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  Combinatorial preparation and testing of heterogeneous catalystsRelated Patent Categories: Chemical Apparatus And Process Disinfecting, Deodorizing, Preserving, Or Sterilizing, Chemical Reactor, For Chemical Recovery Of Chemicals From Waste Paper Making LiquorThe Patent Description & Claims data below is from USPTO Patent Application 20060127287. Brief Patent Description - Full Patent Description - Patent Application Claims
[0001] The invention relates to a process for the combinatorial preparation and testing of heterogeneous catalysts and catalysts obtained by this process. [0002] To prepare and study novel chemical compounds, in addition to classical chemistry which is directed towards the synthesis and study of individual substances, combinatorial chemistry has developed. In this approach, a multiplicity of reactants were reacted in a one-pot synthesis and analyzed as to whether the resultant reaction mixture displays the desired properties, for example a pharmacological activity. If an activity was found for such a reaction mixture, it was necessary to determine in a further step which specific substance in the reaction mixture was responsible for the activity. In addition to the high expenditure for determining the actual active compound, it was difficult with a multiplicity of reactants to exclude to unwanted side reactions. [0003] In another combinatorial synthesis approach, a multiplicity of compounds were synthesized by specific dosage and reaction of a number of reactants in a multiplicity of different reaction vessels. In this process, preferably, in each reaction vessel one reaction product is present, so that in the event of, for example, a given pharmacological activity of a mixture, the starting materials used for its preparation are known immediately. [0004] In addition to the first applications of this more specific combinatorial synthesis in the search for novel pharmacologically active substances, very recently the synthesis method has also been extended to low-molecular-weight organic compounds and to organic and inorganic catalysts. [0005] F. M. Menger et al., "Phosphatase Catalysis Developed via Combinatorial Organic Chemistry", J. Org. Chem. 60 (1995) pages 6666 to 6667, describe the preparation of organic catalysts by combinatorial processes. 8 functionalized different carboxylic acids were bound to a polyallylamine via amide bonds. In addition, different metal ions were bound to the polymer via complex formation. The resultant polymers were then studied for their phosphatase activity. There is no description given as to whether the catalysts were obtained by an automated preparation process. Only the preparation of individual catalysts is described. [0006] C. L. Hill and R. D. Gall, "The first combinatorially prepared and evaluated inorganic catalysts. Polyoxometalates for the aerobic oxidation of the mustard analog tetrahydrothiophene (THT)", J. Mol. Catalysis A: Chemical 114 (1996), pages 103 to 111 describe the combinatorial preparation and testing of polyoxometalates, which were prepared by mixing different proportions of solutions of the desired metal salts. Tungstate, molybdate and vanadate solutions as well as a sodium hydrogen phosphate solution were prepared for this. After the appropriate solutions were metered, the pH was set to a predetermined value and a reaction induced. The resultant catalysts were used in dissolved form for the reaction. No description is given as to whether the catalyst preparation was automated. [0007] Processes for the specific metering of different amounts of various liquid reactants into an array of reaction vessels, which can resemble a spot plate, for example, are described in U.S. Pat. No. 5,449,754. For this purpose, the printer head of an ink jet printer, which is connected to reservoir solutions of the reactants, is moved over the array using an XY positioner and the release of the liquids is controlled by a computer. [0008] F. C. Moathes et al., "Infrared Thermographic Screening of Combinatorial Libraries of Heterogeneous Catalysts", Ind. Eng. Chem. Res. 35, (1996), 4801 to 4803, describe the IR screening of libraries of heterogeneous catalysts which comprise differing elemental metals applied to aluminum oxide. Their catalytic activity with respect to hydrogen oxidation was studied. The individual catalysts were prepared by impregnating aluminum oxide pellets in appropriate metal salt solutions, drying and calcination. There is no specification here as to whether the preparation was automated. [0009] The differing pellets were laid down on a support at predetermined positions and contacted with hydrogen under reaction conditions. In the event of catalytic activity, the catalyst heated up, and the heating was measured using an infrared camera, as result of which the active catalysts could be determined. [0010] B. E. Baker et al., "Solution-Based Assembly of Metal Surfaces by Combinatorial Methods", J. Am. Chem.-Soc. 118, (1996), pages 8721 to 8722 describe the preparation by combinatorial processes of metal surfaces differing in composition. For this purpose, a silane-coated glass plate is immersed at a predetermined rate into a colloidal gold solution so as to give a gold distribution gradient on the substrate. After withdrawing and drying the plate, it is rotated around 90.degree. and immersed into a silver ion solution, so that there is a further concentration gradient on the plate. This results in a continuous change in composition in the surface. [0011] X.-D. Xiang et al., "A Combinatorial Approach for Materials Discovery", Science 268, (1995), pages 1738 to 1740 describe the preparation of BiSrCaCuO and YBaCuO superconductivity films on substrates, a combinatorial array of different metal compositions being obtained by physical masking processes and vapor deposition techniques in the deposition of the appropriate metals. After the calcination, different compositions are present at different positions of the array and can be studied by microprobes, for their conductivity for example. [0012] WO 96/11878 describes, in addition to the preparation of such superconductivity arrays, the preparation of zeolites, the amounts required in each case being metered without prior mixing from a plurality of metal salt solutions using an ink jet onto a type of spot plate, a precipitation starting on addition of the last solution. BSCCO superconductors can also be prepared by separate metering of the individual nitrate solutions of the metals required by spraying onto a type of spot plate and subsequent heating. [0013] Various types of heterogeneous catalysts can be prepared using the known processes. However, testing the catalysts is complex and frequently cannot be performed under realistic conditions, e.g. using the required residence times of the reactants on the catalyst, since the catalysts are present, for example, on a relatively large, generally flat support and this must be charged, for example, with a gas mixture to be reacted. [0014] It is an object of the present invention to provide a process for preparing arrays of inorganic heterogeneous catalysts or their precursors in which the resultant catalysts can be tested with low expenditure and under conditions which resemble an industrial process. In addition, the disadvantages of the existing systems are to be avoided. Corresponding arrays are also to be provided. [0015] We have found that this object is achieved by providing an array of, preferably inorganic, heterogeneous catalysts and/or their precursors made up of a body which has, preferably parallel, through-channels in which at least n channels comprise n different, preferably inorganic, heterogeneous catalysts and/or their precursors, where n is 2, preferably 10, particularly preferably 100, in particular 1000, especially 10,000. [0016] According to one embodiment of the invention, the body is a tube-bundle reactor or heat exchanger and the channels are tubes. [0017] According to a further embodiment of the invention, the body is a block made of a solid material which has the channels, in the form of boreholes for example. [0018] The heterogeneous catalysts and/or precursors are preferably unsupported catalysts or supported catalysts and/or their precursors and are present as a catalyst bed, tube-wall coating or auxiliary support coating. [0019] The term "array of inorganic heterogeneous catalysts or their precursors" describes here an arrangement of different inorganic heterogeneous catalysts or their precursors on predetermined areas of a body which are spatially separate from one another, preferably a body having parallel through-channels, preferably a tube-bundle reactor or heat exchanger. The geometric arrangement of the individual areas to one another can be chosen freely in this case. For example, the areas can be arranged in the manner of a row (quasi one-dimensional) or a chessboard pattern (quasi two-dimensional). In a body having parallel through-channels, preferably a tube-bundle reactor or heat exchanger having a multiplicity of tubes parallel to one another, the arrangement becomes clear when a cross-sectional area perpendicular to the longitudinal axis of the tubes is considered: an area results, in which the individual tube cross sections reproduce the different areas separated from one another. The areas or tubes can, for example for tubes having a circular cross section, also be present in a dense packing, so that different rows are arranged from areas staggered to one another. [0020] The term "body" describes a three-dimensional object which has a multiplicity (at least n) of through-channels. The channels thus connect two surface areas of the body and run through the body. Preferably, the channels are essentially, preferably completely, parallel to one another. In this case, the body can be made up of one or more materials and can be solid or hollow. It can have any suitable geometric shape. Preferably it has two surfaces parallel to one another in which in each case one orifice of the channels is situated. The channels preferably run perpendicularly to these surfaces. An example of a body of this type is a parallelepiped or cylinder in which the channels run between two parallel surfaces. However, a multiplicity of similar geometries is also conceivable. [0021] The term "channel" describes a connection running through the body between two orifices situated on the body surface which, for example, permits the passage of a fluid through the body. The channel here can have any desired geometry. It can have a cross-sectional area changing over the length of the channel or, preferably; can have a constant channel cross-sectional area. The channel cross section can have, for example, an oval, round or polygonal outline with straight or rounded connections between the corners of the polygon. Preference is given to a round or equilateral polygonal cross section. Preferably, all channels in the body have the same geometry (cross section and length) and run parallel to one another. [0022] The terms "tube-bundle reactor" and "heat exchanger" describe collective parallel arrangements of a multiplicity of channels in the form of tubes, where the tubes can have any desired cross section. The tubes are arranged in a fixed spatial relationship to one another, are preferably present spatially separated from one another and are preferably surrounded by a shell which encloses all of the tubes. By this means, for example, a heating or cooling medium can be conducted through the shell, so that all of the tubes can be heated or cooled uniformly. [0023] The term "block of a solid material" describes a body of a solid material (which in turn can be made up of one or more starting materials) which has the channels, for example in the form of boreholes. The geometry of the channels (boreholes) can here be chosen freely as described above for the channels generally. The channels (boreholes) need not be installed by boring, but can be left open, for example even when forming the solid body/block, for instance by extruding an organic and/or inorganic molding composition (for example by an appropriate die geometry during extrusion). In contrast to the tube-bundle reactors or heat exchangers, the space in the body between the channels in the block is always filled by the solid material. Preferably, the block is made up of one or more metals. [0024] The term "predetermined" means that, for example, a number of different catalysts or catalyst precursors is introduced into a tube-bundle reactor or heat exchanger in such a manner that the assignation of the different catalysts or catalyst precursors to the individual tubes is recorded and can later be retrieved, for example, when determining the activity, selectivity and/or long-term stability of the individual catalysts, in order to make possible an unambiguous assignation of defined measured values to defined catalyst compositions. Preferably, the catalysts or their precursors are prepared and distributed to the different tubes of the tube-bundle reactor under computer control, the respective composition of a catalyst and the position of the tube in the tube-bundle reactor into which the catalyst or catalyst precursor is introduced is stored in the computer and can later be retrieved. The term "predetermined" thus serves to differentiate from a chance or random distribution of the generally different catalysts or catalyst precursors to the tubes of a tube-bundle reactor. Continue reading... Full patent description for Combinatorial preparation and testing of heterogeneous catalysts Brief Patent Description - Full Patent Description - Patent Application Claims Click on the above for other options relating to this Combinatorial preparation and testing of heterogeneous catalysts patent application. ###  How KEYWORD MONITOR works... a FREE service from FreshPatents1. Sign up (takes 30 seconds). 2. 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