DE102004025872A1 - Method for measuring the uniform filling of reactors with solids - Google Patents

Method for measuring the uniform filling of reactors with solids Download PDF

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Publication number
DE102004025872A1
DE102004025872A1 DE200410025872 DE102004025872A DE102004025872A1 DE 102004025872 A1 DE102004025872 A1 DE 102004025872A1 DE 200410025872 DE200410025872 DE 200410025872 DE 102004025872 A DE102004025872 A DE 102004025872A DE 102004025872 A1 DE102004025872 A1 DE 102004025872A1
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DE
Germany
Prior art keywords
reactors
solids
gas
flow
measuring
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.)
Withdrawn
Application number
DE200410025872
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German (de)
Inventor
Achim Dr. Fischer
Werner Burkhardt
Jan-Olaf Dr. Barth
Christoph Dr. Weckbecker
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Evonik Operations GmbH
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Degussa GmbH
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Publication date
Application filed by Degussa GmbH filed Critical Degussa GmbH
Priority to DE200410025872 priority Critical patent/DE102004025872A1/en
Priority to PCT/EP2005/004714 priority patent/WO2005118125A1/en
Priority to US11/138,428 priority patent/US20050281717A1/en
Publication of DE102004025872A1 publication Critical patent/DE102004025872A1/en
Withdrawn legal-status Critical Current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

Abstract

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 carrying out the method.

Description

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

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 The chemical reaction technique is the uniform filling of reactors with solids from crucial for the power efficiency of the apparatus. For example, it is with the solids around filler 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 solid 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.Puts you get these solids for example in tube bundle reactors or plate reactors for catalyzed reactions, so the task arises, the uniform filling of these To ensure reactors.

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 durchflossen 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 Einlässe gleichzeitig den Strömungswiderstand mißt und
  • c) die ermittelten Werte zentral registriert.
The invention relates to a method for measuring the uniform filling of reactors with solids, wherein the reactors are constructed so that they are traversed by at least two separately guided gas and liquid streams having the same compositions, and the measurement is carried out so that after the filling with the solids
  • a) simultaneously introducing gas or liquid, each with the same flow rates and pressures, into at least two of the separately installed gas or liquid inlets,
  • b) at each of the inlets simultaneously measures the flow resistance and
  • c) the determined values are registered centrally.

Als Reaktoren besonders gebräuchlich sind Rohrbündelreaktoren oder Reaktoren mit voneinander durch Thermobleche getrennten Reaktions- und Wärmetransporträumen.When Reactors especially in use are tube bundle reactors or reactors with reaction plates separated from each other by thermoplates and heat transport spaces.

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

Als Gase werden im allgemeinen inerte Gase, Luft oder Gemische daraus eingesetzt.When Gases generally become inert gases, air or mixtures thereof used.

Die Festkörperschüttung stellt für den Gasstrom einen Widerstand dar, durch den die Flussgeschwindigkeit vermindert wird und sich ein Staudruck aufbaut.The Provides solid-body packing for the Gas flow is a resistance by which the flow velocity is reduced and builds up a back pressure.

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 l/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.in this connection is crucial that a constant volume flow is passed through the solid-state bed becomes. The volume flow of the gas should generally have a flow rate from 250 to 5000 l / h, the inlet pressure of the gas should be in Range from 1 bar to 50 bar, in particular from 1 to 10 barü, the Temperature of the gas generally in the range of 10 to 50 ° C. Ideally Inert gases, air or mixtures of these are suitable.

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

Die Dosierung wird als konstant angesehen, wenn die Flussrate des Gases mit weniger als +/–2,5 % schwankt, besonders geeignet sind Flussraten mit einer Schwankung von kleiner gleich +/–1%.The Dosage is considered constant when the flow rate of the gas with less than +/- 2.5% varies, flow rates are particularly suitable with a fluctuation less than or equal to +/- 1%.

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.Advantageous For example, the dynamic pressure in up to 15 parallel gas lines, in particular up to 10, particularly advantageously up to 5 measured. If different measured values result, the filling is with as solids For example, catalysts used are not uniform and must be improved.

Die erfindungsgemäß mögliche Messung mehrerer Gasdurchflüsse gleichzeitig ermöglicht eine zeitsparende Methode zur Überprüfung der Befüllung von Reaktoren.The according to the invention possible measurement of several Gas flow rates at the same time allows one time-saving method of checking the filling of reactors.

Als gleichmäßig wird eine Varianz von bis zu + 5 % angesehen.When becomes even a variance of up to + 5%.

Zur Messung des Staudruckes wird der beispielsweise der aus der Apparatur gemäß 1 kommende Gasstrom über eine Apparatur wie sie in 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 Gaseinleitungsvorrichtung wie sie in der 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. Dieser Datenspeicher sollte idealerweise in einem Gerät mit dem Druckaufnehmer untergebracht sein.For measuring the back pressure of the example of the apparatus according to 1 coming gas stream via an apparatus such as in 2 is shown passed through the investigated solid-state package. The generated back pressures are measured with a commercially available pressure transducer, for example the company Ashcroft Inc., which ideally on the gas introduction device as shown in the 2 is shown mounted. The pressure range of the transducer should range from 0 to 2500 mbarü, but especially from 0 to 1000 mbarü. The determined print data are passed on to an electronic memory, which can hold up to 60000 print data. This data memory 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 the measurement of the back 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 other effects of filling of reactors to take the gas flow as a basis for the measurements like For example, the pressure drop in the solids bed or the flow rate.

Der Gasstrom kann als Volumenstrom oder Massenstrom gemessen werden.Of the Gas flow can be measured as volume flow or mass flow.

Kurze Beschreibung der AbbildungenShort description of pictures

1 Apparatur zur gleichmäßigen Dosierung des Gasflusses durch mehrere parallele Gaslinien. 1 Apparatus for uniform metering of gas flow through several parallel gas lines.

2 Apparatur zur Messung des Staudrucks 2 Apparatus for measuring the dynamic pressure

11
Druckmesser u. U. Datenspeicherpressure gauge u. U. Data memory
22
Gaseinlass aus Apparatur 1 Gas inlet from apparatus 1
33
FestkörperschüttungSolid bed
44
Gasaustrittgas outlet
55
Dichtungpoetry

Claims (3)

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 durchflossen 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 Einlässe gleichzeitig den Strömungswiderstand misst und c) die ermittelten Werte zentral registriert.Method of measuring the uniform filling of Reactors or columns with solids, the reactors are constructed in such a way that they are separated from at least two separate gas and liquid streams with flow through the same compositions, and the measurement is done so that after filling with the solids a) in at least two of the separately mounted gas or liquid inlets simultaneously Gas or liquid each initiating the same flow rates and printing, b) at each of the inlets at the same time the flow resistance measures and c) the determined values are registered centrally. Verfahren gemäss Anspruch 1, bei dem man mit Katalysatoren gefüllte Rohrbündelreaktoren einsetzt.Process according to Claim 1, in which one uses catalyst-filled tube bundle reactors. 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.Apparatus for measuring the uniform filling of reactors with solids, the at least two devices for constant metering of gas and associated with each of the same number of devices for measurement backpressure or gas flow in solids-filled reactors or columns and a central data store for receiving the Has measured values.
DE200410025872 2004-05-27 2004-05-27 Method for measuring the uniform filling of reactors with solids Withdrawn DE102004025872A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE200410025872 DE102004025872A1 (en) 2004-05-27 2004-05-27 Method for measuring the uniform filling of reactors with solids
PCT/EP2005/004714 WO2005118125A1 (en) 2004-05-27 2005-04-30 Method for measuring the even charge of reactors with solid bodies
US11/138,428 US20050281717A1 (en) 2004-05-27 2005-05-27 Method for measuring the uniform filling of reactors with solid matter

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Application Number Priority Date Filing Date Title
DE200410025872 DE102004025872A1 (en) 2004-05-27 2004-05-27 Method for measuring the uniform filling of reactors with solids

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005013845B4 (en) 2005-03-24 2010-04-29 Süd-Chemie AG Tube-bundle feed apparatus and method of operation of the feeder
DE102006006009A1 (en) * 2006-02-08 2007-08-09 Degussa Gmbh Method for measuring the uniform filling of reactors with solids
DE102006013488B4 (en) 2006-03-23 2009-03-26 Süd-Chemie AG Shell-loader
DE102006025441A1 (en) 2006-05-31 2007-12-06 Süd-Chemie AG Test device for tube bundle reactors

Citations (3)

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Publication number Priority date Publication date Assignee Title
EP0873783A1 (en) * 1997-04-23 1998-10-28 Basf Aktiengesellschaft Apparatus and method to measure the temperature in tubular reaktors
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
EP1270065A1 (en) * 2001-06-26 2003-01-02 Nippon Shokubai Co., Ltd. Apparatus for pressure and temperature measurements in tube reactors

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DE3020845A1 (en) * 1980-06-02 1981-12-17 Basf Ag, 6700 Ludwigshafen METHOD AND ARRANGEMENT FOR LOADING TUBE REACTORS WITH GRAINY 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
JP3563101B2 (en) * 1994-03-17 2004-09-08 三井化学株式会社 Optimum filling condition test device and method for filling solid filling material into the device
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0873783A1 (en) * 1997-04-23 1998-10-28 Basf Aktiengesellschaft Apparatus and method to measure the temperature in tubular reaktors
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
EP1270065A1 (en) * 2001-06-26 2003-01-02 Nippon Shokubai Co., Ltd. Apparatus for pressure and temperature measurements in tube reactors

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Publication number Publication date
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OP8 Request for examination as to paragraph 44 patent law
8127 New person/name/address of the applicant

Owner name: DEGUSSA GMBH, 40474 DUESSELDORF, DE

8127 New person/name/address of the applicant

Owner name: EVONIK DEGUSSA GMBH, 40474 DUESSELDORF, DE

8139 Disposal/non-payment of the annual fee