potassium, magnesium, calcium, and metals of groups Ib, IIb and VIIIa.

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

13. 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 directly to a drying stage where it is spray dried and wherein the zeolitic material is a Ti, Ge, Te, Ta, V, Cr, Nb or Zr zeolite of the structure type ABW, ACO, AEI, AEL, AEN, AET, AFG, AFI, AFN, AFO, AFR, AFS, AFT, AFX, AFY, AHT, ANA, APC, APD, AST, ATN, ATO, ATS, ATT, ATV, AWO, AWW, BEA, BIK, BOG, BPH, BRE, CAN, CAS, CFI, CGF, CGS, CHA, CHI, CLO, CON, CZP, DAC, DDR, DFO, DFT, DOH, DON, EAB, EDI, EMT, EPI, ERI, ESV, EUO, FAU, FER, GIS, GME, GOO, HEU, IFR, ISV, ITE, JBW, KFI, LAU, LEV, LIO, LOS, LOV, LTA, LTL, LTN, MAZ, MEI, MEL, MEP, MER, MFI, MFS, MON, MOR, MSO, MTF, MTN, MTT, MTW, MWW, NAT, NES, NON, OFF, OSI, PAR, PAU, PHI, RHO, RON, RSN, RTE, RTH, RUT, SAO, SAT, SBE, SBS, SBT, SFF, SGT, SOD, STF, STI, STT, TER, THO, TON, TSC, VET, VFI, VNI, VSV, WEI, WEN, YUG, ZON or ITQ-4, or of a mixed structure comprising two or more of these structures or a mixture of two or more of these zeolites.

14. The solid of claim 13, wherein the zeolitic material comprises at least one element selected from the group consisting of aluminum, titanium, boron, iron, gallium, vanadium, zirconium, zinc, tin, tellurium, germanium, and rare earth metals, and/or at least one element selected from the group consisting of sodium, potassium, magnesium, calcium, and metals of groups Ib, IIb and VIIIa.

23. A method of preparing propylene oxide by reacting propene with H₂O₂ using the crystalline solid of claim 13 as catalyst.

15. 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 in the presence of at least one template compound and the reaction discharge of the crystallization is fed directly to a drying stage, 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, Ge, Te, Ta, V, Cr, Nb or Zr zeolite of the structure type ABW, ACO, AEI, AEL, AEN, AET, AFG, AFI, AFN, AFO, AFR, AFS, AFT, AFX, AFY, AHT, ANA, APC, APD, AST, ATN, ATO, ATS, ATT, ATV, AWO, AWW, BEA, BIK, BOG, BPH, BRE, CAN, CAS, CFI, CGF, CGS, CHA, CHI, CLO, CON, CZP, DAC, DDR, DFO, DFT, DOH, DON, EAB, EDI, EMT, EPT, ERI, ESV, EUO, FAU, FER, GIS, GME, GOO, HEU, IFR, ISV, ITE, JBW, KFI, LAU, LEV, LIO, LOS, LOV, LTA, LTL, LTN, MAZ, MEI, MEL, MEP, MER, MFI, MFS, MON, MOR, MSO, MTF, MTN, MTT, MTW, MWW, NAT, NES, NON, OFF, OSI, PAR, PAU, PHI, RHO, RON, RSN, RTE, RTH, RUT, SAO, SAT, SBE, SBS, SBT, SFF, SGT, SOD, STF, STI, STT, TER, THO, TON, TSC, VET, VFI, VNI, VSV, WEI, WEN, YUG, ZON or ITQ-4, or of a mixed structure comprising two or more of these structures or a mixture of two or more of these zeolites.

16. The process of claim 15, wherein the drying is carried out in an atmosphere comprising less than 10% by volume of oxygen, and at least one inert gas.

17. The solid of claim 15, wherein the zeolitic material comprises at least one element selected from the group consisting of aluminum, titanium, boron, iron, gallium, vanadium, zirconium, zinc, tin, tellurium, germanium, and rare earth metals, and/or at least one element selected from the group consisting of sodium, potassium, magnesium, calcium, and metals of groups Ib, IIb and VIIIa.

24. A method of preparing propylene oxide by reacting propene with H₂O₂ using the crystalline solid of claim 15 as catalyst.

18. 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 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, Ge, Te, Ta, V, Cr, Nb or Zr zeolite of the structure type ABW, ACO, AEI, AEL, AEN, AET, AFG, AFI, AFN, AFO, AFR, AFS, AFT, AFX, AFX, AHT, ANA, APC, APD, AST, ATN, ATO, ATS, ATT, ATV, AWO, AWW, BEA, BIK, BOG, BPH, BRE, CAN, CAS, CFI, CGF, CGS, CHA, CHI, CLO, CON, CZP, DAC, DDR, DFO, DFT, DOH, DON, EAB, EDI, EMT, EPI, ERI, ESV, EUO, FAU, FER, GIS, GME, GOO, HEU, IFR, ISV, ITE, JBW, KFI, LAU, LEV, LIO, LOS, LOV, LTA, LTL, LTN, MAZ, MEI, MEL, MEP, MER, MFI, MFS, MON, MOR, MSO, MTF, MTN, MTT, MTW, MWW, NAT, NES, NON, OFF, OSI, PAR, PAU, PHI, RHO, RON, RSN, RTE, RTH, RUT, SAO, SAT, SBE, SBS, SBT, SFF, SGT, SOD, STF, STI, STT, TER, THO, TON, TSC, VET, VFI, VNI, VSV, WEI, WEN, YUG, ZON or ITQ-4, or of a mixed structure comprising two or more of these structures or a mixture of two or more of these zeolites.

19. The solid of claim 18, wherein the drying is carried out in an atmosphere comprising less than 10% by volume of oxygen, and at least one inert gas.

20. The solid of claim 18, wherein the zeolitic material comprises at least one element selected from the group consisting of aluminum, titanium, boron, iron, gallium, vanadium, zirconium, zinc, tin, tellurium, germanium, and rare earth metals, and/or at least one element selected from the group consisting of sodium, potassium, magnesium, calcium, and metals of groups Ib, IIb and VIIIa.

25. A method of preparing propylene oxide by reacting propene with H₂O₂ using the crystalline solid of claim 18 as catalyst.

21. 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 directly to a drying stage where it is spray dried, and wherein the drying is carried out in an atmosphere comprising less than 10% by volume of oxygen, and at least one inert gas, and wherein the zeolitic material is a Ti, Ge, Te, Ta, V, Cr, Nb or Zr zeolite of the structure type ABW, ACO, AEI, AEL, AEN, AET, AFG, AFI, AFN, AFO, AFR, AFS, AFT, AFX, AFX, AHT, ANA, APC, APD, AST, ATN, ATO, ATS, ATT, ATV, AWO, AWW, BEA, BIK, BOG, BPH, BRE, CAN, CAS, CFI, CGF, CGS, CHA, CHI, CLO, CON, CZP, DAC, DDR, DFO, DFT, DOH, DON, EAB, EDI, EMT, EPI, ERI, ESV, EUO, FAU, FER, GIS, GME, GOO, HEU, IFR, ISV, ITE, JBW, KFI, LAU, LEV, LIO, LOS, LOV, LTA, LTL, LTN, MAZ, MEI, MEL, MEP, MER, MFI, MFS, MON, MOR, MSO, MTF, MTN, MTT, MTW, MWW, NAT, NES, NON, OFF, OSI, PAR, PAU, PHI, RHO, RON, RSN, RTE, RTH, RUT, SAO, SAT, SBE, SBS, SBT, SFF, SGT, SOD, STF, STI, STT, TER, THO, TON, TSC, VET, VFI, VNI, VSV, WEI, WEN, YUG, ZON or ITQ-4, or of a mixed structure comprising two or more of these structures or a mixture of two or more of these zeolites, and wherein the zeolitic material comprises at least one element selected from the group consisting of aluminum, titanium, boron, iron, gallium, vanadium, zirconium, zinc, tin, tellurium, germanium, and rare earth metals, and/or at least one element selected from the group consisting of sodium, potassium, magnesium, calcium, and metals of groups Ib, IIb and VIIIa.

26. A method of preparing propylene oxide by reacting propene with H₂O₂ using the crystalline solid of claim 21 as catalyst.