EP1165218B1 - Dispositif permettant de melanger et de faire reagir des melanges gazeux ou liquides a plusieurs phases et son utilisation - Google Patents

Dispositif permettant de melanger et de faire reagir des melanges gazeux ou liquides a plusieurs phases et son utilisation Download PDF

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Publication number
EP1165218B1
EP1165218B1 EP00902646A EP00902646A EP1165218B1 EP 1165218 B1 EP1165218 B1 EP 1165218B1 EP 00902646 A EP00902646 A EP 00902646A EP 00902646 A EP00902646 A EP 00902646A EP 1165218 B1 EP1165218 B1 EP 1165218B1
Authority
EP
European Patent Office
Prior art keywords
mixing
space
liquid
mixer
chamber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP00902646A
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German (de)
English (en)
Other versions
EP1165218A1 (fr
Inventor
Werner Breuer
Frieder Heydenreich
Günther JEROMIN
Helmut Judat
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bayer AG
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Bayer AG
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Filing date
Publication date
Application filed by Bayer AG filed Critical Bayer AG
Publication of EP1165218A1 publication Critical patent/EP1165218A1/fr
Application granted granted Critical
Publication of EP1165218B1 publication Critical patent/EP1165218B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
    • B01F25/3142—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
    • B01F25/31425—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction with a plurality of perforations in the axial and circumferential direction covering the whole surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
    • B01F25/3142—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S261/00—Gas and liquid contact apparatus
    • Y10S261/75—Flowing liquid aspirates gas

Definitions

  • the invention relates to a device for mixing and reacting multiphase gaseous and liquid mixtures, with homogeneously immiscible liquid homogeneous Solutions with homogeneous solutions in which several solid or liquid substances or several gases are dissolved in intensive contact with each other, and a use of this device and manufactured using the device Diphenyl carbonate and polycarbonate.
  • stirred kettles or mixers can not be arbitrary enlarge, since often a chemical reaction takes place during mixing, so that during the mixing process in the reactor mixing and / or reaction enthalpy is released or is needed.
  • the interior of the reactor is an additional heat exchanger necessary because the ratio of heat exchange area to reactor volume with increasing stirred tank radius is getting smaller.
  • the stirred tank volume reduced by expanding the number of stirred tanks or the heat transfer by attaching additional heat exchangers in the secondary flow be intensified.
  • the invention is therefore based on the object, the known and described in more detail above Device for mixing and reacting multiphase gaseous and to improve liquid mixtures so that with little design effort small mixer is provided, without shaft bearings and shaft bushings needs to avoid the disadvantages described above. Of further the quality of the mixture should be improved.
  • the teaching of the invention provides that the transition between the cylindrical Space and the tapered cylindrical chamber has sharp edges.
  • the first stream of liquid enters the nozzle mixer through the cylindrical chamber towards the conical space, the second stream perpendicular to the middle cylindrical chamber of the nozzle mixer.
  • the vertical entry of the second Solution in the nozzle mixer takes place via several openings that follow one further teaching of the invention in the inner wall of the chamber evenly over the Circumference are arranged on a line.
  • the openings preferably run perpendicular or at any flat angle to the longitudinal axis of the chamber. This significantly increases the mixing intensity and the reaction rate.
  • Part of the homogeneous solutions from solid, liquid and / or gaseous Fabrics can be placed in one or more jacket mixers installed in front of the nozzle mixer getting produced.
  • Each jacket mixer has a cylindrical one Mixing room through which the homogeneous liquid is passed and it is a large number of inlet pipes arranged symmetrically around the mixing room for introducing the second liquid or gas to be dissolved into the jacket mixer intended.
  • means for pulse-like entry of the Liquid or gas in the jacket mixer can be provided to the degree of mixing continue to improve.
  • Another teaching of the invention is the use of the aforementioned device for mixing aqueous alkaline phenolate, bisphenolate solutions or other polyvalent phenolate solutions with dissolved in the solvent solid, liquid and / or gaseous substances.
  • Another teaching of the invention relates to diphenyl carbonate and polycarbonate, each manufactured according to the phase interface process from one by mixing heterogeneous mixture produced in the device according to the invention from a aqueous alkaline phenolate or bisphenolate solution with solution in dichloromethane gaseous or liquid phosgene, the mixture being a very small Has residual phenylpiperidyl urethane content of ⁇ 20 ppm.
  • a cascade of four stirred tanks with a total volume of 23 m 3 is flowed through by an aqueous reaction mixture at 30 ° C with a throughput of 4,500 kg / h, phosgene and dichloromethane being fed continuously into the first reactor.
  • the aqueous phenolate solution is also continuously produced in a mixing vessel connected upstream of the first stirred tank in the cascade.
  • reaction mixture is after the fourth stirred tank in a cascade Separation container separated into two phases, the organic phase cleaned, then the solvent and finally the diphenyl carbonate distilled.
  • reaction mixture is now through the invention with the same throughput Device has been promoted, the solution in the jacket mixer was continuously produced by phosgene in dichloromethane.
  • the watery Phenolate solution was continuously produced in a mixing kettle.
  • reaction to the diphenyl carbonate was carried out in a nozzle mixer according to the invention from, the processing and recovery of the diphenyl carbonate exactly as with The process was carried out using the cascade of stirred tanks.
  • the proportion of Phenylpiperidyl urethane can be safely reduced to values below 20 ppm, thereby better quality of the diphenyl carbonate could be achieved.
  • nozzle mixer In Fig. 1 the nozzle mixer is shown, the cylindrical central space for Mixing two solutions serves.
  • the four-part nozzle mixer D preferred in the exemplary embodiment shown contains a cylindrical space 1 into which a first solution F 1 enters.
  • a second solution F 2 flows through the cylindrical space 2 into a central cylindrical chamber 3.
  • a conical space 4 serves as an outlet.
  • the central chamber 3 has a smaller diameter than the cylindrical space 1 and the transition between room 1 and chamber 3 is provided with sharp edges. With the help of the conically widening space 4 of the nozzle mixer D, it is possible to keep the pressure loss in the system low.
  • the liquid for example the solution of phosgene in dichloromethane F 1
  • the second solution for example the phenolate solution F 2
  • the second solution is introduced into the cylindrical chamber 3 via openings 5 and mixed with the solution flowing perpendicularly therefrom from the room 1 and subjected to the reaction.
  • the openings 5 are in a line on the cylindrical casing of the central chamber.
  • the cylindrical mixing chamber 2 shows a cylindrical jacket mixer M to be connected upstream of the nozzle mixer D.
  • the cylindrical mixing chamber has an outer annular space and inlet pipes are designed as bores in the reactor wall.
  • the bores in the reactor wall preferably run at a flat angle to the flow direction of the reactor. An angle of 45 ° has proven to be particularly advantageous.
  • the jacket mixer has a cylindrical mixing space 6, the wall of which is provided with a plurality of bores 7, of which only the ring-shaped bores 7 near the entry E 1 are provided with reference numerals for the sake of clarity.
  • the holes in the mixer wall are arranged in a ring, whereby expediently the holes evenly over the circumference of each ring are distributed.
  • a particularly good mixture results when eight holes are arranged on each ring and the holes each adjacent rings in the direction of flow at an angle of 45 ° to each other are staggered.
  • the length of the jacket mixer M evenly distributed rows of holes, rings 7A, 7B and 7C, arranged, of which for the sake of clarity only the left three rings closer are designated.
  • Each ring 7A, 7B, 7C preferably has eight bores 7 and they are the openings of two adjacent rings 7A, 7B and 7B, 7C, respectively arranged at 45 ° to each other. In this way, an optimal Mixing in the interior of the mixing chamber 6 of the jacket mixer M is achieved.
  • a first homogeneous liquid such as dichloromethane
  • a first homogeneous liquid is fed into the reactor space 6 of the jacket mixer M by the entry E 1 .
  • the second component to be mixed such as gaseous or liquid phosgene
  • the second component to be mixed is passed into an annular space 8 surrounding the mixing space 6 and introduced into the liquid, preferably in pulsed fashion, through the bores 7.
  • the bores 7 are arranged at an angle of 45 ° to the direction of flow of the liquid. In this way, an optimal mixing of liquid with gas or another liquid can be achieved.
  • FIG. 3 shows a preferred arrangement of the mixers of the device according to the invention, the jacket mixer M being followed by a first heat exchanger WT 1 and the nozzle mixer D being followed by a second heat exchanger WT 2 . In this way, the maintenance of the required mixing and reaction temperature is reliably ensured.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Polyesters Or Polycarbonates (AREA)
  • Accessories For Mixers (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)

Claims (21)

  1. Dispositif permettant de mélanger et de faire réagir des mélanges gazeux ou liquides à plusieurs phases, des solutions liquides homogènes non miscibles étant mises en contact intensif avec des solutions homogènes dans lesquelles plusieurs substances solides ou liquides ou plusieurs gaz sont dissous, caractérisé par un éducteur (D) comme mélangeur et réacteur avec un espace cylindrique (1) pour l'entrée de la première solution, au moins une chambre cylindrique (3) rétrécie par rapport à l'espace cylindrique (1), dans laquelle ont lieu le mélange et la réaction d'au moins deux solutions, la transition entre l'espace cylindrique (1) et la chambre cylindrique rétrécie (3) présentant des arêtes vives, un espace cylindrique (2) disposé perpendiculairement à l'espace (1) pour l'arrivée de la deuxième solution, un espace (4) pour la sortie hors de l'éducteur (D) des solutions mélangées et ayant réagi.
  2. Dispositif suivant la revendication 1, caractérisé en ce que la section de l'espace (4) s'élargit en forme de cône dans le sens de l'écoulement.
  3. Dispositif suivant l'une des revendications 1 ou 2, caractérisé en ce que plusieurs ouvertures (5) disposées essentiellement perpendiculairement au sens de l'écoulement de la première solution sont prévues dans la paroi de la chambre (3) pour l'entrée de la deuxième solution dans la chambre (3).
  4. Dispositif suivant la revendication 3, caractérisé en ce que les ouvertures (5) dans la paroi intérieure de la chambre (3) sont alignées régulièrement à la périphérie.
  5. Dispositif suivant la revendication 4, caractérisé en ce que les ouvertures (5) s'étendent perpendiculairement à l'axe longitudinal de la chambre (3).
  6. Dispositif suivant la revendication 4, caractérisé en ce que les ouvertures (5) forment un angle quelconque par rapport à l'axe longitudinal de la chambre (3).
  7. Dispositif suivant l'une des revendications 1 à 6, caractérisé en ce qu'au moins un mélangeur à chemise (M) est placé en amont de l'éducteur (D), dans lequel des substances gazeuses ou liquides peuvent être mélangées avec des substances liquides.
  8. Dispositif suivant la revendication 7, caractérisé en ce que le mélangeur à chemise (M) présente un espace de mélange cylindrique (6) à travers lequel le liquide homogène est envoyé et en ce qu'un grand nombre de tuyaux d'entrée sont disposés symétriquement autour de l'espace de mélange pour l'introduction dans le mélangeur à chemise (M) du deuxième liquide ou du gaz à dissoudre.
  9. Dispositif suivant la revendication 8, caractérisé en ce que le dispositif présente des moyens pour l'introduction pulsée des composants à mélanger.
  10. Dispositif suivant l'une des revendications 7 à 9, caractérisé en ce que l'espace de mélange cylindrique (6) présente un espace annulaire extérieur (8) et en ce que les tuyaux d'entrée sont réalisés sous la forme de trous (7) dans la paroi du réacteur.
  11. Dispositif suivant la revendication 10, caractérisé en ce que les trous (7) sont disposés en forme d'anneau dans la paroi de l'espace de mélange (6).
  12. Dispositif suivant la revendication 11, caractérisé en ce que les trous (7) sont répartis régulièrement à la périphérie de chaque anneau (7A, 7B, 7C).
  13. Dispositif suivant la revendication 12, caractérisé en ce que les trous (7) d'anneaux adjacents respectifs (7A, 7B ou 7B, 7C) sont décalés l'un par rapport à l'autre dans le sens de l'écoulement.
  14. Dispositif suivant la revendication 13, caractérisé en ce que chaque anneau (7A, 7B, 7C) présente huit trous (7) et en ce que les trous (7) d'anneaux adjacents (7A, 7B ou 7B, 7C) sont décalés de 45° l'un par rapport à l'autre.
  15. Dispositif suivant l'une des revendications 8 à 14, caractérisé en ce que les trous (7) forment un angle plan par rapport au sens de l'écoulement.
  16. Dispositif suivant la revendication 15, caractérisé en ce que l'angle est compris entre 30 et 60°.
  17. Dispositif suivant la revendication 16, caractérisé en ce que l'angle est de 45°.
  18. Dispositif suivant l'une des revendications 1 à 17, caractérisé en ce qu'un échangeur de chaleur (WT) est placé en amont et/ou en aval de l'éducteur (D) et le cas échéant du mélangeur à chemise (M).
  19. Utilisation du dispositif suivant l'une des revendications 1 à 18 pour le mélange de solutions aqueuses alcalines de phénolate, bisphénolate ou d'autres solutions multivalentes de phénolate avec les substances solides, liquides et/ou gazeuses dissoutes dans le solvant.
  20. Carbonate de diphényle, pouvant être fabriqué selon le procédé interfacial à partir d'un mélange hétérogène préparé dans un dispositif suivant l'une des revendications 1 à 18 d'une solution aqueuse de phénolate avec du phosgène gazeux ou liquide dissous dans le dichlorométhane, caractérisé par une très petite teneur résiduelle <20 ppm en phénylpipéridyluréthanne .
  21. Polycarbonate, pouvant être fabriqué selon le procédé interfacial à partir d'un mélange hétérogène préparé dans un dispositif suivant l'une des revendications 1 à 18 d'une solution aqueuse alcaline de bisphénolate avec du phosgène gazeux ou liquide dissous dans le dichlorométhane, caractérisé par une très petite teneur résiduelle <20 ppm en phénylpipéridyluréthanne.
EP00902646A 1999-02-11 2000-02-07 Dispositif permettant de melanger et de faire reagir des melanges gazeux ou liquides a plusieurs phases et son utilisation Expired - Lifetime EP1165218B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19905572A DE19905572A1 (de) 1999-02-11 1999-02-11 Vorrichtung zum Mischen und Reagieren mehrphasiger gasförmiger und flüssiger Gemische und Verwendung dieser Vorrichtung
DE19905572 1999-02-11
PCT/EP2000/000788 WO2000047314A1 (fr) 1999-02-11 2000-02-07 Dispositif permettant de melanger et de faire reagir des melanges gazeux ou liquides a plusieurs phases et son utilisation

Publications (2)

Publication Number Publication Date
EP1165218A1 EP1165218A1 (fr) 2002-01-02
EP1165218B1 true EP1165218B1 (fr) 2003-05-21

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EP00902646A Expired - Lifetime EP1165218B1 (fr) 1999-02-11 2000-02-07 Dispositif permettant de melanger et de faire reagir des melanges gazeux ou liquides a plusieurs phases et son utilisation

Country Status (10)

Country Link
US (1) US6726354B1 (fr)
EP (1) EP1165218B1 (fr)
JP (1) JP4818512B2 (fr)
CN (1) CN1222351C (fr)
AT (1) ATE240776T1 (fr)
AU (1) AU2440800A (fr)
DE (2) DE19905572A1 (fr)
ES (1) ES2199766T3 (fr)
HK (1) HK1044729B (fr)
WO (1) WO2000047314A1 (fr)

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Also Published As

Publication number Publication date
JP2002536163A (ja) 2002-10-29
JP4818512B2 (ja) 2011-11-16
WO2000047314A1 (fr) 2000-08-17
EP1165218A1 (fr) 2002-01-02
AU2440800A (en) 2000-08-29
CN1222351C (zh) 2005-10-12
DE19905572A1 (de) 2000-08-31
ATE240776T1 (de) 2003-06-15
CN1339982A (zh) 2002-03-13
HK1044729A1 (en) 2002-11-01
HK1044729B (zh) 2006-07-14
DE50002263D1 (de) 2003-06-26
ES2199766T3 (es) 2004-03-01
US6726354B1 (en) 2004-04-27

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