EP2629886A2 - Dispositif et procédé pour analyser des catalyseurs par réglage variable de la pression de traitement - Google Patents

Dispositif et procédé pour analyser des catalyseurs par réglage variable de la pression de traitement

Info

Publication number
EP2629886A2
EP2629886A2 EP11771033.5A EP11771033A EP2629886A2 EP 2629886 A2 EP2629886 A2 EP 2629886A2 EP 11771033 A EP11771033 A EP 11771033A EP 2629886 A2 EP2629886 A2 EP 2629886A2
Authority
EP
European Patent Office
Prior art keywords
line
lines
investigation
solid catalysts
reaction chamber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP11771033.5A
Other languages
German (de)
English (en)
Inventor
Armin Lange De Oliveira
Michael Dejmek
Oliver KÖCHEL
Jürgen BECHTEL
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HTE GmbH the High Throughput Experimentation Co
Original Assignee
HTE GmbH
HTE GmbH the High Throughput Experimentation Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HTE GmbH, HTE GmbH the High Throughput Experimentation Co filed Critical HTE GmbH
Priority to EP11771033.5A priority Critical patent/EP2629886A2/fr
Publication of EP2629886A2 publication Critical patent/EP2629886A2/fr
Withdrawn legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00281—Individual reactor vessels
    • B01J2219/00286—Reactor vessels with top and bottom openings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00389—Feeding through valves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00389—Feeding through valves
    • B01J2219/00391—Rotary valves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00423—Means for dispensing and evacuation of reagents using filtration, e.g. through porous frits
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00477—Means for pressurising the reaction vessels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00495—Means for heating or cooling the reaction vessels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00585—Parallel processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00596—Solid-phase processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00583—Features relative to the processes being carried out
    • B01J2219/00601—High-pressure processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/0068—Means for controlling the apparatus of the process
    • B01J2219/00686—Automatic
    • B01J2219/00689—Automatic using computers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/0068—Means for controlling the apparatus of the process
    • B01J2219/00702—Processes involving means for analysing and characterising the products
    • B01J2219/00707—Processes involving means for analysing and characterising the products separated from the reactor apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00718—Type of compounds synthesised
    • B01J2219/00745—Inorganic compounds
    • B01J2219/00747—Catalysts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
    • B01J2219/00792—One or more tube-shaped elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00835—Comprising catalytically active material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00869—Microreactors placed in parallel, on the same or on different supports
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00873—Heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/0095—Control aspects
    • B01J2219/00952—Sensing operations
    • B01J2219/00954—Measured properties
    • B01J2219/00963—Pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/0095—Control aspects
    • B01J2219/00986—Microprocessor

Definitions

  • the invention relates to a device and a method for the investigation of catalysts and for the optimization of process conditions.
  • the device according to the invention and the method according to the invention it is possible to precisely adjust the internal pressure within the individual reaction chambers and also to vary them in a controlled manner.
  • Characteristic of the device according to the invention is a division of the reaction chamber outlet-side lines into two subgroups of lines, the lines being in operative connection with control valves and / or switching valves.
  • the invention is particularly suitable for use in devices in which a plurality or a plurality of reactors are arranged in parallel.
  • the invention is of particular importance in the field of high throughput research for the development of catalysts and for the optimization of process conditions.
  • Numerous devices for the parallel testing of catalysts are known from the prior art. These devices often differ in complexity, which may vary depending on the specific technical requirements.
  • the present invention is in principle in the field of device types equipped with a special process control system, as described in more detail, for example, in US Pat. No. 7,537,739 B2.
  • This special process control system is inter alia also characterized in that the reactors arranged in parallel are equipped with a common pressure control gas supply and a common pressure maintenance gas supply.
  • One of the objects according to the invention is to provide a catalytic converter with the aid of which the process pressure adjustment can be implemented in as variable a manner as possible. At the same time the most accurate process pressure control within the reactors should be made possible and the apparatus should have a comparatively simple technical construction.
  • a catalytic apparatus for the investigation of solid catalysts in a continuous process with at least one reaction space (101), a common educt fluid supply (01) and a reaction chamber exit-side conduit (201) marked that
  • each reaction chamber exit-side line is in operative connection with a main line (411) and a secondary line (311),
  • the main line (411) is in operative connection with a control valve (61) and an exhaust line (62),
  • Analyzer unit (34) is operatively connected.
  • the connection line upstream of the restrictor element (331) has a switching valve (321).
  • each reaction chamber outlet-side line (201) is in operative connection with a line for regulating fluid supply (211).
  • connection point of reaction space outlet line (201), main line (41 1) and secondary line (311) comprises a mixing vessel and / or liquid phase separator (301).
  • the main conduit (50) is equipped with a pressurized gas supply line (50).
  • the catalytic converter according to the invention with a plurality or a multiplicity of reaction spaces (101, 102,%) With a common educt fluid supply (01) and a reaction chamber exit-side conduit (201, 202,...), Is characterized in that
  • each reaction chamber exit-side line (201, 202, 7) is in operative connection with one main line (41 1, 412, 413,.
  • each of the main pipes (411, 412, 413, ...) is connected to a common exhaust pipe (62),
  • each secondary line is optionally in operative connection with its own switching valve (321, 322, 323,...) and is in operative connection with an analysis unit (34), wherein preferably in the individual operative connecting lines between the switching valve (321, 322, 323, ...) and analysis unit (34) in each case a restrictor element (331, 332, 333, 7) is present, and more preferably one or more multiport valves.
  • the apparatus according to the invention is characterized in that the connection points of the individual reaction chamber exit-side lines (201, 202,%) to the main lines (411, 412,. lines (31 1, 312, ...) each comprise a mixing vessel or a liquid phase separator (301, 302, 303, ).
  • each individual main line in each case has a feed line (401, 402, 403,%) For pressurized gas.
  • each individual line of the educt fluid supply is provided with a preferably passive restrictor element.
  • the restrictor elements (331, 332, 333,...) Or (33) are micro-regulating valves.
  • the control valves or micro-regulating valves must have a suitable setting range. Suitable adjustment range means that the adjustment range can be adapted to the prevailing pressure and the prevailing flow velocity, so that the flow can be changed by at least 5% (relative).
  • control valve (61) is a high-temperature control valve or consists of a cascade of control valves or high-temperature control valves.
  • the invention also relates to a method for the investigation of solid catalysts or for the optimization of process conditions by means of the catalytic converter according to the invention, wherein the educt fluid is simultaneously passed through a plurality of reaction spaces (101, 102,...) And the method is characterized in that
  • Reaction spaces through the standing with the respective reaction space in operative connection secondary line (311, 312, ...) to an analysis unit or a plurality of analysis lines (34) are passed, wherein the pressure in the individual reaction chambers by means of the control valve (61) is controlled.
  • the process according to the invention is preferably characterized in that it is used for the investigation of solid catalysts or for the optimization of process conditions, the process being carried out in a pressure range from 0 to 200 bar, preferably from 0 to 100 bar and more preferably from 0 to 30 bar , and preferably the pressure in this case can be varied continuously or discontinuously within the pressure range.
  • the process according to the invention is characterized in that the process is carried out at a reaction chamber internal temperature in the range from 20 to 1200 ° C., a temperature range from 50 to 800 ° C. is preferred, and a temperature range from 100 to 650 ° C. is particularly preferred.
  • the present invention also relates to a computer with a computer program product - or a processor-based control device such as a PLC - for controlling the catalytic converter according to the invention and for carrying out the method according to the invention.
  • a computer program product - or a processor-based control device such as a PLC - for controlling the catalytic converter according to the invention and for carrying out the method according to the invention.
  • Fig. 1 shows the schematic representation of an apparatus according to the invention with a single reactor (101), in which the reaction chamber output side line
  • (201) is divided into two sub-lines (411) and (311), wherein the sub-line (411) leads to the exhaust air and the sub-line (311) to the analysis unit (34).
  • the exhaust air line (411) is provided with control valve (61) and the connecting line (311) to the analysis unit (34) is provided with switching valve (321) and flow restrictor or restriction (331).
  • Fig. 2 shows the schematic representation of an apparatus according to the invention with two parallel reactors (101, 102, ...), in which the with Analyzer unit (34) connected reaction chamber output side connecting lines (311) with a multiport valve (07) are in operative connection.
  • FIG. 3 shows the schematic representation of an apparatus according to the invention with three reactors (101, 102,%) Arranged in parallel, in which the connection lines leading to the reaction chamber exit to mixing elements (301, 302, etc And in the lines to the analysis unit (34 ) no multiport valve is arranged.
  • Fig. 4 shows a schematic representation of an apparatus according to the invention with three parallel reactors (101, 102, ...), which corresponds to the device shown in Fig. 3, wherein the output lines (31 1, 312, 313) for the gaseous compounds via a single flow regulator or via a single throttle element (33) are guided.
  • the output lines (31 1, 312, 313) for the gaseous compounds via a single flow regulator or via a single throttle element (33) are guided.
  • Fig. 3 per gas line (301, 302, ...) each have their own throttle element is arranged.
  • Fig. 5 shows the schematic representation of the apparatus according to the invention, which is equipped with a single reactor (101), wherein in the illustration, the control devices for flow and pressure control are shown.
  • the apparatus shown in the illustration is equipped with a pressurized gas supply.
  • the pressure regulating fluid supply is not present in this embodiment.
  • a feature of the catalytic converter according to the invention is also that the reaction chamber output-side lines (201, 202, ...) do not lead to a common damping container. Moreover, it is preferred that the connecting lines between the output sides of the reactors and the control valve (61) have no check valves.
  • the catalyst apparatus according to the invention it is possible to keep the pressure conditions in the individual reactors during the performance of the catalytic experiments largely constant.
  • the catalytic converter according to the invention has individual line regions, in which the diameters are increased in relation to the lines at the other points.
  • the extended diameter and enlarged volume regions have the function of a mixing section in which the pressurizing gas and the product fluid stream are thoroughly mixed. These regions are also referred to below as mixing containers (301, 302,).
  • a mixing container according to the present invention preferably has at least twice the diameter as the line leading to the mixing container (301, 302, ). Further preferably, a mixing container (301, 302, ...) at least a length to diameter ratio of two to one. It is further preferred that in the mixing vessel flow-breaking internals are included, such as Raschig rings, split, frits, broken granules or packing for distillation columns. It can also be used internals that correspond in their kind to the distillation columns, such as bubble cap.
  • the individual exhaust pipes (31 1, 312,%) Which lead to the analysis unit (34) are connected directly to the respective mixing vessels (301, 302,). In this way, it is achieved that a very well mixed sample can be taken from the product fluid stream leaving the reactor.
  • the apparatus according to the invention is operated as a gas-phase apparatus, which means that predominantly gaseous educt fluids are converted to predominantly gaseous product fluids.
  • the mixing vessel or the mixing vessels (301, 302, for pure mixing function also have the function of a separator or a collecting container (or collection containers) for liquid samples.
  • the exhaust lines leading to the analysis unit (311, 312,...) are preferably connected in a manner to the mixing containers or separators, so that substantially only gaseous product fluid is removed from the separators.
  • the mixing container or separator has the function of a damping container, which ensures that the pressure in the interior of lines and reactors during the gas removal does not change or only slightly.
  • the gas is removed via the exhaust pipes (311, 312, ...) and serves to supply analysis gas to the analysis unit.
  • the catalytic device it is also possible to remove liquid sample from the separator or the separators.
  • This can be done either via a common discharge valve for liquid and gaseous sample or two separate drain valves.
  • the drain valve for liquid sample preferably acts on the bottom of the mixing container or separator.
  • the effect on the floor is represented by the fact that the valve is located at the lower part of the container or that it is connected to a riser inside the container.
  • the gaseous sample discharge valve removes the gaseous sample from the gas space of the mixing vessel or separator in the outflow.
  • the throttling elements (331, 332, 333, ...) in the exhaust pipes, it is preferred that these are passive or active restrictor elements.
  • active Restriktorettin With the passive or set to a constant value active Restriktorettin thus creates a control.
  • a control loop it is also possible for a control loop to be integrated in this plant area. This is realized by providing one or more flow sensors upstream or downstream of throttle elements or actuating elements (331, 332,...) Which act on the element (33).
  • the flow sensor is a mass flow sensor or a volume flow sensor.
  • Suitable passive restrictor elements are, for example, capillaries, pinhole diaphragms, microchannels or porous frits.
  • the active throttle elements are preferably microvalves (fine regulating needle valves), mass flow controllers or even automated fine regulating valves.
  • the automated fine regulating valves may, for example, be ReCO valves from Badger-Meter.
  • the apparatus has a hot gas analyzer as an analysis unit, it is possible to detect both the amount of gas sample taken and the composition. It is also possible that an accurate quantitative detection takes place by correcting the signal of the hot gas flow meter by the gas composition determined by means of the hot gas analyzer. It should be noted that the total product gas flow of the respective reactor is taken to determine an absolute flow rate. However, this also requires the separate supply of pressure-holding gas or additional pressure build-up gas into each individual exhaust gas line (see Figure 4, lines 401, 402, ).
  • a predetermined amount of reference gas which represents an internal standard and makes it possible to quantitatively detect the recovery rate of carrier gas or pressure build-up gas, is added to the fluid streams.
  • This internal standard may be, for example, a certain proportion of argon gas. Due to the addition of a standard, it is not necessary to quantitatively detect the amount that is conveyed through the output lines (31 1, 312, ...) to the analysis unit. This can be advantageous, as a result of the measurement and control effort which would otherwise be required for the quantitative detection of gas flows and the associated balancing of the reaction.
  • the quantitative detection then takes place through the analysis of the gas flow.
  • a gas chromatograph is used as an analysis unit equipped with a heat conductivity or helium ionization detector sensitive to argon.
  • other analytical methods are used accordingly.
  • the configuration disclosed herein of a combination of a GC detector used with argon gas as a standard or tracer gas is exemplified herein. Any other possible combination of internal standard and a substance-specific detector can also be used.
  • the main flow and the product fluid are supplied via a common control valve (61) of the exhaust air.
  • the pressure can be controlled efficiently within the catalytic apparatus and within the individual reaction spaces. It should be emphasized as advantageous in the method and the apparatus of the present invention that in the present case the pressure can be regulated over a wider range than is possible with catalytic converters which are known in the prior art - as for example in US Pat. No. 7,537,739 B2.
  • the individual exhaust pipes (411, 412, 413, ...) are brought together in line (42), wherein the line (42) has a control valve (61) having a variable flow resistance.
  • the variable control valve (61) assumes the function of the parallel arranged restrictors, which - according to the embodiment according to US 7,537,739 B2 - have a fixed flow resistance.
  • control valve (61) depends on the particular use of the catalytic converter and is in this case in no way limited. If the catalytic converter is connected to a large number of reactors, it is possible, and in this case preferred, for a plurality of control valves (61) to be arranged in parallel and for that valve to be actuated with the control range of the master value suitable for the present pressure regime or a group be controlled simultaneously by control valves, as this the pressure control range can be additionally increased in a simple manner.
  • the apparatus is provided with a pressure regulator.
  • the control valve (61) is controlled by a pressure regulator.
  • the reaction chamber output-side line region is in this case in operative connection with a pressure sensor, wherein the controller determines its actual value on the basis of this pressure sensor.
  • FIG. Since the line with the control valve (61) is a main line, the pressure control is carried out in this embodiment of the apparatus via the main line.
  • the pressure regulator receives its actual value from the line (42) or from the lines (411, 412, 413, ).
  • the pressure regulator is arranged in a bypass line. In this case, the pressure regulator acts on the control valve in the pressure hold gas line.
  • the pressure regulator receives values from the system that are not altered by disruptive effects if possible.
  • one or more switchable restrictor elements can be connected in parallel to the line section with the variable restrictor element (331).
  • the circuit takes place here by means of valves.
  • the connection of restrictor elements has the advantage that the adjustment range of the variable restrictor element (331) can be adapted in stages to the experimental conditions, whereby this can preferably also be automated.
  • the adjustment range of the control valve (61) can be adjusted by connecting restrictor elements in parallel by means of valves.
  • the selection of the sampling valve depends on the respective application. It is possible that the control valves are used in exhaust gas streams whose temperature is in a range of 500 to 600 ° C. At the same time, it is possible to vary the pressures within the catalytic apparatus and within the individual reactors over a very wide range.
  • the apparatus according to the invention thus also offers the advantage that the majority of the volume flow can be conducted via the lines to the control valve (61).
  • the control valve is designed so that it is particularly suitable for high-temperature operation. A small part of the volume flow is passed through the output lines (311, 312, 313, ...), whereby the components (321, 322, 323, ...) exposed to a lower thermal load.
  • the direct removal of the product fluid stream compared to US 7,537,739 B2 has the further advantage that the sample is not diluted by pressure holding gas, so that the optimization of the sample analysis in the real composition of the Product fluid flow can take place and any dilution effects (reduction detection limit, etc.) must be disregarded.
  • the device according to the invention is preferably used for the investigation of catalysts in the laboratory or on a technical scale.
  • the catalysts used for the investigations are preferably present as solids and the absorption capacity of the individual reaction space is preferably 0.1 g to 100 g of catalyst, more preferably the absorption capacity of the individual reaction space is 1 g to 50 g.
  • the volume of the individual reaction space is preferably in a range from 0.1 ml to 150 ml, more preferably in a range from 1 ml to 100 ml and most preferably in a range from 5 ml to 50 ml.
  • the GHSV used for the tests is preferably in a range of 300 to 10,000 h -1 , preferably 500 to 3,000 h -1 , whereas the LHSV is in a range of 0.2 to 20 h -1 , preferably 0.5 to 10 h "1 .
  • the apparatus according to the invention can be operated in a pressure range from 0.01 bar to 200 bar, preferably the apparatus according to the invention is operated in a pressure range from 0.1 bar to 100 bar. (The pressures given here are based on the absolute pressures prevailing in the interior of the reaction spaces.)
  • the apparatus can preferably be used for the investigation of reactions which are in a temperature range from 20 ° C to 1200 ° C, preferably from 50 ° C to 800 ° C, particularly preferred is a temperature range of 100 ° C to 650 ° C.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
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  • General Physics & Mathematics (AREA)
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  • Physical Or Chemical Processes And Apparatus (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

La présente invention concerne un appareil de catalyse pour tester des catalyseurs par réglage variable de la pression de traitement dans une plage de pressions de 0,01 Millibar à 300 bar. De préférence, le dispositif dispose d'une pluralité d'espaces réactionnels (101, 102,...) qui sont disposés parallèlement et dont les conduites (211, 212,...) côté sortie des espaces réactionnels sont subdivisées en deux groupes de conduites secondaires. Un groupe de conduites principales (411, 412,...) est en liaison fonctionnelle avec une soupape de réglage (61) commune à toutes les conduites principales et avec une conduite de sortie d'air (62), et le deuxième groupe de conduites secondaires (311, 312, 313,...) dotées de soupapes de commutation (321, 322,...) est en liaison fonctionnelle avec une unité d'analyse (34). De préférence, les conduites (201, 202,...) côté sortie des espaces réactionnels sont respectivement équipées d'une conduite distincte pour l'alimentation en fluide de réglage (211, 212,...). Dans un mode de réalisation préféré, les points de liaison des conduites (201, 202,...) côté sortie des espaces réactionnels vers les conduites principales (411, 412,...) concernées et les conduites secondaires (311, 312,...) présentent respectivement un récipient de mélange (301, 302,...).
EP11771033.5A 2010-10-22 2011-10-17 Dispositif et procédé pour analyser des catalyseurs par réglage variable de la pression de traitement Withdrawn EP2629886A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP11771033.5A EP2629886A2 (fr) 2010-10-22 2011-10-17 Dispositif et procédé pour analyser des catalyseurs par réglage variable de la pression de traitement

Applications Claiming Priority (3)

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EP10013897 2010-10-22
EP11771033.5A EP2629886A2 (fr) 2010-10-22 2011-10-17 Dispositif et procédé pour analyser des catalyseurs par réglage variable de la pression de traitement
PCT/EP2011/005208 WO2012052149A2 (fr) 2010-10-22 2011-10-17 Dispositif et procédé pour analyser des catalyseurs par réglage variable de la pression de traitement

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EP2629886A2 true EP2629886A2 (fr) 2013-08-28

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US (1) US9228985B2 (fr)
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NL2009659C2 (en) * 2012-10-18 2014-04-22 Avantium Technologies B V System and method for operating parallel reactors.
US20140335626A1 (en) * 2013-05-10 2014-11-13 Cdti Test Bench Gas Flow Control System and Method
DE102013016585A1 (de) * 2013-10-08 2015-04-09 Hte Gmbh The High Throughput Experimentation Company Apparatur und Verfahren zur Untersuchung von diskontinuierllichen Produktfluidströmen bei der Umsetzung von Eduktfluidströmen an Feststoffkatalysatoren
JP6141234B2 (ja) * 2014-03-26 2017-06-07 フロンティア・ラボ株式会社 気相成分分析装置
CN110944741A (zh) * 2017-07-28 2020-03-31 Hte高通量实验公司 在0.1-10秒的停留时间下催化转化化学物质的装置和方法
EP3856403A1 (fr) * 2018-09-24 2021-08-04 HTE GmbH The High Throughput Experimentation Company Dispositif et procédé d'analyse de réactions
EP4301505A1 (fr) * 2021-03-04 2024-01-10 HTE GmbH The High Throughput Experimentation Company Appareil d'analyse de systèmes de réaction

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US6063633A (en) * 1996-02-28 2000-05-16 The University Of Houston Catalyst testing process and apparatus
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WO2004009230A1 (fr) * 2002-07-22 2004-01-29 Avantium International B.V. Appareil d'echantillonnage
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US20130273662A1 (en) 2013-10-17
WO2012052149A3 (fr) 2012-06-21
WO2012052149A2 (fr) 2012-04-26
US9228985B2 (en) 2016-01-05

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