DE102007062976A1 - Micro-rectification column for the thermal separation of liquids - Google Patents

Abstract

To provide a rectification column useful for a variety of very different separation tasks in the preparative separation of small quantities of liquid mixtures, e.g. can be used in a fine chemical laboratory or in a scientific laboratory, the invention proposes a micro-rectification column for the thermal separation of liquids, which has a plurality of arranged in the micro-rectification and the column interior dividing column trays, wherein the micro-rectification column is further characterized in that it is a column housing and comprising at least one column insert, wherein the column bottoms are arranged on the column insert, and wherein the column insert is removably arranged in the column housing. With the micro-rectification column proposed according to the invention, better separation performances can be achieved for a plurality of different individual separation tasks than with a conventional rectification column.

Description

The The present invention relates to a micro-rectification column for the thermal Separation of liquids with several arranged in the micro rectification column, and the column interior dividing column bottoms.

distillation and rectification are methods for distillative separation of liquid mixtures. Compared to simple distillation, the rectification is multi-stage trained and thereby offers a significantly higher separation efficiency. The multistage is effected in the rectification by liquid phase and gaseous phase in the column under direct contact in countercurrent to each other guided become. For this purpose, devices are in a rectification column (Packings, fillers, column bottoms) provided, the one possible size contact area between the liquid phase and the gaseous Phase enable.

At the contact surface between liquid phase and gaseous Phase in a given range of a rectification column can at a given temperature and pressure and if sufficient long contact theoretically a balance of substances that in the liquid Phase, and the substances that are in the gaseous phase, adjust. This is indeed but only with the ideal column of the case. Although the ideal state the equilibration in practice usually not achieved Nevertheless, in the rectification by the countercurrent principle accumulate the more volatile Components of the liquid mixture in the direction of the column head and the less volatile in the direction of the bottom of the column. The separation efficiency of a column can then mathematically calculated from the parameters of the actual separation be determined and expressed in the form of the calculated number of theoretical plates.

The Rectification is a commonly used industrial process for substance separation and is used for example during firing alcoholic beverages, in oil refining, in the industrial production of liquid chemicals and in the distillative Separation of liquefied Air in their components.

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 arranged an evaporator and located in the region of the column head generally a capacitor. Usually located in the bottom The rectification column an inlet and at the top of the column or in the region of the condenser an outlet, wherein the inlet and outlet designed so that can be a continuous one or discontinuous operation of the column can take place.

The The present invention relates to a tray column. In a tray column are the devices that are designed to maximize the contact surface between the liquid Phase and the gaseous To enable phase Column trays. column trays are common horizontal, plate-shaped Built-in, at certain intervals in the cylindrical column are installed. The floors of soil columns can screen or lattice-shaped be configured or have other facilities through which the gaseous Phase can penetrate the ground, such. B. holes, slots, bell passages or valves. During rectification, the liquid phase flows on one side the column on the bottom of the column and from there across the Floor and on the other side over a weir on the floor below. The liquid layer, which is located on the bottom of the column, comes here with the gaseous phase in contact. Are provided in the bottom of the column openings, through the gaseous Phase can pass, so forms a so-called bubble layer out. With bubble trays may be a part of passing through the openings provided in the bottom gaseous Phase to the over the openings arranged Gloc ken condense, the condensate from there reaches the bottom of the bell where it accumulates.

The Construction of a tray greatly affects the separation properties a rectification column for a certain separation task. Alone the different flow properties of the mixture to be separated and its components make it necessary to that he for one certain separation task the appropriate column bottom construction and the optimum properties of the column bottoms, such. B. material, surface properties, Size of the pores, openings or slots, detected. In the production of a column these properties usually specifies in advance, whereby one receives a column, for a particular separation task that is optimized for another separation task, however, does not necessarily have to be suitable. As a result, needed one for one different separation tasks may also be several different Rectification columns, which is associated with correspondingly higher acquisition costs is. Especially in areas where you are with very different Separation tasks is faced, such. B. in the production of small quantities of certain chemicals for scientific laboratories or in the manufacture of fine chemicals, this poses a problem represents.

It is therefore an object of the present invention, a rectification column to provide for a variety of very different separation tasks in the preparative Separation of small amounts of liquid mixtures, such. B. in a fine chemical laboratory or in a scientific Laboratory is used. It is also desired that these Rectification column with regard to the respective separation tasks offers better separation performance than a conventional rectification column.

These Task is solved by a micro rectification column of the type mentioned, characterized in that the micro-rectification column a column housing and at least one column insert, wherein the column bottoms at the Column insert are arranged, and wherein the column insert can be removed in the column housing is arranged.

Thereby, that according to the present Invention the column bottoms not directly on the column housing are arranged, but at a column insert, in turn removable in the column housing is arranged in the micro-rectification column according to the invention depending on the separation task different column bottoms for subdivision of the column interior in the column housing be introduced. Particularly advantageous here is that thereby, that the Column bottoms at respective column insert are arranged, all column bottoms simultaneously from the column housing can be taken and then it can be another column insert with other column bottoms or with a different number and arrangement of column bottoms in the column housing be introduced. Furthermore can at the column bottoms arranged in the removed column insert changes be made or it can the column bottoms arranged in the withdrawn column insert by others column trays be exchanged, or it can Number and arrangement of column trays can be changed. The micro-rectification column according to the invention this is for a variety of very different separation tasks can be used and can by selecting the used column bottoms and the selection of the column bottom number and arrangement with regard to the respective separation task can be optimized to those for this Separation task best possible To achieve separation efficiency.

The column trays are preferably under bubble trays, Valve trays, sieve trays or grid floors selected. Preferably, in the column feed, at least 3 and up to 30 column bottoms arranged. More preferably, at least in the column feed 5 and up to 20 column bottoms arranged. In one embodiment all column bottoms have the same construction. at an alternative embodiment of the Invention are the column bottoms constructed differently, so that in a column insert, for example, bubble trays with sieve trays, bubble trays with valve trays or valve bottoms with grid floors combined etc.

The Microresification column according to the invention is due to the possibility the nature, number and arrangement of the trays fast and easy to vary of particular advantage in the preparative separation of small Quantities of different liquid mixtures in a fine chemicals laboratory. Even with the fractionation of only available in very small quantities Mixtures, such. As mixtures of certain essential oils, can the micro-rectification column according to the invention advantageously by selecting the type, number and arrangement the column bottoms be adapted quickly and easily to the respective separation task. About that In addition, the micro-rectification column according to the invention very useful in a development or research laboratory, in which for certain Separation tasks suitable distillative separation systems are sought or in which the parameters of rectification and their interaction in principle to be examined.

The Microresification column according to the invention is especially for designed for use in technical or scientific laboratories. The size of the column is therefore the laboratory scale customized. Thus, the interior of the column housing preferably has an overall height in Be rich from 5 cm to 100 cm, preferably a total height in the range of 10 cm to 50 cm and most preferably an overall height in the range of 10 cm to 30 cm. The number of column bottoms is based on the height of the column interior, 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 bottom per 2 cm.

at an embodiment the micro-rectification column according to the invention there is the column housing from a component in which the column insert gas and liquid-tight can be inserted, thereby the column housing in conjunction with the column insert a closed column interior divided by the column bottoms formed.

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 connected to each other so that thereby the column housing parts optionally in conjunction with the column training the column interior. The advantage of this embodiment is that in a two- or multi-part column housing, the column housing parts can be very firmly interconnected by connecting means to ensure that a gas- and liquid-tightly sealed column interior is formed. Suitable for this purpose connecting means may be, for example, screws, clips or clamps through which the column housing parts can be pressed against each other so that the column housing parts form a gas and liquid-tight sealed column interior.

The Formulation "gas and liquid-tight "is understood here as that from the in this way completed column interior no gases or liquids can escape uncontrollably and no gases or liquids uncontrolled from the outside penetrate into the column interior completed in this way can. Especially the sealing of a column housing and a removable column insert or even from a multipart column housing and a column insert constructed micro-rectification column poses a great challenge because the column is in a wide temperature range, for example from room temperature to above 400 ° C range can, is operated. Furthermore The separation mixtures often comprise organic solvents, the many common ones Attack sealing materials. In addition, certain distillative separations with negative pressure drove in the column interior. Other separations occur in the course of rectification in the column interior a big overpressure. The column interior of the micro-rectification column according to the invention is therefore preferably also at Ko interior temperatures of up to 250 ° C, still more preferably even at column interior temperatures of up to 400 ° C gas and liquid-tight lockable. Preferably is the column interior even with an overpressure in the column interior of up to 3 bar, preferably of up to 5 bar, gas and liquid tight completed. The column interior is also particularly preferred at vacuum, d. H. up to a negative pressure of up to 50 mbar, preferably of up to 10 mbar, in the column interior, gas and liquid tight completed.

In order to the micro-rectification column according to the invention gas and liquid tight is lockable, are preferably seals or pads made of plastic, such as z. Perfluorinated rubber, perfluorinated elastomer, fluoroelastomer, Polytetrafluoroethylene or ethylene, of aluminum or of graphite used to seal the area between column insert and column housing, with multi-part column housings the column housing parts to seal against each other and possibly also the area between column bottoms and column insert or column housing seal or light Unevenness at the contact surfaces between the respective components. Seals or Graphite supports have the advantage that they are favorable and temperature resistant up to 450 ° C.

The Seals or pads can in the respective sealed areas just before assembly the individual components are placed. In a preferred embodiment are partially in the appropriate places in the column housing, the Column housing parts and / or the column insert grooves or depressions provided in the Seals can be inserted or inserted. In certain embodiments At least partial gaskets are preferred in the invention. Especially when using graphite seals, these are preferably designed as flat gaskets. In alternative embodiments the seals are at least partially as ring seals or as seals having a substantially circular or elliptical cross-section executed.

at a preferred embodiment is between the column housing or a column housing part and the column insert and / or between two column housing parts at least one areal Pad provided, preferably on a plane above the entire contact surface extends between the respective components.

Column housing and Column insert can be constructed of any suitable material. It is only essential that this Material is thermostable. Preferably, the material is at least at temperatures of up to 250 ° C stable, more preferably even at temperatures up to 400 ° C. Preferably is the stuff as well solvent resistant and substantially chemically inert. This is particularly preferred Material selected under metal, ceramics and glass.

To ensure that the micro-rectification column according to the invention remains gas-tight and liquid-tight in 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. Under similar coefficient of thermal expansion (coefficient of thermal expansion) is understood here to mean that the coefficients of thermal expansion of one material used do not differ by more than 30% from the thermal expansion coefficient of another material used, the percentage deviation being calculated from the material having the higher coefficient of thermal expansion. Even more preferably, the deviation is less than 20%, more preferably the deviation is less than 10%.

Especially Preferably, the materials used for the column housing, the Column housing parts, the column insert and / or the column bottoms are used similar thermal expansion coefficient in the range of 0 to 250 ° C. Especially Preferably, the materials used for the column housing, the Column housing parts and / or the column insert used are similar thermal expansion coefficients in the range of 0 to 400 ° C on.

A special embodiment a micro-rectification column according to the invention is characterized in that the Column housing off two column housing parts exists, such. B. a column housing front part and a column housing back part, these column housing parts are connected to each other so that thereby the column interior is trained. In an alternative embodiment, the column housing is made three column housing parts, such as B. a column housing front part, a column housing back and a column housing intermediate part, these column housing parts are connected to each other so that thereby the column interior is trained. In further alternative embodiments, the column housing is made several column housing parts, such as B. a column housing front part, a column housing back and several Column housing intermediate parts, these column housing parts are connected to each other so that thereby the column interior is trained.

If Here it is mentioned 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 regardless of the insertable therein column insert becomes. It is understood that depending on Design of column housing and column insert, the column interior at least partially the column housing is formed in connection with the column insert. In this sense is also the formulation that "the column housing parts are connected to each other so that thereby the column housing parts optionally in conjunction with the column insert the column interior train, "to understand.

at a preferred embodiment the column housing or at least one column housing part a window on, over one can also see the column interior during the rectification can. Preferably, at the corresponding point of the inserted Column insert also a viewing window, an opening or a open area provided. In embodiments with column housing intermediate part the viewing window can be arranged in the column housing intermediate part be, in these cases a correspondingly large opening in the Column housing front part or rear sections is provided.

A embodiment the micro-rectification column according to the invention is characterized in that the Column insert at least one point an open area has, over at least when the use of the column is temporary not in the column housing is arranged, carried out a mechanical intervention on the column bottoms can. Preferably, the column insert is on at least one side open so that over the entire width of the individual column bottoms made an intervention on the column bottoms can. Particularly preferably, the column insert is designed in such a way that that on the places where the column bottoms in the column insert stored are an intervention can be done. In the embodiments, where column bottoms are provided with weirs, it is preferred if a mechanical Intervention can be done on the weirs.

Under For example, mechanical intervention is understood here to mean that the column bottoms are cleaned be that between the column bottoms one Pack or packing introduced be removed or already introduced pack or packing is removed again, that one Change in the height of Weed is made that a repair at the location tion of the column bottoms takes place in the column insert or that a solid compound of column trays temporarily with the column insert solved becomes.

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 quickly and easily varying the type, number and arrangement of the column trays arranged in a column tray. 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 bottoms are firmly connected to the column insert via attachment means, wherein the fasteners can be solved by mechanical engagement and tightened again. As fastening means, for example, small screws, clips or clamps may be suitable.

The possibility the mechanical intervention in the field of column bottoms and v. a. also directly at the bottom of the column has the advantage that the micro-rectification column according to the invention This makes it even better with regard to the respective separation tasks optimized and can be adjusted even finer.

at an embodiment has the micro-rectification column according to the invention a substantially cylindrical shape, wherein the bases of column housing and column insert are accordingly substantially circular. With Floor space here is the area meant the column housing or use the column insert in the plan view from above. At a alternative embodiment the column insert has a rectangular base and therefore has an im essential cuboid Shape, wherein the defined by the column housing interior a has corresponding rectangular base, so that the cuboid column insert in this interior fit can be used. The advantage of a cuboid column insert exists in that way several, not arranged in the column housing column inserts for Storage space can be arranged by, for example, saving space be set side by side in a corresponding storage container or beside or be placed on top of each other. In yet another embodiment is also the column housing essentially cuboid, so that Column housing as already for the column inserts described, together with several parallelepiped column inserts very can be stored practically space-saving and stable.

at an embodiment the micro-rectification column according to the invention with a column insert having a substantially cuboidal shape the column insert is a flat, plat tenförmiger column insert. Of the The term "flat" refers here on the small depth of the column insert compared to the Width and height. More preferably, the ratio of width to depth is in the disc-shaped Column insert in the range of 1: 0.5 to 1: 0.001 and preferably in the range of 1: 0.1 to 1: 0.001. In some embodiments the micro-rectification column according to the invention is the depth of the column insert 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 of 1 mm to 5 mm.

The flattened rectangular shape or plate shape has the advantage that the interior the micro rectification column can be tempered more uniformly. Cylindrical rectification columns have a circular base the disadvantage that itself when the column over their entire height from the outside heated becomes, radially a temperature gradient falling to the column center point established. It has been found to be particularly advantageous, micro-rectification columns to be used with a substantially rectangular base which is 'flat', so that the distance from the inside of the column housing to Center of the column interior as possible is kept low to the temperature in the column interior as homogeneous as possible to be able to adjust d. H. without significant temperature drop toward the center of the column interior. Particularly preferred is the ratio of Width to depth of the column interior therefore in the range of about 1: 0.5 to 1: 0.001 and preferably in the range of about 1: 0.1 to 1: 0.001. In some embodiments 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, especially preferably in the range of about 1 mm to 5 mm.

at a preferred embodiment the micro-rectification column according to the invention with a plate-shaped Column insert is in the plate-shaped column insert one size Recess provided, in which the column bottoms 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 is from the column housing in connection with the column insert, a bit more closely related here with the side walls and the back wall of the disc-shaped Column feed. The advantage of this embodiment is that hereby on the one hand, a use of columns is available, which even then, if he is temporarily from the column housing is present, stable and compact, and on the other hand on the open side of the recess made an engagement on the column bottoms can.

Preferably is 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 is with the column housing sealingly comes into contact, so that a substantially gas and liquid-tight completed column interior is formed.

An embodiment of the inventive A micro-rectification column having a plate-shaped column insert is characterized in that the recess in the plate-shaped column insert has substantially rectangular side walls, wherein the ratio of width to depth of the recess in the plate-shaped column insert is in the range of 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 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.

at certain embodiments the column insert has the shape of a box or frame, the in the column housing can be used and in which the column bottoms are arranged. For others, flatter embodiments the column insert has the shape of a disk or plug-in card, in the column housing can be inserted or inserted, and in its shallow recess Sublime places are, which are substantially horizontally from one Side to the other side of the recess extend and designed they are form the bottom of the column dividing column trays. The disc or card-shaped column inserts are extremely practical and a variety of such uses can be stored very space-saving. In addition, the most diverse Ground shapes in these operations economical realize and the performance achieved with these operations are surprising Good.

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

at an embodiment in the column insert is in fluid contact with the column housing interior standing (product) condenser provided at its overflow preferably at least one return valve is provided. Preferably, this is at least one return valve from the outside adjustable. Particularly preferred is the (product) capacitor still one in fluid contact with the condenser and with the column housing interior standing upstream dephlegmator, which also in the column is arranged and which serves to emerge from the column Partially condense gas mixture, wherein the resulting condensate be fed back into the column can and the remaining gas phase then controlled in the product condenser can be directed. In a further embodiment is in the column insert provided in the area of the column bottom a bubble.

A embodiment the micro-rectification column according to the invention is characterized in that in Material of column housing one or more heating or coolant recesses are provided over the heating or cooling agent in the column housing can be introduced, wherein preferably at least one Heizmittelausnehmung so is arranged that over this at least a provided in the column insert bladder can be heated, and / or at least one coolant recess is arranged so that a to be cooled in the column insert provided (product) condenser can. In embodiments with Dephlegmator is preferably in the region of the dephlegmator a recess for a Heating and / or coolant arranged. Preferably, at the height of each tray is one Recess for a heating and / or coolant intended. Examples of "heating or Coolant "are in the recesses plug-in heating or cooling elements or heating or cooling liquids, which can be passed through the recesses. In the case of liquid heating or coolants, which are passed through the recesses are preferably several separate heating or cooling loops provided to temper the different areas of the column separately to be able to.

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

The Microresification column according to the invention has a very good separation performance. Preferably, the Separation efficiency of the micro-rectification column according to the invention in the range of 30 to 180 plates / m, more preferably in the range from 80 to 180 stages / 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-compartmentalized interior, an interior partitioned by column bottoms or an interior packed with packing, preferably a column insert according to any one of claims 1 to 16, wherein the first column insert with the at least one further column insert forming a correspondingly extended or widened total column insert is connectable.

The present invention also a column housing for one micro rectification column according to the invention, wherein the column housing with at least one further column housing for a micro-rectification column according to the invention Training a correspondingly extended or broadened Total column housing is connectable.

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

For purposes the original one Revelation is noted that all features as they are from the present description, the drawings and the claims for a To open up a specialist, even if they are specific only in connection with certain others Characteristics have been described, both individually and in any Compilations with other features disclosed herein or Feature groups are combinable, unless this is expressly excluded or technical conditions such combinations were impossible or make pointless. On the comprehensive, explicit representation of all conceivable combinations of features is here only for brevity and omitted for the readability of the description.

Further Features and example feature combinations of the present invention Invention will now be explained with reference to the accompanying figures. in this connection demonstrate:

1 an exploded view of an embodiment of the micro-rectification column according to the invention,

2 a front view of an embodiment of a micro-rectification column according to the invention,

3 a rear view of an embodiment of a micro-rectification column according to the invention,

4 a plate-shaped column insert for a micro-rectification column according to the invention, wherein sieve-shaped column bottoms are arranged in the column insert,

5 the column use of 4 , where the column bottoms are taken from here,

6 a disk-shaped column insert for a micro-rectification column according to the invention, wherein the column trays are perforated in a tubular manner,

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

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

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

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

11 a graphic representation of the achieved with a micro-rectification column according to the invention separation efficiency in the separation of a liquid mixture of octane and n-octane (for experimental procedure see example).

1 Figure 11 is an exploded view of an embodiment of a micro-rectification column according to the invention, this embodiment having a column housing consisting essentially of three parts of a column housing front section 5 , a column backer 6 and a column housing intermediate 7 is constructed. The connecting means, via which in the present embodiment, the column housing parts can be so firmly connected to each other that a gaseous and liquid-tight sealed column interior is formed, here are a variety of hexagon screws 20 and hex nuts 21 which are arranged along the outer edge of the two flat sides of the column housing. The column housing of in 1 illustrated embodiment of the micro-rectification column according to the invention has the shape of a flattened cuboid. In the column housing front section 5 a large opening is provided, which is of the in the column housing intermediate part 7 arranged viewing window 16 is closed in the assembled state. To protect the viewing window 16 and to the liquid and gas-tight seal is between the column housing front part 5 and the column housing intermediate part 7 an edition 22 intended.

In the plate-shaped column insert 4 a large recess is provided at the top along a seal 24 runs. In the recess, the column trays are substantially horizontally one above the other 2 arranged. At the top of the column there is a dephlegmator 10 who is on one side over the connection 15 with that of the column bottoms 2 subdivided column interior is in fluid contact and on the other hand on the one hand via a return to that of the column bottoms 2 divided column interior and the other with the (product) capacitor 33 is in fluid contact. Over the valve heads 23 . 23 ' can be controlled, whether liquid phase / gas phase in the (product) condenser 33 passes or whether the condensate formed in the dephlegmator is returned via the return again in the column interior. At the in 1 illustrated embodiment of the micro-rectification column according to the invention is between the column insert 4 and the column housing back 6 a flat edition 25 intended.

In the column housing back 6 a recess is provided in which the support 25 and in which the column insert 4 in connection with the column housing intermediate part 7 can be used accurately. For exact positioning of support 25 and in particular column application 4 in the recess are cylindrical pins 28 in the recess in the column housing back 6 provided with corresponding recesses in the overlay 25 and the column insert 4 for the purpose of the exact positioning of these components when assembling the micro-rectification column according to the invention engage. In addition, the in and outlets are located in the column housing back 8th . 9 , via the controlled gaseous or liquid phase can be introduced into the micro-rectification column interior or can be removed therefrom. The inlets / outlets 8th . 9 are with supply / discharge connections 26 connected, can be passed over the gaseous or liquid phase to the column or can be led away from the column. At the column housing back 6 are still cylindrical pins 28 provided with corresponding recesses in the column housing front part 5 for the purpose of the exact positioning of the two column housing parts on each other in assembling the micro-rectification column according to the invention engage. In the side walls of the column housing back are recesses 11 provided in the cooling or heating rods can be inserted in order to temper the inventive micro-rectification column in the desired areas in the desired manner.

In 2 is the in 1 illustrated embodiment of the micro-rectification column according to the invention 1 shown in assembled state in front view. Through the opening in the column housing front part 5 and through the viewing window in the column housing intermediate part 7 is the column insert 4 to recognize. In the column insert 4 There is a large recess, which in conjunction with the column housing intermediate part 7 defined the column interior. At the top of the in the column insert 4 provided recess is a seal 24 intended. The column interior is subdivided by substantially horizontally stacked column trays 2 , The column bottoms extend from left to right between holders provided in the recess 17 into which the column bottoms 2 are pluggable. At the top of the column bottom supports 17 are each small bridges 18 provided, each with a holder 17 on a column floor level in drainpipe 19 pass over, which in a collecting reservoir, which is behind the jetty 18 the next underlying column floor level ends. At least over the area between the drain weir 19 a certain level and the collection reservoir behind the jetty 18 the lower level, the two levels are in fluid contact with it.

In the bottom region of the micro-rectification column, the recess forms in the column insert 4 a bubble 12 , In the column head room 14 the recess opens into a substantially horizontally extending connection 15 , About the connection 15 is the dephlegmator 10 with the column interior in fluid contact. In addition, the dephlegmator stands 10 with the (product) capacitor 33 in fluid contact. Over 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 in the product condenser 33 from where the product can be removed via the outlet. In the 2 illustrated embodiment of the micro-rectification column according to the invention has the shape of an upright flat cuboid with a substantially rectangular base.

The representation of 3 shows the in the 1 and 2 illustrated embodiment of the micro-rectification column according to the invention 1 in the rear view. In addition to the features already from the 1 and 2 clearly show, in the rear view also recognize the following features: the supply / discharge connection 26 on the top of the column housing back 6 , taken over the controlled gas or liquid from the dephlegmator or there to can be performed, the supply / discharge connection 26 , in the upper area at the side of the column housing back 6 is arranged and can be done via a controlled liquid or gas exchange with the condenser of the micro-rectification column, the supply / discharge connections 26 standing on the back of the column housing back 6 are arranged and via which a liquid or gas exchange with the (product) condenser, the column interior at about half the height of the column and the area in the column bottom space (bubble) can take place, and the valve regulator 32 . 32 ' over which the valve heads 23 . 23 ' to be controlled.

In 4 is the column insert 4 who in the in the 1 and 2 illustrated embodiments of the micro-rectification column according to the invention is used, shown in detail. In this illustration, it can be clearly seen again how the column bottoms 2 in the in the column bottom supports 17 provided slots are inserted. In addition, here is the design of the inlet 8th in the column insert 4 to recognize. The column insert 4 is here without seal 24 represented, so that along the upper edge of the recess extending sealing groove 34 It can be clearly seen in the seal 24 , in the 2 is embedded.

In 5 is the column insert 4 from 4 without inserted tray bottoms 2 shown, so that the slots in the column bottom brackets 17 into which the column bottoms 2 can be plugged in, are clearly visible. At the bottom of the recess are in each case at the locations where the column bottoms at the bottom of the recess, sealing strips 35 intended.

In 6 is a disk-shaped or card-shaped embossed column insert 4 represented in which the column bottoms 2 are broken tubular. The column bottoms 2 in this case are formed by raised points, which extend on horizontally superimposed planes from one side to the other side of the recess and are interrupted only partially tubular.

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

In the 8th illustrated embodiment is a disk or card-shaped column insert 4 with modified bell bottoms 2 ,

At the in 9 illustrated embodiment of a disk or card-shaped column insert 4 are the column bottoms 2 in the form of superimposed chambers whose gas phase regions are connected to each other via s-shaped lines formed.

In 10 is a micro-rectification column according to the invention 1 in which a disk or card-shaped column insert 4 as he is in 7 is shown in the column housing 3 is installed. Behind this column deployment 4 There is a column insert adapter, in which in the areas of the inlets and outlets (not shown) and 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 area of the (product) capacitor 33 Recesses are provided which are associated with the corresponding areas of the disk or card-shaped column insert 4 cover.

Example:

The in the 1 and 2 The inventive micro-rectification column according to the invention was used to determine its theoretical maximum separation capacity ("total reflux ratio") relative to a liquid mixture of i-octanol and n-octanol.3 ml of the liquid mixture were introduced into the bubble with a volume of about 5 ml 118 ° C. At about 1/3 of the height of the column, the temperature of the column interior was 110.8 ° C., at about 2/3 of the height of the column the temperature of the column interior was 104.2 ° C. and at the top of the column the temperature was 99-102 ° C. As from the in 11 was determined, the theoretical separation step height was 0.83 cm, which corresponds to a theoretical separation number of 120 / m.

1

Mikrorektifikationskolonne

2

column trays

3

column housing

4

column feed

5

Column housing front part

6

Column mounting panel

7

Column intermediate housing part

8th

liquid or gas inlet

9

liquid or gas outlet

10

dephlegmator

11

heating or coolant recesses

12

bladder

13

temperature sensor

14

Column headspace

15

connection

16

window

17

Column bottom bracket

18

web

19

outlet weir

20

Hex bolt

21

Hex nut

22

edition

23 23 '

valve head

24

poetry

25

edition

26

Supply / exhaust port

27

grounding

28

straight pin

29

O-ring

30

valve pin

31 31 '

recess for valve regulators

32 32 '

valve controller

33

(Product) capacitor

34

seal groove

35

sealing strip

Claims (18)

Micro-rectification column ( 1 ) for the thermal separation of liquids with several in the micro rectification column ( 1 ), and the column interior dividing column trays ( 2 ), characterized in that the micro-rectification column ( 1 ) a column housing ( 3 ) and at least one column insert ( 4 ), the column bottoms ( 2 ) at the column insert ( 4 ) and the column insert ( 4 ) removable in the column housing ( 3 ) is arranged. Micro-rectification column according to claim 1, characterized in that the column housing ( 3 ) from at least two column housing parts ( 5 . 6 ), wherein the column housing parts ( 5 . 6 ) are detachably gas- and liquid-tight so interconnected that thereby the column housing parts ( 5 . 6 ) optionally in conjunction with the column insert ( 4 ) form the column interior. Microcentrifugation column according to one of Claims 1 and 2, characterized in that the column housing ( 3 ) from a column housing front section ( 5 ) and a column back ( 6 ) and optionally a column housing intermediate part ( 7 ), wherein the column housing front part ( 5 ) and the column housing back ( 6 ) with one another or alternatively via at least one intermediate column housing part ( 7 ) detachably gas- and liquid-tight are connected to each other so that thereby the column housing front part ( 5 ) and the column housing back ( 6 ) and optionally the at least one column housing intermediate part ( 7 ) optionally in conjunction with the column insert ( 4 ) form the column interior. Micro-rectification column according to one of claims 1 to 3, characterized in that in the column insert at least 3 column bottoms are arranged, preferably at least 5 column bottoms are arranged. Micro-rectification column according to one of Claims 1 to 4, characterized in that the column insert ( 4 ) has at least one point at an open area over which at least when the column insert ( 4 ) temporarily not in the column housing ( 3 ), a mechanical engagement on the column bottoms ( 2 ). Micro-rectification column according to one of Claims 1 to 5, characterized in that the column bottoms ( 2 ) in the column ( 4 ) are removably arranged. Micro-rectification column according to one of Claims 1 to 6, characterized in that the column insert ( 4 ) 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. 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 ) is in the range of 1: 0.5 to 1: 0.001 and preferably in the range of 1: 0.1 to 1: 0.001. 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 ) is in the range of 1 mm to 30 mm and preferably in the range of 1 mm to 15 mm. 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. Micro-rectification column according to one of claims 1 to 10, characterized in that in the column housing ( 3 ) and in the column ( 4 ) at least one area ( 8th . 9 ) is provided, through which a controlled exchange of gases and / or liquids between the column interior and the area outside the column is possible. Micro-rectification column according to one of claims 1 to 11, characterized in that in the column insert ( 4 ) a product condenser in fluid contact with the column housing interior ( 33 ) is provided, at the overflow preferably a return valve is provided. 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 Kühlmittelausnehmungen ( 11 ) are provided, can be introduced via the heating or cooling means in the column housing, wherein preferably at least one Heizmittelausnehmung ( 11 ' ) is arranged so that on this at least one in the column ( 4 ) provided bladder ( 12 ) can be heated, and / or at least one Kühlmittelausnehmung ( 11 '' ) is arranged so that one in the column insert ( 4 ) provided product capacitor ( 33 ) can be cooled. Micro-rectification column according to one of claims 1 to 13, characterized in that at least one into the interior of the column housing ( 3 ) reaching temperature sensor ( 13 ) is provided, preferably in the immediate vicinity of a liquid or gas inlet ( 8th ), a liquid or gas outlet ( 9 ), a bubble ( 12 ), a column headspace ( 14 ) and / or a product capacitor ( 11 ), the one or more in the Column ( 4 ) is provided. Micro-rectification column according to one of Claims 1 to 14, characterized in that the column bottoms ( 2 ) Are replacement bottoms, which are preferably selected from bubble trays, valve trays, sieve trays or grid trays. Micro-rectification column according to one of claims 1 to 15, characterized in that in the column housing ( 3 ) at least one additional column insert ( 4 ' ), which has an undivided interior space, one of column trays ( 2 ) has a subdivided interior or an interior filled with packing, preferably a column insert according to one of claims 1 to 16, wherein the first column insert ( 4 ) with the at least one further column insert ( 4 ' ) is connectable to form a correspondingly extended or widened total column use. 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 with the formation of a correspondingly extended or widened total column housing is connectable. Plant for the separation of mixtures, characterized in that the plant is a micro-rectification column ( 1 ) according to any one of claims 1 to 16.