CN106198316A - A kind of dissolved gas crude oil emulsifying with pressure is surveyed viscous integration apparatus and surveys adhering method - Google Patents

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

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CN106198316A
CN106198316A CN201610480575.7A CN201610480575A CN106198316A CN 106198316 A CN106198316 A CN 106198316A CN 201610480575 A CN201610480575 A CN 201610480575A CN 106198316 A CN106198316 A CN 106198316A
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viscosity
autoclave
rotating speed
crude oil
kettle
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CN106198316B (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 for dissolved gas crude oil emulsification property with pressure test and the integration apparatus of viscosity measurement, it has installed high-speed stirred system, torque-measuring apparatus and conductivity measuring apparatus on the basis of ordinary high pressure reactor additional, can realize the emulsifying in course of conveying of the casing-head gas flooding produced liquid and flow simulating.High speed stirrer motor 6, magnetic driver device 8, stirring paddle 9 is utilized to realize the emulsifying to dissolved gas crude oil in autoclave kettle 5 Yu aqueous phase, utilize micro-range torductor 7 to realize the real-time measurement of stirring moment of torsion, utilize conductivity meter 26 to realize the real-time monitoring to dissolved gas crude oil in autoclave kettle 5 with aqueous phase emulsified state.The invention also discloses a kind of method utilizing described equipment to carry out viscosity measurement, utilize the method, real time viscosity and the average shear rate of high-pressure fluid can be obtained.This equipment is compared with circuit device, and floor space is little, and required experiment oil sample is few, and cost of investment is relatively low.

Description

A kind of dissolved gas crude oil emulsifying with pressure is surveyed viscous integration apparatus and surveys adhering method
Technical field
The present invention relates to non-conventional crude oil exploitation transportation art, particularly relate to a kind of special for dissolved gas crude oil emulsifying with pressure Property test and viscosity measurement integration apparatus, it is characterized in that to carry out under gases at high pressure existence condition the emulsifying of crude oil and aqueous phase And on-line viscosity measurement.The invention still further relates to the concrete grammar utilizing this equipment to carry out viscosity measurement.
Background technology
At present, oil field at home exploitation progresses into middle and late stage, but growing demand requires that oil field must be improved adopts Yield.To this end, various intensified oil reduction technology are used, such as chemical flooding, gas drive, oil recovery by heating and microbe oil production etc..Wherein, gas Drive oil recovery and include mixed phase or the CO of part mixed phase2Drive, N2Drive, natural gas drive and flue gas flooding etc., its advantage is fairly obvious, performance For: 1. expand crude oil volume, increase liquid kinetic energy, improve oil displacement efficiency;2. reduce viscosity of crude, increase crude oil flow ability; 3. reduce oil water interfacial tension, thus reduce residual oil saturation;4. dissolved gas drive effect, occupies interstitial space, displacement crude oil.
Through the Produced Liquid of gas drive in oil reservoir, ground to be arrived through pit shaft, then arrive connection through surface gathering system Close station, carry out separation and the process of oil gas water.Through pit shaft, oil nozzle, valve member, pump in course of conveying, can be stirred Shear action, often forms water-in-oil type crude oil emulsion between crude oil and aqueous phase.And the existence of gas in gas drive Produced Liquid, The viscosity of the emulsification property of crude oil, Produced Liquid can be produced impact, thus have influence on gathering and transportation technology further.
Accordingly, it would be desirable to a kind of device and a kind of Viscosity Measurement Methods, it is possible to Simulation of Crude Oil and aqueous phase are in high pressure solution gas condition Under emulsification property, and crude oil after molten gas, crude oil emulsion are carried out online survey in real time viscous.But, current existing high pressure is anti- Answer kettle device, the preparation of high pressure dissolved gas crude oil can only be realized, it is impossible to realize the monitoring of emulsification property and the real-time measurement of viscosity.
Summary of the invention
In consideration of it, the technical problem to be solved, it is to provide one and can complete dissolved gas crude oil emulsifying with pressure simultaneously The integration apparatus viscous with survey and supporting survey adhering method thereof, special for the emulsifying when crossing pump, valve of the Simulated gas flooding produced liquid Property, and viscosity when flowing in the duct.
The technical solution adopted for the present invention to solve the technical problems is:
Viscous integration apparatus is surveyed in the dissolved gas crude oil with pressure emulsifying of described one, including: supply pressue device, reaction under high pressure dress Put, agitating device, measurement apparatus and temperature regulating device.Described supply pressue device includes: gas cylinder, annular coil pipe, piston type gas tank And manually-actuated metering pump;Described high pressure reaction assembly includes: autoclave kettle, autoclave top cover;Described agitating device Including: high speed stirrer motor, magnetic driver device, stirring paddle;Described measurement apparatus includes: pressure transducer, temperature sensing Device, micro-range torductor, conductivity meter, concentration digital display program control instrument;Described temperature regulating device includes: annular disk management and control temperature system System, piston type gas tank temperature-controlling system and reactor kettle temperature-controlling system.Described gas cylinder is connected with described piston type gas tank, described work Plug gas tank is connected with described manually-actuated metering pump, regulates the pressure in described piston type gas tank by described manually-actuated metering pump.Institute State piston type gas tank to be connected with described autoclave, by described manually-actuated metering pump, the gas in described piston type gas tank is noted Enter in kettle, regulate the temperature in described autoclave by described reactor kettle temperature-controlling system.By described high-speed stirring Mix motor, described magnetic driver device and described stirring paddle to realize injecting gas and being previously added described autoclave kettle In the mixing of crude oil and water and emulsifying, realized the real time record of stirring moment of torsion by described micro-range torductor, pass through Described conductivity meter realizes the real-time monitoring of emulsified state.
A kind of dissolved gas crude oil Viscosity Measurement Methods with pressure, comprises the steps:
1, idling torque is excluded: be first not added with sample in described autoclave, arranges described stirring paddle empty at different rotating speeds Turn, utilize described micro-range torductor test idling torque now, it is thus achieved that the quantitative pass between idling torque and rotating speed System.This moment of torsion is that the moment of torsion that described magnetic driver device consumes in transmission process produces with air drag in described reactor Moment of torsion sum, need to exclude during subsequent experimental.
2, the relation between viscosity and shaft moment of torsion is set up: flow field unconspicuous for the phenomenon that swirls, a certain constant During rotating speed, be there is relation: μ=aM by between viscosity and the shaft moment of torsion of stirred fluidb.Wherein, μ is fluid viscosity, Pa s;M is to act on the moment of torsion on shaft, N m;A, b are parameters.For fixing stirring system, use several known viscous The fluid of degree, measures stirring moment of torsion under certain rotating speed, i.e. can determine that the relational expression of the viscosity under this rotating speed and moment of torsion.
3, the relation between shear rate and rotating speed and viscosity is set up: according to the relation of energy absorbing device Yu shear rate, described Fluid average shear rate in reactor is represented by:Wherein,For fluid average shear rate, s-1;M For acting on the moment of torsion on shaft, N m;N is rotating speed, r/s;μ is fluid viscosity, Pa s;V is fluid in described reactor Volume, m3
4, viscosity and the average shear rate of molten air-flow body in autoclave are calculated: utilize described micro-range torductor The stirring moment of torsion of molten air-flow body when measuring different rotating speeds, according to relational expression between described viscosity and moment of torsion, when obtaining different rotating speeds Fluid viscosity.According to the relational expression between described average shear rate and rotating speed and viscosity, putting down when calculating corresponding speed of agitator All shear rates.
5, change rotating speed, repeating said steps 4, obtain a series of viscosity-average shear rate relation, so that it is determined that molten air-flow The rheological curve of body.
Described annular disk pipe temperature-controlling system, piston type gas tank temperature-controlling system and reactor kettle temperature-controlling system are temperature control circulation Water-bath, in temperature control circulator bath coolant used be the proportioning of the mixture of water and ethanol, water and ethanol be water-ethanol=(3~ 7) 1, it is preferable that water-ethanol=5 1, in temperature control circulator bath, heating agent used is the mixture of water and glycerol, water and the third three The proportioning of alcohol is water glycerol=(4~8) 1, it is preferable that water glycerol=6 1.
Preferably, it is the closeest that described autoclave internal structure uses annular space structure, top side detachable, and top to use Envelope.
On the basis of apparatus as discussed above and method, the present invention realizes the concrete step of dissolved gas crude oil emulsifying and viscosity measurement Rapid as follows:
1, crude oil fills in advance with aqueous phase: according to the oil-water ratio set, and in described autoclave, filling is overall in advance Amass the crude oil for 300mL and aqueous phase, and according to temperature required, utilize described reactor kettle temperature-controlling system to described reaction under high pressure Still carries out temperature control.
2, gas pipeline purging: utilize described gas cylinder that described piston type gas tank and described autoclave are purged.
3, gas fills and mixes: utilize described manually-actuated metering pump, the gas in described piston type gas tank is injected into institute State in autoclave, until it reaches desirable pressure.
4, dissolved gas crude oil emulsification property with pressure is measured: first, characterizes whether emulsifying reaches balance by moment of torsion.By institute Stating digital display program control instrument and arranging the rotating speed of described stirring motor is more than 1000rpm, from the beginning of high-speed stirred initial time, observes institute Stating the registration of torductor, along with the carrying out of emulsifying, in still, viscosity of mixed liquid increases, and the registration of described torductor should Show as ascendant trend, to be emulsified reach balance after, moment of torsion progressivelyes reach stable.Secondly, electrical conductivity method is utilized to characterize crude oil breast Change degree.Utilize the described conductivity meter installed additional on described autoclave, monitoring molten gas mixed liquor in whole whipping process Conduction situation, reflect emulsification of crude oil degree by the evolution of conductivity parameters.Again, sampling is observed.By described high pressure Emulsion is taken out by the sample tap of reactor, observes point water characteristic of emulsion.
5, dissolved gas crude oil emulsion viscosity measurement: reduced the rotating speed of described stirring motor, root by described digital display program control instrument According to described survey adhering method, measure the viscosity of molten gas emulsion when different shear rate, obtain rheological curve.
The invention has the beneficial effects as follows: be applicable under different temperatures and pressure condition, simulation oil field gas drive Produced Liquid is at well Emulsifying in cylinder and pipeline and conveying, also can simulate supercritical CO under the conditions of oil reservoir simultaneously2Viscosity reducing effect to crude oil.The present invention Described experimental facilities volume is little, and required experiment oil sample, water sample are few, and experimental facilities low cost can realize the sign of emulsion process, with And the real-time measurement of viscosity, it is possible to preferably simulate the emulsifying of dissolved gas crude oil and oil recovery, collect the viscosity B coefficent of defeated process.
Accompanying drawing explanation
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, the present invention is made into one The detailed description of step, wherein:
Fig. 1 is dissolved gas crude oil emulsifying with pressure provided by the present invention and surveys viscous integration apparatus schematic diagram.
Fig. 2 is the structural representation of agitating device of the present invention.
Detailed description of the invention
Below with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail, it will be appreciated that preferred embodiment Only for the explanation present invention rather than in order to limit the scope of the invention.
Embodiment 1: viscous integration apparatus is surveyed in one dissolved gas crude oil with pressure emulsifying as depicted in figs. 1 and 2, including: gas cylinder 1, annular coil pipe 2, piston type gas tank 3, manually-actuated metering pump 4, autoclave kettle 5, high speed stirrer motor 6, micro-range moment of torsion Measuring instrument 7, magnetic driver device 8, stirring paddle 9, annular disk pipe temperature-controlling system 10, piston type gas tank temperature-controlling system 11, reaction Still kettle temperature-controlling system 12, temperature sensor 13, pressure transducer 14, Pressure gauge 15, concentration digital display program control instrument 16, gas cylinder valve 17, gas tank air intake valve 18, gas tank pressure relief valve 19, gas tank are given vent to anger valve 20, reactor air intake valve 21, reactor air bleeding valve Door 22, sample cock 23, pump early gate 24, piston pressurization valve 25, conductivity meter 26, piston 27, torductor top connection Axial organ 28, torductor bottom 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 give vent to anger valve 20, Pump early gate 24, piston pressurization valve 25 and manually-actuated metering pump 4 constitute supply pressue device;Autoclave kettle 5, high pressure are anti- Still top cover 30, reactor air intake valve 21, reactor 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 bottom shaft coupling 29, magnetic driver device 8 and stirring Oar 9 forms agitating device;Temperature sensor 13, pressure transducer 14, micro-range torductor 7, concentration digital display program control instrument 16 Measurement apparatus is constituted with conductivity meter 26;Annular disk pipe temperature-controlling system 10, piston type gas tank temperature-controlling system 11 and reactor kettle Temperature-controlling system 12 constitutes temperature regulating device.
Described gas cylinder 1 through described annular coil pipe 2 be connected with described piston type gas tank 3, described piston type gas tank 3 respectively with Described manually-actuated metering pump 4 and described autoclave 5 connect, and described autoclave top cover 30 is connected to reactor air inlet respectively Valve 21, reactor drain tap 22, sample cock 23, temperature sensor 13, pressure transducer 14, conductivity meter 26, magnetic force Coupled drive device 8, described magnetic driver device 8 is connected with the shaft inside and outside still respectively, described micro-range torductor 7 Respectively by described torductor top shaft coupling 28, described torductor bottom shaft coupling 29 and described high-speed stirred electricity Machine 6 and described magnetic driver device 8 connect, described temperature sensor 13, described pressure transducer 14, described micro-range moment of torsion The measured value of measuring instrument 7 is shown by described concentration digital display program control instrument 16, and the rotating speed of described high speed stirrer motor 6 passes through described collection Middle digital display program control instrument 16 controls and shows, described annular disk pipe temperature-controlling system 10, piston type gas tank temperature-controlling system 11, reactor still Body temperature-controlling system 12 carries out temperature control to described annular coil pipe 2, described piston type gas tank 3, described autoclave 5 respectively.Described Annular disk pipe temperature-controlling system 10, piston type gas tank temperature-controlling system 11 and reactor kettle temperature-controlling system 12 are temperature control recirculated water Bath, in described annular disk pipe temperature-controlling system 10, coolant used is the mixture of water-ethanol=5 1, described piston type gas tank temperature control Heating agent used by system 11 and reactor kettle temperature-controlling system 12 is the mixture of water glycerol=6 1.
The design principle that can be seen that the present invention from the above is: utilize gas cylinder, piston type gas tank, manually-actuated metering pump and Autoclave realizes pressurization and the injection of gas, utilizes stirring motor to realize the emulsifying of dissolved gas crude oil and water, utilizes torquemeter With the measurement that viscosity-torque relationship realizes viscosity, utilize conductivity meter to realize the monitoring of emulsified state, so can solve molten gas former Oil emulsifying under elevated pressure conditions and the engineering problem that viscosity is measured in real time.
Before experiment starts, gas cylinder valve 17, gas tank air intake valve 18, gas tank pressure relief valve 19, gas tank is kept to give vent to anger valve 20, reactor air intake valve 21, reactor drain tap 22, sample cock 23, pump early gate 24, piston pressurization valve 25 are all located In closed mode.
Idling torque is excluded: utilize described concentration digital display program control instrument 16 to control described high speed stirrer motor 6, from rotating speed 50rpm starts, and increases with the interval of 50rpm, increases to 1200rpm always, at each rotating speed, records described micro-range and turns round The registration of square measuring instrument 7, this moment of torsion is the moment of torsion should excluded when each rotating speed surveys viscosity of mixed liquid.
The viscosity of experimental provision-moment of torsion is demarcated: selects Newtonian fluid known to 5 kinds of viscosity, is labeled as A, B, C, D, E, will Described autoclave top cover 30 is dismantled, and adds 300mL fluid A, by described reaction under high pressure in described autoclave kettle 5 Still top cover 30 is installed to described autoclave kettle 5 and seals, and utilizes described concentration digital display program control instrument 16 to control described high speed Stirring motor 6, from the beginning of rotating speed 50rpm, increases with the interval of 50rpm, increases to 400rpm always, at each rotating speed, Record the registration of described micro-range torductor 7, this moment of torsion registration is deducted described idling torque registration, obtain fluid A and exist The actual torque of each rotating speed, convection cell B, C, D, E carry out identical experiment step, obtain 5 kinds of fluids actual torque at each rotating speed, According to formula μ=aMb, fit within viscosity-torque relationship during variant rotating speed, obtain a, b value under different rotating speeds.
Filling crude oil and water: first dismantled by described autoclave top cover 30, add in described autoclave kettle 5 200mL crude oil and 100mL water, install described autoclave top cover 30 to described autoclave kettle 5 and seal, and utilizes Described reactor kettle temperature-controlling system 12 is heated to 60 DEG C to described autoclave kettle 5.
Gas pipeline purging: open gas cylinder valve 17, gas tank air intake valve 18, gas tank pressure relief valve 19, regulates gas tank relief valve The aperture of door 19, cleans described piston type gas tank 3, closes gas tank pressure relief valve 19, opens gas tank and gives vent to anger valve 20, anti- Answering still air intake valve 21, reactor drain tap 22, clean gas in described autoclave 5, orderly close-down reacts Still drain tap 22, reactor air intake valve 21, gas tank are given vent to anger valve 20, gas tank air intake valve 18, gas cylinder valve 17.
Gas pressurized: open pump early gate 24, piston pressurization valve 25, gas tank pressure relief valve 19, utilizes described manual meter Piston 27 in described 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, utilizes described manually-actuated metering pump 4 slowly to reduce the height of described piston type gas tank 3 inner carrier 27, real The filling of gas in existing described piston type gas tank 3, orderly close-down gas tank air intake valve 18 and gas cylinder valve 17, utilize described manually Gas boost in described piston type gas tank 3 to 10MPa, is utilized described piston type gas tank temperature-controlling system 11 to described by dosing pump 4 Piston type gas tank 3 is heated to 60 DEG C.
The filling of gas and emulsifying: open gas tank and give vent to anger valve 20, reactor air intake valve 21, utilize described manual metering Pump 4 is described piston 27 in lifting described piston type gas tank 3, and to described autoclave 5 gas injection to 10MPa, orderly close-down reacts Still air intake valve 21, gas tank are given vent to anger valve 20, utilize described concentration digital display program control instrument 16 control described high speed stirrer motor 6 with The stir speed (S.S.) of 1000r/min carries out emulsifying, institute in record whipping process to the dissolved gas crude oil in described autoclave 5 and water State the registration change of micro-range torductor 7 and described conductivity meter 26, after both registrations reach to stablize, close described high speed Stirring motor 6, slowly opens sample cock 23, by the emulsion taking-up 50mL in described autoclave 5 to color comparison tube, closes Close sample cock 23, by standing the stability observing emulsion.
Emulsion viscosity measurement: utilize described concentration digital display program control instrument 16 to control described high speed stirrer motor 6, from rotating speed 50rpm starts, and increases with the interval of 50rpm, increases to 400rpm always, at each rotating speed, records described micro-range and turns round The registration of square measuring instrument 7, deducts described idling torque registration by this moment of torsion registration, obtains the emulsion actual torsion at each rotating speed Square, according to formula μ=aMbAnd a, b value that each rotating speed obtains, calculate the viscosity of emulsion, then basis when different rotating speeds FormulaCalculate the shear rate that each viscosity is corresponding, draw viscosity-shear rate rheological curve.
It is measured, opens gas tank pressure relief valve 19, reactor drain tap 22, to described piston type, gas tank 3 and described Autoclave 5 carries out pressure release, dismantles described autoclave 5, utilizes petroleum ether to described autoclave 5 and institute State autoclave top cover 30 to be carried out, described autoclave top cover 30 is sealed with described autoclave 5, close institute There is valve.
Embodiment 2: before experiment starts, keeps gas cylinder valve 17, gas tank air intake valve 18, gas tank pressure relief valve 19, gas tank Give vent to anger valve 20, reactor air intake valve 21, reactor drain tap 22, sample cock 23, pump early gate 24, piston pressurization valve Door 25 is in closed mode.
Idling torque is excluded: utilize described concentration digital display program control instrument 16 to control described high speed stirrer motor 6, from rotating speed 50rpm starts, and increases with the interval of 50rpm, increases to 1200rpm always, at each rotating speed, records described micro-range and turns round The registration of square measuring instrument 7, this moment of torsion is the moment of torsion should excluded when each rotating speed surveys viscosity of mixed liquid.
The viscosity of experimental provision-moment of torsion is demarcated: selects Newtonian fluid known to 5 kinds of viscosity, is labeled as A, B, C, D, E, will Described autoclave top cover 30 is dismantled, and adds 300mL fluid A, by described reaction under high pressure in described autoclave kettle 5 Still top cover 30 is installed to described autoclave kettle 5 and seals, and utilizes described concentration digital display program control instrument 16 to control described high speed Stirring motor 6, from the beginning of rotating speed 50rpm, increases with the interval of 50rpm, increases to 400rpm always, at each rotating speed, Record the registration of described micro-range torductor 7, this moment of torsion registration is deducted described idling torque registration, obtain fluid A and exist The actual torque of each rotating speed, convection cell B, C, D, E carry out identical experiment step, obtain 5 kinds of fluids actual torque at each rotating speed, According to formula μ=aMb, fit within viscosity-torque relationship during variant rotating speed, obtain a, b value under different rotating speeds.
Crude oil fills: first dismantled by described autoclave top cover 30, adds in described autoclave kettle 5 300mL crude oil, installs described autoclave top cover 30 to described autoclave kettle 5 and seals, utilizing described reaction Still kettle temperature-controlling system 12 is heated to 80 DEG C to described autoclave kettle 5.
CO2Gas pipeline purging: open gas cylinder valve 17, gas tank air intake valve 18, gas tank pressure relief valve 19, regulates gas tank pressure release The aperture of valve 19, cleans described piston type gas tank 3, close gas tank pressure relief valve 19, open gas tank give vent to anger valve 20, Reactor air intake valve 21, reactor drain tap 22, clean gas in described autoclave 5, and orderly close-down is anti- Still drain tap 22, reactor air intake valve 21, gas tank is answered to give vent to anger valve 20, gas tank air intake valve 18, gas cylinder valve 17.
CO2Liquefaction: open gas tank pressure relief valve 19, pump early gate 24, piston pressurization valve 25, utilize described manual metering Described piston type gas tank 3 inner carrier is risen to gas tank top by pump 4, closes valve closing 19, utilizes described annular disk pipe temperature-controlling system 10 right Described annular coil pipe 2 refrigeration cool-down, to 0 DEG C, is opened gas cylinder valve 17, gas tank air intake valve 18, is utilized described manually-actuated metering pump 4 The slowly height of the piston in the described piston type gas tank 3 of reduction, it is achieved in described piston type gas tank 3, liquid carbon dioxide fills Note, orderly close-down valve 18 and valve 17.
Realize CO2Above-critical state: utilize described manually-actuated metering pump 4 to liquid carbon dioxide liter in described piston type gas tank 3 It is depressed into 25MPa, utilizes described piston type gas tank temperature-controlling system 11 described piston type gas tank 3 to be heated to 80 DEG C, by institute State manually-actuated metering pump 4 the pressure change in piston type gas tank described in temperature-rise period 3 is adjusted.
Supercritical CO2Filling with mix: open gas tank and give vent to anger valve 20, reactor air intake valve 21, utilize described hands Move described piston 27 in dosing pump 4 lifts described piston type gas tank 3, inject supercritical CO to described autoclave 52To pressure Reaching 25MPa, orderly close-down reactor air intake valve 21, gas tank are given vent to anger valve 20, utilize described concentration digital display program control instrument 16 to control Make the described high speed stirrer motor 6 stir speed (S.S.) with 180rpm to the crude oil in described autoclave 5 and supercritical CO2Carry out Mixing, the registration change of micro-range torductor 7 described in record whipping process, until registration reaches stable.
Molten supercritical CO2Measuring crude oil viscosity: utilize described concentration digital display program control instrument 16 to control described high speed stirrer motor 6, from the beginning of rotating speed 50rpm, increase with the interval of 50rpm, increase to 400rpm always, at each rotating speed, record is described The registration of micro-range torductor 7, deducts described idling torque registration by this moment of torsion registration, obtains emulsion at each rotating speed Actual torque, according to formula μ=aMbAnd each turn
A, b value that speed obtains, calculates the viscosity of emulsion when different rotating speeds, then according to formulaMeter Calculate the shear rate that each viscosity is corresponding, draw viscosity-shear rate rheological curve.
It is measured, opens gas tank pressure relief valve 19, reactor drain tap 22, to described piston type gas tank 3 and described Autoclave 5 carries out pressure release, dismantles described autoclave 5, utilizes petroleum ether to described autoclave 5 and institute State autoclave top cover 30 to be carried out, described autoclave top cover 30 is sealed with described autoclave 5, close institute There is valve.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, any skill being familiar with this specialty Art personnel in the range of without departing from technical scheme, when the technology contents of available the disclosure above make few modifications or Modify without departing from the spirit and scope of the present invention, as long as being the content without departing from technical solution of the present invention, according to the present invention's Technical spirit, to any simple modification made for any of the above embodiments, equivalent variations or modification, all still falls within technical solution of the present invention In the range of.

Claims (5)

1. a viscous integration apparatus is surveyed in dissolved gas crude oil emulsifying with pressure, including supply pressue device, high pressure reaction assembly, stirring dress Put, measurement apparatus and temperature regulating device, described supply pressue device include gas cylinder (1), annular coil pipe (2), piston type gas tank (3) and Manually-actuated metering pump (4);Described high pressure reaction assembly includes autoclave kettle (5), autoclave top cover (30);Described stir Mix device and include high speed stirrer motor (6), magnetic driver device (8) and stirring paddle (9);Described measurement apparatus includes that pressure passes Sensor (14), temperature sensor (13), micro-range torductor (7), conductivity meter (26) and concentration digital display program control instrument (16); Described temperature regulating device includes annular disk pipe temperature-controlling system (10), piston type gas tank temperature-controlling system (11) and reactor kettle temperature control system System (12), it is characterised in that: described high speed stirrer motor (6), described magnetic driver device (8) and described stirring paddle (9) phase Connect, it is achieved inject mixing and emulsifying, the institute of gas and the crude oil being previously added in described autoclave kettle (5) and water State micro-range torductor (7) by described torductor top shaft coupling (28) and described high speed stirrer motor (6) phase Connect, be connected with described magnetic driver device (8) by described torductor bottom shaft coupling (29), described electrical conductivity It is internal that instrument (26) stretches into described autoclave kettle (5) through described autoclave top cover (30).
2. according to the equipment described in claim 1, it is characterised in that: the rotating speed >=1500rpm of described high speed stirrer motor (6).
3. according to the equipment described in claim 1, it is characterised in that: described micro-range torductor (7) test torque range For: 0-300mN m, precision is 0.1mN m.
4. according to the equipment described in claim 1, it is characterised in that: described conductivity meter (26) is High Temperature High Pressure type electric conductivity Instrument, minimum resolution is 0.1 μ S/cm.
5. the method measuring dissolved gas crude oil viscosity with pressure, uses the dissolved gas crude oil emulsifying with pressure described in claim 1 to survey viscous Integration apparatus, it is characterised in that specifically include following steps:
Step 1. idling torque is excluded: be first not added with sample in described autoclave kettle (5), arranges described stirring paddle (9) and exists Different rotating speeds dallies, and utilizes described micro-range torductor (7) test idling torque now, it is thus achieved that idling torque and rotating speed Between quantitative relationship;This moment of torsion is the moment of torsion that consumes in transmission process of described magnetic driver device (8) and described high pressure The moment of torsion sum that reactor kettle (5) interior air drag produces, needs to exclude during subsequent experimental;
The viscosity of step 2. device-moment of torsion is demarcated: selects Newtonian fluid known to 5 kinds of viscosity, is labeled as A, B, C, D, E, by institute State autoclave top cover (30) dismounting, in described autoclave kettle (5), add 300mL fluid A, by anti-for described high pressure Answer still top cover (30) install to described autoclave kettle (5) and seal, utilize described concentration digital display program control instrument (16) to control Described high speed stirrer motor (6), from the beginning of rotating speed 50rpm, increases with the interval of 50rpm, increases to 400rpm, each always At individual rotating speed, record the registration of described micro-range torductor (7), this moment of torsion registration deducted described idling torque registration, Obtaining the fluid A actual torque at each rotating speed, convection cell B, C, D, E carry out identical experiment step, obtain 5 kinds of fluids at each rotating speed Actual torque, according to formula μ=aMb, fit within viscosity-torque relationship during variant rotating speed, obtain under different rotating speeds A, b value;
Step 3. testing liquid fills: first described autoclave top cover (30) dismantled, to described autoclave kettle (5) Interior addition 300mL testing liquid, installs described autoclave top cover (30) to described autoclave kettle (5) close Envelope, utilizes described reactor kettle temperature-controlling system (12) to described autoclave kettle (5) temperature control;
Step 4. testing liquid viscosity measurement: utilize described concentration digital display program control instrument (16) to control described high speed stirrer motor (6), From the beginning of rotating speed 50rpm, increase with the interval of 50rpm, increase to 400rpm always, at each rotating speed, record described micro- The registration of range torductor (7), deducts described idling torque registration by this moment of torsion registration, obtains the liquid reality at each rotating speed Border moment of torsion, according to formula μ=aMbAnd a, b value that each rotating speed obtains, calculate the viscosity of emulsion when different rotating speeds, then According to formulaCalculate the shear rate that each viscosity is corresponding, draw viscosity-shear rate rheological curve.
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