EP0022442B1 - Verfahren und Vorrichtung zum Herstellen von Emulsionen - Google Patents

Verfahren und Vorrichtung zum Herstellen von Emulsionen Download PDF

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Publication number
EP0022442B1
EP0022442B1 EP79301398A EP79301398A EP0022442B1 EP 0022442 B1 EP0022442 B1 EP 0022442B1 EP 79301398 A EP79301398 A EP 79301398A EP 79301398 A EP79301398 A EP 79301398A EP 0022442 B1 EP0022442 B1 EP 0022442B1
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EP
European Patent Office
Prior art keywords
emulsion
enclosure
oil
orifice
packed
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
Application number
EP79301398A
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English (en)
French (fr)
Other versions
EP0022442A1 (de
Inventor
Norman Nian-Tze Li
Taras Hucal
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.)
ExxonMobil Technology and Engineering Co
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Exxon Research and Engineering Co
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Filing date
Publication date
Application filed by Exxon Research and Engineering Co filed Critical Exxon Research and Engineering Co
Priority to DE7979301398T priority Critical patent/DE2967203D1/de
Priority to EP79301398A priority patent/EP0022442B1/de
Publication of EP0022442A1 publication Critical patent/EP0022442A1/de
Application granted granted Critical
Publication of EP0022442B1 publication Critical patent/EP0022442B1/de
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/32—Liquid carbonaceous fuels consisting of coal-oil suspensions or aqueous emulsions or oil emulsions
    • C10L1/328—Oil emulsions containing water or any other hydrophilic phase
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • B01F23/4105—Methods of emulsifying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/41—Emulsifying
    • B01F23/414—Emulsifying characterised by the internal structure of the emulsion
    • B01F23/4144—Multiple emulsions, in particular double emulsions, e.g. water in oil in water; Three-phase emulsions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/45—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads
    • B01F25/452—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by elements provided with orifices or interstitial spaces
    • B01F25/4524—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by elements provided with orifices or interstitial spaces the components being pressed through foam-like inserts or through a bed of loose bodies, e.g. balls
    • B01F25/45242—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by elements provided with orifices or interstitial spaces the components being pressed through foam-like inserts or through a bed of loose bodies, e.g. balls through a bed of fibres, steel wool or wood chips
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0418—Geometrical information
    • B01F2215/0431—Numerical size values, e.g. diameter of a hole or conduit, area, volume, length, width, or ratios thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/044—Numerical composition values of components or mixtures, e.g. percentage of components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2215/00—Auxiliary or complementary information in relation with mixing
    • B01F2215/04—Technical information in relation with mixing
    • B01F2215/0413—Numerical information
    • B01F2215/0436—Operational information
    • B01F2215/0477—Numerical time values

Definitions

  • Emulsions can be visualised in simple terms as one discontinuous internal phase or fluid enveloped in a second dissimilar continuous external phase or fluid.
  • emulsions fall into two broad categories, oil-in-water emulsions wherein the oil is the discontinuous internal phase and the water is the continuous external phase, or a water in oil emulsion, where the above rules are reversed.
  • oil-in-water emulsions wherein the oil is the discontinuous internal phase and the water is the continuous external phase
  • a water in oil emulsion where the above rules are reversed.
  • multiple emulsions such as water-oil-water emulsion wherein there is a discontinuous external oil phase suspended in a continuous water external phase; or an oil-water-oil multiple emulsion wherein the above roles are reversed, i.e. in all liquid membrane systems.
  • Emulsions whether they are water-in-oil or oil-in-water are further characterised as being low ratio or high ratio.
  • Low ratio emulsions are generally no higher than 4/1 internal phase to external phase whereas high ratio emulsions are normally greater than 4/1, preferably greater than 8/1 internal phase to external phase.
  • Low ratio emulsions possess very small droplet sizes, usually of the order of 1 micron, while high ratio emulsions possess relatively larger particle sizes of the order of 20 micron or more.
  • the immiscible fluids which are introduced into the packed enclosure through the entrance orifice or orifices may be fed into the enclosure by fluid feeding means selected from pumping means, gravity conduit means, syringe means and combinations thereof, in communication with fluid storage means such as tanks or reservoirs, etc. Preferably single or multiple pumps are used.
  • the fluids fed into the packed enclosure may be introduced into the enclosure either through the same entrance orifice serviced by the fluid feeding means or each fluid through individual entrance orifices in close proximity one to another so as to ensure maximum intermixing of the different fluids.
  • any number of packed enclosure emulsion generators can be used, with each generator mixing two or more fluids, or a single generator can be used with the fluids introduced either simultaneously through a single entrance orifice or with each fluid fed into the packed enclosure through individual entrance orifices situated on the apparatus, it being preferred that all fluids desired to be mixed are fed into the enclosure simultaneously. If necessary, however, the individual fluids can be fed into the enclosure sequentially.
  • the packed enclosure can also be equipped with a return loop conduit whereby either all or part of the emulsion leaving the exit orifice is reintroduced into the entrance orifice for recirculation through the packed enclosure either alone or along with added component fluids. In this way a higher degree of emulsification can be obtained if desired. It is most preferred that separate packed enclosure emulsifiers be used to prepare individual emulsions when the final emulsion comprises a multiple emulsion, such as a water/oil/water system.
  • the emulsion is formed using an apparatus which as for example illustrated in the accompanying drawing, comprises an emulsion-forming enclosure (3) which has (a) at least one inlet orifice (1) for the introduction of immiscible fluids, (b) a zone or bed (4) in communication with the inlet orifice(s) and packed with at least one material selected from steel metal sponge, metal shavings, ceramic chips, cannon packing, animal hair or plastic brush, metal tubes shorter than the internal diameter of the enclosure and Berl saddle, and (c) at least one outlet orifice (2) in communication with the zone or bed (4) for removal of formed emulsion; said enclosure (3) preferably having a cross-sectional profile, when viewed at right angles to the flow-path therethrough, of a regular or irregular figure having at least three sides.
  • the apparatus comprises an enclosure, typically a pipe or column.
  • This enclosure can be of any cross-sectional profile, i.e., any regular or irregular multi-sided configuration of n sides wherein n ranges from 3 to infinity (i.e. circular).
  • the enclosure has orifices so as to permit the entrance of the fluids and the exit of said fluids. These orifices can be either the normal open ends of a piece of pipe or, if the enclosure has no "normally" open end the orifice can be specially constructed in the wall of the enclosure. What is necessary is that there be at least one entrance orifice and one exit orifice.
  • these entrances and exit orifices are situated at the maximum possible distance away from each other along the axis of fluid flow in the enclosure so as to ensure maximum mixing between the fluids introduced into the enclosure. It is possible, and in some instances desirable, that there be multiple entrance orifices in which case each individual fluid can be introduced into the enclosure through its own entrance orifice. When multiple entrance orifices are employed they can be either serially located parallel to the fluid flow or radially in the enclosure wall in the perimeter of the enclosure defined by a plane passing perpendicular to the direction of flow in the enclosure.
  • the enclosure is packed with a material which causes the fluids introduced into the enclosure through the entrance orifice to split into many fine streams and to re-mix rapidly and repeatedly resulting in the formation of the desired emulsion.
  • This material is packed into the enclosure in a random manner to as high a degree of density as is possible, short of plugging the enclosure, i.e. the fluid pressure drop between the entrance and exit may not equal zero.
  • Suitable packing material includes steel metal sponge (such as Kurly Kate), metal shavings, ceramic chips, Berl Saddle (e.g. certain porcelain forms available from Fisher Scientific Company-their catalogue Stock No.
  • the length of the enclosure from entrance orifices to exit orifices, the amount of packing, the density of the packing, and the type of material packed is left to the discretion of the practitioner, depending on the type of emulsion desired, the density of the fluids used and the final ratio of internal to external phase desired.
  • the component fluids fed into the packed enclosure are fed into the enclosure by fluid feed means.
  • These fluid feed means are typically selected from pumps for each individual fluid or group of fluids or gravity feed tanks and conduits or syringes for each fluid or group of fluids or any combination of the above.
  • the preferred fluid feed means comprises pumps for the component fluids.
  • a water and oil combination can be added to the enclosure in sufficient ratio to give a water in oil (w/o) emulsion.
  • a separate water stream can be introduced, in sufficient quantity to result in the w/o emulsion being suspended in a continuous water phase resulting in a water/oil/water (w/o/w) emulsion.
  • the fluids typically used in preparing a water-oil-water emulsion include an internal water phase wherein is dissolved or suspended any desirable material such as medicinals, acids, bases, etc.
  • the oil phase typically comprises an oil component, such as paraffin oil, mineral oil, petroleum distillate, etc. or animal or vegetable oils, depending upon the use to which the ultimate composition will be put.
  • the oil phase may contain a surfactant, i.e. an oil soluble surfactant of HLB smaller than 8, and/or a strengthening agent. This surfactant and/or strengthening agent may be the same material.
  • the final water component is the suspending phase and may comprise the aqueous phase upon which the basic water-in-oil emulsion is to act (i.e. detoxification, minerals recovery, etc.) or it may comprise a diluent phase permitting easy injection either into the body (if in medicinal use) or into a well (if in drilling use).
  • the emulsion prepared by use of the present apparatus may have internal phase to external phase ratios ranging from 1:1 to 32:1, preferably 1:1 to 3:1 for the low ratio type emulsions and 10:1 or greater, more preferably 17.1 or greater for the high ratio type emulsions. These apply to both water-in-oil and oil-in-water type emulsions.
  • the emulsions prepared by the use of the present apparatus may have droplet size from 0.1 micron to greater than 50 micron, preferably from about 0.5 micron to 5 micron for the low ratio type emulsions and 6 micron to 20 micron for the high ratio type emulsions.
  • the amount of the metal sponge used is important in determining the number of recycles needed to make a high ratio emulsion.
  • Table I shows that when 9.5 g of the metal sponge were used, 3 cycles of the feed phase (oil and water) were required to make an emlusion of 18/1 ratio (94% internal phase), whereas only 2 cycles were required when 28.5 gm of the metal sponge were used and 1 cycle was needed to emulsify more than 90% of the feed when 57 g of the metal sponge were used.
  • a cycle is defined as a once-through operation.
  • Table II shows the results of the duplicate runs.
  • the drop sizes obtained are identical or close to those in Table I, indicating the excellent reproductibility of the packed tube device.
  • flow rate ccm/min.
  • pressure drop across the tube a measure of the pressure drop across the tube.
  • viscosities at various shear rates were measured and summarized in Tables II and III.
  • the packed tube like Kenics mixer, is a type of static or motionless mixer, it is much more effective in making high ratio emulsions than Kenics because of the structure difference between the two devices. As discussed previously, the packed tube is much more densely packed in a random manner as compared to Kenics (Kenics is a registered Trade Mark in the United Kingdom).
  • the centrifugal pump was able to make the relatively low ratio emulsions in the class of the high ratio emulsions, such as 4/1 or 5/1, by first making a 2/1 ratio emulsion and then gradually increasing the ratio to 3/1, 4/1 and 5/1 with slow addition of the internal phase during the recirculation of the feed phase through the centrifugal pump.
  • the ratio of 5/1 was the highest that could be achieved.
  • the not-completely-emulsified 6/1 ratio emulsion was recycled many times through the pump, a large portion of the emulsion was broken and the remaining emulsion had a ratio of roughly 2/1.
  • the standard lab emulsification equipment used in the liquid membrane project-fluted beaker with marine propeller type stirrer was proved incapable of making high ratio emulsions.
  • “Cannon” packing is a small, half-cylindrical shape material. It is also very effective in forming high ratio emulsions, such as 17/1 w/o emulsion.
  • the packed tube is also effective in making low ratio emulsions with uniform droplet size.
  • Table VIII when a tube which was packed with 2 metal sponges and connected to a centrifugal pump was used, drop size distribution of 2 to 3 micron was observed after 2 cycles and 1-2 micron after 3 cycles. When 3 metal sponges were used, 1-2 micron drop size distribution was obtained in 1 cycle. In contrast, 4-14 micron drop size distribution was produced when a centrifugal pump was used alone. (Table VIII). Similar wide drop size distribution was obtained with the lab standard set-up of fluted beaker and marine propeller type stirrer.
  • the membrane phase was an aqueous solution of 1 % Saponin, 70% glycerol and 29% water.
  • the phase to be encapsulated was a mixture of toluene and heptane at a wt. ratio of 1/1.
  • the wt. ratio of the encapsulated phase to the membrane phase was 4/1. Both of these phases blended at 4/1 ratio were sent to the packed tube via a gear pump. Specification of the pump is given in Table I.
  • a very stable emulsion of the o/w type was made by the pump-packed tube combination.
  • Drop size range of the emulsion was from 4 to 12 micron with an average drop size of 8 micron. the above data indicate that the emulsion made had a M/IP ratio 2 1/2.
  • the existing emulsion was recycled many times, almost half of the emulsion was broken, the emulsion left had a M/IP ratio 1/2.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Dispersion Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Colloid Chemistry (AREA)

Claims (11)

1. Verfahren zur Herstellung einer Emulsion durch Emulgierung von nichtmischbaren Flüssigkeiten, bei dem
(a) die nichtmischbaren Flüssigkeiten durch mindestens eine Eintrittsöffnung in einen Behälter eingeführt werden,
(b) die Flüssigkeiten anschließend in im wesentlichen axialer Richtung durch den Behälter strömen, eine Zone oder ein Bett passieren, das mit mindestens einem Material gefüllt ist, um ein schnelles und wiederholtes Mischen und Wiedervermischen der nichtmischbaren Flüssigkeiten in dem Behälter und somit die Bildung der gewünschten Emulsion zu bewirken, und
(c) die so gebildete Emulsion aus dem Behälter durch eine oder mehrere Austrittsöffnungen entfernt wird, dadurch gekennzeichnet, daß das Material aus Stahlschwamm, Metallspänen, keramischen Splittern, "Cannon"-Material, Tierhaar oder Kunststoffborsten, Metallröhrchen, die kürzer sind als der Innendurchmesser des Behälters, oder Berl-Sätteln besteht.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die nichtmischbaren Flüssigkeiten durch die Eintrittsöffnungen(en) mittels Flüssigkeitseinspeisvorrichtungen, vorzugsweise Pumpen, Fallleitungen Spritzen oder Kombinationen derselben, eingeführt werden, die in Verbindung mit Flüssigkeitslagervorrichtungen stehen.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß die gesamte aus der (den) Austrittsöffnung(en) austretende Emulsion oder ein Teil davon nochmals durch den Behälter geleitet wird.
4. Verfahren nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, daß die gebildete Emulsion vom Wasser-in-ÖI-Typ oder vom ÖI-in-Wasser-Typ ist.
5. Verfahren nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, daß die hergestellte Emulsion ein Verhältnis von interner Phase zu externer Phase von 1:1 bis 32:1 besitzt.
6. Verfahren nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, daß die hergestellete Emulsiion eine Tröpfchengröße von 0,1 µ bis mindestens 50 µ besitzt.
7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß die hergestellte Emulsion ein Verhältnis von interner zu externer Phase von 1:1 bis 3:1, eine Tröpfchengröße von vorzugsweise 0,511 bis 5 µ oder ein Verhältnis von interner zu externer Phase von mindestens 10:1 und eine Tröpfchengröße von vorzugsweise 6 µ bis 20 µ besitzt.
8. Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß die hergestellte Emulsion ein Verhältnis von interner zu externer Phase von mindestens 17:1 besitzt.
9. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß die aus der (den) Austrittsöffnung(en) austretende Emulsion in die Eintrittsöffnung(en) eines zweiten gefüllten Behälters eingespeist wird, in den eine dritte nicht mischbare Flüssigkeit eingespeist wird, so daß eine Mehrphasenemulsion erzeugt und dann an der (den) Austrittsöffnung(en) des zweiten gefüllten Behälters gesammelt wird.
10. Verfahren nach Anspruch 9, dadurch gekennzeichnet, daß die gebildete Mehrphasenemulsion vom Öl-in-Wasser-in-Öl-Typ oder vom Wasser-in-Öl-in-Wasser-Typ ist.
11. Verfahren nach einem der vorangehenden Ansprüche, dadurch gekennzeichnet, daß die Emulsion unter verwendung einer Vorrichtung hergestellt wird, die einen emulsionsbildenden Behälter (3) aufweist, der (a) mindestens eine Eintrittsöffnung (1) für die Einführung der nicht mischbaren Flüssigkeiten, (b) eine Zone oder ein Bett (4) in Verbindung mit der (den) Eintrittsöffnung(en) und (c) mindestens eine Austrittsöffnung (2) in Verbindung mit der Zone oder dem Bett (4) zur Entfernung der gebildeten Emulsion besitzt, wobei der Behälter (3) bei Blockrichtung rechtwinklich zum Strömungsweg vorzugsweise ein Querschnittsprofil von regulärer oder irregulärer Gestalt mit mindestens drei Seiten besitzt und wobei die Zone oder das Bett (4) mit mindestens einem Material gemäß Anspruch 1 gefüllt ist.
EP79301398A 1979-07-13 1979-07-13 Verfahren und Vorrichtung zum Herstellen von Emulsionen Expired EP0022442B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE7979301398T DE2967203D1 (en) 1979-07-13 1979-07-13 Method and apparatus for preparing emulsions
EP79301398A EP0022442B1 (de) 1979-07-13 1979-07-13 Verfahren und Vorrichtung zum Herstellen von Emulsionen

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP79301398A EP0022442B1 (de) 1979-07-13 1979-07-13 Verfahren und Vorrichtung zum Herstellen von Emulsionen

Publications (2)

Publication Number Publication Date
EP0022442A1 EP0022442A1 (de) 1981-01-21
EP0022442B1 true EP0022442B1 (de) 1984-09-05

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EP79301398A Expired EP0022442B1 (de) 1979-07-13 1979-07-13 Verfahren und Vorrichtung zum Herstellen von Emulsionen

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DE (1) DE2967203D1 (de)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2002882A1 (de) * 2007-06-15 2008-12-17 Wageningen University Herstellungsverfahren für eine Emulsion
GB201615066D0 (en) 2016-09-06 2016-10-19 Ge Healthcare Bioprocess R&D Ab Packed bed emulsification
DE102019104646A1 (de) 2018-02-26 2019-08-29 Adelheid Holzmann Verfahren zum Betreiben einer Verbrennungskraftmaschine, eine Anordnung zur Durchführung des Verfahrens zum Betreiben einer Verbrennungskraftmaschine und eine Vorrichtung zur Erzeugung einer Emulsion

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB684926A (en) * 1949-12-01 1952-12-24 Separator Ab A method and device for homogenization
US3416320A (en) * 1967-07-14 1968-12-17 Exxon Research Engineering Co Turbo-jet propulsion method using emulsified fuels and demulsification
US3704006A (en) * 1971-01-25 1972-11-28 Kenics Corp Dispersion producing method
FR2225199A1 (en) * 1973-04-12 1974-11-08 Lombard Jacques Static mixer for fluids - has steel balls (partly) filling chamber
US3865352A (en) * 1973-11-16 1975-02-11 Minnesota Mining & Mfg Static mixing device
DE2532355C3 (de) * 1975-07-19 1979-06-07 Bayer Ag, 5090 Leverkusen Vorrichtung zum statischen Mischen von fließfähigen Stoffen
US4018426A (en) * 1976-03-17 1977-04-19 Petrolite Corporation System for producing emulsions

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DE2967203D1 (en) 1984-10-11
EP0022442A1 (de) 1981-01-21

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