WO2013135613A1

WO2013135613A1 - Device for the rectificative separation of material mixtures

Info

Publication number: WO2013135613A1
Application number: PCT/EP2013/054842
Authority: WO
Inventors: Rolf Marr; Lukas WIESEGGER
Original assignee: Rolf Marr; Wiesegger Lukas
Priority date: 2012-03-13
Filing date: 2013-03-11
Publication date: 2013-09-19
Also published as: AT516938A5; AT516938B1

Abstract

The invention relates to a microstructured device for the rectificative separation of a material mixture, comprising a plate I which has a channel-shaped microstructure and a plate II which is attached as a mating piece for the plate I such that passages are produced for the material mixture to be rectificated. The invention is characterized in that the material which makes up both plates I and II has a thermal conductivity of 0.001 to 10 W.m^-1.K^-1. The invention also relates to the use of said microstructured device and to a method for separating material mixtures using such a device.

Description

Apparatus for the rectificative separation of mixtures

The present invention relates to an apparatus for the rectificative separation of

Mixtures of substances, in particular a microstructure apparatus.

Distillation as a method of separating hemic mixtures has long been known and well researched. The mixture to be separated is heated so that individual components boil, pass through the steam space into other parts of the apparatus and are condensed there. The distillation is used on a large scale. If the distillation is carried out for the separation of mixtures in a single apparatus by repeated evaporation and condensation in several stages, the evaporated and

Condensed streams are repeatedly brought to thermal equilibrium, it is called rectification. The respective height of an apparatus or a column results, depending on the substance mixture to be separated, from the number of necessary separation stages times the height of a theoretical separation unit, the HETP value (height equivalent of theoretical plate) or the HTU value (height of transfer unit). If many separation stages are required, suitable equipment can reach considerable heights. For example, these are 50 m and more in columns, with all the resulting problems in terms of statics and stability. There was therefore no lack of attempts by special installations in columns, the height of a single stage and thus the entire

To reduce apparatus. Ordered column packings make it possible to reduce the overall height of a single separation stage up to about 83 [mm] (Sulzer packing - type CY), K. Sattler, thermal separation process, 3rd edition, 2001, Weinheim, Wiley-VCH.

In order to be able to separate both process and energy-efficient, it is necessary to increase the mass transfer and thus to reduce the HTU value. This is where the

Microstructure technology, which greatly increases the mass transfer, the

Reduced working volume and consequently the apparatus can be miniaturized. In addition to cost reduction both in operation and in investment, this results in many other advantages such as flexibility and mobility. Especially with the separation of

Fine chemicals that are characterized by high purity, thermal or optical instability provides this new technology essential over conventional methods Advantages. In addition to a gentle and effective microstructures ensure

Processing of the substances involved also safety in the case of explosive substances due to the low working volume (hold-up).

So far, there are only a few concepts for rectification in microstructures, although most are not industrially applicable and can be classified as research. The process described in US Pat. No. 7,305,850 involves repeatedly vaporizing the mixture to be separated in microchannels, separating the vapor from the liquid, and transferring the vapor and liquid to different parts of the apparatus in which liquid and vapor are in turn contacted , The process requires equipment of high complexity, which is correspondingly expensive and error-prone in operation.

In WO 2009/080591 a miniaturized sieve tray column is described. It has been reported in separation tests of various mixtures of 12 plates or a HETP value of 10.8 mm. Disadvantages of this design, in addition to the usual disadvantages of a perforated plate column, such as non-gentle separation of substances or high pressure drop, the complex design that is necessary to produce a temperature gradient along the apparatus. Another major disadvantage is the narrow operating window in terms of throughput. The construction does not allow equalization up in the

Micro process technology usual form of scale-up. In order to achieve higher throughputs than specified by the geometry, an external parallelization of several apparatuses is necessary, which greatly increases the capital expenditure.

The present invention now provides an apparatus in the form of a

Microstructure apparatus for the rectificative separation of a mixture of substances, which has the following properties: Simple structure, cheap construction material, simple production, Easy increase of the capacity up to the industrial scale by "Equaling up", low HETP and thus high number of separation stages with low overall height.

In one aspect, the present invention provides a microstructure apparatus for the rectificative separation of a mixture of matter comprising a plate I having a Has channel-shaped micro structure, and a plate II, which is mounted as a counterpart for the plate I, such that passages for the substance to be rectified mixture result, characterized in that the material from which the two plates I and II are made each have a thermal conductivity of 0.001 to 10 Wm ^ .K ^"1 , for example 0.01 to 10 Wm ^ .K ^{" 1} .

An apparatus provided in accordance with the present invention is also referred to herein as an "apparatus according to (the present invention)".

A microstructure apparatus is an apparatus that has microstructures that

Transport processes of matter and heat influence. Microstructures are known from the microstructure principle.

By "rectificative separation" or "rectification" in a process of the present invention is the multiple; complete or partial evaporation and condensation of a mixture of substances in order to achieve separation into individual components or the enrichment of individual components to understand. Depending on the mixture, the rectification is carried out by heating the mixture to a certain temperature and / or applying a suitable pressure.

In a microstructure apparatus according to the present invention, the plates I and II, which may for example also be designed block-shaped, arranged substantially horizontally to one another. By "substantially horizontal" in an apparatus according to the present invention is meant that the plates I and II are arranged to the base so that the liquid which is to be rectified can flow over the microstructure of the plate I, eg by means of gravity The plates I and II are preferably arranged more or less vertically, for example practically perpendicular to the base surface in the apparatus, Preferably, the plates I and II are substantially parallel, for example, aligned practically parallel.

In a microstructure apparatus according to the present invention, the microstructure in plate I is shaped in its entirety in a certain way, also referred to herein as "patterned", but has no profile Connection with the plate II and its profiling the cross-section of the channel-shaped passage for the substance to be rectified mixture, in which in operation of the

Microstructure apparatus vapor and liquid are located. The surface of the plate II or its profile preferably has a distance to the liquid surface, e.g. as shown in Fig. 6c, a distance of s / 2. Depending on the material properties and throughput, s / 2 should be sufficiently large to prevent flooding of the apparatus.

An apparatus according to the present invention is thereby in another aspect

in that the plate I is semicircular, rectangular, square, trapezoidal, triangular or elliptical, for example as shown in FIG. 8.

For this purpose, for example, a semicircular, rectangular, square, trapezoidal, triangular or elliptical microchannel can be milled into a plate consisting of a material with a thermal conductivity of 0.001 to 10 Wm ^ K ¹ .

The plate II has in particular a surface which favors a vortex formation in the steam, or causes. In an apparatus according to the present invention, the plate II has no profile or the plate II has a profile.

"A profile" in a plate in an apparatus according to the present invention is intended to mean that the surface of the plate has desired, irregular or regular elevations and depressions, for example, regular elevations and depressions

For example, could have a wave-like shape, the waves

may be configured differently, e.g. For example, the waves may be sinusoidal, trapezoidal or triangular units, or semi-elliptic or semicircular units in which semicircles are formed side by side on one side of a plane, or in which semicircles are interleaved, alternately on one and the other Side of a plane are formed.

A microstructure apparatus according to the present invention is characterized in a further aspect in that the plate II is designed so that it has a horizontal wave-like profile, in particular a profile, the sinusoidal, trapezoidal, or triangular units, or semi-elliptical or semicircular units in which semicircles are respectively formed side by side on one side of a plane, or in which semicircles are formed alternately on one side and on the other side of a plane, for example as in FIG Fig. 7 is shown.

A microstructure apparatus according to the present invention further contains off and

Inlets, e.g. Drilling, for the substance to be rectified, or for the

Rectifying resultant substances or mixtures of substances, e.g. the resulting steam, the distillate, the bottoms produced by the rectification of the mixture.

The substance mixture to be rectified or the substances or mixtures produced during rectification can be heated or cooled with the aid of one or more heat exchangers which are attached at a suitable location, preferably outside the microstructure apparatus, namely outside the inlets or outlets.

The plates I and II in a microstructure apparatus according to the present invention are tightly connected to each other in operation, in particular so connected that the connection can be released without destroying the apparatus Connecting the plates I and II only from the designated inputs and outlets can enter or exit.

In particular, the plates I and II are screwed together, including, for example, to the two plates I and II perforated plates, namely plates with holes for attachments, such as glands mounted and the two plates using

Fasteners, such as e.g. Screws are tightly connected. In Fig. 1 shows by way of example how the two plates can be connected by means of such perforated plates.

Fig. 6c shows a possible embodiment of structuring or profiling of both plates in side view. In Fig. 6c mean

r _K = depth of structuring on plate I

s, a or λ = constructive dimensions of the wave structure on plate II. Regardless of the design of the panels, with or without structuring, possible base dimensions (height, width and depth) of the two panels are represented by IL, ty / tL, and b _v / b _L in Table 5 and schematically in Figure 6 (a).

Table 5

In Table 5, the index "L" refers to a disk I, the index "V" to a disk II in an apparatus according to the present invention.

In a particular embodiment, a microstructure apparatus according to the present invention is characterized in that the depth and the width of the plates I and II are from 20 to 100 mm and the length is at least 80 mm, for example up to 10000 mm.

Exemplary dimensions of an apparatus according to the present invention may also be taken from the design drawings in Figures 6 (Figures 6a to 6g) and Figures 9 (Figures 9a and 9b).

The plates in an apparatus according to the present invention are said to be made of a material having good temperature resistance, low thermal conductivity and high

Corrosion resistance exist. The material of the plate I should also a small Low thermal conductivity of the material is preferred to allow a large temperature gradient along the height of the plates, Such material includes suitable glass, suitable plastics, and suitable ceramic materials. wherein glass and plastics, in particular plastics are preferred.

Suitable plastics, suitable glass or suitable ceramic materials in an apparatus according to the present invention are plastics, glass materials or ceramic materials which are stable at the temperatures of the rectification and resistant to the mixture of substances which is to be rectified and the individual components of the substance.

Plastics with low thermal conductivity are, in particular, plastics which have a thermal conductivity of 1 μm 2 K ² and below, preferably of 0.3 μm 2 K ² and below, for example from 0.001 to 1 μm ² K ¹ .

Suitable plastics include, for example, polyolefins, polyamides, polyesters,

Polyether, polyether ether ketones and polysulfones, wherein, for example, polyether ether ketones such as PEEK and polysulfones (PSU) are particularly suitable.

Glass materials with low thermal conductivity are, in particular, those which have a thermal conductivity of 2 Wm ^ .K ^"1 , for example 1.5 Wm ^ .K ^{" 1} and below, preferably 0.3 Wm ^ .K ^"1 and below, for example from 0.001 to 2 Wm ^ .K ^"1 . Suitable glass materials include, for example, a Li-Al-silicate glass, optionally with fractions of Ce and / or Ag ions, such as FOTURAN®, or glass material of alkali aluminum silicate, eg Gorilla Glass.

Ceramic materials with low thermal conductivity are in particular those which have a thermal conductivity of 7 Wm ^ .K ^"1 and below, preferably 0.001 to 7 Wm ^ .K ^{" 1} . Suitable ceramic materials include silicate ceramics, eg: Si0 _2, etc.,

Oxide ceramics, eg: Zr0 ₂ , A1 ₂ 0 ₃ , etc., and non-oxide ceramics, eg: SiC, Si ₃ N ₄ , Diamond, etc. a. Suitable critical angle "δ" between the liquid and the plate material, eg

Polymer / glass / ceramics include, for example, critical angles of δ = 70 ° and less, preferably δ = 40 ° and less, whereby good wetting and a high surface area to the vapor can be ensured.

An apparatus according to the present invention preferably includes openings through which one can see inside the apparatus such that one can observe the microstructure of the apparatus. These openings are closed with a transparent "sight glass" which encloses the glass, eg normal window glass, but also transparent or semi-transparent plastics such as polysulfone (PSU) or polyethersulfone (PES) The sight glass can be at the front and at the opposite end of the two Plates mounted by means of perforated plates, for example screwed, for example, as shown in Fig. 1.

An apparatus according to the present invention can be designed as an amplifier column, as a stripping column, or as an amplifier and stripping column, for example according to the

FIGS. 2, 3 and 4.

When using an apparatus according to the present invention as an amplifier column according to FIG. 2 for the separation of a substance mixture G into less volatile and more volatile components, a substance mixture G is completely vaporized by the heat exchanger W2 and introduced into the gap via the opening XI. The more volatile components of the mixture G, after entering the apparatus, flow as vapor in the gap between the downwardly flowing liquid and the plate II upwards. They reach the upper end of the gap between the plates I and II. Via opening IX, the steam passes into the heat exchanger W3, where it is condensed. Part of the now liquid phase is discharged as distillate. The remaining part enters the opening VII, is introduced into the apparatus at the upper end of the plate I and flows downwards as a liquid. In turn, intensive contact between the vapor and the liquid flowing down the surface of the plate I takes place, whereby the more volatile components of the downwardly flowing liquid pass into the vapor and the less volatile components of the vapor pass into the liquid. The less volatile Components pass through opening VIII from the apparatus and are discharged as bottom product B.

When using an apparatus according to the present invention as a stripping column according to FIG. 3 for the separation of a substance mixture G in less volatile and more volatile

Components is a substance mixture G heated by the heat exchanger Wl to the boiling point at the selected pressure and introduced through the opening VII in the apparatus. The less volatile components of the mixture flow as a liquid on the surface of the vertical plate I down. They reach the lower end of the gap. Part of the liquid flowing through the opening VIII is discharged as bottom product B, the remaining part of the liquid is totally vaporized by the heat exchanger W2, introduced as vapor at the lower end of the gap between plates I and II in this gap and flows upwards as vapor , The more volatile components of the

Mixture G, after entering the apparatus, moves upwards as vapor in the gap between the liquid flowing downwards and the plate II. They reach the upper end of the gap between the plates I and II. Via opening IX, the steam passes through the heat exchanger W3, where it is condensed and discharged as distillate.

When using an apparatus according to the present invention with amplifier and

4 for the separation of a mixture G in less volatile and more volatile components, a substance mixture G is heated by the heat exchanger Wl to the boiling point at the selected pressure and introduced through the opening VI in the selected height i in the apparatus. The less volatile components of the

Substance mixtures flow as liquid on the surface of the vertical plate I down. They reach the lower end of the gap. Part of the liquid flowing through the opening VIII is discharged as bottom product B, the remaining part of the liquid is totally vaporized by the heat exchanger W2, introduced as vapor at the lower end of the gap between plates I and II in this gap and moves behind as vapor above. In this case, due to the surface structure of the plate II, an intensive contact between the vapor and the surface of the plate I flowing downwards

Liquid instead, causing the more volatile components of the flowing down

Liquid into the vapor and the less volatile components of the vapor go into the liquid. As a result, the liquid arriving at the lower end of the gap no longer contains the more volatile components or only in a very small amount. The more volatile components of the composition G, after entering the apparatus, move upwards as vapor in the gap between the downwardly flowing liquid and the plate II. They reach the upper end of the gap between the plates I and II. Via opening IX, the steam passes through the heat exchanger W3, where it is condensed. Part of the now liquid phase is discharged as distillate. The remaining part passes into the opening VII and is introduced into the apparatus at the upper end of the plate I and flows downwards as a liquid. In turn, intensive contact between the vapor and the liquid flowing down the surface of the plate I takes place, whereby the more volatile components of the downwardly flowing liquid pass into the vapor and the less volatile components of the vapor pass into the liquid.

In operating a microstructure apparatus according to the present invention, there is continuous contact between the downflowing liquid and the upwardly flowing vapor so that particularly low HETP values of 30 mm and below can be achieved. The HETP value here means the height of a theoretical separation unit (height equivalent of theoretical plate), which depends on various conditions and which is determined experimentally. Due to the intensive contact of

Liquid and vapor is achieved a very good separation of the upwardly flowing more volatile components from the flowing down less volatile components of the mixture, so that in an apparatus according to the invention a small height is achieved with good separation efficiency.

The capacity of the apparatus according to the invention is determined by the width b and the number of pairs of opposing plates I and II. The quality of the separation of the substance mixture is determined by the height of the plate pairs H. It correlates with the number of theoretical plates of the apparatus.

In a further aspect, the present invention provides an apparatus according to

present invention, in which the plates I and II parallelizations have horizontal (micro) structures, namely in that there are multiple channels / passages in the plates I and II plates in the apparatus, or that there are several plates I and II plates and multiple channels / passages in the apparatus.

In an apparatus according to the present invention, in contrast to

discontinuous contacting of previous methods by continuous contact of liquid and vapor to realize a gentle separation with lower pressure drop and higher separation efficiency.

The continuous contact between the downwardly flowing liquid and the upwardly flowing vapor, an intensive mass transfer and thus a rapid adjustment of the liquid-vapor balance is achieved. As a result, a low HETP is achieved and an apparatus of given height has particularly many separation stages or an apparatus with a certain number of separation stages has low height.

In a further aspect, the present invention provides an apparatus for the rectificative separation of a liquid mixture characterized by

Combination of the features that it comprises at least one flat plate I and at least one plate II, wherein liquid flows down along the at least one flat plate I in the form of a film flow and steam on the surface of, the flat plates I opposite, vertical plates II With smooth surface structure, which preferably causes a vortex formation in the steam, flows upward, so that there is a continuous contact between the downflowing liquid and the upwardly flowing vapor, so that a HETP of less than 30 mm is achieved.

Description of the pictures

Fig. 1 shows an overall schematic view of a microstructure apparatus according to the present invention.

Fig. 2 shows a schematic view of a microstructure apparatus according to the present invention as an amplifier column. Fig. 3 shows a schematic view of a microstructure apparatus according to the present invention as a stripping column.

Fig. 4 shows a schematic view of a microstructure apparatus according to the present invention as an amplifier and output column, wherein the output column below the

Amplifier column is attached.

Fig. 5 shows a schematic representation of a vacuum rectification according to Example 2 of the present application.

The figures 6 show schematically possible execution details of

Microstructure apparatus according to the present invention:

Fig. 6a shows schematically a possible steam distributor in the event that several units of plates I and II with profiles and multiple channels in the

Microstructure apparatus are present. In this case, the diffuser area baffles, or no baffles included (not shown).

Fig. 6b shows schematically a bionic system for liquid distribution in the case where several units of plates I and II with profiles and multiple channels in the

Microstructure apparatus are present ..

Fig. 6c shows schematically a detail of the microstructure apparatus of Fig. 9a, namely the detail "DET" .The dimensions are given in mm.

Fig. 6d shows schematically a microstructure apparatus according to the present invention, showing the two plates I and II in oblique view.

Fig. 6e shows schematically a plate II according to the present invention with the

Wave structure in an oblique angle.

Fig. 6f shows schematically the front view of plates I and II according to the present invention.

Fig. 6g shows schematically a plate I according to the present invention in an oblique view.

Fig. 7 shows schematically profile variants of the surface of the plate II according to the present invention, namely from left to right wave structures which are sinusoidal, trapezoidal, triangular, or elliptical or circular. Fig. 8 shows various designs (structuring) of the plate I according to the present invention and thus forms of the microchannel formed on the plate I.

Figures 9 show schematically constructive representations of a

Microstructure apparatus according to the present invention:

Fig. 9a shows schematically a front view. All sizes are in "mm".

Fig. 9b shows schematically a side view. All sizes are in "mm".

Figures 10 show schematically constructive representations of a

Microstructure apparatus according to the present invention for higher throughputs with multiple channels and profiles on plates I and II:

Fig. 10a shows schematically the plate II with an amplifier column (top) and a

Output column below.

Fig. 10b shows schematically the plate I, wherein the amplifier column (top) and the

Output column below are in operation.

Fig. 10c shows schematically the plate I, wherein only one amplifier column or a

Drive column is in operation.

In the figures Fig. 1 to Fig. 10 mean

I plate I according to the present invention

II plate II according to the present invention

III steam inlet area

IV wave structure

VI opening (bore) inlet

VII opening (bore) return

VIII liquid outlet area

IX steam outlet opening (bore)

X steam outlet area

XI steam inlet opening (hole)

XII fluid outlet port (bore)

B bottom product

F liquid D distillate

DA steam

DB nozzle area

DE steam inlet

DET detailed view (see FIG. 6c)

DF diffuser area

DP steam outlet

E evacuation

FA fluid outlet

FE liquid entry

G feed mixture

h height

LP perforated plate

MK microchannels

μ Apparatus according to the present invention

R return

R _s bottom return

r _K depth of structuring on plate I

s, a, λ each design dimensions of the shaft structure on plate II (in mm)

SCH sight glass

t temperature

Var. Ii Variation 1 of plate I: semicircular

Var. 21 Variation 2 of plate I: square, rectangular

Var. 3i Variation 3 of plate I: trapezoidal

Var. 41 Variation 4 of the plate I: triangular

Var. 5i Variation 5 of plate I: elliptical

Var. l _n Variation 1 of plate II: sinusoidal

Var. 2 _n Variation 2 of plate II: trapezoidal

Var. 3n Variation 3 of plate II: triangular

Var. 4n Variation 4 of plate II: elliptical or circular units on one side of a plane next to each other Var. 5n Variation 5 of plate II: elliptical or circular units adjacent to one another, alternately on one side and on the other side of a plane

VG distribution geometry

W heat exchanger

1V / 1L, ty tL, and by / bL denote basic dimensions (height, width and depth) of the two plates (plate II with index "V", plate I with index "L"

In the following, examples of the construction of an apparatus according to the present invention and examples of its use for performing rectifications will be given.

example 1

An apparatus according to the present invention is outlined in FIG. Its application can be carried out as an amplifier column according to FIG. 2 or as a stripping column according to FIG. 3.

An apparatus according to the present invention can be realized from the following components:

Plate I and plate II are arranged so that their media leading surfaces (smooth or profiled) as shown in Fig. 6c at a selectable distance s / 2 are opposite. The holes XI of the plate II and XII of the plate I are in a vertical position at the bottom of the apparatus. Thus, the liquid outlet portion VIII and the steam inlet portion III are adjacent to each other. The holes VII of the plate I and IX of the plate II are therefore located at the head of the apparatus. The heights of plates II and I, I _v and I _L are usually the same and can be chosen according to Table 5. While the widths by and bL are within the range given in Table 5, the depths are based on the choice of throughput. The length h _{3 of} the contact zone of the phases, consequently the amplifier or output column, results from the choice of the substance mixture. This length determines roughly the height of the plates II and I (ly and 1L) and thereby the height of the apparatus. Figures 6 (Figures 6a to 6g), Figures 7, 8, Figures 9 (Figures 9a and 9b) and Table 5 illustrate structural details of the apparatus.

_p ee _t xr _i mn 16

In an apparatus as described in Example 1 is a mixture consisting of

Methanol and water introduced in the specified ratios and in the

given temperatures, the following separation is carried out. The were

Ratios of methanol and water at VIII and VII determined by density measurement.

From the ratios of the number of plates and thus the HETP were determined on the known boiling curve of methanol and water (system pressure: 1 atm). The results are summarized in Table 1:

Table 1: Results Rectification CH ₃ OH / H ₂ O - Amplifier column - according to Example 1

Temperature WCH30H number

Mixture G

m [° C] [g / g] of

HTU

theoretiTyp

V

Inlet WCH30H plate II tl t ₈ t ₂ BD [mm]

[g / min] [g / g] stages

( ^η _ώ )

1 0.509 0.501 79.35 63.35 44.2 0.699 0.901 1.31 51.87 sine

Sine

2 0.651 0.501 79.59 68.48 67.39 0.677 0.884 1.16 58.55

SZ

3 0,696 0,501 79,37 65,32 32,12 0,686 0,87 0,995 68,34 smooth

Example 2

An apparatus according to the present invention is outlined in FIG. Its application can be carried out as an amplifier column according to FIG. 2 or as a stripping column according to FIG. 3. The apparatus according to the present invention can be realized, for example, from the following components:

Plate I and Plate II are arranged so that their media leading surfaces (smooth or profiled) as shown in Figure 6c at a selectable distance s / 2

face. The holes XI of the plate II and XII of the plate I are in a vertical position at the bottom of the apparatus. Thus, the liquid outlet portion VIII and the steam inlet portion III are adjacent to each other. The holes VII of the plate I and IX of the plate II are therefore located at the head of the apparatus. Bore VI on the plate I, depending on the choice of the length of the amplifier column h ₂ in a thereby resulting vertical distance, length of the output column h _1; be positioned to the liquid outlet area VIII. The heights of plates II and I, I _v and I _L are usually the same and can be chosen according to Table 5. While the widths b _v and bL are in the range according to Table 5, the depths are determined by the choice of the throughput. The length of the contact zone of the phases (tu + t ^), consequently the amplifier and output column, results after the choice of the substance mixture. This length determines to a large extent the height of the plates II and I (l _v and 1 _L ) and thereby the height of the apparatus. Figures 6 (Figures 6a to 6g), Figures 7, 8, Figures 9 (Figures 9a and 9b) and Table 5 illustrate structural details of the apparatus.

In an apparatus as described in Example 2, a mixture of methanol and water in the specified proportions is introduced and in the

given temperatures, the following separation is carried out. The were

Ratios of methanol and water at VIII and VII determined by density measurement. From the ratios were determined on the known boiling curve of methanol and water, the number of separation stages and thus the HETP (system pressure: 1 atm): The

Results are summarized in Table 2:

TABLE 2 Results Rectification CH ₃ OH / H ₂ O - according to Example 2

It is clearly evident from Table 2 that the present invention far surpasses the prior art results. Sotowa reports a HETP value of 40 [mm] in the separation of a methanol / water mixture (K.-I. Sotowa, K.

Kusakabe, 4th European Congress of Chemical Engineering, Topic 6, Granada, September, 2003). However, this value resulted from the calculation, whereby only one separation step was achieved. Consequently, obtaining 40 [mm] at multiple stages is questionable. Exe _p _{r i} men _t

Also, 40 [mm] were achieved by Tonkovich (A. L. Tonkovich, L. Silva, R. Arora, T. Hickey, AIKhE Spring National Meeting, Atlanta, GA, April 2005). However, these results are doubted in the circle of experts, as already mentioned above.

In an apparatus as described in Example 2, a mixture of cyclohexane and n-heptane is introduced in the proportions indicated and the following separation is carried out at the indicated pressures and temperatures

(System pressure: 1 atm). The results as shown in Table 3 were obtained.

Table 3: Results of rectification C ₆ H ₁₂ / C ₇ H ₁₆ - according to Example 2

Example 3

Here, the apparatus of Example 2 is used and the system as shown in Fig. 5, evacuated. By generating a negative pressure via a water jet at the end of the system, an operating pressure of up to 0.01 [bar] can be set.

In an apparatus as described in Example 3, a mixture of N, N-dimethylformamide (DMF) and water is introduced in the proportions indicated and carried out at the indicated pressures and temperatures, the following separation (system pressure: 0, 1 bar). Results were obtained as shown in Table 4:

Table 4: Results of rectification C ₃ H ₇ NO / H ₂ O - according to Example 3

Temperature WH20

Mixture G

[° C] [g / g] HETP

Inlet WH20 [mm] ti t ₈ te BD

[g / min] [g / g]

1 0.6821 0.5491 61.14 55.66 67.13 0.154 0.549 2.59 73.88

2 0.4565 0.5491 62.42 51.37 75.68 0.018 0.549 3.79 50.35

3 0.5169 0.2132 60.11 53.90 69.80 0.071 0.383 1.33 143.82 Example 4

Based on the illustrations 10 (10a, 10b and 10c) is the constructive

Design of an apparatus for higher throughputs. This apparatus is suitable for the laboratory, pilot or production scale. It can be assumed from the construction of Example 1 or 2 and it will be the (micro) structures of

Phase contact zone according to Figure 6 parallelized. This procedure allows 2 to implement> 1000 such (micro) structures, whereby throughputs of 60 g / h to 100 kg / h can be realized. For uniform distribution of the liquid in the (micro) structures at the head and inlet of the apparatus, a bionic system according to Fig. 6b is used. For the uniform distribution of the steam in the (micro) structures at the bottom of the apparatus, a specially developed steam distributor according to Fig. 6a, which shows the structural design of this manifold schematically.

Claims

claims

1. A microstructure apparatus for the rectificative separation of a mixture comprising a plate I having a channel-shaped microstructure, and a plate II, which is mounted as a counterpart for the plate I, such that passages for the mixture to be rectified, thereby characterized in that the material from which the two plates I and II are made, each having a thermal conductivity of 0.001 to 10 Wm ^ .K ¹ .

2. A microstructured apparatus according to claim 1, wherein liquid substance mixture to be rectified is guided along the plate I in the form of a film flow.

3. Microstructure apparatus according to one of claims 1 or 2, wherein steam is guided along the plate II in the opposite direction of the film flow of the liquid mixture.

4. Microstructure apparatus according to one of claims 1 to 3, characterized in that the plate II has a surface structure which favors a vortex formation in the vapor.

5. Microstructure apparatus according to one of claims 1 to 4, characterized in that the channel-shaped microstructure in the plate I in the form of a rectangular, square, semicircular, trapezoidal, triangular or elliptical passage is formed.

6. Microstructure apparatus according to one of claims 1 to 5, characterized in that the plate II designed such that it has a horizontal, wave-like profile.

7. Microstructure apparatus according to claim 6, characterized in that the profile

Sinusoidal, trapezoidal or triangular units, or semi-elliptical or semicircular units in which semi-circles or semi-ellipses are each formed on one side of a plane next to each other, or in which semicircles or Semi-ellipses to each other, alternately formed on one side and on the other side of a plane having.

8. Microstructure apparatus according to one of claims 1 to 7, characterized in that there are a plurality of channels / passages in the plates I and II plates in the apparatus.

9. Microstructure apparatus according to one of claims 1 to 7, characterized in that there are a plurality of plates I and II plates and a plurality of channels / passages in the apparatus.

10. A microstructure apparatus according to any one of claims 1 to 9, characterized in that are used as construction materials for the plates I and II plastics having a thermal conductivity of 1 Wm ^ .K ^"1 and below, in particular polyolefins, polyamides, polyesters, polyethers, Polyether ether ketones, polysulfones and

Polyethersulfone, especially polyether ether ketone (PEEK) or polysulfone (PSU).

11. A microstructure apparatus according to any one of claims 1 to 9, characterized in that glass materials having a thermal conductivity of 2 Wm ^ .K ^"1 , in particular 1.5 Wm ^ .K ^{" 1} and below, especially quartz glass, a Li Al-silicate glass, optionally with proportions of Ce and / or Ag ions, or glass material of alkali aluminum silicate can be used.

12. Microstructure apparatus according to one of claims 1 to 9, characterized in that a ceramic material with a thermal conductivity of 7 Wm ^"1 K ^{" 1} and below is used as the construction materials.

13. Use of a microstructure apparatus according to any one of claims 1 to 12 in the rectificative separation of a substance mixture as an amplifier column, as a stripping column, or as an amplifier and output column.

14. A method for the rectificative separation of a mixture of substances, characterized in that a microstructure apparatus according to one of claims 1 to 12 is used. A method according to claim 13, characterized in that the rectificative separation at pressures of 0.001 mbar to 5 bar and / or at temperatures of 20 ° C to 250 ° C is performed.