Apparatus for testing catalysts using spectroscopy

• US 6,630,111 B1
• Filed: 07/10/2000
• Issued: 10/07/2003
• Est. Priority Date: 02/28/1996
• Status: Expired due to Term

• Current Assignee: University of Houston Law Center (University of Houston System)
• Original Assignee: University of Houston (University of Houston System)
• Inventors: Willson, Richard C. III
• Primary Examiner(s): Soderquist, Arlen
• Application Number:
  US09/613,879
• Time in Patent Office: 1,184 Days
• Field of Search: 422/62, 422/93, 422/104, 422/196, 422/197, 422/130, 422/129, 436/37, 436/147, 436/159, 436/161, 436/164, 436/172, 436/173
• US Class Current: 506/22
• 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 2219/00286 Reactor vessels with top and bottom openings
• CPC Class Codes: B01J 2219/00315 Microtiter plates
• CPC Class Codes: B01J 2219/00364 Pipettes
• CPC Class Codes: B01J 2219/00527 Sheets
• CPC Class Codes: B01J 2219/00585 Parallel processes
• CPC Class Codes: B01J 2219/00596 Solid-phase processes
• CPC Class Codes: B01J 2219/00659 Two-dimensional arrays
• CPC Class Codes: B01J 2219/00691 using robots
• CPC Class Codes: B01J 2219/00704 integrated with the reactor apparatus
• CPC Class Codes: B01J 2219/00745 Inorganic compounds
• CPC Class Codes: B01J 2219/00747 Catalysts
• 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: G01N 31/10 using catalysis
• CPC Class Codes: Y10T 436/214 Acyclic [e.g., methane, octane, isoparaffin, etc.]
• CPC Class Codes: Y10T 436/24 Nuclear magnetic resonance, electron spin resonance or other spin effects or mass spectrometry

Abstract

Apparatus for evaluating catalysts, including a multicell holder, e.g., a honeycomb or plate, or a collection of individual support particles, is treated with solutions/suspensions of catalyst ingredients to produce cells, spots or pellets holding each of a variety of combinations of the ingredients, is dried, calcined or treated as necessary to stabilize the ingredients in the cells, spots or pellets, then is contacted with a potentially reactive feed stream or batch, e.g., biochemical, gas oil, hydrogen plus oxygen, propylene plus oxygen, CCl₂F₂ and hydrogen, etc. The reaction occurring in each cell can be measured, e.g., by infrared thermography, spectroscopic detection of products or residual reactants, or by sampling, e.g., multistreaming through low volume tubing, from the vicinity of each combination, followed by analysis, e.g., spectral analysis, chromatography, etc., or by observing temperature change in the vicinity of the catalyst, e.g., by thermographic techniques, to determine the relative efficacy of the catalysts in each combination. Robotic techniques can be employed in producing the cells, spots, pellets, etc.

Claims

1. An apparatus for evaluating a plurality of differing compositions for catalysis, the apparatus comprising

a parallel flow reactor comprising (i) a plurality of reaction channels defining a plurality of reaction sites, each of the plurality of reaction sites being adapted for containing a different candidate catalyst, (ii) one or more radiation-transparent windows, and (iii) a header comprising multiple delivery tubes for uniform flow distribution, each delivery tube being inserted into a reaction channel, such that one or more reactants flow simultaneously through each of the plurality of reaction channels so that the plurality of candidate catalysts can be simultaneously contacted with the one or more reactants under reaction conditions,

a radiation source adapted for simultaneously irradiating a plurality of reaction products with radiation through the one or more radiation-transparent windows, and

a camera for simultaneously determining radiation absorbed or emitted by a reaction product or unreacted reactant through the one or more radiation-transparent windows during the course of a reaction to determine the relative efficacy of the plurality of candidate catalysts.

4. The apparatus of claims 1, 2 or 3 further comprising a plurality of different candidate catalysts situated in respective reaction sites.

8. The apparatus of claims 1 or 5 wherein the plurality of reaction sites are a plurality of reaction channels in a monolithic support.

9. The apparatus of claims 1 or 5 wherein the parallel reactor comprises a plurality of reaction channels arranged in an array with a density of at least 9 reaction channels per square inch.

10. The apparatus of claims 1, 2, 3 or 5 wherein the reactor is adapted such that the plurality of candidate catalysts can be simultaneously contacted with one or more reactants under reaction conditions comprising a temperature greater than 100°

C., and additionally, or alternatively, a pressure of greater than 1 bar.

11. The apparatus of claims 1, 2, 3 or 5 wherein the plurality of reaction sites comprises ten or more reaction sites.

12. The apparatus of claims 1, 2, 3 or 5 wherein the plurality of reaction sites comprises fifteen reaction sites.

2. An apparatus for evaluating a plurality of differing compositions for catalysis, the apparatus comprising

a parallel reactor comprising a plurality of reaction sites, each of the plurality of reaction sites being adapted for containing a different candidate catalyst, and one or more radiation-transparent windows, the reactor being adapted such that the plurality of candidate catalysts can be simultaneously contacted with one or more reactants under reaction conditions, wherein the parallel reactor is a batch reactor pressurized with the one or more reactants,

a radiation source adapted for simultaneously irradiating a plurality of reaction products with radiation through the one or more radiation-transparent windows, and

a camera for simultaneously determining radiation absorbed or emitted by a reaction product or unreacted reactant through the one or more radiation-transparent windows during the course of a reaction to determine the relative efficacy of the plurality of candidate catalysts.

3. An apparatus for evaluating a plurality of differing compositions for catalysis, the apparatus comprising

a parallel reactor comprising a plurality of reaction sites, each of the plurality of reaction sites being adapted for containing a different candidate catalyst, and one or more radiation-transparent windows, the reactor being adapted such that the plurality of candidate catalysts can be simultaneously contacted with one or more reactants under reaction conditions, wherein the plurality of reaction sites are a plurality of wells,

a radiation source adapted for simultaneously irradiating a plurality of reaction products with radiation through the one or more radiation-transparent windows, and

a camera for simultaneously determining radiation absorbed or emitted by a reaction product or unreacted reactant through the one or more radiation-transparent windows during the course of a reaction to determine the relative efficacy of the plurality of candidate catalysts.

5. An apparatus for evaluating a plurality of differing compositions for catalysis, the apparatus comprising

a parallel reactor comprising a plurality of reaction sites, each of the plurality of reaction sites being adapted for containing a different candidate catalyst, and one or more radiation-transparent windows, the reactor being adapted such that the plurality of candidate catalysts can be simultaneously contacted with one or more reactants under reaction conditions,

a plurality of different candidate catalysts situated in respective reaction sites,

a radiation source adapted for simultaneously irradiating a plurality of reaction products with radiation through the one or more radiation-transparent windows, and

a camera for simultaneously determining radiation absorbed or emitted by a reaction product or unreacted reactant through the one or more radiation-transparent windows during the course of a reaction to determine the relative efficacy of the plurality of candidate catalysts.

6. The apparatus of claim 5 wherein the parallel reactor is a flow reactor adapted such that the one or more reactants flow simultaneously through each of the plurality of reaction channels.

7. The apparatus of claim 5 wherein the plurality of reaction sites are a plurality of reaction channels.

13. The apparatus of claim 5 wherein the plurality of catalyst candidates are chemical conversion catalysts.

14. The apparatus of claim 5 wherein the plurality of catalyst candidates are hydrocarbon conversion catalysts.

15. The apparatus of claim 5 wherein the plurality of catalyst candidates are inorganic catalysts.

16. The apparatus of claim 5 wherein the plurality of catalyst candidates are metals or metal oxides.

17. The apparatus of claim 5 wherein the plurality of catalyst candidates are transition metals or transition metal oxides.

18. The apparatus of claim 5 wherein the plurality of catalyst candidates are zeolites.

19. The apparatus of claim 5 wherein the plurality of catalyst candidates are metallocenes.

20. The apparatus of claim 5 wherein the plurality of catalyst candidates are enzymes.

21. The apparatus of claim 5 wherein the plurality of catalyst candidates are chiral catalysts.

22. The apparatus of claim 5 wherein the plurality of catalyst candidates are supported catalysts.

23. An apparatus for evaluating a plurality of differing compositions for catalysis, the apparatus comprising

a parallel reactor comprising a plurality of reaction channels, each of the plurality of reaction channels comprising a different candidate catalyst, a first infrared-transparent window, and a second infrared-transparent window, the reactor being adapted such that plurality of candidate catalysts can be simultaneously contacted with one or more reactants under reaction conditions,

a radiation source adapted for simultaneously irradiating a plurality of reaction products with radiation through the first infrared-transparent window, and

a camera for simultaneously determining radiation absorbed by a reaction product or unreacted reactant through the second infrared-transparent window during the course of a reaction to determine the relative efficacy of the plurality of candidate catalysts.

24. The apparatus of claim 23 wherein the radiation source is an infrared radiation source and the camera is an infrared-sensitive camera.

25. The apparatus of claim 23 wherein the plurality of reaction channels are formed in a common support.

26. An apparatus for evaluating a plurality of differing compositions for catalysis, the apparatus comprising

a parallel reactor adapted such that a plurality of candidate catalysts can be simultaneously contacted with one or more reactants under reaction conditions,

a polarized light source adapted for simultaneously irradiating a plurality of reaction products with polarized light, and

a polarizer positioned between the polarized light source and a detector for determining an angle of rotation of the polarized light during the course of a reaction to determine the relative efficacy of the plurality of candidate catalysts.

27. The apparatus of claim 26 wherein the detector is a camera for simultaneously detecting the polarized light.

28. The apparatus of claim 26 wherein the parallel reactor is a parallel flow reactor.

29. The apparatus of claim 26 wherein

the parallel reactor comprises a plurality of reaction channels, a first window and a second window, each of the plurality of reaction channels comprising a different candidate catalyst, and

the polarized light source is adapted for simultaneously irradiating the plurality of reaction products through the first window, the apparatus further comprising

a camera for simultaneously detecting the polarized light passed through the second window and the polarizer.

30. The apparatus of claim 26 further comprising a plurality of different candidate catalysts, the plurality of different candidate catalysts being provided at a plurality of reaction sites on a common support.