EP0732144A1 - Système de fabrication d'une émulsion et dispositif de mélange - Google Patents

Système de fabrication d'une émulsion et dispositif de mélange Download PDF

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Publication number
EP0732144A1
EP0732144A1 EP95104001A EP95104001A EP0732144A1 EP 0732144 A1 EP0732144 A1 EP 0732144A1 EP 95104001 A EP95104001 A EP 95104001A EP 95104001 A EP95104001 A EP 95104001A EP 0732144 A1 EP0732144 A1 EP 0732144A1
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EP
European Patent Office
Prior art keywords
emulsion
droplet size
newtonian liquid
cylinder
water
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.)
Granted
Application number
EP95104001A
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German (de)
English (en)
Other versions
EP0732144B1 (fr
Inventor
Gustavo Nunez
Roger Qta. La Bretana Marzin
Maria Luisa Ventresca
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.)
Intevep SA
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Intevep SA
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Publication date
Application filed by Intevep SA filed Critical Intevep SA
Priority to DE69502929T priority Critical patent/DE69502929T2/de
Priority to ES95104001T priority patent/ES2118464T3/es
Priority to DK95104001T priority patent/DK0732144T3/da
Priority to EP95104001A priority patent/EP0732144B1/fr
Publication of EP0732144A1 publication Critical patent/EP0732144A1/fr
Application granted granted Critical
Publication of EP0732144B1 publication Critical patent/EP0732144B1/fr
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Expired - Lifetime legal-status Critical Current

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    • 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
    • B01F23/4141—High internal phase ratio [HIPR] emulsions, e.g. having high percentage of internal phase, e.g. higher than 60-90 % of water in oil [W/O]
    • 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
    • B01F23/4143—Microemulsions
    • 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
    • B01F23/43—Mixing liquids with liquids; Emulsifying using driven stirrers
    • 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
    • B01F2215/0409—Relationships between different variables defining features or parameters of the apparatus or process

Definitions

  • the invention relates to the field of emulsions and, more particularly, to a method and apparatus for continuous preparation of high internal phase ratio emulsions characterized by small droplet size and narrow droplet size distribution.
  • the present invention relates to a method and apparatus for forming emulsions of the crude oil in water to obtain an emulsion which flows easily for conventional transportation. Obviously, such transportation is more efficient when the emulsion formed has a high ratio of internal phase crude oil or hydrocarbon as compared to the external phase of water.
  • emulsions are known as High Internal Phase Ratio (HIPR) emulsions and are the further subject of the present invention.
  • HIPR High Internal Phase Ratio
  • U.S. Patent No. 4,018,426 to Mertz et al. discloses a system for continuous production of high internal phase ratio emulsions.
  • U.S. Patent No. 4,018,426 teaches that the HIPR final emulsion is formed from a homogeneously mixed preliminary dispersion in a conventional pump which provides shear forces sufficient to create an emulsion.
  • Conventional pumps create flow patterns which vary with the properties of the fluids being emulsified as the fluid emulsifies and becomes non-Newtonian, and can result in non-uniform application of shear forces to the fluids resulting in non-uniform droplet size of the internal phase in the emulsion.
  • Such a non-uniform droplet size has been found to adversely effect the flow characteristics of the emulsion, particularly over time.
  • the liquid is preferably subjected to said shear forces in a cylinder selected to provide a residence time of between about 1 to 5 minutes and having an inlet for said Newtonian liquid, an outlet for said HIPR emulsion, and a plurality of means for providing shear force to said mixture, said plurality of shear means each having a diameter (d) and said cylinder having a length (L) and diameter (D).
  • a first shear means of said plurality of shear means is positioned at a distance from said inlet of about 1/3L; a second shear means of said plurality of shear means is positioned at a distance from said first shear means of about 1.5d; a ratio of cylinder length to cylinder diameter (L/D) is selected between about 1.5 to 3.0; a ratio of shear means diameter to cylinder diameter (d/D) is selected between about 0.35 to 0.45.
  • the invention relates to a method and apparatus for continuous preparation of high internal phase ratio (HIPR) emulsions characterized by small droplet size and narrow droplet size distribution.
  • HIPR high internal phase ratio
  • Fig. 1 illustrates a typical system for preparing HIPR emulsions according to the prior art, which includes a mixing device 10, a static mixer 12, a conduit 14 for an internal viscous hydrocarbon phase and a conduit 16 for an external water phase and emulsifying additive.
  • the conduits 14, 16 join and introduce the internal and external phase to static mixer 12, where the phases are mixed to form a mixture or dispersion which flows to mixing device 10 where the emulsion is formed and is passed on to subsequent processing or storage through outlet 18.
  • Prior art mixing devise 10 is typically a conventional pump which provides a shear force to the dispersion sufficient to form an emulsion of the internal phase in the external phase.
  • Conventional mixing devices 10 typically have a single rotating mixing member or blade, and are sized to provide a residence time for incoming fluids of about 10 seconds. As described above, such devices require high energy and large amounts of emulsifying additive to form HIPR emulsions with small droplet diameters, and frequently cause an inversion of the phases when too much shear is applied. Large amounts of shear are required in conventional mixing devices, however, to obtain HIPR emulsions with droplet diameters less than 7.0 microns. Thus, phase inversions frequently result before the desired droplet size is obtained by such conventional mixing devices.
  • Fig. 2 illustrates a mixing device 20 according to the invention.
  • Mixing device 20 may preferably be disposed in a system such as that of Fig. 1, replacing conventional mixing device 10.
  • Mixing device 20, according to the invention comprises a cylinder 22 having an inlet 24 and an outlet 26 and a plurality of means 28 for providing shear force which shear means 28 are serially positioned in cylinder 22 along a flow path of the mixture.
  • Cylinder 22 is preferably oriented substantially vertically, with inlet 24 being located in a bottom surface 30 thereof, and with outlet 26 being located in a top surface 32.
  • Shear means 28 preferably comprise a plurality of blades 34, 36 serially disposed rotatably, for example on a shaft 38, along a longitudinal axis of cylinder 22.
  • Shear means 28 may alternatively be any structure known in the art to apply shear to flowing fluids, such as vanes, turbines, spiral flow passages, and the like.
  • Inlet 24 is preferably aligned substantially concentric with the longitudinal axis or shaft 38 of cylinder 22. This alignment helps to direct the mixture to blade 34 in the most effective manner.
  • Rotation can be imparted to blades 34, 36 through any type of motive means 40 known in the art (schematically depicted in Fig. 2).
  • Motive means 40 preferably imparts rotation to blades 34, 36 so as to subject the mixture being emulsified to shear forces corresponding to a power input of between about 0.1 x 10 6 to 1.0 x 10 7 Watt ⁇ s/m 3 , so as to form an emulsion having the desired droplet size and droplet size distribution characteristics.
  • the power input varies within the foregoing range as a function of the capacity of the mixing device, that is, the greater the capacity of the mixing device, the greater the power input required to obtain the desired droplet size and distribution.
  • Cylinder 22 has a geometry which cooperates with size and positioning of shear means 28, according to the invention, to provide thorough mixing of the mixture within cylinder 22, despite changes in thixotropic or rheological properties of the phases to be emulsified.
  • the process begins with a mixture of water, hydrocarbon and emulsifier that is substantially a Newtonian liquid.
  • Newtonian Liquid is meant a liquid which flows substantially immediately on application of force and for which the rate of flow is directly proportional to the force applied.
  • the mixture takes on the characteristics of a viscoelastic or non-Newtonian fluid, that is, its viscosity is dependent upon the rate of shear.
  • the cylinder geometry and shear means arrangement allows the preparation of HIPR emulsions having substantially uniform internal phase droplet sizes in a range of about 1 to 30 microns, and preferably less than about 7.0 microns. Still referring to Fig. 2, the cylinder geometry and shear means arrangements of the present invention will be illustrated.
  • shear means 28 are positioned serially along the flow path of the Newtonian liquid mixture. This serial positioning is illustrated in Fig. 2 as the serial positioning of blades 34, 36.
  • first blade 34 radially displaces a substantial portion of incoming Newtonian liquid mixture against the walls of cylinder 22. Preferably, about 80% of the total flow is thus displaced. This portion strikes the walls of cylinder 22 resulting in a minimum pressure at the cylinder wall and a maximum pressure at the tip of blade 34. This results in a further circulation of the liquid being mixed.
  • the remaining non-radially displaced Newtonian liquid which is not radially displaced by blade 34, flows or climbs up shaft 38, particularly in light of the rigid flow of the mixed non-Newtonian portion.
  • This flow of the remaining portion of Newtonian liquid, up rod or shaft 38, is referred to as "rod climbing" flow.
  • blade 36 subjects the remaining non-radially displaced portion of Newtonian liquid to an additional shear force to mix the remaining portion into the non-Newtonian liquid. Rod climbing flow is thus eliminated and an emulsion having desired characteristics is formed without excessive emulsifier or increased risk of phase inversion. Blade 36 also further mixes the rigidly rotating non-Newtonian substantial portion so as to eliminate rigid flow and further increase mixing effectiveness.
  • the preferred cylinder geometry is expressed in terms of suitable ratios of shear means 28 or blade 34, 36 diameter (d), cylinder length (L) and cylinder diameter (D).
  • Cylinder 22 preferably has a length and diameter selected to provide a ratio of length to diameter (L/D) of between about 1.5 to 3.0.
  • Blades 34, 36 are preferably positioned within cylinder 22 at predetermined distances from inlet 24.
  • First blade 34 is disposed at a distance from inlet 24 of about one third of the length of cylinder 22 (L/3).
  • Second blade 36 is disposed at a distance form first blade 34 of about 1.5 times the blade diameter (1.5d).
  • a ratio of blade diameter to cylinder diameter (d/D) is preferably between about 0.35 to 0.45, and is preferably about 0.4.
  • cylinder 22 induces a flow pattern in cylinder 22 which is not adversely affected by changes in the rheological or thixotropic properties of the fluid phases being emulsified. Stagnation of flow in cylinder 22 is avoided, as are rod climbing flow and rigid rotation, thus preventing application of non-uniform shear forces to the mixture and preventing the formation of bimodal emulsions, or emulsions having non-uniform droplet sizes.
  • the cylinder volume is preferably selected, in conjunction with the expected flow rate of mixture, to provide a residence time for the fluids in the cylinder of between about 1 to 5 minutes.
  • This increased residence time allows the emulsifying additive to adequately disperse the internal phase and stabilize internal phase droplet size without the previously required large amounts of shear force.
  • the internal viscous hydrocarbon phase and external water phase may preferably be supplied to mixing device 28 through any flow conducting means known in the art such as, for example, conduits 14, 16 as shown in Fig. 1.
  • the emulsifying additive may preferably be an anionic, cationic or non-ionic surfactant, and more preferably is a nonylphenol ethoxylated surfactant.
  • An example of a suitable emulsifying additive is a composition of 97% by weight of an alkyl phenol ethoxylate based surfactant compound (such as INTAN-100TM by INTEVEP, S.A.) and 3% by weight of a phenol formaldehyde ethoxylate resin having about 5 units of ethylene oxide.
  • the emulsifying additive is preferably added to external water phase at a concentration, to viscous hydrocarbon content, of no greater than about 3000ppm.
  • the system operates as follows.
  • the internal viscous hydrocarbon phase and the external water phase and emulsifying additive are supplied by respective conduits, such as conduits 14, 16 of Fig. 1, where a mixture of the phases is formed, preferably in mixing means 12.
  • the mixture then passes to inlet 24 of mixing device 20.
  • the flow of mixture enters cylinder 22 where a substantial portion, preferably at least approximately 80% of the flow, is radially displaced by first blade 34 against the walls of cylinder 22.
  • a static head is provided by the cylinder geometry which promotes recirculation of the fluid and prevents the formation of regions of uneven stress or shear forces, thereby helping to provide a narrow droplet size distribution.
  • the mixing induced by first blade 34 serves to create a non-Newtonian liquid having viscoelastic properties. This results in the liquid rotating around shaft 38 in rigid motion, and causes the remaining portion of Newtonian liquid to flow up shaft 38 in a rod climbing type flow of the liquid.
  • Second blade 36 serves to eliminate such rod climbing flow by mixing the remaining portion into the mixed non-Newtonian portion and eliminates the rigid flow or rotation of the substantial portion, thus providing improved mixing and an emulsion having the desired characteristics, particularly when a droplet size of 7.0 microns or less is desired.
  • Second blade 36 thus helps to reduce non-uniformity of droplet size and to provide a narrow droplet size distribution (x), defined as (D90 - D10)/D50 , which is no greater than about 1, wherein:
  • the y-axis represents the entire droplet family, ordered by increasing droplet diameter.
  • D10 corresponds to the droplet diameter of the droplet at the tenth percentile along the y-axis.
  • D50 and D90 correspond in the same fashion to the 50th and 90th percentile, respectively.
  • the x-axis represents the droplet size in microns.
  • Fig. 3 is merely illustrative of the general meaning of the droplet size distribution factor, actual droplet size values are not included on the x-axis.
  • the droplet size distribution factor as described above is reflective of the uniformity of droplet size contained in the emulsion.
  • a small distribution factor indicates a narrow droplet size distribution and a substantially uniform droplet size.
  • Table I BITUMEN CNR Gravity API (60) 8.4 Saturated % (TLC/FID) 11.8 Aromatic % (TLC/FID) 45.8 Resins %(TLC/FID) 30.9 Asphaltenes % (TLC/FID) 11.5 Acidity, mgKOH/g (ASTM D-664) 3.07 Basic nitrogen mg/Kg (SHELL-1468) 1,546.1 Total nitrogen mg/Kg (ASTM D-3228) 5,561 Sulphur % 3.91 Nickel (mg/l) 105.9 Vanadium (mg/l) 544.2
  • the surfactant used was a composition consisting of 97% (weight) of an alkyl of a phenol ethoxylate-based surfactant compound identified as INTAN-100TM supplied by INTEVEP, S.A., and 3% (weight) of a phenol formaldehyde ethoxylate resin having about 5 units of ethylene oxide.
  • the objective in each example was to obtain an average droplet size of 4 microns or less with a ratio of internal phase to external phase of at least 85:15 and a droplet size distribution factor of 1 or less.
  • Viscous hydrocarbon as described above was mixed with water and emulsifying additive in a preliminary static mixer.
  • the mixture provided by the static mixer was then fed to a conventional dynamic mixer (trademark: TKK, model: PHM, manufacturer: Tokushu Kika Kogyo LTD., Osaka, Japan) at a flow rate providing a residence time of 10 seconds.
  • a conventional dynamic mixer trademark: TKK, model: PHM, manufacturer: Tokushu Kika Kogyo LTD., Osaka, Japan
  • a premixing tank was substituted for the static mixer of Example 1 to provide a substantially homogeneous preliminary dispersion to the conventional dynamic mixer, as in aforedescribed U.S. Patent No. 4,018,426.
  • the phases were mixed in the premixing tank for about 30 minutes before passing through the conventional mixer with a residence time of 10 seconds.
  • a droplet size of less than 4 microns was achieved only when emulsifying additive was added in a concentration, to viscous hydrocarbon content, of 6000 ppm and significant amounts of energy were supplied.
  • Table II The results of these tests are summarized below in Table II.
  • Emulsions were formed in a system as in Example 1, but substituting an apparatus according to the invention for the conventional dynamic mixer.
  • the mixer utilized in accord with the present invention had the following dimensions:
  • Emulsions prepared in accordance with the present invention are an excellent alternative for the transportation of viscous hydrocarbons.
  • the emulsion can be broken through known techniques once the emulsion has reached its destination.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Liquid Carbonaceous Fuels (AREA)
  • Colloid Chemistry (AREA)
EP95104001A 1995-03-17 1995-03-17 Système de fabrication d'une émulsion et dispositif de mélange Expired - Lifetime EP0732144B1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
DE69502929T DE69502929T2 (de) 1995-03-17 1995-03-17 Ein Emulsionsherstellungssystem und Mischapparat
ES95104001T ES2118464T3 (es) 1995-03-17 1995-03-17 Un sistema de formacion de una emulsion y dispositivo de mezcla.
DK95104001T DK0732144T3 (da) 1995-03-17 1995-03-17 Emulgeringssystem og blandeanordning
EP95104001A EP0732144B1 (fr) 1995-03-17 1995-03-17 Système de fabrication d'une émulsion et dispositif de mélange

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP95104001A EP0732144B1 (fr) 1995-03-17 1995-03-17 Système de fabrication d'une émulsion et dispositif de mélange

Publications (2)

Publication Number Publication Date
EP0732144A1 true EP0732144A1 (fr) 1996-09-18
EP0732144B1 EP0732144B1 (fr) 1998-06-10

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EP95104001A Expired - Lifetime EP0732144B1 (fr) 1995-03-17 1995-03-17 Système de fabrication d'une émulsion et dispositif de mélange

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DE (1) DE69502929T2 (fr)
DK (1) DK0732144T3 (fr)
ES (1) ES2118464T3 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0808889A2 (fr) * 1996-05-23 1997-11-26 Kao Corporation Méthode de production d'un combustible comprenant une émulsion d'une huile super lourde et combustible ainsi obtenue
WO2003075879A2 (fr) * 2002-03-06 2003-09-18 Dow Global Technologies Inc. Procede de preparation d'une formulation cosmetique et composition associee
CN106362634A (zh) * 2016-11-01 2017-02-01 重庆瑞恩涂料有限公司 一种基于多搅拌协同生产的涂料生产设备

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1099283A (en) * 1964-08-04 1968-01-17 Bayer Ag Process for the preparation of reverse emulsions
GB2117666A (en) * 1982-03-09 1983-10-19 Univ Manchester Emulsification
WO1985003646A1 (fr) * 1984-02-18 1985-08-29 The British Petroleum Company P.L.C. Preparation d'emulsions
EP0184433A2 (fr) * 1984-12-07 1986-06-11 The British Petroleum Company p.l.c. Préparation d'émulsions
EP0214843A2 (fr) * 1985-09-04 1987-03-18 The British Petroleum Company p.l.c. Préparation d'émulsions
WO1994026401A1 (fr) * 1993-05-18 1994-11-24 Explosive Developments Limited Dispositifs de melange

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1099283A (en) * 1964-08-04 1968-01-17 Bayer Ag Process for the preparation of reverse emulsions
GB2117666A (en) * 1982-03-09 1983-10-19 Univ Manchester Emulsification
WO1985003646A1 (fr) * 1984-02-18 1985-08-29 The British Petroleum Company P.L.C. Preparation d'emulsions
EP0184433A2 (fr) * 1984-12-07 1986-06-11 The British Petroleum Company p.l.c. Préparation d'émulsions
EP0214843A2 (fr) * 1985-09-04 1987-03-18 The British Petroleum Company p.l.c. Préparation d'émulsions
WO1994026401A1 (fr) * 1993-05-18 1994-11-24 Explosive Developments Limited Dispositifs de melange

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0808889A2 (fr) * 1996-05-23 1997-11-26 Kao Corporation Méthode de production d'un combustible comprenant une émulsion d'une huile super lourde et combustible ainsi obtenue
EP0808889A3 (fr) * 1996-05-23 1998-03-18 Kao Corporation Méthode de production d'un combustible comprenant une émulsion d'une huile super lourde et combustible ainsi obtenue
US5851245A (en) * 1996-05-23 1998-12-22 Kao Corporation Method for producing superheavy oil emulsion fuel and fuel produced thereby
WO2003075879A2 (fr) * 2002-03-06 2003-09-18 Dow Global Technologies Inc. Procede de preparation d'une formulation cosmetique et composition associee
WO2003075879A3 (fr) * 2002-03-06 2004-03-25 Dow Global Technologies Inc Procede de preparation d'une formulation cosmetique et composition associee
US6783766B2 (en) 2002-03-06 2004-08-31 Dow Global Technologies Inc. Process for preparing a cosmetic formulation
US7056496B2 (en) 2002-03-06 2006-06-06 Dow Global Technologies Inc. Sunscreen composition and a process for preparing it
CN106362634A (zh) * 2016-11-01 2017-02-01 重庆瑞恩涂料有限公司 一种基于多搅拌协同生产的涂料生产设备

Also Published As

Publication number Publication date
ES2118464T3 (es) 1998-09-16
DK0732144T3 (da) 1999-03-22
DE69502929D1 (de) 1998-07-16
EP0732144B1 (fr) 1998-06-10
DE69502929T2 (de) 1999-03-04

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