EP1239944B1 - Procede et dispositif pour produire un melange homogene constitue d'un hydrocarbure aromatique a l'etat de vapeur et d'un gaz contenant de l'oxygene - Google Patents

Procede et dispositif pour produire un melange homogene constitue d'un hydrocarbure aromatique a l'etat de vapeur et d'un gaz contenant de l'oxygene Download PDF

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Publication number
EP1239944B1
EP1239944B1 EP00985245A EP00985245A EP1239944B1 EP 1239944 B1 EP1239944 B1 EP 1239944B1 EP 00985245 A EP00985245 A EP 00985245A EP 00985245 A EP00985245 A EP 00985245A EP 1239944 B1 EP1239944 B1 EP 1239944B1
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EP
European Patent Office
Prior art keywords
aromatic hydrocarbon
oxygen
containing gas
xylene
nozzles
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
EP00985245A
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German (de)
English (en)
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EP1239944A1 (fr
Inventor
Ulrich Block
Rolf Seubert
Bernhard Ulrich
Helmut Wunschmann
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BASF SE
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BASF SE
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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
    • B01F23/20—Mixing gases with liquids
    • 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
    • B01F23/20—Mixing gases with liquids
    • B01F23/21—Mixing gases with liquids by introducing liquids into gaseous media
    • B01F23/213—Mixing gases with liquids by introducing liquids into gaseous media by spraying or atomising of the liquids
    • B01F23/2132—Mixing gases with liquids by introducing liquids into gaseous media by spraying or atomising of the liquids using nozzles
    • 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
    • B01F25/313—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit
    • B01F25/3131—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit with additional mixing means other than injector mixers, e.g. screens, baffles or rotating elements
    • 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
    • B01F2025/91—Direction of flow or arrangement of feed and discharge openings
    • B01F2025/916—Turbulent flow, i.e. every point of the flow moves in a random direction and intermixes
    • 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
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions

Definitions

  • the invention relates to a method and a device for generating a homogeneous mixture of a vaporous aromatic Hydrocarbon and an oxygen-containing gas for catalytic gas phase reactions, especially a homogeneous one Mixture of vaporous o-xylene and / or naphthalene and Air for the production of phthalic anhydride.
  • PSA Phthalic anhydride
  • Equipment for carrying out such a PSA production process consist essentially of the functional units for the production the o-xylene vapor-air mixture, the reactor for the reaction the o-xylene vapor-air mixture and a device for PSA separation and workup.
  • the reaction by catalytic gas phase oxidation is usually carried out on V 2 O 5 -containing catalysts.
  • o-xylene is evaporated, mixed with an excess of air and passed at 340 ° C to 440 ° C over the catalyst in the tubes of a tube bundle reactor.
  • the catalyst consists for example of a mixture of V 2 O 5 and TiO 2 with promoters on ceramic bodies, such as porcelain or SiC spheres or rings, for example, 6 x 6 mm dimension. Large reactors have 10,000 to 40,000 tubes in the tube bundle.
  • the o-xylene is oxidized to PSA with a selectivity of 78% to 80%. This oxidation itself is highly exothermic at -1,110 kJ / mol.
  • the raw materials can be more or less contaminated.
  • the air may include NO x , H 2 S, sulfur oxides such as SO 2 , NH 3 and their salts, eg with CO 2 , which may lead to constrictions of one or more nozzles.
  • corrosion particles can change the droplet size and shape of the atomized o-xylene beam. Similar effects are caused by erosion of the nozzles in long-term operation.
  • the o-xylene may also contain m- and p-xylene, toluene, ethylbenzene, isopropylbenzene, nonane and small amounts of styrene. Such compounds can affect the surface tension of o-xylene.
  • the present invention is therefore based on the object improved method and apparatus for generating a homogeneous mixture of a vaporous aromatic hydrocarbon, such as o-xylene and / or naphthalene, and an oxygen containing gas, in particular air, for catalytic gas phase reactions to provide.
  • a vaporous aromatic hydrocarbon such as o-xylene and / or naphthalene
  • an oxygen containing gas in particular air
  • the invention solves the above-mentioned problems in that in a generic method, the atomization of the liquid aromatic hydrocarbon by using a nozzle for Formation of an atomizing hollow cone, preferably a swirl nozzle, he follows.
  • the atomizing cone may initially be a continuous one Be film from the liquid hydrocarbon, the tearing into small pieces at a greater distance from the swirl nozzle, which by surface forces to single drops with a Contract diameter less than 1 mm.
  • the present invention is therefore a method for Generation of a homogeneous mixture of a vaporous aromatic Hydrocarbon, such as o-xylene and / or naphthalene and an oxygen-containing gas, such as air, for catalytic Gas phase reactions, wherein the liquid aromatic hydrocarbon to drops with a diameter of less than 1 mm atomized and in one above the boiling point of the aromatic hydrocarbon preheated, oxygen-containing gas stream einst, wherein the method is characterized in that the mixture is generated in a room that exceeds the boiling point the hydrocarbon heated side walls is limited, and the liquid aromatic hydrocarbon by means of nozzles for Forming a hollow cone, preferably by means of swirl nozzles, atomized.
  • a vaporous aromatic Hydrocarbon such as o-xylene and / or naphthalene
  • an oxygen-containing gas such as air
  • the inventive method allows the generation of a very homogeneous, strandselle mixture of gaseous oxygen, preferably in air or other oxygen-containing Gas, and a hydrocarbon vapor.
  • the inventive method is preferably used in the Production of carboxylic acids or carboxylic anhydrides by catalytic Gas-phase oxidation of aromatic hydrocarbons, such as xylenes, in particular o-xylene and / or naphthalene, in Fixed bed reactors.
  • aromatic hydrocarbons such as xylenes, in particular o-xylene and / or naphthalene
  • PSA Called phthalic anhydride
  • the aromatic hydrocarbon is o-xylene and the oxygen-containing gas air.
  • the sputtering hollow cone preferably has an opening angle of 30 ° to 70 °.
  • the atomizing hollow cone preferably has an opening angle of about 60 °.
  • the axis of the sputtering hollow cone lies in the flow direction of the oxygen-containing gas, that is about the air, but can to deviate from this by up to 30 °.
  • Another measure can be in particular, be a certain distance, about one third of the Pipe radius of the wall to comply. It is preferably used several nozzles, about 2 to 6, preferably 4 to 6 in about the same Intervals.
  • swirl nozzles for atomizing of the liquid hydrocarbon.
  • Hollow cone nozzles designated vortex nozzles preferably present the outlet opening a guide with oblique flow surfaces on, the liquid to be atomized a twist or a Give rotation around the flow axis.
  • Such swirl nozzles are for other uses, such as fast pulse transmission in water jet pumps, injection condensers, etc. known (see. Grassmann "Physical Principles of Process Engineering", publisher Sauerlander (1970), pages 355 and 805).
  • the use of hollow cone nozzles in the method according to the invention is particularly preferred is, in other embodiments of the invention also full cone nozzles or slot nozzles can be used.
  • the Use of two-fluid nozzles, which with about to be sprayed o-xylene and the propellant air can be charged possible.
  • the liquid hydrocarbon stream to drops with a diameter of less than 1 mm, preferably less than 0.8 mm atomized.
  • the liquid stream is atomized to droplets of 0.02 to 0.2 mm.
  • the formation of the sputtering hollow cone with an opening angle From 30 ° to 70 ° used swirl nozzles are beneficial within a tube through which the oxygen gas flows on a pipe with supply line for the liquid to be atomized arranged. But you can also the annular feed pipe arrange for the liquid around the oxygen pipe and insert the nozzles into the oxygen pipe from the outside. In this case, the nozzle outlet openings are in Directed towards the gas flow.
  • the axis of the hollow cone by up to 30 ° from the Deviate flow direction of the gas. This can be achieved that fewer drops of the hollow cone touch the wall.
  • Axial hollow cone nozzles type KS 1 (Lechler, Metzingen, Germany). Such nozzles enable the production a hollow cone with the preferred cone angle of 60 °. Of the Hollow cone diameter is then at a distance of 250 mm from the outlet about 200 mm. According to the invention form small drops with a diameter of less than 1 mm, preferred less than 0.8 mm, more preferably 0.02 to 0.2 mm. The latter evaporate very fast and are already at a distance from 200 to 500 mm from the nozzle exit opening completely evaporated. However, drops of 0.8 to 1 mm may be up to complete evaporation 50 to 100 cm far and fly while the Touch and moisten the wall.
  • the mixture for example, the o-xylene-air mixture to produce in a room that of above the boiling point of the hydrocarbon heated Sidewalls is limited.
  • a heated tube such as a double-jacket tube, in particular a thermoplate tube formed (such thermal sheets become in Germany for example from the companies BUCO, Geesthacht or DEG, Gelsenmün produced).
  • Hydrocarbon droplets on the heated Pipe meet, can not be deposited as a liquid film, but are evaporated immediately. This eventually creates the desired mixture of hydrocarbon vapor and, for example Air.
  • the tube gap of the double-jacket tube can be heated with high-pressure steam be, preferably with water vapor of about 20 bar with a Temperature of 214 ° C.
  • the aforesaid thermoplates can have a particularly narrow pipe gap. Thermoshelf pipes are relatively simple and thus cheaper. Intensive heating can be used with thermoplate tubes cold spots are excluded.
  • the mixing device used is preferably static mixers. These are attached in the flow-through pipe Baffles that divide the stream to be mixed several times and bring together again, causing complete homogenization he follows.
  • static mixers are used for example by Sulzer, Winterthur, Switzerland.
  • Static mixers are also in the German patent applications DE 25 250 20 A1, DE 196 223 051 A1 and DE 196 23 105 A1.
  • the subject of the present invention is also a device for producing a homogeneous mixture of a vaporous aromatic hydrocarbon and an oxygen-containing Gas with a pipe for a preheated, oxygen-containing Gas stream, an atomizing device opening into the pipe for a stream of a liquid aromatic hydrocarbon, which is characterized in that the atomizing device Having swirl nozzles, and that the tube at least downstream of the swirl nozzles has walls that at least heated to the boiling point of the hydrocarbon are.
  • the tube preferably comprises a double-jacket tube or a tube Thermoshelf. Particularly preferred is downstream of the swirl nozzles a static mixer arranged in the gas channels.
  • the temperature on the hot tube wall is adjusted so that 5 to 50% by weight of the liquid hydrocarbon, especially 5 to 40 wt.%, Particularly preferably 5 to 30 wt.% Of the pipe wall meet and can be evaporated there, with the exact proportion from the impurities of raw materials, from the hollow cone shape and Nozzle change (erosion) during operation depends.
  • functional unit can be more
  • connect functional units to make PSA e.g. the reactor for converting the o-xylene to PSA, and the device for PSA separation and PSA recovery, as they are from the State of the art are known.
  • the device has a tube 11, which a preheated air flow (in the figure Arrow 12 symbolizes) introduce.
  • a sputtering device 13 provided from the supply lines 14th for liquid o-xylene and arranged at the end of the lines Swirl nozzles 15 exist.
  • the supply lines 14 are of a the pipe 11 concentrically surrounding supply pipe (not shown) fed.
  • the swirl nozzles 15 produce a hollow cone 16 from liquid o-xylene, which in finest drops with a middle Diameter between 0.02 and 0.2 mm decays.
  • the apparatus for o-xylene evaporation in a plant for PSA production consisted of a vertical thermobalance pipe of 1200 mm diameter. Through this, the oxidation air preheated to 200 ° C with a preheater was sent to the reactor. The pressure was about 1.5 bar absolute. The air was charged with o-xylene with a loading of 100 g per Nm 3 . The air was sucked without special cleaning, only via an air filter from the environment. The thermoplate tube was heated to 214 ° C with 20 bar steam. The o-xylene was injected via 6 swirl nozzles, which were mounted on a ring of 600 mm diameter and whose axis was pointing vertically upwards. These were axial hollow cone nozzles (KS 1 of type 216.324 made of steel, Lechler). The form was 8 bar. At a distance of 4.5 m behind the nozzles static mixers were mounted in the horizontally extending pipe section.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Accessories For Mixers (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Claims (11)

  1. Procédé de production d'un mélange homogène à partir d'un hydrocarbure aromatique sous forme de vapeur et d'un gaz contenant de l'oxygène pour des réactions catalytiques en phase gazeuse, sachant que
       l'on vaporise l'hydrocarbure aromatique liquide en gouttes de diamètre inférieur à 1 mm et que
       l'on injecte dans un gaz contenant de l'oxygène préchauffé au-delà du point dé vaporisation de l'hydrocarbure aromatique, caractérisé en ce que l'on produit le mélange dans un espace qui est délimité par des parois latérales chauffées au-delà du point de vaporisation de l'hydrocarbure aromatique, et
       que l'on vaporise l'hydrocarbure aromatique liquide au moyen de buses pour la création d'un cône creux.
  2. Procédé selon la revendication 1, caractérisé en ce que le cône creux de vaporisation possède un angle d'ouverture de 30° à 70°.
  3. Procédé selon l'une quelconque des revendications 1 ou 2, caractérisé en ce que l'axe central du cône creux de vaporisation est placé à un angle de -30° à +30° par rapport à l'axe central du flux gazeux préchauffé.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que l'on vaporise l'hydrocarbure aromatique liquide au moyen de buses à turbulence.
  5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que les parois latérales de l'espace sont constituées d'un tuyau chauffé.
  6. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que 5 à 50 % en poids de l'hydrocarbure aromatique vaporisé s'évapore sur les parois latérales chauffées.
  7. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'on introduit le mélange après l'évaporation de l'hydrocarbure aromatique par un mélangeur statique.
  8. Procédé selon l'une quelconque des revendications précédentes pour l'application à la synthèse de l'anhydride phtalique, l'hydrocarbure aromatique étant le o-xylol et/ou la naphtaline, et le gaz contenant de l'oxygène étant l'air.
  9. Dispositif de production d'un mélange homogène à partir d'un hydrocarbure aromatique sous forme de vapeur et d'un gaz contenant de l'oxygène avec
       un tuyau (11) pour un flux gazeux chauffé contenant de l'oxygène (12),
       un dispositif de vaporisation (13) débouchant dans le tuyau (11) pour un flux d'hydrocarbure aromatique liquide,
       caractérisé en ce que
       le dispositif de vaporisation (13) comporte des buses à turbulence (15),
       et que le tuyau (11) comporte au moins en aval des buses à turbulence (15) des parois (18) qui peuvent être chauffées au moins jusqu'à la température de vaporisation de l'hydrocarbure aromatique.
  10. Dispositif selon la revendication 9, caractérisé en ce que le tuyau (11) entoure un tuyau à double enveloppe ou un tuyau constitué d'une plaque thermique.
  11. Dispositif selon l'une quelconque des revendications 9 ou 10, caractérisé en ce qu'un mélangeur statique est disposé dans le tuyau en aval des buses à turbulence.
EP00985245A 1999-12-23 2000-12-22 Procede et dispositif pour produire un melange homogene constitue d'un hydrocarbure aromatique a l'etat de vapeur et d'un gaz contenant de l'oxygene Expired - Lifetime EP1239944B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19962616A DE19962616A1 (de) 1999-12-23 1999-12-23 Verfahren und Vorrichtung zur Erzeugung eines homogenen Gemisches aus einem dampfförmigen aromatischen Kohlenwasserstoff und einem Sauerstoff enthaltenden Gas
DE19962616 1999-12-23
PCT/EP2000/013165 WO2001047622A1 (fr) 1999-12-23 2000-12-22 Procede et dispositif pour produire un melange homogene constitue d'un hydrocarbure aromatique a l'etat de vapeur et d'un gaz contenant de l'oxygene

Publications (2)

Publication Number Publication Date
EP1239944A1 EP1239944A1 (fr) 2002-09-18
EP1239944B1 true EP1239944B1 (fr) 2004-03-24

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EP00985245A Expired - Lifetime EP1239944B1 (fr) 1999-12-23 2000-12-22 Procede et dispositif pour produire un melange homogene constitue d'un hydrocarbure aromatique a l'etat de vapeur et d'un gaz contenant de l'oxygene

Country Status (13)

Country Link
US (1) US20030013931A1 (fr)
EP (1) EP1239944B1 (fr)
JP (1) JP4669184B2 (fr)
KR (1) KR100655339B1 (fr)
CN (1) CN1174793C (fr)
AT (1) ATE262372T1 (fr)
AU (1) AU2172001A (fr)
DE (2) DE19962616A1 (fr)
ES (1) ES2218265T3 (fr)
MX (1) MXPA02005852A (fr)
MY (1) MY125936A (fr)
TW (1) TW581710B (fr)
WO (1) WO2001047622A1 (fr)

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DE102005030416B4 (de) * 2005-06-30 2007-06-21 Stockhausen Gmbh Anordnung und Verfahren zur Erwärmung und Begasung eines polymerisationsfähigen Stoffes sowie Vorrichtung und Verfahren zur Herstellung hochreiner (Meth)Acrylsäure
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CN103949171A (zh) * 2014-04-28 2014-07-30 德合南京智能技术有限公司 一种气体与溶液快速混合的方法及装置
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JP6941473B2 (ja) * 2017-04-26 2021-09-29 株式会社日本製鋼所 ディスプレイの製造方法、ディスプレイ及び液晶テレビ
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CN112546889B (zh) * 2020-11-16 2021-07-20 哈尔滨工业大学 一种用于储释热系统热稳定输出的气体混合装置
KR102469555B1 (ko) * 2020-11-26 2022-11-22 현대제철 주식회사 입자 및 가스 물질 처리장치

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Publication number Publication date
TW581710B (en) 2004-04-01
CN1174793C (zh) 2004-11-10
EP1239944A1 (fr) 2002-09-18
ES2218265T3 (es) 2004-11-16
US20030013931A1 (en) 2003-01-16
DE50005821D1 (de) 2004-04-29
MXPA02005852A (es) 2002-10-23
KR20020062374A (ko) 2002-07-25
AU2172001A (en) 2001-07-09
JP2003518433A (ja) 2003-06-10
WO2001047622A1 (fr) 2001-07-05
ATE262372T1 (de) 2004-04-15
KR100655339B1 (ko) 2006-12-08
CN1411392A (zh) 2003-04-16
JP4669184B2 (ja) 2011-04-13
DE19962616A1 (de) 2001-06-28
MY125936A (en) 2006-09-29

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