EP2244799A1

EP2244799A1 - Distillation device

Info

Publication number: EP2244799A1
Application number: EP09702695A
Authority: EP
Inventors: Evelyn Jost; Frank Ziermann
Original assignee: Individual
Current assignee: Individual
Priority date: 2008-01-15
Filing date: 2009-01-12
Publication date: 2010-11-03
Also published as: WO2009090021A1; CN101918096A; US20110011726A1; DE102008005861B3

Abstract

The invention relates to a distillation device (1), comprising at least one first distillation region (5) with at least one first gas outlet line (6), at least one second distillation region (8) with at least one further gas outlet line (9, 9'), wherein the distillation regions (5, 8) are connected to each other. The first distillation region (5) is formed by a first line, the second distillation region (8) by a second line, and both lines forming the distillation regions (5, 8) are connected to each other in a controllable way. The invention further relates to methods for operating such a distillation device (1).

Description

Distillation s device

The invention relates to a distillation apparatus, as used for distilling liquids, in particular for separating liquid mixtures.

DE 1 773 893 A discloses a multi-stage distillation apparatus comprising a first evaporation vessel and a distillation column arranged thereon, a subsequent condenser and further evaporation vessels and associated condensers, the condensers each being connected to the subsequent evaporation vessel and the condenser of the last vessel being a drainage line having. In this case, all other evaporation vessels are arranged in a ring around the distillation column and the lines leading from the evaporation vessels to the condensers extend in the interior of the distillation column. Each of the evaporation vessels is electrically heated.

From WO 98/11395 Al a heat exchanger is known in which branching out of the line for the liquid to be treated steam outlets are provided for the vapors generated in the heat exchanger. These steam outlets will be at the end of the Heat exchange area merged again.

The US 4,760,742 shows a system for monitoring a petroleum stream, which includes a line for the petroleum stream, passed over the branching lines resulting in petroleum streams for flow measurement in a manifold and then the manifold again the main line with the liquid petroleum stream, whose flow also is measured, is supplied.

EP 0 344 566 A1 discloses a distillation apparatus which comprises a heating device, a distillation medium inlet, a steam outlet, a distillation space between the distillation medium inlet and the steam outlet and a discharge for the separated constituents leaving the bottom of the distillation space. In a heating vessel, which can be filled with a heating medium which can be heated by the heating means, a downpipe extending from above to below, adjoining the distillation medium inlet at the top, and a riser pipe running from bottom to top towards the steam outlet are arranged. During operation, the two tubes are surrounded by the heating medium. They are also connected to each other below and form the distillation room. The drain is located below the juncture of the downcomer with the riser and contains a siphon.

Such known distillation devices still leave something to be desired. In particular, the efficiency of the distillation apparatus leaves something to be desired.

The invention is therefore based on the object to improve a distillation apparatus. In this case, the distillation apparatus should also be used in particular for heavy-boiling liquid mixtures. This object is achieved by a distillation device with the features of claim 1. Advantageous embodiments are the subject of the dependent claims.

According to the invention, a distillation device is provided, comprising at least one first distillation region having at least one first gas outlet line, at least one second distillation region having at least one second gas outlet line, wherein the distillation regions are directly connected to one another, the first distillation region through a first line and the second Distillation region is formed by a second line. Here, the two, the distillation areas forming lines are controllably connected to each other, for example by means of a controllable valve.

The tubes are preferably tubes with a circular cross section, but also pipes with a rectangular or other cross section are possible. In addition, elements may be provided in the interior of the tubes which influence the flow, in particular ensure continuous mixing during the flow, so that the temperature of the liquid to be distilled is as uniform as possible. The design of the distillation zones as conduits allows for the provision of a large heat transfer surface due to a large conduit surface. Furthermore, by flowing the medium to be distilled in the line a good mixing and thus a more uniform temperature profile in the flowing medium as in the case of a container with stagnant liquid.

By providing a controllable connection between the two distillation regions, a demand-based overflow can take place from the first distillation zone into the second distillation zone. Further is For example, only the use of one of the two distillation sections for the distillation possible, so that the device can be used for different media. Furthermore, the separation into two distillation zones allows a separate removal of the gases produced in the course of the distillation. The second distillation zone is particularly preferably an area in which a medium with a high boiling point can be degassed.

Particularly preferably, at least one supply line for the admixing of a degassing accelerator is provided between the first distillation zone and the second distillation zone. Since part of the liquid to be separated has already been removed in the first distillation zone, less degassing accelerator is required. The degassing accelerator also allows for improved separation of the liquid to be separated. Furthermore, the degree of purity of the part of the liquid to be separated is increased and the remainder is minimized.

Two feed lines for degassing accelerators are particularly preferably provided, wherein the first feed line opens at the end of the first distillation zone and the second feed line opens at the beginning of the second distillation zone.

In order to lower the temperature required for the distillation and thus to reduce the energy required, the distillation apparatus can be operated particularly preferably at reduced pressure.

Particularly preferably, the distillation regions are arranged in a heatable container. The container can in this case define the boiler room and be thermally insulated even outside, from the outside, a tempered medium, such as hot water, hot oil or steam, can be fed. This allows a uniform temperature distribution within the container and thus a uniform heat transfer within the container.

Alternatively, the heat required for distilling may be provided by electric heating elements, such as heating coils or foils wrapped around the tubes or heating coils projecting into the interior of the tubes, tubes wound around or disposed in the heating fluid flowing through the tubes, which serve as heating elements, for example. In the form of coaxial tubes, are generated by a directly below the tubes arranged burner or directly in the medium to be distilled by ultrasound and / or microwaves.

The tubes used in the distillation apparatus may be made of a metal, plastic, glass, porcelain or ceramic, combinations also being possible. In the case of aggressive media, the pipes can also be provided with suitable coatings. Particularly preferred are heat-conductive pipes made of metal, such as copper pipes or stainless steel pipes, possibly also aluminum pipes.

Particularly preferably, the first distillation region is formed like a helix. A coil allows a compact design in conjunction with a large length. Here, the helix may also be formed by a plurality of straight pipe sections, which are connected with a corresponding bend or a curvature together to form a kind of helical shape, in particular welded, are.

Particularly preferably, the helix runs in such a way that the Coriolis force slows down the flow, the direction depending on the location of use - northern or southern hemisphere.

Particularly preferably, a plurality of gas outlet lines are provided in the first distillation zone. This allows a faster and better separation of the distilled Component of the liquid. In the case of a helical configuration of the line in the first distillation zone, the gas outlet lines can be guided to run upward in the interior of the helix, resulting in a space-saving design.

Preferably, in a helical configuration of the conduit in the first distillation zone per coil, in particular preferably from the second or third coil, a gas outlet conduit branches off, and the last gas outlet conduit branches off at the end of the last coil. The outgoing gas from the coil gas outlet can be easily guided inside the coil upwards. In this case, the individual gas outlet lines preferably branch off from the individual coils slightly offset relative to one another.

The free flow cross section in the first distillation zone is preferably greater than in the second distillation zone, but it may also be smaller or equal.

Furthermore, the gradient in the first distillation zone is preferably somewhat greater than in the second distillation zone. Particularly preferably, the gradient of the first distillation zone is at least twice as large as the gradient of the second distillation zone.

In the second distillation zone, preferably at least one gas outlet conduit is provided for gases which are heavier and at least one gas outlet conduit for gases which are lighter.

Preferably, a common gas collecting outlet pipe is provided for the gas outlet pipes of the second distillation zone over which gas is discharged, which is heavier. Particularly preferably, in the case of gases which are heavier, the gas collecting outlet is arranged lower than the line of the second distillation zone. This allows easy collection and removal of the gas.

The gas collecting outlet conduit is preferably connected to the conduit of the second distillation zone for heavier gases via the gas outlet conduits which are bent or kinked. The bent or kinked or obliquely downwardly extending configuration ensures that - even with the arrangement of the gas collecting outlet below the line of the second distillation zone - no liquid enters the gas collecting outlet.

Preferably, the gas outlet lines provided in the first distillation zone are individually led out of the vessel, and the gas outlet lines provided in the second distillation zone for the gases which are heavier are led out of the vessel via a common gas collecting outlet pipe. The gas outlet duct for lighter gases may be vented out of the tank with the gas outlet ducts of the first distillation zone. This enables separate further processing of the gases distilled in the corresponding regions, which gases may have a different purity or, in particular in the case of a gas mixture which forms, composition. However, it is also possible, for example, a plurality of individual gas outlet lines from both areas.

In the following the invention with reference to an embodiment with reference to the accompanying drawings is explained in more detail. In the drawing show:

1 is a highly schematized and not to scale shown, wound representation of the distillation apparatus according to the first embodiment, 2 is a detail view of a part of the distillation apparatus in the direction of arrow II in Fig. 1,

FIG. 3 is a perspective view of the distillation apparatus of FIG. 1; FIG.

Fig. 4 is a view of the distillation apparatus of Fig. 1 obliquely from below, and

FIG. 5 is a detail view, partially in section, of a portion of the distillation apparatus of FIG. 1. FIG.

A distillation device 1 comprises a container 2, which by means of a heating device, not shown here, formed in a separately formed boiler steam, which is introduced into the container 2, is heated, and a arranged in the container 2 line arrangement, wherein the line arrangement. 3 a plurality of supply and disposal lines are inserted into and out of the container 2. The container 2 is pressure-resistant and well insulated. The line arrangement 3 consists in the present case of copper pipes, which are good heat-conducting.

The line arrangement 3 has a distillation medium inlet line 4 into the container 2, a further, helically formed line of significantly larger diameter than the inlet line 4 forming a first distillation zone 5, different first gas outlet lines 6 branching off from the first distillation zone 5 with one of the helical lines corresponding diameter, which hereinafter also referred to as the first group of gas outlet pipes a first feed line 7 for a first degassing accelerator which terminates at the end of the first distillation zone 5, a second starting distillation zone 8 which is connected via a valve to the first distillation zone 5, and at the beginning of which a second feed line 7 '(FIG. indicated in the drawing only in Fig. 1) opens for a second degassing accelerator. From the second distillation zone 8 branches off a second group of gas outlet ducts 9, which open into a common gas collecting outlet duct 10, and a residual medium outlet duct 11.

According to a variant, a plurality of separately formed gas outlet conduits are provided corresponding to the first gas outlet conduits instead of a common gas collecting outlet conduit, which gas conduits are each led out of the container individually.

In the present case, the line forming the present, first distillation zone 5 extends downward in a helical manner with a constant cross section and a slight gradient. Each helix is formed by six straight pieces of pipe, which are welded together at the ends. From each helix branches from the end of the second helix from one of the gas outlet lines 6 from above, which are individually guided above the container 2. To illustrate the course of the height, a contour line E is drawn in the wound-up representation of FIG. 1, which in the erected state of the device lie in a horizontal plane. Furthermore, the lengths are not drawn to scale, so the second distillation zone 8 is formed significantly shorter than the first distillation zone 5. The slope of the first distillation zone 5 is at an angle α and the slope of the second distillation zone 8 at an angle ß. In the present case, the angle α is about twice as large as the angle β.

Below the last branch of a gas outlet line 6 from the first distillation zone 5, with which it ends, the line is in the radial direction led inwards and bent down about in the middle of the coil down and closed at the end. The line of the first distillation zone 5 has a constant, relatively large cross-section until the end. In the region of the line end, both the confluence of the first feed line 7 for the degassing accelerator and the beginning of the line which forms the second distillation zone 8 and at the end of the second distillation zone 8 to the residual media outlet conduit 11 are provided from opposite sides. Here, at the beginning of the line of the second distillation zone 8, said valve is arranged to control the overflow of the remaining liquid from the first distillation zone 5 into the second distillation zone 8. The remaining liquid is fed via the second supply line 7 'another degassing accelerator fed, which - depending on the application - the first and second Entgasungsbeschleuniger may be identical, is supplied via one of the supply lines 7 or T Entgasungsbeschleuniger, or possibly no degassing supplied becomes. The line of the second distillation zone 8 as well as the feed lines 7, T have a significantly smaller diameter than the line of the first distillation zone 5, wherein the diameter of the conduit forming the second distillation zone 8 to the residual media outlet line 11 is constant.

The line in the second distillation section 8 extends to increase the length present in a zig-zag shape with a slight slope, the kinks in the present case have no influence on the height profile of the line, i. the gradient is essentially constant.

In the present case, four second gas outlet lines 9 branch off from the second distillation zone 8 and open into the gas collecting outlet line 10 assigned to the second distillation zone 8 and leading out of the container 2. The second gas outlet lines 9 branch parallel to the plane E and in the upper region, present approximately tangential to the highest point of the conduit, from the conduit of the second distillation zone 8, the gas outlet conduits 9 being kinked or curved and extending first horizontally and then vertically downwards and / or alternatively obliquely downwards, then it the deeper than the second distillation section 8 arranged gas collecting outlet line 10 open from above (see Fig. 2). Here, the gas outlet conduits 9 have a smaller diameter than the conduit of the second distillation zone 8. This embodiment ensures that no liquid components get into the gas collecting outlet 10. Furthermore, it is ensured that, in particular, gases which are heavier get into the gas collecting outlet line 10.

In addition to these second gas outlet lines 9, a third gas outlet line 9 'is presently provided, via which gases which are lighter can be removed. In the present case, this third gas outlet line 9 'branches off behind the valve which separates the two distillation regions 5 and 8 from one another. The third gas outlet line can also be arranged in the end region of the second distillation region 8. Furthermore, a plurality of third gas outlet conduits may be provided in the second distillation zone 8 for the removal of gases which are lighter. The one or, if appropriate, a plurality of third gas outlet lines 9 'can also be further downstream, i. further shifted to the left in Fig. 1, branch off.

Between the third gas outlet line 9 'and the collecting outlet line 10, in which the gas outlet lines 9 are brought together, according to the present embodiment, a connecting line 9 "is arranged, so that - for example, changes in the distillation temperature - sinking gases from the third gas outlet line. 9 can enter the collection outlet line 10. The connection line 9 "is shown in the drawing only in FIG. According to a variant of the embodiment not shown in the drawing eliminates the connecting line 9 ", the rest of the structure corresponds to the previously described.

The line of the second distillation zone 8 passes directly into the residual-medium outlet line 11, which is led out of the container 2 substantially in the horizontal direction. Here, at the end of the second distillation zone 8, a diameter reduction of the line in the form of an orifice 15 is provided, which retains both a portion of the liquid residual medium, as well as prevents degassed medium from leaking uncontrollably over the residual media outlet.

The function of the distillation apparatus 1 under reduced pressure is as follows: A liquid mixture of high boiling point, referred to below as the distillation medium, is introduced into a system in which there is a negative pressure for separation into two (or possibly more individual liquids or liquid mixtures). Part of this system is the distillation device 1. About the distillation medium inlet line 4, the distillation medium enters the heated container 2. From the distillation medium inlet line 4, the liquid distillation medium enters the helical first distillation zone 5 and is in the same during the slow downflow in consequence of Heat, supported by the negative pressure, gradually degassed, ie a part of the liquid mixture evaporates. The gas, which is lighter than the remaining liquid mixture, is sucked upwards from the container 2 via the various first gas outlet lines 6, where the gas passes into downstream filters and condensers (not shown), which however are not part of the distillation device 1 , and further processed. The installation of filters in the region of the line arrangement within the container is possible in principle. At the end of the first distillation zone 5, part of the liquid mixture is vaporized. In addition, a first degassing accelerator can be fed to the liquid mixture via the first supply line 7, which acts in particular in the first distillation zone 5 and accelerates the distillation. The regulation of the overflow into the second distillation zone 8 takes place with the aid of the valve arranged at the beginning of the second distillation zone 8. In order to degas as far as possible also the remainder of the liquid mixture, which enters the second distillation zone 8, a degassing accelerator can be supplied via the second feed line T and added to the liquid mixture. Subsequently, the newly assembled liquid mixture enters the second distillation zone 8.

In this zigzag-shaped second distillation zone, which is designed to lengthen the path length, another part of the liquid mixture to be separated evaporates with the aid of the degassing accelerator, which is part of the liquid mixture in the second distillation zone. This gaseous part is guided via the second gas outlet lines 9 to the common gas manifold 10, via which the gas passes from the container 2. The remaining liquid passes through the residual media outlet 11 to the outside. In order to ensure a sufficient residence time of the liquid in the container 2 and, in order as far as possible to convey no gas through this outlet line 11 to the outside, the outlet line at the end, i. in the region of the container wall, an aperture 15. The gas discharged via the outlet line 11 is supplied to a filter and condenser in accordance with the gas discharged upward via the first gas outlet lines 6 and further processed. Of course, any other treatment of the gas is possible.

The distillation is carried out in this case to accelerate the degassing and the temperatures required for this at a negative pressure, ie in the line arrangement together with the associated lines and devices prevails over the Environment, a reduced pressure, which is usually a negative pressure to a so-called rough vacuum (1 to 300 mbar). In extreme cases, a further pressure reduction is possible.

Alternatively, degassing at normal pressure is possible with the device described above.

Furthermore, degassing can also take place without degassing accelerator with the device described above. Optionally, the supply lines 7 and / or 7 'thus also omitted.

The distillation device can also be operated in such a way, for example in the case of a heating device which is formed by electric heating elements arranged around the tubes, that heating takes place, for example, only in the second distillation region 8, and thus a distillation, in particular of a medium having a low boiling point. In this case, the medium to be distilled flows through the distillation medium inlet line 4 via the unheated first distillation zone 5 into the second, heated distillation zone 8, a degassing accelerator being admixed by one of the degassing accelerator feed lines 7 or T.

LIST OF REFERENCE NUMBERS

1 distillation device

2 containers

3 line arrangement

4 distillation medium inlet line

5 first distillation area

6 gas outlet line

7, 7 'feed line (degassing accelerator) 8 second distillation section 9, 9' gas outlet line 9 "connecting line

10 gas collecting outlet pipe

11 Remaining medium outlet line 15 Aperture

E contour line O. ß angle

Claims

claims

1. Distillation apparatus, comprising at least one first distillation zone (5) with at least one first gas outlet outlet (6), at least one second distillation zone (8) with at least one further gas outlet line (9, 9 '), wherein the distillation zones (5, 8) are connected to one another, the first distillation zone (5) is formed by a first line, the second distillation zone (8) is formed by a second line, and the two lines forming the distillation zones (5, 8) are controllably connected to one another.

2. Distillation device according to claim 1, characterized in that between the first distillation zone (5) and the second distillation zone (8) at least one supply line (7, 7 ¹ ) is provided for the admixture of a degassing accelerator.

3. Distillation apparatus according to claim 1 or 2, characterized in that a first feed line (7) at the end of the first distillation zone (5) opens, and a second feed line (7 ') at the beginning of the second distillation zone (8) opens, wherein the first and the second distillation zone (5, 8) are controllably connected to each other by a valve.

4. Distillation device according to one of the preceding claims, characterized in that the first distillation region (5) is formed by a line which is formed like a helix.

5. Distillation device according to claim 4, characterized in that a plurality of gas outlet conduits (6) are provided in the first distillation zone (5).

6. Distillation device according to one of the preceding claims, characterized in that in the second distillation region (8) a plurality of gas outlet conduits (9, 9 ') are provided, wherein in each case at least one gas outlet conduit (9 ¹ ) for gases which are lighter, and at least one gas outlet duct (9) is provided for gases which are heavier.

7. Distillation device according to one of the preceding claims, characterized in that the distillation regions (5, 8) have a different slope, wherein the slope of the first distillation zone (5) is greater than the gradient of the second distillation zone (8).

A distillation apparatus according to any one of the preceding claims, characterized in that a common gas collecting outlet duct (10) for the gas outlet ducts (9) of the second distillation zone (8), over which gas is heavier, can be discharged, and in that Gas collecting outlet (10) is arranged lower than the line of the second distillation zone (8).

9. Distillation device according to claim 8, characterized in that the gas Sammelauslassleitung (10) with the line of the second distillation zone (8) via the gas outlet lines (9) are connected, which are formed obliquely downwardly extending, bent or kinked.

10. A method for operating a distillation apparatus according to any one of the preceding claims, characterized in that the distillation device (1) is heated, and / or there is a negative pressure in the line system.