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US20060243342A1 - Method for filling apparatuses with solids - Google Patents

Method for filling apparatuses with solids Download PDF

Info

Publication number
US20060243342A1
US20060243342A1 US11/399,451 US39945106A US2006243342A1 US 20060243342 A1 US20060243342 A1 US 20060243342A1 US 39945106 A US39945106 A US 39945106A US 2006243342 A1 US2006243342 A1 US 2006243342A1
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US
United States
Prior art keywords
tube
filling
filled
tubes
solids
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.)
Abandoned
Application number
US11/399,451
Other languages
English (en)
Inventor
Jan-Olaf Barth
Achim Fischer
Wolfgang Bock
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
Assigned to DEGUSSA AG reassignment DEGUSSA AG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BARTH, JAN-OLAF, BOCK, WOLFANG, WECKBECKER, CHRISTOPH, BURKHARDT, WERNER, FISCHER, ACHIM, HUTHMACHER, KLAUS
Assigned to DEGUSSA AG reassignment DEGUSSA AG CORRECTED COVER SHEET TO CORRECT THE NAME OF ASSIGNOR #3, PREVIOUSLY RECORDED AT REEL/FRAME 018062/0608 (ASSIGNMENT OF ASSIGNOR'S INTEREST) Assignors: BARTH, JAN-OLAF, BOECK, WOLFGANG, WECKBECKER, CHRISTOPH, BURKHARDT, WERNER, FISCHER, ACHIM, HUTHMACHER, KLAUS
Publication of US20060243342A1 publication Critical patent/US20060243342A1/en
Assigned to DEGUSSA GMBH reassignment DEGUSSA GMBH CHANGE OF ENTITY Assignors: DEGUSSA AG
Assigned to EVONIK DEGUSSA GMBH reassignment EVONIK DEGUSSA GMBH CHANGE ADDRESS Assignors: EVONIK DEGUSSA GMBH
Assigned to EVONIK DEGUSSA GMBH reassignment EVONIK DEGUSSA GMBH CHANGE OF NAME Assignors: DEGUSSA GMBH
Abandoned 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
    • B01J8/0015—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 apparatuses used in chemical production with solids using a regulatable metering device, and an apparatus, displaceable from place to place, for carrying out the method.
  • the apparatus is particularly suitable for filling heat exchangers, absorption columns, distillation columns or tube-bundle reactors with solids.
  • the uniform filling of solids into tubes, tube-bundles or heat exchangers is of decisive importance for the efficiency of these apparatuses.
  • the solids may be, for example, packings, such as Raschig rings, ceramic balls or catalysts and may have different compositions and geometries, such as, for example, those of spheres, solid cylinders, hollow cylinders or rings.
  • the prior art discloses methods and apparatuses for filling tube reactors with shaped catalysts.
  • U.S. Pat. No. 4,402,643 and EP 0 904 831 B (U.S. Pat. No. 6,170,67-0 B1) describe the feeding of particulate material and the associated apparatuses, the material being transported via a channel caused to vibrate into the tubes to be filled.
  • the invention relates to a method for filling tubes with solids, in which the solid is discharged from a filling funnel (2) onto a skew plane having vibrating channels (4), which is arranged in an approximately horizontal position and extends from the discharge orifice of the funnel up to at least the connection to the drop tube (5) or a flexibile hose connection, through which the solid is fed to the tube to be filled, characterized in that in each case
  • the solid is thus metered in a uniform manner by control or regulation of the vibration frequency of the vibrating channel (4).
  • the amount metered or the metering rate can also be adjusted, optionally simultaneously, by means of the flow controller (3) which is adjustable in height and has the form of a weir.
  • drop tubes which are adjustable in their height or the flexibile hose connections prove to be particularly advantageous because in this way small differences in the height of the tubes to be filled can also be compensated and gaps between drop tube and reactor tube are avoided.
  • the solids to be filled which preferably have a mean particle size of at least 1 mm, may be mouldings of different type and suitability, such as, for example, Raschig rings, ceramic balls, inert bodies or shaped catalysts, for example in the form of granules, extrudates or pelletts in the commercial dimensions.
  • Reactions with such catalylsts are, for example, the preparation of ethylene oxide, phthalic anhydride, acrolein, acrylic acid, methyl mercaptan, hydrogen sulphide and others.
  • the object of the invention is to obtain a homogeneous solid bed and to avoid mechanical destruction of the solids.
  • Zone-by-zone filling of the solids can advantageously be achieved by the method described here, so that different fillings of solids having exactly defined volume can simultaneously be introduced along the axial profile of the tube.
  • the method according to the invention is characterized by a uniform distribution of the heights of fill, so that, when the tubes are fed with a constant gas flow, differential dynamic pressures with a mean standard deviation from the mean value of in general less than 10% result.
  • the filling of the solid is effected by means of an apparatus as shown in FIGS. 1 and 5 .
  • the amount of solid to be filled for each reaction tube is first determined volumetrically or gravimetrically and initially introduced into a collecting vessel.
  • the amount to be filled is preferably determined gravimetrically.
  • the collecting vessel has at least the volume of the solids to be filled.
  • the collecting vessel is opened and is introduced with the opening facing downwards into a filling funnel 2 .
  • the solids are loosened by means of an apparatus initially by vibrations, are caused to execute oscillatory and translational movement and are fed via a skew plane 4 (vibrating channel) uniformly to a metering device.
  • the number of channels on the skew plane corresponds to the number of tubes to be filled simultaneously each time.
  • the metering device is connected to the apparatus to be filled (for example a reaction tube in tube-bundle reactors) by means of drop tubes 5 adjustable in height, and permits loss-free feeding of the solids by means of an outflow tube 6 adjustable in height.
  • Apparatuses which permit a direct connection between the apparatus for filling solid beds and the apparatus to be filled are used as the metering device. Funnels, tubes and flexible hose connections are expedient for this purpose.
  • FIG. 1 shows that one connection each for an extraction apparatus 1 and an extraction tube 10 , by means of which the dust optionally occurring as a result of application of reduced pressure and solid particles are extracted, is present in the vicinity of the filling funnel and the drop tubes adjustable in height.
  • the solid bed be fed in a uniform, slow and reproducible mass flow to the apparatus.
  • This apparatus may be a heat exchanger, an absorption column, a distillation column and a tube-bundle reactor. Tube-bundle heat exchangers which are used as reactors are particularly preferred. These reaction tubes may also have internals (e.g. thermocouples).
  • the apparatus according to the invention permits control of the mass flow by variation of the vibration frequency of the apparatus, advantageously by means of electrical thyristor control 7 . Regulation of the mass flow is also possible by means of the flow controller 3 at the transition from the filling funnel to the vibrating channels, which flow regulator is adjustable in height.
  • the solid bed should be fed to the apparatus by a uniform vibratory movement of the collecting container, of the skew plane and of the metering device.
  • a collecting apparatus (filling funnel) for the solid filling, a feed device (skew plane) and a metering device are integrated in one apparatus.
  • Up to 50, preferably up to 20, of these apparatuses can be integrated in a portioning device in order to fill a plurality of tubes or the like simultaneously and efficiently.
  • FIG. 1 shows, for example, an apparatus by means of which 5 tubes can be filled simultaneously. By the simultaneous filling of a plurality of tubes, reproducible, uniform filling is ensured.
  • the solids are set into motion by vibration of a skew plane.
  • vibration of a skew plane Of particular importance here is the exact and fine adjustment of the vibration in order to keep the flow rate as uniform as possible. This requirement is met by commercial electrical vibrator motors.
  • Variation of the vibration frequency by means of an electronic control enables the intensity of vibration of the solid and hence the outflow rate thereof to be influenced.
  • This plane is advantageously closed by a preferably transparent cover (e.g. of plastic) in order to avoid a loss of solids and dust emissions.
  • a tube orifice 10 which, when connected to an extraction device, ensures removal of solid dust and impurities is advantageously present in the vicinity of the orifices of the metering device.
  • the apparatus is mounted on rollers or rolls 11 so that it can be operated and moved simultaneously by one person.
  • the roll can be adjusted in height.
  • the invention also relates to an apparatus, displaceable from place to place, for filling tubes with solids, comprising
  • the cross section of the drop tube is at most equal to the cross section of the tube to be filled.
  • it has a smaller cross section and tapers conically at its ends so that it fits into the tube to be filled.
  • FIG. 1 shows an arrangement according to the invention (side view) of a portioning device for the simultaneous filling of five tubes with particulate solids.
  • FIG. 2 shows an arrangement according to the invention of the filling funnel and of the connection for an extraction apparatus of a portioning device for the simultaneous filling of five tubes with particulate solids (view from above)
  • FIG. 3 shows an arrangement according to the invention of the drop tubes and of the height-adjustable outflow of a portioning device for the simultaneous filling of five tubes with particulate solids (view from the front).
  • FIG. 4 shows an arrangement according to the invention of the vibrating channels of a portioning device for the simultaneous filling of five tubes with particulate solids (view from above).
  • FIG. 5 shows an arrangement according to the invention (side view) of a portioning device for the filling of a tube with particulate solids.
  • FIGS. 6 shows an arrangement according to the invention (view from above) of a portioning device for the filling of a tube with particulate 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)
US11/399,451 2005-04-08 2006-04-07 Method for filling apparatuses with solids Abandoned US20060243342A1 (en)

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
DK102005016078.6 2005-04-08

Publications (1)

Publication Number Publication Date
US20060243342A1 true US20060243342A1 (en) 2006-11-02

Family

ID=36405883

Family Applications (1)

Application Number Title Priority Date Filing Date
US11/399,451 Abandoned US20060243342A1 (en) 2005-04-08 2006-04-07 Method for filling apparatuses with solids

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
US20110083769A1 (en) * 2009-10-01 2011-04-14 IFP Energies Nouvelles Device for loading particles of catatlyst into tubes having an annular zone
US20110131930A1 (en) * 2009-12-09 2011-06-09 Fernando Antonio Pessoa Cavalcanti Method for blending and loading solid catalyst material into tubular structures

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE202007019017U1 (de) 2007-09-14 2010-03-25 Süd-Chemie AG Befüllvorrichtung zum Befüllen eines Rohres eines Rohrbündelreaktors mit einem Schüttgut
JP5593600B2 (ja) * 2008-03-31 2014-09-24 三菱化学株式会社 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
SG11201406831WA (en) * 2012-04-23 2014-11-27 Mourik Internat B V Catalyst loading tool
KR102030924B1 (ko) * 2018-04-13 2019-10-17 유한기술주식회사 촉매 로딩 장치 및 이를 포함하는 시스템
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 (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
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
US5626455A (en) * 1994-01-27 1997-05-06 Basf Corporation Ethylene oxide catalyst loading device
US5890868A (en) * 1996-10-01 1999-04-06 Comardo; Mathis P. Catalytic reactor charging system and method for operation thereof
US5906229A (en) * 1996-04-26 1999-05-25 Total Raffinage Distribution S.A. Method and device for the uniform filling of particles of a solid catalyst into a tubular reactor
US6032828A (en) * 1997-10-20 2000-03-07 Arbo Engineering Inc. Catalyst exchange device
US6170670B1 (en) * 1997-01-23 2001-01-09 Nippon Shokubai Co., Ltd. Methods of and apparatus for feeding granular material
US6409977B2 (en) * 1998-05-12 2002-06-25 Shell Oil Company Reactor tube loading device
US6981529B2 (en) * 2002-06-28 2006-01-03 Catalyst Services, Inc. Measuring catalyst(s) for filling reactor tubes in reactor vessels
US7309201B2 (en) * 2005-12-21 2007-12-18 Catalyst Services, Inc. Providing automated delivery of catalyst and/or particulate to any filling system device used to fill tubes

Family Cites Families (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
AU7476496A (en) * 1996-10-22 1998-04-24 Mathis P. Comardo Catalytic reactor charging system and method

Patent Citations (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
US5626455A (en) * 1994-01-27 1997-05-06 Basf Corporation Ethylene oxide catalyst loading device
US5906229A (en) * 1996-04-26 1999-05-25 Total Raffinage Distribution S.A. Method and device for the uniform filling of particles of a solid catalyst into a tubular reactor
US5890868A (en) * 1996-10-01 1999-04-06 Comardo; Mathis P. Catalytic reactor charging system and method for operation thereof
US5897282A (en) * 1996-10-01 1999-04-27 Comardo; Mathis P. Catalytic reactor charging system and method for operation thereof
US6132157A (en) * 1996-10-01 2000-10-17 Comardo; Mathis P. Catalytic reactor charging system and method for operation thereof
US6170670B1 (en) * 1997-01-23 2001-01-09 Nippon Shokubai Co., Ltd. Methods of and apparatus for feeding granular material
US6032828A (en) * 1997-10-20 2000-03-07 Arbo Engineering Inc. Catalyst exchange device
US6409977B2 (en) * 1998-05-12 2002-06-25 Shell Oil Company Reactor tube loading device
US6905660B2 (en) * 1998-05-12 2005-06-14 Cat Tech, Inc. Process for loading a reactor
US6981529B2 (en) * 2002-06-28 2006-01-03 Catalyst Services, Inc. Measuring catalyst(s) for filling reactor tubes in reactor vessels
US7309201B2 (en) * 2005-12-21 2007-12-18 Catalyst Services, Inc. Providing automated delivery of catalyst and/or particulate to any filling system device used to fill tubes

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110083769A1 (en) * 2009-10-01 2011-04-14 IFP Energies Nouvelles Device for loading particles of catatlyst into tubes having an annular zone
US8578978B2 (en) * 2009-10-01 2013-11-12 IFP Energies Nouvelles Device for loading particles of catalyst into tubes having an annular zone
US20110131930A1 (en) * 2009-12-09 2011-06-09 Fernando Antonio Pessoa Cavalcanti Method for blending and loading solid catalyst material into tubular structures
EP2332641A1 (fr) 2009-12-09 2011-06-15 Rohm and Haas Company Procédé de mélange et de chargement d un matériau catalyseur solide dans des structures tubulaires

Also Published As

Publication number Publication date
MX2007012334A (es) 2007-11-21
EP1866069A1 (fr) 2007-12-19
DE102005016078A1 (de) 2006-10-12
CN101151092A (zh) 2008-03-26
BRPI0608662A2 (pt) 2010-01-19
WO2006106019A1 (fr) 2006-10-12
JP2008534410A (ja) 2008-08-28
RU2007140897A (ru) 2009-05-20
CA2603521A1 (fr) 2006-10-12

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Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:BARTH, JAN-OLAF;FISCHER, ACHIM;BOCK, WOLFANG;AND OTHERS;REEL/FRAME:018062/0608;SIGNING DATES FROM 20060531 TO 20060612

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