Process for testing catalysts using thermography

• US 6,908,768 B2
• Filed: 12/21/2001
• Issued: 06/21/2005
• Est. Priority Date: 02/28/1996
• Status: Expired due to Fees

• Current Assignee: University of Houston (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:
  US10/029,891
• Publication Number:
  US 20020127725A1
• Time in Patent Office: 1,278 Days
• Field of Search: 436/37, 436/63, 436/147, 436/159, 436/164, 436172-173, 436/183, 422/62, 422/93, 422/104, 422130-131, 422196-197, 435/4
• US Class Current: 436/37
• 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 testing catalyst candidates including a multi-cell holder e.g. a honeycomb or plate, or a collection of individual support particles that have been treated with solutions/suspensions of catalyst ingredients to produce cells, spots or pellets holding each of a variety of combinations of the ingredients and dried, calcined or treated as necessary to stabilize the ingredients in the cells, spots or pellets. The apparatus also includes structure for contacting the catalyst candidates 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. by 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. A method for evaluating a plurality of candidate catalysts, the method comprising

providing a plurality of candidate catalysts having differing compositions in a parallel reactor, the reactor comprising one or more temperature sensors adapted to measure the temperature near the plurality of candidate catalysts, each of the plurality of candidate catalysts being tagged or labeled to identify particular catalyst candidates,

simultaneously contacting the plurality of candidate catalysts with one or more reactants under reaction conditions to catalyze at least one reaction with each of the plurality of candidate catalysts,

detecting temperature changes due to the heat of reaction of the catalyzed reactions using the temperature sensors,

determing the relative efficacy of the plurality of candidate catalysts based on the detected temperature changes,

collecting candidate catalysts showing catalytic activity, and

analyzing the tag or label of the collected candidate catalysts to determine the catalyst candidates having catalytic activity.

3. The method of claims 1 or 2 wherein the plurality of catalyst candidates are inorganic catalysts.

4. The method of claims 1 or 2 wherein the plurality of catalyst candidates are metals or metal oxides.

5. The method of claims 1 or 2 wherein the plurality of catalyst candidates are transition metals or transition metal oxides.

6. The method of claims 1 or 2 wherein the plurality of candidate catalysts are formed by calcining catalyst precursors at different temperatures.

9. The method of claims 1, 7, 8 or 2 wherein the plurality of catalyst candidates are chemical conversion catalysts.

10. The method of claims 1, 7, 8 or 2 wherein the plurality of catalyst candidates are hydrocarbon conversion catalysts.

11. The method of claims 1, 7, 8 or 2 wherein the plurality of candidate catalysts are contacted with the one or more reactants under reaction conditions that include a temperature greater than 100°

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

15. The method of claims 1, 7, 8, 13, 14 or 2 wherein the plurality of candidate catalysts are provided at a plurality of sites on a common support.

16. The method of claim 15 wherein the support is a plate or sheet having a surface comprising the candidate-catalyst-containing sites.

17. The method of claim 15 wherein the support is a plate having a plurality of wells as candidate-catalyst-containing sites.

18. The method of claim 15 wherein the support is a monolithic support comprising a plurality of reaction channels as candidate-catalyst-containing sites.

19. The method of claim 15 wherein each of the plurality of candidate catalysts is in its own site on the support.

20. The method of claim 15 wherein the temperature sensors are adapted to observe temperature change in the vicinity of the candidate catalysts.

21. The method of claims 1, 7, 8, 13, 14, or 2 wherein the plurality of candidate catalysts are simultaneously contacted with the one or more reactants in a plurality of reactor channels formed in a monolithic support.

22. The method of claims 1, 7, 8, 13, 14 or 2 wherein the plurality of candidate catalysts comprises fifteen candidate catalysts.

23. The method of claims 1, 7, 8, 13, 14 or 2 wherein the plurality of candidate catalysts comprises twenty-four candidate catalysts.

24. The method of claims 1, 7, 8, 13, 14 or 2 wherein the plurality of candidate catalysts are simultaneously contacted with the one or more reactants in parallel rcactor comprising a plurality of reaction channels, each of the plurality of candidate catalysts being in its own reaction channel.

25. The method of claim 24 wherein the parallel reactor comprises a plurality of reaction channels in a monolithic support.

26. The method of claim 24 wherein the parallel reactor is a flow reactor and the one or more reactants flow through each of the plurality of reaction channels.

27. The method of claims 1, 7, 8, 13, 14 or 2 wherein

the plurality of candidate catalysts are simultaneously contacted with the one or more reactants in a parallel reactor, the parallel reactor being a batch reactor pressurized with the one or more reactants.

28. The method of claims 1, 8, 13, 14 or 2 wherein the plurality of catalyst candidates are supported catalysts.

2. A method for evaluating a plurality of candidate catalysts, the method comprising

providing a plurality of candidate catalysts having differing compositions in a parallel reactor, the reactor comprising one or more temperature sensors adapted to measure the temperature near each of the plurality of candidate catalysts,

simultaneously contacting the plurality of candidate catalysts with one or more reactants under reaction conditions to catalyze at least one reaction with each of the plurality of candidate catalysts, the one or more reactants being in the liquid phase,

detecting temperature changes due to the heat of reaction of the catalyzed reactions using the temperature sensors, and

determining the relative efficacy of the plurality of candidate catalysts based on the detected temperature changes.

7. A method for evaluating a plurality of candidate catalysts, the method comprising

providing a plurality of candidate catalysts having differing compositions in a parallel reactor, the reactor comprising one or more temperature sensors adapted to measure the temperature near each of the plurality of candidate catalysts, the plurality of catalyst candidates being zeolites,

simultaneously contacting the plurality of candidate catalysts with one or more reactants under reaction conditions to catalyze at least one reaction with each of the plurality of candidate catalysts,

detecting temperature changes due to the heat of reaction of the catalyzed reactions using the temperature sensors, and

determining the relative efficacy of the plurality of candidate catalysts based on the detected temperature changes.

12. The method of claims 7 or 8 wherein the one or more reactants are in the gas phase.

8. A method for evaluating a plurality of candidate catalysts, the method comprising

providing a plurality of candidate catalysts having differing compositions in a parallel reactor, the reactor comprising one or more temperature sensors adapted to measure the temperature near each of the plurality of candidate catalysts, the plurality of catalyst candidates being metallocenes,

simultaneously contacting the plurality of candidate catalysts with one or more reactants under reaction conditions to catalyze at least one reaction with each of the plurality of candidate catalysts,

detecting temperature changes due to the heat of reaction of the catalyzed reactions using the temperature sensors, and

determining the relative efficacy of the plurality of candidate catalysts based on the detected temperature changes.

13. A method for evaluating a plurality of candidate catalysts, the method comprising

providing a plurality of candidate catalysts having differing compositions in a parallel reactor, the reactor comprising one or more temperature sensors adapted to measure the temperature near each of the plurality of candidate catalysts, the plurality of catalyst candidates being enzymes,

simultaneously contacting the plurality of candidate catalysts with one or more reactants under reaction conditions to catalyze at least one reaction with each of the plurality of candidate catalysts,

detecting temperature changes due to the heat of reaction of the catalyzed reactions using the temperature sensors, and

determining the relative efficacy of the plurality of candidate catalysts based on the detected temperature changes.

14. A method for evaluating a plurality of candidate catalysts, the method comprising

providing a plurality of candidate catalysts having differing compositions in a parallel reactor, the reactor comprising one or more temperature sensors adapted to measure the temperature near each of the plurality of candidate catalysts, the plurality of catalyst candidates being cells,

simultaneously contacting the plurality of candidate catalysts with one or more reactants under reaction conditions to catalyze at least one reaction with each of the plurality of candidate catalysts,

detecting temperature changes due to the heat of reaction of the catalyzed reactions using the temperature sensors, and

determining the relative efficacy of the plurality of candidate catalysts based on the detected temperature changes.