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WO2005118125A1 - Method for measuring the even charge of reactors with solid bodies - Google Patents

Method for measuring the even charge of reactors with solid bodies Download PDF

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Publication number
WO2005118125A1
WO2005118125A1 PCT/EP2005/004714 EP2005004714W WO2005118125A1 WO 2005118125 A1 WO2005118125 A1 WO 2005118125A1 EP 2005004714 W EP2005004714 W EP 2005004714W WO 2005118125 A1 WO2005118125 A1 WO 2005118125A1
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WO
WIPO (PCT)
Prior art keywords
reactors
gas
measuring
solids
flow
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/EP2005/004714
Other languages
German (de)
French (fr)
Inventor
Achim Fischer
Werner Burkhardt
Jan-Olaf Barth
Christoph Weckbecker
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.)
Evonik Operations GmbH
Original Assignee
Degussa GmbH
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 Degussa GmbH filed Critical Degussa GmbH
Publication of WO2005118125A1 publication Critical patent/WO2005118125A1/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
    • B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
    • 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
    • B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of 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
    • 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
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00539—Pressure
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00743—Feeding or discharging of solids
    • B01J2208/00769—Details of feeding or discharging
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796—Details of the reactor or of the particulate material
    • B01J2208/00805—Details of the particulate material
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/02—Processes carried out in the presence of solid particles; Reactors therefor with stationary particles
    • B01J2208/021—Processes carried out in the presence of solid particles; Reactors therefor with stationary particles comprising a plurality of beds with flow of reactants in parallel
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/02—Processes carried out in the presence of solid particles; Reactors therefor with stationary particles
    • B01J2208/021—Processes carried out in the presence of solid particles; Reactors therefor with stationary particles comprising a plurality of beds with flow of reactants in parallel
    • B01J2208/022—Plate-type reactors filled with granular catalyst

Definitions

  • the invention relates to a method for measuring the uniform filling of reactors or columns with solids and an apparatus for performing the method.
  • the uniform filling of reactors with solids is of crucial importance for the performance efficiency of the apparatus.
  • the solids are fillers or catalysts.
  • These solids can have different compositions and geometries. It can be balls, solid or hollow cylinders or rings, but other geometries are also possible.
  • the invention relates to a method for measuring the uniform filling of reactors with solids, the reactors being constructed in such a way that at least two separate gas and liquid streams with the same compositions flow through them, and the measurement is carried out in such a way that the filling with the solids
  • Tube reactors or reactors with reaction and heat transport spaces separated from one another by thermal sheets are particularly common as reactors.
  • the columns are, for example, absorption columns.
  • Inert gases air or mixtures thereof are generally used as gases.
  • the solid bed represents a resistance for the gas flow, through which the flow velocity is reduced and a back pressure builds up.
  • the volume flow of the gas should generally have a flow rate of 250 to 5000 l / h, the admission pressure of the gas should be in the range from 1 bar to 50 bar, in particular from 1 to 10 bar, and the temperature of the gas generally in the range of 10 up to 50 ° C. Inert gases, air or mixtures of these are ideally suitable.
  • a device with a structure as shown in Figure 1 is used, in which a corresponds to the number of parallel gas lines.
  • the dosage is considered constant if the
  • Flow rate of the gas fluctuates with less than +/- 2.5%, flow rates with a variation of less than or equal to +/- 1% are particularly suitable.
  • the dynamic pressure is advantageously measured in up to 15 parallel gas lines, in particular up to 10, particularly advantageously up to 5. Surrender different measured values, the filling with the catalysts used as solids, for example, is not uniform and must be improved.
  • the measurement of several gas flows possible simultaneously according to the invention enables a time-saving method for checking the filling of reactors.
  • a variance of up to + 5% is considered to be uniform.
  • the gas flow coming from the apparatus shown in Figure 1 is passed through the solid-state packing to be examined via an apparatus as shown in Figure 2.
  • the dynamic pressures generated are measured using a commercially available pressure transducer, for example from Ashcroft Inc., which is ideally mounted on the gas inlet device as shown in FIG. 2.
  • the pressure range of the transducer should range from 0 to 2500 mbar, but in particular from 0 to 1000 mbar.
  • the determined print data are forwarded to an electronic memory, which can hold up to 60,000 print data. This
  • Data storage should ideally be housed in a device with the pressure transducer.
  • the method is not limited to measuring the dynamic pressure as a measure of the flow resistance.
  • the gas flow can be measured as volume flow or mass flow. Brief description of the pictures

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Measuring Volume Flow (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The invention relates to a method for measuring the even charge of reactors or columns with solid bodies and to a device for carrying out said method.

Description

Verfahren zur Messung der gleichmäßigen Befüllung von Reaktoren mit Festkörpern Method for measuring the uniform filling of reactors with solids

Die Erfindung betrifft ein Verfahren zur Messung der gleichmäßigen Befüllung von Reaktoren oder Kolonnen mit Festkörpern und eine Apparatur zur Durchführung des Verfahrens .The invention relates to a method for measuring the uniform filling of reactors or columns with solids and an apparatus for performing the method.

In der chemischen Reaktionstechnik ist die gleichmäßige Befüllung von Reaktoren mit Festkörpern von entscheidender Bedeutung für die Leistungseffizienz des Apparates. Beispielsweise handelt es sich bei den Festkörpern um Füllkörper oder Katalysatoren.In chemical reaction technology, the uniform filling of reactors with solids is of crucial importance for the performance efficiency of the apparatus. For example, the solids are fillers or catalysts.

Diese Festkörper können unterschiedliche Zusammensetzungen und Geometrien besitzen. Es können Kugeln, Voll- oder Hohlzylinder oder Ringe sein, aber andere Geometrien sind ebenfalls möglich.These solids can have different compositions and geometries. It can be balls, solid or hollow cylinders or rings, but other geometries are also possible.

Setzt man diese Festkörper zum Beispiel in Rohrbündelreaktoren oder Plattenreaktoren für katalysierte Umsetzungen ein, so stellt sich die Aufgabe, die gleichmäßige Befüllung dieser Reaktoren zu gewährleisten.If these solids are used, for example, in tube bundle reactors or plate reactors for catalyzed reactions, the task is to ensure that these reactors are filled evenly.

Gegenstand der Erfindung ist ein Verfahren zur Messung der gleichmäßigen Befüllung von Reaktoren mit Festkörpern, wobei die Reaktoren so aufgebaut sind, dass sie von mindestens zwei getrennt geführten Gas- und Flüssigkeitsströmen mit denselben Zusammensetzungen durchflössen werden, und die Messung so vorgenommen wird, dass man nach der Befüllung mit den FestkörpernThe invention relates to a method for measuring the uniform filling of reactors with solids, the reactors being constructed in such a way that at least two separate gas and liquid streams with the same compositions flow through them, and the measurement is carried out in such a way that the filling with the solids

a) in mindestens zwei der getrennt angebrachten Gas- oder Flüssigkeitseinlässe gleichzeitig Gas oder Flüssigkeit mit jeweils den gleichen Mengenflüssen und Drucken einleitet,a) simultaneously introduces gas or liquid with the same volume flows and pressures into at least two of the separately installed gas or liquid inlets,

b) an jedem der Einlasse gleichzeitig den Strömungswiderstand mißt und c) die ermittelten Werte zentral registriert.b) simultaneously measures the flow resistance at each of the inlets and c) the determined values are registered centrally.

Als Reaktoren besonders gebräuchlich sind Rohrbündelreaktoren oder Reaktoren mit voneinander durch Thermobleche getrennten Reaktions- und Wärmetransporträumen.Tube reactors or reactors with reaction and heat transport spaces separated from one another by thermal sheets are particularly common as reactors.

Bei den Kolonnen handelt es sich beispielsweise um Absorptionskolonnen.The columns are, for example, absorption columns.

Als Gase werden im allgemeinen inerte Gase, Luft oder Gemische daraus eingesetzt.Inert gases, air or mixtures thereof are generally used as gases.

Die Festkörperschüttung stellt für den Gasstrom einen Widerstand dar, durch den die Flussgeschwindigkeit vermindert wird und sich ein Staudruck aufbaut.The solid bed represents a resistance for the gas flow, through which the flow velocity is reduced and a back pressure builds up.

Hierbei ist entscheidend, dass ein konstanter Volumenstrom durch die Festkörperschüttung geleitet wird. Der Volumenstrom des Gases sollte im allgemeinen eine Flussrate von 250 bis 5000 1/h besitzen, der Vordruck des Gases sollte im Bereich von 1 barü bis 50 barü, insbesondere von 1 bis 10 barü liegen, die Temperatur des Gases im allgemeinen im Bereich von 10 bis 50°C. Idealerweise eignen sich Inertgase, Luft oder Gemische aus diesen.It is crucial that a constant volume flow is passed through the solid bed. The volume flow of the gas should generally have a flow rate of 250 to 5000 l / h, the admission pressure of the gas should be in the range from 1 bar to 50 bar, in particular from 1 to 10 bar, and the temperature of the gas generally in the range of 10 up to 50 ° C. Inert gases, air or mixtures of these are ideally suitable.

Zur konstanten Dosierung der Gase wird beispielsweise eine Vorrichtung mit einem Aufbau, wie er in Abbildung 1 gezeigt ist, benutzt, in der a der Zahl der parallelen Gaslinien entspricht.For constant dosing of the gases, for example, a device with a structure as shown in Figure 1 is used, in which a corresponds to the number of parallel gas lines.

Die Dosierung wird als konstant angesehen, wenn dieThe dosage is considered constant if the

Flussrate des Gases mit weniger als +/-2,5 % schwankt, besonders geeignet sind Flussraten mit einer Schwankung von kleiner gleich +/- 1%.Flow rate of the gas fluctuates with less than +/- 2.5%, flow rates with a variation of less than or equal to +/- 1% are particularly suitable.

Vorteilhaft wird zum Beispiel der Staudruck in bis zu 15 parallelen Gaslinien, insbesondere bis zu 10, besonders vorteilhaft bis zu 5 gemessen. Ergeben sich unterschiedliche Messwerte, ist die Befüllung mit den als Festkörpern zum Beispiel eingesetzten Katalysatoren nicht gleichmäßig und muss nachgebessert werden.For example, the dynamic pressure is advantageously measured in up to 15 parallel gas lines, in particular up to 10, particularly advantageously up to 5. Surrender different measured values, the filling with the catalysts used as solids, for example, is not uniform and must be improved.

Die erfindungsgemäß mögliche Messung mehrerer Gasdurchflüsse gleichzeitig ermöglicht eine zeitsparende Methode zur Überprüfung der Befüllung von Reaktoren.The measurement of several gas flows possible simultaneously according to the invention enables a time-saving method for checking the filling of reactors.

Als gleichmäßig wird eine Varianz von bis zu + 5 % angesehen.A variance of up to + 5% is considered to be uniform.

Zur Messung des Staudruckes wird der beispielsweise der aus der Apparatur gemäß Abbildung 1 kommende Gasstrom über eine Apparatur wie sie in Abbildung 2 dargestellt ist durch die zu untersuchende Festkörperpackung geleitet. Die erzeugten Staudrücke werden mit einem handelsüblichen Druckaufnehmer, beispielsweise der Firma Ashcroft Inc. gemessen, der idealerweise auf der GaseinieitungsVorrichtung wie sie in der Abbildung 2 gezeigt ist, montiert ist. Der Druckbereich des Aufnehmers soll von 0 bis 2500 mbarü, insbesondere aber von 0 bis 1000 mbarü reichen. Die ermittelten Druckdaten werden an einen elektronischen Speicher weitergegeben, der bis zu 60000 Druckdaten aufnehmen kann. DieserTo measure the dynamic pressure, the gas flow coming from the apparatus shown in Figure 1, for example, is passed through the solid-state packing to be examined via an apparatus as shown in Figure 2. The dynamic pressures generated are measured using a commercially available pressure transducer, for example from Ashcroft Inc., which is ideally mounted on the gas inlet device as shown in FIG. 2. The pressure range of the transducer should range from 0 to 2500 mbar, but in particular from 0 to 1000 mbar. The determined print data are forwarded to an electronic memory, which can hold up to 60,000 print data. This

Datenspeicher sollte idealerweise in einem Gerät mit dem Druckaufnehmer untergebracht sein.Data storage should ideally be housed in a device with the pressure transducer.

Das Verfahren ist nicht auf die Messung des Staudruckes als Maß für den Strömungswiderstand beschränkt.The method is not limited to measuring the dynamic pressure as a measure of the flow resistance.

Es ist ebenso möglich, andere Auswirkungen der Befüllung von Reaktoren auf den Gasfluss als Grundlage für die Messungen zu nehmen wie zum Beispiel den Druckabfall in der Feststoffschüttung oder die Strömungsgeschwindigkeit.It is also possible to take other effects of the filling of reactors on the gas flow as the basis for the measurements, such as the pressure drop in the solid bed or the flow rate.

Der Gasstrom kann als Volumenstrom oder Massenstrom gemessen werden. Kurze Beschreibung der AbbildungenThe gas flow can be measured as volume flow or mass flow. Brief description of the pictures

Abbildung 1illustration 1

Apparatur zur gleichmäßigen Dosierung des Gasflusses durch mehrere parallele Gaslinien.Apparatus for uniform metering of the gas flow through several parallel gas lines.

Abbildung 2Figure 2

Apparatur zur Messung des StaudrucksApparatus for measuring the dynamic pressure

1) Druckmesser u. U. Datenspeicher1) pressure gauge U. data storage

2) Gaseinlass aus Apparatur 12) Gas inlet from apparatus 1

3 ) Festkörperschüttung3) Solid bed

4) Gasaustritt4) Gas leak

5) Dichtung 5) Seal

Claims

Patentansprüche claims 1. Verfahren zur Messung der gleichmäßigen Befüllung von Reaktoren oder Kolonnen mit Festkörpern, wobei die Reaktoren so aufgebaut sind, dass sie von mindestens zwei getrennt geführten Gas- und Flüssigkeitsströmen mit denselben Zusammensetzungen durchflössen werden, und die Messung so vorgenommen wird, dass man nach der Befüllung mit den Festkörpern a) in mindestens zwei der getrennt angebrachten Gas- oder Flüssigkeitseinlässe gleichzeitig Gas oder Flüssigkeit mit jeweils den gleichen Mengenflüssen und Drucken einleitet, b) an jedem der Einlasse gleichzeitig den Strömungswiderstand misst und c) die ermittelten Werte zentral registriert.1. A method for measuring the uniform filling of reactors or columns with solids, the reactors being constructed in such a way that they are flowed through by at least two separately guided gas and liquid streams with the same compositions, and the measurement is carried out in such a way that Filling with the solids a) simultaneously introduces gas or liquid, each with the same volume flow and pressure, into at least two of the separately installed gas or liquid inlets, b) simultaneously measures the flow resistance at each of the inlets and c) centrally registers the determined values. 2. Verfahren ge äss Anspruch 1, bei dem man mit Katalysatoren gefüllte Rohrbündelreaktoren einsetzt.2. The method according to claim 1, in which tube-bundle reactors filled with catalysts are used. 3. Apparatur zur Messung der gleichmäßigen Befüllung von Reaktoren mit Festkörpern, die mindestens zwei Vorrichtungen zur konstanten Dosierung von Gas und damit verbunden die jeweils gleiche Zahl von Vorrichtungen zur Messung des Stauddrucks oder Gasdurchflusses in mit Festkörpern gefüllten Reaktoren oder Kolonnen und einen zentralen Datenspeicher zur Aufnahme der Messwerte besitzt. 3. Apparatus for measuring the uniform filling of reactors with solids, the at least two devices for constant metering of gas and, in each case, the same number of devices for measuring the dynamic pressure or gas flow in reactors or columns filled with solids and a central data storage for recording who has measured values.
PCT/EP2005/004714 2004-05-27 2005-04-30 Method for measuring the even charge of reactors with solid bodies Ceased WO2005118125A1 (en)

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DE200410025872 DE102004025872A1 (en) 2004-05-27 2004-05-27 Method for measuring the uniform filling of reactors with solids
DE102004025872.4 2004-05-27

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007090705A1 (en) * 2006-02-08 2007-08-16 Evonik Degussa Gmbh Process for measuring the uniform filling of reactors with solid bodies
WO2007137645A1 (en) * 2006-05-31 2007-12-06 Süd-Chemie AG Testing device for tube bundle reactors
US7776288B2 (en) 2006-03-23 2010-08-17 Süd-Chemie AG Charging device for a tubular reactor
US7897120B2 (en) 2005-03-24 2011-03-01 Sud-Chemie Ag Feeding device for bundled tube reactor

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US4461327A (en) * 1980-06-02 1984-07-24 Basf Aktiengesellschaft Process and arrangements for charging a tubular reactor with granular solids
DE3935636A1 (en) * 1989-10-26 1991-05-02 Wacker Chemie Gmbh Monitoring flow resistance changes in solid bed reactor column - from pressure changes in initially standardised test flow gas
JPH07256082A (en) * 1994-03-17 1995-10-09 Mitsui Petrochem Ind Ltd Optimal filling condition testing device and method for filling solid filling in this device
WO2002074428A2 (en) * 2001-03-16 2002-09-26 Tubemaster, Inc. Device and method for blowing down and measuring the back pressure of chemical reactor tubes
NL1020901C2 (en) * 2002-06-19 2003-12-22 Mourik Internat B V Test method, e.g. for packing of catalyst particles inside reactor pipe, involves supplying flow of air to pipe inlet at constant mass flow rate

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US4461327A (en) * 1980-06-02 1984-07-24 Basf Aktiengesellschaft Process and arrangements for charging a tubular reactor with granular solids
DE3935636A1 (en) * 1989-10-26 1991-05-02 Wacker Chemie Gmbh Monitoring flow resistance changes in solid bed reactor column - from pressure changes in initially standardised test flow gas
JPH07256082A (en) * 1994-03-17 1995-10-09 Mitsui Petrochem Ind Ltd Optimal filling condition testing device and method for filling solid filling in this device
WO2002074428A2 (en) * 2001-03-16 2002-09-26 Tubemaster, Inc. Device and method for blowing down and measuring the back pressure of chemical reactor tubes
NL1020901C2 (en) * 2002-06-19 2003-12-22 Mourik Internat B V Test method, e.g. for packing of catalyst particles inside reactor pipe, involves supplying flow of air to pipe inlet at constant mass flow rate

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7897120B2 (en) 2005-03-24 2011-03-01 Sud-Chemie Ag Feeding device for bundled tube reactor
WO2007090705A1 (en) * 2006-02-08 2007-08-16 Evonik Degussa Gmbh Process for measuring the uniform filling of reactors with solid bodies
US7776288B2 (en) 2006-03-23 2010-08-17 Süd-Chemie AG Charging device for a tubular reactor
WO2007137645A1 (en) * 2006-05-31 2007-12-06 Süd-Chemie AG Testing device for tube bundle reactors
US7984654B2 (en) 2006-05-31 2011-07-26 Süd-Chemie AG Testing device for tube bundle reactors

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