EP1483049A1 - Führungsstrukturreaktor - Google Patents
FührungsstrukturreaktorInfo
- Publication number
- EP1483049A1 EP1483049A1 EP03714779A EP03714779A EP1483049A1 EP 1483049 A1 EP1483049 A1 EP 1483049A1 EP 03714779 A EP03714779 A EP 03714779A EP 03714779 A EP03714779 A EP 03714779A EP 1483049 A1 EP1483049 A1 EP 1483049A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- liquid
- guide structures
- reactor
- reactor according
- guide
- 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- Withdrawn
Links
Classifications
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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
- B01J19/32—Packing elements in the form of grids or built-up elements for forming a unit or module inside the apparatus for mass or heat transfer
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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
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
- B01J10/02—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor of the thin-film type
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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
- 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
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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
- 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
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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
- 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
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00873—Heat exchange
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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
- 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
- B01J2219/00961—Temperature
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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
- 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
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
- B01J2219/322—Basic shape of the elements
- B01J2219/32279—Tubes or cylinders
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
- B01J2219/322—Basic shape of the elements
- B01J2219/32282—Rods or bars
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
- B01J2219/322—Basic shape of the elements
- B01J2219/32286—Grids or lattices
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
- B01J2219/324—Composition or microstructure of the elements
- B01J2219/32408—Metal
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
- B01J2219/324—Composition or microstructure of the elements
- B01J2219/32466—Composition or microstructure of the elements comprising catalytically active material
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
- B01J2219/324—Composition or microstructure of the elements
- B01J2219/32466—Composition or microstructure of the elements comprising catalytically active material
- B01J2219/32475—Composition or microstructure of the elements comprising catalytically active material involving heat exchange
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
- B01J2219/33—Details relating to the packing elements in general
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
- B01J2219/332—Details relating to the flow of the phases
- B01J2219/3322—Co-current flow
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- C—CHEMISTRY; METALLURGY
- C40—COMBINATORIAL TECHNOLOGY
- C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
- C40B30/00—Methods of screening libraries
- C40B30/08—Methods of screening libraries by measuring catalytic activity
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- C—CHEMISTRY; METALLURGY
- C40—COMBINATORIAL TECHNOLOGY
- C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
- C40B40/00—Libraries per se, e.g. arrays, mixtures
- C40B40/18—Libraries containing only inorganic compounds or inorganic materials
Definitions
- the invention relates to a reactor with guide structures for the generation and conduction of liquid films or liquid drops through a reaction zone in a reactor housing.
- the invention relates to a reactor for carrying out gas / liquid reactions, liquid / liquid reactions, solid / liquid reactions or only liquid reactions such as electrochemical reactions, catalytic solid phase reactions, etc.
- Known reactors for chemical liquid phase reactions guide liquid streams or liquid films along a flow path with at least one, often two or three flat wall contacts.
- the liquid is conducted over a smooth surface or more often in channels with a round or rectangular or groove-shaped cross section tapering towards the bottom of the channel or in a tube with a closed wall surface.
- Gas / liquid, liquid / liquid, solid / liquid or only liquid reactions are carried out in such reactors.
- reactions includes not only chemical reactions, but also the implementation of media exchange and concentration changes in solutions, and the mixing, heating, cooling and evaporation of liquids and solutions.
- a disadvantage of the known reactors is the relatively small reactive surface of the liquid film, which is available, for example, for contact with a reaction gas.
- the laminar flow in the wall regions of the conduction paths by braking the flow velocity means that different flow velocities prevail in the liquid within the liquid film, depending on whether a liquid region flows closer to a wall or further away near the liquid surface. Parts of a liquid volume introduced into the reactor at the same time therefore pass the same reaction path more slowly and with a longer residence time in the reactor than other liquid components. The greater the differences in flow velocities within the liquid film, the wider the residence time distribution.
- liquid flow paths with a high proportion of wall contact have the disadvantage that only a correspondingly small proportion of liquid on and near the liquid surface for reactions, e.g. B. with a gas is available. It comes with some reac- Although door designs are used to mix the liquid by swirling, and diffusion effects can also cause an exchange of surface liquid and deeper flowing components, these effects are often not sufficient for a uniform reaction. There are thus differences in the concentration of liquid components within the liquid film which have already been subjected to the intended reaction and those for which this is not the case. Concentration differences include differences with regard to chemically reacted liquid itself or substances dissolved in it, but also e.g. B. Understand temperature differences or gradients.
- a broad distribution of residence times and / or a broad distribution of concentrations have the disadvantage that undesired reaction by-products or product mixtures are formed in some reactions, which may require further purification, concentration or the like.
- a further disadvantage of the known reactors is that the shape and thickness of the liquid stream or film cannot be set at all, or only to a very limited extent, because of the fixed structures for guiding the liquid, and can thus be adapted to specific reaction conditions and requirements.
- the object of the present invention was therefore to provide liquid phase reactors which are improved compared to the prior art and which permit a narrower residence time distribution and / or concentration distribution, flexibly and uniformly adjustable liquid films or liquid drops and a high mass and / or temperature transfer.
- Reactor housing in the sense of this invention is to be understood as a closed housing, an open housing or else a simple frame or a suspension for the guide structures.
- the spacing of adjacent guide structures in the reactor according to the invention is advantageously selected such that the liquid between the adjacent guide structures can form a coherent liquid film or, alternatively, individual drops.
- the liquid films and drops formed in the reactor according to the invention can be adjusted uniformly and with flexible parameters. This enables, for example, precisely defined chemical reactions to be carried out with one or more gas components flowing in on all sides with very little effort. Thanks to the new liquid flow, a narrow distribution of the residence time can be achieved and a high mass and / or heat transfer can be guaranteed.
- the leadership or Line structures of the reactor according to the invention allow a functional and universal use for a mass transfer between two or more media and / or for carrying out chemical reactions of these media with one another.
- the reactor can also be used to determine kinetics and / or residence times for these media in the liquid and / or gaseous state.
- the reactor according to the invention differs from known reactors, for example also known falling film reactors, in that the liquid film does not flow in channels with large wall contact, but the liquid component is clamped and guided between at least two guide structures, such as wires, due to the capillary forces.
- the liquid film moves e.g. B. with the help of gravity along these guide structures.
- the liquid can also roll or be guided on the guide structures as drops with only very little surface contact. Drops can be with two or more management structures, but also with only a single management structure, e.g. B. a single wire.
- Another advantage of the reactor according to the invention over known arrangements is that it is relatively easy and quick to clean and maintain, which saves time and money.
- At least two adjacent guide structures formed as wires, rods, extruded profiles, strips, strips or hollow profiles are arranged essentially parallel and at a distance from one another.
- the liquid film or the drop is guided essentially uniformly over the entire reaction path. It is particularly useful for one parallel arrangement of the guide structures when the guide structures are biased in the reactor housing.
- At least two adjacent guide structures are arranged in the longitudinal direction from the liquid supply towards the liquid outlet with increasing or decreasing distance from one another. This enables the guiding properties to be changed over the length of the reaction path, i. H. For example, a change in the shape and / or thickness of the liquid film and, as a result, a change in the flow properties, the residence time distribution, the concentration distribution and / or the liquid surface available for reactions.
- the reactor according to the invention offers the advantage of easily increasing or also reducing the reaction area of liquid surfaces in reactors, if this is necessary.
- a defined, uniformly thin falling film of up to micrometer thickness is produced in a stable, almost free space.
- the only wall contacts on the guide structures are extremely small or minimized compared to known reactors.
- by manually or motor-driven adjustment of the spacing of the guide structures to one another it is possible to vary the thickness and / or shape of the liquid films. The same applies to droplet formation and droplet guidance.
- Liquids can be guided or rolled off in droplet or droplet form with the aid of the guide structures in order to bring these droplets of the liquids into contact and react with gaseous media.
- the gaseous media can only be used as a protective atmosphere.
- An essential part of the reactor according to the invention are the guide structures designed as wires, rods, strips, strips or extruded profiles.
- the shapes of the guide structures, their size or external dimensions and the material used for these guide structures depend on the application and use of the reactor according to the invention, in particular on the chemical and physical properties of the liquids and gases used and the reaction conditions, such as temperature, pressure etc.
- the guide structures can have different shapes in cross section perpendicular to the longitudinal axis. Circular wires are particularly preferred in cross section.
- the guide structures in cross section perpendicular to the longitudinal axis can also have an elliptical shape, a square shape, a rectangular shape, an isosceles or isosceles triangular shape, a pentagonal, a hexagonal, a diamond shape, a uniform rhombus shape with rounded corners and a concave arch Side faces, a cross shape, a cross shape with rounded corners or a star shape with radially extending outward from a common center
- the webs can be straight, curved or kinked.
- the guide structures consist of wires, rods, strips, strips or extruded profiles with surfaces modified areas.
- One or more webs with surface areas that have better wettability for the liquid to be used than the surface areas lying next to these webs extend over the length of a guide structure.
- Several webs of areas with good or “better” wettability on a guide structure are separated from one another by “poorly” wettable surface areas.
- the tracks on the guide structures can be straight or zigzag-shaped, curved or in any other non-linear manner on the surface. If several tracks are provided on a guide structure, these preferably run essentially parallel to one another.
- Methods for modifying the wettability of surfaces for certain liquids are known to the person skilled in the art and are not the subject of the invention.
- methods for modifying the surface wettability are chemical and physical surface treatment, such as treating the surface with acids or bases, roughening or smoothing the surface, coating the surface, e.g. B. by means of PVD or CVD, or application of an organic polymer.
- the liquid films span between adjacent guide structures with surface-modified areas of the type mentioned above between the more wettable areas or webs on the guide structures. The poorly wettable areas remain essentially free of liquid. If several better wettable webs are provided on the guide structures, this allows several liquid films to be guided next to one another between adjacent guide structures.
- drops where several drops can also be guided or run along a single guide structure.
- other liquids can also be guided along the regions which are less wettable with respect to the liquid film.
- areas with better wettability for apolar liquids can be arranged next to one another with areas with better wettability for polar liquids. This allows the management of appropriate liquids such.
- the diameter ser using the example of wires with a circular cross section as guide structures in the range from about 100 nm to about 1 mm.
- the diameters of the guide structures are in the range from approximately 0.5 mm to approximately 5 mm.
- the guide structures can be made of all materials as are also used for the known reactors according to the prior art.
- the surface condition of the guide structures is of crucial importance for special applications. In order to be able to produce a falling film with a specific liquid, according to the invention, depending on the liquid, a precisely determinable surface roughness of the guide structures is necessary. If the surface of the guide structure is smooth, that is to say with very little roughness, the liquid or drops easily roll off or slide away or slide off on one, two or more guide structures.
- the guide structures expediently run in a straight line in the longitudinal direction from the liquid feed in the direction of the liquid outlet.
- Alternative embodiments with non-rectilinear guide structures are also suitable for certain applications, e.g. B. to increase the length of the liquid path in the reactor.
- the guide structures preferably run in a zigzag shape, curved or helical.
- the guide structures in the reactor are designed as hollow profiles. Since the guide structures are arranged in the immediate reaction space, multiple use of these guide structures is possible.
- the cavities in the guide structures can be used, for example, for cooling or heating or for the removal or supply of energy. It is therefore expedient for supply lines and discharge lines for the passage of a cooling or heating fluid through the guide structures on these guide structures designed as hollow profiles.
- Such temperature control can be carried out in all usable temperature ranges. However, it is particularly effective at higher temperatures above 100 ° C, because the temperature setting or control takes place directly in the reaction space and not indirectly outside the reactor space.
- the guide structures are designed to be electrically conductive and connections are provided for connecting the guide structures to a power source.
- two adjacent guide structures each have opposite polarity for the passage of an electrical current through a liquid film formed between the guide structures.
- the guide structures can also be designed as a pole and part of the reactor housing as a counter pole. If a current flows in the liquid phase, whether as a film or drops, electrochemical reactions such as electrochemical gas / liquid reactions are possible.
- the reactor housing of the reactor according to the invention can be an open or a closed housing.
- the reactor housing is preferably designed as a closed housing which has feed lines and discharge lines for the liquid to be conducted along the guide structures. If reactions of the liquid with one or more other media (gases or liquids) are to be carried out, the reactor housing expediently has further supply lines and discharge lines for the passage of gas and liquid through the reactor housing.
- These last-mentioned supply lines and discharge lines are advantageously arranged on the reactor housing in such a way that a gas or a liquid passed through the reactor housing is essentially perpendicular to the longitudinal direction of the guide structures, ie. H. the main direction of flow of the liquid carried thereon flows.
- the supply of further media can also advantageously take place parallel to the supply of the liquid guided on the guide structures, so that these media flow together with the liquid.
- the liquid which is to flow along the guide structures is distributed uniformly to the beginning of the reaction zone inside the reactor, where it meets defined or adjustable gaps between at least two guide structures. If the arrangement of the guide structures is correctly selected in accordance with the liquid used, the shape and surface of the guide structures, the introduced liquid forms around the guide structures, e.g. B. wires, by capillary forces a liquid film, spans between the guide structures and moves under gravity or by means of other driving forces, such as. B. particularly preferred by electroosmotic flow or capillary forces, along the guide structures. It is clear that for effective throughput it is advantageous to provide several guide structures for a plurality of spanned liquid films or drops in parallel or in another arrangement in the reactor housing.
- the liquid component which is guided along the guide structures from the liquid supply towards a liquid outlet, is preferably driven by means of gravity. It is particularly expedient for the liquid to be driven by gravity. ßig when the guide structures in the reactor housing from the liquid supply in
- the guide structures are arranged essentially vertically. This ensures that gravity is fully effective as the driving force for the liquid.
- a tilting close to a horizontal alignment of the guide structures is recommended according to the invention. With a horizontal orientation, the liquid must be driven by a pressure difference, a gas flow or a driving force other than gravity.
- volume effects such as gravity, take a back seat to surface effects, even when the guide structures are arranged vertically or only slightly.
- driving forces which are based on surface effects such as electroosmotic flow.
- driving forces for the liquid flow are capillary forces, pressure difference, temperature difference, gas flow etc. and are described in more detail below.
- the liquid streams or drops in the reactor can be driven along the guide structures by a gas stream introduced into the reactor housing, e.g. B. by droplets are transported by the shear forces exerted by gas. This would have the advantage of high mass and heat transfer coefficients from the gas to the liquid phase.
- the liquid can be driven by providing a temperature gradient along the guide structures. It is possible to control the transport of liquid films or drops by the temperature dependence of the surface tension.
- the contact angle of drops to the surface of a wire or other guide structure depends on the local temperature and the surface roughness, so that a drop is driven from the poorer to the more wettable area.
- Temperature gradients can cause Marangoni convection in a liquid film.
- the surface tension forces depend essentially on the temperature, so that liquid is transported to the areas with lower surface tension.
- a further drive option for the liquid which is suitable according to the invention consists in pulling or transporting charged or electrically polarized droplets along the guide structures through an electric field in the reactor housing.
- a further drive option suitable according to the invention for a liquid film or a drop is the electroosmotic flow (EOF), by means of which it is possible to transport the liquid along the wires.
- EEF electroosmotic flow
- the liquid contains ions that attach to the surface of the management structures.
- the liquid film contains a charge and can be transported by an electrical potential difference. It was found that in this case the flow profile in the liquid film was a plug-flow
- the materials suitable for the manufacture of the reactor depend on the use or the type of operation.
- Preferred materials for the reactor housing and components that come into contact with liquid or gas are stainless steel and particularly preferably higher-grade steel grades that meet a wide range of possible operating conditions, such as temperatures from -200 ° C. to 800 ° C. or negative pressures of up to 10 5 Pa or pressures of up to 10 7 Pa or more.
- Stainless steel and high-quality steel grades are also suitable for a large number of liquids or gases.
- plexiglass or other transparent materials for the reactor housing and other components are suitable if the temperatures achieved and the other conditions make use of such materials allow.
- a further advantageous application of the reactor according to the invention is screening technologies, such as finding catalysts for chemical reactions.
- the guide structures or wires are therefore designed as solid catalysts.
- the guide structures either consist entirely of catalyst material or are at least coated on their surface with catalyst material.
- Another advantage is that the management structures can be exchanged quickly and easily, so that different catalysts can be tested. Alternatively, different management structures can be placed in the same reactor. have different catalyst materials, so that parallel studies on different
- the reactor according to the invention allows reaction conditions to be determined or simulated experimentally in a flexible manner. For example, the residence time required for a particular reaction and the concentrations of reactants can be exactly determined before a reaction is carried out on a synthetic scale. This offers the possibility of reducing or avoiding the formation of undesired by-products.
- a large number of different gas / liquid, liquid / liquid, solid / liquid or only liquid reactions can be carried out in the reactor according to the invention.
- gas / liquid reactions are the fluorination of toluene with fluorine gas or the sulfonation of aromatics with sulfur trioxide.
- liquid / liquid reactions are esterifications with two phases, e.g. B. according to the Schotten-Baumann method.
- Examples of rapid liquid reactions are nucleophilic substitutions, electrophilic substitutions, such as nitration of aromatics, esterifications, amidations, etc.
- Photochemical reactions can also be carried out with particular advantage in the reactor according to the invention. The special liquid flow ensures almost 100% availability of the liquid.
- photochemical reactions are cycloadditions, radical formation and conversion or decomposition reactions. All reactions listed here and the possible uses described below can be implemented or carried out on an equal footing with the reactor according to the invention.
- the use of the reactor for gas / liquid reactions described in detail herein by way of example also applies to all other of the reaction types described above.
- the gas component described can be replaced by one or, in special applications, by several immiscible liquid phases or liquids.
- FIGS 1a, 1b show schematic perspective views of various embodiments of the reactor according to the invention.
- FIGS. 2a, 2b show schematic views of alternative embodiments of holding devices for guide structures in the reactor from above.
- FIG. 2 c shows a schematic view of a further alternative embodiment of a holding device for the guide structures in the reactor from the front.
- FIG. 3 shows a schematic partial view of two guide structures according to the invention with a liquid film stretched between them.
- FIGS. 4a to f show top views of the guide structures from FIG. 3 with different forms of the liquid film or drop that can be produced.
- Figures 5a to m show cross-sectional views of various guide structures according to the invention from above.
- FIG. 6 shows various views of guide structures designed as a hollow profile.
- FIGS. 7a to d show various alternative forms of the guide structures over their length.
- FIGS 8a, 8b show alternative arrangements of the guide structures according to the invention.
- FIGS. 9a, 9b show further alternative arrangements of the guide structures according to the invention.
- Figure 10 shows a schematic representation of the inclination adjustment of the reactor.
- FIGS 11a, 11b show applications for the reactor according to the invention.
- FIG. 12 shows an example of a further alternative application for the reactor according to the invention.
- FIG. 13 shows various embodiments of guide structures according to the invention with surface-modified areas.
- FIG. 1a shows a schematic perspective view of an embodiment of the guide structure reactor 1 according to the invention with a reactor housing which comprises a liquid inlet unit 2, reactor side walls 2 'and a liquid outlet unit 2 ".
- the reactor 1 is shown open in FIG. 1a with a view into the reactor space 7.
- the liquid inlet unit 2 of the reactor housing has a liquid inlet opening 4 for the introduction of liquid 3 into the housing.
- guide structure holding parts 12 are arranged in the reactor housing, to which the guide structures 6 designed as wires in the embodiment according to FIG. 1 are fastened.
- the guide structures 6 extend in the reaction space 7 from the liquid inlet in the direction of the liquid outlet and can also be fastened to corresponding holding parts or to the liquid outlet unit at the liquid outlet.
- the guide structure holding parts 12 have distributor openings 5, through which the introduced liquid 3 is fed to the guide structures 6.
- the guide structures 6 are arranged essentially parallel and at equal distances from one another.
- the distributor openings 5 are each arranged essentially centrally over the distance between two guide structures.
- Liquid 3, which is introduced into the reactor housing through the liquid inlet opening 4 first distributes itself over the plate-shaped guide structure holding part 12 and then flows through the distributor openings 5 in the guide structure holding part 12 to the guide structures 6. Due to the vertical arrangement of the reactor 1 and the feed of the Liquid 3 from above, the liquid in the embodiment according to FIG. 1a is driven essentially by gravity.
- the liquid After the liquid 3 has emerged from the distributor openings 5, the liquid is first guided on the underside of the guide structure holding part 12 due to the adhesive forces and then to the respectively adjacent guide structures below a distributor opening 5. Due to the adhesive forces and the surface tension of the liquid, a liquid film 3a spans on the liquid structures 6 and flows down through the reaction space 7 in the direction of the liquid outlet unit 2 ′′ driven by gravity.
- the reactor housing of the embodiment according to FIG. 1 has two reaction gas inlet openings 10, 10 'and two reaction gas outlet openings 11, 11' on the side walls.
- a reaction gas 9 is introduced through the reaction gas inlet opening 10 into the reactor housing into the reaction space 7 and is discharged through the reaction gas outlet opening 11 ′ which is arranged vertically lower.
- the openings 10 'and 11 are closed, but the gas inlet and the gas outlet can also take place at any combination of the openings 10, 10', 11 and 11 '.
- different gases can also be introduced through the reaction gas inlet openings 10 or 10 'simultaneously or in succession and discharged through the reaction gas outlet openings 11 or 11'.
- the liquid outlet unit 2 " is located at the lower end of the reactor housing.
- FIG. 1a shows two different variants thereof.
- the liquid outlet unit 2" shown in the left half of the figure is ver inside the reactor with inner surfaces converging obliquely in the direction of a single centrally arranged liquid outlet opening 4 ' - see.
- the liquid outlet unit 2 "(alternative embodiment) shown in the right half of the figure has a plurality of liquid outlet openings 4" immediately below the individual guide structures 6.
- the liquid at the liquid outlet unit 2 "is, depending on the embodiment, through the liquid outlet opening / s 4 'or 4" dissipated.
- Figure 1b shows an alternative embodiment to Figure 1a, in which the guide structures 6 all have the same length and are attached to a lower guide structure holding part 12 '.
- the lower guide structure holding part 12 ′ is provided with holes for the drainage of the liquid in accordance with the upper guide structure holding part 12.
- the lower guide structure holding part 12 ′ can be displaceable in the vertical direction for prestressing the guide structures 6.
- the liquid outlet unit 2 "at the lower end of the reactor housing is shown in two different design variants. Both design variants are provided in the interior of the reactor with inner surfaces converging obliquely in the direction of a single centrally arranged liquid outlet opening 4 '.
- the design variant shown in the left half of the figure shows a steeper slope towards the liquid outlet opening 4 'than the liquid outlet unit 2 "shown in the right half of the figure (alternative embodiment).
- FIGS. 2a and 2b show two different embodiments of guide structure holding parts 12a and 12b, each with guide structures 6 fastened thereon, wherein the guide structure holding parts 12b are each arranged to be movable in the direction of the arrows shown in the figures.
- the guide structure holding part 12b from FIG. 2a can be moved perpendicularly to or away from the guide structure holding part 12a, as a result of which the distance between the guide structures 6 lying opposite one another can be variably adjusted.
- Adjustment mechanisms 13 are provided thereon for the mobility of the guide structure holding parts 12b.
- the guide structure holding part 12b is designed to be displaceable parallel to the guide structure holding part 12a.
- an appropriate adjustment mechanism the construction of which lies within the range of the skilled person's skill in the art, both directions of movement can also be realized simultaneously (not shown).
- FIG. 2c shows from the front two guide structures 6 with liquid film 3a flowing in between, the guide structures 6 being fastened to guide structure holding parts 12a, 12b, 12c and 12d.
- the guide structure holding parts 12b and 12d can be displaced in the horizontal direction in FIG. 2c relative to the guide structure holding parts 12a and 12c, which is represented by corresponding double arrows which represent adjustment mechanisms 13.
- the guide structure holding parts 12c and 12d can be displaced in the vertical direction Y, as a result of which the prestressing of the guide structures 6 can be changed.
- FIG. 3 is a schematic partial view of two guide structures 6 with liquid 3 flowing along them, which adheres to the guide structures 6 due to adhesive forces and between which they stretch a liquid film 3a.
- the length L of the guide structures 6 can be selected variably, and the distance X between these guide structures is freely adjustable.
- FIG. 3 illustrates how a reaction gas 9 can flow on all sides of the liquid 3 flowing along the guide structures 6 and the liquid film 3a stretched between them.
- FIG. 4 shows a top view of two guide structures 6, as shown in FIG. 3.
- FIGS. 4a to f illustrate various possible forms which the liquid can take as liquid film 3a (FIGS. 4a to d) or as drops (FIGS. 4e and f).
- the shape of the liquid film 3a or the formation of drops are significantly influenced by the distance between the guide structures 6 and the properties of the liquid itself, such as viscosity, density, capillary forces and surface tension. Furthermore, the material of the guide structures and its surface roughness influences the formation of the liquid film or the drops.
- Figure 4a shows a concave shape of the liquid film 3a.
- Figure 4b shows a curved shape of the liquid film 3a, which can be transported both hanging and lying on.
- FIG. 1 shows a concave shape of the liquid film 3a.
- FIG. 4c shows a liquid film with essentially parallel liquid surfaces lying opposite one another.
- Figure 4d shows an oval shape of the liquid film 3a.
- FIG. 4e shows the droplet guidance between two guiding structures, wherein the droplets can be transported lying on the guiding structures or hanging on them.
- FIG. 4f shows the droplet guidance on only one guidance structure.
- FIG. 5a to m show various guide structures suitable according to the invention in cross section from above.
- the shape which is particularly preferred according to the invention is the circular cross section (FIG. 5a).
- Other suitable shapes are a square cross-sectional profile (Figure 5b), a hexagonal cross-sectional profile (Figure 5c), a rectangular cross-sectional profile (Figure 5e), a Diamond shape (Figure 5f), an elliptical or oval shape (Figure 5g) or a triangular shape ( Figure
- a round shape with a web (FIG. 5d) can be suitable for two adjacent guide structures in order to be able to set the liquid film very thinly down to a few micrometers in thickness.
- the inflow surface for the gas on the liquid film can be set approximately horizontally on both sides. In the embodiment according to FIG. 5i, three are evenly distributed
- Bridges are staggered around a common center by 120 °.
- the webs are bent again in the middle.
- FIG. 51 shows a cross-sectional shape of a uniform rhombus with round corners and inwardly curved side faces.
- FIG. 5 m shows a cross-sectional profile with a cross shape with rounded corners.
- FIG. 6 shows an alternative embodiment of the guide structures 6 according to the invention, which here is designed as a hollow profile and is shown on the left side in FIG. 6 in cross section from above and on the right side schematically in cross section from the side.
- a flowing down liquid film 3a is shown between the guide structures 6 designed as hollow profiles.
- a liquid or gaseous heating or cooling medium 14 can flow through the cavity therein.
- sensors 15, such as pressure sensors or temperature sensors, can be accommodated in the cavity of some of the guide structures 6.
- FIGS. 7a to d show alternative arrangements of the guide structures for a parallel guide (FIG. 7a), a zigzag guide (FIG. 7b), a curved guide (FIG. 7c) and a helical guide (FIG. 7d) of the liquid film.
- the guide paths according to FIGS. 7b to d permit an extension of the residence time of the liquid in the reactor by lengthening the distance.
- FIGS. 8a and b show alternative arrangements of the guide structures 6 in a triangular arrangement (FIG. 8a) and a quadrangular arrangement (FIG. 8b).
- the distances between the adjacent guide structures 6, each forming a triangle or a quadrilateral, are essentially the same, so that liquid films 3 a span between all adjacent guide structures at equal distances and thereby form a channel surrounded by liquid.
- a gas 9 flows around the liquid films from the outside, a gas 9a also being able to flow in the channel formed by liquid.
- the gases 9 and 9a can be the same or different.
- FIGS. 9a and 9b show further alternative arrangements of guide structures 6 in a reactor housing.
- a plurality of guide structures are arranged in two concentric circles or polygons, adjacent guide structures 6 of a circle being arranged in a have substantially the same distances and each stretch liquid films between two adjacent guide structures.
- Reaction gas 9 and 9a flow around the liquid films, gas 9a flowing in the space between the two concentric circles being the same or a different gas than gas 9.
- FIG. 9b shows an alternative embodiment, the guide structure holding parts 12 also being shown are shown.
- FIG. 10 is a schematic illustration of the stepless inclination adjustment of the reactor 1 according to the invention about an axis of rotation 16, the reactor 1 being arranged vertically on the left side in FIG. 10 and horizontally on the right side in FIG. Any angle of inclination between 0 ° and 90 ° to the horizontal can be set. In this way, the liquid flow in the reactor, in particular the influence of gravity on the drive of the liquid, can be varied.
- FIG. 11a schematically shows the arrangement of a plurality of reactors 1 according to the invention, two reactors 1 arranged in parallel, followed by a mixing unit 17 and a further reactor 1 adjoining them being shown.
- These reactors 1 can be operated identically or independently of one another with the same or different drive options for the liquids or media supplied.
- FIG. 11 b shows two reactors 1 according to the invention arranged in a row, the inclination of which can be individually adjusted via axes of rotation 16.
- FIG. 12 shows an overall arrangement in which one or more, identical or different liquid media L1, L2 are transported via pressure monitors 18 to a mixing unit 17 and are subsequently introduced into the reactor according to the invention.
- Reaction gases or reaction liquids can be supplied to or removed from the reactor via the inlet and outlet openings g1 to g6. After the converted liquid has escaped, it is fed to a residence zone 19 and then to a gas chromatograph 21 via valves 20.
- a downstream pressure switch 18 can take over a control function in order to control the liquid feeds to downstream arrangements, if necessary.
- FIG. 13 shows various embodiments of guide structures 6 according to the invention with areas of different wettability 22, 23 for the liquid used.
- the areas of better wettability 22 extend in webs over the entire length of the guide structures 6. In between, areas of poorer wettability run.
- FIG. 13a shows a guide structure 6 with only one web of better wettability 22 from the front and from above.
- FIG. 13 shows a guide structure 6 with a plurality of tracks of better wettability 22 arranged in parallel from the front and from above. Between adjacent management structures 6 stretch liquid films 3a between the more wettable areas 22. The poorly wettable areas 23 remain essentially free of liquid.
- FIG. 13 shows various embodiments of guide structures 6 according to the invention with areas of different wettability 22, 23 for the liquid used.
- the areas of better wettability 22 extend in webs over the entire length of the guide structures 6. In between, areas of poorer wettability run.
- FIG. 13a shows a guide structure 6 with only one web of better wettability 22 from the front and from
- FIG. 13b also allows a gas or another liquid to be passed through the channels formed by two liquid films and the adjacent guide structures.
- the guide structures according to FIGS. 13a and 13b can also be provided on their rear sides with corresponding tracks 22 and 23, so that a plurality of guide structures can be arranged one behind the other with liquid films stretching between them.
- the guide structures are additionally provided with webs of better and poorer wettability on adjacent side surfaces. This allows the arrangement of four guide structures, liquid films stretching between two adjacent guide structures to form a larger channel. A reaction gas or a liquid can be passed through this channel.
- Liquid inlet unit 'reactor side walls' Liquid outlet unit
- Reaction gas 0, 10 'Reaction gas inlet openings 1, 11' Reaction gas outlet openings 2, 12 'Guide structure holding part 3 Adjustment mechanism 4 Heating or cooling medium 5 Sensors 7 Mixing unit 8 Pressure switch 9 Dwell section 0 Valve 1 Gas chromatograph 2 surface-modified areas with better wettability 3 Surface-modified areas with poorer wettability
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- Chemical & Material Sciences (AREA)
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Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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DE10210097 | 2002-03-08 | ||
DE2002110097 DE10210097B4 (de) | 2002-03-08 | 2002-03-08 | Führungsstrukturreaktor |
PCT/EP2003/002266 WO2003076065A1 (de) | 2002-03-08 | 2003-03-06 | Führungsstrukturreaktor |
Publications (1)
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EP1483049A1 true EP1483049A1 (de) | 2004-12-08 |
Family
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Application Number | Title | Priority Date | Filing Date |
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EP03714779A Withdrawn EP1483049A1 (de) | 2002-03-08 | 2003-03-06 | Führungsstrukturreaktor |
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EP (1) | EP1483049A1 (de) |
DE (1) | DE10210097B4 (de) |
WO (1) | WO2003076065A1 (de) |
Families Citing this family (3)
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DE10248599A1 (de) | 2002-10-17 | 2004-04-29 | Degussa Ag | Verfahren zur Gewinnung einer gasförmigen Phase aus einem flüssigen Medium und Vorrichtung zu seiner Durchführung |
EP2206551B1 (de) * | 2008-12-23 | 2019-08-07 | Corning Incorporated | Mikrokanalreaktoren |
DE102010041289B4 (de) * | 2009-09-23 | 2017-09-07 | L-Dcs Technology Gmbh | Stoff- und Wärmeaustauscherplatte sowie ein Stoff- und Wärmeaustauschreaktor mit einer solchen Stoff- und Wärmeaustauscherplatte |
Family Cites Families (12)
Publication number | Priority date | Publication date | Assignee | Title |
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DE1990947U (de) * | 1968-08-08 | Carl Georg Mun ters Stocksund (Schweden) | Rieselkorpereinsatz fur Kuhltur me u dgl | |
GB171507A (en) * | 1920-08-25 | 1921-11-24 | Jean Henri Bregeat | Improvements in means for effecting an intimate intermingling of fluid streams |
FR1073449A (fr) * | 1952-12-20 | 1954-09-24 | Lorraine Carbone | Perfectionnements aux éléments de garnissage d'appareils industriels |
DE1102701B (de) * | 1957-03-18 | 1961-03-23 | Julius Montz Fa | Einbauten fuer Waerme- und Stoffaustausch-kolonnen |
US4224257A (en) * | 1979-04-19 | 1980-09-23 | Robinson Elbert W | Cooling tower construction and fill |
DE4128827A1 (de) * | 1991-08-30 | 1993-03-04 | Henkel Kgaa | Verfahren zum katalysierten alkoxylieren von fettderivaten |
DE4234093A1 (de) * | 1992-10-09 | 1994-04-14 | Siemens Ag | Bauelement zum Einbau in eine verfahrenstechnische Einrichtung |
NO951178L (no) * | 1995-03-28 | 1996-09-30 | Isc Intersulphoconsultant | Reaktordyser i en fallende film reaktor |
DE19945978A1 (de) * | 1999-09-24 | 2001-08-30 | Univ Stuttgart Lehrstuhl Und I | Fluidverteilungsrahmen für Mehrkammerstacks |
AU7274300A (en) * | 1999-10-18 | 2001-04-30 | Rolf P. C. Manteufel | Method and device for material and/or energy exchange in a wash column |
EP1163952A1 (de) * | 2000-06-14 | 2001-12-19 | Sulzer Chemtech AG | Mikrokanäle enthaltendes Festbett angeordnet in einem rohrförmigen Reaktorteil |
DE10036602A1 (de) * | 2000-07-27 | 2002-02-14 | Cpc Cellular Process Chemistry | Mikroreaktor für Reaktionen zwischen Gasen und Flüssigkeiten |
-
2002
- 2002-03-08 DE DE2002110097 patent/DE10210097B4/de not_active Expired - Fee Related
-
2003
- 2003-03-06 WO PCT/EP2003/002266 patent/WO2003076065A1/de active Application Filing
- 2003-03-06 EP EP03714779A patent/EP1483049A1/de not_active Withdrawn
Non-Patent Citations (1)
Title |
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See references of WO03076065A1 * |
Also Published As
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DE10210097B4 (de) | 2005-03-24 |
WO2003076065A1 (de) | 2003-09-18 |
DE10210097A1 (de) | 2003-10-09 |
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