CN104155217A - High-temperature and high-pressure interfacial tension measurement device and method - Google Patents
High-temperature and high-pressure interfacial tension measurement device and method Download PDFInfo
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- CN104155217A CN104155217A CN201410346184.7A CN201410346184A CN104155217A CN 104155217 A CN104155217 A CN 104155217A CN 201410346184 A CN201410346184 A CN 201410346184A CN 104155217 A CN104155217 A CN 104155217A
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Abstract
The invention provides a high-temperature and high-pressure interfacial tension measurement device and method. The measurement device is provided with a buffer bottle and a gas injection pump between a steel cylinder and a visual kettle; a sample injection pump is connected with a pump flow control box and a pump temperature measurement probe; the gas injection pump is arranged in a cold trap which is connected with a low-temperature thermostatic bath; the gas injection pump is provided with an outer cavity and an inner cavity; a window of the visual kettle is a sapphire window; a temperature measurement probe and a pressure sensor in the kettle are respectively arranged on the two sides of a suspension dropper; a gas-liquid inlet and outlet pipe is vertically opposite to the suspension dropper at the bottom of the visual kettle. After the device and the method are adopted, the problems that pressurization is difficult when a pendant-drop method is used for interfacial tension measurement under the conditions of high temperature and high pressure, liquid drops easily fall off under mixed-phase condition, and the window needs high pressure resistance, high temperature resistance and high light transmittance can be solved; an experimental facility is safe and explosion-proof; the device and the method for interfacial tension measurement within the high experimental temperature range (over 100 DEG C) and under the high pressure (over 10 MPa) can be provided.
Description
Technical field
The invention belongs to the technical field of measuring high pressure property interfacial tension, relate to and under high-temperature and high-pressure conditions, adopt sessile drop method to measure oil-gas (CO
2, N
2, gaseous hydrocarbon etc.) measurement mechanism and the method for testing of interfacial tension.
Background technology
CO
2the displacement of reservoir oil (CO
2-EOR) refer to CO
2in gas inject oil reservoir, reduce Crude viscosity, improve crude oil tar productivity.CO
2technology of reservoir sweep can buried CO
2time improve oil recovery.CO
2the mechanism of action of-EOR can be divided into CO
2mixed phase drives and CO
2non-phase-mixing driving.CO
2in oil displacement process, when oil gas interface tension force is zero, the pressure that reaches mixed phase is minimum miscible pressure-MMP (Minimum Miscibility Pressure), so interfacial tension and MMP are judgement CO
2whether technology of reservoir sweep reaches an important parameter of mixed phase.
The method of measuring interfacial tension is more, mainly contains capillary tube technique, decylization method, hangs sheet method, bubble maximum pressure method, sessile drop method and drop-volume method, and wherein capillary tube technique and sessile drop method can be used for measuring interfacial tension under high-temperature and high-pressure conditions.Capillary tube technique is applicable to energy complete wetting liquid capillaceous, and the method can be used for measuring interfacial tension under High Temperature High Pressure, but temperature can not surpass 100 ℃, and pressure can not surpass 13.8MPa.Sessile drop method can meet the measurement of interfacial tension under high temperature and high pressure condition simultaneously, and temperature is more than 100 ℃, more than pressure 10Mpa.The method has significant advantage, except to the wettability of sample without being strict with, also have the wide advantage of measurement range.The method measure interfacial tension fast, accurately, not disturbance surface, amount of samples be few, also can be used for the measurement of low interfacial tension.
China's oil field heavy constituent content is high, viscosity is large, formation temperature is high, causes minimum miscible pressure high, and for example, during Canada 49 ℃ of certain oil field stratum temperature, MMP is 10MPa left and right, and Daqing oil field is crude oil and CO when 45 ℃ of reservoir temperature conditions
2mMP more than 25MPa, Tarim Oilfield MMP when formation temperature is 108 ℃ is 38.094MPa.Therefore interfacial tension experiments of measuring need be carried out under High Temperature High Pressure.
Within 2013, Chinese patent CN103411854A has described high pressure interface tension measuring device and measuring method, yet at CO
2in oil displacement experiment, experiment condition needs higher temperature range and larger pressure limit, and experimental temperature is more than 100 ℃, more than pressure 10MPa.In prior art without pressue device, CO in steel cylinder
2pressure be generally about 7MPa, only depend on the pressure in steel cylinder cannot realize high pressure; Visual still form is high pressure resistant glass, can only under 20Mpa, use; Liquid charge pump does not have temperature and flow control, easily causes drop landing; In device, without burst disk, there is potential safety hazard.The present invention, for addressing these problems, has developed High Temperature High Pressure interfacial tension measurement mechanism and method of testing.
Summary of the invention
The invention provides a kind of new High Temperature High Pressure interfacial tension measurement mechanism and method of testing, solved the related defects of measuring interfacial tension under current high-temperature and high-pressure conditions.
Technical scheme of the present invention is as follows:
A High Temperature High Pressure interfacial tension measurement mechanism is provided with surge flask (11) and gas injection pump (17) between steel cylinder and visual still (31); Sample syringe pump (23) setting is connected with pump discharge control box (24) and pump temperature probe (25).
Gas inject pump (17) is placed in cold-trap (16), and cold-trap (16) is connected with low temperature thermostat bath (19), and low temperature thermostat bath (19) provides low-temperature circulating water; Gas inject pump (17) is divided into exocoel (111) and inner chamber (112); Exocoel gas access (113) is at the top of exocoel (111), exocoel liquid gas outlet (114) is in the bottom of exocoel (111), assurance exocoel (111) enters the gas of inner chamber (112) for liquid, exocoel liquid gas enters inner chamber (112) by the liquid gas access of inner chamber (115), then by the liquid gas vent of inner chamber (116), enters visual still.
Gas inject pump (17) can adjust flux.
The form of visual still (31) is sapphire form (317); In still, temperature probe (34) and pressure transducer (35) are respectively in the both sides of hanging drop pipe (28), and gas-liquid inlet/outlet pipe (312) is vertically opposite with hanging drop pipe (28) in visual still bottom.
On visual still (31), be provided with burst disk (41) and waste gas exhaust valve (42).
Hanging drop pipe (28) is cutting ferrule sealing with the sealing means that visual still pressure chamber (313) adopts, the hanging drop pipe that replaceable internal diameter is different; Hanging drop pipe (28) is connected with the outer part temperature probe (26) of hanging drop pipe still.
Between described sapphire form (317) and kettle, adopt and fix and seal with poroid screw.
Visual still pressure chamber (313) heating rod (311) of around evenly arranging; Kettle temperature probe (33) is positioned at visual still (31) thermograde maximum, guarantees that temperature in the kettle is constant.
Utilize device of the present invention to carry out the method for interfacial tension measurement, comprise the following steps:
1) visual still pressurization steps: open steel cylinder main valve to gas inject pump pressure table (13) registration and no longer raise, open low temperature thermostat bath (19) and cold-trap (16), by the liquid CO in exocoel (111)
2suck inner chamber (112), close exocoel connection valve (14) in gas inject pump, open gas and enter still valve (15), by the liquid CO in inner chamber (112)
2squeeze in visual still, by sapphire form (317), observe liquid CO in still
2liquid level, open still heater switch, be heated to temperature required;
2) injecting step: sample joins samples pre-heated pond (21), sample is sucked to sample syringe pump (23), be heated to test temperature required, open sample syringe pump flow control case (24), adjust flux is maximum, open sample injection valve (27), treat that hanging drop pipe (28) exit has drop to occur; Can turn flow down;
3) according to image acquisition and treatment step, calculate interfacial tension.
Beneficial effect of the present invention is: solved under high-temperature and high-pressure conditions, adopt sessile drop method to carry out the pressurization difficulty running into when interfacial tension is measured, approaching miscible conditions drop easily comes off, problem high pressure resistant, high temperature resistant, high printing opacity that form needs, and experimental provision safety anti-explosive problem, provide under higher temperature scope and larger pressure condition, experimental temperature is more than 100 ℃, more than pressure 10MPa, carry out the apparatus and method of interfacial tension measurement.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of apparatus of the present invention
Fig. 2 is gas inject pump structure figure in the present invention
Fig. 3 (a) is high-temperature high-pressure visual still structural drawing in the present invention
Fig. 3 (b) is high-temperature high-pressure visual still side view in the present invention
In figure: 11: surge flask, 12: gas inject pump blowdown valve, 13: gas inject pump pressure table, 14: exocoel connection valve in gas inject pump, 15: gas enters still valve, 16: cold-trap, 17: gas inject pump, 18: gas enters still pipeline, 19: low temperature thermostat bath, 21: samples pre-heated pond, 22: sample enters pump valve, 23: sample syringe pump, 24: pump discharge control box, 25: pump temperature probe, 26: the outer part temperature probe of hanging drop pipe still, 27: sample injection valve, 28: hanging drop pipe, 31: visual still, 32: waste liquid exhaust valve, 33: kettle temperature probe, 34: temperature probe in still, 35: pressure transducer, 36: still support, 41: burst disk, 42: waste gas exhaust valve, 51:LED light source, 52: precise manual translation stage, 53: industrial lens and CCD camera, 54: computing machine, 111: exocoel, 112: inner chamber, 113: exocoel gas access, 114: the outlet of exocoel liquid gas, 115: the liquid gas access of inner chamber, 116: the liquid gas vent of inner chamber, 311: heating rod, 312: gas-liquid inlet/outlet pipe, 313: visual still pressure chamber, 314: still large sealing packing ring, 315: form O-ring seal, 316: back-up ring after form, 317: sapphire form, 318: insulation material.
Embodiment
For technical characterictic of the present invention, object and effect being had more clearly, understand, existing combination technology scheme and accompanying drawing explanation elaborate the specific embodiment of the present invention.
As shown in Fig. 1,2,3 (a), 3 (b): this High Temperature High Pressure interfacial tension measurement mechanism, comprises gas injection apparatus, fluid infusion apparatus, high-temperature high-pressure visual still, safe explosion-proof device, image acquisition and treating apparatus:
Gas injection apparatus comprises surge flask (11) and gas injection pump (17), gas inject pump (17) is placed in cold-trap (16), cold-trap (16) is connected with low temperature thermostat bath (19), and low temperature thermostat bath (19) provides low-temperature circulating water; Gas inject pump (17) is divided into exocoel (111) and inner chamber (112), this gas inject pump (17) capable of regulating flow quantity.
Fluid infusion apparatus comprises samples pre-heated pond (21), sample syringe pump (23) and hanging drop pipe (28), and heating plate is equipped with in side, samples pre-heated pond (21), and rubber plug is arranged at top; Sample syringe pump (23) and hanging drop pipe (28) are outer heating jacket and temperature probe, is respectively the outer part temperature probe (26) of pump temperature probe (25) and hanging drop pipe still; Sample syringe pump (23) connects pump discharge control box (24), capable of regulating flow quantity.
High-temperature high-pressure visual still comprises visual still (31), pressure transducer (35) and still support (36), visual still (31) material is Stainless steel 316 austenite, be shaped as cylindrical barrel, comprise visual still pressure chamber (313) and sapphire form (317); Visual still pressure chamber (313) two ends have with the screw of circular hole fixes and seals sapphire form (317), and around four heating rods (311) are evenly arranged in insulation material (318); Two temperature controls are housed in still, are respectively temperature probe (34) in kettle temperature probe (33) and still, still support (36) is connected with still by heat insulation structural; Temperature probe (34) and pressure transducer (35) are respectively in the both sides of hanging drop pipe (28) in still, gas-liquid inlet/outlet pipe (312) is vertically opposite with hanging drop pipe (28) in visual still bottom, be connected with threeway, threeway one tunnel connects waste liquid exhaust valve (32), waste liquid exhaust valve (32) is vertically opposite with hanging drop pipe (28), another road connects gas and enters still pipeline (18), and pipeline outer wrapping heating tape and temperature probe, prevent CO
2gas decompression frosting.
Safe explosion-proof device comprises burst disk (41), waste gas exhaust valve (42), gas inject pump pressure table (13), kettle temperature probe (33), pressure transducer (35), burst disk (41) pressure release Way out is horizontal direction, each of left and right; Gas inject pump pressure table (13), pressure transducer (35) and kettle temperature probe (33) are all connected with warning device.
Image acquisition and treating apparatus comprise LED light source (51), precise manual translation stage (52), industrial lens and CCD camera (53), computing machine (54), and industrial lens and CCD camera (53) are screwed on precise manual translation stage (52).
Described gas inject pump (17) is divided into exocoel (111) and inner chamber (112), exocoel gas access (113) is at the top of exocoel (111), exocoel liquid gas outlet (114) is in the bottom of exocoel (111), assurance exocoel (111) enters the gas of inner chamber (112) for liquid, exocoel liquid gas enters inner chamber (112) by the liquid gas access of inner chamber (115), then by the liquid gas vent of inner chamber (116), enters visual still.
Described sample syringe pump (23) connects pump discharge control box (24), capable of regulating flow quantity, and minimum flow is less than 0.025mL/min, accurately controls the speed that drop forms; Hanging drop pipe (28) is cutting ferrule sealing with the sealing means that visual still pressure chamber (313) adopts, detachable, changes the different hanging drop pipe of internal diameter, for the measurement of different range interfacial tension.
Described sapphire form (317) is the high printing opacity of thickness 18mm, high pressure resistant, resistant to elevated temperatures corundum, high pressure resistant 40MPa; Between this form and kettle, adopt and fix and seal with poroid screw, detachable; This sapphire form (317) is elasticity, thermostable fluorine rubber seal with form O-ring seal (315) and still large sealing packing ring (314) that visual still pressure chamber (313) adopts; Back-up ring after form (316) is PEK material, high temperature high voltage resistant.
Described visual still pressure chamber (313) four heating rods (311) of around evenly arranging, homogeneous heating, volume is little, does not affect image acquisition; Kettle temperature probe (33) is positioned at visual still thermograde maximum, and insulation material (318) adopts double-layer stainless steel interlayer, adopts line to contact with still, allows hear rate to a certain degree, guarantees that temperature in the kettle is constant.
Described precise manual translation stage (52), can adjust in XYZ tri-directions the position of industrial lens and CCD camera (53).
Above-mentioned High Temperature High Pressure interfacial tension measurement mechanism carries out interfacial tension experiments of measuring, comprises the following steps:
Visual still pressurization, close waste liquid exhaust valve (32), gas inject pump blowdown valve (12), waste gas exhaust valve (42), opening steel cylinder main valve to gas inject pump pressure table (13) registration no longer raises, open low temperature thermostat bath (19) and cold-trap (16), when the registration of gas inject pump pressure table (13) is less than 2MPa, the CO in gas inject pump (17)
2liquefy, again open steel cylinder main valve, no longer raise to the registration of gas inject pump pressure table (13), now existing a large amount of liquid CO in gas inject pump (17)
2, open gas inject pump (17), by the liquid CO in exocoel (111)
2suck inner chamber (112), close exocoel connection valve (14) in gas inject pump, open gas and enter still valve (15), by liquid CO
2squeeze in visual still (31), if gas enters still pipeline there is not CO in (18)
2gas decompression frosting, heating tape switch can not opened, and so repeatedly several times, opens LED light source (51), by sapphire form (317), observes liquid CO in still
2liquid level, estimate CO in still
2amount, in still, squeeze into appropriate liquid CO
2, open still heater switch, be heated to temperature required.
Sample injects, sample adds samples pre-heated pond (21), the larger liquid of viscosity need be opened the preheating of heating plate switch, open sample and enter pump valve (22), laboratory sample is sucked to sample syringe pump (23), close sample and enter pump valve (22), open heating jacket, be heated to test temperature required, open pump discharge control box (24), adjust flux is maximum, open sample injection valve (27), when there is drop in hanging drop pipe (28) exit, turn sample syringe pump flow down and make the speed speed of hanging drop pipe (28) exit end face place drop formation suitable, avoid the rapid landing of drop.
Image acquisition, adjusts precise manual translation stage (52), makes hanging drop pipe (28) exit end face be in visual field central authorities, when drop drips soon, click " starting to gather ", setting-up time is spaced apart 1 second, CCD camera can automatically snap, and clicks " stopping gathering " after drop drippage.
The photo autostore collecting is in computing machine (54), and runs image processing software, calculates interfacial tension.
Experiment finishes, open waste gas exhaust valve (42) pressure release, pressure transducer (35) registration is 0 o'clock, open waste liquid exhaust valve (32) effluent discharge, open the fixedly screw of form and kettle, sapphire form (317) taken out, with lens paper by form wiped clean, change O-ring seal, clean visual still pressure chamber (313).
The example of the above enforcement, object is to illustrate better object of the present invention, technical scheme and beneficial effect.Certainly; according to the difference of concrete application, size, material; response parameter of the present invention (structure, connected mode, size, material, process details, installation method etc.) can be made corresponding variation; what person skilled was done on its basis substitutes or conversion, within the present invention's protection.
Claims (8)
1. a High Temperature High Pressure interfacial tension measurement mechanism, is characterized in that being provided with surge flask (11) and gas injection pump (17) between steel cylinder and visual still (31); Sample syringe pump (23) setting is connected with pump discharge control box (24) and pump temperature probe (25).
2. device as claimed in claim 1, is characterized in that gas inject pump (17) is placed in cold-trap (16), and cold-trap (16) is connected with low temperature thermostat bath (19), and low temperature thermostat bath (19) provides low-temperature circulating water; Gas inject pump (17) is divided into exocoel (111) and inner chamber (112); Exocoel gas access (113) is at the top of exocoel (111), exocoel liquid gas outlet (114) is in the bottom of exocoel (111), assurance exocoel (111) enters the gas of inner chamber (112) for liquid, exocoel liquid gas enters inner chamber (112) by the liquid gas access of inner chamber (115), then by the liquid gas vent of inner chamber (116), enters visual still.
3. device as claimed in claim 1, the form that it is characterized in that visual still (31) is sapphire form (317); In still, temperature probe (34) and pressure transducer (35) are respectively in the both sides of hanging drop pipe (28), and gas-liquid inlet/outlet pipe (312) is vertically opposite with hanging drop pipe (28) in visual still bottom.
4. device as claimed in claim 1, is characterized in that being provided with on visual still (31) burst disk (41) and waste gas exhaust valve (42).
5. device as claimed in claim 1, is characterized in that the sealing means that hanging drop pipe (28) and visual still pressure chamber (313) adopt is cutting ferrule sealing, and hanging drop pipe (28) is connected with the outer part temperature probe (26) of hanging drop pipe still.
6. device as claimed in claim 1, is characterized in that adopting and fixing and seal with poroid screw between described sapphire form (317) and kettle.
7. device as claimed in claim 1, is characterized in that visual still pressure chamber (313) heating rod (311) of evenly arranging around; Kettle temperature probe (33) is positioned at visual still (31) thermograde maximum.
8. the method for utilizing the device of claim 1 to carry out interfacial tension measurement, is characterized in that comprising the following steps:
1) visual still pressurization steps: open steel cylinder main valve to gas inject pump pressure table (13) registration and no longer raise, open low temperature thermostat bath (19) and cold-trap (16), by the liquid CO in exocoel (111)
2suck inner chamber (112), close exocoel connection valve (14) in gas inject pump, open gas and enter still valve (15), by the liquid CO in inner chamber (112)
2squeeze in visual still, by form (317), observe liquid CO in still
2liquid level, open still heater switch, be heated to temperature required;
2) injecting step: sample joins samples pre-heated pond (21), sample is sucked to sample syringe pump (23), be heated to test temperature required, open pump discharge control box (24), adjust flux is maximum, open sample injection valve (27), make hanging drop pipe (28) exit have drop to occur;
3) according to image acquisition and treatment step, calculate interfacial tension.
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Application publication date: 20141119 |