WO2013082681A1 - Équipement pour la déstabilisation électrostatique d'émulsions de fluides sous pression dans un système hermétique et procédé de test - Google Patents

Équipement pour la déstabilisation électrostatique d'émulsions de fluides sous pression dans un système hermétique et procédé de test Download PDF

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Publication number
WO2013082681A1
WO2013082681A1 PCT/BR2011/000445 BR2011000445W WO2013082681A1 WO 2013082681 A1 WO2013082681 A1 WO 2013082681A1 BR 2011000445 W BR2011000445 W BR 2011000445W WO 2013082681 A1 WO2013082681 A1 WO 2013082681A1
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WO
WIPO (PCT)
Prior art keywords
fluid
conductive
vessel
emulsion
equipment
Prior art date
Application number
PCT/BR2011/000445
Other languages
English (en)
Portuguese (pt)
Inventor
Marcio NELE DE SOUZA
Marcio De Figueiredo Portilho
Raquel CAMPOS CAUBY COUTINHO
Flavio CORTINAS ALBUQUERQUE
Maurício Souza de Alencar
Original Assignee
Petróleo Brasileiro S.A. - Petrobras
Universidade Federal Do Rio De Janeiro - Ufrj
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.)
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Application filed by Petróleo Brasileiro S.A. - Petrobras, Universidade Federal Do Rio De Janeiro - Ufrj filed Critical Petróleo Brasileiro S.A. - Petrobras
Priority to PCT/BR2011/000445 priority Critical patent/WO2013082681A1/fr
Priority to BR112014007064-4A priority patent/BR112014007064B1/pt
Publication of WO2013082681A1 publication Critical patent/WO2013082681A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/06—Separation of liquids from each other by electricity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C5/00—Separating dispersed particles from liquids by electrostatic effect
    • B03C5/02—Separators
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; Viscous liquids; Paints; Inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids
    • G01N33/2835—Specific substances contained in the oils or fuels
    • G01N33/2847—Water in oils

Definitions

  • the present invention belongs to the field of equipment for assessing emulsion stability, more specifically, to an equipment that evaluates emulsion stability to the electrocoalescence process in a batch system.
  • water-in-oil (W / O) emulsions and dispersions are usually formed either by the reservoir conditions themselves or by injecting water into the secondary well recovery process.
  • Oil-emulsified water is actually a contaminant, because in addition to causing operational problems during refining, it is an extra burden that overloads pumping systems, pipelines and tanks, as well as increasing the energy cost of transporting and storing production.
  • the emulsification of water in petroleum occurs due to the immiscibility between these two liquid phases, the shear imposed on the fluids during production flow and the existence of natural surfactants in petroleum. These amphiphilic surfactants are adsorbed on the surface of the generated water droplets and create a physical barrier (interfacial film) that prevents coalescence between the water droplets.
  • the water in oil (W / O) type emulsion is preferably formed depending on the dominant lipophilic character of such natural surfactants.
  • every resting emulsion separates over time.
  • this time may be very practical or even long. phase resolution it can become impossible.
  • the electrocoalescence process is already employed in production units to reduce the water content in petroleum.
  • the efficiency of the demulsification process is related to the emulsion stability, and can be improved if the applied electric field undergoes controlled variations of intensity (voltage) and frequency.
  • these electrostatic destabilization equipment consists of a demulsifying cell and a high voltage source.
  • the cell is composed of two electrodes that form a capacitor, allowing an intense electric field to be applied to emulsions.
  • the electrodes may be arranged to form a cylindrical or parallel plate capacitor, depending on the characteristics of the emulsions.
  • a non-conductive liquid contains in the emulsified form water (a conductive liquid) in its environment and these are subjected to an electric field, water droplets tend to interact by the following phenomena:
  • U.S. Patent 6,136,174 describes an equipment for emulsion electrocoalescence which, unlike known equipment that handles static emulsions in large tanks, makes use of a compact device that passes an alternating current over emulsions maintained in turbulent flow.
  • this US document deals with a compact equipment for the coalescence of finely dispersed droplets of an emulsified conductive fluid into a nonconductive fluid stream by the use of a high intensity electric field acting on the emulsion as it flows. through a narrow gap under non-laminar flow conditions.
  • the emulsion is introduced into the top of a vertical cylindrical shell, and flows through one or more narrow annular gaps formed between one or more electrodes, or an inner wall of the device.
  • the broken emulsion is discharged from the bottom of the vessel after a short residence time in the high intensity electrostatic field.
  • Emulsion flow at or all narrow annular gaps is non-laminar to provide substantially smaller equipment size, even for emulsions with high water content.
  • the Brazilian Application PI 0605199-5 describes an equipment for assessing the stability of liquid emulsions, the equipment consisting of a set of vessels, valves and temperature, pressure and agitation control means, the emulsions. being treated in an airtight system.
  • the emulsion separation occurs by the gravitational sedimentation process, while in the equipment proposed in the present application the emulsion separation occurs by the electrocoalescence process which is much more efficient and consequently more industrially used.
  • the main shortcoming of the equipment object of the Brazilian application is that by inferring the stability of an emulsion, it is based on the gravitational sedimentation process, which does not always reproduce the conditions of equipment used in industrial separation, where the separation is by electrocoalescence. Thus, a given emulsion can be judged as easy to separate (unstable) by the gravitational process and in industrial equipment using electrocoalescence it may be difficult to separate.
  • the present equipment is suitable for the electrocoalescence process of water / oil emulsions at high temperature and bench scale pressure.
  • US 7,166,218 deals with a device for separating an effluent comprising phases of different density and conductivity, the device comprising a pair of electrodes (12, 13), device (10) for separation (3) and discharge (4). ) of the separate phases.
  • the separating device comprises at least one centrifugation element including a helical channel (19) in which the effluent is centrifuged after passing between the electrodes. An opening extends along the entire periphery of the centrifuged effluent to discharge part of the centrifuged effluent.
  • a stirrer (51) centrally positioned in the vessel (1), the upper end (56) thereof being connected to a motor (57) while its lower end includes a propeller ( 53) stirring immersed in the liquid being mixed;
  • a supply vessel (32) provided with a screw cap (33) including a connection (34) to generate pressure in the vessel (1) by gas inlet through valve (31) and a transfer line (36);
  • Use of the present apparatus includes the preparation of immiscible fluid mixtures, a conductive fluid and a nonconductive fluid under controlled pressure, temperature and agitation conditions, an electric field being established within the vessel by electrodes associated with a voltage variation controller system, the current being monitored during the electrocoalescence process.
  • test method for assessing the stability of a fluid emulsion obtained under predefined pressure, temperature, stirring speed, time and stress intensity conditions applied to the emulsion utilizes the apparatus according to the invention.
  • the equipment of the invention for electrostatic destabilization of hermetic pressure fluid emulsions provides the evaluation of the emulsion stability under high electric field. temperature and pressure, under conditions similar to those used in industrial processes.
  • the equipment of the invention further provides as electrostatic destabilization test products the process efficiency and the electric current curve between the electrodes, so that the higher the value of the electric current observed, the higher the water content within the emulsion and the higher the transfer of energy from the electrodes to the water droplets or other conductive fluid.
  • the equipment of the invention also provides an estimate of the total energy expended during the dehydration process by numerically integrating the product of the current and voltage measurements obtained during the test as a function of time.
  • the total energy value is then used as a metric to evaluate the emulsion stability against the electrocoalescence process where emulsions whose energies for separation are higher are obviously more stable against electrocoalescence.
  • the invention further provides, with the aid of the described apparatus, a test method for assessing the stability of a fluid emulsion obtained under predefined pressure, temperature, stirring speed, time and stress intensity conditions applied to the emulsion.
  • FIGURE 1 shows a cross-sectional view of the separation vessel with the supply and outlet system for the equipment of the invention.
  • the attached FIGURE 3 shows a cross-sectional view of the separation vessel lid with the supply and outlet systems for the equipment of the invention.
  • the attached FIGURE 4 shows a surface view of the separation vessel lid for the equipment of the invention.
  • FIGURE 5 shows a cross-sectional view of the separation vessel in the holder and the mechanical stirrer for the equipment of the invention.
  • FIGURE 6 shows a cross-sectional view of the separation vessel with the internal display in detail for the equipment of the invention.
  • FIGURE 8 shows a sectional side view of the stirrer rod for the equipment of the invention.
  • FIGURE 9 is a graph illustrating a current versus time curve for Example 1 of the invention.
  • the present invention provides an equipment for assessing the stability of water-oil emulsions useful for guiding primary processing operations in the petroleum industry, especially in electrostatic dehydration and petroleum desalting processes.
  • the equipment is generally useful for assessing the emulsion stability of an emulsified L1 conductive fluid in an L2 nonconductive fluid.
  • the present equipment is by no means limited to the emulsion fluids preferably described herein, where the conductive fluid is water and the nonconductive fluid is petroleum or a fraction thereof.
  • L1 conductive fluid emulsions in L2 nonconductive fluids are prepared in varying proportions, ranging from 1% w / w L1 fluid to 99% w / w L2 fluid to 50% w / w fluid conductor L1 for 50% w / w non-conductive fluid L2, preferably up to 20% w / w conductor L1 for up to 80% w / w non-conductive fluid L2.
  • an electric field is established within the fluid separation vessel by means of electrodes associated with a voltage variation controller system, the current being monitored during the electrocoalescence process.
  • the test method using the present equipment includes the transfer of fluids into a mixing vessel in an airtight system, the liquid content being subjected to agitation, temperature and pressure, when an electric field is then applied to the mixture of fluids for a certain time.
  • the apparatus 100 comprises a fully airtight system with the following parts and features:
  • the apparatus 100 of the invention comprises a generally cylindrical separating vessel (1) for mixing droplets of an emulsified conductive fluid into a tapered base non-conductive fluid stream to facilitate the flow of liquids contained within it.
  • Visors (5) and (5a) made of transparent material and inserted into the lateral wall of the vessel (1) in diametrically opposite positions and longitudinally allow the view of the interior of the separation vessel (1).
  • the upper end of the separation vessel (1) is sealed by a lid (20) (see Figures 3 and 5) of circular shape and flat surfaces.
  • the base of said vessel (1) is sealed by a lower lid (9) (see Figure 1) with tapered inner surface to facilitate flow of liquids contained within the vessel (1) and flat outer surface.
  • the caps (20) and (9) are fitted to the inner edges of the separation vessel (1) and threaded to the outer edge thereof.
  • the top cover (20) is perforated at six points, see Figure 4, with one central point (A) and five other points (B), (C), (D), (E), and (F) aligned radial to point (A) and coupled to cap (20) to maintain the airtight system.
  • the central point (A) is traversed by a Teflon coated tube (52) that axially surrounds the stirrer rod (51).
  • the upper end of the agitator (51) is connected via (56) to an electromechanical agitator (57) to print rotation to the agitator (51) and propeller (53), see Figure 5.
  • point (C) allows positive electrode (21) to enter the separation vessel body (1), attached to the separation vessel lid (20) by means of threaded connections (35a) of keep the interior tightly closed.
  • Point (D) allows the negative electrode (22) to enter the separation vessel body (1) and is attached to the separation vessel lid (20) by means of threaded connections (35b). mode keeping the inside of the vessel (1) tightly closed.
  • Point (E) allows pressure relief from the separation vessel (1) to the atmosphere by means of an outlet valve (41) in a row (36a) with threaded connection (35c).
  • a pressure gauge (43) for measuring line pressure (36a) and a safety valve (42) are coupled to line (36a) by means of a "T".
  • Point (F) (see Figure 2) allows a temperature gauge (23) to pass through the separation vessel (1), connected by threaded connections (35d) to keep the interior tightly sealed.
  • the lower cap (9) is perforated at the center (G) for the passage of an exhaust valve (8) with threaded connection (35e) to allow the flow of the liquids contained in the separation vessel (1), maintaining the hermetic system;
  • a feed vessel (32) transfers the fluids to be mixed (emulsified) into the separation vessel (1) by means of a feed valve (31).
  • the lid (33) of the supply vessel (32) is provided with a gas inlet fitting (34) and thereby generates pressure on the liquid content within the separation vessel (1).
  • a support (58) is designed to clamp (58a) the electromechanical stirrer (57) and allow the positioning of the rod (51) by means of an endless screw (59), keeping firm and all parts of the equipment are aligned (100).
  • An auxiliary thermostatic bath (not shown) circulates a thermal fluid in the coil (2) which internally surrounds the separation vessel wall (1) and heats the fluid content.
  • Test operating parameters using the equipment of the invention include pressure, temperature, stirring speed, time and stress intensity data applied to the emulsion.
  • the emulsion stability prepared between L1 fluid (conductive) and L2 fluid (non-conductive) is a relative assessment of the time the two liquids remain emulsified and subsequent phase separation followed by measurement of residual water content after testing. under the conditions used.
  • L1 being a conductive fluid and L2 a non-conductive fluid, to be subjected to a mixing procedure to obtain a fluid emulsion, presetting the pressure, temperature, stirring mixing conditions of the fluids, stress intensity and application time on said emulsion;
  • fluid 1 deionized water
  • fluid 2 (17 ° API oil) are employed.
  • Fluid 2 is heated to the temperature close to the experiment, where 10 mass% (%, w / w) of fluid 2 is added at the same temperature as fluid 1.
  • the present percentage of fluid 1 in the emulsion is measured, and the separation efficiency is calculated by considering the initial water content present in fluid 2 plus the 10% added mass content for emulsification against the residual content.
  • Example 2 For Example 2 are employed first fluid (deionized water) and the third fluid (oil of 13 API).
  • Fluid 3 is heated to the temperature close to the experiment, where 10 mass% (%, w / w) of fluid 3 is added at the same temperature as fluid 1.
  • the system is closed and an internal nitrogen purge is performed.
  • the system is kept pressurized at 70 psi and 4 kV is applied to the system for 30 minutes. After the voltage is interrupted, the heating system is turned off, the pressure is relieved and after cooling to near ambient temperature, a new 5 mL aliquot is removed from the system. inside the separation vessel (1) to verify the separation efficiency.
  • the present percentage of fluid 1 in the emulsion is measured, and the separation efficiency is calculated by considering the initial water content present in fluid 3 plus the 10% added mass content for emulsification against the residual content.
  • Example 1 the current reaches a minimum value approximately twenty-three minutes after the start of the experiment, while in Example 2 the minimum value is reached in approximately 15 minutes, indicating that the emulsion is less. stable at 125 ° C, a result confirmed by the energy expended for separation and the efficiency of separation.
  • test products are process efficiency and the electric current curve between the electrodes, the higher the value of the electric current observed, the higher the water content within the emulsion and the greater the energy transfer from the electrodes to the water droplets.
  • the total energy expended during the dehydration process can be estimated by numerically integrating the product of the current and voltage measurements obtained during the test as a function of time.
  • This value can be used as a metric to evaluate the emulsion stability against the electrocoalescence process and the emulsions whose energies for separation are higher, are obviously more stable compared to the electrocoalescence.

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  • Chemical & Material Sciences (AREA)
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  • Engineering & Computer Science (AREA)
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  • Food Science & Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
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Abstract

L'invention concerne un équipement (100) pour la déstabilisation électrostatique d'émulsions de fluides L1 conducteur et L2 non conducteur sous pression dans un système étanche, la séparation de l'émulsion étant réalisée au moyen d'un procédé d'électro-coalescence à rendement élevé utilisé industriellement. L'équipement (100) comprend une cuve de séparation (1), une cuve d'alimentation (32) pour alimenter la cuve (1) en fluides L1 et L2 et en gaz en vue de la mise sous pression de ladite cuve (1), un agitateur (51) pour émulsionner les fluides L1 et L2, la cuve (1) étant maintenue étanche par des raccords filetés (35, 35a, 35b, 35c, 35d, 35e) adaptés aux couvercles supérieurs (20) et (9) de la cuve (1). L'invention concerne également le procédé de test pour évaluer la stabilité électrostatique de fluides L1 et L2 à l'aide de l'équipement (100).
PCT/BR2011/000445 2011-12-05 2011-12-05 Équipement pour la déstabilisation électrostatique d'émulsions de fluides sous pression dans un système hermétique et procédé de test WO2013082681A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/BR2011/000445 WO2013082681A1 (fr) 2011-12-05 2011-12-05 Équipement pour la déstabilisation électrostatique d'émulsions de fluides sous pression dans un système hermétique et procédé de test
BR112014007064-4A BR112014007064B1 (pt) 2011-12-05 2011-12-05 equipamento para desestabilização eletrostática de emulsões de fluidos sob pressão em sistema hermético e método de teste

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PCT/BR2011/000445 WO2013082681A1 (fr) 2011-12-05 2011-12-05 Équipement pour la déstabilisation électrostatique d'émulsions de fluides sous pression dans un système hermétique et procédé de test

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114354691A (zh) * 2021-12-31 2022-04-15 北京石油化工学院 原油乳化液电场破乳特性评价装置

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3105739B1 (fr) 2019-12-30 2023-06-30 Charles Adriano Duvoisin Systeme et procede de separation d'emulsions petrole/eau par electrocoalescence

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2678911A (en) * 1950-10-25 1954-05-18 California Research Corp Emulsion testing
US5529675A (en) * 1994-12-16 1996-06-25 Shell Oil Company Electrostatic coalescer testing apparatus
US6136174A (en) * 1998-06-03 2000-10-24 Kvaerner Process Systems Compact electrostatic coalescer
WO2001085297A1 (fr) * 2000-05-05 2001-11-15 Abb Research Ltd. Coalesceur electrostatique

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2678911A (en) * 1950-10-25 1954-05-18 California Research Corp Emulsion testing
US5529675A (en) * 1994-12-16 1996-06-25 Shell Oil Company Electrostatic coalescer testing apparatus
US6136174A (en) * 1998-06-03 2000-10-24 Kvaerner Process Systems Compact electrostatic coalescer
WO2001085297A1 (fr) * 2000-05-05 2001-11-15 Abb Research Ltd. Coalesceur electrostatique

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114354691A (zh) * 2021-12-31 2022-04-15 北京石油化工学院 原油乳化液电场破乳特性评价装置
CN114354691B (zh) * 2021-12-31 2023-10-27 北京石油化工学院 原油乳化液电场破乳特性评价装置

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Publication number Publication date
BR112014007064A2 (pt) 2019-09-24
BR112014007064B1 (pt) 2021-06-08

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