US20030013931A1 - Method and device for production of a homogeneous mixture of a vapour-forming aromatic hydrocarbon and an oxygen-containing gas - Google Patents

Method and device for production of a homogeneous mixture of a vapour-forming aromatic hydrocarbon and an oxygen-containing gas Download PDF

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Publication number
US20030013931A1
US20030013931A1 US10/168,953 US16895302A US2003013931A1 US 20030013931 A1 US20030013931 A1 US 20030013931A1 US 16895302 A US16895302 A US 16895302A US 2003013931 A1 US2003013931 A1 US 2003013931A1
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United States
Prior art keywords
aromatic hydrocarbon
oxygen
tube
containing gas
xylene
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Abandoned
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US10/168,953
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Ulrich Block
Rolf Seubert
Bernhard Ulrich
Helmut Wunschmann
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BASF SE
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Assigned to BASF AKTIENGESELLSCHAFT reassignment BASF AKTIENGESELLSCHAFT ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BLOCK, ULRICH, SEUBERT, ROLF, ULRICH, BERNHARD, WUNSCHMANN, HELMUT
Publication of US20030013931A1 publication Critical patent/US20030013931A1/en
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    • 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 present invention relates to a process and an apparatus for producing a homogeneous mixture of a gaseous aromatic hydrocarbon and an oxygen-containing gas for catalytic gas-phase reactions, in particular a homogeneous mixture of gaseous o-xylene and/or naphthalene and air for the preparation of phthalic anhydride.
  • Phthalic anhydride is an important intermediate for producing synthetic resins, phthalate plasticizers, phthalocyanine dyes and further fine chemicals. PA is nowadays prepared primarily from o-xylene, predominantly by gas-phase oxidation of o-xylene by means of air as oxidant.
  • Plants for carrying out such a PA production process consist essentially of the functional units for producing the o-xylene vapor/air mixture, the reactor for reacting the o-xylene vapor/air mixture and a facility for separating off and working up the PA.
  • the catalytic gas-phase oxidation reaction is usually carried out over V 2 O 5 -containing catalysts.
  • o-xylene is vaporized, mixed with an excess of air and passed at from 340° C. to 440° C. over the catalyst in the tubes of a shell-and-tube reactor.
  • the catalyst comprises, for example, a mixture of V 2 O 5 and TiO 2 with promoters on ceramic bodies, e.g. porcelain or SiC spheres or rings having dimensions of, for example, 6 ⁇ 6 mm. Large reactors have from 10 000 to 40 000 tubes arranged within the shell.
  • the o-xylene is usually oxidized to PA with a selectivity of from 78% to 80%. This oxidation itself is strongly exothermic, with an enthalpy change of ⁇ 1110 kJ/mol.
  • DE-A 1 793 453 discloses a process for producing a homogeneous mixture of gaseous o-xylene and air for the catalytic oxidation to phthalic anhydride.
  • a stream of o-xylene is atomized to form droplets having a diameter of less than 1 mm, for example a size of predominantly below 0.3 mm, and introduced into a stream of air which has been preheated to above the boiling point of o-xylene.
  • This stream of air is turbulent; a Reynolds number of above 200 000 is recommended.
  • the residence time from injection of the o-xylene to the reactor has to be at least 0.2 seconds so as to obtain a homogeneous gas mixture and thus uniform flow into all tubes.
  • the raw materials can have a varying level of contamination.
  • the air can contain, inter alia, NO x , H 2 S, sulfur oxides such as SO 2 , NH 3 and its salts, e.g. with CO 2 , which can lead to constriction of one or more nozzles.
  • Corrosion particles can also change the droplet size and shape of the atomized o-xylene jet. Similar effects are caused by erosion of the nozzles in long-term operation.
  • the o-xylene can also contain m- and p-xylene, toluene, ethylbenzene, isopropylbenzene, nonane and small amounts of styrene.
  • Such compounds can influence the surface tension of the o-xylene. It is possible for droplets which fly further than the abovementioned droplets having a size of, for example, predominantly below 0.3 mm to be formed. These can wet the wall of the reaction tube and form a liquid film there. An additional difficulty is that it is not possible in practice to install the nozzles serving for atomization of the o-xylene stream in such a way that no droplets of the atomized o-xylene stream come into contact with the wall of the guide tube.
  • a gaseous aromatic hydrocarbon e.g. o-xylene and/or naphthalene
  • an oxygen-containing gas in particular air
  • this object is achieved by, in a process of this type, carrying out the atomization of the liquid aromatic hydrocarbon by means of a nozzle which forms a hollow atomization cone, preferably a swirl nozzle.
  • the hollow atomization cone can initially be a coherent film of the liquid hydrocarbon which at a greater distance from the swirl nozzle breaks up into small fragments which are transformed by surface forces into individual droplets having a diameter of less than 1 mm.
  • the present invention accordingly provides a process for producing a homogeneous mixture of a gaseous aromatic hydrocarbon, e.g. o-xylene and/or naphthalene, and an oxygen-containing gas, e.g. air, for catalytic gas-phase reactions, by atomizing the liquid aromatic hydrocarbon to form droplets having a diameter of less than 1 mm and injecting it into an oxygen-containing gas stream preheated to above the boiling point of the aromatic hydrocarbon, wherein the liquid aromatic hydrocarbon is atomized by means of nozzles which form a hollow cone, preferably by means of swirl nozzles.
  • a gaseous aromatic hydrocarbon e.g. o-xylene and/or naphthalene
  • an oxygen-containing gas e.g. air
  • the process of the present invention makes it possible to produce a very homogeneous, streaming-free mixture of gaseous oxygen, preferably in air or another oxygen-containing gas, and a hydrocarbon vapor.
  • the process of the present invention is preferably used in the preparation of carboxylic acids or carboxylic anhydrides by catalytic gas-phase oxidation of aromatic hydrocarbons, for example, xylenes, in particular o-xylene and/or naphthalene, in fixed-bed reactors.
  • aromatic hydrocarbons for example, xylenes, in particular o-xylene and/or naphthalene
  • An example which may be mentioned is the preparation of phthalic anhydride (PA).
  • the hollow atomization cone preferably has an opening angle of from 30° to 70°.
  • the hollow atomization cone particularly preferably has an opening angle of about 60°.
  • the axis of the hollow atomization cone is aligned in the flow direction of the oxygen-containing gas, i.e., for instance, the air, but can deviate by up to 30° from this.
  • a further measure to achieve this can be, in particular, to maintain a certain distance, for instance one third of the tube radius, from the wall. Preference is given to using a plurality of nozzles, for instance from 2 to 6, preferably from 4 to 6, with approximately equal spacing.
  • swirl nozzles for atomizing the liquid hydrocarbon.
  • These swirl nozzles also referred to as hollow cone nozzles, preferably have, upstream of the outlet orifice, a guide body having oblique impingement surfaces which impart a swirl or rotation about the flow axis to the liquid to be atomized.
  • Such swirl nozzles are known for other applications, for example rapid impulse transmission in water jet pumps, spray condensers, etc. (cf. Grassmann “Physikalische Kunststoffn der Maschinenstechnik”, Verlag Sauerators (1970), pages 355 and 805).
  • hollow cone nozzles is particularly preferred in the process of the present invention
  • solid cone nozzles or slit nozzles can also be used in other embodiments of the invention.
  • two-fluid nozzles which can be supplied, for example, with the o-xylene to be sprayed and the propellent air is also possible.
  • a swirl or hollow cone nozzle is used for generating the hollow atomization cone according to the present invention, this is preferably operated at an admission pressure of from 2 to 20 bar so as to ensure that a hollow atomization cone having the opening angle of from 30° to 70° preferred according to the present invention is formed.
  • the liquid hydrocarbon stream is atomized to form droplets having a diameter of less than 1 mm, preferably less than 0.8 mm.
  • the liquid stream is particularly preferably atomized to form droplets of from 0.02 to 0.2 mm.
  • the swirl nozzles used to form the hollow atomization cone having an opening angle of from 30° to 70° are advantageously located within a tube through which the oxygen gas flows in a circular arrangement on a tube having an inlet for the liquid to be atomized.
  • the annular feed tube for the liquid can also be arranged around the oxygen feed tube and the nozzles can be passed from the outside into the oxygen feed tube.
  • the nozzle outlet orifices are directed in the direction of gas flow.
  • the axis of the hollow cone can deviate by up to 30° from the flow direction of the gas. This can reduce the number of droplets of the hollow cone which touch the wall.
  • KS 1 axial hollow cone nozzles are particularly suitable. Such nozzles make it possible to generate a hollow cone having the preferred cone angle of 60°.
  • the hollow cone diameter is then about 200 mm at a distance of 250 mm from the outlet orifice.
  • small droplets having a diameter of less than 1 mm, preferably less than 0.8 mm, particularly preferably from 0.02 to 0.2 mm, are formed. The latter vaporize very quickly and are completely vaporized at a distance of only 200-500 mm from the outlet orifice of the nozzle.
  • droplets having a size of from 0.8 to 1 mm can fly 50-100 cm before they are completely vaporized and can thus touch and wet the wall.
  • a particularly preferred embodiment of the process of the present invention provides for the mixture, for example the o-xylene/air mixture, to be produced in a chamber which is bounded by side walls heated to above the boiling point of the hydrocarbon.
  • Hydrocarbon droplets which impinge on the heated tube cannot deposit as a liquid film but instead are immediately vaporized. This finally produces the desired mixture of hydrocarbon vapor and, for example, air.
  • the annular gap of the double-walled tube can be heated by high-pressure steam, preferably steam having a pressure of about 20 bar and a temperature of 214° C.
  • high-pressure steam preferably steam having a pressure of about 20 bar and a temperature of 214° C.
  • the above-mentioned “Thermoblech” tubes can have a particularly narrow annular gap.
  • “Thermoblech” tubes have a relatively simple construction and are therefore relatively inexpensive. Intensive heating enables cold spots to be ruled out in “Thermoblech” tubes.
  • the vapor/air mixture is, in a further advantageous process variant, subsequently passed through a mixing device.
  • static mixers are guide plates which are installed in the tube through which flow occurs and which divide and recombine the stream to be mixed, resulting in complete homogenization.
  • static mixers are manufactured by, for example, Sulzer, Winterthur, Switzerland. Static mixers are also described in the German Patent Applications DE 25 250 20 A1, DE 196 223 051 A1 and DE 196 23 105 A1.
  • the present invention also provides an apparatus for producing a homogeneous mixture of a gaseous aromatic hydrocarbon and an oxygen-containing gas having gas channels for a preheated, oxygen-containing gas stream and an atomization device for a stream of a liquid aromatic hydrocarbon opening into the gas channels, wherein the atomization device has swirl nozzles and the gas channels have, at least downstream of the swirl nozzles, walls which can be heated to at least the boiling point of the hydrocarbon.
  • the gas channels preferably comprise a heatable tube, in particular a double-walled tube or a tube of “Thermoblech”. Particularly preferably, there is a static mixer installed in the gas channels downstream of the swirl nozzles.
  • the temperature at the hot tube wall is set so that from 5 to 50% by weight of the liquid hydrocarbon, in particular from 5 to 40% by weight, particularly preferably from 5 to 30% by weight, can impinge on the tube wall and be vaporized there, with the precise proportion depending on the impurities in the raw materials, on the shape of the hollow cone and on changes in the nozzle (erosion) during operation.
  • the abovementioned functional unit can be followed by further functional units for, for example, preparing PA, e.g. the reactor for converting the o-xylene into PA and the apparatus for separating off PA and isolating pure PA, as are known from the prior art.
  • preparing PA e.g. the reactor for converting the o-xylene into PA and the apparatus for separating off PA and isolating pure PA, as are known from the prior art.
  • the FIGURE shows an apparatus 10 for producing a homogeneous mixture of gaseous o-xylene and/or naphthalene and air.
  • the apparatus has gas channels 11 which conduct a preheated stream of air (symbolized by the arrow 12 in the FIGURE).
  • the gas channels 11 are configured as tubes.
  • the tube 11 is provided with an atomization device 13 which comprises feed lines 14 for liquid o-xylene and swirl nozzles 15 located at the end of the lines.
  • the feed lines 14 are fed by a supply tube (not shown) which concentrically surrounds the tube 11 .
  • the swirl nozzles 15 produce a hollow cone 16 of liquid o-xylene which breaks up into very fine droplets having a mean diameter of from 0.02 to 0.2 mm.
  • the fine droplets vaporize very quickly in the preheated air stream, so that a homogeneous mixture of air and o-xylene vapor is formed.
  • a static mixer 17 is installed in the tube 11 so that the vapor/air mixture is passed through this mixer. Downstream of the swirl nozzles 15 , the tube 11 is configured as a heatable double-walled tube 18 .
  • the tube is heated by means of steam to a temperature above the boiling point of o-xylene.
  • Droplets of atomized o-xylene which impinge on the tube wall are thus vaporized immediately and do not deposit as a liquid film.
  • the tube 11 opens into a shell-and-tube reactor in which phthalic anhydride is prepared by catalytic gas-phase oxidation of the o-xylene.
  • the apparatus for vaporizing o-xylene comprised a vertical “Thermoblech” tube having a diameter of 1200 mm.
  • the oxidation air which had been preheated to 200° C. in a preheating apparatus, was conveyed through this to the reactor.
  • the pressure was about 1.5 bar absolute.
  • the air was loaded with 100 g of o-xylene per standard m 3 .
  • the air was drawn in from the surroundings without particular purification, merely through an air filter.
  • the “Thermoblech” tube was heated to 214° C. by means of 20 bar steam.
  • the o-xylene was injected via six swirl nozzles which were arranged in a circle having a diameter of 600 mm and whose axis pointed vertically upward. These were axial hollow cone nozzles (KS 1 of the type 216.324 made of steel, from Lechler). The admission pressure was 8 bar. Static mixers were installed at a distance of 4.5 m downstream of the nozzles in a horizontal section of tube.
  • This swirl nozzle/hot wall mixer system produced a homogeneous, streaming-free o-xylene vapor/air mixture whose homogeneity was not upset by fluctuating operating parameters. This was established by means of the PA output which was constant over a long period of time. In addition, no ignitions within the production plant caused by inhomogeneities in the mixture and adversely affecting plant safety were observed. Damage or emergency shutdowns due to high temperatures in individual reactor regions or in reactor tubes were not observed. Between the annual routine maintenance shutdowns, the plant availability was above 99%.

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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)
US10/168,953 1999-12-23 2000-12-22 Method and device for production of a homogeneous mixture of a vapour-forming aromatic hydrocarbon and an oxygen-containing gas Abandoned US20030013931A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19962616.2 1999-12-23
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

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

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US20040240312A1 (en) * 2002-02-01 2004-12-02 Jean-Louis Gass Method and device for mixing gases
US20080197086A1 (en) * 2005-04-11 2008-08-21 Mosler Juergen Assembly for the Treatment of a Polymerizable Material
US20080308955A1 (en) * 2005-12-15 2008-12-18 Gerd Beckmann Apparatus for Mixing a Fluid with a Large Gas Stream, Especially for Introducing a Reducing Agent into a Flue Gas Containing Nitrogen Oxides
US20090003127A1 (en) * 2006-01-28 2009-01-01 Gerd Beckmann Method and Apparatus for Mixing a Gaseous Fluid With a Large Gas Stream, Especially for Introducing a Reducing Agent Into a Flue Gas That Contains Nitrogen Oxides
WO2009040246A1 (en) * 2007-09-28 2009-04-02 Exxonmobil Chemical Patents Inc. Improved vaporisation in oxidation to phthalic anhydride
US20110196159A1 (en) * 2007-09-28 2011-08-11 Nicolaas Anthony De Munck Improved Mixing In Oxidation To Phthalic Anhydride
US20140154148A1 (en) * 2008-04-22 2014-06-05 Fina Technology, Inc. Vaporization and Transportation of Alkali Metal Salts
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
US20150360837A1 (en) * 2014-06-12 2015-12-17 The Procter & Gamble Company Water soluble pouch comprising an embossed area
US20180315782A1 (en) * 2017-04-26 2018-11-01 The Japan Steel Works, Ltd. Method of manufacturing display, display, and liquid crystal television
KR20220073288A (ko) * 2020-11-26 2022-06-03 현대제철 주식회사 입자 및 가스 물질 처리장치

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DE102004052827B4 (de) * 2004-11-02 2010-05-06 Lurgi Gmbh Vorrichtung zur Erzeugung eines o-Xylol-Luft-Gemisches für die Phthalsäureanhydrid-Herstellung
CN107096405A (zh) * 2017-06-08 2017-08-29 江苏天宇石化冶金设备有限公司 一种高效气液混合器
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

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Cited By (19)

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Publication number Priority date Publication date Assignee Title
US20040240312A1 (en) * 2002-02-01 2004-12-02 Jean-Louis Gass Method and device for mixing gases
US20080197086A1 (en) * 2005-04-11 2008-08-21 Mosler Juergen Assembly for the Treatment of a Polymerizable Material
US8033531B2 (en) 2005-12-15 2011-10-11 Fisia Babcock Environment Gmbh Apparatus for mixing a fluid with a large gas stream, especially for introducing a reducing agent into a flue gas containing nitrogen oxides
US20080308955A1 (en) * 2005-12-15 2008-12-18 Gerd Beckmann Apparatus for Mixing a Fluid with a Large Gas Stream, Especially for Introducing a Reducing Agent into a Flue Gas Containing Nitrogen Oxides
US20090003127A1 (en) * 2006-01-28 2009-01-01 Gerd Beckmann Method and Apparatus for Mixing a Gaseous Fluid With a Large Gas Stream, Especially for Introducing a Reducing Agent Into a Flue Gas That Contains Nitrogen Oxides
US8517599B2 (en) 2006-01-28 2013-08-27 Fisia Babcock Environment Gmbh Method and apparatus for mixing a gaseous fluid with a large gas stream, especially for introducing a reducing agent into a flue gas that contains nitrogen oxides
WO2009040246A1 (en) * 2007-09-28 2009-04-02 Exxonmobil Chemical Patents Inc. Improved vaporisation in oxidation to phthalic anhydride
US20110230667A1 (en) * 2007-09-28 2011-09-22 Nicolaas Anthony De Munck Vaporization In Oxidation To Phthalic Anhydride
US20110196159A1 (en) * 2007-09-28 2011-08-11 Nicolaas Anthony De Munck Improved Mixing In Oxidation To Phthalic Anhydride
US8703974B2 (en) 2007-09-28 2014-04-22 Exxonmobil Chemical Patents Inc. Vaporization in oxidation to phthalic anhydride
US8968671B2 (en) 2007-09-28 2015-03-03 Exxonmobil Chemical Patents Inc. Mixing in oxidation to phthalic anhydride
US9156018B2 (en) 2007-09-28 2015-10-13 Exxonmobil Chemical Patents Inc. Vaporisation in oxidation to phthalic anhydride
US20140154148A1 (en) * 2008-04-22 2014-06-05 Fina Technology, Inc. Vaporization and Transportation of Alkali Metal Salts
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JP2003518433A (ja) 2003-06-10
ES2218265T3 (es) 2004-11-16
KR20020062374A (ko) 2002-07-25
AU2172001A (en) 2001-07-09
WO2001047622A1 (de) 2001-07-05
ATE262372T1 (de) 2004-04-15
DE19962616A1 (de) 2001-06-28
EP1239944B1 (de) 2004-03-24
EP1239944A1 (de) 2002-09-18
JP4669184B2 (ja) 2011-04-13
CN1411392A (zh) 2003-04-16
KR100655339B1 (ko) 2006-12-08
MXPA02005852A (es) 2002-10-23
MY125936A (en) 2006-09-29
CN1174793C (zh) 2004-11-10
DE50005821D1 (de) 2004-04-29

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