Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D1/00—Evaporating
  • B01D1/22—Evaporating by bringing a thin layer of the liquid into contact with a heated surface
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D1/00—Evaporating
  • B01D1/26—Multiple-effect evaporating
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
  • B01D3/14—Fractional distillation or use of a fractionation or rectification column
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F28—HEAT EXCHANGE IN GENERAL
  • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
  • F28D9/00—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F28—HEAT EXCHANGE IN GENERAL
  • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
  • F28D9/00—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
  • F28D9/0031—Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one heat-exchange medium being formed by paired plates touching each other
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F28—HEAT EXCHANGE IN GENERAL
  • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
  • F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
  • F28F21/06—Constructions of heat-exchange apparatus characterised by the selection of particular materials of plastics material
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F28—HEAT EXCHANGE IN GENERAL
  • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
  • F28D21/00—Heat-exchange apparatus not covered by any of the groups F28D1/00 - F28D20/00
  • F28D2021/0019—Other heat exchangers for particular applications; Heat exchange systems not otherwise provided for
  • F28D2021/0061—Other heat exchangers for particular applications; Heat exchange systems not otherwise provided for for phase-change applications
  • F28D2021/0063—Condensers
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F28—HEAT EXCHANGE IN GENERAL
  • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
  • F28F2210/00—Heat exchange conduits
  • F28F2210/02—Heat exchange conduits with particular branching, e.g. fractal conduit arrangements
• • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
  • F28—HEAT EXCHANGE IN GENERAL
  • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
  • F28F2260/00—Heat exchangers or heat exchange elements having special size, e.g. microstructures
  • F28F2260/02—Heat exchangers or heat exchange elements having special size, e.g. microstructures having microchannels

Definitions

• the present invention relates to an apparatus for the rectificative separation of
• 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
• Fine chemicals that are characterized by high purity, thermal or optical instability provides this new technology essential over conventional methods Advantages.
• Fine chemicals that are characterized by high purity, thermal or optical instability provides this new technology essential over conventional methods Advantages.
• Fine chemicals that are characterized by high purity, thermal or optical instability provides this new technology essential over conventional methods Advantages.
• Fine chemicals that are characterized by high purity, thermal or optical instability provides this new technology essential over conventional methods Advantages.
• a gentle and effective microstructures ensure that are characterized by high purity, thermal or optical instability.
• 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.
• 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
• Microstructures are known from the microstructure principle.
• 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.
• the rectification is carried out by heating the mixture to a certain temperature and / or applying a suitable pressure.
• the plates I and II which may for example also be designed block-shaped, arranged substantially horizontally to one another.
• 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.
• 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.
• s / 2 should be sufficiently large to prevent flooding of the apparatus.
• the plate I is semicircular, rectangular, square, trapezoidal, triangular or elliptical, for example as shown in FIG. 8.
• 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.
• 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
• the waves may be configured differently, e.g.
• 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 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.
• 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
• 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.
• Fig. 6c mean
• the index "L” refers to a disk I
• the index "V” to a disk II in an apparatus according to the present invention.
• a microstructure apparatus 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
• 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 ⁇ m 2 K 2 and below, preferably of 0.3 ⁇ m 2 K 2 and below, for example from 0.001 to 1 ⁇ m 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.
• non-oxide ceramics eg: SiC, Si 3 N 4 , Diamond, etc. a.
• Suitable critical angle " ⁇ " between the liquid and the plate material eg
• An apparatus 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)
• PSU polysulfone
• PES polyethersulfone
• 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
• 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.
• 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 ,
• 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.
• 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.
• 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
• HETP value 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.
• the present invention provides an apparatus according to
• 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.
• the present invention provides an apparatus for the rectificative separation of a liquid mixture characterized by
• 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.
• 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.
• the diffuser area baffles, or no baffles included are present.
• 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 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 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
• Fig. 10b shows schematically the plate I, wherein the amplifier column (top) and the
• Fig. 10c shows schematically the plate I, wherein only one amplifier column or a
• Fig. 1 to Fig. 10 mean
• 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
• FIG. 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.
• 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.
• 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.
• Example 1 In an apparatus as described in Example 1 is a mixture consisting of
• Ratios of methanol and water at VIII and VII determined by density measurement.
• FIG. 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
• the holes XI of the plate II and XII of the plate I are in a vertical position at the bottom of the apparatus.
• 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.
• 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
• Example 2 the apparatus of Example 2 is used and the system as shown in Fig. 5, evacuated.
• an operating pressure of up to 0.01 [bar] can be set.
• 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.
• a bionic system according to Fig. 6b is used for uniform distribution of the liquid in the (micro) structures at the head and inlet of the apparatus.
• a specially developed steam distributor according to Fig. 6a which shows the structural design of this manifold schematically.

Landscapes

• Engineering & Computer Science (AREA)
• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Physics & Mathematics (AREA)
• Thermal Sciences (AREA)
• Mechanical Engineering (AREA)
• General Engineering & Computer Science (AREA)
• Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
• Extraction Or Liquid Replacement (AREA)

Priority Applications (1)

Applications Claiming Priority (2)

Publications (1)

Family

ID=47844340

Family Applications (1)

Country Status (2)

Citations (5)

• 2013
  • 2013-03-11 WO PCT/EP2013/054842 patent/WO2013135613A1/fr not_active Ceased
  • 2013-03-11 AT ATA9001/2013A patent/AT516938B1/de not_active IP Right Cessation

Patent Citations (5)

Non-Patent Citations (3)

Also Published As

Similar Documents

Legal Events