EP1796897B1 - Device and method for compressing particles - Google Patents

Device and method for compressing particles Download PDF

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Publication number
EP1796897B1
EP1796897B1 EP05777307A EP05777307A EP1796897B1 EP 1796897 B1 EP1796897 B1 EP 1796897B1 EP 05777307 A EP05777307 A EP 05777307A EP 05777307 A EP05777307 A EP 05777307A EP 1796897 B1 EP1796897 B1 EP 1796897B1
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EP
European Patent Office
Prior art keywords
container
particle
piston
containers
arrester
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Not-in-force
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EP05777307A
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German (de)
French (fr)
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EP1796897A1 (en
Inventor
Andreas Strasser
Alexander Cross
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HTE GmbH
HTE GmbH the High Throughput Experimentation Co
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HTE GmbH
HTE GmbH the High Throughput Experimentation Co
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Publication of EP1796897A1 publication Critical patent/EP1796897A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B11/00—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses
    • B30B11/02—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a ram exerting pressure on the material in a moulding space
    • B30B11/022—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a ram exerting pressure on the material in a moulding space whereby the material is subjected to vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B11/00—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses
    • B30B11/02—Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a ram exerting pressure on the material in a moulding space
    • B30B11/027—Particular press methods or systems
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B30—PRESSES
    • B30B—PRESSES IN GENERAL
    • B30B15/00—Details of, or accessories for, presses; Auxiliary measures in connection with pressing
    • B30B15/26—Programme control arrangements

Definitions

  • the present invention relates to an apparatus and a method for the controlled production of compacted particle beds.
  • the present invention is in the technical field of high throughput materials research, particularly high throughput catalyst research. It is known that the use of such high throughput methods can significantly increase the efficiency for finding new materials for particular purposes. It is u.a. important already in the preparation of the corresponding materials, e.g. in the production of heterogeneous catalysts to increase the production rate significantly, the reproducibility of the production and the implementation of the production and the receipt of well-defined products is particularly important. This is necessary, for example, in the preparation of heterogeneous catalysts because reliable test conditions can only be obtained in the subsequent catalyst screening if the heterogeneous catalysts, which are in the present case in the form of compacted particle beds as fixed-bed catalysts, are used with a predetermined degree of compaction. For this purpose, it is advantageous to prepare the heterogeneous catalysts underlying materials (compacted particle beds), also parallelized, preferably parallelized fully automated.
  • the generation of measurement data is based on the inclusion of powdery or particulate materials, which are used as compressed particle packages in the process Containers must be present.
  • the properties of a particle package and the reproducibility of the production of particle packages are decisive factors that significantly influence the quality of the measurement data.
  • the compaction of particles in containers by means of rammers is known.
  • the ramming devices consist of a sample container, which is subjected by means of electric motor drive a hammer-like impact movement.
  • the scope of application for such rammers is the physical characterization of particles.
  • the containers equipped with uncompressed particles are moved by means of the ramming device, whereby the ramming time and the ramming frequency are predetermined.
  • the particle bed is first compressed and occupies a certain volume, which has a characteristic size depending on the particular sample. Using the sample weight and sample volume parameters, the tamped density of the sample can be calculated after tamping the container.
  • the tube packages thus produced have several disadvantages.
  • the predominantly serial production of packages is very time-consuming and the compression of the used particle beds is not sufficiently high enough.
  • the reproducibility of the column packages produced by conventional methods also has limitations that reduce the size of test stands for catalytic and chromatographic investigations. Due to the inadequate reproducibility in the packing of columns, the production of complex column packings is extremely limited.
  • the parallelization of the method for packing columns using vibrators is technically associated with a very high cost.
  • a device for producing compressed particle beds with a container for receiving particles, a guide device for holding and guiding the container and a compacting device, wherein the compacting device is in operative connection with the container, as set forth in claim 1.
  • the device according to the invention has an adjustable stop, which is preferably adjustable in a multi-dimensional manner.
  • an adjustable stop which is preferably adjustable in a multi-dimensional manner.
  • the combination of linear uniaxial adjustment with a rotatable adjustment about a rotation axis may be mentioned here.
  • the stop can be designed such that in addition to the adjustability a complete disassembly of the stopper is possible.
  • the stop also preferably has clamping means with which the stop can be fixed in predetermined positions.
  • the stopper is also adapted to cooperate with means for guiding it.
  • the device according to the invention may further comprise one or more guide means for a plurality of containers, wherein the compression means comprises one or more reciprocating pistons.
  • This embodiment which is aimed particularly at the point of parallelization, makes it possible to produce a larger number of compacted particle beds in parallel.
  • one container is in operative connection with one reciprocating piston or several containers are operatively connected to a reciprocating piston.
  • the number of containers is preferably in the range from 2 to 1000, in particular in the range from 2 to 100.
  • the compression device of the device according to the invention preferably has one or more solenoid valves.
  • the one or more reciprocating piston of the compression device of the present invention are preferably operated pneumatically.
  • the supply of the pneumatic medium to the reciprocating piston is preferably controlled by means of the solenoid valves.
  • the containers of the device according to the invention also preferably have a closure or a plurality of closures, which are preferably gas-permeable.
  • the containers are tube reactors, which have at least one side such a gas-permeable closure.
  • This closure may, for example, be a frit or a fine-meshed wire net, which prevents the escape of the particles in the container.
  • the compression process can also be enhanced or assisted if a negative pressure is applied to the gas-permeable end side of the container by means of a vacuum pump.
  • the guide device of the device according to the invention can also have a closure in a further preferred embodiment, wherein this closure can replace the function of the stop.
  • this closure can replace the function of the stop.
  • after insertion of the container in the guide means this closed by the closure on one side.
  • the closure is preferably located on the the reciprocating piston opposite side.
  • the guide device can be designed in several parts, whereby a similar function of the closure or stop is achieved. Conceivable in this context would be, for example, a pipe construction in which two coaxial tubes of different diameters are adjustable and fixable against each other, wherein a tube is formed closed on one side and thus takes over the stop function.
  • the direction of movement of the reciprocating piston and the container of the device according to the invention is preferably vertical.
  • a horizontal reciprocating motion or a direction of movement of the reciprocating piston other than the vertical movement is also possible, wherein the backward movement of the container from the stop to the reciprocating piston can be supported in addition to the recoil pulse of spring elements.
  • the present invention comprises a data processing system.
  • this data processing system the control and / or regulation of the entire device or individual components and the method according to the invention is possible, which will be described in more detail below.
  • the particle size of the particles to be compacted is preferably in the particle size range from 4 ⁇ m to 5000 ⁇ m, particularly preferably in the particle size range from 40 ⁇ m to 600 ⁇ m.
  • the process according to the invention can be repeated in accordance with steps (a) to (c) with one or more further particulate materials.
  • the steps (a) to (c) with the other particulate materials are preferably carried out with one container each. Further, it is possible to sequentially fill and compact a container with various particulate materials, as well as compressing each individual particulate material sequentially in a container so as to achieve a stratified compacted particulate fill. In particular, for a clean layering of the individual particulate materials one above the other, the implementation of steps (a) to (c) is preferred in succession with each individual particulate material.
  • steps (a) to (c) are preferably carried out in parallel in the inventive method with multiple containers. This is of particular importance because the present process is used in high-throughput catalyst research and requires a large number of catalyst samples in the form of compacted particle beds with the same compaction properties.
  • the reciprocating pistons preferably execute a number of strokes in the range from 200 to 1200 strokes per minute. With a number of strokes in this range, the best compaction results are achieved, depending on the type and quantity of the particulate material to be compacted. However, a stroke rate outside this range is also conceivable.
  • the energy acting on the particulate material during compression is preferably predetermined by predetermined parameters. These parameters are preferably selected from the group: moving speed of the piston, acceleration of the piston, frequency of the piston strokes, distance from container to stop, elasticity of the stop, container and reciprocating material, total stroke rate and lifting force of the piston. This list is not exhaustive.
  • the enumerated parameters are preferably predetermined by means of the data processing system on the basis of stored nominal values for the respective particle type and particle quantity, and varied during the process depending on the degree of compaction to be achieved, which is achieved by means of the control and / or regulation of the device according to the invention or of individual components thereof.
  • the particles or the particulate material in the container or containers are compacted by means of an inhomogeneous movement and / or harmonic-rich oscillation.
  • the properties of the particulate materials - such as particle size, particle size distribution and density - significantly influence the compaction process.
  • the particle sizes of the particles to be compacted are generally in a range from 4 .mu.m to 5000 .mu.m, the particle size range from 40 .mu.m to 600 .mu.m being preferred.
  • a single particulate material can have different particle size distribution and density characteristics especially to one another.
  • the experimental conditions should be selected so that a separation of the particulate materials is excluded if possible during the experiment.
  • the container (s) are particularly preferably automatically transferred into the device with the particulate materials and removed again.
  • the device according to the invention can be automated in such a way that the containers are serially processed automatically, for example with a gripping arm for insertion or removal of the containers, which are provided, for example, by means of a conveyor belt.
  • the containers can be handled in the apparatus according to the invention, during insertion and / or execution of the container in or out of the device and outside the device, both individually in succession as well as several parallel automated.
  • the present invention further relates to a computer program with program code means for controlling or regulating the device according to the invention or for carrying out the method according to the invention as well as data carriers with this computer program.
  • This data carrier stores, for example, the parameters carried out in reference experiments as well as sequence routines which serve to control the device and the method by means of the computer program and the data processing system.
  • the method according to the invention is based inter alia on the fact that containers filled with particulate materials are exposed to a preferably mechanical action of energy by means of the device according to the invention.
  • the action of energy on the container filled with particles is controlled by means of the control or regulation of the device according to the invention, so that the degree of compaction of the particle bed and the time to reach the desired degree of compaction can be precisely specified.
  • a structure of complex packing structures in particular structured beds with layer structures
  • a compression of the different particle types, each with a different degree of compaction is possible.
  • Each type of particle is compacted in a container to a different degree of compaction. This is of course also possible with only one type of particle per container, which is compacted in layers in several consecutively performed steps (a) to (c) with different degrees of compaction.
  • the energy acting on the container filled with particulate materials is dictated by several control parameters.
  • control parameters include the speed of the pneumatically driven piston, the number of piston strokes per unit time and the distance from the top of the particle-filled container to the stop plate.
  • material and the elasticity of the stop plate can be specified.
  • the use of the stop plate for transmitting a recoil pulse to the container which is preferably in the form of a tubular reactor, in particular in the form of a liner, enables the container filled with particles to be twice the number of containers during an entire cycle of motion as compared with a container moved with rammers experiences of attacks.
  • the device according to the invention is operated without suspension or without the use of springs and is therefore much cheaper than the known apparatuses.
  • Another advantage of the device according to the invention is that the container is driven by an inhomogeneous movement, which leads to a harmonic richer than in the hitherto known devices or methods.
  • Example 1 relates to an embodiment of the device according to the invention, in which the pneumatic drive of the reciprocating piston is operated via an electronically clocked solenoid valve.
  • the steatite samples used in this case had a particle size in the range from 125 to 160 ⁇ m.
  • As a container for receiving the particles an approximately 300 mm long tube reactor was selected, the lower end - was provided with a gas-permeable plug - according to the usual and known in the art procedure. The inner diameter of the tube reactor was about 7 mm. Packing tests were carried out using stroke rates ranging between 200 and 1200 strokes per minute.
  • Comparative particle compaction investigations on the tubular reactor shown in Example 1 were carried out with a tamping volumeter and by means of ultrasonic excitation.
  • the variations in the height of the packed particulate beds in the case of the reactor packings produced by the apparatus according to the invention were substantially lower than the fluctuations in the height of the packed powder beds (particle beds) made according to the known methods.
  • the relative deviations in the package height produced by the device according to the invention packs was max. 2%.
  • the relative deviation of the packing height of packages made by known equipment was 5% and more.
  • the packing height of the particle beds produced by means of the device according to the invention was at least 20 mm lower than the height of the beds (packs) produced by known methods. As a result, it could be shown that the efficiency of the compression by means of the device according to the invention is higher than the effectiveness of known methods or devices.
  • the time required to achieve a constant height of the particle packing was substantially lower with the device according to the invention than with the use of the known apparatuses.
  • stable and more highly compressed particulate packages could be produced by the apparatus of the invention within one-third of the time compared to particle packages made according to known methods.
  • the inventive method using the device according to the invention is highly suitable for the simultaneous compression of a plurality of particle-filled reactors, which can be moved preferably as a reactor bundle in parallel.
  • a correspondingly designed lifting apparatus it is possible by means of a correspondingly designed lifting apparatus to simultaneously compact the particle beds in a large number of reactors.
  • the reproducibility of the compressed catalyst beds produced in this way is also higher than the beds produced according to known methods.
  • the method is particularly suitable for the production of compressed catalyst beds, in which the particulate catalyst material is compacted together with particulate, for example, inert material.
  • particulate for example, inert material.
  • inert material to the catalyst material allows the dilution of the catalyst material to be tested.
  • the inert material should have similar properties as the catalyst material with regard to the density and the particle size distribution have to exclude a particle separation during the compression process.
  • densified catalyst packs are used which are located in glass or ceramic containers.
  • the device according to the invention for particle compaction, it is possible that the particle beds are compacted in containers made of glass or ceramic.
  • the device according to the invention for example, elastic damping elements within the device or sheaths of the container, which prevent the breakage of the container.
  • the device according to the invention can be operated in an oven. This can be advantageous when it is necessary to heat the particulate materials to be compressed during the compression process.
  • the device according to the invention can be operated in a glove box, if the particles to be compressed should not be air-resistant.
  • the particulate material may be, for example, pulverulent material and the particles may be powder, for example.
  • FIG. 1 shows a device 10 according to the invention with a container 22, which is guided vertically by a guide device 14.
  • the guide device 14 is connected by means of two clamping elements 18 with a rod-shaped guide 16.
  • the clamping elements can be linearly displaced on the rod-shaped guide 16 in the direction of the longitudinal axis (rotation axis) of the rod-shaped guide 16 and rotated about the longitudinal axis of the rod-shaped guide 16.
  • the rod-shaped guide 16 is connected at the end to a carrier unit 12.
  • a compression device 20 is provided, which is arranged vertically in extension of the longitudinal axis of the guide device 14.
  • the compression device 20 may partially protrude on one side into the guide device 14.
  • the container 22 is due to its gravity on one side on a pneumatically operated reciprocating piston of the compression device 20.
  • the axes of rotation of the rotationally symmetrical device components compression device 20, guide device 14 and container 22 are preferably aligned vertically and congruent.
  • a stop 24 is further provided, which is displaceable along the rod-shaped guide 16 and rotatable about the longitudinal axis of the rod-shaped guide 16.
  • the stop 24 has a fastening element 26.
  • the plate-shaped stop 24 is fixed in operation at a certain distance from the end face 28 of the container 22 on the rod-shaped guide 16. In this case, the distance is dimensioned such that the container 22 strikes against the stop 24 during its vertical movement in the direction of the stop 24, even before it leaves the guide device 14. This ensures that the container 22 is always held or guided by the guide device 14 during the compression process and does not leave it.
  • the container 22 is closed during the compression process, so that no particles can leave the container 22. This is ensured, for example, by a closure which is provided at the location of the end face 28, in FIG. 1 however, is not shown in detail.
  • the guide device 14 is preferably provided in the form of a cylindrical holder, which serves to receive a container 22 filled with uncompressed particle beds and as a guide for the container 22 during the compression process.
  • the particle-filled container 22 is greatly accelerated by means of the linearly moving lifting piston of the compression device 20 along the cylindrical holder (guide device 14), so that the container is thrown in the direction of the stop 24 becomes.
  • the particle-filled container 22 can completely escape from the cylindrical support (guide means 14), it strikes with the end face 28 on the stopper 24, rebounds from the stop 24 and moves, due to gravity and from the stop 24th on the container 22 exerted recoil pulse, back into the cylindrical holder (guide means 14).
  • the container 22 strikes the reciprocating piston of Compressor 20 and is accelerated by the movement again in the direction of the stop 24.
  • FIG. 2 an embodiment of the device 10 according to the invention for receiving a plurality of containers 22 is shown.
  • each container 22 in this embodiment in each case a closure 30.
  • a larger stop 24 provided in this embodiment with a stop surface, which preferably corresponds to the cross-sectional area of the guide device 14, is fixed to a rod-shaped guide 16.
  • a likewise larger-sized compacting device 20 replaces the in FIG. 1 Provided support unit 12.
  • the compression device 20 serves in this embodiment as a receptacle for both the rod-shaped guide 16 and the guide means 14.
  • the guide means 14 may have a large recess for receiving the container 22 for all containers or a plurality of small recesses for each container , Accordingly, the compression device 20 is designed, which in the case of a large recess of the guide device 14 preferably has a reciprocating piston for all containers 22 or in the case of several small recesses in each case one reciprocating piston per container 22. In the latter case, the use of a reciprocating piston is conceivable which has a plurality of projections whose number and position corresponds to the container 22.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Basic Packing Technique (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)

Abstract

The present invention concerns a device (10) for the manufacture of compressed particle beds having a container (22) for receiving particles respectively materials in particle form, a guiding device (14) for the support and guidance of the container (22) and a compression equipment (22), whereby the compression equipment (20) is in effective connection with the container (22).

Description

Die vorliegende Erfindung betrifft eine Vorrichtung sowie ein Verfahren zur kontrollierten Herstellung von verdichteten Partikelschüttungen.The present invention relates to an apparatus and a method for the controlled production of compacted particle beds.

Die vorliegende Erfindung liegt auf dem technischen Gebiet der Hochdurchsatz-Materialforschung, insbesondere der Hochdurchsatz-Katalysatorforschung. Es ist bekannt, dass durch die Anwendung von derartigen Hochdurchsatz-Methoden die Effizienz bzw. Effektivität zum Auffinden neuer Materialien für bestimmte Zwecke signifikant erhöht werden kann. Dabei ist es u.a. wichtig, bereits bei der Herstellung der entsprechenden Materialien, z.B. bei der Herstellung von Heterogenkatalysatoren, die Herstellungsgeschwindigkeit deutlich zu steigern, wobei der Reproduzierbarkeit der Herstellung und der Durchführung der Herstellung und der Erhalt genau definierter Produkte besonders große Bedeutung zukommt. Dies ist beispielsweise bei der Herstellung von Heterogenkatalysatoren deshalb notwendig, weil beim anschließenden Katalysator-Screening verlässliche Testbedingungen nur erhalten werden können, wenn die Heterogenkatalysatoren, welche im vorliegenden Fall in Form von verdichteten Partikelschüttungen als Festbettkatalysatoren vorliegen, mit einem vorbestimmtem Verdichtungsgrad eingesetzt werden. Dazu ist es vorteilhaft, die den Heterogenkatalysatoren zugrundeliegenden Materialien (verdichtete Partikelschüttungen), ebenfalls parallelisiert, vorzugsweise voll automatisiert parallelisiert, herzustellen.The present invention is in the technical field of high throughput materials research, particularly high throughput catalyst research. It is known that the use of such high throughput methods can significantly increase the efficiency for finding new materials for particular purposes. It is u.a. important already in the preparation of the corresponding materials, e.g. in the production of heterogeneous catalysts to increase the production rate significantly, the reproducibility of the production and the implementation of the production and the receipt of well-defined products is particularly important. This is necessary, for example, in the preparation of heterogeneous catalysts because reliable test conditions can only be obtained in the subsequent catalyst screening if the heterogeneous catalysts, which are in the present case in the form of compacted particle beds as fixed-bed catalysts, are used with a predetermined degree of compaction. For this purpose, it is advantageous to prepare the heterogeneous catalysts underlying materials (compacted particle beds), also parallelized, preferably parallelized fully automated.

Bei vielen technischen Untersuchungen, wie beispielsweise bei der Testung von Katalysatoren und bei analytischen Tests basiert die Generierung von Messdaten auf einem Einbezug von pulver- beziehungsweise partikelförmigen Materialien, die während der Verfahrensdurchführung als verdichtete Partikelpackungen in Behältern vorliegen müssen. Die Eigenschaften einer Partikelpackung und die Reproduzierbarkeit der Herstellung von Partikelpackungen sind entscheidende Faktoren, die die Güte der Messdaten wesentlich beeinflussen.In many technical investigations, such as in the testing of catalysts and in analytical tests, the generation of measurement data is based on the inclusion of powdery or particulate materials, which are used as compressed particle packages in the process Containers must be present. The properties of a particle package and the reproducibility of the production of particle packages are decisive factors that significantly influence the quality of the measurement data.

Bekannt ist die Verdichtung von Partikeln in Behältern mittels Stampfgeräten. Die Stampfgeräte bestehen dabei aus einem Probenbehälter, der mittels Elektromotorantrieb einer hammerartigen Schlagbewegung unterworfen wird. Anwendungsbereich für solche Stampfgeräte ist die physikalische Charakterisierung von Partikeln. Die mit unverdichtetem Partikeln bestückten Behälter werden mittels des Stampfgerätes bewegt, wobei die Stampfzeit und die Stampffrequenz vorgegeben werden. Nachdem ein mit Partikeln befüllter Behälter einer ausreichenden Stampfbehandlung ausgesetzt wurde, wird die Partikelschüttung zunächst komprimiert und nimmt ein bestimmtes Volumen ein, das in Abhängigkeit von der jeweiligen Probe eine charakteristische Größe besitzt. Unter Verwendung der Parameter Probeneinwaage und Probenvolumen lässt sich nach der Stampfung des Behälters die Stampfdichte der Probe berechnen.The compaction of particles in containers by means of rammers is known. The ramming devices consist of a sample container, which is subjected by means of electric motor drive a hammer-like impact movement. The scope of application for such rammers is the physical characterization of particles. The containers equipped with uncompressed particles are moved by means of the ramming device, whereby the ramming time and the ramming frequency are predetermined. After a particle-filled container has been subjected to a sufficient ramming treatment, the particle bed is first compressed and occupies a certain volume, which has a characteristic size depending on the particular sample. Using the sample weight and sample volume parameters, the tamped density of the sample can be calculated after tamping the container.

Ferner ist bekannt, die Verdichtung von Partikelschüttungen in Behältern mittels Vibration der Behälter durchzuführen, wobei die mit Pulver beziehungsweise Partikeln befüllten Behälter wahlweise mittels mechanischer Vibratoren oder Ultraschallsonden behandelt werden.Furthermore, it is known to carry out the compression of particle beds in containers by means of vibration of the containers, wherein the containers filled with powder or particles are optionally treated by means of mechanical vibrators or ultrasonic probes.

Zur Herstellung von säulen- bzw. zylinderförmigen Pulver- beziehungsweise Partikelpackungen für Anwendungen in den Bereichen der Chromatografie und der Katalyse sind Methoden mittels Vibratoren allgemein etabliert.For the production of columnar or cylindrical powder or particle packages for applications in the fields of chromatography and catalysis methods are generally established by means of vibrators.

Die so hergestellten Röhrenpackungen weisen jedoch mehrere Nachteile auf. Die überwiegend seriell durchgeführt Herstellung von Packungen ist sehr zeitaufwendig und die Verdichtung des zum Einsatz kommenden Partikelschüttungen ist nicht ausreichend hoch genug. Die Reproduzierbarkeit der nach herkömmlichen Verfahren hergestellten Säulenpackungen weist zudem Limitierungen auf, die eine Verkleinerung von Testständen für katalytische und chromatografische Untersuchungen erschweren. Bedingt durch die mangelhafte Reproduzierbarkeit bei der Packung von Säulen, ist die Herstellung von komplex aufgebauten Säulenpakkungen äußerst eingeschränkt. Die Parallelisierung des Verfahrens zur Packung von Säulen unter Verwendung von Vibratoren ist technisch mit einem sehr hohen Aufwand verbunden.However, the tube packages thus produced have several disadvantages. The predominantly serial production of packages is very time-consuming and the compression of the used particle beds is not sufficiently high enough. The reproducibility of the column packages produced by conventional methods also has limitations that reduce the size of test stands for catalytic and chromatographic investigations. Due to the inadequate reproducibility in the packing of columns, the production of complex column packings is extremely limited. The parallelization of the method for packing columns using vibrators is technically associated with a very high cost.

Eine Aufgabe der vorliegenden Erfindung bestand demnach darin, eine Vorrichtung und ein Verfahren zur Verfugung zu stellen, womit eine schnellere Herstellung von verdichteten Partikelpackungen möglich ist, wobei die Partikelpackungen eine höhere Verdichtung aufweisen, die Reproduzierbarkeit verbessert wird, die Größe der Versuchsapparatur, innerhalb derer die verdichteten Partikelpakkungen zum Einsatz kommen, verkleinert und somit eine Parallelisierung von mehreren Vorrichtungen erreicht werden kann.It is therefore an object of the present invention to provide an apparatus and a method which allows faster production of compressed particulate packages, the particulate packages having a higher densification, reproducibility being improved, the size of the experimental apparatus within which compressed particle packages are used, downsized and thus parallelization of multiple devices can be achieved.

Diese und weitere Aufgaben werden gelöst durch eine Vorrichtung zur Herstellung von verdichteten Partikelschüttungen mit einem Behälter zur Aufnahme von Partikel, einer Führungseinrichtung zur Halterung und Führung des Behälters und einer Verdichtungseinrichtung, wobei die Verdichtungseinrichtung mit dem Behälter in Wirkverbindung steht, wie in Anspruch 1 ausgeführt.These and other objects are achieved by a device for producing compressed particle beds with a container for receiving particles, a guide device for holding and guiding the container and a compacting device, wherein the compacting device is in operative connection with the container, as set forth in claim 1.

Die erfindungsgemäße Vorrichtung weist einen verstellbaren Anschlag auf, welcher vorzugsweise mehrdimensional verstellbar ist. Beispielhaft sei hier die Kombination von linearer einachsiger Verstellung mit einer drehbaren Verstellung um eine Rotationsachse genannt. Ferner kann der Anschlag derart ausgestaltet sein, dass neben der Verstellbarkeit eine vollständige Demontage des Anschlags möglich ist. Der Anschlag weist zudem vorzugsweise Klemmmittel auf, mit welchen der Anschlag in vorbestimmten Positionen fixierbar ist. Der Anschlag ist ferner geeignet, mit Mitteln zu dessen Führung zusammenzuwirken.The device according to the invention has an adjustable stop, which is preferably adjustable in a multi-dimensional manner. As an example, the combination of linear uniaxial adjustment with a rotatable adjustment about a rotation axis may be mentioned here. Furthermore, the stop can be designed such that in addition to the adjustability a complete disassembly of the stopper is possible. The stop also preferably has clamping means with which the stop can be fixed in predetermined positions. The stopper is also adapted to cooperate with means for guiding it.

Die erfindungsgemäße Vorrichtung kann weiterhin eine oder mehrere Führungseinrichtungen für mehrere Behälter aufweisen, wobei die Verdichtungseinrichtung einen oder mehrere Hubkolben aufweist. Diese, insbesondere unter dem Gesichtspunkt der Parallelisierung angestrebte Ausführungsform, ermöglicht es, eine größere Anzahl von verdichteten Partikelschüttungen parallel herzustellen. Bevorzugt steht dabei jeweils ein Behälter mit jeweils einem Hubkolben in Wirkverbindung oder mehrere Behälter mit einem Hubkolben in Wirkverbindung. Die Anzahl der Behälter liegt dabei bevorzugt im Bereich von 2 bis 1000, insbesondere im Bereich von 2 bis 100.The device according to the invention may further comprise one or more guide means for a plurality of containers, wherein the compression means comprises one or more reciprocating pistons. This embodiment, which is aimed particularly at the point of parallelization, makes it possible to produce a larger number of compacted particle beds in parallel. Preferably, in each case one container is in operative connection with one reciprocating piston or several containers are operatively connected to a reciprocating piston. The number of containers is preferably in the range from 2 to 1000, in particular in the range from 2 to 100.

Des weiteren weist die Verdichtungseinrichtung der erfindungsgemäßen Vorrichtung bevorzugt ein oder mehrere Magnetventile auf. Der oder die Hubkolben der Verdichtungseinrichtung der vorliegenden Erfindung werden bevorzugt pneumatisch betrieben. Dabei wird mittels der Magnetventile vorzugsweise die Zufuhr des Pneumatikmediums zum Hubkolben gesteuert.Furthermore, the compression device of the device according to the invention preferably has one or more solenoid valves. The one or more reciprocating piston of the compression device of the present invention are preferably operated pneumatically. In this case, the supply of the pneumatic medium to the reciprocating piston is preferably controlled by means of the solenoid valves.

Die Behälter der erfindungsgemäßen Vorrichtung weisen zudem bevorzugt einen Verschluss beziehungsweise mehrere Verschlüsse auf, welche vorzugsweise gasdurchlässig sind. In einer bevorzugten Ausführungsform sind die Behälter Rohrreaktoren, welche wenigstens einseitig einen solchen gasdurchlässigen Verschluss aufweisen. Bei diesem Verschluss kann es sich beispielsweise um eine Fritte oder um ein feinmaschiges Drahtnetz handeln, wodurch der Austritt der in dem Behälter befindlichen Partikel verhindert wird. Der Verdichtungsvorgang kann zudem verstärkt bzw. unterstützt werden, wenn mittels einer Vakuumpumpe ein Unterdruck an der gasdurchlässigen Endseite des Behälters angelegt wird.The containers of the device according to the invention also preferably have a closure or a plurality of closures, which are preferably gas-permeable. In a preferred embodiment, the containers are tube reactors, which have at least one side such a gas-permeable closure. This closure may, for example, be a frit or a fine-meshed wire net, which prevents the escape of the particles in the container. The compression process can also be enhanced or assisted if a negative pressure is applied to the gas-permeable end side of the container by means of a vacuum pump.

Die Führungseinrichtung der erfindungsgemäßen Vorrichtung kann in einer weiterhin bevorzugten Ausführungsform ebenfalls einen Verschluss aufweisen, wobei dieser Verschluss die Funktion des Anschlags ersetzen kann. Dabei wird nach Einführen des Behälters in die Führungseinrichtung diese durch den Verschluss einseitig geschlossen. Der Verschluss befindet sich dabei vorzugsweise auf der dem Hubkolben gegenüberliegenden Seite. Weiterhin kann die Führungseinrichtung mehrteilig gestaltet sein, wodurch eine ähnliche Funktion des Verschlusses bzw. Anschlags erreicht wird. Denkbar in diesem Zusammenhang wäre beispielsweise eine Rohrkonstruktion, bei welcher koaxial zwei Rohre verschiedenen Durchmessers gegeneinander verstellbar und fixierbar sind, wobei ein Rohr einseitig geschlossen ausgebildet ist und somit die Anschlagsfunktion übernimmt.The guide device of the device according to the invention can also have a closure in a further preferred embodiment, wherein this closure can replace the function of the stop. In this case, after insertion of the container in the guide means this closed by the closure on one side. The closure is preferably located on the the reciprocating piston opposite side. Furthermore, the guide device can be designed in several parts, whereby a similar function of the closure or stop is achieved. Conceivable in this context would be, for example, a pipe construction in which two coaxial tubes of different diameters are adjustable and fixable against each other, wherein a tube is formed closed on one side and thus takes over the stop function.

Die Bewegungsrichtung des Hubkolbens sowie des Behälters der erfindungsgemäßen Vorrichtung ist bevorzugt vertikal. Dadurch kann auf Federelemente verzichtet werden, da der oder die Behälter aufgrund der Schwerkraft und aufgrund eines vom Anschlag auf die Behälter ausgeübten Rückstoßimpulses wieder zurück auf den Hubkolben fällt. Eine horizontale Hubkolbenbewegung bzw. eine Bewegungsrichtung des Hubkolbens verschieden von der vertikalen Bewegung ist ebenfalls möglich, wobei das Zurückbewegen des Behälters vom Anschlag zum Hubkolben zusätzlich zum Rückstoßimpuls von Federelementen unterstützt werden kann.The direction of movement of the reciprocating piston and the container of the device according to the invention is preferably vertical. As a result, it is possible to dispense with spring elements, since the container or containers falls back onto the reciprocating piston due to gravity and due to a recoil impulse exerted by the stop on the containers. A horizontal reciprocating motion or a direction of movement of the reciprocating piston other than the vertical movement is also possible, wherein the backward movement of the container from the stop to the reciprocating piston can be supported in addition to the recoil pulse of spring elements.

Vorteilhafterweise weist die vorliegende Erfindung eine Datenverarbeitungsanlage auf. Mit dieser Datenverarbeitungsanlage ist die Steuerung und/oder Regelung der gesamten Vorrichtung bzw. einzelner Komponenten sowie des erfindungsgemäßen Verfahrens möglich, welches im Folgenden näher beschrieben wird.Advantageously, the present invention comprises a data processing system. With this data processing system, the control and / or regulation of the entire device or individual components and the method according to the invention is possible, which will be described in more detail below.

Die Partikelgröße der zu verdichtenden Partikel liegt bevorzugt im Teilchengrößenbereich von 4 µm bis 5000 µm, insbesondere bevorzugt im Teilchengrößenbereich von 40 µm bis 600 µm.The particle size of the particles to be compacted is preferably in the particle size range from 4 μm to 5000 μm, particularly preferably in the particle size range from 40 μm to 600 μm.

Die vorliegende Erfindung betrifft neben der bereits beschriebenen Vorrichtung ein Verfahren zur Herstellung von verdichteten Partikelschüttungen, welches die Schritte:

  1. (a) Befüllen eines Behälters mit einem ersten partikelförmigen Material,
  2. (b) Verschließen des Behälters und
  3. (c) Verdichten des ersten partikelförmigen Materials
umfasst, wobei ein Hubkolben derart auf den Behälter einwirkt, dass der Behälter in einer Führungseinrichtung in Richtung eines Anschlags beschleunigt wird und sich nach Aufprall auf den Anschlag wieder in Richtung des Hubkolbens zurück bewegt. Dieser Bewegungsablauf des Behälters wird entsprechend einer bestimmten Hubzahl solange wiederholt, bis ein vordefinierter Verdichtungsgrad des ersten partikelförmigen Materials erreicht ist. Dabei kann beispielsweise die Hubzahl sowie die Hubgeschwindigkeit von der Datenverarbeitungsanlage entsprechend dem erreichten Verdichtungsgrad in Abhängigkeit zum vordefinierten Verdichtungsgrad variiert werden.The present invention relates, in addition to the apparatus already described, to a method for the production of compacted particle beds, which comprises the steps:
  1. (a) filling a container with a first particulate material,
  2. (b) closing the container and
  3. (c) compacting the first particulate material
wherein a reciprocating piston acts on the container such that the container is accelerated in a guide device in the direction of a stop and moves back after impact on the stop back in the direction of the reciprocating piston. This movement of the container is repeated according to a certain stroke number until a predefined degree of compaction of the first particulate material is reached. In this case, for example, the number of strokes and the lifting speed of the data processing system can be varied according to the achieved degree of compaction in dependence on the predefined degree of compaction.

Das erfindungsgemäße Verfahren kann entsprechend der Schritte (a) bis (c) mit einem oder mehreren weiteren partikelförmigen Materialien wiederholt werden. Dabei werden die Schritte (a) bis (c) mit den weiteren partikelförmigen Materialien vorzugsweise mit jeweils einem Behälter durchgeführt. Ferner ist es möglich, einen Behälter mit verschiedenen partikelförmigen Materialien nacheinander zu befüllen und zu verdichten, wie auch das Verdichten jedes einzelnen partikelförmigen Materials nacheinander in einem Behälter, um so eine geschichtete verdichtete Partikelschüttung zu erreichen. Insbesondere für eine saubere Schichtung der einzelnen partikelförmigen Materialien übereinander ist die Durchführung der Schritte (a) bis (c) nacheinander mit jedem einzelnen partikelförmigen Material bevorzugt.The process according to the invention can be repeated in accordance with steps (a) to (c) with one or more further particulate materials. The steps (a) to (c) with the other particulate materials are preferably carried out with one container each. Further, it is possible to sequentially fill and compact a container with various particulate materials, as well as compressing each individual particulate material sequentially in a container so as to achieve a stratified compacted particulate fill. In particular, for a clean layering of the individual particulate materials one above the other, the implementation of steps (a) to (c) is preferred in succession with each individual particulate material.

Die Schritte (a) bis (c) werden bei dem erfindungsgemäßen Verfahren bevorzugt mit mehreren Behältern parallel durchgeführt. Dies ist insbesondere deshalb von Bedeutung, da das vorliegende Verfahren in der Hochdurchsatz-Katalysatorforschung zur Anwendung kommt und dabei eine hohe Anzahl von Katalysatorproben in Form von verdichteten Partikelschüttungen mit gleichen Verdichtungseigenschaften benötigt werden.The steps (a) to (c) are preferably carried out in parallel in the inventive method with multiple containers. This is of particular importance because the present process is used in high-throughput catalyst research and requires a large number of catalyst samples in the form of compacted particle beds with the same compaction properties.

Bevorzugt führen die Hubkolben bei dem erfindungsgemäßen Verfahren eine Hubzahl im Bereich von 200 bis 1200 Hüben pro Minute aus. Mit einer Hubzahl in diesem Bereich werden je nach Art und Menge des zu verdichtenden partikelförmigem Material die besten Verdichtungsergebnisse erzielt Eine Hubzahl außerhalb dieses Bereiches ist jedoch ebenfalls denkbar.In the method according to the invention, the reciprocating pistons preferably execute a number of strokes in the range from 200 to 1200 strokes per minute. With a number of strokes in this range, the best compaction results are achieved, depending on the type and quantity of the particulate material to be compacted. However, a stroke rate outside this range is also conceivable.

Die während der Verdichtung auf das partikelförmige Material einwirkende Energie wird bevorzugt durch vorbestimmte Parameter vorgegeben. Diese Parameter werden vorzugsweise ausgewählt aus der Gruppe: Bewegungsgeschwindigkeit des Kolbens, Beschleunigung des Kolbens, Frequenz der Kolbenhübe, Abstand von Behälter zu Anschlag, Elastizität des Anschlag-, Behälter- und Hubkolbenmaterials, Gesamthubzahl sowie Hubkraft des Kolbens. Diese Aufzählung ist nicht abschließend. Die aufgezählten Parameter werden vorzugsweise mittels der Datenverarbeitungsanlage anhand von gespeicherten Sollwerten für die jeweilige Partikelart und Partikelmenge vorbestimmt, und während des Verfahrens je nach zu erreichendem Verdichtungsgrad variiert, was mittels der Steuerung und/oder Regelung der erfindungsgemäßen Vorrichtung bzw. einzelner ihrer Komponenten erreicht wird.The energy acting on the particulate material during compression is preferably predetermined by predetermined parameters. These parameters are preferably selected from the group: moving speed of the piston, acceleration of the piston, frequency of the piston strokes, distance from container to stop, elasticity of the stop, container and reciprocating material, total stroke rate and lifting force of the piston. This list is not exhaustive. The enumerated parameters are preferably predetermined by means of the data processing system on the basis of stored nominal values for the respective particle type and particle quantity, and varied during the process depending on the degree of compaction to be achieved, which is achieved by means of the control and / or regulation of the device according to the invention or of individual components thereof.

Charakteristisch für das erfindungsgemäße Verfahren ist weiterhin, dass die Partikel beziehungsweise das partikelförmige Material in dem oder den Behältern mittels einer inhomogenen Bewegung und/oder oberwellenreichen Schwingung verdichtet werden.It is furthermore characteristic of the method according to the invention that the particles or the particulate material in the container or containers are compacted by means of an inhomogeneous movement and / or harmonic-rich oscillation.

In diesem Zusammenhang wird darauf hingewiesen, dass die Eigenschaften der partikelförmigen Materialien - wie beispielsweise Teilchengröße, Teilchengrößenverteilung und Dichte - den Verdichtungsvorgang entscheidend beeinflussen. Die Teilchengrößen der zu verdichtenden Partikel liegen im allgemeinen in einem Bereich von 4 µm bis 5000 µm, wobei der Teilchengrößenbereich von 40 µm bis 600 µm bevorzugt ist. Ein einzelnes partikelförmiges Material kann unterschiedliche Eigenschaften bezüglich der Teilchengrößenverteilungen und Dichte aufweisen insbesondere gegenüber einem anderen. Die experimentellen Bedingungen sollten so gewählt werden, dass bei der Versuchsdurchführung eine Entmischung der partikelförmigen Materialien möglichst ausgeschlossen wird.In this context, it should be noted that the properties of the particulate materials - such as particle size, particle size distribution and density - significantly influence the compaction process. The particle sizes of the particles to be compacted are generally in a range from 4 .mu.m to 5000 .mu.m, the particle size range from 40 .mu.m to 600 .mu.m being preferred. A single particulate material can have different particle size distribution and density characteristics especially to one another. The experimental conditions should be selected so that a separation of the particulate materials is excluded if possible during the experiment.

Besonders bevorzugt werden bei dem erfindungsgemäßen Verfahren der oder die Behälter, mit den partikelförmigen Materialien automatisiert in die Vorrichtung übergeben und wieder entnommen. Die erfindungsgemäße Vorrichtung kann dabei so automatisiert werden, dass die Behälter seriell automatisch abgearbeitet werden, beispielsweise mit einem Greifarm zum Ein- beziehungsweise Ausführen der Behälter, welche zum Beispiel mittels eines Fließbands bereitgestellt werden. Die Behälter können dabei in der erfindungsgemäßen Vorrichtung, beim Ein- und/oder Ausführen der Behälter in oder aus der Vorrichtung sowie außerhalb der Vorrichtung, sowohl einzeln nacheinander als auch zu mehreren parallel automatisiert gehandhabt werden.In the method according to the invention, the container (s) are particularly preferably automatically transferred into the device with the particulate materials and removed again. The device according to the invention can be automated in such a way that the containers are serially processed automatically, for example with a gripping arm for insertion or removal of the containers, which are provided, for example, by means of a conveyor belt. The containers can be handled in the apparatus according to the invention, during insertion and / or execution of the container in or out of the device and outside the device, both individually in succession as well as several parallel automated.

Die vorliegende Erfindung betrifft ferner ein Computerprogramm mit Progammcodemitteln zur Steuerung oder Regelung der erfindungsgemäßen Vorrichtung oder zur Durchführung des erfindungsgemäßen Verfahrens sowie Datenträger mit diesem Computerprogramm. Auf diesem Datenträger sind beispielsweise die in Referenzversuchen durchgeführten Parameter sowie Ablaufroutinen gespeichert, welche mittels des Computerprogramms und der Datenverarbeitungsanlage zur Steuerung bzw. Regelung der Vorrichtung und des Verfahrens dienen.The present invention further relates to a computer program with program code means for controlling or regulating the device according to the invention or for carrying out the method according to the invention as well as data carriers with this computer program. This data carrier stores, for example, the parameters carried out in reference experiments as well as sequence routines which serve to control the device and the method by means of the computer program and the data processing system.

Das erfindungsgemäße Verfahren basiert unter anderem darauf, dass mit partikelförmigen Materialien befüllte Behälter mittels der erfindungsgemäßen Vorrichtung einer vorzugsweise mechanischen Energieeinwirkung ausgesetzt werden. Insbesondere die Energieeinwirkung auf die mit Partikeln befüllten Behälter wird mittels der Steuerung bzw. Regelung der erfindungsgemäßen Vorrichtung kontrolliert, so dass der Verdichtungsgrad der Partikelschüttung und die Zeit zum Erreichen des gewünschten Verdichtungsgrades genau vorgegeben werden kann. Durch die wiederholte Anwendung des Verfahrens auf einen oder mehrere Behälter, die sukzessive mit unterschiedlichen Partikelsorten befüllt werden, ist ein Aufbau von komplexen Packungsstrukturen (insbesondere strukturierten Schüttungen mit Schichtstrukturen) möglich. Ferner ist eine Verdichtung der unterschiedlichen Partikelsorten mit jeweils unterschiedlichem Verdichtungsgrad möglich. Dabei wird jede Partikelsorte in einem Behälter auf einen anderen Verdichtungsgrad verdichtet. Dies ist selbstverständlich auch mit nur einer Partikelsorte je Behälter möglich, welche schichtweise in mehreren nacheinander durchgeführten Schritten (a) bis (c) mit unterschiedlichem Verdichtungsgrad verdichtet wird.The method according to the invention is based inter alia on the fact that containers filled with particulate materials are exposed to a preferably mechanical action of energy by means of the device according to the invention. In particular, the action of energy on the container filled with particles is controlled by means of the control or regulation of the device according to the invention, so that the degree of compaction of the particle bed and the time to reach the desired degree of compaction can be precisely specified. By repeatedly applying the method to one or more containers, which are successively filled with different types of particles, a structure of complex packing structures (in particular structured beds with layer structures) is possible. Furthermore, a compression of the different particle types, each with a different degree of compaction is possible. Each type of particle is compacted in a container to a different degree of compaction. This is of course also possible with only one type of particle per container, which is compacted in layers in several consecutively performed steps (a) to (c) with different degrees of compaction.

Die Energie, die auf den mit partikelförmigen Materialien befüllten Behälter einwirkt, wird durch mehrere Steuerparameter vorgegeben. Zu den bevorzugten Steuerparametern gehören dabei die Geschwindigkeit des pneumatisch angetriebenen Kolbens, die Zahl der Kolbenhübe pro Zeiteinheit sowie die Entfernung von der Oberkante des mit Partikeln befüllten Behälters bis zur Anschlagplatte. Darüber hinaus kann auch das Material und die Elastizität der Anschlagplatte vorgegeben werden. Die Nutzung der Anschlagplatte zur Übertragung eines Rückstoßimpulses auf den Behälter, welcher bevorzugt in Form eines Rohrreaktors, insbesondere in Form eines Liners vorliegt, ermöglicht es, dass der mit Partikeln befüllte Behälter im Vergleich zu einem mit Stampfgeräten bewegten Behälter während eines gesamten Bewegungszyklus die doppelte Anzahl von Anschlägen erfährt. Bei Stampfgeräten bewegt sich nur der Stampfkolben, nicht aber der Behälter mit dem zu verdichtenden partikelförmigen Material, wodurch das partikelförmige Material pro Hub nur einmal verdichtet wird, im Gegensatz zur vorliegenden Erfindung, bei welcher das partikelförmige Material pro Hub zweimal verdichtet wird. Die erfindungsgemäße Vorrichtung wird ohne Federung beziehungsweise ohne den Einsatz von Federn betrieben und ist daher viel kostengünstiger als die bekannten Apparaturen. Ein weiterer Vorteil der erfindungsgemäßen Vorrichtung ist, dass der Behälter durch eine inhomogene Bewegung angetrieben wird, die zu einer oberwellenreicheren Schwingung führt, als bei den bisher bekannten Geräten bzw. Verfahren.The energy acting on the container filled with particulate materials is dictated by several control parameters. Among the preferred control parameters include the speed of the pneumatically driven piston, the number of piston strokes per unit time and the distance from the top of the particle-filled container to the stop plate. In addition, the material and the elasticity of the stop plate can be specified. The use of the stop plate for transmitting a recoil pulse to the container, which is preferably in the form of a tubular reactor, in particular in the form of a liner, enables the container filled with particles to be twice the number of containers during an entire cycle of motion as compared with a container moved with rammers experiences of attacks. In rammers, only the ram, but not the container moves with the particulate material to be compacted, whereby the particulate material is compressed only once per stroke, in contrast to the present invention, in which the particulate material is compressed twice per stroke. The device according to the invention is operated without suspension or without the use of springs and is therefore much cheaper than the known apparatuses. Another advantage of the device according to the invention is that the container is driven by an inhomogeneous movement, which leads to a harmonic richer than in the hitherto known devices or methods.

Weitere bevorzugte Ausführungsformen der erfindungsgemäßen Vorrichtung sind im nachfolgenden Teil beispielhaft aufgeführt und sind in keiner Weise als Einschränkung des erfindungsgemäßen Gegenstands zu verstehen.Further preferred embodiments of the device according to the invention are exemplified in the following part and are in no way to be understood as a limitation of the subject matter of the invention.

Beispiel 1:Example 1:

Beispiel 1 bezieht sich auf eine Ausführungsform der erfindungsgemäßen Vorrichtung, bei der der Pneumatikantrieb des Hubkolbens über ein elektronisch getaktetes Magnetventil betrieben wird. Zur Untersuchung der Eigenschaften von Packungen (verdichtete Partikelschüttungen) wurden Untersuchungen mit Steatit durchgeführt. Die hierbei eingesetzten Steatitproben hatten eine Teilchengröße im Bereich von 125 bis 160 µm. Als Behälter für die Aufnahme der Partikel wurde ein etwa 300 mm langer Rohrreaktor ausgewählt, dessen unteres Ende - gemäß der üblichen und dem Fachmann bekannten Vorgehensweise - mit einem gasdurchlässigen Stopfen versehen wurde. Der Innendurchmesser des Rohrreaktors betrug etwa 7 mm. Packungsuntersuchungen wurden unter Verwendung von Hubzahlen im Bereich zwischen 200 und 1200 Hüben pro Minute durchgeführt.Example 1 relates to an embodiment of the device according to the invention, in which the pneumatic drive of the reciprocating piston is operated via an electronically clocked solenoid valve. To investigate the properties of packages (compacted particle beds), tests were carried out with steatite. The steatite samples used in this case had a particle size in the range from 125 to 160 μm. As a container for receiving the particles, an approximately 300 mm long tube reactor was selected, the lower end - was provided with a gas-permeable plug - according to the usual and known in the art procedure. The inner diameter of the tube reactor was about 7 mm. Packing tests were carried out using stroke rates ranging between 200 and 1200 strokes per minute.

Beispiele 2 und 3:Examples 2 and 3:

Vergleichende Partikelverdichtungsuntersuchungen an dem im Beispiel 1 dargestellten Rohrreaktor wurden mit einem Stampfvolumeter und mittels Ultraschallanregung durchgeführt.Comparative particle compaction investigations on the tubular reactor shown in Example 1 were carried out with a tamping volumeter and by means of ultrasonic excitation.

Die Schwankungen in der Höhe der gepackten Partikelbetten waren im Fall der mittels der erfindungsgemäßen Vorrichtung hergestellten Reaktorpackungen wesentlich geringer, als die Schwankungen in der Höhe der gepackten Pulverbetten (Partikelbetten), welche gemäß den bekannten Verfahren hergestellt wurden. Die relativen Abweichungen in der Packungshöhe mittels der erfindungsgemäßen Vorrichtung hergestellter Packungen betrug max. 2 %. Die relative Abweichung der Packungshöhe von mittels bekannten Apparaturen hergestellter Packungen betrug demgegenüber 5 % und mehr. Die Packungshöhe der mittels der erfindungsgemäßen Vorrichtung hergestellten Partikelbetten war mindestens 20 mm niedriger als die Höhe der Betten (Packungen), die nach bekannten Verfahren hergestellt wurden. Daraus resultierend konnte gezeigt werden, dass die Wirksamkeit der Verdichtung mittels der erfindungsgemäßen Vorrichtung höher ist, als die Wirksamkeit bekannter Verfahren bzw. Vorrichtungen.The variations in the height of the packed particulate beds in the case of the reactor packings produced by the apparatus according to the invention were substantially lower than the fluctuations in the height of the packed powder beds (particle beds) made according to the known methods. The relative deviations in the package height produced by the device according to the invention packs was max. 2%. The relative deviation of the packing height of packages made by known equipment was 5% and more. The packing height of the particle beds produced by means of the device according to the invention was at least 20 mm lower than the height of the beds (packs) produced by known methods. As a result, it could be shown that the efficiency of the compression by means of the device according to the invention is higher than the effectiveness of known methods or devices.

Die Zeitdauer zur Erreichung einer konstanten Höhe der Partikelpackung war mit der erfindungsgemäßen Vorrichtung zudem wesentlich geringer, als unter Verwendung der bekannten Apparaturen. Bei der Herstellung von Partikelpackungen unter Verwendung der gleichen Hubfrequenz konnten mittels der erfindungsgemäßen Vorrichtung innerhalb von einem Drittel der Zeitdauer stabile und höher komprimierte Partikelpackungen im Vergleich zu gemäß bekannten Verfahren hergestellten Partikelpackungen hergestellt werden.In addition, the time required to achieve a constant height of the particle packing was substantially lower with the device according to the invention than with the use of the known apparatuses. In the production of particle packages using the same stroke frequency, stable and more highly compressed particulate packages could be produced by the apparatus of the invention within one-third of the time compared to particle packages made according to known methods.

Das erfindungsgemäße Verfahren unter Verwendung der erfindungsgemäßen Vorrichtung eignet sich in hohem Maße zur gleichzeitigen Verdichtung von mehreren mit Partikeln befüllten Reaktoren, die vorzugsweise als Reaktorbündel parallel bewegt werden können. Innerhalb von kurzen Zeiträumen ist es mittels einer entsprechend ausgelegten Hubapparatur möglich, die Partikelschüttungen in einer Vielzahl von Reaktoren gleichzeitig zu verdichten. Die Reproduzierbarkeit der auf diese Weise hergestellten komprimierten Katalysatorbetten ist zudem höher, als die, gemäß bekannter Verfahren hergestellten Betten.The inventive method using the device according to the invention is highly suitable for the simultaneous compression of a plurality of particle-filled reactors, which can be moved preferably as a reactor bundle in parallel. Within a short period of time, it is possible by means of a correspondingly designed lifting apparatus to simultaneously compact the particle beds in a large number of reactors. The reproducibility of the compressed catalyst beds produced in this way is also higher than the beds produced according to known methods.

Das Verfahren eignet sich insbesondere für die Herstellung von verdichteten Katalysatorbetten, bei denen das partikelförmige Katalysatormaterial gemeinsam mit partikelförmigem beispielsweise Inertmaterial verdichtet wird. Die Beimischung von Inertmaterial zum Katalysatormaterial ermöglicht die Verdünnung des zu testenden Katalysatormaterials. Das Inertmaterial sollte bezüglich der Dichte und der Partikelgrößenverteilung ähnliche Eigenschaften wie das Katalysatormaterial besitzen, um eine Partikelseparation während des Verdichtungsvorgangs auszuschließen.The method is particularly suitable for the production of compressed catalyst beds, in which the particulate catalyst material is compacted together with particulate, for example, inert material. The addition of inert material to the catalyst material allows the dilution of the catalyst material to be tested. The inert material should have similar properties as the catalyst material with regard to the density and the particle size distribution have to exclude a particle separation during the compression process.

Bei katalytischen Testuntersuchungen kommt es vor, dass die mit Inertmaterial verdünnten Katalysatoren in unverdichteten Schüttungen untersucht werden. Es wäre demnach denkbar, dass die katalytischen Testdaten, die in Verbindung mit dem erfindungsgemäßen Verfahren erzielt werden, auf Grund der hohen Reproduzierbarkeit bei der Herstellung der Katalysatorpackung geringere Streuungen aufweisen, als diejenigen, die mit unverdichteten Katalysatorbetten erzielt werden.In catalytic test studies, it is possible that the catalysts diluted with inert material are investigated in unconsolidated beds. It would thus be conceivable that the catalytic test data obtained in connection with the method according to the invention, due to the high reproducibility in the preparation of the catalyst pack, have lower scattering than those achieved with uncompacted catalyst beds.

Bei einigen technischen Anwendungen werden verdichtete Katalysatorpackungen eingesetzt, die sich in Glas- oder Keramikbehältem befinden. Bei speziellen Ausführungsformen der erfindungsgemäßen Vorrichtung zur Partikelverdichtung ist es möglich, dass die Partikelschüttungen in Behältern aus Glas oder Keramik verdichtet werden. Bei diesen speziellen Ausführungsformen weist die erfindungsgemäße Vorrichtung beispielsweise elastische Dämpfungselemente innerhalb der Vorrichtung bzw. Ummantelungen der Behälter auf, die das Zerbrechen der Behälter verhindern.In some engineering applications, densified catalyst packs are used which are located in glass or ceramic containers. In special embodiments of the device according to the invention for particle compaction, it is possible that the particle beds are compacted in containers made of glass or ceramic. In these specific embodiments, the device according to the invention, for example, elastic damping elements within the device or sheaths of the container, which prevent the breakage of the container.

In weiteren möglichen Ausführungsformen kann die erfindungsgemäße Vorrichtung in einem Ofen betrieben werden. Dies kann dann von Vorteil sein, wenn es erforderlich ist, die zu verdichtenden partikelförmigen Materialien während des Verdichtungsvorgangs zu erhitzen. Darüber hinaus kann die erfindungsgemäße Vorrichtung in einer Glove-Box betrieben werden, falls die zu komprimierenden Partikel nicht luftbeständig sein sollten.In further possible embodiments, the device according to the invention can be operated in an oven. This can be advantageous when it is necessary to heat the particulate materials to be compressed during the compression process. In addition, the device according to the invention can be operated in a glove box, if the particles to be compressed should not be air-resistant.

Bei dem partikelförmigen Material kann es sich beispielsweise um pulverförmiges Material und bei den Partikeln beispielsweise um Pulver handeln.The particulate material may be, for example, pulverulent material and the particles may be powder, for example.

Weitere Merkmale der Erfindung ergeben sich aus der Beschreibung der beiliegenden Zeichnungen.Further features of the invention will become apparent from the description of the accompanying drawings.

Die Erfindung wird im Folgenden an Hand weiterer in den Zeichnungen dargestellter Ausführungsbeispiele näher erläutert. Dabei zeigen

Fig. 1
eine schematische Darstellung der erfindungsgemäßen Vorrichtung zur Aufnahme eines Behälters, und
Fig. 2
eine schematische Darstellung einer erfindungsgemäßen Vorrichtung zur Aufnahme mehrerer Behälter.
The invention is explained in more detail below with reference to further exemplary embodiments illustrated in the drawings. Show
Fig. 1
a schematic representation of the device according to the invention for receiving a container, and
Fig. 2
a schematic representation of a device according to the invention for receiving a plurality of containers.

Figur 1 zeigt eine erfindungsgemäße Vorrichtung 10 mit einem Behälter 22, welcher vertikal von einer Führungseinrichtung 14 geführt wird. Die Führungseinrichtung 14 ist mittels zweier Klemmelemente 18 mit einer stabförmigen Führung 16 verbunden. Die Klemmelemente können an der stabförmigen Führung 16 linear in Richtung der Längsachse (Rotationsachse) der stabförmigen Führung 16 verschoben und drehbar um die Längsachse der stabförmigen Führung 16 verdreht werden. Die stabförmige Führung 16 ist stirnseitig mit einer Trägereinheit 12 verbunden. FIG. 1 shows a device 10 according to the invention with a container 22, which is guided vertically by a guide device 14. The guide device 14 is connected by means of two clamping elements 18 with a rod-shaped guide 16. The clamping elements can be linearly displaced on the rod-shaped guide 16 in the direction of the longitudinal axis (rotation axis) of the rod-shaped guide 16 and rotated about the longitudinal axis of the rod-shaped guide 16. The rod-shaped guide 16 is connected at the end to a carrier unit 12.

Zwischen Führungseinrichtung 14 und Trägereinheit 12 ist eine Verdichtungseinrichtung 20 vorgesehen, welche in Verlängerung der Längsachse der Führungseinrichtung 14 vertikal angeordnet ist. Die Verdichtungseinrichtung 20 kann einseitig zum Teil in die Führungseinrichtung 14 hineinragen. Nach dem Einsetzen des zylinderförmigen Behälters 22 in die ebenfalls zylinderförmige Ausnehmung der Führungseinrichtung 14, liegt der Behälter 22 aufgrund seiner Schwerkraft einseitig auf einem pneumatisch betriebenen Hubkolben der Verdichtungseinrichtung 20 auf. Die Rotationsachsen der rotationssymmetrischen Vorrichtungskomponenten Verdichtungseinrichtung 20, Führungseinrichtung 14 und Behälter 22 sind bevorzugt vertikal ausgerichtet und deckungsgleich.Between the guide device 14 and the carrier unit 12, a compression device 20 is provided, which is arranged vertically in extension of the longitudinal axis of the guide device 14. The compression device 20 may partially protrude on one side into the guide device 14. After insertion of the cylindrical container 22 in the likewise cylindrical recess of the guide device 14, the container 22 is due to its gravity on one side on a pneumatically operated reciprocating piston of the compression device 20. The axes of rotation of the rotationally symmetrical device components compression device 20, guide device 14 and container 22 are preferably aligned vertically and congruent.

An der stabförmigen Führung 16 ist weiterhin ein Anschlag 24 vorgesehen, welcher entlang der stabförmigen Führung 16 verschiebbar und um die Längsachse der stabförmigen Führung 16 drehbar ist. Zur Lagefixierung relativ zur stabförmigen Führung 16 weist der Anschlag 24 ein Befestigungselement 26 auf. Der plattenförmige Anschlag 24 wird im Betrieb mit einem bestimmten Abstand zur Stirnseite 28 des Behälters 22 an der stabförmigen Führung 16 fixiert. Dabei ist der Abstand so bemessen, dass der Behälter 22 bei seiner vertikalen Bewegung in Richtung des Anschlags 24 an den Anschlag 24 anschlägt, noch bevor er die Führungseinrichtung 14 verlässt. Somit ist sichergestellt, dass der Behälter 22 während des Verdichtungsvorgangs immer von der Führungseinrichtung 14 gehalten bzw. geführt wird und diese nicht verlässt. Der Behälter 22 ist während des Verdichtungsvorgangs verschlossen, so dass kein Partikel den Behälter 22 verlassen kann. Das wird beispielsweise durch einen Verschluss sichergestellt, welcher an der Stelle der Stirnseite 28 vorgesehen, in Figur 1 jedoch nicht näher dargestellt ist.On the rod-shaped guide 16, a stop 24 is further provided, which is displaceable along the rod-shaped guide 16 and rotatable about the longitudinal axis of the rod-shaped guide 16. For fixing the position relative to the rod-shaped guide 16, the stop 24 has a fastening element 26. The plate-shaped stop 24 is fixed in operation at a certain distance from the end face 28 of the container 22 on the rod-shaped guide 16. In this case, the distance is dimensioned such that the container 22 strikes against the stop 24 during its vertical movement in the direction of the stop 24, even before it leaves the guide device 14. This ensures that the container 22 is always held or guided by the guide device 14 during the compression process and does not leave it. The container 22 is closed during the compression process, so that no particles can leave the container 22. This is ensured, for example, by a closure which is provided at the location of the end face 28, in FIG FIG. 1 however, is not shown in detail.

Die Führungseinrichtung 14 ist vorzugsweise in Form einer zylinderförmigen Halterung vorgesehen, welche der Aufnahme eines mit unverdichtetem Partikelschüttungen gefüllten Behälters 22 und als Führung für den Behälter 22 während des Verdichtungsvorgangs dient. Zur Verdichtung der Partikelschüttungen bzw. zur Herstellung einer verdichteten säulenförmigen Partikelpackung, wird der mit Partikeln befüllte Behälter 22 mittels des sich linear bewegenden Hubkolbens der Verdichtungseinrichtung 20 entlang der zylinderförmigen Halterung (Führungseinrichtung 14) stark beschleunigt, so dass der Behälter in Richtung des Anschlags 24 geschleudert wird. Noch bevor der mit Partikeln gefüllte Behälter 22 vollständig aus der zylinderförmigen Halterung (Führungseinrichtung 14) austreten kann, schlägt er mit der Stirnseite 28 auf den Anschlag 24 auf, prallt von dem Anschlag 24 ab und bewegt sich, aufgrund der Schwerkraft und des vom Anschlag 24 auf den Behälter 22 ausgeübten Rückstoßimpulses, zurück in die zylinderförmige Halterung (Führungseinrichtung 14). In der zylinderförmigen Halterung (Führungseinrichtung 14) schlägt der Behälter 22 auf den Hubkolben der Verdichtungseinrichtung 20 auf und wird durch dessen Bewegung erneut in Richtung des Anschlags 24 beschleunigt.The guide device 14 is preferably provided in the form of a cylindrical holder, which serves to receive a container 22 filled with uncompressed particle beds and as a guide for the container 22 during the compression process. For compacting the particle beds or for producing a compacted columnar particle packing, the particle-filled container 22 is greatly accelerated by means of the linearly moving lifting piston of the compression device 20 along the cylindrical holder (guide device 14), so that the container is thrown in the direction of the stop 24 becomes. Even before the particle-filled container 22 can completely escape from the cylindrical support (guide means 14), it strikes with the end face 28 on the stopper 24, rebounds from the stop 24 and moves, due to gravity and from the stop 24th on the container 22 exerted recoil pulse, back into the cylindrical holder (guide means 14). In the cylindrical holder (guide means 14), the container 22 strikes the reciprocating piston of Compressor 20 and is accelerated by the movement again in the direction of the stop 24.

In Figur 2 ist eine Ausführungsform der erfindungsgemäßen Vorrichtung 10 zur Aufnahme mehrerer Behälter 22 dargestellt. Dabei weist jeder Behälter 22 in dieser Ausführungsform jeweils einen Verschluss 30 auf. Ein in dieser Ausführungsform größer vorgesehener Anschlag 24 mit einer Anschlagfläche, welche vorzugsweise der Querschnittsfläche der Führungseinrichtung 14 entspricht, ist an einer stabförmigen Führung 16 fixiert. In dieser Ausführungsform ersetzt eine ebenfalls größer gestaltete Verdichtungseinrichtung 20 die in Figur 1 vorgesehene Trägereinheit 12. Die Verdichtungseinrichtung 20 dient in dieser Ausführungsform als Aufnahme sowohl für die stabförmige Führung 16 als auch für die Führungseinrichtung 14. Die Führungseinrichtung 14 kann zur Aufnahme der Behälter 22 eine große Ausnehmung für alle Behälter oder mehrerer kleine Ausnehmungen für jeweils einen Behälter aufweisen. Entsprechend ist die Verdichtungseinrichtung 20 gestaltet, welche im Falle einer großen Ausnehmung der Führungseinrichtung 14 vorzugsweise einen Hubkolben für alle Behälter 22 oder im Falle mehrerer kleiner Ausnehmungen jeweils einen Hubkolben pro Behälter 22 aufweist. Im letzteren Fall ist auch die Verwendung eines Hubkolbens denkbar, welcher mehrere Vorsprünge aufweist, deren Anzahl und Lage der der Behälter 22 entspricht.In FIG. 2 an embodiment of the device 10 according to the invention for receiving a plurality of containers 22 is shown. In this case, each container 22 in this embodiment in each case a closure 30. A larger stop 24 provided in this embodiment with a stop surface, which preferably corresponds to the cross-sectional area of the guide device 14, is fixed to a rod-shaped guide 16. In this embodiment, a likewise larger-sized compacting device 20 replaces the in FIG. 1 Provided support unit 12. The compression device 20 serves in this embodiment as a receptacle for both the rod-shaped guide 16 and the guide means 14. The guide means 14 may have a large recess for receiving the container 22 for all containers or a plurality of small recesses for each container , Accordingly, the compression device 20 is designed, which in the case of a large recess of the guide device 14 preferably has a reciprocating piston for all containers 22 or in the case of several small recesses in each case one reciprocating piston per container 22. In the latter case, the use of a reciprocating piston is conceivable which has a plurality of projections whose number and position corresponds to the container 22.

Bezugszeichenliste:LIST OF REFERENCE NUMBERS

10 -10 -
erfindungsgemäße Vorrichtunginventive device
12 -12 -
Trägereinheitsupport unit
14 -14 -
Führungseinrichtungguide means
16 -16 -
stabförmige Führungrod-shaped guide
18 -18 -
Klemmelementclamping element
20 -20 -
Verdichtungseinrichtungcompacting device
22 -22 -
Behältercontainer
24 -24 -
Anschlagattack
26 -26 -
Befestigungselementfastener
28 -28 -
Stirnseite eines Behälters 22Front side of a container 22
30 -30 -
Verschluss eines Behälters 22Closure of a container 22

Claims (15)

  1. Device (10) for the manufacture of compressed particle bulks comprising a container (22) for receiving particle-shaped materials, a guidance equipment (14) for supporting and guiding the container (22) and a compression equipment (20), wherein the compression equipment (20) comprises a piston, which is in operative connection with container (22), characterized in that the device comprises an adjustable arrester (24), wherein the piston acts on the container (22) such that the container is accelerated in a guidance equipment (14) in direction of an arrester (24) and, after the impact on arrester (24), moves back in direction of the piston.
  2. Device (10) according to claim 1, which comprises one or several guidance equipments (14) for several containers (22).
  3. Device (10) according to claim 1 or 2, in which the compression equipment (20) comprises one or several magnetic valves.
  4. Device (10) according to any one of the preceding claims, in which one container (22), respectively, is in operative connection with one piston, respectively, or in which several containers (22) are in operative connection with a piston.
  5. Device (10) according to any one of the preceding claims, in which the containers (22) comprise one or several closings (30), or in which the containers (22) are tubular reactors, which comprise at least on one side a gas-permeable closing.
  6. Device (10) according to any one of the preceding claims, in which the guidance equipment (14) comprises a closing.
  7. Device (10) according to any one of the preceding claims, in which the particle size of the particles to be compressed is in a particle size range of from 4 µm to 5,000 µm, particularly preferred in a particle size range of from 40 µm to 600 µm.
  8. Process for the manufacture of compressed particle bulks comprising the following steps:
    (a) filling a container (22) with a first particle-shaped material,
    (b) closing the container (22), and
    (c) compressing the first particle-shaped material, wherein a piston acts on the container (22) such that the container is accelerated in a guidance equipment (14) in direction of an arrester (24) and, after the impact on arrester (24), moves back in direction of the piston.
  9. Process according to claim 8, in which the course of movement of container (22) is repeated according to a number of strokes until a pre-defined degree of compression of the first particle-shaped material is achieved.
  10. Process according to claim 8 or 9, in which the steps (a) to (c) are repeated with one or several further particle-shaped materials, or in which the steps (a) to (c) are parallelly performed with several containers (22).
  11. Process according to any one of claims 8 to 10, in which the pistons perform a number of strokes in the range of from 200 to 1,200 strokes per minute.
  12. Process according to any one of claims 8 to 11, in which the energy which acts on the particle-shaped material is provided by pre-determined parameters.
  13. Process according to claim 12, in which the parameter is selected from the group: speed of movement of the piston, acceleration of the piston, frequency of the piston strokes, distance from container (22) to arrester (24), elasticity of the arrester material, container material and piston material, total number of strokes, lifting power of the piston.
  14. Process according to any one of claims 8 to 13, in which the particle-shaped material is compressed in container (22) by means of an inhomogeneous movement and/or a harmonic-rich oscillation.
  15. Process according to any one of claims 8 to 14, in which the container or the containers (22) comprising particle-shaped materials are automatedly transferred into the device and are re-taken from the device.
EP05777307A 2004-08-24 2005-08-23 Device and method for compressing particles Not-in-force EP1796897B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004040939A DE102004040939A1 (en) 2004-08-24 2004-08-24 Apparatus and method for compacting particles
PCT/EP2005/009100 WO2006021424A1 (en) 2004-08-24 2005-08-23 Device and method for compressing particles

Publications (2)

Publication Number Publication Date
EP1796897A1 EP1796897A1 (en) 2007-06-20
EP1796897B1 true EP1796897B1 (en) 2010-08-04

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EP05777307A Not-in-force EP1796897B1 (en) 2004-08-24 2005-08-23 Device and method for compressing particles

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US (1) US20090166906A1 (en)
EP (1) EP1796897B1 (en)
AT (1) ATE476286T1 (en)
DE (2) DE102004040939A1 (en)
WO (1) WO2006021424A1 (en)

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Publication number Priority date Publication date Assignee Title
WO2021048373A1 (en) 2019-09-13 2021-03-18 Hte Gmbh The High Throughput Experimentation Company Method for filling reactors and for examining catalytic reactors

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DE102014211278A1 (en) 2014-06-12 2015-12-17 Hte Gmbh The High Throughput Experimentation Company Compact catalyst test stand and filling it

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US2855628A (en) * 1953-08-17 1958-10-14 Benjamin Lassman & Son Pressure bonding system for solid particles
US3332456A (en) * 1965-03-23 1967-07-25 Joseph J Hasch Tamping machine
DE2552852C3 (en) * 1975-11-25 1980-12-11 Schlosser & Co Gmbh, 6209 Aarbergen Method for compacting molded bodies made of concrete or the like. plastic masses
DK29785A (en) * 1984-05-29 1985-11-30 L & N Int As PROCEDURE FOR COMPRESSING NEW CASTED CONCRETE AND APPARATUS FOR EXERCISING THE PROCEDURE
DE3630869A1 (en) * 1986-09-11 1988-03-17 Meissner Gmbh & Co Kg Josef PRESS FOR COMPRESSING POWDERED GOODS
FR2638118A1 (en) * 1988-10-20 1990-04-27 Adl Automation METHOD AND APPARATUS FOR COMPRESSION AND CONTROL OF COMPRESSION OF PULVERULENT AND PRESSED MATERIALS BY APPLYING
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021048373A1 (en) 2019-09-13 2021-03-18 Hte Gmbh The High Throughput Experimentation Company Method for filling reactors and for examining catalytic reactors
US11738316B2 (en) 2019-09-13 2023-08-29 Hte Gmbh The High Throughput Experimentation Method for filling reactors and for examining catalytic reactors

Also Published As

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US20090166906A1 (en) 2009-07-02
DE502005010049D1 (en) 2010-09-16
EP1796897A1 (en) 2007-06-20
WO2006021424A1 (en) 2006-03-02
DE102004040939A1 (en) 2006-03-02
ATE476286T1 (en) 2010-08-15

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