WO2009080591A1

WO2009080591A1 - Micro-rectification column for the thermal separation of fluids

Info

Publication number: WO2009080591A1
Application number: PCT/EP2008/067556
Authority: WO
Inventors: Athanassios Ziogas; Hans-Joachim Kost; Bernd Werner
Original assignee: INSTITUT FüR MIKROTECHNIK MAINZ GMBH
Priority date: 2007-12-21
Filing date: 2008-12-15
Publication date: 2009-07-02
Also published as: DE102007062976A1

Abstract

In order to provide a rectification column which can be employed in e.g. a fine chemicals laboratory or in a scientific laboratory for a plurality of very different separation tasks in the preparative separation of small amounts of fluid mixtures, a micro-rectification column for the thermal separation of fluids is suggested according to the invention, said column having multiple column floors arranged in the micro-rectification column and dividing the column interior. The micro-rectification column is characterized in that the same has a column housing and at least one column insert, wherein the column floors are arranged on the column insert, and wherein the column insert is arranged in the column housing in a removable manner. Using the micro-rectification column as suggested according to the invention, better separation performance can be achieved for multiple different individual separation tasks than using a conventional rectification column.

Description

Micro-rectification column for the thermal separation of liquids

The present invention relates to a micro-rectification column for the thermal separation of liquids with a plurality of column trays arranged in the micro-rectification column and subdividing the column interior.

Distillation and rectification are processes for the distillative separation of liquid mixtures. Compared to simple distillation, the rectification is multi-stage and thus offers a significantly higher separation efficiency. The multi-step is effected in the rectification, characterized in that liquid phase and gaseous phase in the column are conducted under direct contact in countercurrent to each other. For this purpose, devices (packings, fillers, column trays) are provided in a rectification column, which allow the largest possible contact area between the liquid phase and the gaseous phase.

At the contact surface between the liquid phase and the gaseous phase in a certain region of a rectification column, a balance of the substances which are present in the liquid phase and the substances which are in the gaseous phase can theoretically occur at a given temperature and pressure and with sufficiently long contact present, adjust. This is actually only the case with the ideal column. Although the ideal state of equilibrium adjustment is usually not achieved in practice, in rectification by the countercurrent principle, the more volatile components of the liquid mixture accumulate in the direction of the top of the column and the less volatile in the direction of the bottom of the column. The separation efficiency of a column can then be calculated from the parameters of the actual separation and is expressed in terms of the calculated number of theoretical plates.

Rectification is an industrially widely used process for separating substances and is used, for example, in the burning of alcoholic beverages, in petroleum refining, in the industrial production of liquid chemicals and in the distillative separation of liquefied air into its constituents.

Rectification columns are columnar or tower-like devices or apparatuses made of, for example, glass, metallic materials or ceramics. In the area of the column bottom is usual example, an evaporator arranged and in the region of the column head is generally a capacitor. As a rule, there is an inlet in the lower region of the rectification column and an outlet at the top of the column or in the region of the condenser, wherein the inlet and outlet can be designed such that a continuous or discontinuous operation of the column can take place.

The present invention relates to a tray column. In a tray column, the devices which are provided to allow the largest possible contact area between the liquid phase and the gaseous phase, column trays. Column trays are usually horizontal, plate-shaped internals, which are installed at certain intervals in the cylindrical column. The trays of tray columns may be screen or grid shaped or have other means by which the gaseous phase can penetrate the soil, e.g. Holes, slots, bell-shaped passages or valves. During rectification, the liquid phase flows on one side of the column onto the bottom of the column and from there across the bottom and on the other side via a weir to the soil below. The liquid layer, which is located on the bottom of the column, in this case comes into contact with the gaseous phase. If openings are provided in the column bottom through which the gaseous phase can pass, a so-called bubble layer is formed. In bubble-cap trays, a portion of the gaseous phase passing through the apertures provided in the bottom may condense on the bells located above the apertures, the condensate passing from there to the bubble-cap where it accumulates.

The construction of a column tray greatly affects the separation properties of a rectification column for a particular separation task. Only the different flow properties of the mixture to be separated and its components make it necessary to determine the appropriate column bottom construction and the optimal properties of the column bottoms, such as material, surface properties, size of the pores, openings or slots for a particular separation task. In the preparation of a column, these properties are usually predetermined in advance, whereby a column is obtained which is optimized for a particular separation task, however, which need not necessarily be suitable for another separation task. Accordingly, it may be necessary for different separation tasks, several different rectification columns, which is associated with correspondingly higher acquisition costs. Especially in areas where you are confronted with very different separation tasks, such as the production of small quantities of If chemicals were used in scientific laboratories or in the production of fine chemicals, this poses a problem.

It is therefore an object of the present invention to provide a rectification column which can be used for a variety of very different separation tasks in the preparative separation of small amounts of liquid mixtures, such as. can be used in a fine chemical laboratory or in a scientific laboratory. It is also desired that this rectification column offers better separation performance than a conventional rectification column in view of the respective separation tasks.

This object is achieved by a micro-rectification column of the type mentioned, which is characterized in that the micro-rectification column comprises a column housing and at least one column insert, the column trays are arranged on the column insert, and wherein the column insert is removably disposed in the column housing.

Characterized in that according to the present invention, the column trays are not arranged directly on the column housing, but on a column insert, which in turn is removably arranged in the column housing, depending on the separation task different column trays for subdividing the interior of the column into the column housing in the inventive micro-rectification onskolonne be introduced. It is particularly advantageous that the fact that the column trays are arranged on the respective column insert, all columns bottoms can be removed simultaneously from the column housing, and it can then another column insert introduced with other column trays or with a different number and arrangement of column trays in the column housing become. In addition, changes can be made to the column bottoms arranged in the withdrawn column insert, or the column trays arranged in the withdrawn column insert can be exchanged for other column trays, or the number and arrangement of column trays can be changed. The micro-rectification column according to the invention can thereby be used for a large number of very different separation tasks and can be optimized by selecting the column bottoms used and the selection of column tray number and arrangement with respect to the respective separation task in order to achieve the best possible separation performance for this separation task.

The column trays are preferably selected from bubble-cap trays, valve trays, sieve trays or grid trays. Preferably, at least 3 and up to 30 co-solvents are used in the column feed. - A -

arranged. Even more preferably at least 5 and up to 20 column bottoms are arranged in the column insert. In one embodiment of the invention, all column trays have the same construction. In an alternative embodiment of the invention, the column trays are constructed differently, so that in a column insert, for example, bubble trays with sieve trays, bubble trays with valve trays or valve trays are combined with grid trays, etc.

The micro-rectification column according to the invention is due to the ability to quickly and easily vary the type, number and arrangement of the column trays of particular advantage in the preparative separation of small amounts of different liquid mixtures in a fine chemical laboratory. Also in the fractionation of available only in very small amounts mixtures, such. Mixtures of certain essential oils, the micro-rectification column according to the invention can be adapted in an advantageous manner by selecting the type, number and arrangement of the tray quickly and easily to the respective separation task. In addition, the micro-rectification column according to the invention is extremely useful in a development or research laboratory in which distillative separation systems suitable for certain separation tasks are sought or in which the parameters of the rectification and their interaction are investigated in principle.

The micro-rectification column according to the invention is especially designed for use in technical or scientific laboratories. The size of the column is therefore adapted to the laboratory scale. Thus, the interior of the column housing preferably has an overall height in the range of 5 cm to 100 cm, preferably an overall height in the range of 10 cm to 50 cm and particularly preferably an overall height in the range of 10 cm to 30 cm. The number of column trays, based on the height of the column interior, is preferably from 1 column tray per 0.5 cm to 1 column tray per 3 cm, preferably from 1 column tray per 1 cm to 1 column tray per 2 cm.

In one embodiment of the micro-rectification column according to the invention, the column housing consists of a component into which the column insert can be inserted in a gas-tight and liquid-tight manner, whereby the column housing in conjunction with the column insert forms a closed column interior subdivided by the column trays.

In another embodiment of the micro-rectification column according to the invention, the column housing consists of at least two column housing parts, wherein the column housing parts are releasably gas- and liquid-tight interconnected so that thereby form the column housing parts optionally in conjunction with the column insert the column interior. The advantage of this embodiment is that in the case of a or multi-part column housing, the column housing parts can be very firmly interconnected by connecting means to ensure that a gas and liquid-tight sealed column interior is formed. Suitable connecting means for these purposes may be, for example, screws, clips or clamps, by means of which the column housing parts can be pressed against one another in such a way that the column housing parts form a gas-tight and liquid-tight sealed column interior.

The phrase "gas and liquid tightly sealed" is understood here to mean that no gases or liquids can escape uncontrolled from the column interior closed in this way and also that no gases or liquids can penetrate uncontrollably from the outside into the column interior sealed off in this manner. Especially the sealing of a built from a column housing and a removable column insert or even from a multi-part column housing and a column insert micro-rectification column is a major challenge, since the column in a wide temperature range, which can range for example from room temperature to about 400 ⁰ C, In addition, the separation mixtures often comprise organic solvents which attack many common sealing materials, and certain distillative separations are carried out under reduced pressure in the column interior In the course of rectification, a large overpressure occurs in the column interior. The cavities of the Kolonneninnen- Mikrorektifikationskolonne according to the invention is, therefore, preferably also in co lonneninnenraumtemperaturen of up to 250 ⁰ C, more preferably even at Kolonneninnen- room temperatures of up to 400 ° C gas and liquid tight lockable. Preferably, the column interior is also closed at a positive pressure in the column interior of up to 3 bar, preferably up to 5 bar, gas and liquid tight. Particularly preferably, the column interior is also closed under vacuum, ie, up to a reduced pressure of up to 50 mbar, preferably of up to 10 mbar, in the column interior, sealed in a gas-tight and liquid-tight manner.

In order for the micro-rectification column according to the invention to be gas-tight and liquid-tight, it is preferable to use seals or pads made of plastic, such as perfluorinated rubber, perfluorinated elastomer, fluoroelastomer, polytetrafluoroethylene or ethylene, of aluminum or of graphite, in order to seal the region between column insert and column housing in order to seal off the column housing parts from one another in the case of multipart column housings and, if appropriate, also to seal off the area between column bottoms and column insert or column housing or to compensate for slight unevenness at the contact surfaces between the respective components. Seals or bearings made of graphite have the advantage that they are cheap and are resistant to temperatures above 450 ⁰ C.

The seals or pads can be placed in the respective sealed areas just before assembling the individual components. In a preferred embodiment, grooves or depressions are provided partly at the corresponding locations in the column housing, the column housing parts and / or the column insert into which the seals can be inserted or inserted. In certain embodiments of the invention, at least partial gaskets are preferred. In particular, when using graphite seals, they are preferably designed as flat gaskets. In alternative embodiments, the seals are at least partially designed as ring seals or as seals with a substantially circular or elliptical cross-section.

In a preferred embodiment, at least one flat support is provided between the column housing or a column housing part and the column insert and / or between two column housing parts, which preferably extends on one level over the entire contact surface between the respective components.

Column housing and column insert can be constructed of any suitable material. It is only essential that the material is thermostable. Preferably, the material is stable at least at temperatures of up to 250 ^° C., more preferably even at temperatures of up to 400 ^° C. Preferably, the material is also solvent resistant and substantially chemically inert. Most preferably, the material is selected from metal, ceramic and glass.

To ensure that the micro-rectification column according to the invention remains gas-tight and liquid-tight during operation, the materials of which the column housing or the column housing parts and the column insert mainly comprise preferably have similar thermal expansion coefficients. More preferably, the materials that make up the column insert and the column bottoms mainly have similar thermal expansion coefficients. More preferably, the materials of which the column housing or column housing parts, the column insert and the column trays are made mainly have similar thermal expansion coefficients. By similar coefficients of thermal expansion (coefficients of thermal expansion) is meant here that the coefficients of thermal expansion of a material used differ by no more than 30% from the thermal expansion coefficient of another material used, the percentage deviation being based on the material with the higher coefficient of thermal expansion. efficient is calculated. Even more preferably, the deviation is less than 20%, more preferably the deviation is less than 10%.

Particularly preferably, the materials used for the column housing, the column housing parts, the column insert and / or the column trays have similar coefficients of thermal expansion in the range from 0 to 250 ^° C. Most preferably, the materials used for the column housing, column housing parts and / or column insert have similar thermal expansion coefficients in the range of 0 to 400 ^° C.

A particular embodiment of a micro-rectification column according to the invention is characterized in that the column housing consists of two column housing parts, e.g. a column housing front part and a column housing rear part, wherein these column housing parts are connectable to each other so that thereby the column interior is formed. In an alternative embodiment, the column housing consists of three column housing parts, e.g. a column housing front part, a column housing rear part and a column housing intermediate part, wherein these column housing parts are connectable to each other so that thereby the column interior is formed. In further alternative embodiments, the column housing consists of several column housing parts, e.g. a column housing front part, a column housing rear part and a plurality of column housing intermediate parts, wherein these column housing parts are connectable with each other so that thereby the column interior is formed.

If it is mentioned here that the column housing parts are connected to each other so that thereby the column interior is formed, this means that thereby the column interior is formed regardless of the insertable therein column insert. It is understood that, depending on the design of column housing and column insert, the column interior is at least partially formed by the column housing in conjunction with the column insert. In this sense, the formulation that "the column housing parts are connectable to one another in such a way that the column housing parts form the column interior, if appropriate in conjunction with the column insert," is to be understood.

In a preferred embodiment, the column housing or at least one column housing part has a viewing window, by means of which the column interior can also be seen during the recognition. Preferably, a viewing window, an opening or an open area is also provided at the corresponding location of the column insert used. In embodiments with column housing intermediate part, the viewing window in the column housing be arranged between the intermediate part, in these cases, a correspondingly large opening in the Kolonen- nenonen front part or back part is provided.

An embodiment of the micro-rectification column according to the invention is characterized in that the column insert has an open region at least at one point, via which at least when the column insert is temporarily not arranged in the column housing, a mechanical engagement can take place on the column trays. Preferably, the column insert is open on at least one side, so that over the entire width of the individual column plates can be made an engagement on the column trays. Particularly preferably, the column insert is designed such that an intervention can take place at the points at which the column bottoms are stored in the column insert. In the embodiments in which column trays are provided with weirs, it is preferred if a mechanical engagement can take place on the weirs.

By mechanical intervention is here understood, for example, that the column bottoms are cleaned, that between the column bottoms a packing or packing are introduced or already introduced pack or packing is removed again, that a change in the height of the weirs is made that repair the storage of the column bottoms is carried out in the column insert or that a solid compound of the column bottoms is temporarily dissolved with the column insert.

In a preferred embodiment of the micro-rectification column according to the invention, the column trays are arranged removably in the column insert, so that thereby the possibility exists of rapidly and easily varying the type, number and arrangement of the column trays arranged in a column insert. In one embodiment of the invention, the column trays are placed on corresponding storage areas in the column insert and can therefore be easily removed and reused. In another embodiment, the column trays are fixedly connected to the column insert via fastening means, wherein the fastening means can be released by mechanical engagement and tightened again. As fastening means, for example, small screws, clips or clamps may be suitable.

The possibility of mechanical intervention in the region of the column bottoms and especially also directly on the column bottoms has the advantage that the inventive micro-rectification column can be even better optimized with respect to the respective separation tasks and set even finer. In one embodiment, the micro-rectification column according to the invention has a substantially cylindrical shape, wherein the base areas of column housing and column insert are accordingly substantially circular. By footprint is meant here the area occupied by the column housing or column insert in the plan view from above. In an altematic embodiment, the column insert has a rectangular base and therefore has a substantially cuboid shape, wherein the defined by the column housing interior has a corresponding rectangular base, so that the cuboid column insert in this interior is accurately inserted. The advantage of a cuboid column insert is that a plurality of column inserts not arranged in the column housing can be arranged in a space-saving manner for storage, for example by setting them next to one another in a corresponding storage container or laying them next to or on top of each other. In yet another embodiment, the column housing is also substantially cuboid, so that the column housing, as just described for the column inserts, can be stored very compactly and stably, together with several parallelepiped column inserts.

In one embodiment of the micro-rectification column according to the invention with a column insert having a substantially cuboidal shape, the column insert is a flat, plate-shaped column insert. As used herein, the term "shallow" refers to the shallow depth of the column insert as compared to its width and height, More preferably, the width to depth ratio in the plate-shaped column insert ranges from 1: 0.5 to 1: 0.001 and preferably in the range of 1: 0.1 to 1: 0.001 In some embodiments of the microreacting column of the invention, the depth of the column insert is in the range of 0.1 mm to 30 mm, and preferably in the range of 1 mm to 15 mm, more preferably in the range from 1 mm to 5 mm.

The flattened rectangular shape or plate shape has the advantage that the interior of the micro-rectification column can be tempered more uniformly. Cylindrical rectification columns having a circular base area have the disadvantage that, even when the column is heated from the outside over its entire height, a temperature gradient decreasing radially to the column center occurs radially. It has been found to be particularly advantageous to use micro-rectification columns having a substantially rectangular base surface, which are designed "flat", so that the distance from the inside of the column housing to the center of the interior of the column is kept as low as possible in order to maintain the temperature in the Therefore, the ratio of width to depth of the column interior is particularly in the range of about 1: 0.5 to 1: 0.001, and preferably in the range from about 1: 0.1 to 1: 0.001. In some embodiments of the micro-rectification column according to the invention, the depth of the column interior is in the range of about 0.1 mm to 30 mm and preferably in the range of about 1 mm to 15 mm, particularly preferably in the range of about 1 mm to 5 mm.

In a preferred embodiment of the micro-rectification column according to the invention having a plate-shaped column insert, a large recess is provided in the plate-shaped column insert, in which the column trays are arranged one above the other. The embodiment with a flat, plate-shaped column insert with a large recess is an example of an embodiment in which the column interior is defined not only by the column housing but by the column housing in connection with the column insert, more closely here in connection with the side walls and the rear wall of the plate-shaped column insert. The advantage of this embodiment is that, on the one hand, a column insert is available which, even if temporarily removed from the column housing, is stable and compact, and on the other hand engages the column trays via the open side of the recess can.

Preferably, in the plate-shaped column insert a seal extending along the edge of the recess is provided, which, when the column insert is arranged in the column housing, sealingly comes into contact with the column housing so that a column interior substantially closed in gas and liquid is formed.

An embodiment of the micro-rectification column according to the invention having a plate-shaped column insert is characterized in that the recess in the plate-shaped column insert has substantially rectangular side walls, the ratio of width to depth of the recess in the plate-shaped column insert being in the range from 1: 0.5 to 1: Is 0.001 and preferably in the range of 1: 0.1 to 1: 0.001. In some embodiments of the micro-rectification column according to the invention, the depth of the recess in the plate-shaped column insert is in the range of 0.1 mm to 30 mm and preferably in the range of 1 mm to 15 mm, particularly preferably in the range of 1 mm to 5 mm.

In certain embodiments, the column insert has the shape of a box or frame which can be inserted into the column housing and in which the column trays are arranged. In other, flatter embodiments, the column insert has the shape of a disk or plug-in card which is insertable or insertable into the column housing, and in the flat recess of which are raised portions extending substantially horizontally from one side to the other Extend side of the recess and are designed so that they form the interior of the column dividing column trays. The disk or cartridge-shaped column inserts are extremely practical and a variety of such inserts can be stored very compactly. In addition, a wide variety of bottom shapes can be realized cost-effectively in these applications, and the separation efficiencies achieved with these inserts are surprisingly good.

An embodiment of the micro-rectification column according to the invention is characterized in that in the column housing and in the column insert at least one region is provided, via which a controlled exchange of gases and / or liquids is possible between the column interior and the region outside the column. Preferably, in the micro rectification column at least one inlet suitable for this purpose is provided in the lower region of the column and at least one outlet suitable for this purpose is provided in the upper region of the column. The micro-rectification column according to the invention can therefore be operated both batchwise and semi-continuously or continuously.

In one embodiment, a (product) condenser standing in fluid contact with the column housing interior is provided in the column insert, at the overflow of which preferably at least one return valve is provided. Preferably, the at least one return valve is adjustable from the outside. The (product) condenser is also preferably preceded by a dephlegmator which is in fluid contact with the condenser and with the column housing interior, which is likewise arranged in the column insert and which serves to partially condense the gas mixture leaving the column, the condensate resulting therefrom can be fed back into the column and the remaining gas phase then controlled in the product condenser can be passed. In a further embodiment, a bubble is provided in the column insert in the region of the column bottom.

An embodiment of the micro-rectification column according to the invention is characterized in that in the material of the column housing one or more heating or Kühlmittelausnehmungen are provided, via the heating or cooling medium can be introduced into the column housing, preferably at least one Heizmittelausnehmung is arranged so that hereby at least one in the Column insert provided bladder can be heated, and / or at least one Kühlmittelausnehmung is arranged so that a provided in the column insert (product) capacitor can be cooled. In embodiments with dephlegmator, a recess for a heating and / or coolant is preferably arranged in the region of the dephlegmator. Preferably, a recess for a heating and / or cooling agent is provided at the level of each column bottom. Examples of "heating or cooling means" are heating or cooling elements which can be inserted into the recesses, or heating or cooling liquids which can be passed through the recesses, in the case of liquid heating or cooling means which are conducted through the recesses, Preferably, a plurality of separate heating or cooling loops are provided in order to temper the different areas of the column separately.

In one embodiment of the micro-rectification column, at least one temperature sensor extending into the interior of the column housing is provided, preferably in the immediate vicinity of a liquid or gas inlet, a liquid or gas outlet, a bubble, a column head space and / or a (product) condenser, which is provided in the column insert.

The micro-rectification column according to the invention has a very good separation efficiency. Preferably, the separation performance of the micro-rectification column according to the invention is in the range of 30 to 180 plates / m, more preferably in the range of 80 to 180 plates / m.

An embodiment of the micro-rectification column according to the invention is characterized in that at least one further column insert is removably arranged in the column housing, which has a non-subdivided inner space, a subdivided by column trays interior or charged with packing interior, preferably a column insert according to one of claims 1 to 16, wherein the first column insert with the at least one further column insert to form a correspondingly extended or widened total column insert is connectable.

The present invention also includes a column housing for a micro-rectification column according to the invention, wherein the column housing can be connected to at least one further column housing for a micro-rectification column according to the invention to form a correspondingly extended or widened overall column housing.

The present invention also includes a plant for the separation of mixtures, the plant comprising a micro-rectification column according to the invention.

For purposes of the original disclosure, it is to be understood that all such features as will become apparent to those skilled in the art from the present description, drawings, and claims, even though they have been specifically described only in connection with certain further features, both individually and separately any combination with other of the features or feature groups disclosed herein are combinable, unless this has been expressly excluded or technical conditions make such combinations impossible or pointless. On the comprehensive, explicit representation of all conceivable combinations of features is omitted here only for the sake of brevity and readability of the description. Further features and exemplary combinations of features of the present invention will now be explained with reference to the attached figures. Hereby show:

Figure 1 is an exploded view of an embodiment of the invention

Mikrorektifikationskolonne,

FIG. 2 shows a front view of an embodiment of a microcertification column according to the invention,

FIG. 3 shows a rear view of an embodiment of a microcertification column according to the invention,

FIG. 4 shows a plate-shaped column insert for a microrichification column according to the invention, sieve-shaped column bottoms being arranged in the column insert,

FIG. 5 shows the column insert of FIG. 4, the columns bottoms being removed here,

FIG. 6 shows a disk-shaped column insert for a micro-rectification column according to the invention, the column bottoms being perforated in a tubular manner,

FIG. 7 shows a disk-shaped column insert for a micro-rectification column according to the invention, the column bottoms being bubble-cap trays,

FIG. 8 shows a disk-shaped column insert for a micro-rectification column according to the invention, the column bottoms being modified bubble-cap trays,

FIG. 9 shows a disk-shaped column insert for a micro-rectification column according to the invention, wherein the individual column trays are designed like a chamber,

Figure 10 shows an embodiment of a micro-rectification column according to the invention with inserted disc-shaped column insert with bubble trays and

Figure 1 1 is a graphical representation of achieved with a micro rectification column according to the invention separation efficiency in the separation of a liquid mixture of i-octane and n-octane (for experimental procedure see example). FIG. 1 is an exploded view of an embodiment of a micro-rectification column according to the invention, this embodiment having a column housing constructed essentially in three parts from a column housing front section 5, a column housing rear section 6 and a column housing intermediate section 7. The connecting means, via which in the present embodiment, the column housing parts can be so firmly connected to each other that a gas- and liquid-tight sealed column interior is formed, here are a plurality of hex bolts 20 and hex nuts 21, which are arranged along the outer edge of the two flat sides of the column housing are. The column housing of the embodiment of the micro-rectification column according to the invention shown in FIG. 1 has the shape of a flattened cuboid. In the column housing front part 5, a large opening is provided, which is closed by the arranged in the column housing intermediate part 7 viewing window 16 in the assembled state. To protect the viewing window 16 and the liquid and gas-tight seal a support 22 is provided between the column housing front part 5 and the column housing intermediate part 7.

In the plate-shaped column insert 4, a large recess is provided, at the upper edge along a seal 24 extends. In the recess, the column trays 2 are arranged substantially horizontally one above the other. At the top of the column there is a dephlegmator 10, which is in fluid contact with the column interior divided by the column bottoms 2 on one side and on the other side with a return with the column interior divided by the column bottoms 2 and another is in fluid contact with the (product) capacitor 33. Via the valve heads 23, 23 'it can be controlled whether liquid phase / gas phase enters the (product) condenser 33 or whether the condensate formed in the dephlegmator is recirculated via the return once again into the column internal space. In the embodiment of the micro-rectification column according to the invention shown in FIG. 1, a flat support 25 is provided between the column insert 4 and the column housing rear part 6.

In the column housing rear part 6, a recess is provided in which the support 25 rests and in which the column insert 4 can be used in register with the column housing intermediate part 7 in register. For exact positioning of support 25 and in particular of column insert 4 in the recess, cylindrical pins 28 are provided in the recess in the column housing back 6, which are provided with corresponding recesses in the support 25 and the column insert 4 for the exact positioning of these components in the assembly of micro-rectification column according to the invention engage. In addition, the inlets and outlets 8, 9, can be introduced via the controlled gaseous or liquid phase in the micro-rectification column interior or can be removed therefrom in the column housing back part. The inlets / outlets 8, 9 are connected to supply / discharge terminals 26, can be passed through the gaseous or liquid phase to the column or can be led away from the column. Cylinder pins 28 are furthermore provided on the column housing rear part 6, which engage with corresponding recesses in the column housing front part 5 for the purpose of exact positioning of the two column housing parts on each other during assembly of the microcertification column according to the invention. Recesses 11 are provided in the side walls of the column housing rear part, into which cooling or heating rods can be inserted, in order to temper the micro rectification column according to the invention in the desired areas in the desired manner.

FIG. 2 shows the embodiment of the microcentrifugation column 1 according to the invention shown in FIG. 1 in an assembled state in a front view. Through the opening in the column housing front part 5 and through the viewing window in the column housing intermediate part 7 of the column insert 4 can be seen. In the column insert 4 is a large recess which defines the column interior in connection with the column housing intermediate part 7. At the upper edge of the recess provided in the column insert 4, a seal 24 is provided. The column interior is subdivided by column bottoms 2 arranged essentially horizontally above one another. The column bottoms extend from left to right between holders 17 provided in the recess into which the column bottoms 2 can be inserted. At the top of the column bottom brackets 17 each small webs 18 are provided, which merge in each case a holder 17 on a column bottom plane in Ablaufwehre 19, which ends in a collecting reservoir, which is located behind the web 18 of the next underlying column bottom plane. At least over the area between the drain weir 19 a certain level and the collection reservoir behind the web 18 of the underlying level, the two levels are thus in fluid contact.

In the bottom region of the micro-rectification column, the recess in the column insert 4 forms a bubble 12. In the column head space 14, the recess opens into a substantially horizontally extending connection 15. Via the connection 15, the dephlegmator 10 is in fluid contact with the column interior. In addition, the dephlegmator 10 is in fluid contact with the (product) condenser 33. Via the valve heads 23 and 23 'can be controlled from the outside, whether the condensate from the dephlegmator 10 is returned to the column interior, or whether liquid phase / gas phase enters the product condenser 33, from where the product can be removed via the outlet. The embodiment of the micro-rectification column according to the invention shown in FIG. 2 has the shape of an upright flat cuboid with a substantially rectangular base area.

The representation of FIG. 3 shows the embodiment of the microreactivation column 1 according to the invention shown in FIGS. 1 and 2 in the rear view. In addition to the features that The following features can also be seen in the rear view: the supply / discharge connection 26 on the upper side of the column rear part 6, via which gas or liquid is withdrawn from the dephlegmator and fed there can be, the Zuleitungs- / discharge port 26, which is arranged in the upper area seit- lieh the column housing back 6 and via a controlled liquid or gas exchange with the condenser of the micro-rectification can be done, the supply / discharge ports 26 on the Rear side of the column housing rear part 6 are arranged and via which a liquid or gas exchange with the (product) condenser, the column ninnenraum at about half the height of the column and the area in the column bottom space (bubble) can take place, and the valve controller 32, 32nd ', over which the valve heads 23, 23' are controlled.

FIG. 4 shows in detail the column insert 4 which is used in the embodiments of the microcertification column according to the invention shown in FIGS. 1 and 2. In this illustration, it can once again be clearly seen how the column bottoms 2 are inserted into the slots provided in the column bottom holders 17. In addition, the design of the inlet 8 in the column insert 4 can be seen here. The column insert 4 is shown here without a seal 24, so that the sealing groove 34 running along the upper edge of the recess can be clearly seen, in which the seal 24, which is shown in FIG. 2, is embedded.

FIG. 5 shows the column insert 4 of FIG. 4 without column bottoms 2 inserted therein, so that the slots in the column bottom holders 17, into which the column bottoms 2 can be inserted, are clearly visible. At the bottom of the recess in each case sealing strips 35 are provided at the locations where the column bottoms bear against the bottom of the recess.

FIG. 6 shows a disk-shaped or plug-in-shaped column insert 4, in which the column bottoms 2 are perforated in a tubular manner. The column bottoms 2 are in this case formed by raised areas, which extend on horizontally superimposed planes from one side to the other side of the recess and are interrupted only in sections in a tubular manner.

In Figure 7, a disk or card-shaped column insert 4 is also shown, wherein in this embodiment, the raised portions are designed so that form flat bell bottoms 2 corresponding to the depth of the recess.

The embodiment shown in FIG. 8 is a disk-type or card-type column insert 4 with modified bubble trays 2. In the embodiment of a disk-shaped or card-type column insert 4 shown in FIG. 9, the column bottoms 2 are formed in the form of chambers arranged one above the other, the gas-phase regions of which are connected to one another via s-shaped lines.

FIG. 10 shows a microreactification column 1 according to the invention, in which a disk-shaped or card-type column insert 4, as shown in FIG. 7, is installed in the column housing 3. Behind this column insert 4 is a column insert adapter, in which in the areas of the inlets and outlets (not shown) as well as in the area of the bubble 12, in the area of the dephlegmator 10, in the area of the valve head 23 and in the region of (product) Condenser 33 recesses are provided, which coincide with the corresponding areas of the disk or card-shaped column insert 4.

Example:

1 and 2 was used to determine its theoretical maximum separation efficiency ("total reflux ratio") based on a liquid mixture of i-octanol and n-octanol liquid mixture is introduced. the bladder was maintained at 1 18 ⁰ C. at about 1/3 of the height of the column was the temperature of the column interior 110.8 ⁰ C, to about 2/3 of the height of the column was the temperature of the column interior 104.2 ⁰ C and at the top of the column, the temperature was 99 - 102 ⁰ C. As was determined from the graphical evaluation shown in Figure 11, the theoretical separation step height was 0.83 cm, which corresponds to a theoretical separation stage number of 120 / m.

Reference numerals:

1 micro-rectification column

2 column bottoms

3 column housing

4 column insert

5 Column housing front part

6 column housing back

7 Column housing intermediate part

8 liquid or gas inlet

9 liquid or gas outlet

10 dephlegmator

11 heating or coolant recesses

12 bubble

13 temperature sensors

14 Column Headspace

15 connection

16 viewing windows

17 Column bottom bracket

18 footbridge

19 drainage

20 hex screw

21 hex nut

22 edition

23, 23 'valve head

24 seal

25 edition

26 supply / discharge connection

27 earthing

28 cylinder pin

29 O-ring

30 valve pin

31, 31 'recess for valve regulator

32, 32 'valve regulator

33 (product) capacitor

34 sealing groove

35 sealing strip

Claims

PATENT APPLICATIONS

Characterized in that the micro-rectification column (1) a column housing (3) and at least one Column insert (4), wherein the column trays (2) are arranged on the column insert (4), and wherein the column insert (4) removably in the column housing (3) is arranged.

2. micro-rectification column according to claim 1, characterized in that the column housing (3) consists of at least two column housing parts (5, 6), wherein the column housing parts (5, 6) are detachably gas- and liquid-tight interconnected so that thereby the column housing parts ( 5, 6) optionally in conjunction with the column insert (4) form the column interior.

3. micro-rectification column according to one of claims 1 and 2, characterized in that the column housing (3) consists of a column housing front part (5) and a Kolonnengehäuserückteil (6) and optionally a column housing intermediate part (7), wherein the column housing front part (5 ) and the column housing back (6) with each other or optionally at least one additionally arranged between intermediate column housing part (7) are gas-tight and liquid-tight connected to each other so that thereby the column housing front part (5) and the column housing back (6) and optionally at least one column housing intermediate part ( 7) optionally in conjunction with the column insert (4) form the column interior.

4. micro-rectification column according to one of claims 1 to 3, characterized in that in the column insert at least 3 column trays are arranged, preferably at least 5 column trays are arranged.

5. micro-rectification column according to one of claims 1 to 4, characterized in that the column insert (4) at least one point has an open area over which at least when the column insert (4) is temporarily not arranged in the column housing (3), a mechanical intervention on the column bottoms (2) can take place.

6. micro-rectification column according to one of claims 1 to 5, characterized in that the column trays (2) in the column insert (4) are removably arranged.

7. micro-rectification column according to one of claims 1 to 6, characterized in that the column insert (4) is a flat, plate-shaped column insert (4), wherein in the plate-shaped column insert (4) is provided a large recess in which the column bottoms (2 ) are arranged and which defines the column interior in connection with the column housing.

8. micro-rectification column according to claim 7, characterized in that the recess in the plate-shaped column insert (4) has substantially rectangular side walls, wherein the ratio of width to depth of the recess in the plate-shaped column insert (4) in the range of 1: 0.5 to 1: 0.001 and preferably in the range of 1: 0.1 to 1: 0.001.

9. micro-rectification column according to one of claims 7 or 8, characterized in that the depth of the recess in the plate-shaped column insert (4) in the range of 1 mm to 30 mm and is preferably in the range of 1 mm to 15 mm.

10. micro-rectification column according to one of claims 1 to 9, characterized in that the interior of the column housing (3) has an overall height in the range of 5 cm to 50 cm and preferably has an overall height in the range of 10 cm to 20 cm.

11. micro-rectification column according to one of claims 1 to 10, characterized in that in the column housing (3) and in the column insert (4) at least one region (8, 9) is provided, on the between the column interior and the area outside the column a controlled Exchange of gases and / or liquids is possible.

12. micro-rectification column according to one of claims 1 to 11, characterized in that in the column insert (4) with the column housing interior in fluid contact standing product condenser (33) is provided at its overflow preferably a return valve is provided.

13. micro-rectification column according to one of claims 1 to 12, characterized in that in the material of the column housing (3) one or more heating or Kühlmittelaus- recesses (11) are provided, via the heating or cooling medium can be introduced into the column housing, wherein preferably at least one Heizmittelausnehmung (1 1 ') so is ordered that over this at least one in the column insert (4) provided bubble (12) can be heated, and / or at least one Kühlmittelausnehmung (11 ") is arranged so that in the column insert (4) provided product capacitor (33) can be cooled ,

14. Microread column according to one of claims 1 to 13, characterized in that at least one in the interior of the column housing (3) reaching temperature sensor (13) is provided, preferably in the immediate vicinity of a liquid or gas inlet (8), a liquid or gas outlet (9), a bubble (12), a column head space (14) and / or a product condenser (11) which is provided in the column insert (4).

15. micro-rectification column according to one of claims 1 to 14, characterized in that the column trays (2) are exchange trays, which are preferably under Blockenbö-, valve trays, trays or grid floors selected.

16. micro-rectification column according to one of claims 1 to 15, characterized in that in the column housing (3) at least one further column insert (4 ') is removably arranged, which has a non-compartmented interior, one of column trays (2) sub-divided interior or a Having filled with packing interior, preferably one

Column insert according to one of claims 1 to 16, wherein the first column insert (4) is connectable to the at least one further column insert (4 ') to form a correspondingly extended or widened total column insert.

17. Column housing (3) for a micro-rectification column (1) according to one of claims 1 to 16, characterized in that the column housing (3) with at least one further column housing (3 ') according to one of claims 1 to 16 to form a correspondingly extended or widened total column housing is connectable.

18. Plant for the separation of mixtures, characterized in that the plant comprises a micro-rectification column (1) according to one of claims 1 to 16.