CN106198316B - A kind of dissolved gas crude oil with pressure emulsification surveys viscous integration apparatus and surveys adhering method - Google Patents

A kind of dissolved gas crude oil with pressure emulsification surveys viscous integration apparatus and surveys adhering method Download PDF

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Publication number
CN106198316B
CN106198316B CN201610480575.7A CN201610480575A CN106198316B CN 106198316 B CN106198316 B CN 106198316B CN 201610480575 A CN201610480575 A CN 201610480575A CN 106198316 B CN106198316 B CN 106198316B
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autoclave
torque
viscosity
crude oil
revolving speed
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CN106198316A (en
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孙广宇
李传宪
杨飞
魏国庆
姚博
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China University of Petroleum East China
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China University of Petroleum East China
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N11/10Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
    • G01N11/14Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane

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Abstract

The invention discloses a kind of integration apparatus for dissolved gas crude oil emulsification property with pressure test and viscosity measurement, it has installed high-speed stirred system, torque-measuring apparatus and conductivity measuring apparatus additional on the basis of ordinary high pressure reaction kettle, it can be achieved that the emulsification during transportation of casing-head gas flooding produced liquid and flow simulating.The emulsification to dissolved gas crude oil and water phase in autoclave autoclave body 5 is realized using high speed stirrer motor 6, magnetic driver device 8, agitating paddle 9, the real-time measurement that stirring torque is realized using micro-range torductor 7 realizes the real-time monitoring to dissolved gas crude oil and water phase emulsified state in autoclave autoclave body 5 using conductivity meter 26.The invention also discloses a kind of methods for carrying out viscosity measurement using the equipment can get the real time viscosity and average shear rate of high-pressure fluid using this method.For this equipment compared with circuit device, occupied area is small, and required experiment oil sample is few, and cost of investment is relatively low.

Description

A kind of dissolved gas crude oil with pressure emulsification surveys viscous integration apparatus and surveys adhering method
Technical field
The present invention relates to non-conventional crude oils to exploit transportation art, special for dissolved gas crude oil with pressure emulsification more particularly to one kind Property test and viscosity measurement integration apparatus, it is characterized in that the emulsification of crude oil and water phase can be carried out under high pressure gas existence condition And on-line viscosity measurement.The invention further relates to the specific methods that viscosity measurement is carried out using the equipment.
Background technique
Currently, oil field at home exploitation progresses into the middle and later periods, but growing demand requirement oil field must improve and adopt Yield.For this purpose, various intensified oil reduction technologies are used, such as chemical flooding, gas drive, oil recovery by heating and microbe oil production.Wherein, gas Drive the CO including mixed phase or part mixed phase that recovers the oil2It drives, N2Drive, natural gas drive and flue gas flooding etc., advantage is fairly obvious, performance Are as follows: crude oil volume is 1. expanded, liquid kinetic energy is increased, improves oil displacement efficiency;2. reducing viscosity of crude, increase crude oil flow ability; 3. oil water interfacial tension is reduced, to reduce residual oil saturation;4. dissolved gas drive acts on, interstitial space, displacement crude oil are occupied.
Produced Liquid in oil reservoir Jing Guo gas drive will reach ground by pit shaft, then reach and join through surface gathering system Station is closed, the separation and processing of oil gas water are carried out.When passing through pit shaft, oil nozzle, valve member, pump during transportation, stirring will receive Shear action often will form water-in-oil type crude oil emulsion between crude oil and water phase.And in gas drive Produced Liquid gas presence, The emulsification property of crude oil, the viscosity of Produced Liquid can be had an impact, to further influence gathering and transportation technology.
Therefore, it is necessary to a kind of device and a kind of Viscosity Measurement Methods, can Simulation of Crude Oil and water phase in high pressure solution gas bar part Under emulsification property, and to crude oil after molten gas, crude oil emulsion carry out it is online survey in real time it is viscous.However, existing high pressure is anti-at present Kettle device is answered, can only realize the preparation of high pressure dissolved gas crude oil, cannot achieve the monitoring of emulsification property and the real-time measurement of viscosity.
Summary of the invention
In consideration of it, the technical problems to be solved by the invention, being to provide a kind of can be completed at the same time dissolved gas crude oil emulsification with pressure Viscous integration apparatus and its matched survey adhering method with survey, it is special for simulating emulsification of the gas drive Produced Liquid when crossing pump, valve Property, and in the duct flow when viscosity.
The technical solution adopted by the present invention to solve the technical problems is:
Viscous integration apparatus is surveyed in a kind of dissolved gas crude oil emulsification with pressure, comprising: gas supply pressurizing device, reaction under high pressure dress It sets, agitating device, measuring device and temperature regulating device.The gas supply pressurizing device includes: gas cylinder, annular coil pipe, piston type gas tank And manually-actuated metering pump;The high pressure reaction assembly includes: autoclave autoclave body, autoclave top cover;The agitating device It include: high speed stirrer motor, magnetic driver device, agitating paddle;The measuring device includes: pressure sensor, temperature sensing Device, conductivity meter, concentrates digital display program control instrument at micro-range torductor;The temperature regulating device includes: annular disk control temperature system System, piston type gas tank temperature-controlling system and reaction kettle autoclave body temperature-controlling system.The gas cylinder is connect with the piston type gas tank, the work Plug gas tank is connect with the manually-actuated metering pump, adjusts the pressure in the piston type gas tank by the manually-actuated metering pump.Institute It states piston type gas tank to connect with the autoclave, is infused the gas in the piston type gas tank by the manually-actuated metering pump Enter in autoclave body, the temperature in the autoclave is adjusted by the reaction kettle autoclave body temperature-controlling system.Pass through the high-speed stirring Motor, the magnetic driver device and the agitating paddle is mixed to realize injection gas and be previously added the autoclave autoclave body The mixing and emulsification of interior crude oil and water are realized the real-time record of stirring torque by the micro-range torductor, passed through The conductivity meter realizes the real-time monitoring of emulsified state.
A kind of dissolved gas crude oil Viscosity Measurement Methods with pressure, include the following steps:
1, idling torque is excluded: sample is first not added in the autoclave, the agitating paddle is arranged in different rotating speeds sky Turn, using the idling torque of micro-range torductor test at this time, obtains the quantitative pass between idling torque and revolving speed System.The torque is that the torque that the magnetic driver device consumes in transmission process is generated with air drag in the reaction kettle The sum of torque, need to exclude during subsequent experimental.
2, the relationship established between viscosity and agitating shaft torque: flow field unconspicuous for the phenomenon that swirls, a certain constant When revolving speed, by there are relationships: μ=aM between the viscosity and agitating shaft torque of stirred fluidb.Wherein, μ is fluid viscosity, Pa s;M is the torque acted on agitating shaft, Nm;A, b is parameter.For fixed stirring system, using several known viscous The fluid of degree, measurement stirring torque, that is, can determine the relational expression of the viscosity and torque under the revolving speed under certain revolving speed.
3, the relationship between shearing rate and revolving speed and viscosity is established: described according to the relationship of energy absorbing device and shearing rate Fluid average shear rate in reaction kettle may be expressed as:Wherein,For fluid average shear rate, s-1;M To act on the torque on agitating shaft, Nm;N is revolving speed, r/s;μ is fluid viscosity, Pas;V is fluid in the reaction kettle Volume, m3
4, the viscosity and average shear rate of molten air-flow body in autoclave are calculated: utilizing the micro-range torductor The stirring torque for measuring molten air-flow body when different rotating speeds, according to relational expression between the viscosity and torque, when obtaining different rotating speeds Fluid viscosity.According to the relational expression between the average shear rate and revolving speed and viscosity, putting down when calculating corresponding speed of agitator Equal shearing rate.
5, change revolving speed, repeating said steps 4 obtain a series of viscosity-average shear rate relationship, so that it is determined that molten air-flow The rheological curve of body.
The annular disk pipe temperature-controlling system, piston type gas tank temperature-controlling system and reaction kettle autoclave body temperature-controlling system are temperature control circulation Water-bath, refrigerant used is the mixture of water and ethyl alcohol in temperature control circulator bath, the proportion Wei Shui ︰ ethyl alcohol of water and ethyl alcohol=(3~ 7) 1 ︰, it is preferable that Shui ︰ ethyl alcohol=5 ︰ 1, heating agent used is the mixture of water and glycerine in temperature control circulator bath, water and the third three The proportion Wei Shui ︰ glycerine of alcohol=(4~8) ︰ 1, it is preferable that Shui ︰ glycerine=6 ︰ 1.
Preferably, the autoclave internal structure uses annulus structure, top side detachable, and top using linear close Envelope.
On the basis of apparatus as discussed above and method, the present invention realizes the specific step of dissolved gas crude oil emulsification and viscosity measurement It is rapid as follows:
1, crude oil and water phase fill in advance: according to the oil-water ratio of setting, into the autoclave, filling is overall in advance Product is the crude oil and water phase of 300mL, and according to required temperature, using the reaction kettle autoclave body temperature-controlling system to the reaction under high pressure Kettle carries out temperature control.
2, gas pipeline purging: the piston type gas tank and the autoclave are purged using the gas cylinder.
3, gas is filled and is mixed: utilizing the manually-actuated metering pump, the gas in the piston type gas tank is injected into institute It states in autoclave, until reaching required pressure.
4, dissolved gas crude oil emulsification property measurement with pressure: firstly, characterizing whether emulsification reaches balance by torque.Pass through institute Stating digital display program control instrument the revolving speed of the stirring motor is arranged is 1000rpm or more, since high-speed stirred initial time, observes institute The registration for stating torductor, with the progress of emulsification, viscosity of mixed liquid increases in kettle, and the registration of the torductor should Show as ascendant trend, it is to be emulsified reach balance after, torque progressivelyes reach stabilization.Secondly, utilizing electrical conductivity method characterization crude oil cream Change degree.Utilize the conductivity meter installed additional on the autoclave, monitoring molten gas mixed liquor in entire whipping process Conductive condition, emulsification of crude oil degree is reflected by the evolution of conductivity parameters.Again, sampling observation.Pass through the high pressure The sample tap of reaction kettle takes out emulsion, and that observes emulsion divides water characteristic.
5, the revolving speed of the stirring motor, root dissolved gas crude oil emulsion viscosity measurement: are reduced by the digital display program control instrument According to the survey adhering method, the viscosity of the molten gas emulsion in different shearings rate is measured, rheological curve is obtained.
The beneficial effects of the present invention are: being suitable under different temperatures and pressure condition, simulation oil field gas drive Produced Liquid is in well Emulsification and conveying in cylinder and pipeline, while also supercritical CO under analog reservoir condition2To the viscosity reducing effect of crude oil.The present invention The experimental facilities is small in size, and required experiment oil sample, water sample are few, experimental facilities it is at low cost, it can be achieved that emulsion process characterization, with And the real-time measurement of viscosity, it is capable of the viscosity change of emulsification and the oil recovery, the defeated process of collection of preferable simulation dissolved gas crude oil.
Detailed description of the invention
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made into one below in conjunction with attached drawing The detailed description of step, in which:
Fig. 1 is dissolved gas crude oil emulsification with pressure provided by the present invention and surveys viscous integration apparatus schematic diagram.
Fig. 2 is the structural schematic diagram of agitating device of the present invention.
Specific embodiment
Below with reference to attached drawing, a preferred embodiment of the present invention will be described in detail, it should be understood that preferred embodiment Only for illustrating the present invention, rather than limiting the scope of protection of the present invention.
Embodiment 1: viscous integration apparatus is surveyed in a kind of dissolved gas crude oil emulsification with pressure as depicted in figs. 1 and 2, comprising: gas cylinder 1, annular coil pipe 2, piston type gas tank 3, manually-actuated metering pump 4, autoclave autoclave body 5, high speed stirrer motor 6, micro-range torque Measuring instrument 7, magnetic driver device 8, agitating paddle 9, annular disk pipe temperature-controlling system 10, piston type gas tank temperature-controlling system 11, reaction Kettle autoclave body temperature-controlling system 12, pressure sensor 14, pressure gauge 15, concentrates digital display program control instrument 16, gas cylinder valve at temperature sensor 13 17, gas tank air intake valve 18, gas tank pressure relief valve 19, gas tank outlet valve 20, reaction kettle air intake valve 21, reaction kettle exhaust valve Door 22, sample cock 23, pump early gate 24, piston pressurization valve 25, conductivity meter 26, piston 27, torductor top connection Axis device 28, torductor lower part shaft coupling 29, autoclave top cover 30.Wherein, gas cylinder 1, gas cylinder valve 17, pressure gauge 15, annular coil pipe 2, gas tank air intake valve 18, piston type gas tank 3, piston 27, gas tank pressure relief valve 19, gas tank outlet valve 20, It pumps early gate 24, piston pressurization valve 25 and manually-actuated metering pump 4 and constitutes gas supply pressurizing device;Autoclave autoclave body 5, high pressure are anti- Kettle top lid 30, reaction kettle air intake valve 21, reaction kettle drain tap 22 and sample cock 23 is answered to form high pressure reaction assembly;At a high speed Stirring motor 6, torductor top shaft coupling 28, torductor lower part shaft coupling 29, magnetic driver device 8 and stirring Paddle 9 forms agitating device;Temperature sensor 13, micro-range torductor 7, concentrates digital display program control instrument 16 at pressure sensor 14 Measuring device is constituted with conductivity meter 26;Annular disk pipe temperature-controlling system 10, piston type gas tank temperature-controlling system 11 and reaction kettle autoclave body Temperature-controlling system 12 constitutes temperature regulating device.
The gas cylinder 1 is connect by the annular coil pipe 2 with the piston type gas tank 3, the piston type gas tank 3 respectively with The manually-actuated metering pump 4 and the autoclave 5 connect, and are connected to reaction kettle air inlet respectively on the autoclave top cover 30 Valve 21, reaction kettle drain tap 22, sample cock 23, temperature sensor 13, pressure sensor 14, conductivity meter 26, magnetic force Coupled drive device 8, the magnetic driver device 8 respectively with the stirring axis connection inside and outside kettle, the micro-range torductor 7 Pass through torductor top shaft coupling 28, torductor lower part shaft coupling 29 and high-speed stirred electricity respectively Machine 6 and the magnetic driver device 8 connection, the temperature sensor 13, the pressure sensor 14, the micro-range torque The measured value of measuring instrument 7 shows that the revolving speed of the high speed stirrer motor 6 passes through the collection by the concentration digital display program control instrument 16 The middle control of digital display program control instrument 16 and display, the annular disk pipe temperature-controlling system 10, piston type gas tank temperature-controlling system 11, reaction kettle kettle Body temperature-controlling system 12 carries out temperature control to the annular coil pipe 2, the piston type gas tank 3, the autoclave 5 respectively.It is described Annular disk pipe temperature-controlling system 10, piston type gas tank temperature-controlling system 11 and reaction kettle autoclave body temperature-controlling system 12 are temperature control recirculated water Bath, refrigerant used is water ︰ ethyl alcohol=5 ︰ 1 mixture, the piston type gas tank temperature control in the annular disk pipe temperature-controlling system 10 Heating agent Wei Shui ︰ glycerine=6 ︰ 1 mixture used in system 11 and reaction kettle autoclave body temperature-controlling system 12.
From the above it can be seen that design principle of the invention are as follows: using gas cylinder, piston type gas tank, manually-actuated metering pump and Autoclave realizes the pressurization and injection of gas, and the emulsification of dissolved gas crude oil and water is realized using stirring motor, utilizes torquemeter The monitoring of emulsified state is realized in the measurement that viscosity is realized with viscosity-torque relationship using conductivity meter, and it is former can to solve molten gas in this way Oil emulsifies under high pressure and carries out to viscosity the engineering problem of real-time measurement.
Before experiment starts, gas cylinder valve 17, gas tank air intake valve 18, gas tank pressure relief valve 19, gas tank outlet valve are kept 20, reaction kettle air intake valve 21, reaction kettle drain tap 22, sample cock 23, pump early gate 24, piston pressurization valve 25 are located In closed state.
Idling torque is excluded: the high speed stirrer motor 6 is controlled using the concentration digital display program control instrument 16, from revolving speed 50rpm starts, and is increased with the interval of 50rpm, increases to 1200rpm always, at each revolving speed, records the micro-range and turns round The registration of square measuring instrument 7, the torque are the torque that should be excluded when each revolving speed surveys viscosity of mixed liquid.
The viscosity of experimental provision-torque calibration: Newtonian fluid known to 5 kinds of viscosity of selection is labeled as A, B, C, D, E, will The autoclave top cover 30 is dismantled, and 300mL fluid A is added into the autoclave autoclave body 5, by the reaction under high pressure The installation of kettle top lid 30 is to the autoclave autoclave body 5 and seals, and controls the high speed using the concentration digital display program control instrument 16 Stirring motor 6 is increased with the interval of 50rpm since revolving speed 50rpm, increases to 400rpm always, at each revolving speed, The torque registration is subtracted the idling torque registration, obtains fluid A and exist by the registration for recording the micro-range torductor 7 The actual torque of each revolving speed carries out identical experiment step to fluid B, C, D, E, obtains 5 kinds of fluids in the actual torque of each revolving speed, According to formula μ=aMb, viscosity-torque relationship when variant revolving speed is fitted within, a, b value under different rotating speeds are obtained.
Filling crude oil and water: first the autoclave top cover 30 is dismantled, is added into the autoclave autoclave body 5 The autoclave top cover 30 is installed to the autoclave autoclave body 5 and is sealed, utilized by 200mL crude oil and 100mL water The reaction kettle autoclave body temperature-controlling system 12 is heated to 60 DEG C to the autoclave autoclave body 5.
Gas pipeline purging: opening gas cylinder valve 17, gas tank air intake valve 18, gas tank pressure relief valve 19, adjusts gas tank relief valve The aperture of door 19, cleans the piston type gas tank 3, closes gas tank pressure relief valve 19, opens gas tank outlet valve 20, anti- Kettle air intake valve 21, reaction kettle drain tap 22 are answered, gas in the autoclave 5 is cleaned, orderly close-down reaction Kettle drain tap 22, reaction kettle air intake valve 21, gas tank outlet valve 20, gas tank air intake valve 18, gas cylinder valve 17.
Gas pressurized: pump early gate 24, piston pressurization valve 25, gas tank pressure relief valve 19 are opened, the manual meter is utilized Piston 27 in the piston type gas tank 3 is risen to gas tank top by amount pump 4, closes gas tank pressure relief valve 19, opens gas cylinder valve 17, gas tank air intake valve 18 slowly reduces the height of 3 inner piston 27 of piston type gas tank using the manually-actuated metering pump 4, real The filling of gas, orderly close-down gas tank air intake valve 18 and gas cylinder valve 17 in the existing piston type gas tank 3, using it is described manually Metering pump 4 is to gas boost in the piston type gas tank 3 to 10MPa, using the piston type gas tank temperature-controlling system 11 to described Piston type gas tank 3 is heated to 60 DEG C.
The filling and emulsification of gas: gas tank outlet valve 20, reaction kettle air intake valve 21 are opened, the manual metering is utilized The piston 27 in the 4 lifting piston type gas tank 3 of pump, to 5 gas injection of autoclave to 10MPa, orderly close-down reacts Kettle air intake valve 21, gas tank outlet valve 20, using the concentration digital display program control instrument 16 control the high speed stirrer motor 6 with The stirring rate of 1000r/min emulsifies the dissolved gas crude oil in the autoclave 5 with water, records institute in whipping process The registration variation for stating micro-range torductor 7 and the conductivity meter 26 closes the high speed after the two registration reaches stable Stirring motor 6 slowly opens sample cock 23, and the emulsion in the autoclave 5 is taken out 50mL into colorimetric cylinder, is closed Sample cock 23 is closed, by the stability for standing observation emulsion.
Emulsion viscosity measurement: the high speed stirrer motor 6 is controlled using the concentration digital display program control instrument 16, from revolving speed 50rpm starts, and is increased with the interval of 50rpm, increases to 400rpm always, at each revolving speed, records the micro-range and turns round The torque registration is subtracted the idling torque registration by the registration of square measuring instrument 7, obtains emulsion in the practical torsion of each revolving speed Square, according to formula μ=aMbAnd a, b value that each revolving speed obtains, the viscosity of the emulsion in different rotating speeds is calculated, then basis FormulaThe corresponding shearing rate of each viscosity is calculated, viscosity-shearing rate rheological curve is drawn.
It is measured, opens gas tank pressure relief valve 19, reaction kettle drain tap 22, to the piston type, gas tank 3 and described Autoclave 5 carries out pressure release, dismantles to the autoclave 5, using petroleum ether to the autoclave 5 and institute It states autoclave top cover 30 to be cleaned, the autoclave top cover 30 and the autoclave 5 is sealed, close institute There is valve.
Embodiment 2: before experiment starts, gas cylinder valve 17, gas tank air intake valve 18, gas tank pressure relief valve 19, gas tank are kept Outlet valve 20, reaction kettle air intake valve 21, reaction kettle drain tap 22, sample cock 23, pump early gate 24, piston pressurization valve Door 25 is in closed state.
Idling torque is excluded: the high speed stirrer motor 6 is controlled using the concentration digital display program control instrument 16, from revolving speed 50rpm starts, and is increased with the interval of 50rpm, increases to 1200rpm always, at each revolving speed, records the micro-range and turns round The registration of square measuring instrument 7, the torque are the torque that should be excluded when each revolving speed surveys viscosity of mixed liquid.
The viscosity of experimental provision-torque calibration: Newtonian fluid known to 5 kinds of viscosity of selection is labeled as A, B, C, D, E, will The autoclave top cover 30 is dismantled, and 300mL fluid A is added into the autoclave autoclave body 5, by the reaction under high pressure The installation of kettle top lid 30 is to the autoclave autoclave body 5 and seals, and controls the high speed using the concentration digital display program control instrument 16 Stirring motor 6 is increased with the interval of 50rpm since revolving speed 50rpm, increases to 400rpm always, at each revolving speed, The torque registration is subtracted the idling torque registration, obtains fluid A and exist by the registration for recording the micro-range torductor 7 The actual torque of each revolving speed carries out identical experiment step to fluid B, C, D, E, obtains 5 kinds of fluids in the actual torque of each revolving speed, According to formula μ=aMb, viscosity-torque relationship when variant revolving speed is fitted within, a, b value under different rotating speeds are obtained.
Crude oil filling: first the autoclave top cover 30 is dismantled, is added into the autoclave autoclave body 5 The autoclave top cover 30 is installed to the autoclave autoclave body 5 and is sealed, utilizes the reaction by 300mL crude oil Kettle autoclave body temperature-controlling system 12 is heated to 80 DEG C to the autoclave autoclave body 5.
CO2Gas pipeline purging: opening gas cylinder valve 17, gas tank air intake valve 18, gas tank pressure relief valve 19, adjusts gas tank pressure release The aperture of valve 19 cleans the piston type gas tank 3, closing gas tank pressure relief valve 19, opening gas tank outlet valve 20, Reaction kettle air intake valve 21, reaction kettle drain tap 22 clean gas in the autoclave 5, and orderly close-down is anti- Answer kettle drain tap 22, reaction kettle air intake valve 21, gas tank outlet valve 20, gas tank air intake valve 18, gas cylinder valve 17.
CO2Liquefaction: gas tank pressure relief valve 19, pump early gate 24, piston pressurization valve 25 are opened, the manual metering is utilized 3 inner piston of piston type gas tank is risen to gas tank top by pump 4, closes valve 19, right using the annular disk pipe temperature-controlling system 10 Annular 2 refrigeration cool-down of coil pipe opens gas cylinder valve 17, gas tank air intake valve 18, utilizes the manually-actuated metering pump 4 to 0 DEG C The height for slowly reducing the piston in the piston type gas tank 3 realizes filling for liquid carbon dioxide in the piston type gas tank 3 Note, orderly close-down valve 18 and valve 17.
Realize CO2Above-critical state: using the manually-actuated metering pump 4 to liquid carbon dioxide liter in the piston type gas tank 3 It is depressed into 25MPa, 80 DEG C are heated to the piston type gas tank 3 using the piston type gas tank temperature-controlling system 11, passes through institute Manually-actuated metering pump 4 is stated the pressure change in piston type gas tank described in temperature-rise period 3 is adjusted.
Supercritical CO2Filling with mix: open gas tank outlet valve 20, reaction kettle air intake valve 21, utilize the hand Dynamic metering pump 4 lifts the piston 27 in the piston type gas tank 3, injects supercritical CO to the autoclave 52To pressure Reach 25MPa, orderly close-down reaction kettle air intake valve 21, gas tank outlet valve 20 are controlled using the concentration digital display program control instrument 16 The high speed stirrer motor 6 is made with the stirring rate of 180rpm to the crude oil and supercritical CO in the autoclave 52It carries out Mixing records the registration variation of micro-range torductor 7 described in whipping process, until registration reaches stable.
Molten supercritical CO2Measuring crude oil viscosity: the high speed stirrer motor is controlled using the concentration digital display program control instrument 16 6, since revolving speed 50rpm, is increased with the interval of 50rpm, 400rpm is increased to always, at each revolving speed, described in record The torque registration is subtracted the idling torque registration, obtains emulsion in each revolving speed by the registration of micro-range torductor 7 Actual torque, according to formula μ=aMbAnd each turn
A, b value that speed obtains calculate the viscosity of the emulsion in different rotating speeds, then according to formulaThe corresponding shearing rate of each viscosity is calculated, viscosity-shearing rate rheological curve is drawn.
It is measured, opens gas tank pressure relief valve 19, reaction kettle drain tap 22, to the piston type gas tank 3 and described Autoclave 5 carries out pressure release, dismantles to the autoclave 5, using petroleum ether to the autoclave 5 and institute It states autoclave top cover 30 to be cleaned, the autoclave top cover 30 and the autoclave 5 is sealed, close institute There is valve.
The above description is only a preferred embodiment of the present invention, is not intended to restrict the invention, any skill for being familiar with this profession Art personnel are not departing within the scope of technical solution of the present invention, when the technology contents using the disclosure above make few modifications or It modifies without departing from the spirit and scope of the present invention, but anything that does not depart from the technical scheme of the invention content, according to the present invention Technical spirit any simple modification, equivalent variations or modification made to the above embodiment, still fall within technical solution of the present invention In the range of.

Claims (4)

1. viscous integration apparatus, packet are surveyed in the dissolved gas crude oil with pressure emulsification of a kind of method for measuring dissolved gas crude oil viscosity with pressure, use Including gas supply pressurizing device, high pressure reaction assembly, agitating device, measuring device and temperature regulating device, the gas supply pressurizing device includes Gas cylinder (1), annular coil pipe (2), piston type gas tank (3) and manually-actuated metering pump (4);The high pressure reaction assembly includes reaction under high pressure Kettle autoclave body (5), autoclave top cover (30);The agitating device includes high speed stirrer motor (6), magnetic driver device (8) and agitating paddle (9);The measuring device includes pressure sensor (14), temperature sensor (13), micro-range torductor (7), conductivity meter (26) and concentration digital display program control instrument (16);The temperature regulating device includes annular disk pipe temperature-controlling system (10), lives Plug gas tank temperature-controlling system (11) and reaction kettle autoclave body temperature-controlling system (12), it is characterised in that: the high speed stirrer motor (6), The magnetic driver device (8) and the agitating paddle (9) are connected with each other, and realize injection gas and to be previously added the high pressure anti- The mixing and emulsification of the crude oil and water in kettle autoclave body (5) are answered, the micro-range torductor (7) passes through the torductor Top shaft coupling (28) is connected with the high speed stirrer motor (6), by torductor lower part shaft coupling (29) with The magnetic driver device (8) is connected, and the conductivity meter (26) protrudes into institute through the autoclave top cover (30) It is internal to state autoclave autoclave body (5);It is characterized in that, specifically includes the following steps:
Step 1. idling torque is excluded: sample is first not added in the autoclave autoclave body (5), the agitating paddle (9) is arranged and exists Different rotating speeds idle running obtains idling torque and revolving speed using the idling torque of the micro-range torductor (7) test at this time Between quantitative relationship;The torque is the torque and the high pressure that the magnetic driver device (8) is consumed in transmission process The sum of the torque that the interior air drag of reaction kettle autoclave body (5) generates, needs to exclude during subsequent experimental;
The viscosity of step 2. device-torque calibration: Newtonian fluid known to 5 kinds of viscosity of selection is labeled as A, B, C, D, E, by institute Autoclave top cover (30) disassembly is stated, 300mL fluid A is added into the autoclave autoclave body (5), the high pressure is anti- Kettle top lid (30) installation is answered to the autoclave autoclave body (5) and is sealed, is controlled using the concentration digital display program control instrument (16) The high speed stirrer motor (6) is increased with the interval of 50rpm since revolving speed 50rpm, 400rpm is increased to always, each At a revolving speed, the registration of the micro-range torductor (7) is recorded, which is subtracted into the idling torque registration, Fluid A is obtained in the actual torque of each revolving speed, identical experiment step is carried out to fluid B, C, D, E, obtains 5 kinds of fluids in each revolving speed Actual torque fit within viscosity-torque relationship when variant revolving speed according to formula μ=aMb, obtain under different rotating speeds A, b value;
The filling of step 3. testing liquid: first the autoclave top cover (30) is dismantled, to the autoclave autoclave body (5) Interior addition 300mL testing liquid, by the autoclave top cover (30) installation to the autoclave autoclave body (5) and close Envelope, using the reaction kettle autoclave body temperature-controlling system (12) to autoclave autoclave body (5) temperature control;
Step 4. testing liquid viscosity measurement: controlling the high speed stirrer motor (6) using the concentration digital display program control instrument (16), Since revolving speed 50rpm, is increased with the interval of 50rpm, increase to 400rpm always, at each revolving speed, record described micro- The torque registration is subtracted the idling torque registration, obtains liquid in the reality of each revolving speed by the registration of range torductor (7) Border torque, according to formula μ=aMbAnd a, b value that each revolving speed obtains, the viscosity of the emulsion in different rotating speeds is calculated, then According to formulaThe corresponding shearing rate of each viscosity is calculated, it is bent to draw viscosity-shearing rate rheology Line.
2. the method for measurement dissolved gas crude oil viscosity with pressure described in accordance with the claim 1, it is characterised in that: the high-speed stirred electricity Revolving speed >=1500rpm of machine (6).
3. the method for measurement dissolved gas crude oil viscosity with pressure described in accordance with the claim 1, it is characterised in that: the micro-range torque Measuring instrument (7) tests torque range are as follows: 0-300mNm, precision 0.1mNm.
4. the method for measurement dissolved gas crude oil viscosity with pressure described in accordance with the claim 1, it is characterised in that: the conductivity meter It (26) is high-temp and-pressure conductivity meter, minimum resolution is 0.1 μ S/cm.
CN201610480575.7A 2016-06-27 2016-06-27 A kind of dissolved gas crude oil with pressure emulsification surveys viscous integration apparatus and surveys adhering method Expired - Fee Related CN106198316B (en)

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CN105004838A (en) * 2015-07-03 2015-10-28 中国石油大学(华东) Equipment for processing crude oil with supercritical carbon dioxide and processing method thereof
CN105181526A (en) * 2015-07-17 2015-12-23 江苏恒神股份有限公司 Viscosity detection method in sizing agent production process
CN105486609A (en) * 2015-12-22 2016-04-13 成都孚吉科技有限责任公司 High-temperature and high-pressure viscosity tester for testing viscosity of crude oil

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CN104155344A (en) * 2014-07-31 2014-11-19 广东省昆虫研究所 Method for rapidly, simply and conveniently detecting illegal cooking oil
CN105004838A (en) * 2015-07-03 2015-10-28 中国石油大学(华东) Equipment for processing crude oil with supercritical carbon dioxide and processing method thereof
CN105181526A (en) * 2015-07-17 2015-12-23 江苏恒神股份有限公司 Viscosity detection method in sizing agent production process
CN105486609A (en) * 2015-12-22 2016-04-13 成都孚吉科技有限责任公司 High-temperature and high-pressure viscosity tester for testing viscosity of crude oil

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