Process and facility for examining chemical reactions in...

Details Process and facility for examining chemical reactions in... Process and facility for examining chemical reactions in...

1999-11-22

2003-06-10

Warden, Jill (Department: 1743)

Chemistry: analytical and immunological testing

Cancer

C422S068100, C422S071000, C422S139000, C422S140000, C422S141000, C422S146000, C422S159000

Reexamination Certificate

active

06576470

ABSTRACT:

The invention relates to a process for the study of chemical reactions in the presence of potentially catalytic substances, in which the reactions are carried out in parallel in reactors. The invention further relates to an apparatus, in particular for carrying out this process, the apparatus having a plurality of parallel-connected reactors which are provided with feedlines and discharge lines.
Processes and apparatuses of said type are known and are used, inter alia, in the search for catalysts for the heterogeneous or homogeneous catalysis of industrial chemical processes.
However, most recently, novel techniques have made it posible to prepare substances in a great number, which could be potential catalysts for a multiplicity of chemical processes (P. G. Schultz et al., Science 1995, 1738). The study of this multiplicity of potential catalysts is scarcely possible any longer using the conventional series screening processes, since these screening processes are limited with respect to throughput and analytical resolution, as well as in reproducibility. Frequently, for pure activity screening, integral effects such as heating of the catalyst etc. are used completely inadequately without direct product mixture analysis or efficiency analysis. Furthermore, optimizing the conditions of catalyst activation and process procedure make special requirements of quantitative analytical processes and of the reproducibility of the reaction conditions.
The object underlying the invention was therefore to develop an inexpensive process or an inexpensive apparatus by which a multiplicity of chemical reactions can be studied in a short time and thus reproducible, qualitative and quantitative data can be obtained with respect to the composition of the different reaction mixtures and reaction products.
This object is achieved by a process of the type mentioned at the outset, which is characterized in that the reactions are carried out in miniaturized reactors and the reaction mixture or the reaction products are analyzed with respect to nature and amount during the reaction period.
The object is further achieved by an apparatus of said type, which is characterized in that the reactors are miniaturized, at a volume from the range from 0.001 cm
3
to 1 cm
3
.
The invention thus relates to a process for the study of chemical reactions in the presence of potentially catalytic substances, in which the reactions are carried out in parallel in reactors, characterized in that the reactions are carried out in miniaturized reactors and the reaction mixture is analyzed with respect to nature and amount during the reaction period.
The invention further relates to an apparatus, in particular for carrying out this process, the apparatus having a plurality of parallel-connected reactors which are provided with feedlines and discharge lines, characterized in that the reactors are miniaturized, at a volume from the range from 0.001 cm
3
to 1 cm
3
.
Particular embodiments or developments of the invention result from the corresponding subclaims. Individual or a plurality of individual features mentioned in the claims can also each themselves represent solutions of the invention, and the features within the claim categories can also be combined as desired.
A particular embodiment of the process according to the invention is characterized in that the reaction starting materials are fed continuously to the reactors and the reaction products are discharged continuously from the reactors. However, the batch mode of operation is equally possible.
A further particular embodiment is characterized in that use is made of starting materials which are at least in part labeled with isotopes, preferably with deuterium (
2
H) or heavy oxygen (
18
O) or heavy carbon (
13
C) or mixtures thereof. These generate characteristic spectral shifts in rotation-vibration spectra, which, in addition to labeling the reaction pathway, owing to starting material mixed variants, can lead to novel interesting reactions or reaction products and relatively small by-product contents can be contrasted systematically.
Individual reactors or reactors combined to form groups can also be fed with different starting material mixtures, in order to reveal or detect any synergies present in this manner using the methods of combinatory chemistry.
The starting material mixtures, reaction mixtures or product mixtures can be analyzed with respect to nature and amount of the substances present at any time points of the course of the reaction by spectroscopic analysis, preferably by infrared spectroscopy (IR), particularly preferably by Fourier IR spectroscopy. Other spectroscopic methods, such as laser spectroscopy or UV spectroscopy, are equally suitable for the study. The process can be carried out at differing temperatures and pressures, at temperatures of the range from −50° C. up to and including 600° C., preferably from room temperature to 500° C., or at various pressures, at absolute pressures from 10
−3
to 10
3
bar, preferably from 10
−2
to 200 bar. The data obtained can then be supplied to a comprehensive parametric and data analysis.
The invention is further characterized in that the reactions can be carried out in the presence of a heterogeneous or homogeneous catalyst and in that it is possible to screen the catalytic activity (ie. product detection) and selectivity (main product distribution) of catalyst amounts less than 10 mg, preferably less than 1 mg, in a reactor.
In a particular embodiment of the apparatus according to the invention, a plurality of miniaturized reactors separated from one another can be disposed in a block. The volume of these reactors can be in the range from 0.001 cm
3
to 1 cm
3
, preferably from 0.01 cm
3
to 0.5 cm
3
, particularly preferably from 0.05 cm
3
to 0.2 cm
3
. In a further preferred embodiment of the apparatus according to the invention, the reactors are disposed as a square or rectangular pattern in a metal block, which can be parallelepipedal or cubic. The metal block can be provided with heating block elements or cooling elements and can be fitted with a temperature sensor in the vicinity of each reactor. This makes monitored and reproducible temperature control possible. For example, by this means, a defined temperature gradient can be set over the metal block. The reactors are advantageously disposed in a plane which is parallel to a surface of the parallelepiped. Advantageously, at least some of the feedlines and discharge lines of the individual reactors are perpendicular to this plane. They can be designed as through-holes in the metal block. The reactors can be designed as boreholes. The number of reactors in one block can be greater than 20, preferably greater than 40, particularly preferably greater than 100, very particularly preferably greater than 200. Using these reactors, under defined reaction conditions, a small amount of potential catalysts (also termed samples below) can be brought into contact and reacted in parallel, ie. simultaneously, with starting material or starting material mixtures in liquid and/or gaseous form batchwise or continuously. Automation of the apparatus according to the invention is possible, in particular charging the reactors with catalysts can proceed automatically, preferably by a laboratory robot or a pipetting machine.
In a further preferred embodiment, the miniaturized reactors are designed in the metal block as 4 mm bore holes and disposed in such a manner that differing starting material and inert gases can flow through them through 2.5 mm capillary bore holes. The gases then pass into a spacer, preferably a distancing plate, which is mounted on the metal block and in which the bore holes of the metal block continue. The arrangement of metal block and spacer is provided with a customary cuvette bore hole in which the gases can be analyzed by spectroscopy. For this purpose, the bore hole is sealed at both ends with a transparent window. If infrared spectroscopy is to be used for analysis, use is preferably made of windows of 1-1-1 silic

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