Method and system for the situ synthesis of a combinatorial library of supported catalyst materials

• US 6,627,571 B1
• Filed: 03/01/2000
• Issued: 09/30/2003
• Est. Priority Date: 03/01/2000
• Status: Expired due to Fees

• Current Assignee: Freeslate Inc. (Unchained Labs Inc.)
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA)
• Inventors: Poojary, Damodara M., Lugmair, Claus G., Hagemeyer, Alfred
• Primary Examiner(s): WOOD, ELIZABETH D
• Application Number:
  US09/516,669
• Time in Patent Office: 1,308 Days
• Field of Search: 502/2, 502/439, 502/527.14, 502/527.23, 502/527.24, 502/180, 502/232, 502/300, 502/349, 502/350, 502/355, 436/37
• US Class Current: 502/2
• CPC Class Codes: B01J 19/0046 Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays synthesis methods per se C40B50/00
• CPC Class Codes: B01J 2219/00315 Microtiter plates
• CPC Class Codes: B01J 2219/00317 Microwell devices, i.e. having large numbers of wells
• CPC Class Codes: B01J 2219/00527 Sheets
• CPC Class Codes: B01J 2219/00585 Parallel processes
• CPC Class Codes: B01J 2219/0059 Sequential processes
• CPC Class Codes: B01J 2219/00659 Two-dimensional arrays
• CPC Class Codes: B01J 2219/00702 Processes involving means for analysing and characterising the products
• CPC Class Codes: B01J 2219/00745 Inorganic compounds
• CPC Class Codes: B01J 2219/00747 Catalysts
• CPC Class Codes: B01J 23/892 Nickel and noble metals
• CPC Class Codes: B01J 37/0201 Impregnation
• CPC Class Codes: C40B 30/08 by measuring catalytic activity
• CPC Class Codes: C40B 40/18 Libraries containing only inorganic compounds or inorganic materials
• CPC Class Codes: C40B 60/14 for creating libraries

Abstract

A method and system for the in situ synthesis of a combinatorial library including impregnating a first component with a second component. The method and system advantageously may be employed in the synthesis of materials for screening for usefulness as a catalyst.

Claims

1. A method for forming an array of supported catalyst materials, said method comprising the steps of:

a)discretely providing a catalyst carrier in a liquid suspension to each of at least four regions on a substrate said liquid suspension further including at least one agent to alter its viscosity, surface or wetting characteristics and facilitate handling;

b)removing at least a portion of said liquid from said suspension to form an array of porous catalyst carriers;

c)providing in a liquid medium a catalytically active component or a precursor thereof to said at least four regions on said;

d)impregnating said array of catalyst carriers with said catalytically active component or a precursor thereof on said substrate to form an array of supported materials for screening for heterogeneous catalytic properties; and

e) removing at least a portion of said liquid medium.

2. A method according to claim 1 further comprising treating said substrate for modifying the local surface free energy of said deposition surface.

3. The method according to claim 1 further comprising heat treating said array.

4. The method according to claim 1 further comprising calcining said array.

5. The method according to claim 1 further comprising screening said array for heterogeneous catalytic properties while said materials are on said substrate.

6. The method according to claim 1 wherein the composition of said catalyst carrier is different at different locations across the substrate.

7. The method according to claim 1 wherein the composition of said catalytically active component or a precursor thereof is different at different locations across the substrate.

8. The method according to claim 1 wherein said catalyst carrier is selected from carbon, oxides of Zr, Ti, Al, Si, or mixtures thereof.

9. The method according to claim 1 wherein said catalytically active component or a precursor thereof includes a metal selected from the group consisting of noble metals, transition metals, transition-metal containing compounds or mixtures thereof.

10. The method according to claim 1 wherein said supported materials are physically separated.

11. The method according to claim 1 wherein said supported materials are physically continuous.

12. The method according to claim 1 wherein said catalyst carrier is provided in a slurry.

13. The method according to claim 1 wherein catalyst carrier is provided in a sol-gel.

14. The method according to claim 1 wherein said catalyst carrier is provided in a colloidal suspension.

15. The method according to claim 1 wherein said array includes at least 5 different materials.

16. The method according to claim 1 wherein said array includes at least 12 different materials.

17. The method according to said claim 1 wherein said array includes at least 24 different materials.

18. The method according to claim 1, wherein said providing of said carrier is after said providing of said catalytically active component or precursor thereof.

19. The method according to claim 1, wherein said providing of said carrier precedes said providing of said catalytically active component or precursor thereof.

20. The method according to claim 1, wherein said porous catalyst carriers have a surface area of about 80 m²/g to about 110 m²/g.

21. The method according to claim 1, wherein said porous catalyst carriers have a surface area of at least about 90 m²/g.

22. The method according to claim 1, wherein said porous catalyst carriers have a pore volume of about 0.3 to about 0.8 cc/g.

23. The method according to claim 1, wherein said porous catalyst carriers have a pore diameter of about 4 to about 10 nm.

24. The method according to claim 1, wherein said porous catalyst carriers have a surface area of about 80 m²/g to about 110 m²/g, a pore volume of about 0.3 to about 0.8 cc/g, and a pore diameter of about 4 to about 10 nm.

25. The method of claim 24 wherein said providing steps are performed with an automated fluid dispensing system.

26. The method of claim 25 wherein each of said providing steps includes dispensing simultaneously to each of said regions.

27. The method according to claim 22, wherein said liquid medium impregnates said porous catalyst carrier by way of capillary action.

28. The method according to claim 1, further comprising conducting X-ray diffraction analysis of said array of supported materials while said materials are on said substrate.

42. The method according to claim 1 wherein said catalyst carrier is comprised of spherical beads.

43. The method according to claim 42 wherein variation in diameter size for said spherical beads is less than about 25 percent.

44. The method according to claim 43 wherein variation in diameter size for said spherical beads is less than about 10 percent.

45. The method according to claim 44 wherein variation in diameter size for said spherical beads is less than about 5 percent.

46. The method according to claim 1 wherein said catalyst carrier has a particulate size in the range from about 0.01 micron to about 300 microns.

47. The method according to claim 12, wherein said catalyst carrier has a particulate size in the range from about 0.01 micron to about 100 microns.

48. The method according to claim 12 wherein said catalyst has a particulate size in the range from about 1 micron to about 20 microns.

29. A method for forming an array of supported catalyst materials, said method comprising the steps of:

a) discretely providing a catalyst carrier in a liquid suspension to each of at least four regions on a substrate;

b) drying said suspension to form an array of porous catalyst carriers having a surface area of about 80 m²/g to about 110 m²/g, a pore volume of about 0.3 to about 0.8 cc/g, and a pore diameter of about 4 to about 10 nm;

c) providing in a liquid medium a catalytically active component or a precursor thereof to said at least four regions on said substrate;

d) impregnating said array of catalyst carriers with said catalytically active component or a precursor thereof on said substrate to form an array of supported materials;

e) calcining said impregnated array; and

f) screening said calcined array of supported materials.

30. The method according to claim 29 wherein catalyst carrier is provided in a sol-gel.

31. The method according to claim 29 wherein said catalyst carrier is provided in a colloidal suspension.

32. The method according to claim 29, further comprising conducting X-ray diffraction analysis of said array of supported materials while said materials are on said substrate.

33. The method according to claim 30, further comprising conducting X-ray diffraction analysis of said array of supported materials while said materials are on said substrate.

34. The method according to claim 31, further comprising conducting X-ray diffraction analysis of said array of supported materials while said materials are on said substrate.

35. The method according to claim 29, wherein said catalyst carrier is an oxide.

36. A method for forming an array of supported catalyst materials, said method comprising the steps of:

a) discretely providing a plurality of liquid suspensions each consisting essentially of a different catalyst carrier, to a different region on a substrate;

b) drying said suspensions to form a plurality of different porous oxide catalyst carriers on said substrate;

c)providing in a liquid medium a catalytically active component or a precursor thereof to said at least four regions on said substrate, said catalytically active component or a precursor thereof including at least 3 component materials;

d) impregnating said array of catalyst carriers with an amount of said catalytically active component or a precursor thereof that corresponds approximately with the amount of pore volume of said catalyst carrier on said substrate to form an array of supported materials;

e) calcining said impregnated array; and

f) conducting X-ray diffraction analysis of said array of supported materials while said materials are on said substrate.

37. The method according to claim 36, wherein at least one of said suspensions is a sol-gel.

38. The method according to claim 36, wherein at least one of said suspensions is a colloidal suspension.

39. The method according to claim 36, wherein said liquid suspension includes at least one agent to alter its viscosity, surface or wetting characteristics and facilitate handling.

40. A method for forming an array of supported catalyst materials, said method comprising the steps of:

a) discretely providing a plurality of liquid suspensions each consisting essentially of a different catalyst carrier, to a different region on a substrate;

b) drying said suspensions to form a plurality of different porous oxide catalyst carriers on said substrate;

c) providing in a liquid medium a catalytically active component or a precursor thereof to said at least four regions on said substrate;

d)impregnating said array of catalyst carriers with an amount of said catalytically active component or a precursor thereof that corresponds approximately with the amount of pore volume of said catalyst carrier on said substrate to form an array of supported materials;

e) calcining said impregnated array; and

f) conducting X-ray diffraction analysis of said array of supported materials while said materials are on said substrate.

41. A method for forming an array of supported catalyst materials, said method comprising the steps of:

a) discretely providing a catalyst carrier in a liquid suspension to each of at least four regions on a substrate,

b) drying said suspensions to form a plurality of different porous oxide catalyst carriers on said substrate;

c) providing in a liquid medium a catalytically active component or a precursor thereof to said at least four regions on said substrate, said catalytically active component or a precursor thereof including at least 3 component materials;

d) impregnating said array of catalyst carriers with an amount of said catalytically active component or a precursor thereof that corresponds approximately with the amount of pore volume of said catalyst carrier on said substrate to form an array of supported materials;

e) calcining said impregnated array; and

f) screening said array of supported materials while said materials are on said substrate.