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WO2001087477A1 - Longitudinal flow reactor with a bundle of contact tubes - Google Patents

Longitudinal flow reactor with a bundle of contact tubes Download PDF

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Publication number
WO2001087477A1
WO2001087477A1 PCT/EP2001/004976 EP0104976W WO0187477A1 WO 2001087477 A1 WO2001087477 A1 WO 2001087477A1 EP 0104976 W EP0104976 W EP 0104976W WO 0187477 A1 WO0187477 A1 WO 0187477A1
Authority
WO
WIPO (PCT)
Prior art keywords
reactor
ring line
heat exchange
exchange medium
contact tubes
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.)
Ceased
Application number
PCT/EP2001/004976
Other languages
German (de)
French (fr)
Inventor
Gerhard Olbert
Franz Corr
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.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Priority to AU67400/01A priority Critical patent/AU6740001A/en
Priority to DE10191932T priority patent/DE10191932D2/en
Priority to JP2001583929A priority patent/JP2004518519A/en
Publication of WO2001087477A1 publication Critical patent/WO2001087477A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • B01J8/067—Heating or cooling the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/2415—Tubular reactors
    • B01J19/2425—Tubular reactors in parallel
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D7/16—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being arranged in parallel spaced relation
    • F28D7/1615—Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits being arranged in parallel spaced relation the conduits being inside a casing and extending at an angle to the longitudinal axis of the casing; the conduits crossing the conduit for the other heat exchange medium
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F13/00—Arrangements for modifying heat-transfer, e.g. increasing, decreasing
    • F28F13/003—Arrangements for modifying heat-transfer, e.g. increasing, decreasing by using permeable mass, perforated or porous materials
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F9/00—Casings; Header boxes; Auxiliary supports for elements; Auxiliary members within casings
    • F28F9/02—Header boxes; End plates
    • F28F9/0202—Header boxes having their inner space divided by partitions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094—Jackets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00103—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor in a heat exchanger separate from the reactor

Definitions

  • the invention relates to a reactor with a contact tube bundle, through the space surrounding the contact tubes, a heat exchange medium circuit is passed, and the use of the reactor for carrying out oxidation reactions.
  • the usual design of generic reactors consists of a, usually cylindrical container in which a bundle, i.e. H. a plurality of contact tubes, usually housed in a vertical arrangement. These contact tubes, which may contain supported catalysts, are sealed with their ends in tube sheets and each open into a hood connected to the container at the upper or lower end. The reaction mixture flowing through the catalyst tubes is supplied or discharged via these hoods. A heat exchange medium circuit is passed through the space surrounding the contact tubes in order to balance the heat balance, in particular in the case of reactions with a strong exotherm.
  • reactors with the largest possible number of contact tubes are used, the number of contact tubes accommodated often being in the range from 10,000 to 50,000.
  • the heat exchange medium circuit it is known to achieve a largely homogeneous temperature distribution of the heat exchange medium in each horizontal section of the reactor in order to involve all contact tubes as evenly as possible in the reaction process (e.g. DE-C 16 01 162).
  • the heat distribution or heat dissipation is used to smooth the temperature distribution each attached to the reactor ends outer ring lines with a plurality of jacket openings, as described for example in DE-C 34 09 159.
  • a further improvement in the heat transfer is achieved by installing deflection disks that alternately leave a passage cross section in the middle of the reactor and at the reactor edge.
  • deflection disks that alternately leave a passage cross section in the middle of the reactor and at the reactor edge.
  • Such an arrangement is particularly suitable for ring-shaped tube bundles with a free central space and is known, for example, from GB-B 31 01 75.
  • the pressure loss of the heat exchange medium is comparatively very large.
  • the eutectic salt melt of potassium nitrate and sodium nitrite which is frequently used to remove the heat released during oxidation reactions and which has a water-like viscosity at an application temperature of preferably approximately 250 ° C. to 400 ° C., must be fed into a reactor of the size mentioned above with a delivery head pumped from approx. 4 to 5 m to overcome the pressure loss.
  • the high pressure drop can be reduced by dispensing with the installation of deflection disks and thus the cross flow of the heat exchange medium. Dispensing with deflection disks results in a longitudinal flow of the heat exchange medium through the space surrounding the contact tubes. By braking the heat exchange medium on the tube walls, a flow profile is formed in the longitudinal direction, with the result that the heat transfer becomes increasingly poor, with negative effects on the selectivity of the reaction and the catalyst life.
  • the object of the invention was to provide a reactor with a longitudinal flow of the heat exchange medium, one ensures improved heat transfer on the tube walls of the contact tube bundle and does not have the above-mentioned shortcomings in reactors with longitudinal current guidance.
  • the solution is based on a reactor with a contact tube bundle, through the space surrounding the contact tubes, a heat exchange medium circuit is passed, with ring lines at both reactor ends with jacket openings for the supply and discharge of a heat exchange medium by means of one or more pumps, possibly with transfer of the heat exchange medium or a partial flow of the heat exchange medium via one or more external heat exchangers, the heat exchange medium being fed to the lower ring line and returned via the upper ring line to the pump (s), and with a throttle disk in the space surrounding the contact tubes at the level of the lower one and the upper ring line.
  • the invention is characterized in that packing elements are introduced into the space between the throttle disks.
  • the fillers introduced according to the invention disrupt the longitudinal flow of the heat exchange medium, in particular in the boundary layer on the tube walls which is particularly important for the heat transfer.
  • the heat transfer coefficient increases significantly, namely to values in the range of two to six times based on the same apparatus without packing.
  • fillers are introduced into the space through which the heat exchange medium flows, between the two throttle disks.
  • the heat exchange medium now flows through the openings and channels remaining between the packing elements, the heat exchange with the walls of the contact tubes being significantly improved by the packing elements.
  • the heat exchange medium usually a molten salt
  • the lower ring line is usually supplied via the lower ring line and discharged via the upper ring line.
  • the lower throttle plate is preferably arranged at the height of the upper end of the lower ring line and / or the upper throttle plate at the height of the lower end of the upper ring line , Because fillers are only introduced into the space between the two throttle disks, an empty space is thus available through which the heat exchange medium is largely uniform over Can distribute reactor cross-section.
  • the empty space below the lower and / or above the upper throttle plate is in the range of approximately 1/10 to 1/3 of the total cylindrical reactor length.
  • the packing elements can be metallic packings, as are known, for example, from distillation technology. However, it is also possible to use metal foams. It should always be noted that the heat exchange medium can still flow through the space filled with packing. It is also possible to insert fillers in the form of woven fabrics.
  • a preferably ceramic bulk material as the packing, in particular in the form of rings or balls.
  • Spherical fillers should have a diameter corresponding to the inequality d ⁇ (td a ) / 2, where t denotes the pitch, ie the center-to-center distance of two adjacent tubes, and d a the outer diameter of the contact tubes.
  • Spherical fillers with a diameter d of 2 to 10 mm are preferably used.
  • the reaction mixture is preferably preheated to the heat exchanger inlet temperature into the reactor by means of an external heat exchanger before it is fed to the reactor.
  • the reaction mixture and heat exchange medium are particularly preferably conducted in cocurrent.
  • the flow through the reactor is preferably from top to bottom. However, it is also possible to run the reaction mixture and heat exchange medium in countercurrent.
  • the heat exchange medium can be fed to the lower ring line and returned to the pump (s) via the upper ring line by dividing the upper and lower ring lines into an inner and an outer ring line by means of a cylinder-wall-shaped partition Heat exchange medium of the outer lower ring line, via an area outside the reactor of the inner upper ring line, via the jacket openings of which are fed to the space surrounding the contact tubes, via the jacket openings into the inner lower ring line and then via an area outside the reactor via the outer upper ring line.
  • the reactor is not limited in the type of heat exchange medium; this can also be used to remove heat, i. H. for conducting exothermic reactions, as well as for supplying heat to the reaction mixture flowing through the contact tubes, d. H. to carry out endothermic reactions.
  • the reactor is particularly suitable for carrying out oxidation reactions, in particular for producing phthalic anhydride, maleic anhydride, glyoxal, (meth) acrolein and (meth) acrylic acid.
  • oxidation reactions in particular for producing phthalic anhydride, maleic anhydride, glyoxal, (meth) acrolein and (meth) acrylic acid.
  • the single figure shows in the left half a reactor according to the invention with countercurrent flow of the reaction mixture and heat exchange medium and in the right half a particularly preferred embodiment with direct current flow of the reaction mixture and heat exchange medium, in each case from top to bottom through the reactor.
  • the reactor 1 shown schematically in longitudinal section, contains a vertical contact tube bundle 2, with a lower ring line 4, to which heat exchange medium is supplied, and with an upper ring line 3, via which heat exchange medium is discharged, the supply and discharge of the heat exchange medium via jacket openings 5 and 6 takes place, and with a lower throttle disk 7 and an upper throttle disk 8.
  • the space between the throttle disks is filled by fillers, which are shown in the drawing as hatching.
  • the upper ring line is separated by a cylinder jacket-shaped intermediate wall 9 into an inner upper ring line 11 and an outer upper ring line 12;
  • the lower ring line 4 is separated into an inner lower ring line 13 and an outer lower ring line 14 by means of the cylinder-wall-shaped intermediate wall 10.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Thermal Sciences (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Furan Compounds (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention relates to a reactor (1) comprising a bundle of contact tubes (2). A heat-exchanging medium is guided through the area surrounding the contact tubes. Both ends of the reactor have annular ducts (3,4) with jacket orifices (5,6) for supplying or educting a heat-exchanging medium by means of at least one pump, optionally transferring the heat-exchanging medium or a partial current of the heat-exchanging medium via at least one external heat exchanger. The heat-exchanging medium is fed to the lower annular duct (4) and is returned to the pump(s) via the upper annular duct (3). Throttle diaphragms (7,8) are situated in the area surrounding the contact tubes in the vicinity of the lower and upper annular duct (3, 4), filling bodies being placed in the area between the throttle diaphragms.

Description

Längsstromreaktor mit einem Kontaktrohrbündel Longitudinal flow reactor with a contact tube bundle

Die Erfindung betrifft einen Reaktor mit einem Kontaktrohrbündel, durch dessen die Kontaktrohre umgebenden Raum ein Wärmetauschmittelkreislauf geleitet wird sowie die Verwendung des Reaktors zur Durchfuhrung von Oxidationsreaktionen.The invention relates to a reactor with a contact tube bundle, through the space surrounding the contact tubes, a heat exchange medium circuit is passed, and the use of the reactor for carrying out oxidation reactions.

Die übliche Bauart gattungsgemäßer Reaktoren besteht aus einem, in der Regel zylinderförmigen Behälter, in dem ein Bündel, d. h. eine Vielzahl von Kontaktrohren, in üblicherweise vertikaler Anordnung untergebracht ist. Diese Kontaktrohre, die gegebenenfalls geträgerte Katalysatoren enthalten können, sind mit ihren Enden in Rohrböden abdichtend befestigt und münden in jeweils eine am oberen bzw. am unteren Ende mit dem Behälter verbundene Haube. Über diese Hauben wird das die Kontaktrohre durchströmende Reaktionsgemisch zu- bzw. abgeführt. Durch den die Kontaktrohre umgebenden Raum wird ein Wärmetauschmittelkreislauf geleitet, um die Wärmebilanz, insbesondere bei Reaktionen mit starker Wärmetönung, auszugleichen.The usual design of generic reactors consists of a, usually cylindrical container in which a bundle, i.e. H. a plurality of contact tubes, usually housed in a vertical arrangement. These contact tubes, which may contain supported catalysts, are sealed with their ends in tube sheets and each open into a hood connected to the container at the upper or lower end. The reaction mixture flowing through the catalyst tubes is supplied or discharged via these hoods. A heat exchange medium circuit is passed through the space surrounding the contact tubes in order to balance the heat balance, in particular in the case of reactions with a strong exotherm.

Aus wirtschaftlichen Gründen werden Reaktoren mit einer möglichst großen Zahl von Kontaktrohren eingesetzt, wobei die Zahl der untergebrachten Kontaktrohre häufig im Bereich von 10000 bis 50000 liegt.For economic reasons, reactors with the largest possible number of contact tubes are used, the number of contact tubes accommodated often being in the range from 10,000 to 50,000.

Bezüglich des Wärmetauschmittelkreislaufs ist es bekannt, in jedem waagerechten Schnitt des Reaktors eine weitgehend homogene Temperaturverteilimg des Warmetauschmittels zu realisieren, um möglichst alle Kontaktrohre gleichmäßig am Reaktionsgeschehen zu beteiligen (z . DE-C 16 01 162). Der Glättung der Temperaturverteilung dient die Wämezuführung bzw. Wärmeabfuhrung über jeweils an den Reaktorenden angebrachten äußeren Ringleitungen mit einer Vielzahl von Mantelöffnungen, wie sie beispielsweise in DE-C 34 09 159 beschrieben sind.With regard to the heat exchange medium circuit, it is known to achieve a largely homogeneous temperature distribution of the heat exchange medium in each horizontal section of the reactor in order to involve all contact tubes as evenly as possible in the reaction process (e.g. DE-C 16 01 162). The heat distribution or heat dissipation is used to smooth the temperature distribution each attached to the reactor ends outer ring lines with a plurality of jacket openings, as described for example in DE-C 34 09 159.

Eine weitere Verbesserung des Wärmeüberganges wird durch den Einbau von Umlenkscheiben erreicht, die abwechselnd in der Reaktormitte und am Reaktorrand einen Durchtrittsquerschnitt freilassen. Eine derartige Anordnung ist insbesondere für ringförmig angeordnete Rohrbündel mit einem freien zentralen Raum geeignet und beispielsweise aus GB-B 31 01 75 bekannt.A further improvement in the heat transfer is achieved by installing deflection disks that alternately leave a passage cross section in the middle of the reactor and at the reactor edge. Such an arrangement is particularly suitable for ring-shaped tube bundles with a free central space and is known, for example, from GB-B 31 01 75.

In großen Reaktoren mit einer Zahl von Kontaktrohren im oben angegebenen Bereich von etwa 10000 bis 50000, die zusätzlich mit Umlenkscheiben ausgestattet sind, ist der Druckverlust des Warmetauschmittels vergleichsweise sehr groß. So muß die zum Abtransport der bei Oxidationsreaktionen frei werdenden Wärme häufig verwendete eutektische Salzschmelze von Kaliumnitrat und Natriumnitrit, die bei einer Anwendungstemperatur von bevorzugt ca. 250°C bis 400°C eine wasserähnliche Viskosität aufweist, in einen Reaktor der oben erwähnten Größe mit einer Förderhöhe von ca. 4 bis 5 m gepumpt werden, um den Druckverlust zu überwinden.In large reactors with a number of contact tubes in the range from about 10,000 to 50,000, which are additionally equipped with deflection disks, the pressure loss of the heat exchange medium is comparatively very large. For example, the eutectic salt melt of potassium nitrate and sodium nitrite, which is frequently used to remove the heat released during oxidation reactions and which has a water-like viscosity at an application temperature of preferably approximately 250 ° C. to 400 ° C., must be fed into a reactor of the size mentioned above with a delivery head pumped from approx. 4 to 5 m to overcome the pressure loss.

Der hohe Druckverlust kann durch Verzicht auf den Einbau von Umlenkscheiben und somit auf die Querstromführung des Warmetauschmittels reduziert werden. Der Verzicht auf Umlenkscheiben ergibt eine Längsströmung des Warmetauschmittels durch den die Kontaktrohre umgebenden Raum. Durch Abbremsen des Warmetauschmittels an den Rohrwänden bildet sich ein Strömungsprofil in Längsrichtung aus mit der Folge, daß der Wärmeübergang zunehmend schlechter wird, mit negativen Auswirkungen auf die Selektivität der Reaktion und die Katalysatorstandzeit.The high pressure drop can be reduced by dispensing with the installation of deflection disks and thus the cross flow of the heat exchange medium. Dispensing with deflection disks results in a longitudinal flow of the heat exchange medium through the space surrounding the contact tubes. By braking the heat exchange medium on the tube walls, a flow profile is formed in the longitudinal direction, with the result that the heat transfer becomes increasingly poor, with negative effects on the selectivity of the reaction and the catalyst life.

Aufgabe der Erfindung war es demgegenüber, einen Reaktor mit Längsstromfuhrung des Warmetauschmittels zur Verfügung zu stellen, der einen verbesserten Wärmeübergang an den Rohrwänden des Kontaktrohrbündels gewährleistet und die oben genannten Mängel bei Reaktoren mit Längssttomführung nicht aufweist.In contrast, the object of the invention was to provide a reactor with a longitudinal flow of the heat exchange medium, one ensures improved heat transfer on the tube walls of the contact tube bundle and does not have the above-mentioned shortcomings in reactors with longitudinal current guidance.

Die Lösung geht aus von einem Reaktor mit einem Kontaktrohrbündel, durch dessen die Kontaktrohre umgebenden Raum ein Wärmetauschmittelkreislauf geleitet wird, mit Ringleitungen an beiden Reaktorenden mit Mantelöffnungen für die Zu- bzw. Abfnhrung eines W rmetauschmittels mittels einer oder mehrerer Pumpen gegebenenfalls unter Überleitung des Warmetauschmittels oder eines Teilstroms des Warmetauschmittels über einen oder mehrere außenliegende Wärmetauscher, wobei das Warmetauschmittel der unteren Ringleitung zugeführt und über die obere Ringleitung zur (zu den) Pumpe(n) zvjrückgeführt wird, sowie mit je einer Drosselscheibe im die Kontaktrohre umgebenden Raum auf der Höhe der unteren und der oberen Ringleitung.The solution is based on a reactor with a contact tube bundle, through the space surrounding the contact tubes, a heat exchange medium circuit is passed, with ring lines at both reactor ends with jacket openings for the supply and discharge of a heat exchange medium by means of one or more pumps, possibly with transfer of the heat exchange medium or a partial flow of the heat exchange medium via one or more external heat exchangers, the heat exchange medium being fed to the lower ring line and returned via the upper ring line to the pump (s), and with a throttle disk in the space surrounding the contact tubes at the level of the lower one and the upper ring line.

Die Erfindung ist dadurch gekennzeichnet, daß in den Raum zwischen den Drosselscheiben Füllkörper eingebracht sind.The invention is characterized in that packing elements are introduced into the space between the throttle disks.

Es wurde gefunden, daß durch Einbringen von Füllkörpern in den von Wärmetauschmitel durchströmten Raum zwischen den Drosselscheiben eine wesentliche Verbesserung des thermischen Übergangs und einer Vergleichmäßigung der Temperatur über den Reaktorquerschnitt mit der Folge einer verbesserten Selektivität der Reaktion, einer Absenkung des Hot-spots und somit eine Erhöhung der Katalysatorstandzeit erreicht werden konnte.It was found that by introducing packing elements into the space between the throttle disks through which heat exchange media flowed, a significant improvement in the thermal transition and an equalization of the temperature across the reactor cross section, with the result of improved selectivity of the reaction, a lowering of the hot spots and thus a Increased catalyst life could be achieved.

Die erfindungsgemäß eingebrachten Füllkörper stören die Längsströmung des Warmetauschmittels, insbesondere in der für den Wärmeübergang besonders wichtigen Grenzschicht an den Rohrwänden. Überraschend wurde gefunden, daß dabei der Wärmeübergangskoeffizient wesentlich ansteigt, und zwar auf Werte im Bereich des zwei- bis sechsfachen bezogen auf denselben Apparat ohne Füllkörper. Reaktoren mit einem Kontaktrohrbündel sowie mit einem Wärmetauschmittelkreislauf durch den Zwischenraum zwischen den Kontaktrohren, mit Abmhrung und Zxώϊhrung des Warmetauschmittels jeweils über eine Ringleitung an den beiden Reaktorenden sind bekannt. Bekannt ist auch, zur Vergleichmäßigung der Verteilung des Warmetauschmittels über den Reaktorquerschnitt nach der Zuleitung über die erste Ringleitung und vor der Ableitung über die zweite Ringleirung Drosselscheiben, d. h. in der Regel Lochbleche mit einer geeigneten Anzahl und Größe von Öffnungen für den Durchtritt und die Vergleichmäßigung der Strömung des Warmetauschmittels über den Reaktorquerschnitt vorzusehen.The fillers introduced according to the invention disrupt the longitudinal flow of the heat exchange medium, in particular in the boundary layer on the tube walls which is particularly important for the heat transfer. Surprisingly, it was found that the heat transfer coefficient increases significantly, namely to values in the range of two to six times based on the same apparatus without packing. Reactors with a contact tube bundle and with a heat exchange medium circuit through the space between the contact tubes, with a reduction and supply of the heat exchange medium, in each case via a ring line at the two reactor ends, are known. It is also known to equalize the distribution of the heat exchange medium over the reactor cross-section after the feed line via the first ring line and before the discharge via the second ring throttle disks, that is, as a rule, perforated plates with a suitable number and size of openings for the passage and the equalization of the Provide flow of the heat exchange medium over the reactor cross section.

Erfindungsgemäß werden in den von Warmetauschmittel durchströmten Raum zwischen den beiden Drosselscheiben Füllkörper eingebracht. Das Warmetauschmittel durchströmt nun die zwischen den Füllkörpern verbleibenden Öffnungen und Kanäle, wobei der Wärmeaustausch mit den Wänden der Kontaktrohre durch die Füllkörper bedeutend verbessert ist.According to the invention, fillers are introduced into the space through which the heat exchange medium flows, between the two throttle disks. The heat exchange medium now flows through the openings and channels remaining between the packing elements, the heat exchange with the walls of the contact tubes being significantly improved by the packing elements.

Bei großen Reaktoren, d. h. mit Kontaktrohren im angegebenen Bereich von etwa 10000 bis 50000, wird das Warmetauschmittel, in der Regel eine Salzschmelze üblicherweise über die untere Ringleitung zugeführt und über die obere Ringleitung abgeführt.For large reactors, i.e. H. with contact tubes in the specified range from about 10,000 to 50,000, the heat exchange medium, usually a molten salt, is usually supplied via the lower ring line and discharged via the upper ring line.

Um eine verbesserte Verteilung des Warmetauschmittels über den Reaktorquerschnitt und somit eine verbesserte Isothermie über den Reaktorquerschnitt zu gewährleisten, wird bevorzugt die untere Drosselscheibe auf der Höhe des oberen Endes der unteren Ringleitung und/oder die obere Drosselscheibe auf der Höhe des unteren Endes der oberen Ringleitung angeordnet. Dadurch, daß Füllkörper lediglich in den Raum zwischen den beiden Drosselscheiben eingebracht werden, steht somit ein Leerraum zur Verfügung, über den sich das Warmetauschmittel weitgehend gleichmäßig über den Reaktorquerschnitt verteilen kann. Der leere Raum unterhalb der unteren und/oder oberhalb der oberen Drosselscheibe liegt jeweils im Bereich von ca. 1/10 bis 1/3 der gesamten zylindrischen Reaktorlänge.In order to ensure an improved distribution of the heat exchange medium over the reactor cross section and thus an improved isothermal energy over the reactor cross section, the lower throttle plate is preferably arranged at the height of the upper end of the lower ring line and / or the upper throttle plate at the height of the lower end of the upper ring line , Because fillers are only introduced into the space between the two throttle disks, an empty space is thus available through which the heat exchange medium is largely uniform over Can distribute reactor cross-section. The empty space below the lower and / or above the upper throttle plate is in the range of approximately 1/10 to 1/3 of the total cylindrical reactor length.

Die Füllkörper können in einer bevorzugten Ausführungsvariante metallische Packungen sein, wie sie beispielsweise aus der Destillationstechnik bekannt sind. Es ist jedoch auch möglich, Metallschäume einzusetzen. Dabei ist stets zu beachten, daß das Warmetauschmittel den mit Füllkörper gefüllten Raum noch durchströmen kann. Weiterhin ist es möglich, Füllkörper in Form von Geweben einzubringen.In a preferred embodiment, the packing elements can be metallic packings, as are known, for example, from distillation technology. However, it is also possible to use metal foams. It should always be noted that the heat exchange medium can still flow through the space filled with packing. It is also possible to insert fillers in the form of woven fabrics.

In einer weiteren Ausführungsvariante ist es möglich, als Füllkörper ein bevorzugt keramisches Schüttgut einzubringen, insbesondere in Form von Ringen oder Kugeln. Kugelförmige Füllkörper sollen einen Durchmesser entsprechend der Ungleichung d<(t-da)/2, wobei t die Teilung, d. h. den Mittelpunktsabstand zweier benachbarter Rohre und da den Außendurchmesser der Kontaktrohre bezeichnet.In a further embodiment variant, it is possible to introduce a preferably ceramic bulk material as the packing, in particular in the form of rings or balls. Spherical fillers should have a diameter corresponding to the inequality d <(td a ) / 2, where t denotes the pitch, ie the center-to-center distance of two adjacent tubes, and d a the outer diameter of the contact tubes.

Bevorzugt werden kugelförmige Füllkörper mit einem Durchmesser d von 2 bis 10 mm eingesetzt.Spherical fillers with a diameter d of 2 to 10 mm are preferably used.

Gemäß einer weiteren AusfLihrungsvariante ist es möglich, die Isothermie über den Reaktorquerschnitt dadurch weiter zu verbessern, das im Zentralbereich des Reaktors über die gesamte Reaktorhöhe, ein Raum ohne Reaktion vorgesehen ist, insbesondere mittels Einbringen eines Dummy-Körpers in den zentralen Bereich des Reaktors im Raum zwischen den Kontaktrohren und oder mittels Blindrohren im zentralen Bereich des Reaktors. In bevorzugter Weise wird das Reaktionsgemisch vor der Zuführung zum Reaktor mittels eines außen liegenden Wärmetauschers auf die Wärmetauschmitteleintrittstemperatur in den Reaktor vorgewärmt.According to a further embodiment variant, it is possible to further improve the isothermal energy over the reactor cross-section by providing a space without reaction in the central area of the reactor over the entire reactor height, in particular by introducing a dummy body into the central area of the reactor in the room between the contact tubes and or by means of dummy tubes in the central area of the reactor. The reaction mixture is preferably preheated to the heat exchanger inlet temperature into the reactor by means of an external heat exchanger before it is fed to the reactor.

Besonders bevorzugt werden Reaktionsgemisch und W rmetauschmittel im Gleichstrom geführt. Dabei wird der Reaktor bevorzugt von oben nach unten durchströmt. Es ist jedoch auch möglich, Reaktionsgemisch und Warmetauschmittel im Gegenstrom zu führen.The reaction mixture and heat exchange medium are particularly preferably conducted in cocurrent. The flow through the reactor is preferably from top to bottom. However, it is also possible to run the reaction mixture and heat exchange medium in countercurrent.

In besonders geeigneter Weise kann das Warmetauschmittel der unteren Ringleitung zugeführt und über die obere Ringleitung zu der (den) Pumpe(n) zurückgeführt werden, indem die obere und untere Ringleitung jeweils mittels einer zylindermantelförmigen Zwischenwand in eine innere und eine äußere Ringleitung geteilt werden und das Warmetauschmittel der äußeren unteren Ringleitung, über einen Bereich außerhalb des Reaktors der inneren oberen Ringleitung, über deren Mantelöffnungen dem die Kontaktrohre umgebenden Raum zugeführt über die Mantelöffnungen in die innere untere Ringleitung und anschließend über einen Bereich außerhalb des Reaktors über die äußere obere Ringleitung abgeführt wird.In a particularly suitable manner, the heat exchange medium can be fed to the lower ring line and returned to the pump (s) via the upper ring line by dividing the upper and lower ring lines into an inner and an outer ring line by means of a cylinder-wall-shaped partition Heat exchange medium of the outer lower ring line, via an area outside the reactor of the inner upper ring line, via the jacket openings of which are fed to the space surrounding the contact tubes, via the jacket openings into the inner lower ring line and then via an area outside the reactor via the outer upper ring line.

Der Reaktor ist nicht eingeschränkt bezüglich der Art des Warmetauschmittels; dieses kann gleichermaßen zur Abfiihrung von Wärme, d. h. zur Durcriführung exothermer Reaktionen, wie auch für die Zuführung von Wärme an das die Kontaktrohre durchströmende Reaktionsgemisch, d. h. zur Durchführung endothermer Reaktionen, eingesetzt werden.The reactor is not limited in the type of heat exchange medium; this can also be used to remove heat, i. H. for conducting exothermic reactions, as well as for supplying heat to the reaction mixture flowing through the contact tubes, d. H. to carry out endothermic reactions.

Der Reaktor ist besonders geeignet zur Dirrchfuhrung von Oxidatonsreaktionen, insbesondere zur Herstellung von Phthalsäureanhydrid, Malemsäureanhydrid, Glyoxal, (Meth)acrolein und (Meth)acrylsäure. Die Erfindung wird im folgenden anhand einer Zeichnung und eines Ausfuhrungsbeispiels näher erläutert.The reactor is particularly suitable for carrying out oxidation reactions, in particular for producing phthalic anhydride, maleic anhydride, glyoxal, (meth) acrolein and (meth) acrylic acid. The invention is explained in more detail below with reference to a drawing and an exemplary embodiment.

Die einzige Figur zeigt in der linken Hälfte einen erfindungsgemäßen Reaktor mit Gegenstromführung von Reaktionsgemisch und Warmetauschmittel und in der rechten Hälfte eine besonders bevorzugte Ausführungsvariante mit Gleichstromführung von Reaktionsgemisch und Warmetauschmittel, jeweils von oben nach unten durch den Reaktor.The single figure shows in the left half a reactor according to the invention with countercurrent flow of the reaction mixture and heat exchange medium and in the right half a particularly preferred embodiment with direct current flow of the reaction mixture and heat exchange medium, in each case from top to bottom through the reactor.

Der im Längsschnitt schematisch dargestellte Reaktor 1 enthält ein vertikales Kontaktrohrbündel 2, mit unterer Ringleitung 4, der Warmetauschmittel zugeführt wird, sowie mit oberer Ringleitung 3, über die Warmetauschmittel abgeführt wird, wobei die Zu- bzw. Abführung des Warmetauschmittels über Mantelöffnungen 5 bzw. 6 erfolgt, sowie mit einer unteren Drosselscheibe 7 und einer oberen Drosselscheibe 8. Erfindungsgemäß ist der Raum zwischen den Drosselscheiben durch Füllkörper, die in der Zeichnung als Schraffur dargestellt sind, gefüllt.The reactor 1, shown schematically in longitudinal section, contains a vertical contact tube bundle 2, with a lower ring line 4, to which heat exchange medium is supplied, and with an upper ring line 3, via which heat exchange medium is discharged, the supply and discharge of the heat exchange medium via jacket openings 5 and 6 takes place, and with a lower throttle disk 7 and an upper throttle disk 8. According to the invention, the space between the throttle disks is filled by fillers, which are shown in the drawing as hatching.

In der bevorzugten Ausführungsvariante gemäß der rechten Seite der schematischen Darstellung in der Figur ist die obere Ringleitung durch eine zylindermantelförmige Zwischenwand 9 in eine innere obere Ringleitung 11 und eine äußere obere Ringleitung 12 getrennt; analog ist die untere Ringleitung 4 mittels der zylindermantelförrnigen Zwischenwand 10 in eine innere untere Ringleitung 13 und eine äußere untere Ringleitung 14 getrennt.In the preferred embodiment variant according to the right-hand side of the schematic illustration in the figure, the upper ring line is separated by a cylinder jacket-shaped intermediate wall 9 into an inner upper ring line 11 and an outer upper ring line 12; Similarly, the lower ring line 4 is separated into an inner lower ring line 13 and an outer lower ring line 14 by means of the cylinder-wall-shaped intermediate wall 10.

In einem Reaktor zur Herstellung von Glyoxal wurde durch Einbringen von Pall-In a reactor for the production of glyoxal, pallets were introduced by

Ringen in den Zwischenraum zwischen den Kontaktrohren der Wert desWrestling in the space between the contact tubes the value of the

Wärmeübergangskoeffizienten verdoppelt, der Hot-spot um 40°C abgesenkt und die Ausbeute um 2 % angehoben. Durch die bessere Temperaturverteilung konnte der Reaktor mit höherer Belastung gefahren werden; die Kapazitätserhöhung betrag 10 bis 15 %. Heat transfer coefficient doubled, the hot spot lowered by 40 ° C and the yield increased by 2%. Because of the better temperature distribution the reactor is operated with higher loads; the capacity increase was 10 to 15%.

Claims

Patentansprüche claims 1. Reaktor (1) mit einem Kontaktrohrbündel (2), durch dessen die Kontaktrohre umgebenden Raum ein Wäfmetauschmittelkreislauf geleitet wird, mit Ringleitungen (3, 4) an beiden Reaktorenden mit Mantelöffnungen (5, 6) für die Zu- bzw. Abführung eines Warmetauschmittels mittels einer oder mehrerer Pumpen gegebenenfalls unter Überleitung des Warmetauschmittels oder eines Teilstroms des Warmetauschmittels über einen oder mehrere außenliegende Wärmetauscher, wobei das1. Reactor (1) with a contact tube bundle (2), through the space surrounding the contact tubes of which a heat exchange medium circuit is passed, with ring lines (3, 4) at both reactor ends with jacket openings (5, 6) for the supply and discharge of a heat exchange medium by means of one or more pumps, optionally with the heat exchange medium or a partial flow of the heat exchange medium being transferred via one or more external heat exchangers, the Warmetauschmittel der unteren Ringleitung (4) zugeführt und über die obere Ringleitung (3) zur (zu den ) Pumpe(n) zurückgeführt wird, sowie mit je einer Drosselscheibe (7, 8) im die Kontaktrohre umgebenden Raum auf der Höhe der unteren und der oberen Ringleitung (3, 4), dadurch gekennzeichnet, daß in den Raum zwischen den Drosselscheiben (7, 8)Heat exchange medium is fed to the lower ring line (4) and is returned via the upper ring line (3) to the pump (s), as well as with a throttle disc (7, 8) in the space surrounding the contact tubes at the level of the lower and the upper ring line (3, 4), characterized in that in the space between the throttle discs (7, 8) Füllkörper eingebracht sind.Packings are introduced. 2. Reaktor nach Anspruch 1, dadurch gekennzeichnet, daß die untere Drosselscheibe (7) auf der Höhe des oberen Endes der unteren Ringleitung (4) und/oder die obere Drosselscheibe (8) auf der Höhe des unteren Endes der oberen Ringleitung (3) angeordnet ist.2. Reactor according to claim 1, characterized in that the lower throttle plate (7) at the level of the upper end of the lower ring line (4) and / or the upper throttle plate (8) at the level of the lower end of the upper ring line (3) is arranged. 3. Reaktor nach Ansprach 1 oder 2, dadurch gekennzeichnet, daß die Füllkörper metallische Packungen sind.3. Reactor according spoke 1 or 2, characterized in that the packing elements are metallic packings. 4. Reaktor nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß die Füllkörper ein bevorzugt keramisches Schüttgut sind, insbesondere in Form von Ringen oder Kugeln.4. Reactor according to claim 1 or 2, characterized in that the packing is a preferably ceramic bulk material, in particular in the form of rings or balls. 5. Reaktor nach Anspruch 4, dadurch gekennzeichnet, daß kugelförmige Füllkörper mit einem Durchmesser von 2 bis 10 mm eingesetzt werden. 5. Reactor according to claim 4, characterized in that spherical packing with a diameter of 2 to 10 mm are used. 6. Reaktor nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß im Zentralbereich des Reaktors, über die gesamte Reaktorhöhe, ein Raum ohne Reaktion vorgesehen ist, insbesondere mittels Einbringen eines Dummy-Körpers in den zentralen Bereich des Reaktors im Raum zwischen den Kontaktrohren und /oder mittels Blindrohren im zentralen Bereich des Reaktors.6. Reactor according to one of claims 1 to 5, characterized in that in the central region of the reactor, over the entire reactor height, a space without reaction is provided, in particular by introducing a dummy body into the central region of the reactor in the space between the contact tubes and / or by means of blind pipes in the central area of the reactor. 7. Reaktor nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß das Reaktionsgemisch vor dessen Zuleitung in die Kontaktrohre auf die7. Reactor according to one of claims 1 to 6, characterized in that the reaction mixture before being fed into the catalyst tubes on the Wärmetauschmitteleintrittstemperatur in den Reaktor vorgewärmt wird.Heat exchanger inlet temperature is preheated in the reactor. 8. Reaktor nach einem der Ansprüche 1 bis 7, gekennzeichnet durch eine Gleichstrornführung von Reaktionsgemisch und Warmetauschmittel.8. Reactor according to one of claims 1 to 7, characterized by a DC flow of the reaction mixture and heat exchange medium. 9. Reaktor nach Anspruch 8, dadurch gekennzeichnet, daß das Reaktionsgemisch von oben nach unten durch die Kontakrohre geführt wird und daß das Warmetauschmittel der unteren Ringleitung (4) zugeführt und über die obere Ringleitung (3) zu der(n) Pumpe(n) zurückgeführt wird, wobei die obere (3) und untere (4) Ringleitung jeweils mittels einer zylindermantelförmigen Zwischenwand (9, 10) in eine innere (11, 13) und eine äußere (12, 14) Ringleitung geteilt sind, und daß das Warmetauschmittel der äußeren unteren Ringleitung (14), über einen Bereich außerhalb des Reaktors der inneren oberen Ringleitung (11), über deren Mantelöffnungen (5) dem die Kontakrohre (2) umgebenden Raum zugeführt, über die Mantelöffnungen (6) in die innere untere Ringleitung (13) und anschließend über einen Bereich außerhalb des Reaktors über die äußere obere Ringleitung (12) abgeführt wird.9. Reactor according to claim 8, characterized in that the reaction mixture is passed from top to bottom through the contact tubes and that the heat exchange medium is fed to the lower ring line (4) and via the upper ring line (3) to the (n) pump (s) is returned, wherein the upper (3) and lower (4) ring line are each divided into an inner (11, 13) and an outer (12, 14) ring line by means of a cylindrical wall-shaped partition (9, 10), and that the heat exchange medium outer lower ring line (14), via an area outside the reactor of the inner upper ring line (11), via its jacket openings (5) to the space surrounding the contact tubes (2), via the jacket openings (6) into the inner lower ring line (13 ) and then discharged over an area outside the reactor via the outer upper ring line (12). 10. Verwendung des Reaktors nach einem der Ansprüche 1 bis 9 zur Durchf hrung von Oxidationsreaktionen, insbesondere zur Herstellung von Phthalsäureanhydrid, Maleinsäureanhydrid, Glyoxal, (Meth)acrolein oder (Meth)acrylsäure. 10. Use of the reactor according to one of claims 1 to 9 for carrying out oxidation reactions, in particular for the production of Phthalic anhydride, maleic anhydride, glyoxal, (meth) acrolein or (meth) acrylic acid.
PCT/EP2001/004976 2000-05-17 2001-05-03 Longitudinal flow reactor with a bundle of contact tubes Ceased WO2001087477A1 (en)

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AU67400/01A AU6740001A (en) 2000-05-17 2001-05-03 Longitudinal flow reactor with a bundle of contact tubes
DE10191932T DE10191932D2 (en) 2000-05-17 2001-05-03 Longitudinal flow reactor with a contact tube bundle
JP2001583929A JP2004518519A (en) 2000-05-17 2001-05-03 Long reactor with multiple catalyst tubes

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DE10024348.7 2000-05-17
DE2000124348 DE10024348A1 (en) 2000-05-17 2000-05-17 Reactor having a contact tube bundle, useful for oxidation reactions, contains a throttle disk with filler particles contained within the cavity between the throttle disks.

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Publication number Priority date Publication date Assignee Title
FR2968388A1 (en) * 2010-12-07 2012-06-08 Valeo Systemes Thermiques HEAT EXCHANGER, IN PARTICULAR FOR A MOTOR VEHICLE

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US7115776B2 (en) 2002-07-18 2006-10-03 Basf Aktiengesellschaft Heterogeneously catalyzed gas-phase partial oxidation of at least one organic compound

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EP0042613A2 (en) * 1980-06-24 1981-12-30 Richard Adolf Holl Apparatus and process for heat transfer
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JPS6222991A (en) * 1985-07-22 1987-01-31 Toshiba Corp Multi-tubular heat exchanger
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EP0042613A2 (en) * 1980-06-24 1981-12-30 Richard Adolf Holl Apparatus and process for heat transfer
JPS6111133A (en) * 1984-06-26 1986-01-18 Toshiba Corp Endothermic reaction device
JPS6222991A (en) * 1985-07-22 1987-01-31 Toshiba Corp Multi-tubular heat exchanger
DE19836792A1 (en) * 1998-08-13 2000-02-17 Basf Ag Tube bundle reactor, for oxidation reactions, has partitioned headers allowing heat exchange medium supply to the lower header to be combined with co-current passage within the reactor

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2968388A1 (en) * 2010-12-07 2012-06-08 Valeo Systemes Thermiques HEAT EXCHANGER, IN PARTICULAR FOR A MOTOR VEHICLE
EP2463610A1 (en) * 2010-12-07 2012-06-13 Valeo Systemes Thermiques Heat exchanger, in particular for an automobile

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