DE19526628C1 - Column for microwave reactors - Google Patents

Column for microwave reactors

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Publication number
DE19526628C1
DE19526628C1 DE1995126628 DE19526628A DE19526628C1 DE 19526628 C1 DE19526628 C1 DE 19526628C1 DE 1995126628 DE1995126628 DE 1995126628 DE 19526628 A DE19526628 A DE 19526628A DE 19526628 C1 DE19526628 C1 DE 19526628C1
Authority
DE
Germany
Prior art keywords
column
microwave
microwaves
tube
transparent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
DE1995126628
Other languages
German (de)
Inventor
Dieter Bathen
Henner Schmidt-Traub
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Individual
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Individual
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Priority to DE1995126628 priority Critical patent/DE19526628C1/en
Application granted granted Critical
Publication of DE19526628C1 publication Critical patent/DE19526628C1/en
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Expired - Fee Related 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3441—Regeneration or reactivation by electric current, ultrasound or irradiation, e.g. electromagnetic radiation such as X-rays, UV, light, microwaves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/32—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by electrical effects other than those provided for in group B01D61/00
    • 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
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122—Incoherent waves
    • B01J19/126—Microwaves
    • 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
    • B01J8/0285—Heating or cooling the reactor
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/48—Separation; Purification; Stabilisation; Use of additives
    • C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
    • B01D2259/806—Microwaves
    • 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
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12—Processes employing electromagnetic waves
    • B01J2219/1203—Incoherent waves
    • B01J2219/1206—Microwaves
    • B01J2219/1209—Features relating to the reactor or vessel
    • B01J2219/1212—Arrangements of the reactor or the reactors
    • B01J2219/1215—Single reactor

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Toxicology (AREA)
  • Electromagnetism (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Catalysts (AREA)

Abstract

A column (8) for incorporation into microwave reactors is novel in that it has a concentric tube (3) within the column wall (1). It is filled from outside with a loose material (4) to reflect microwaves or a body of the desired geometry of a microwave-reflecting material is incorporated into the tube. The tube material is transparent to microwaves.

Description

Es ist bekannt, daß Mikrowellen zur Eintragung von Energie in ein Dielektrikum verwendet werden können. Im Rahmen verfahrenstechnischer Anwendungen wird die zugeführte elektromagnetische Energie u. a. benutzt, um chemische Reaktionen auszulösen und zu un­ terhalten oder um aus einem Feststoff eine unerwünschte Komponente auszutreiben (Mikrowellen-Trocknung bzw. -Desorption). Insbesondere im Bereich der Trocknung von Lebensmitteln und keramischen Werkstoffen sind industrielle Anwendungen veröffentlicht worden (z. B. Orth/Walter, Mikrowellenerwärmung-Anwendungen in der Industrie, Elek­ trowärme International 49 (1991) B3, B149-B155).It is known that microwaves are used to introduce energy into a dielectric can be. In the context of process engineering applications, the supplied electromagnetic energy u. a. used to trigger chemical reactions and to un maintain or to drive out an unwanted component from a solid (Microwave drying or desorption). Especially in the area of drying Food and ceramic materials are published in industrial applications (e.g. Orth / Walter, microwave heating applications in industry, elec trowärme International 49 (1991) B3, B149-B155).

Sowohl im Rahmen der Katalyse als auch bei der Trocknung / Desorption sind bei der Auswahl der Reaktoren verschiedene Konzepte verfolgt worden, die im folgenden skizziert werden sollen.Both in the context of catalysis as well as in the drying / desorption Selection of reactors different concepts have been followed, outlined below should be.

Neben Desorptionskammern, die über Sicherheitsschleusen und durchlaufende Förderbän­ der befüllt werden (Gebrauchsmuster G 91 03 529.5), werden einfache vertikale Glasroh­ re, durch die das beladene Adsorbens mittels Schwerkraft gefördert wird (DE 35 11 766 A1), sowie zylindrische Kolonnen verwendet (DE 28 57 134 A1). Zusätzlich werden wabenförmige Adsorber beschrieben, bei denen einzelne Waben von den übrigen getrennt und mittels beweglicher Mikrowellen-Schlitten bestrahlt werden (CA 20 82 690 A1 (Application)).In addition to desorption chambers, which pass through security gates and continuous conveyor belts which are filled (utility model G 91 03 529.5) become simple vertical glass tubes re, through which the loaded adsorbent is promoted by gravity (DE 35 11 766 A1) and cylindrical columns are used (DE 28 57 134 A1). In addition described honeycomb-shaped adsorbers in which individual honeycombs are separated from the rest and are irradiated by means of movable microwave slides (CA 20 82 690 A1 (Application)).

Die vorliegende Erfindung beschreibt eine zylindrische Kolonne, die, wie in Fig. 1 darge­ stellt, in einen Mikrowellenreaktor eingebaut wird und sowohl für den batch-Betrieb im Rahmen von Adsorptions-/Desorptions-Zyklen als auch für den kontinuierlichen Betrieb im Rahmen von katalytischen Reaktionen eingesetzt werden kann.The present invention describes a cylindrical column which, as shown in FIG. 1, is installed in a microwave reactor and is used both for batch operation in the context of adsorption / desorption cycles and for continuous operation in the context of catalytic reactions can be used.

Der Erfindung liegt die folgende Problemstellung zu Grunde:The invention is based on the following problem:

Werden in Mikrowellenreaktoren mit einem Dielektrikum (z. B. Katalysatoren oder Adsor­ bentien wie Aktivkohle oder Zeolithe) befüllte Kolonnen eingebracht, deren Radius kleiner oder gleich der Eindringtiefe der Mikrowellen in das Dielektrikum ist, so entsteht im Zentrum der Kolonne ein Bereich, in dem sich die eingestrahlten Mikrowellen überlagern. Diese Interferenz führt zu einer starken Temperaturerhöhung im Inneren des Dielektrikums. Die Folge sind unerwünschte Nebenreaktionen, Zersetzung des Dielektrikums und bei Vorhandensein entzündlicher Substanzen Brände und kleinere Explosionen. Durch diese Gefahren wird der Einsatz der Mikrowellentechnologie in der Festbett-Katalyse und bei der Regeneration beladener Adsorbentien stark eingeschränkt.Are used in microwave reactors with a dielectric (e.g. catalysts or adsor bentien like activated carbon or zeolites) filled columns whose radius is smaller or is the same as the depth of penetration of the microwaves into the dielectric, so arises in  Center of the column an area in which the radiated microwaves overlap. This interference leads to a sharp increase in temperature inside the dielectric. The result is undesirable side reactions, decomposition of the dielectric and Presence of flammable substances, fires and minor explosions. Through this The use of microwave technology in fixed bed catalysis and in Regeneration of loaded adsorbents is severely restricted.

Dieses Problem wird durch die Erfindung nach den Patentansprüchen 1 und 2 gelöst.This problem is alleviated by the invention the claims 1 and 2 solved.

In Fig. 2 ist ein Querschnitt der Erfindung dargestellt.In Fig. 2 a cross section of the invention is shown.

Die in den Mikrowellenreaktor einzubauende Kolonne besteht aus einer für Mikrowellen transparenten Umhüllung (1), in die eine Fritte (5) eingesetzt wird. In der Mitte der Kolon­ ne wird konzentrisch zur Behälterwand ein transparentes Rohr (3) eingebaut, das über einen außerhalb der Kolonne befindlichen Stutzen (6) mit einem Mikrowellen reflektieren­ den Material (4) befüllt werden kann. Der zu bestrahlende Feststoff (2) wird über die Austrittsöffnung der Kolonne (8) in den Raum zwischen dem transparenten Rohr (3) und der äußeren Kolonnenwand (1) eingefüllt.The column to be installed in the microwave reactor consists of an envelope ( 1 ) which is transparent to microwaves and into which a frit ( 5 ) is inserted. In the middle of the column ne, a transparent tube ( 3 ) is installed concentrically to the container wall, which can be filled with a microwave reflecting material ( 4 ) via a nozzle ( 6 ) located outside the column. The solid ( 2 ) to be irradiated is introduced into the space between the transparent tube ( 3 ) and the outer column wall ( 1 ) via the outlet opening of the column ( 8 ).

Die Wände der Kolonne und des Rohres, können z. B. aus Glas ausgeführt sein, während sich als reflektierendes Material ölfreie Aluminiumspäne als geeignet erwiesen haben. Alternativ zur Befüllung mit einer Schüttung eines reflektierenden Materials (Patentan­ spruch 1) kann das Rohr auch mit einem Körper beliebiger Geometrie (Patentanspruch 2) befüllt werden.The walls of the column and the tube can, for. B. made of glass while Oil-free aluminum chips have proven to be suitable as a reflective material. As an alternative to filling with a bed of reflective material (patent no Proof 1) the tube can also have a body of any geometry (claim 2) be filled.

Die so präparierte Kolonne kann anschließend in der in Fig. 1 gezeigten Art und Weise in den Mikrowellenreaktor eingebaut und mit Gas zur Reaktion oder Adsorption/Desorption beaufschlagt werden.The column prepared in this way can then be installed in the microwave reactor in the manner shown in FIG. 1 and gas can be applied for the reaction or adsorption / desorption.

Die Wirkung der Erfindung beruht darauf, daß durch das Dielektrikum dringende Mikrowel­ len an der Oberfläche des Reflektors diffus reflektiert werden, wodurch eine Interferenz der eingestrahlten Mikrowellen und somit die Erzeugung eines ausgeprägten Temperatur­ maximums im Zentrum der Kolonne verhindert wird. Aus dieser Reflexion resultierende lokale Interferenzen in den Randbereichen der Kolonne sind aufgrund des diffusen Charak­ ters der reflektierten Strahlung extrem unwahrscheinlich und in jedem Fall deutlich geringer als die ohne den Einbau des Reflektors festgestellte Interferenz im Zentrum der Kolonne. Die Wirksamkeit der Erfindung wurde an folgenden Verfahren exemplarisch getestet:The effect of the invention is based on the fact that microwaves penetrating through the dielectric len are diffusely reflected on the surface of the reflector, causing interference of the radiated microwaves and thus the generation of a pronounced temperature maximums in the center of the column is prevented. Resulting from this reflection local interferences in the edge areas of the column are due to the diffuse character reflected radiation is extremely unlikely and in any case significantly lower than the interference found without the installation of the reflector in the center of the column. The effectiveness of the invention was tested using the following methods:

Beispiel 1: Entfernung von Ethanol bzw. Essigsäureethylester aus Zeolith NaX (Eindringtie­ fe der Mikrowellen: ca. 15,7 cm) durch Mikrowellen unter Spülung mit Luft bzw. Stick­ stoff in einer Kolonne mit dem Durchmesser d = 5 cm (Reflektor: Aluminium-Späne).Example 1: Removal of ethanol or ethyl acetate from zeolite NaX (penetration of the microwaves: approx. 15.7 cm) by microwaves with air or stick rinsing fabric in a column with diameter d = 5 cm (reflector: aluminum chips).

Beispiel 2: Katalytische Reaktion von Ethanol an Zeolith NaX (Eindringtiefe der Mi­ krowellen: ca. 15,7 cm) durch Mikrowellen unter Spülung mit Luft in einer Kolonne mit dem Durchmesser d = 5 cm (Reflektor: Aluminium-Späne).Example 2: Catalytic reaction of ethanol on zeolite NaX (penetration depth of the Mi crown waves: approx. 15.7 cm) by microwaves with rinsing with air in a column the diameter d = 5 cm (reflector: aluminum chips).

Beispiel 3: Entfernung von Ethanol bzw. Essigsäureethylester aus Zeolith DAY (Eindringtie­ fe der Mikrowellen: < 1,5 m) durch Mikrowellen unter Spülung mit Luft bzw. Stickstoff in einer Kolonne mit dem Durchmesser d = 5 cm (Reflektor: Aluminium-Späne).Example 3: Removal of ethanol or ethyl acetate from zeolite DAY (penetration Fe of the microwaves: <1.5 m) by microwaves with flushing with air or nitrogen in a column with the diameter d = 5 cm (reflector: Aluminum chips).

Claims (2)

1. Kolonne zum Einbau in Mikrowellenreaktoren, dadurch gekennzeichnet, daß in die Kolonne konzentrisch zur Kolonnenwand ein von außen befüllbares Rohr aus einem für Mikrowellen transparenten Material eingebaut und mit einer Schüttung eines Mikrowellen reflektierenden Materials befüllt ist.1. Column for installation in microwave reactors, characterized in that an externally fillable tube made of a material which is transparent to microwaves is installed in the column concentrically with the column wall and is filled with a bed of microwave-reflecting material. 2. Kolonne zum Einbau in Mikrowellenreaktoren, dadurch gekennzeichnet, daß in die Kolonne konzentrisch zur Kolonnenwand ein von außen befüllbares Rohr aus einem für Mikrowellen transparenten Material eingebaut ist, in das ein Körper beliebiger Geometrie aus einem Mikrowellen diffus reflektierenden Material einge­ bracht ist.2nd column for installation in microwave reactors, characterized in that into the column concentrically to the column wall from outside fillable tube a material that is transparent to microwaves is built into which a body any geometry from a microwave diffusely reflective material is brought.
DE1995126628 1995-07-21 1995-07-21 Column for microwave reactors Expired - Fee Related DE19526628C1 (en)

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DE1995126628 DE19526628C1 (en) 1995-07-21 1995-07-21 Column for microwave reactors

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999003565A1 (en) * 1997-07-15 1999-01-28 Daimler-Chrysler Ag Method and installation for eliminating gaseous organic substances in the air
DE102006062651A1 (en) * 2006-11-14 2008-05-15 Helmholtz-Zentrum Für Umweltforschung Gmbh - Ufz Procedure for warming a solid material bed having inflow and outflow areas, for initiating thermochromatographic pulses, comprises introducing an electromagnetic radiation in the bed and bringing a transmission medium in the bed
WO2018092160A1 (en) * 2016-11-17 2018-05-24 Gruppo Distribuzione Petroli S.R.L. Device for abatement of liquid, gaseous and/or solid pollutant substances of various kind, contained into the exhaust smokes, and process for treatment and abatement of such pollutant substances

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2857134A1 (en) * 1977-10-31 1981-01-08 Battelle Development Corp ADSORBENT REGENERATION AND GAS SEPARATION UTILIZING DIELECTRIC HEATING
DE9103529U1 (en) * 1991-03-22 1991-11-21 HAK-Anlagenbau GmbH für Verfahrenstechnik, Strahlungstechnik und Trocknungstechnik, 22119 Hamburg Plant for reconditioning activated carbon and for recovering the absorbent
CA2082690A1 (en) * 1991-12-23 1993-06-24 Donald Ernest Woodmansee In place regeneration of adsorbents using microwaves

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2857134A1 (en) * 1977-10-31 1981-01-08 Battelle Development Corp ADSORBENT REGENERATION AND GAS SEPARATION UTILIZING DIELECTRIC HEATING
DE9103529U1 (en) * 1991-03-22 1991-11-21 HAK-Anlagenbau GmbH für Verfahrenstechnik, Strahlungstechnik und Trocknungstechnik, 22119 Hamburg Plant for reconditioning activated carbon and for recovering the absorbent
CA2082690A1 (en) * 1991-12-23 1993-06-24 Donald Ernest Woodmansee In place regeneration of adsorbents using microwaves

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
iew elektrowärme international Bd.49 (1991)B3, S.B149-155 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999003565A1 (en) * 1997-07-15 1999-01-28 Daimler-Chrysler Ag Method and installation for eliminating gaseous organic substances in the air
US6296823B1 (en) 1997-07-15 2001-10-02 Daimlerchrysler Ag Method and installation for eliminating gaseous organic substances in the air
DE102006062651A1 (en) * 2006-11-14 2008-05-15 Helmholtz-Zentrum Für Umweltforschung Gmbh - Ufz Procedure for warming a solid material bed having inflow and outflow areas, for initiating thermochromatographic pulses, comprises introducing an electromagnetic radiation in the bed and bringing a transmission medium in the bed
DE102006062651B4 (en) * 2006-11-14 2009-12-31 Helmholtz-Zentrum Für Umweltforschung Gmbh - Ufz Method and device for thermochromatographic heating of solid beds
WO2018092160A1 (en) * 2016-11-17 2018-05-24 Gruppo Distribuzione Petroli S.R.L. Device for abatement of liquid, gaseous and/or solid pollutant substances of various kind, contained into the exhaust smokes, and process for treatment and abatement of such pollutant substances

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