EP1019713A1 - Activation de rayonnement et criblage de bibliotheques de catalyseurs permettant d'evaluer un catalyseur et reacteurs correspondants - Google Patents

Activation de rayonnement et criblage de bibliotheques de catalyseurs permettant d'evaluer un catalyseur et reacteurs correspondants

Info

Publication number
EP1019713A1
EP1019713A1 EP98947652A EP98947652A EP1019713A1 EP 1019713 A1 EP1019713 A1 EP 1019713A1 EP 98947652 A EP98947652 A EP 98947652A EP 98947652 A EP98947652 A EP 98947652A EP 1019713 A1 EP1019713 A1 EP 1019713A1
Authority
EP
European Patent Office
Prior art keywords
catalyst
product
reactant
zone
screening
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP98947652A
Other languages
German (de)
English (en)
Inventor
Martin Philip Atkins
Selim Mehmet Senkan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lubrizol Adibis Holdings UK Ltd
Laser Catalyst Systems Inc
Original Assignee
BP Chemicals Additives Ltd
Laser Catalyst Systems Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from GBGB9807836.3A external-priority patent/GB9807836D0/en
Application filed by BP Chemicals Additives Ltd, Laser Catalyst Systems Inc filed Critical BP Chemicals Additives Ltd
Publication of EP1019713A1 publication Critical patent/EP1019713A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
    • H01J49/161—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission using photoionisation, e.g. by laser
    • H01J49/162—Direct photo-ionisation, e.g. single photon or multi-photon ionisation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00306—Reactor vessels in a multiple arrangement
    • B01J2219/00313—Reactor vessels in a multiple arrangement the reactor vessels being formed by arrays of wells in blocks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00497—Features relating to the solid phase supports
    • B01J2219/00527—Sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00585—Parallel processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00596—Solid-phase processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00603—Making arrays on substantially continuous surfaces
    • B01J2219/00605—Making arrays on substantially continuous surfaces the compounds being directly bound or immobilised to solid supports
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00603—Making arrays on substantially continuous surfaces
    • B01J2219/00659—Two-dimensional arrays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/0068—Means for controlling the apparatus of the process
    • B01J2219/00702—Processes involving means for analysing and characterising the products
    • B01J2219/00707—Processes involving means for analysing and characterising the products separated from the reactor apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00718—Type of compounds synthesised
    • B01J2219/00745—Inorganic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00718—Type of compounds synthesised
    • B01J2219/00745—Inorganic compounds
    • B01J2219/00747—Catalysts
    • C—CHEMISTRY; METALLURGY
    • C40—COMBINATORIAL TECHNOLOGY
    • C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B30/00—Methods of screening libraries
    • C40B30/08—Methods of screening libraries by measuring catalytic activity
    • C—CHEMISTRY; METALLURGY
    • C40—COMBINATORIAL TECHNOLOGY
    • C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B40/00—Libraries per se, e.g. arrays, mixtures
    • C40B40/18—Libraries containing only inorganic compounds or inorganic materials
    • C—CHEMISTRY; METALLURGY
    • C40—COMBINATORIAL TECHNOLOGY
    • C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B60/00—Apparatus specially adapted for use in combinatorial chemistry or with libraries
    • C40B60/14—Apparatus specially adapted for use in combinatorial chemistry or with libraries for creating libraries

Definitions

  • Coatings by Pulsed-Laser Deposition can be used to create large solid state catalyst libraries. These techniques provide good control of surface chemistry and are ideally suited to generate a wide spectaim of solid materials. Other well established preparation techniques, such as co-precipitation and impregnation, can also be used to generate catalyst libraries according to Satterfield, CN. in "Heterogeneous Catalysts in Practice", 2nd Ed., Chap. 4, 87, McGraw Hill, New York, 1991.
  • Heterogeneous catalyst libranes can also be prepared by using monolithic, or honeycomb, structures according to Sattei f ield, C N , 1991, supra These materials provide parallel, uniform, straight and nonconnecting channels, thereby providing a convenient matrix foi creating large catalyst libraries
  • a variety of cell shapes and sizes with cell densities varying from about 10 to about 500 cells per square inch can be produced with catalyst library sites
  • a wide variety of desired custom cell densities can be fabricated within and beyond the above ranges
  • Monolithic structui es can be made from metals oi they can be extruded from inoi anic dough, such as magnesia-alumina silicate, through a die followed by drying and filing
  • Catalyst libraries can also be prepared by coating metal monoliths with inoiganic substrates, wherein the metal inlay serves as a barrier to prevent intercell diffusion of species Catalysts can then be incorporated into the library substrate using any of the variety of methods described above Monolith
  • the catalyst sites must be sufficiently separated from each other so that product formation from each site and its unambiguous detection can be achieved
  • Monolithic, or honeycomb, structures offer advantages by providing clear physical separation of the library sites
  • reaction products or their fragmentation products may emit unique radiation signatures involving, for example, luminescence, fluorescence or phosphorescence. These emissions can then be used to rapidly screen the catalyst libraries using, for example, monochromators and diode array and charge coupled device (CCD) detectors.
  • CCD charge coupled device
  • the catalyst sites upstream from the test catalyst site, 21, must be masked to prevent signal crossover from different sites If the upstream sites are not masked and if some of these sites are catalytic, products formed at these sites would be transported downstream and interfere with the row screening process
  • Masking can be accomplished by using a physical mask to cover upstream catalysts sites, as shown in Fig 2, or by introducing reactant gases directly onto the catalyst sites using dedicated gas reactant feed tubes, shown as 34 in Fig. 3.
  • test sites 21t can be tilted, as shown in Fig 4, during the screening process to promote the transport of products away from the catalyst surface
  • any library pattern having specific addresses for individual test sites can be screened by moving the library with a computer controlled two-dimensional translation device
  • the smallest site size, providing the highest library density is determined by the gas phase dispersion rate of product gas between test sites Consequently, different products can allow the generation and testing of different library densities
  • laser beams 23 pass through window 39 of reactor 45 and through the product gases above the test sites 21 , perpendicular to the reactant gas flow from reactant feed tubes 34 and passes through the product gas plumes of all of the sites in a row, as indicated by the dotted line, and exits reactor 45 to laser beam dump 46
  • Reactant feed tubes 34 are supplied by reactor gas supply manifold 48
  • two lasers are indicated, however, any number of lasers may be used in a given application.
  • the magnitude of the REMPI signals produced by the photoionisation of product species will be proportional to their concentration.
  • the generated signals are also influenced by the operational parameters, such as, the power of the UV laser used, the DC bias voltage applied to collect the photoions/photoelectrons, the separation distance of the anode and cathode and the position of the microelectrode relative to the laser beam.
  • the operational variables can be fixed so that the measured REMPI signals can be directly attributed to product concentrations generated by the catalyst sites. Consequently, in addition to the qualitative, active versus inactive, screening of catalyst libraries, the REMPI microelectrode technique of this invention can be used to quantitatively rank the activities and selectivities of catalysts.
  • the library screening process demands the unambiguous detection of benzene in a cyclohexane, hydrogen and argon mix.
  • a suitable liv laser wave length for selectively producing benzene REMPI ions was identified in separate tests using a laser photoionization time of flight mass spectromer, TOF-MS.
  • Gas pulses of cyclohexane and benzene, each at a concentration of about 50 ppm in argon, were expanded into the vacuum chamber of the TOF-MS using a pulsed valve and the resulting jet/molecular beam was crossed by a pulsed UV laser beam in the 258-262 nm range to generate their photoionisation and mass spectra.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Molecular Biology (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Organic Chemistry (AREA)
  • Optics & Photonics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Catalysts (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

La présente invention concerne le criblage rapide d'activités et de sélectivités de bibliothèques de catalyseur possédant des sites de tests adressables, effectué en mettant en contact des catalyseurs potentiels au niveau de sites de test avec des flux de réactif qui forment des panaches de produit au niveau des sites de test adressables. Ces panaches de produit sont criblés par passage d'un faisceau de rayonnement d'un niveau d'énergie quelconque de façon à promouvoir la formation de photoions et de photoélectrons détectés par un groupe de microélectrodes in situ à proximité du site de test adressable respectif. Les panaches de produit peuvent être criblés rangée par rangée et tous les panaches de produit émanant de la bibliothèque complète de catalyseur peuvent être criblés simultanément. La présente invention concerne également des réacteurs et des microréacteurs adaptés pour un triage d'activation de ryonnement.
EP98947652A 1997-10-10 1998-10-08 Activation de rayonnement et criblage de bibliotheques de catalyseurs permettant d'evaluer un catalyseur et reacteurs correspondants Withdrawn EP1019713A1 (fr)

Applications Claiming Priority (7)

Application Number Priority Date Filing Date Title
US94920397A 1997-10-10 1997-10-10
US949203 1997-10-10
GB9807836 1998-04-14
GBGB9807836.3A GB9807836D0 (en) 1998-04-14 1998-04-14 Reactors
US8741798A 1998-05-29 1998-05-29
US87417 1998-05-29
PCT/GB1998/003023 WO1999019724A1 (fr) 1997-10-10 1998-10-08 Activation de rayonnement et criblage de bibliotheques de catalyseurs permettant d'evaluer un catalyseur et reacteurs correspondants

Publications (1)

Publication Number Publication Date
EP1019713A1 true EP1019713A1 (fr) 2000-07-19

Family

ID=27269278

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98947652A Withdrawn EP1019713A1 (fr) 1997-10-10 1998-10-08 Activation de rayonnement et criblage de bibliotheques de catalyseurs permettant d'evaluer un catalyseur et reacteurs correspondants

Country Status (12)

Country Link
EP (1) EP1019713A1 (fr)
JP (1) JP2001520380A (fr)
KR (1) KR20010031021A (fr)
CN (1) CN1281551A (fr)
AU (1) AU736438B2 (fr)
BR (1) BR9812909A (fr)
CA (1) CA2306256A1 (fr)
ID (1) ID24631A (fr)
NO (1) NO20001787L (fr)
NZ (1) NZ503731A (fr)
PL (1) PL339834A1 (fr)
WO (1) WO1999019724A1 (fr)

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US6602714B1 (en) 1999-11-09 2003-08-05 Sri International Viscosity and mass sensor for the high-throughput synthesis, screening and characterization of combinatorial libraries
DE19959974A1 (de) 1999-12-13 2001-06-21 Basf Ag Verfahren zur Herstellung von Materialbibliotheken durch elektrochemische Abscheidung
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US6776963B1 (en) 1999-12-15 2004-08-17 Uop Llc Multiple parallel catalytic reactor assembly
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Also Published As

Publication number Publication date
NO20001787D0 (no) 2000-04-06
PL339834A1 (en) 2001-01-02
CN1281551A (zh) 2001-01-24
NZ503731A (en) 2001-05-25
AU736438B2 (en) 2001-07-26
JP2001520380A (ja) 2001-10-30
KR20010031021A (ko) 2001-04-16
WO1999019724A1 (fr) 1999-04-22
NO20001787L (no) 2000-06-09
CA2306256A1 (fr) 1999-04-22
AU9449498A (en) 1999-05-03
ID24631A (id) 2000-07-27
BR9812909A (pt) 2002-02-05

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