EP1296753B1 - Verfahren und vorrichtung zur verringerung von nebenprodukten bei der vermischung von eduktströmen - Google Patents

Verfahren und vorrichtung zur verringerung von nebenprodukten bei der vermischung von eduktströmen Download PDF

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Publication number
EP1296753B1
EP1296753B1 EP01960430A EP01960430A EP1296753B1 EP 1296753 B1 EP1296753 B1 EP 1296753B1 EP 01960430 A EP01960430 A EP 01960430A EP 01960430 A EP01960430 A EP 01960430A EP 1296753 B1 EP1296753 B1 EP 1296753B1
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EP
European Patent Office
Prior art keywords
mixing
feed
component
stream
mixing zone
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
EP01960430A
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German (de)
English (en)
French (fr)
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EP1296753A1 (de
Inventor
Andreas Wölfert
Ulrich Penzel
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BASF SE
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BASF SE
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Publication date
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Publication of EP1296753A1 publication Critical patent/EP1296753A1/de
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Publication of EP1296753B1 publication Critical patent/EP1296753B1/de
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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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/71—Feed mechanisms
    • B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
    • B01F35/7179—Feed mechanisms characterised by the means for feeding the components to the mixer using sprayers, nozzles or jets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/71—Feed mechanisms
    • B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
    • B01F35/71805—Feed mechanisms characterised by the means for feeding the components to the mixer using valves, gates, orifices or openings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/80—Forming a predetermined ratio of the substances to be mixed
    • B01F35/83—Forming a predetermined ratio of the substances to be mixed by controlling the ratio of two or more flows, e.g. using flow sensing or flow controlling devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/2805—Mixing plastics, polymer material ingredients, monomers or oligomers
    • 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
    • B01F25/312—Injector mixers in conduits or tubes through which the main component flows with Venturi elements; Details thereof
    • 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
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
    • B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions

Definitions

  • the invention relates to a method and an apparatus for Reduction of by-product formation when mixing at least two Educt streams for example in the production of organic mono- or Polyisocyanates by mixing mono- or polyamines with phosgene elevated temperatures.
  • Reactants on the mixing room surfaces can be diluted strongly avoid the reactants.
  • the strong dilution of the reactants in turn causes higher processing costs for the product in the next one Process stage and is therefore only an inadequate alternative Mixing two or more components in the liquid phase are also the pressure losses occurring in the mixing device of concern which the Mixing energy to be used by increasing turbulent diffusion processes not negligible influence.
  • mixing devices for mixing educt streams become known who are in mixing facilities with unmoving and those with have moving components divided.
  • Mixing devices with moving Parts are for example from DE-AS-2 153 268 or US-3,947,484 or as Mixing devices with rotor and stator disks from EP-0 291 819 B1, DE-37 17 057 C2 and US-4,915,509 become known.
  • a static mixer for example known from EP-0 322 647 B1 ring hole nozzle.
  • the ring-hole nozzle becomes one of the two educt streams constricted.
  • the other educt stream becomes smaller in the form of a multitude Rays, which are generated by the holes arranged in a ring, in the constricted beam initiated.
  • the main disadvantage when using a Ring nozzle is, however, the fact that solid deposits already in individual Holes can lead to a lower flow.
  • the one about a scheme Set total volume flow flowing through all holes in the ring nozzle remains constant since the remaining holes are now more heavily loaded. The easing the flow, however, promotes further solid deposition, so that it generally comes earlier that a single one from a multitude of holes clogged.
  • DE-OS 29 50 216 relates to an alternative to a ring hole nozzle, namely a cylindrical mixing chamber into which fan-like spray jets be initiated. Due to the high pre-pressures required for the procedure are necessary, as well as experience-related blockages caused by Growth and build-up of the liquid phases on the walls of the mixing chamber this approach is unsatisfactory.
  • US 3,507,626 relates to a venturi mixing device.
  • This Mixing device is specially designed for mixing phosgene with amine Production of isocyanates with a first and a second inlet as well an outlet.
  • a first line section includes a venturi section a converging section, a narrow section and a diverging section Section.
  • a second line section is coaxial in the first line section recorded and acts as the first entry.
  • the second line section includes a bevel leading to the converging section corresponds.
  • the second line section opens into a mixing chamber extends around the venturi section of the first line section.
  • the Mixing device ensures mixing and prevents clogging by the Formation of by-products.
  • DE AS 17 92 660 B2 relates to a method and an apparatus for Mixing and reacting an amine with phosgene to an isocyanate.
  • the amine and phosgene processes are carried out coaxially and mixed with one another, the two streams of amine and phosgene being ring-shaped or conical are formed at an acute angle to each other at a crossing and mixing point cut and immediately before, at and after this intersection when entering an expanded reaction space can be accelerated.
  • the device can be used to increase the opening configured in the form of a gap the gap width is adjusted depending on their increase become. Taking into account the axial travel of the conical Bodies that adjust in the axial direction can be adjusted in relation to the gap-shaped or annular-gap-shaped outlet openings maximum Achieve injection angles of 45 ° to 60 °.
  • EP-0 830 894 A1 discloses one Solution.
  • the cleaning mandrel which is a movable component, an attempt is made to keep an introduction point free of deposits, whereby - if that highly toxic phosgene is one of the starting materials - a high security risk, as above already mentioned, through the formation of a new potential phosgene exit point is created.
  • a deposit can be removed using the solution carry out solids from the mixing chamber using the cleaning dome, however, this is paid for by the formation of a danger zone in the form of the Storage location of the movable cleaning mandrel.
  • the object of the invention based on a blending process with unmoving components available too make with which organic mono- or polyisocyanates continuously and free of deposits while avoiding the formation of by-products have it made.
  • the mixing room in the intake area to be mixed to the deficit component.
  • the distribution ratio of the excess component stream, supplied via two separate feed lines to 1: 1 define so that the part-duct flows as an internal or a outer ring jet can be fed.
  • the distribution ratio of the educt partial flows the excess component can also be varied within wide limits, so the mass flow ratios of the inner part of the educt flow can be admitted outer part educt flow between 0.01 and 1 or also between 100 and 1 vary to the mixing process depending on the selected excess or deficit component to influence.
  • the Partial product streams that can be fed separately into the mixing room from 1 ° to Feed an angle range of 179 °.
  • the feed of the component reduct is preferably carried out at an angle of 90 ° based on the exiting at the front of the mixing room Deficit component.
  • the Methods proposed according to the invention the inner radius of the inside Mixing room wall and the outer radius of the outside of the mixing room bounding wall, adjust so that there is an enlarged inner Passage area for the mixing and the adjoining it Product discharge sets while keeping the passage speed and the annular gap between the surfaces delimiting the mixing area.
  • the Mixing device is provided with a number of reactant feed points and the reactant entry points and the mixing space are designed as annular gaps and at the front of the mixing room the entry point for one of the Educt flows is.
  • the mixing space itself can be designed as an annular gap has an adjustable gap between its boundary surfaces.
  • the Entry points of the educt streams which flow into the mixing room can preferably also be formed as a radially extending column, the Length of the mixing space is preferably between 7 and 10 gap widths.
  • 1 is a Y-shaped one Mixing device shown.
  • the Y-shaped mixing configuration 16 shows the two Mixing chamber 12 with respective excess component partial flows Leads. Partial product streams enter the feed lines at the entry points 17, 18 a. The leads are at their respective mouth 22 with connected to the mixing room 12. Not in its configuration from FIG. 1 Mixing chamber 12, which appears in more detail, also occurs on the end face of the Mixing chamber 12, the deficit component 5 - for example by a Axial annular gap amine flowing into the mixing chamber 12. To the Mixing space 12 of the Y-shaped mixing configuration 16 closes an extension of the mixing room 12 in a certain length 14. At the extension 14 of the Mixing room 12 follows the conveyor line for the product stream 10, the leaves the Y-shaped mixing configuration at the product discharge 19.
  • Fig. 2 shows a T-shaped mixing configuration
  • the two educt partial flows occur in the illustrated 2 at 90 ° based on the axis of the mixing chamber 12 extending below along its extension 14 into the Mixing room and call yourself through the extremely short cross diffusion paths quickly established mixing reaction.
  • the two supply lines which the part-educt flows about phosgene - via the Product entry points 17 and 18 of the feed lines in the direction of the mouths 22 can promote with swirl-generating components, such as be internally extending internals.
  • the swirl generating Components accelerate the mixing reaction of the two educt streams of the excess component with that at the front of the Mixing chamber 12 entering deficit component, for example of the amine.
  • Fig. 3 shows an annular gap mixing chamber with radial inlet openings for Excess component substreams.
  • the face 9 the mixing room 12 need not be a flat surface, it can be section by section be conical, concave or convex.
  • the face 9 opposite edges 23 which limit the mixing space length 14 Areas are preferably rounded so that there are no swirls and Form dead zones at the beginning of the mixing room 12.
  • the the mixing room 12 in Axial direction 14 delimiting side surfaces 6 and 7 are ideal as Cylinder walls executed. However, you can also use sections as Tapered or as a concave or convex extension or narrowing. With such a shape, which limit the mixing space length 14 Walls, there is a continuous transition of the outer boundary surface 7 reach the pipe system connected to the mixing device.
  • the excess component flow is in two partial educt streams 1, 2 split.
  • the partial educt streams, 1, 2 of Excess component with one of these partial educt streams for example, vertically injected deficiency component in one mixed annular mixing space 12.
  • the partial educt streams are preferred 1, 2 of the excess component in the suction areas 3, 4 of the Free jet of sub-component stream 5 emerging from a nozzle mixed.
  • the feed openings are for the inner Ring beam 1, the outer ring beam 2 and for the deficit component the end face 9 each formed as an annular gap.
  • they could go through a series of closely spaced holes.
  • the Orientation of the openings in relation to the mixing space 12 - here as 90 ° angled to each other - could use other angles are shown, the inlet openings of the excess components in relation on the free jet of the deficit component 8 could in the angular range of 1 up to 179 ° to each other.
  • the mouths 22 of the feed lines into the mixing space 12 1 and 2 it must be ensured that as far as possible no backflow in of the mixing device occur in that backflows in the mixing device product-rich fluid comes back into contact with educt-rich fluid, which increases the risk of by-product formation, such as urea arises.
  • the inner boundary surface 24 of an inner cylindrical element 6 when increasing the throughput by proposed mixing device as a core increasing its radius designed the throughput can be increased, the desired enlarged passage area of the mixing device a constant Passage speed allows, as well as a constant to be maintained Gap width allowed. Because the cross diffusion path and because of the same Velocity gradients, the turbulent cross diffusion remains constant at constant passage speeds, about 10 m / s, through the Mixing device according to the present invention with constant mixing times constant specific power input into the mixing device.
  • the method proposed according to the invention is broad regardless of the amount enforced, so that with the invention Procedures also adequately meet the requirements of scale-up capability Dimensions has been taken into account.
  • the length of the mixing chamber 14 is as shown in FIG. 1 and 2 show the product discharge 19, through which the product 10 mixing configuration according to the invention leaves to further process steps run through.
  • a mixing process is shown in the following example: about 420 kg / h, 2,4-toluenediamine (TDA) are dissolved in 2450 kg / h o-sealing benzene (ODB) premixed and together with 8100 kg / h of a 65% phosgene solution initiated in the mixing device shown in Figure 3.
  • ODB o-sealing benzene
  • the phosgene represents the excess component
  • that in the Dichlorobenzene dissolved TDA is the deficit component 5.
  • the Phosgene solution flows can be in a ratio of 1: 1 in the feed lines to the Educt entry points are divided, the entry diameter of the Mixing device and the gap between the mixing room bounding areas are chosen so that there is a medium Entry rate of the excess component phosgene and Deficit component amine of about 10 m / s and a Exit speed of the product stream 19 of about 10 m / s.
  • a medium Entry rate of the excess component phosgene and Deficit component amine of about 10 m / s
  • Exit speed of the product stream 19 of about 10 m / s.
  • Fig. 4 shows an arranged in a feed line of the mixing chamber 12 swirl-promoting element.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Apparatuses For Bulk Treatment Of Fruits And Vegetables And Apparatuses For Preparing Feeds (AREA)
  • Detergent Compositions (AREA)
  • Silicon Compounds (AREA)
  • Accessories For Mixers (AREA)
EP01960430A 2000-07-03 2001-06-29 Verfahren und vorrichtung zur verringerung von nebenprodukten bei der vermischung von eduktströmen Expired - Lifetime EP1296753B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10032269A DE10032269A1 (de) 2000-07-03 2000-07-03 Verfahren und Vorrichtung zur Verringerung von Nebenprodukten bei der Vermischung von Eduktströmen
DE10032269 2000-07-03
PCT/EP2001/007502 WO2002002217A1 (de) 2000-07-03 2001-06-29 Verfahren und vorrichtung zur verringerung von nebenprodukten bei der vermischung von eduktströmen

Publications (2)

Publication Number Publication Date
EP1296753A1 EP1296753A1 (de) 2003-04-02
EP1296753B1 true EP1296753B1 (de) 2004-03-10

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EP01960430A Expired - Lifetime EP1296753B1 (de) 2000-07-03 2001-06-29 Verfahren und vorrichtung zur verringerung von nebenprodukten bei der vermischung von eduktströmen

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Country Link
US (1) US6896401B2 (ko)
EP (1) EP1296753B1 (ko)
JP (1) JP4884639B2 (ko)
KR (1) KR100691574B1 (ko)
CN (1) CN1197643C (ko)
AT (1) ATE261335T1 (ko)
AU (1) AU2001281925A1 (ko)
DE (2) DE10032269A1 (ko)
ES (1) ES2217180T3 (ko)
HU (1) HU228715B1 (ko)
PT (1) PT1296753E (ko)
WO (1) WO2002002217A1 (ko)

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CA2851533C (en) 2011-10-24 2020-01-14 United States Gypsum Company Multi-piece mold and method of making slurry distributor
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Also Published As

Publication number Publication date
PT1296753E (pt) 2004-07-30
JP2004501758A (ja) 2004-01-22
ATE261335T1 (de) 2004-03-15
HUP0301313A2 (en) 2003-08-28
KR100691574B1 (ko) 2007-03-12
CN1197643C (zh) 2005-04-20
AU2001281925A1 (en) 2002-01-14
EP1296753A1 (de) 2003-04-02
WO2002002217A1 (de) 2002-01-10
US6896401B2 (en) 2005-05-24
DE10032269A1 (de) 2002-01-31
KR20030028494A (ko) 2003-04-08
CN1434742A (zh) 2003-08-06
DE50101667D1 (de) 2004-04-15
HU228715B1 (en) 2013-05-28
JP4884639B2 (ja) 2012-02-29
US20040091406A1 (en) 2004-05-13
ES2217180T3 (es) 2004-11-01

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