EP3199230A1 - Dispositif de melange continu d'au moins deux substances - Google Patents

Dispositif de melange continu d'au moins deux substances Download PDF

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Publication number
EP3199230A1
EP3199230A1 EP16153557.0A EP16153557A EP3199230A1 EP 3199230 A1 EP3199230 A1 EP 3199230A1 EP 16153557 A EP16153557 A EP 16153557A EP 3199230 A1 EP3199230 A1 EP 3199230A1
Authority
EP
European Patent Office
Prior art keywords
mixing
substances
mixing chamber
rotor
magnetic
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.)
Withdrawn
Application number
EP16153557.0A
Other languages
German (de)
English (en)
Inventor
Jurgen Arras
Jan Busch
Joachim Ritter
Holger CONZELMANN
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.)
Covestro Deutschland AG
Original Assignee
Covestro Deutschland AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Covestro Deutschland AG filed Critical Covestro Deutschland AG
Priority to EP16153557.0A priority Critical patent/EP3199230A1/fr
Publication of EP3199230A1 publication Critical patent/EP3199230A1/fr
Withdrawn legal-status Critical Current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
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/10—Mixing gases with gases
    • B01F23/14—Mixing gases with gases with moving mixing elements, e.g. with liquid seal
    • 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
    • B01F25/40—Static mixers
    • B01F25/45—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads
    • B01F25/451—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by means for moving the materials to be mixed or the mixture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
    • B01F27/271—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed radially between the surfaces of the rotor and the stator
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/45—Magnetic mixers; Mixers with magnetically driven stirrers
    • B01F33/453—Magnetic mixers; Mixers with magnetically driven stirrers using supported or suspended stirring elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/45—Magnetic mixers; Mixers with magnetically driven stirrers
    • B01F33/453—Magnetic mixers; Mixers with magnetically driven stirrers using supported or suspended stirring elements
    • B01F33/4531—Magnetic mixers; Mixers with magnetically driven stirrers using supported or suspended stirring elements using an axis supported in several points for mounting the stirring element
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/45—Magnetic mixers; Mixers with magnetically driven stirrers
    • B01F33/453—Magnetic mixers; Mixers with magnetically driven stirrers using supported or suspended stirring elements
    • B01F33/4532—Magnetic mixers; Mixers with magnetically driven stirrers using supported or suspended stirring elements using a bearing, tube, opening or gap for internally supporting the stirring element

Definitions

  • the invention relates to a device for continuously mixing at least two substances.
  • this device is used for mixing di- and polyamines of the diphenylmethane series (hereafter MDA total) with carbon monoxide (phosgene) for the preparation of di- and polyisocyanates of the diphenylmethane series (henceforth MDI).
  • MDI polyurethanes
  • MDA carbon dioxide dichloride
  • the phosgene should be used in hermetically closed circuits.
  • the mixing devices used must be hermetically sealed; Sealing rings on rotating components can not adequately provide this hermetic seal according to the required safety.
  • Phosgene is added to the reaction in proportion to MDA in excess of the stoichiometrically exact amount.
  • the supplied MDA should be fully implemented, while a certain amount of phosgene remains unreacted in the starting material. The excess should be adjusted as low as possible for economic reasons, so that the amount of recirculated phosgene is minimized.
  • the input materials MDA and phosgene are dissolved in the preparation of MDI in a solvent such as monochlorobenzene (MCB) or ortho-dichlorobenzene, which promotes viscosity and miscibility.
  • a solvent such as monochlorobenzene (MCB) or ortho-dichlorobenzene, which promotes viscosity and miscibility.
  • MBB monochlorobenzene
  • ortho-dichlorobenzene which promotes viscosity and miscibility.
  • the solvent in the purchase and disposal is quite expensive; therefore it is processed by distillation and used several times. This distillation is associated with an energy input and is therefore costly. For economic reasons, therefore, efforts are always made to keep the proportion of solvent as low as possible.
  • the reaction of MDA and phosgene is an exothermic reaction. Due to the reactivity, local temperature peaks arise, which have to be reduced; the local temperatures in the mixing room should not exceed about 145 ° C, in order to produce no unwanted by-products.
  • the cooling is usually provided by the solvent. However, if you reduce the proportion of the solvent, so the cooling agent is also saved to cool the reaction.
  • MDA * HCl solid MDA hydrochloride
  • MDA * HCl solid MDA hydrochloride
  • MDA * HCl solid MDA hydrochloride
  • This reaction is undesirable in itself, but can not be completely avoided.
  • the more critical the formation of MDA * HCl the finer the MDA * HCl.
  • the MDA * HCl can in turn be converted to the MDI with phosgene, so it is not lost for the target reaction. This reaction proceeds the better, the finer the MDA * HCl.
  • Another factor that influences this reaction is the solubility of MDA * HCl in the solvent, which increases with increasing temperature.
  • phosgene tends to outgas at too high a temperature. This can be counteracted by increasing the pressure in the mixing chamber to at least 20 bar, preferably more than 30 bar.
  • Such a mixer comprises a rotor with a plurality of radially aligned bolts.
  • the mixing takes place here on an outer circumference of the mixer (see also EP 2 077 150 A1 ).
  • rotational speeds of more than 1000 U / min are set.
  • rotational speeds of the rotor-stator mixer of at least 3000 U / min are desired.
  • the device according to the invention for continuously mixing at least two substances comprises a mixing space in which a mixing element, in particular a rotor-stator mixer is arranged, at least two inlets through which the substances to be mixed are introduced separately and continuously into the mixing space, at least one drain for the continuous filling of the mixing chamber produced product from the mixing chamber and also a drive arrangement for driving the mixing element.
  • the device is suitable and is especially used for mixing MDA with carbon monoxide (phosgene) to produce MDI.
  • the solvent used is in particular MCB (chlorobenzene).
  • the mixing chamber is hermetically enclosed by a housing. Rotating members rotatably connected to the mixing element are disposed entirely within the hermetic enclosure. This means in particular that no rotating parts penetrate the hermetically enclosing housing, which is a prerequisite for a high level of safety against undesired escape of highly toxic substances.
  • the invention is characterized in that the drive arrangement comprises an arrangement for generating a rotating magnetic field, which is arranged completely outside the hermetically enclosing housing.
  • This arrangement may comprise a motor and a first magnet element rotatably driven therewith, and is disposed entirely outside the hermetically enclosing housing.
  • the drive arrangement comprises a second magnetic element, which is arranged completely within the hermetically enclosing housing and is in magnetic drive connection with the arrangement, in particular the first magnetic element.
  • the second magnetic element is rotatably connected to the mixing element.
  • the second magnetic element in this case represents a kind of stirring fish, which is arranged in the mixing chamber, and causes by its rotation a mixing of the introduced substances.
  • the second magnetic element may be formed integrally with the mixing element.
  • the second magnetic element is a spiked ring, which is associated with a rotor-stator mixer.
  • the second magnetic element is mounted in contrast to known magnetic stirrers in the mixing chamber, in particular based on magnetic bearings.
  • the device comprises a rotor-stator mixer arrangement with a spiked ring.
  • a spiked ring is rotatably supported in the mixing space about an axis of rotation.
  • a plurality of circular and coaxial arranged around the axis of rotation of the spiked inflows is provided for the separate introduction of the substances into the mixing chamber.
  • Continuous mixing is understood in particular to mean that the substances undergo a largely constant flow during the mixing process, and that in the mixing chamber produced product is constantly discharged.
  • static mixing operations are understood as those in which first all the substances to be mixed are introduced in a mixing chamber in a chord, then the inflow is stopped and mixing takes place and after complete mixing the end product is removed from the mixing chamber; only then refilling with substances to be mixed. Such static mixing operations are not encompassed by the term continuous introduction.
  • the spiked ring is arranged directly axially adjacent to the tributaries.
  • Axially adjacent means that in the axial direction (ie in a direction parallel to the axis of rotation) a maximum of a narrow gap, in particular less than 2 mm, is provided between the outlet of the inflows and the spiked ring.
  • the mixing element is supported by magnetic bearings.
  • Such magnetic bearings may be formed without contact; that is, there is no contact between relative moving parts at these bearings.
  • high rotational speeds can be realized without friction and thus heat exposure between the elements involved occurs.
  • the device described above is used for the continuous mixing of at least two substances, in particular diaminodiphenylmethane MDA and carbon dioxide dichloride (phosgene).
  • the pressure in the mixing chamber is preferably at least 19 bar, preferably at least 20 bar, more preferably at least 30 bar.
  • the mixing element is operated at a rotational speed of at least 3000 revolutions per minute.
  • the temperature in the mixing chamber is in particular a maximum of 135 ° C, preferably 85 ° C.
  • a magnetic coupling is essentially designed such that the interior of the magnetic coupling becomes the mixing and reaction space.
  • the second magnetic element can be embodied as an anchor stirrer or stirring fish with, for example, Teflon-coated permanent magnets, which are driven by the first magnetic element arranged outside the housing. So can be very high Torques in the range of a few Nm achieve in small gap cans, which allows the required mechanical power inputs in the range of several kW. Similarly, very high speeds are possible, so that the peripheral speeds (20-30 m / s) of the production mixers are achieved, which is an important parameter for scale-up investigations.
  • the required high speeds can be made possible with magnetic and / or hydraulic storage of the inner rotor. Since the question of the need for purge and cooling flows also applies to larger magnetically driven intensive mixers (eg rotor-stator mixers in the production of MDI), an application of the invention on a larger scale, in particular in the production of MDI, advantageous because so inert side streams can be avoided in particular by solvent, which is beneficial to a reduction of cycle streams.
  • larger magnetically driven intensive mixers eg rotor-stator mixers in the production of MDI
  • the excess of phosgene at given target NCO levels can be reduced if free MDA is no longer available for side reactions to ureas. In this case, the excess can be reduced to almost zero, so that a use of phosgene is possible quite close to or exactly at the stoichiometric ratio.
  • the phosgene holdup in the plant part can significantly reduce, which is seen as increasingly critical safety aspect.
  • FIG. 1 to FIG. 3 show a mixing device 1 with a rotor-stator mixer assembly of the conventional type.
  • a mixing chamber 4 two substances X, Y are supplied separately and continuously via inlets 3.
  • the substances X, Y are dissolved in a solvent L.
  • a mixing device 6 is provided in the form of a rotor-stator mixer.
  • This rotor-stator mixer 6 comprises a plurality of spiked rings 7. At each spiked ring 7 protrude radially single spikes 8.
  • the spiked rings 7 are held on a common rotary shaft 14 and rotatably connected to each other.
  • the motor 9 includes a stator 10 and a rotor 11.
  • An electrical lead 12 is connected to the stator.
  • the rotor 11 is rotatably connected to the shaft 14.
  • the mixing device 1 comprises a hermetically sealed housing 2, in which all rotating parts of the mixing device 1 are located, in particular the spiked ring 7, the rotor 11 and the shaft 14. Also bearings 13 for supporting the shaft 14 are held within the hermetically sealed housing 2 , The stators 10 of the motor are held outside the housing 2.
  • a partition 22 separates the interior of the housing 2 in two different spaces, to one the mixing chamber 4, on the other hand, the rotor chamber 21. In the last is the rotor 12 is received. Essentially, it is prevented by the partition 22 that fluid can flow from the mixing chamber 4 into the rotor chamber 21, only individual slots 23 in the region of the partition or the bearings are provided to allow a solvent flow L from the rotor chamber 21 into the mixing chamber 4. This solvent flow serves for a cooling of the rotor 11; On the other hand, this solvent flow L should ensure that none of the substances X, Y or the final product Z reaches the rotor space 21.
  • the two substances X and Y are mixed to the final product Z.
  • the substances X and Y are dissolved in the solvent L before.
  • the final product Z is dissolved in the solvent L.
  • the end product Z flows in dissolved form completely from the mixing chamber 4 and enters a solvent separator 18, in which the solvent L is separated from the end product X.
  • the separated solvent L passes into a solvent treatment 19, and from there the solvent passes again into the Rotor space 21 for cooling and purging the rotor; Further, the solvent L is used again for dissolving the substances X, Y (not shown).
  • FIG. 2 and FIG. 3 Details of the rotor-stator mixer are shown.
  • the spiked ring 7 rotates in the direction of rotation D about the axis of rotation A.
  • the spiked ring 7 also has twelve spikes, the inlets are arranged adjacent to each other in the circumferential direction.
  • the number of spikes 8 on a spiked ring 7 coincides with the number of circumferentially distributed inlets 3.
  • the spikes 8 are shown in cross-section. It can be seen that the spikes 8 are only spaced from the tributaries 3 by an axial gap of a few millimeters. In the radially outer region, which is in overlap with the tributaries 3, the spike 8 has a bevel 15. This chamfer 15 serves to entrain the flow S of the inflowing substances from the axial direction, as it first flows out of the inflows 3, in the direction of rotation D. First, an acceleration of the substances in the circumferential direction is thus effected by the rotor-stator mixer.
  • FIG. 4 is now a modification of the mixing device according to FIG. 1 shown, wherein the described details of the mixing device according to the figures FIG. 1 to FIG. 3 largely on the mixing devices according to the invention according to the figures FIG. 4 and FIG. 5 are applicable.
  • FIG. 4 shows a mixing device 1 with a rotor-stator mixer 6, comprising a significantly smaller hermetically sealed housing 2 as the mixing device according to FIG. 1 ,
  • the motor 9 is a commercial motor, which is supplied via a power line 12 with electrical energy.
  • a magnetic disk 16 (first magnetic element) is driven via a shaft 14 "The motor 9, the shaft 14 and the magnetic disk 16 are arranged outside the housing 2.
  • Within of the housing 16 is a magnetic stirring fish 17 (second magnetic element) is arranged, which is integrally formed with a spiked ring 7.
  • the spiked ring 7 rotates and causes a mixture, as it already has FIG. 1 was shown.
  • the separate solvent flow for cooling and purging parts of the engine can be omitted.
  • FIG. 5 shows a modification of the device according to FIG. 4 ,
  • the rotor-stator mixer 17 which is integrally formed with a spiked ring 7 more spiked rings 7 are provided, which are arranged axially adjacent to the stirring fish 17 and are connected to each other via a shaft 14 '.
  • the shaft 14 ' is mounted in the housing 2.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Mixers With Rotating Receptacles And Mixers With Vibration Mechanisms (AREA)
EP16153557.0A 2016-02-01 2016-02-01 Dispositif de melange continu d'au moins deux substances Withdrawn EP3199230A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP16153557.0A EP3199230A1 (fr) 2016-02-01 2016-02-01 Dispositif de melange continu d'au moins deux substances

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP16153557.0A EP3199230A1 (fr) 2016-02-01 2016-02-01 Dispositif de melange continu d'au moins deux substances

Publications (1)

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EP3199230A1 true EP3199230A1 (fr) 2017-08-02

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EP16153557.0A Withdrawn EP3199230A1 (fr) 2016-02-01 2016-02-01 Dispositif de melange continu d'au moins deux substances

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4303384A1 (fr) 2022-06-22 2024-01-10 ASSA ABLOY Sicherheitstechnik GmbH Gâche électrique

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0291820A1 (fr) * 1987-05-21 1988-11-23 Bayer Ag Mélangeur pour mélanger deux ou plusieurs fluides, en particulier pour initier ou entretenir une réaction sous agitation
DE102007054233A1 (de) * 2007-11-12 2009-05-20 Ika-Werke Gmbh & Co. Kg Vorrichtung zum Dispergieren oder Homogenisieren
EP2077150A1 (fr) 2007-12-19 2009-07-08 Bayer MaterialScience AG Procédé et agrégat mixte destinés à la fabrication d'isocyanates par phosgénation d'amines primaires

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0291820A1 (fr) * 1987-05-21 1988-11-23 Bayer Ag Mélangeur pour mélanger deux ou plusieurs fluides, en particulier pour initier ou entretenir une réaction sous agitation
DE102007054233A1 (de) * 2007-11-12 2009-05-20 Ika-Werke Gmbh & Co. Kg Vorrichtung zum Dispergieren oder Homogenisieren
EP2077150A1 (fr) 2007-12-19 2009-07-08 Bayer MaterialScience AG Procédé et agrégat mixte destinés à la fabrication d'isocyanates par phosgénation d'amines primaires

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4303384A1 (fr) 2022-06-22 2024-01-10 ASSA ABLOY Sicherheitstechnik GmbH Gâche électrique

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