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WO2006106019A1 - Procede pour remplir des appareils avec des matieres solides - Google Patents

Procede pour remplir des appareils avec des matieres solides Download PDF

Info

Publication number
WO2006106019A1
WO2006106019A1 PCT/EP2006/060329 EP2006060329W WO2006106019A1 WO 2006106019 A1 WO2006106019 A1 WO 2006106019A1 EP 2006060329 W EP2006060329 W EP 2006060329W WO 2006106019 A1 WO2006106019 A1 WO 2006106019A1
Authority
WO
WIPO (PCT)
Prior art keywords
solids
filled
filling
hopper
rollers
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/EP2006/060329
Other languages
German (de)
English (en)
Inventor
Jan-Olaf Barth
Achim Fischer
Wolfgang BÖCK
Werner Burkhardt
Christoph Weckbecker
Klaus Huthmacher
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
Priority to BRPI0608662-4A priority Critical patent/BRPI0608662A2/pt
Priority to JP2008504719A priority patent/JP2008534410A/ja
Priority to MX2007012334A priority patent/MX2007012334A/es
Priority to EP06708556A priority patent/EP1866069A1/fr
Priority to CA002603521A priority patent/CA2603521A1/fr
Publication of WO2006106019A1 publication Critical patent/WO2006106019A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

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
    • B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
    • B01J8/003—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor in a downward flow
    • 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
    • B01J2208/00743—Feeding or discharging of solids
    • B01J2208/00752—Feeding

Definitions

  • the invention relates to a method for filling apparatus used in chemical production with solids using a controllable metering device and a locally displaceable
  • the device is particularly suitable for the filling of heat exchangers, absorption columns, distillation columns or shell-and-tube reactors with solids.
  • the uniform filling of solids in pipes, tube bundles or heat exchangers is of crucial importance for the power efficiency of these devices.
  • the solids may be, for example, packing such as Raschig rings, ceramic balls or catalysts and have different compositions and geometries such as those of balls, solid cylinders, hollow cylinders or rings.
  • US Pat. No. 4,402,643 and EP 0 904 831 B (US Pat. No. 6,170,670 B1) describe the supply of granular material and the associated devices, the material being transported via a vibrated channel into the tubes to be filled.
  • Finely divided dust thereby falls in accordance with EP 0 904 831 through the sieve-shaped bottom of the channel into a separate container.
  • the resulting catalyst bed is no longer homogeneous. Fine abrasion (dust) and catalyst breakage lead to the formation of cavities and channels, so that uneven flow through the tube leads to decreased or increased pressure drops. This affects the power efficiency or throughput of the apparatus.
  • the invention relates to a method for filling pipes with solids, in which one discharges the solid from a hopper (2) on an inclined plane with Rüttelrinnen (4), which is arranged in an approximately horizontal position and from the discharge opening of the
  • Funnel extends at least for connection to the downpipe (5) or a flexible hose connection through which the solid is fed to the pipe to be filled, characterized in that one respectively
  • the solid is metered in a uniform manner by controlling or regulating the vibration frequency of the vibrating trough (4).
  • the metering or metering rate can also be adjusted if necessary simultaneously via the height-adjustable flow regulator (3), which has the shape of a weir.
  • the height-adjustable downpipes or the flexible hose connections prove to be particularly advantageous because even small differences in the height of the pipes to be filled are compensated and gaps between downpipe and reactor tube can be avoided.
  • Particle size of preferably at least 1 mm may be moldings of various types and suitability such as Raschig rings, ceramic balls, inert body or shaped catalysts z. B. in the form of granules extrudates or compacts in the commercial dimensions.
  • Reactions with such catalysts include, for example, the preparation of ethylene oxide, phthalic anhydride, acrolein, acrylic acid, methyl mercaptan, hydrogen sulfide and others.
  • the aim of the invention is to obtain a homogeneous solid bed and to avoid mechanical destruction of the solids.
  • a zonewise filling of the solids can be achieved, so that along the axial profile of the tube different fillings of solids with precisely defined volumes can be introduced simultaneously.
  • the method according to the invention is characterized by a uniform distribution of the filling heights so that when the tubes are exposed to a constant gas flow, differential pressure pressures with a mean standard deviation from the mean value of generally less than 10% result. At the same time a dust nuisance in the filling process should be avoided.
  • the amount of solids to be filled for each reaction tube is first determined volumetrically or gravimetrically and placed in a collecting vessel.
  • the amount to be filled is determined gravimetrically.
  • the collecting vessel has at least the volume of solids to be filled. The collection vessel is opened and introduced with the opening down into a hopper 2.
  • the solids are first loosened by a device by means of vibrations, set in vibration and translational movement and fed via an inclined plane 4 (vibrating channel) evenly to a metering device.
  • the number of channels on the inclined plane corresponds to the number of pipes to be filled at the same time.
  • the metering device is connected to the apparatus to be filled (for example, reaction tube in tube bundle reactors) via height-adjustable downpipes 5 and allows a lossless supply of solids by means of a in the
  • Height-adjustable outlet pipe 6 As a metering device find use that allow a direct connection between the apparatus for the backfilling of solid beds and the apparatus to be filled. Suitable for this are funnels, pipes and flexible hose connections. These metering devices are preferably designed as length-adjustable downpipes (5 and 6) or flexible hose connections, so that there is a continuous connection between the apparatus to be filled (for example tube-bundle reactor) and the metering device. This allows the Solid particles without scattering losses or dosed into the apparatus to be filled. Furthermore, the dust emission is minimized during the filling process.
  • Figure 1 shows that in spatial proximity to the hopper and the height-adjustable downpipes ever a connection for a suction device 1 and a suction pipe 10 is provided, are sucked on the possibly by applying a vacuum occurring dust and solid particles.
  • This apparatus may be a heat exchanger, an absorption column, a distillation column and a tube bundle reactor. Particularly preferred
  • Tube bundle heat exchangers which are used as reactors. These reaction tubes may also have internals (e.g., thermocouples).
  • the device according to the invention allows a control of the mass flow via a variation of the vibration frequency of the apparatus advantageously via an electric thyristor control 7.
  • a regulation of the mass flow is also possible via the height-adjustable flow regulator 3 at the transition from the hopper to the Rüttelrinnen.
  • the solid bed should be characterized by a uniform
  • Oscillation movement of the collecting container, the inclined plane and the metering device are supplied to the apparatus.
  • a collecting device for the solid filling, a feeder (inclined plane) and a
  • Dosing device housed in an apparatus Up to 50, preferably up to 20, of these devices can be integrated in one metering device in order to efficiently fill a plurality of pipes at the same time.
  • Figure 1 shows, for example, a device with which 5 tubes can be filled simultaneously. By the simultaneous Backfilling of several pipes ensures a reproducible, even filling.
  • the solids are set in motion by vibration of an inclined plane.
  • the exact and fine adjustment of the vibration in order to keep the flow rate as uniform as possible.
  • This requirement is achieved by commercially available electric vibrator motors.
  • a variation of the vibration frequency via an electronic control allows influencing the vibration intensity of the solid and thus their outflow speed.
  • this plane is terminated by a preferably transparent cover (e.g., plastic) to prevent loss of solids and dust emissions.
  • a pipe opening 10 is provided which, connected to a suction device, ensures removal of solid dusts and impurities.
  • the apparatus is mounted on rollers or rollers 11 so that it can be operated and moved by one person at a time.
  • the roller can be adjusted in height.
  • the filling machine is structured as follows:
  • the filling time can be set via two parameters: • By means of the adjustable height butterfly valve with wing nuts 3, at the outlet to the vibrating plate,
  • the first fillings are used to further optimize the machine.
  • the fill level is used to check the correct filling of the pipes. If the pipe is too high, the machine is too fast, or if the pipe is too low, the machine will feed the catalyst too slowly into the pipe. In both cases, the filling speed is readjusted with the two above-mentioned parameters so that the tubes are filled as homogeneously as possible.
  • the solids are filled in zones, so that along the axial profile of the reaction tube different fillings of solids with precisely definable filling heights, filling volumes and masses are introduced simultaneously.
  • Reaction tubes containing internals to control the reactor are preferably filled so that at least one catalyst particle is metered into the tube per second, thereby avoiding the formation of dead zones and channels resulting in increased differential pressure loss.
  • the feed roller 11 of the filling machine is adjusted so that after each filling of a row, the machine can be easily pushed forward.
  • the catalyst to be filled is packed in collecting vessels, eg cans (1 can / tube).
  • the invention also relates to a locally displaceable device for filling pipes with solids, comprising
  • the device is mounted on rollers or rollers (11).
  • the cross section of the downpipe is at most equal to the cross section of the pipe to be filled. It preferably has a smaller cross-section and tapers at its ends, so that it fits into the tube to be filled.
  • Figure 1 shows an arrangement according to the invention (side view) of an allocation device for the simultaneous filling of five tubes with granular solids.
  • Figure 2 shows an inventive arrangement of the hopper and the connection for a suction device of an allocator for the simultaneous filling of five tubes with granular solids (top view).
  • Figure 3 shows an inventive arrangement of the downpipes and the height-adjustable outlet of an allocator for the simultaneous filling of five pipes with granular solids (front view).
  • Figure 4 shows an inventive arrangement of the vibrating troughs of an allocating device for the simultaneous filling of five tubes with granular solids (top view).
  • Figure 5 shows an arrangement according to the invention (side view) of an allocation device for filling a pipe with granular solids.
  • Figure 6 shows an arrangement according to the invention (top view) of an allocation device for filling a pipe with granular solids.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Basic Packing Technique (AREA)
  • Filling Or Emptying Of Bunkers, Hoppers, And Tanks (AREA)
  • Supply Of Fluid Materials To The Packaging Location (AREA)
  • Feeding Of Articles To Conveyors (AREA)

Abstract

La présente invention concerne un procédé pour remplir des appareils de production chimique avec des matières solides, par utilisation d'un dispositif de dosage réglable, et un dispositif qui peut être déplacé localement, destiné à mettre en oeuvre le procédé. Le dispositif convient particulièrement au remplissage d'échangeurs thermiques, de colonnes d'absorption, de colonnes de distillation ou de réacteurs à faisceaux de tubes, avec des matières solides.
PCT/EP2006/060329 2005-04-08 2006-02-28 Procede pour remplir des appareils avec des matieres solides Ceased WO2006106019A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
BRPI0608662-4A BRPI0608662A2 (pt) 2005-04-08 2006-02-28 processo para o enchimento de aparelhos com materiais sàlidos
JP2008504719A JP2008534410A (ja) 2005-04-08 2006-02-28 固形物を装置に充填するための方法
MX2007012334A MX2007012334A (es) 2005-04-08 2006-02-28 Metodo para llenar aparatos con solidos.
EP06708556A EP1866069A1 (fr) 2005-04-08 2006-02-28 Procede pour remplir des appareils avec des matieres solides
CA002603521A CA2603521A1 (fr) 2005-04-08 2006-02-28 Procede pour remplir des appareils avec des matieres solides

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005016078A DE102005016078A1 (de) 2005-04-08 2005-04-08 Verfahren zur Befüllung von Apparaturen mit Feststoffen
DE102005016078.6 2005-04-08

Publications (1)

Publication Number Publication Date
WO2006106019A1 true WO2006106019A1 (fr) 2006-10-12

Family

ID=36405883

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2006/060329 Ceased WO2006106019A1 (fr) 2005-04-08 2006-02-28 Procede pour remplir des appareils avec des matieres solides

Country Status (10)

Country Link
US (1) US20060243342A1 (fr)
EP (1) EP1866069A1 (fr)
JP (1) JP2008534410A (fr)
CN (1) CN101151092A (fr)
BR (1) BRPI0608662A2 (fr)
CA (1) CA2603521A1 (fr)
DE (1) DE102005016078A1 (fr)
MX (1) MX2007012334A (fr)
RU (1) RU2007140897A (fr)
WO (1) WO2006106019A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009262123A (ja) * 2008-03-31 2009-11-12 Mitsubishi Chemicals Corp プレート式触媒層反応器、該プレート式触媒層反応器に触媒を充填する方法及び該プレート式触媒層反応器を用いた反応生成物の製造方法
KR102030924B1 (ko) * 2018-04-13 2019-10-17 유한기술주식회사 촉매 로딩 장치 및 이를 포함하는 시스템

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102007043839A1 (de) 2007-09-14 2009-04-16 Süd-Chemie AG Verfahren zum Befüllen eines Rohres eines Rohrbündelreaktors
FR2950822B1 (fr) * 2009-10-01 2012-02-24 Inst Francais Du Petrole Dispositif de chargement de particules de catalyseur dans des tubes presentant une zone annulaire
JP2011121048A (ja) 2009-12-09 2011-06-23 Rohm & Haas Co 固体触媒物質をブレンドし、管状構造物に装填する方法
WO2013160311A2 (fr) * 2012-04-23 2013-10-31 Mourik International B.V. Outil de chargement de catalyseur
CN112934137A (zh) * 2021-01-28 2021-06-11 常州飞达新材料科技有限公司 一种苯佐卡因用多层填充床微反应器及反应方法

Citations (3)

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Publication number Priority date Publication date Assignee Title
EP0311712A1 (fr) * 1987-10-16 1989-04-19 Catalyst Technology, Inc. Trémie modulaire à tuyaux multiples pour charger un catalyseur
WO1993008907A1 (fr) * 1991-11-08 1993-05-13 Catalyst Technology, Inc. Gouttiere transporteuse de chargement de pellets catalytiques dans des reacteurs verticaux tubulaires
WO1998014392A1 (fr) * 1996-10-22 1998-04-09 Comardo Mathis P Systeme et procede de chargement d'un reacteur catalytique

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US3409411A (en) * 1965-07-26 1968-11-05 Exxon Research Engineering Co Apparatus for separating solids and loading reactor vessel
US3788370A (en) * 1972-02-10 1974-01-29 Shell Oil Co Particulate solids tube loading apparatus
US4402643A (en) * 1981-02-18 1983-09-06 Ppg Industries, Inc. Catalyst loader
US4479521A (en) * 1982-09-20 1984-10-30 Gte Products Corporation Phosphor manufacturing process
US4994241A (en) * 1983-07-15 1991-02-19 Catalyst Technology, Inc. Catalyst recovery through and process for unloading multi-tube reactors with maximum dust containment
US4701101A (en) * 1984-03-13 1987-10-20 Catalyst Technology, Inc. Modular multi-tube catalyst loading funnel
US4737269A (en) * 1986-05-15 1988-04-12 Catalyst Technology, Inc. Catalyst loading hopper
CA2141156A1 (fr) * 1994-01-27 1995-07-28 James S. Keller Dispositif pour le chargement de catalyseur pour oxyde d'ethylene
FR2747937B1 (fr) * 1996-04-26 1998-07-17 Total Raffinage Distribution Procede et dispositif pour le chargement homogene de particules d'un catalyseur solide dans un reacteur tubulaire
US5897282A (en) * 1996-10-01 1999-04-27 Comardo; Mathis P. Catalytic reactor charging system and method for operation thereof
JP4299891B2 (ja) * 1997-01-23 2009-07-22 株式会社日本触媒 粒状触媒の供給方法及びその供給装置
US6032828A (en) * 1997-10-20 2000-03-07 Arbo Engineering Inc. Catalyst exchange device
DE69906417T2 (de) * 1998-05-12 2004-01-08 Cat Tech Inc., Pasadena Vorrichtung zum füllen von Reaktorröhren
US6981529B2 (en) * 2002-06-28 2006-01-03 Catalyst Services, Inc. Measuring catalyst(s) for filling reactor tubes in reactor vessels
BRPI0620300A2 (pt) * 2005-12-21 2011-11-08 Catalyst Services Inc provisão para a liberação automática de catalisador e/ou particulados para qualquer dispositivo de sistema de enchimento utilizado para encher tubos

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0311712A1 (fr) * 1987-10-16 1989-04-19 Catalyst Technology, Inc. Trémie modulaire à tuyaux multiples pour charger un catalyseur
WO1993008907A1 (fr) * 1991-11-08 1993-05-13 Catalyst Technology, Inc. Gouttiere transporteuse de chargement de pellets catalytiques dans des reacteurs verticaux tubulaires
WO1998014392A1 (fr) * 1996-10-22 1998-04-09 Comardo Mathis P Systeme et procede de chargement d'un reacteur catalytique

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009262123A (ja) * 2008-03-31 2009-11-12 Mitsubishi Chemicals Corp プレート式触媒層反応器、該プレート式触媒層反応器に触媒を充填する方法及び該プレート式触媒層反応器を用いた反応生成物の製造方法
KR102030924B1 (ko) * 2018-04-13 2019-10-17 유한기술주식회사 촉매 로딩 장치 및 이를 포함하는 시스템

Also Published As

Publication number Publication date
RU2007140897A (ru) 2009-05-20
BRPI0608662A2 (pt) 2010-01-19
JP2008534410A (ja) 2008-08-28
EP1866069A1 (fr) 2007-12-19
DE102005016078A1 (de) 2006-10-12
US20060243342A1 (en) 2006-11-02
MX2007012334A (es) 2007-11-21
CN101151092A (zh) 2008-03-26
CA2603521A1 (fr) 2006-10-12

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