EP0759059B1 - Elektroflokkulator zur entfernung von feststoffen in kohlenwasserstoffumsetzungen - Google Patents

Elektroflokkulator zur entfernung von feststoffen in kohlenwasserstoffumsetzungen Download PDF

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Publication number
EP0759059B1
EP0759059B1 EP95920393A EP95920393A EP0759059B1 EP 0759059 B1 EP0759059 B1 EP 0759059B1 EP 95920393 A EP95920393 A EP 95920393A EP 95920393 A EP95920393 A EP 95920393A EP 0759059 B1 EP0759059 B1 EP 0759059B1
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EP
European Patent Office
Prior art keywords
catalyst particles
solid catalyst
electric field
process fluid
particles
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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.)
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EP95920393A
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English (en)
French (fr)
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EP0759059A1 (de
Inventor
Edward C. Hsu
Barry L. Tarmy
Costantine A. Coulaloglou
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ExxonMobil Technology and Engineering Co
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Exxon Research and Engineering Co
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G32/00—Refining of hydrocarbon oils by electric or magnetic means, by irradiation, or by using microorganisms
    • C10G32/02—Refining of hydrocarbon oils by electric or magnetic means, by irradiation, or by using microorganisms by electric or magnetic means

Definitions

  • the present invention is directed to a continuous method of removing solid catalyst particles from hydrocarbon process fluids, including Fischer-Tropsch process fluids, using an electric field preferably an electric field generated by an electroflocculating apparatus.
  • the invention is further directed to such apparatus.
  • WO 85/03017 a method and apparatus are described for removing particulate matter (for example catalyst fines) suspended in low dielectric, low conductivity liquids (for example oil). A unipolar current of extrinsic ions is passed through the flowing liquid to charge the particles. The charged particles are then removed by agglomeration or sedimentation.
  • particulate matter for example catalyst fines
  • low dielectric, low conductivity liquids for example oil
  • a method for separating solid catalyst particles from hydrocarbon process fluids comprises the steps of:
  • the process further comprises the step of:
  • the process further comprises the step of:
  • the present invention advantageously allows substantially catalyst particle-free fluid to be removed from a process without the use of filters which become blinded (clogged) necessitating interrupting the process for filter replacement or cleaning.
  • the method of the invention has no effect on the catalyst surface area, particle density, particle size, or catalyst activity.
  • the apparatus provides for the continuous removal of solid catalyst particles from process fluids and conveyance of the removed solid catalyst particles, which deagglomerate once removed from the electric field back into the reaction zone, if desired.
  • the electroflocculator can be located within or without (outside) the reactor.
  • Figure 1 schematically depicts one example of an electroflocculating apparatus where the electroflocculator is located inside a hydrocarbon synthesis bubble column.
  • FIG. 2 schematically shows another example of an electroflocculator apparatus.
  • the instant invention teaches a method for separating catalyst particles from process fluids having such particles suspended therein.
  • the method is capable of separating particles which are 1 micron in size up to and including a 0.3 cm particles.
  • the invention can remove suspended particles from any type of hydrocarbon liquid.
  • the invention is particularly useful for removing catalyst particles from slurry process fluids, particularly bubble column slurry process fluids, ebulating bed processes and stirred process fluids.
  • catalyst particles can be separated from the process fluids in accordance with the instant invention without any pretreatment of the process fluids. Thus, they can be introduced directly into the electroflocculator apparatusus from the hydrocarbon reaction vessel.
  • the invention merely requires that the solid catalyst particles contain at least 0.1 wt.%, based on the total particle weight, of a metal in its zero valence state.
  • Applicants have discovered that applying an electric field to a process fluid which contains about 0.1 to 50 wt.%, preferably 0.3 to 50 wt.% suspended solid catalyst particles containing at least 0.1 wt.% metal in the zero valence state, causes the solid catalyst particles to be temporarily agglomerated, causing them to settle, through gravity, out of the process fluid enabling the ready removal of process fluid from the fluid/solid mixture.
  • the catalyst particles Once the catalyst particles have settled and passed out of the electric field, they deagglomerate to their original size and are usable once again. Hence, they can be immediately returned to the reaction zone without interruption of the process being performed and a recirculating process (which reutilizes the deagglomerated catalyst particles) can be conducted.
  • the present invention can be utilized to reclaim, e.g., supported Fischer-Tropsch catalysts from slurry Fischer-Tropsch media.
  • the invention can additionally be used on promoted cobalt catalyst such as rhenium promoted cobalt.
  • the invention can be used to separate a cobalt-rhenium on titania catalyst from Fischer-Tropsch media.
  • the above catalysts are merely illustrative and are not meant to be limiting.
  • the instant invention is capable of removing >95% of the solid catalyst particles directly from the process fluid without the aid of any pretreatment steps.
  • a slurry process fluid can be passed through an electroflocculator, in accordance with the instant invention, whereupon the catalyst particles present will agglomerate and settle to the electroflocculator vessel bottom. Once the catalyst particles are outside of the forces of the electrical field, they deagglomerate. The catalyst particles can then be passed back into the slurry process reaction zone if desired. Process fluid having catalyst particles removed therefrom can be withdrawn from the electroflocculator vessel by any suitable means. In the instant process there is substantially no migration of the catalyst to the electrodes, preferably no such migration will occur.
  • the preferred mode of carrying out the instant invention is to pass the process fluid having suspended solid catalyst particle therein through an electroflocculator by utilizing techniques such as the "downcomer" effect commonly practiced in chemical engineering.
  • the term "downcomer effect” used herein refers to a well-known technique for causing liquid in a first upwardly or downwardly extending volume (e.g., in a tube or vessel) to have a higher apparent density than liquid in a second upwardly or downwardly extending volume (e.g., in another tube or vessel) wherein liquid can flow between the upper regions of both volumes and between the lower regions of both volumes.
  • the apparent liquid density in the second volume is reduced by bubbles of gas therein.
  • the differing liquid densities in the two connected volumes cause upward liquid flow in the second volume and downward liquid flow in the first volume.
  • the flocculator is a vessel equipped with an AC voltage source across two electrodes (one electrode being "hot” (i.e. connected to a source of alternating current), and the other earthed or ground) capable of producing AC voltage of from about 0.1 hertz, up to and including about 5000 hertz of current.
  • the electrical field strength produced will be from about 100 volts/cm up to and including about 100,000 volts/cm, preferably from about 200 to about 50,000 volts/cm.
  • the electroflocculator will be equipped with a metal screen, at the area where the process fluid and catalyst particles enter to exclude gas bubbles.
  • the openings of the screen should be adequate to exclude most gas bubbles in the process fluid but allow the passing of the particles.
  • the electroflocculator will be equipped with both a baffle and a metal screen. The baffle helps to further exclude gas bubbles. Once the solid catalyst particles experience the electric field, they agglomerate and settle through the opening at the bottom of the electroflocculator. They can thus be readily removed.
  • the departiculated process stream can be collected by any suitable means such as siphoning from near the top of the electroflocculator, decanting, etc.
  • the instant method can be carried out with an electroflocculator inside the reaction vessel, enabling the agglomerated catalyst particles, which deagglomerate without any change in size, surface area, particle density or catalyst activity, to be passed back into the reaction zone once removed from the electroflocculator.
  • the electroflocculator could alternatively be external to the reaction vessel itself. In the external setup, the deagglomerated particles may be returned to the reaction zone by any suitable means such as pumping.
  • the small catalyst particles having zero valence metal therein, will experience electric dipole/dipole interactions and will flocculate to agglomerates that exhibit a much higher settling velocity than deagglomerated particles. Because gas will have preferably been removed from the fluid, there will be a driving force for the liquid to flow downward due to the Downcomer effect. This Downcomer effect will be countered by any process fluid removal during settling. Provided the net rising velocity of the process liquid is less than the settling velocity of the agglomerated particles, most particles can be removed through enhanced settling of the agglomerates.
  • the electroflocculator may be equipped with a screen or filter at the product withdrawal outlet to filter any solid residual catalyst particles that might be present near the siphoning outlet due to inadequate residence times.
  • the horizontal cross-sectional area of the upper zone of the electroflocculator, the zone of high electric field above the entrance and below the exit port for clarified product, will be sized such that the liquid upflow velocity in this zone is about a factor of 2 to about 40 of the Stokes velocity of the particles being separated.
  • the height of this zone should be such that it allows a residence time of at least 0.1 minutes, preferably at least about 0.5 minutes. The longer the residence time, the greater the departiculation efficiency.
  • the apparatus which will preferably be used to carry out the method of the instant invention will consist of a reactor vessel equipped with an electroflocculator attached to the outside of the reactor or present within the reactor. Additionally, the electrodes of the electroflocculator may be within or external to the flocculator shell. The electrodes need only produce an electric field which penetrates the process fluid having suspended catalyst particles therein, they needn't directly contact the fluid.
  • the electroflocculator on the outside of the reactor vessel will be piped to the reactor and will contain a valve for process fluid drawoff.
  • the bottom of the flocculator will be piped back into the reactor to enable the agglomerated catalyst particles to be removed from the electric field, deagglomerated and passed back into the reactor to participate in the reaction being carried out if a recirculating process is desired.
  • the electroflocculator When the electroflocculator is contained within the reactor, its vessel walls will preferably have a portion composed of wire mesh of about 200-2000 micron opening size, which will allow the slurry process fluid to flow into the electroflocculator.
  • the bottom of the flocculator will be open, allowing agglomerated particles to pass out of the flocculator and into the process vessel.
  • a portion of the flocculator, preferably the top, will protrude from the reactor vessel, enabling process fluid having catalyst removed therefrom to be siphoned off.
  • the process fluid withdrawal port will be inside the process vessel allowing liquid to be returned to the reaction zone.
  • the electroflocculator is located inside a hydrocarbon synthesis bubble column reactor. It consists of a hollow metal shell (A) which serves as a ground electrode, a center electrode (b) connected to a high voltage source (C) which electrode is insulated from the shell (A). Slurry process fluid enters through ports (D) which are metal screens and serve also as grounded grid electrodes. The bottom of the shell is open (E) to the reactor to allow for deagglomerated particles to be expelled from the shell. The top of the shell is connected to a tube (F) which serves as a drawoff port for the removal of product fluid.
  • the efficiency of the cylinder has been increased by the addition of a baffle plate (G) external to the shell beneath the screen.
  • the baffle prevents gas bubbles from contacting the screen. Removal of gas bubbles sets up a gradient which promotes the continuous flow of slurry from the reactor into the shell and exit through the opening (E) due to the Downcomer effect.
  • the system comprises a shell (A) equipped with an electrode pair consisting of a metal rod (B) connected to a high voltage source (D) and a metal mesh screen (C) connected to the ground.
  • a recirculating pump (H) is used to pump feed to the electroflocculator through port (E). Concentrated slurry exits the flocculator via exit port (F) and is then recirculated via the pump. Departiculated raffinate is withdrawn via port (G).
  • the process fluids which are clarified by use of the instant invention have a dielectric constant of about 2 to about 4, preferably about 2 to about 3. They exhibit an electric conductivity less than about 1 x 10 -10 ohm -1 m -1 , preferably less than 5 x 10 -11 ohm -1 m -1 .
  • the experiments were carried out in a 4 ⁇ 76 cm ID by 13 ⁇ 97 cm long (1 7/8" ID by 5.5" long) glass vessel fitted with an electrode pair consisting of a 4 ⁇ 32 cm D x 7 ⁇ 62 cm L (1.7"D x 3"L) cylindrical metal screen and a central electrode.
  • the electrodes were connected to the terminals of a high voltage power source capable of generating up to 10 thousand volts of electric potential at frequencies ranging from 40 hertz to 250 hertz.
  • a second series of experiments were carried out in an apparatus shown in Figure 2 which was designed to simulate the operation of which was designed to simulate the operation of an electroflocculator to confine catalyst in a chemical reactor.
  • a 4 ⁇ 76 cm ID by 13 ⁇ 97 cm high (1 7/8" ID by 5.5" high) glass vessel was fitted with an electrode pair consisting of a 4 ⁇ 32 cm D x 7 ⁇ 62 cm L (1.7"D x 3"L) cylindrical metal screen and a central electrode. They were connected to the terminals of a high voltage power source capable of generating up to 10 thousand volts, producing an electric field of 2000 to 4000 volts/cm at frequencies from 50 to 250 hertz.
  • Slurry was fed from a pump into the side of the electroflocculator vessel close to the bottom of the electrode pair at a flow rate of about 1300 cc/min.
  • the solid particles were to be electroflocculated in the zone between the two electrodes, settled to the bottom of the vessel, and removed as a concentrated slurry at flow rates from 840 to 1080 cc/min.
  • the raffinate with solids removed exited from the top of the vessel at flow rates from 280 to 420 cc/min.
  • the returned concentrated slurry and raffinate streams were remixed to reconstitute the feed for a continuous test to reach steady state.
  • a small batch electroflocculation test tube was set up to allow a visual confirmation of the flocculation when the electric voltage was applied to the slurry.
  • two aluminum foil electrodes were attached to the outside of the glass tube, and connected to the 10 KV/200 hertz voltage source.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Claims (10)

  1. Verfahren zum Abtrennen von festen Katalysatorteilchen aus Kohlenwasserstoffverfahrensfluiden, bei dem in Stufen
    (a) eine Mischung aus Verfahrensfluid und festen Katalysatorteilchen einem elektrischen Feld ausgesetzt wird, wobei die festen Katalysatorteilchen mindestens 0,1 Gew.% Metall im Wertigkeitszustand Null enthalten, das Verfahrens fluid eine elektrische Leitfähigkeit von weniger als 1 x 10-10 ohm-1m-1 zeigt und das elektrische Feld eine elektrische Feldstärke von mehr als 100 Volt/cm und eine Frequenz von mindestens 0,1 Hertz hat, um agglomerierte feste Katalysatorteilchen zu erzeugen,
    (b) mittels Schwerkraft die agglomerierten festen Katalysatorteilchen von dem Kohlenwasserstoffverfahrensfluid abgetrennt werden.
  2. Verfahren nach Anspruch 1, das Stufe (c) umfaßt, in der die abgetrennten agglomerierten festen Katalysatorteilchen aus dem elektrischen Feld entfernt werden, um desagglomerierte feste Katalysatorteilchen zu erzeugen.
  3. Verfahren nach Anspruch 2, das -Stufe (d) umfaßt, in der die desagglomerierten festen Katalysatorteilchen wieder in eine Kohlenwasserstoffverfahrensreaktionszone eingebracht werden.
  4. Verfahren nach einem der Ansprüche 1 bis 3, bei dem die festen Katalysatorteilchen 1 µm bis 0,3 cm Teilchen sind.
  5. Verfahren nach einem der Ansprüche 1 bis 4, bei dem die Mischung aus Verfahrensfluid und festen Katalysatorteilchen 0,1 bis 50 Gew.% feste Katalysatorteilchen enthält.
  6. Verfahren nach einem der Ansprüche 1 bis 5, bei dem die Mischung aus Verfahrens fluid und festen Katalysatorteilchen ohne jede Vorbehandlung direkt in das elektrische Feld eingebracht wird.
  7. Verfahren nach einem der Ansprüche 1 bis 6, bei dem > 95 % der festen Katalysatorteilchen aus der Mischung aus Verfahrensfluid und festen Katalysatorteilchen entfernt werden.
  8. Verfahren nach einem der Ansprüche 1 bis 7, bei dem das Verfahrens fluid eine Aufschlämmung, ein Sprudelbett oder ein gerührtes Verfahrensfluid ist.
  9. Reaktorapparatur zur kontinuierlichen Entfernung von festen Katalysatorteilchen, die mindestens 0,1 Gew.% Metall im Wertigkeitszustand Null enthalten, aus Aufschlämmungsverfahrensfluiden, wobei ein Kohlenwasserstoffverfahrensgefäß an einer Elektroflockulatorapparatur befestigt oder mit dieser verbunden ist, wobei die Elektroflockulatorapparatur
    (a) einen Hohlmantel mit mindestens einem Einlaß zur Einbringung einer Mischung aus Kohlenwasserstoffverfahrensfluiden und festen Katalysatorteilchen, wobei die Katalysatorteilchen mindestens 0,1 Gew.% Metall im Wertigkeitszustand Null enthalten, einem oberen Auslaß zum Abziehen von Produktfluid und einem Bodenauslaß zum Ablassen von desagglomerierten Katalysatorteilchen,
    (b) eine Vielzahl von Elektroden in funktioneller Beziehung zu dem Hohlmantel, wobei sich die Elektroden über den Einlaß des Hohlmantels hinaus erstrecken, und
    (c) eine Hochspannungsquelle umfaßt, die mit den Elektroden gekoppelt ist und in der Lage ist, eine elektrische Feldstärke von mehr als 100 Volt/cm und eine Frequenz von 0,1 bis 5000 Hz innerhalb des Hohlmantels zu erzeugen.
  10. Verfahren nach Anspruch 9, bei dem der Elektroflockulator innerhalb oder außerhalb des Reaktors angeordnet ist.
EP95920393A 1994-05-10 1995-05-10 Elektroflokkulator zur entfernung von feststoffen in kohlenwasserstoffumsetzungen Expired - Lifetime EP0759059B1 (de)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US24030894A 1994-05-10 1994-05-10
US240308 1994-05-10
US41832495A 1995-04-07 1995-04-07
US418324 1995-04-07
PCT/US1995/005869 WO1995030726A1 (en) 1994-05-10 1995-05-10 Electroflocculator for solids removal in hydrocarbon processes

Publications (2)

Publication Number Publication Date
EP0759059A1 EP0759059A1 (de) 1997-02-26
EP0759059B1 true EP0759059B1 (de) 1999-01-20

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EP95920393A Expired - Lifetime EP0759059B1 (de) 1994-05-10 1995-05-10 Elektroflokkulator zur entfernung von feststoffen in kohlenwasserstoffumsetzungen

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EP (1) EP0759059B1 (de)
AU (1) AU694231B2 (de)
CA (1) CA2190026C (de)
DE (1) DE69507468T2 (de)
NO (1) NO964737D0 (de)
WO (1) WO1995030726A1 (de)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB0306307D0 (en) * 2003-03-19 2003-04-23 Bp Exploration Operating Electromechanical filter
GB2404885B (en) * 2003-08-12 2006-03-01 Mi Llc Electrical treatment for oil based drilling or completion fluids
US8142634B2 (en) 2007-03-09 2012-03-27 M-I L.L.C. Method and apparatus for electrophoretic separation of solids and water from oil based mud
CN108165298B (zh) * 2018-01-04 2020-03-31 中石化炼化工程（集团）股份有限公司 油浆净化方法、油浆净化装置及油浆净化设备
CN111303937A (zh) * 2019-08-20 2020-06-19 武汉兰兆科技有限公司 一种费托合成催化剂在线回收利用的电分离装置及电分离工艺

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3928158A (en) * 1973-05-22 1975-12-23 Gulf Research Development Co Electrofilter
US4358379A (en) * 1980-11-21 1982-11-09 Noboru Inoue Process for refining electric insulating liquids
US4579637A (en) * 1984-01-10 1986-04-01 American Filtrona Corporation Method and apparatus for separating impurities from low conductivity liquids
US5308586A (en) * 1992-05-01 1994-05-03 General Atomics Electrostatic separator using a bead bed

Also Published As

Publication number Publication date
CA2190026C (en) 2005-04-12
DE69507468T2 (de) 1999-09-02
NO964737L (no) 1996-11-08
WO1995030726A1 (en) 1995-11-16
DE69507468D1 (de) 1999-03-04
EP0759059A1 (de) 1997-02-26
NO964737D0 (no) 1996-11-08
CA2190026A1 (en) 1995-11-16
AU694231B2 (en) 1998-07-16
AU2585895A (en) 1995-11-29

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