CN106290045A - Unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental method - Google Patents

Unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental method Download PDF

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CN106290045A
CN106290045A CN201610757406.3A CN201610757406A CN106290045A CN 106290045 A CN106290045 A CN 106290045A CN 201610757406 A CN201610757406 A CN 201610757406A CN 106290045 A CN106290045 A CN 106290045A
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oil
valve
unconventional
temperature
tight sand
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CN106290045B (en
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张居和
冯子辉
霍秋立
迟焕远
李景坤
张琨
王淑芝
郭伟
王雪
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Petrochina Co Ltd
Daqing Oilfield Co Ltd
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Daqing Oilfield Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; viscous liquids; paints; inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids
    • G01N33/2823—Oils, i.e. hydrocarbon liquids raw oil, drilling fluid or polyphasic mixtures
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N2030/009—Extraction

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Abstract

The invention discloses a kind of unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental method, the method uses the method for pressure maintaining sealed coring to be evaluated the performance that unconventional Sandstone Gas Reservoir different existence state is oily, solves unconventionaloil pool exploration Sandstone Gas Reservoir free oil and absorption oil mensuration and oiliness and mobility evaluates difficult problem.Reservoir rock will make free oil scatter and disappear because of blood pressure lowering degassing especially long-term placement, free oil test result can simulate underground situation, having accomplished the objective evaluation of tight sand oiliness and mobility and production capacity, the present invention is effectively the employing of unconventional Sandstone Gas Reservoir different existence state oil, reserves and exploration and development provide new laboratory facilities and foundation.

Description

Unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental method
Technical field
The present invention relates to unconventionaloil pool geological analysis experimental technique, be specifically related to a kind of unconventional Sandstone Gas Reservoir and contain Oiliness and mobility evaluation experimental method, belong to unconventionaloil pool Exploration Domain.
Background technology
In recent years, the unconventional petroleum resources such as fine and close oil gas, shale gas, heavy oil and oil-sand realizes scale development, promotes complete Ball petroleum industry enters the conventional new stage laid equal stress on unconventional petroleum resources.China's densification oil gas makes substantial progress, and sends out Having showed league (unit of length) tight gas district of Ordos Basin Soviet Union, Song-liao basin northern high estrade and Fuyu County's densification oil reservoir etc., fine and close oil gas is Become the unconventional petroleum resources of presently the most reality, become important making & breaking.
Fine and close oil gas refers to be clipped in or be close in the compact reservoir of hydrocarbon source rock series of strata, without extensive long-distance migration The oil-gas accumulation formed；Mud shale oil refers to compose that to be stored in rich organic, nano aperture be the oil in main mud shale stratum, is into The abbreviation of ripe organic mud shale oil；Fine and close and mud shale is oily general without natural production capacity, need to through massive hydraulic fracture technology Industry production capacity can be formed.Fine and close and mud shale oil resource abundance generally is low, reservoir poor quality, anisotropism are strong.
Since 2011, it is non-that Daqing oil field has carried out tight sand oil, tight sandy gravel gas, coal bed gas and mud shale oil etc. Conventional gas and oil exploration and on-site development test, obtain the important breakthrough of tight sand exploration activity, SS9H well in QP2, YP1 wellblock etc. Shahe subgroup realizes the breakthrough of tight sandy gravel gas reservoir industry production capacity first, illustrates tight sand oil, tight sandy gravel gas The great potential of exploration and good prospect.Unconventional tight sand oil is mainly (immovable with free oil (moveable oil) and absorption oil Oil) existence of both occurrence status, wherein free oil (moveable oil) refers to can flow in compact reservoir under existing DP technology Dynamic and can from oil reservoir the part oil of output, absorption oil (non-movable oil) refers under existing DP technology in compact reservoir not Flowing and can not from oil reservoir output part oil.Sandstone Gas Reservoir different existence state oil can be divided into I class and II class, and I The oiliness of class is mainly oil immersion, and the oiliness of II class includes oil immersion, oil mark, oil stain etc., dissociating of every class Sandstone Gas Reservoir Oil content is different with absorption oil content and oiliness, gets free oil and absorption oil in Sandstone Gas Reservoir clear and is distributed and feature, right Tight sand oilreserves, effectively the exploration and development such as to employ significant.
At present, unconventionaloil pool conventional survey sampling technique is general it cannot be guaranteed that the initial condition of underground rock core, especially The long-term rock core placed, owing to departing from underground primal environment and pressure declines and makes free oil scatter and disappear, therefore, it is thus achieved that experiment test Result cannot embody the real conditions of subsurface reservoir free oil content.
Although having the evaluation experimental methods such as document report reservoir moveable gel, free hydrocarbon, such as (1) Zhou Shangwen, Xue Hua Qing, Guo Wei " Jurassic system densification oil reservoir movable fluid experiment in river " (Liaoning Project Technology University's journal (natural science edition), 6th phase in 2014), wherein application nuclear magnetic resonance technique carries out movable fluid test to fine and close oil reservoir rock sample, it is thus achieved that fine and close oil Reservoir moveable gel；(2) " NMR logging technique is in western slope Saar oil reservoir group for Ke Qingming Application " (well logging engineering, the 4th phase in 2013), be application NMR logging technique obtain porosity of sandstones, permeability, The parameter such as initial oil saturation, mobile oil saturation；(3) Wang Min " key parameter and acquiring method that shale oil is evaluated are studied " (deposition journal, the 1st phase in 2014), the core analysis data such as porosity, oil saturation is utilized to be deduced reflection shale page The evaluation model of rock free hydrocarbon content, by free hydrocarbon organic carbon content absolute value, and organic carbon content and ground in free hydrocarbon The ratio of layer organic carbon content achieves the instruction etc. to shale oil stratum movable hydrocarbon abundance zone.But, these methods are the most not Free oil and absorption oil quantitative simulation and the problem of test in tight sand can be solved.
Summary of the invention
The invention aims to solve free oil and absorption oil quantitative simulation and test problem in tight sand, it is provided that A kind of unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental method, comprise the steps of
1) rock core drilling through unconventional Sandstone Gas Reservoir makees core column sample, after core column sample washing oil, often measures Rule ground porosity and permeability；
2) by step 1) core column sample after washing oil, after scales/electronic balance weighing, obtain core column quality mThe heart, then to Wherein irrigate saturated normal saline solution, obtain saturated normal saline solution core column sample；
3) by step 2) the saturated normal saline solution core column sample that obtains is real by unconventional tight sand oil quantitative simulation Test the preparation method of sample, obtain unconventional tight sand oil Quantitative simulation experiment sample；
4) by step 3) the unconventional tight sand oil Quantitative simulation experiment sample that obtains, by free Oil and gas displacement test side Method measures and obtains tight sand and dissociate oil mass (mTrip, mg)；
5) by step 4) weigh after tight sand oil simulation experiment sample comminution after the free oil mass of test, obtain rock matter Amount mStone, recycle unconventional tight sand oil quantitative simulation and experimental apparatus for testing, measure by absorption oil extraction method of testing Oil mass (m is adsorbed to tight sandInhale, mg)；
6) by step 4) and 5) tight sand that obtains dissociates oil mass (mg) and absorption oil mass (mg), calculate and obtain fine and close sand Rock different existence state oil evaluating free oil content (mg/g), absorption oil content (mg/g), oil content (mg/g), trip From oil rate (%), absorption oil rate (%)；Free oil content (mg/g) and free oil rate (%) is the biggest, absorption oil content (mg/g) and Absorption oil rate (%) the least explanation unconventional tight sand oil mobility is the best, i.e. oil recoverable is the biggest；Free oil content (mg/ G), absorption oil content (mg/g) the least with free oil rate (%) and absorption oil rate (%) the biggest explanation unconventional tight sand oil can Dynamic property is the poorest, i.e. oil recoverable is the least；Oil content (mg/g) the biggest explanation unconventional Sandstone Gas Reservoir oiliness is the best, i.e. contains Oil mass is the highest, and the least explanation of oil content unconventional Sandstone Gas Reservoir oiliness is the poorest, i.e. oil content is the lowest.
Step 4) described free Oil and gas displacement method of testing is:
Slowly open unconventional tight sand oil quantitative simulation and the gas source valve of experimental apparatus for testing, use carbon dioxide gas Crude oil in pipeline is blown clean by body；Open the turnover valve holding gas piston container, select constant current or constant voltage mode, input Flow or force value, flow is usually set to 2～10mL/min, and pressure is set smaller than this unconventional tight sand oil quantitatively mould The fracture pressure of draft experiment sample, displacement, until the weight of the metrology devices port of export is not further added by, obtains tight sand free oil Amount (mg).
Step 5) described absorption oil extraction method of testing be:
Tight sand oil simulation experiment sample after pulverizing being weighed puts into unconventional tight sand oil quantitative simulation and survey In the extraction kettle of examination experimental provision, open heater switch and the temperature control of carbon dioxide air source, condenser parts, extraction kettle and separating still Instrument；When condenser parts reaches cryogenic temperature-5 DEG C, open gas source valve and make CO2Sequentially enter filter, condenser parts, gas storage Tank, high-pressure pump and/or carry agent pump, depurator and blender, finally enter extraction kettle, regulation extraction kettle and the pressure of separating still It is respectively 20MPa, 10MPa and 50 DEG C, 40 DEG C with temperature；When oil mass is not further added by, recording quality, it is tight sand absorption Oil mass；
Described free oil content (mg/g)=mTrip/mThe heart, absorption oil content (mg/g)=mInhale/mStone, oil content (mg/g)=trip From oil content (mg/g)+absorption oil content (mg/g), free oil rate (%)=free oil content (mg/g)/oil content (mg/g) × 100%, absorption oil rate (%)=absorption oil content (mg/g)/oil content (mg/g) × 100%.
Step 3) manufacture method of unconventional tight sand oil Quantitative simulation experiment sample, use unconventional tight sand oil Quantitative simulation and experimental apparatus for testing carry out the making of saturated core post sample, and described experimental provision includes clamper (1), temperature control Case (2), confined pressure pump (30), backpressure pump (33), displacement pump (34), vacuum pump (35), computer control part (31), piston container (21C, 21D, 22C, 22D) and multiple valve,
Described manufacture method is characterised by, comprises the following steps:
Step one: stainless steel column is loaded in the lead set (13) of clamper (1), and clamper (1) is put into temperature-controlled box (2) In, connect arrival end channel valve (1A) and waste liquid valve (3A), outlet end passageways valve (2A) and the valve of clamper (1) (29A) with confined pressure interface (18), open temperature-controlled box (2) and the power supply of computer control part (31), set the temperature of temperature-controlled box (2) Degree carrys out simulated formation temperature, and the design temperature the constant temperature that are heated to temperature-controlled box (2) are no less than 3h；
Open confined pressure valve (30A), start confined pressure pump (30), set confined pressure value 70MPa, constant 2h after reaching setting value； Open vacuum-pumping valve (35A), arrival end channel valve (1A), start vacuum pump (35) evacuation 20min, close valve (35A), vacuum pump (34), open valve (11A, 12A) or valve that the piston container (21C or 21D) equipped with crude oil is imported and exported Door (13A, 14A), valve (29A, 33A), start displacement pump (34), backpressure pump (33), sets and injects flow and back pressure value；
Under the control of displacement pump (34), backpressure pump (33), confined pressure pump (30) and computer control part (31), to clamping Device (1) injects crude oil, records a certain injection pressure i.e. displacement pressure PiThe crude oil volume of the most full arrival end pipelineIf it is real Test and need to obtain displacement pressure PiValue is more than 67MPa'sMore than injection pressure 2MPa can be higher than by setting confined pressure value or setting is enclosed Press pump (30) is automatic tracing mode；Repeat said process, use standardizition, record different pressures point PiCorresponding full pipe Road crude oil volumeExperimental provision as described in the orderly close-down contrary with beginning；
Step 2: core column sample is loaded in the lead set (13) of clamper (1), and clamper (1) is put into temperature-controlled box (2) in, connect the arrival end channel valve (1A) of clamper (1) and waste liquid valve (3A), outlet end passageways valve (2A) and Valve (29A), confined pressure interface (18), open temperature-controlled box (2) and the power supply of computer control part (31), sets temperature-controlled box (2) Temperature carry out simulated formation temperature, be heated to the design temperature of temperature-controlled box (2) constant temperature no less than 3h；
Step 3: open confined pressure valve (30A), starts confined pressure pump (30), sets confined pressure value 70MPa, after reaching setting value Constant no less than 1h；Open vacuum-pumping valve (35A), arrival end channel valve (1A), start vacuum pump (35) evacuation many In 20min, close valve (35A), vacuum pump (34)；
Step 4: open valve (11A, 12A) or valve that the piston container (21C or 21D) equipped with crude oil is imported and exported (13A, 14A), valve (29A, 33A), start displacement pump (34), sets displacement flow, fracture pressure, injection crude oil volume parameter Deng；Start backpressure pump (33), set back pressure value；Starting and inject crude oil, record injects crude oil amountStep one is utilized to obtain It is full of passage crude oil amountWith injection crude oil amountObtain the saturated crude oil amount of realityI.e.Calculate Machine controller part 31 monitors automaticallyWhenDuring equal to the injection crude oil volume set, computer control part 31 automatically controls Stop injecting crude oil, obtain unconventional tight sand oil Quantitative simulation experiment sample.
Described unconventional tight sand oil quantitative simulation and experimental apparatus for testing mainly include tight sand oil quantitative simulation And free oil displacement portion and carbon dioxide supercritical fluid extraction adsorb oil test department, it is provided with one between two parts and can make both Connection or the intake valve of isolation；
Free oil displacement portion includes the model module for simulating oil reservoir, injects crude oil and displacing medium to model module Injection module, effluent to model module are acquired and the effluent acquisition testing module that detects and to model module Temperature, pressure carry out the detection control module that detection controls.
Described model module includes the clamper being placed in temperature-controlled box, and described clamper includes:
Base (11)；
The holder body (12) being fixed on base (11)；
It is placed in the lead set (13) that holder body (12) is internal；
It is installed on the sealing lid (14) at lead set (13) two ends；
It is arranged in and seals the inside and outside inner seal ring of lid (14) and exterior seal ring；
It is fixed on the end cap (16) at holder body (12) two ends；
At two push rods (17) threadeded with end cap (16) in holder body (12) end；
Push rod outwardly directed one end in one end is provided with the first arrival end passage that be connected internal with holder body (12) (19) and the second arrival end passage (110), outwardly directed one end of push rod of the other end is provided with phase internal with holder body (12) First outlet end passageways (111) of connection and the second outlet end passageways (112)；Holder body (12) is provided with confined pressure interface (18), it is used for connecting confined pressure pump (30) to control the work confined pressure within clamper；First arrival end passage 19 passes through entrance End channel valve (1A) is connected with injection module, intake valve (4A)；First outlet end passageways (111) passes through outlet end passageways valve (2A) it is connected with injection module, intake valve (4A)；Second arrival end passage (110) is connected with waste liquid valve (3A), the second outlet End passage (112) is connected with effluent acquisition testing module by valve (29A).
Described carbon dioxide supercritical fluid extraction absorption oil test department includes carbon dioxide supply and processing module, supercritical two Carbonoxide extraction absorption oil module and Oil-gas Separation module, wherein:
Carbon dioxide supply and processing module include carbon dioxide air source (36) and gas source valve (36A) and under its place Trip passage on be sequentially connected in series in filtering carbon dioxide the filter (37) of impurity, be used for measuring carbon dioxide Amount effusion meter (38), Filter valve (37A), for the condenser system (39) of cooled carbon dioxide gas, for storage two The air accumulator (40) of carbonoxide, for compressing the high-pressure pump (41) of carbon dioxide and carrying agent pump (42), be used for purifying titanium dioxide The depurator (43) of carbon and blender (44).
Described supercritical carbon dioxide extraction absorption oil module includes extraction kettle (45) and the extraction kettle (46) being connected in parallel, The two ends of extraction kettle (45,46) respectively connect a valve, temperature controller, heater element and pressure transducer；
Oil-gas Separation module include the separating still (47) that is sequentially connected in series on the downstream passage that valve (19A) is connected and Separating still (48), is connected by valve (10A) therebetween；
Carbon dioxide supply and processing module are connected to supercritical carbon dioxide extraction absorption oil module by valve (5A), Supercritical carbon dioxide extraction absorption oil module is connected to Oil-gas Separation module by valve (19A)；
Supercritical carbon dioxide extraction absorption oil module is connected to carbon dioxide by valve (8A) and supplies and processing module Gas source valve (36A), Oil-gas Separation module by valve (9A) connecting valve (8A) and gas source valve (36A) formation loop； The supply of described carbon dioxide and processing module and supercritical carbon dioxide extraction absorption oil module are connected by valve (4A) respectively To tight sand oil quantitative simulation and free oil displacement portion thereof.
Described unconventional Sandstone Gas Reservoir refers to packsand, siltstone, shale or containing mud or calcic or considers flour sand to be worth doing containing being situated between The reservoir of rock.
The present invention passes through simulated formation temperature and pressure and irreducible water condition, the most with this understanding to unconventional fine and close sand The performance of rock oil different existence state oil is measured and evaluates, and solves unconventionaloil pool exploration Sandstone Gas Reservoir free oil Mensuration oily with absorption and oiliness and mobility evaluate difficult problem, and free oil test result can reflect underground situation, accomplish Tight sand oiliness and the objective evaluation of mobility, the present invention be effectively the employing of unconventional tight sand oil, reserves and Exploration and development provides new laboratory facilities and foundation.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the used device of the inventive method；
Fig. 2 is the structural representation of clamper；
Fig. 3 is quantitative simulation I class oil immersion tight sand free oil and permeability graph of a relation；
Fig. 4 is quantitative simulation I class oil immersion tight sand free oil and porosity graph of a relation.
In figure, reference is expressed as:
1: clamper, 11: base, 12: holder body, 13: lead set, 14: seal and cover, 15: inner seal ring, 15 ': external seal Circle, 16: end cap, 17: push rod, 18: confined pressure interface, 19: the first arrival end passages, 110: the second arrival end passages, 1A: arrival end Channel valve, 111: the first outlet end passageways, 112: the second outlet end passageways, 2A: outlet end passageways valve；
2: temperature-controlled box；
29: back-pressure valve, 30: confined pressure pump, 30A: confined pressure valve；31: computer control part, 32: metrology devices, 33: return Press pump, 34: displacement pump (ISCO pump), 35: vacuum pump, 35A: vacuum-pumping valve；36: carbon dioxide air source, 36A: gas source valve； 37: filter, 37A: Filter valve；38: effusion meter, 39: condenser parts, 40: air accumulator, 41: high-pressure pump, 42: carry agent Pump, 43: depurator, 44: blender, 45,46: extraction kettle, 45A, 46A: extraction kettle valve；47,48: separating still, 47A, 48A: Separating still valve；
3A: waste liquid valve；4A: intake valve；5A、6A、7A、8A、9A、10A、11A、12A、13A、14A、15A、16A、17A、 18A, 19A, 29A, 33A: valve；
21C, 21D, 22C, 22D: piston container；
1B, 2B, 3B, 4B, 5B, 40B, 45B, 46B, 47B, 48B: pressure transducer；
100: core holding unit, 101: confined pressure force (forcing) pump, 102: back pressure controller part, 103: discrete device, 104: dioxy Change carbon refrigeration device, 105: carbon dioxide conveying and carry agent hybrid device, 106: profit injection device, 107: apparatus for vacuum producing Part, 108: heater.
Detailed description of the invention
The present invention proposes unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental method, its mainly by Different oiliness tight sand samples are detected by Quantitative simulation experiment technology, are included in airtight, vacuum, formation temperature, pressure Measure, for method of testing, the evaluating that free oil is relevant by gas drive under the conditions of power, irreducible water, use supercritical extraction test side Method measures the evaluating that absorption oil phase closes, and reaches the purpose evaluating unconventional reservoir oiliness and mobility, meets very The rule oil-gas exploration and development demand to geological experiment.The experimental technique of the present invention is composed for unconventional Sandstone Gas Reservoir difference and is deposited The performance parameter of state oil includes free oil content (mg/g), absorption oil content (mg/g), oil content (mg/g), free oil rate (%), absorption oil rate (%) etc. be measured and calculate, recycle these parameters to unconventional Sandstone Gas Reservoir oiliness and Mobility is evaluated.
The present invention is described in detail below from several respects.
One, unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental method
The present invention unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental method complete in the steps below:
1) rock core drilling through unconventional Sandstone Gas Reservoir makees core column sample, after core column sample washing oil, often measures Rule ground porosity and permeability；
2) by step 1) measure the core column sample of face porosity and permeability routinely, after scales/electronic balance weighing, Obtain core column quality mThe heart, (formula of saturated normal saline solution is: NaCl in mass ratio to irrigate saturated normal saline solution wherein CaCl2MgCl2·6H2The saturated sodium-chloride water solution that O=7 0.6 0.4 obtains), obtain saturated normal saline solution core column sample Product；
3) by step 2) the saturated normal saline solution core column sample that obtains loads in clamper, places into unconventional fine and close sand In rock oil quantitative simulation and experimental apparatus for testing, carry out the preparation method of unconventional tight sand oil Quantitative simulation experiment sample, Obtain unconventional tight sand oil Quantitative simulation experiment sample；
4) by step 3) the unconventional tight sand oil Quantitative simulation experiment sample that obtains, by free Oil and gas displacement test side Method measures and obtains tight sand and dissociate oil mass (mTrip, mg)；
5) by step 4) weigh after tight sand oil simulation experiment sample comminution after the free oil mass of test, obtain rock matter Amount mStone, recycle unconventional tight sand oil quantitative simulation and experimental apparatus for testing, measure by absorption oil extraction method of testing Oil mass (m is adsorbed to tight sandInhale, mg)；
6) by step 4) and 5) tight sand that obtains dissociates oil mass (mg) and absorption oil mass (mg), calculate and obtain fine and close sand Rock different existence state oil evaluating free oil content (mg/g), absorption oil content (mg/g), oil content (mg/g), trip From oil rate (%), absorption oil rate (%)；The calculating process of above evaluating is: free oil content (mg/g)=mTrip/mThe heart, absorption Oil content (mg/g)=mInhale/mStone, oil content (mg/g)=free oil content (mg/g)+absorption oil content (mg/g), free oil rate (%)=free oil content (mg/g)/oil content (mg/g) × 100%, absorption oil rate (%)=absorption oil content (mg/g)/contain Oil mass (mg/g) × 100%；Free oil content (mg/g) and free oil rate (%) is the biggest, absorption oil content (mg/g) and absorption oily Rate (%) the least explanation unconventional tight sand oil mobility is the best, i.e. oil recoverable is the biggest；Free oil content (mg/g) and trip From oily rate (%), the least, absorption oil content (mg/g) and absorption oil rate (%) the biggest explanation unconventional tight sand oil mobility are more Difference, i.e. oil recoverable is the least；Oil content (mg/g) the biggest explanation unconventional Sandstone Gas Reservoir oiliness is the best, and i.e. oil content is more Height, the least explanation of oil content unconventional Sandstone Gas Reservoir oiliness is the poorest, i.e. oil content is the lowest.
Step 1) sampling principle be to take the different classification reservoir samples without well section, I class reservoir porosity 8%～ 12%, permeability 0.1～1mD, II class reservoir porosity 5%～8%, permeability 0.03～0.1mD, the II following reservoir pore space of class Degree ＜ 5%, permeability ＜ 0.03mD；By sample sent by requirement or according to research need sampling.
The inventive method step 3) and step 5) used in apparatus structure example with reference to Fig. 1, this device is unconventional Tight sand oil quantitative simulation and experimental apparatus for testing, this device mainly includes two parts, i.e. tight sand oil quantitative simulation And free oil displacement portion (the free oil displacement portion W in Fig. 1) and carbon dioxide supercritical fluid extraction absorption oil test department (absorption oil Test department U), it is provided with an intake valve 4A between two parts, is opened or closed by operation intake valve 4A, make free oil displacement Portion W can connect or isolate with absorption oil test department U, and the two can either be used alone, it is also possible to is applied in combination.
Free oil displacement portion W includes the model module for simulating oil reservoir, injects crude oil and displacing medium to model module Injection module, the effluent of model module is acquired and the effluent acquisition testing module that detects and to model module Temperature, pressure carry out detection control detection control module, wherein:
Model module in the present embodiment includes clamper 1, and in order to ensure that clamper 1 operating temperature is stable, clamper 1 is put It is placed in temperature-controlled box 2, as in figure 2 it is shown, clamper 1 is provided with base 11 and the holder body 12 being fixed on base 11, clamping Body 12 is internally provided with a lead set 13, is used for placing core column；Two seal lid 14 and are respectively arranged in the two ends of lead set 13, close Cover 14 inside and outside inner seal ring 15 and the exterior seal rings 15 ' of being respectively disposed with to prevent liquid from sealing leakage at lid 14； Two end caps 16 are respectively arranged in the two ends of holder body 12, and push rod 17 is threadedly connected in end cap 16 screwed hole, a push rod 17 Outwardly directed one end is provided with first arrival end passage 19 and the second arrival end passage that be connected internal with holder body 12 110, outwardly directed one end of push rod 17 of the other end is provided with first outlet end passageways 111 that be connected internal with holder body 12 With the second outlet end passageways 112；Holder body 12 is provided with confined pressure interface 18, is used for connecting confined pressure pump 30 to control clamper The confined pressure of 1.First arrival end passage 19 is connected with injection module, intake valve 4A by arrival end channel valve 1A, it is provided that Xiang Xiang Clamper 1 injects oil or the passage of gas；First outlet end passageways 111 by outlet end passageways valve 2A and injection module, enter Air valve 4A is connected.The purpose that first arrival end passage 19 is connected with intake valve 4A with the first outlet end passageways 111 is, free The front opening intake valve 4A of oil quantitative test and arrival end channel valve 1A, waist valve 3A, by arrival end channel valve 1A, waste liquid Crude oil gas blow-out in valve 3A, the first arrival end passage 19 and the second arrival end passage 110, in order to avoid affecting follow-up test trip From oil quantitative.Second arrival end passage 110 is connected with waste liquid valve 3A, and the second outlet end passageways 112 is by valve 29A and stream Go out liquid acquisition testing module to be connected.
Temperature-controlled box 2 is additionally provided with and extracts the survey mouth controlling temperature and pressure signal for detection control module.In the present embodiment Detection control module includes for detecting the temperature device and pressure sensing devices controlling temperature, wherein, temperature detection device bag Include the temperature sensor of clamper 1 relevant position temperature signal and meter is changed, shows and be transported to temperature sensor signal Calculating the testing circuit of machine controller part 31, temperature detection device belongs to prior art, is not drawn in fig. 1 and 2.
Pressure transducer 1B, 2B, 3B, 4B that pressure sensing devices includes gathering clamper 1 relevant position pressure signal and The testing circuit of computer control part 31, detection are changed, shown and be transported to 5B and the signal obtained by pressure transducer Circuit and pressure transducer 1B, 2B, 3B, 4B and 5B broadly fall into prior art, and the present embodiment is carrying out tight sand oil quantitatively mould When draft experiment and displacement test experiments, owing to rock core densification permeability is low, before rock core in after different parts pressure oscillation big, use Multiple different parts, pressure transducer 1B, 2B, 3B, 4B and 5B parallel connection detection of different range, it is ensured that different measuring point pressure Measurement and precision.
Injection module in the present embodiment includes for corresponding crude oil, the displacement pump of displacing medium offer displacement pressure (ISCO pump) 34 and accommodate piston container 21C and 21D, 22C and 22D of corresponding crude oil and displacing medium respectively.As shown in Figure 1 Piston container 21C and 21D in the embodiment of the present invention, 22C and 22D are positioned in temperature-controlled box 2, to ensure to enter in clamper 1 Crude oil or displacing medium are maintained at predetermined temperature；Four groups of piston containers are connected in parallel, and often the two ends of group piston container are gone here and there respectively Joining a valve, for controlling order of work and the duty of four groups of piston containers, i.e. four groups piston containers can make simultaneously With, be used alone or any be applied in combination；Piston one end is connected to clamper by valve 11A, 13A, 15A, 17A respectively The arrival end channel valve 1A of 1 arrival end, air intake valve 4A, the other end is connected to by valve 12A, 14A, 16A, 18A respectively Displacement pump 34.
Vacuum pump 35 is connected to the arrival end channel valve 1A of clamper 1 arrival end by vacuum-pumping valve 35A, for mould Before intending tight sand oil samples, air in model module is taken away, be conducive to injecting crude oil and preventing pressure oscillation.
Confined pressure pump 30 is connected on the confined pressure interface 18 of clamper 1 by confined pressure valve 30A, is used for regulating in clamper 1 The work confined pressure in portion, its effect is mainly: one is to add enough pressure to the rock core in lead set 13 and lead set 13, makes lead overlap 13 Hes Between rock core seamless, it is ensured that inject crude oil time enter rock core, it is to avoid crude oil from lead set 13 and rock core gap enter flow out Liquid acquisition testing module, affects crude oil injection rate, makes fine and close oil mass experiment inaccurate；Two is that confined pressure pump 30 has from motion tracking tune Whole function (selects the automatic tracing mode of confined pressure), remains that confined pressure is higher than more than injection pressure 2MPa (also in experimentation Constant voltage mode can be selected, set one higher than confined pressure more than maximum injection pressure 2MPa), confined pressure pressure oscillation≤ 0.1Mpa, it is ensured that clamper and operation safety.
Effluent acquisition testing module in the present embodiment includes gauge assembly 32, in free oil test experiments, from folder The liquid that second outlet end passageways 112 of holder 1 flows out flows in gauge assembly 32 through valve 29A and back-pressure valve 29, carries out Metering.Backpressure pump 33 is connected with back-pressure valve 29 by valve 33A, and the effect of backpressure pump 33 and back-pressure valve 29 is simulated formation hydrostatic Column pressure, the general back pressure of sample (stratum liquid column hydrostatic pressure) of identical well depth is identical, input back pressure value, experiment when experiment Process need not regulation, and backpressure pump is from motion tracking；When changing the sample of another block difference well depth, need to input another back pressure value, After setting in experimentation backpressure pump from motion tracking, back pressure pressure oscillation≤0.1Mpa.
Detection control module computer control part 31 respectively with confined pressure pump 30, metrology devices 32 and backpressure pump 33, drive Being connected for pump 34, for automatically controlling the work of above-mentioned each parts, the most above-mentioned each parts can also control the most voluntarily.Calculate Machine controller part 31 is provided with operation interface, it arranges various operation buttons, can operate startup and the end of this device, also may be used With setting device mode of operation, confined pressure value, experimental temperature value and various setup parameter (such as, fracture pressure, flow velocity, saturated Volume, saturation pressure etc.).
Absorption oil test department U includes carbon dioxide supply and processing module, supercritical carbon dioxide extraction absorption oil module With Oil-gas Separation module, wherein:
Carbon dioxide supply and processing module are for obtaining pure supercritical carbon dioxide, including carbon dioxide gas Source 36 and gas source valve 36A and the filter 37 of connected impurity in filtering carbon dioxide, it is used for measuring carbon dioxide gas The effusion meter 38 of the scale of construction, Filter valve 37A, for cooled carbon dioxide gas condenser parts 39, be used for storing titanium dioxide The air accumulator 40 of carbon, for compressing the high-pressure pump 41 of carbon dioxide and carrying agent pump 42, for purifying the depurator of carbon dioxide 43 and blender 44, air accumulator 40 is provided with the pressure transducer 40B for measuring air accumulator 40 pressure, and blender 44 will be for will Carbon dioxide and carry the i.e. chemical reagent mix homogeneously of agent and obtain supercritical carbon dioxide, it is connected to supercritical by valve 5A Carbon dioxide abstraction absorption oil module, is connected to tight sand oil quantitative simulation and free oil displacement portion thereof by intake valve 4A.
Supercritical carbon dioxide extraction absorption oil module includes extraction kettle 45 and the extraction kettle 46 being connected in parallel, extraction kettle 45 Two ends respectively connect a valve (extraction kettle valve 45A and valve 6A), the two ends of same extraction kettle 46 respectively connect a valve (extraction Take still valve 46A and valve 7A), extraction kettle 45,46 is respectively provided with temperature controller and heater element, and be provided with pressure transducer 45B, 46B, for measuring the pressure in extraction kettle 45,46；Clamper 1 institute in tight sand oil quantitative simulation and free oil displacement portion thereof Put into after the core column sample comminution generated in extraction kettle 45 or 46 and seal, after carbon dioxide enters extraction kettle 45 or 46, according to Temperature controller predetermined temperature heating extraction kettle 45 or 46, carries out supercritical carbon dioxide extraction.Supercritical carbon dioxide extracts Take absorption oil module and be connected to carbon dioxide supply and the gas source valve 36A of processing module by valve 8A, can be by titanium dioxide Carbon returns and re-uses；Supercritical carbon dioxide extraction absorption oil module is connected to Oil-gas Separation module by valve 19A, carries out Next step Oil-gas Separation operation.
Oil-gas Separation module includes the separating still 47 being sequentially connected in series on the downstream passage that valve 19A is connected and separates Still 48, is connected by valve 10A therebetween, and separating still 47 is connected to separating still valve 47A and pressure transducer 47B, Same separating still 48 is connected to separating still valve 48A and pressure transducer 48B.Can by control valve 19A, 10A and 9A Controlling the pressure of separating still 47,48, the upper pressure limit of separating still 47,48 is 30MPa, is measured by pressure transducer 47B, 48B The pressure of separating still 47,48, by the two Stress control at predetermined value, and prevents pressure from exceeding the upper limit of the two.Oil-gas Separation Module forms closed loop by valve 9A connecting valve 8A and gas source valve 36A.
All of temperature sensor in free oil displacement portion W and absorption oil test department U, pressure transducer are all connected to calculate Machine controller part 31, is automatically controlled by a computer.
The most each parts are attached forming the unconventional fine and close sand that the inventive method is used according to above-mentioned annexation Rock oil quantitative simulation and experimental apparatus for testing, the experimental provision that the inventive method is used operationally, by each valve member Combination, coordinate pressure detecting control device, temperature control device etc. can carry out unconventional tight sand oil Quantitative simulation experiment sample Making.
Above-mentioned unconventional tight sand oil quantitative simulation and experimental apparatus for testing is used to carry out unconventional tight sand oil fixed Amount simulation experiment, this experiment is under the environmental conditions such as simulation subsurface reservoir temperature, pressure, by injecting crude oil in core column Mode makes the unconventional tight sand oil samples of different oil bearing grade, and the party's normal direction core column is injected the mode of crude oil and used Constant current saturation mode, its operation principle is as follows:
(1) as depicted in figs. 1 and 2, first stainless steel column is loaded in the lead set 13 of clamper 1, the entrance of clamper 1 End pipeline, first arrival end passage the 19, second arrival end passage 110, arrival end channel valve 1A and the pipeline of waste liquid valve 3A Volume is fixed amount, at different displacement pressure PiUnder the conditions of, crude oil is full of arrival end pipeline, the first arrival end passage 19, second The crude oil volume of the pipeline of arrival end passage 110, arrival end channel valve 1A and waste liquid valve 3ABe one along with pressure The amount of change, but corresponding uniform pressure, the crude oil volume being every time full ofShould be the same for the previous, use standardizition, record is every The full pipeline crude oil volume that individual pressure spot is corresponding
Wherein, the displacement flow set scope of displacement pump (ISCO pump) is generally 0.1～1ml/min, can estimate arrival end Pipeline, first arrival end passage the 19, second arrival end passage 110, arrival end channel valve 1A and the pipeline body of waste liquid valve 3A Long-pending (about 1.5ml), if displacement flow set is 1ml/min, then injects 1.5min and can be full of crude oil；This simulation experiment preparation causes Crude oil need not be determined when during close sandstone oil samples and be full of pipeline, but utilize at different displacement pressure PiUnder the conditions of obtain correspondence Full pipeline crude oil volumeIt should be noted that using the effect of stainless steel column is at different displacement pressure PiUnder the conditions of Crude oil does not the most enter stainless steel column, accurately to obtain corresponding pipeline different crude oils volumeAdopt with next step (2) With difference displacement pressure P during core column sampleiUnder the conditions of be full of passage crude oil volumeIdentical, in order to calculate and enter core column Crude oil amount.
(2) stainless steel column is changed to core column sample, uses constant crude oil to inject flow velocity and continue to core column and passage Pressurization, when pressure increases to a certain value, crude oil will be flowed in core column, now inject crude oil amountFormer by full passage The amount of oilWith the amount injecting core column crude oilConstitute, the displacement pressure P of the corresponding time point of recordi, total with the crude oil injected VolumeDeduct the volume of full passage crude oilI.e. can obtain entering the volume of core column crude oilI.e.Monitored by computer control part 31When it is equal to the quantitatively injection crude oil volume set, meter Calculate machine controller part 31 and automatically control stopping injection crude oil.
Therefore, step 3 of the present invention) unconventional tight sand oil Quantitative simulation experiment is unconventional tight sand oil quantitatively mould The manufacture method of draft experiment sample, uses above-mentioned unconventional tight sand oil quantitative simulation and experimental apparatus for testing to carry out containing oil rock During the making of stem sample, use the saturated principle of above-mentioned constant current to inject crude oil to core column and form fine and close oil samples, including following Step:
Step one: stainless steel column is loaded in the lead set 13 of clamper 1, and clamper 1 is put in temperature-controlled box 2, connect Good clamper 1 arrival end channel valve 1A and waste liquid valve 3A, outlet end passageways valve 2A and valve 29A, confined pressure interface 18, beat Open temperature-controlled box 2 and the power supply of computer control part 31, set the temperature i.e. simulated formation temperature of temperature-controlled box 2, be heated to Design temperature constant temperature are no less than 3h；
Opening confined pressure valve 30A, start confined pressure pump 30, set confined pressure 70MPa, Time constant is no less than 1h；
Open vacuum-pumping valve 35A, arrival end channel valve 1A, start vacuum pump 35 evacuation no less than 20min, closedown Valve 35A, vacuum pump 34, open piston container 21C or 21D terminal valve 11A and 12A or 13A equipped with crude oil and 14A, valve 29A and 33A, start displacement pump 34, backpressure pump 33, set displacement flow (the general set point of displacement flow 0.1～ 1ml/min), back pressure value (strata pressure residing for the back pressure value being normally set up and core column sample is consistent)；
Under the control of displacement pump 34, backpressure pump 33, confined pressure pump 30 and computer control part 31, note in clamper 1 Enter crude oil, record a certain injection pressure i.e. displacement pressure PiThe crude oil volume of the most full arrival end pipelineRepeat said process, Use standardizition, record different pressures point PiCorresponding full pipeline crude oil volumeReal by the orderly close-down contrary with beginning Experiment device；
Step 2: core column sample is loaded in the lead set 13 of clamper 1, put in temperature-controlled box 2, connect clamper 1 Arrival end channel valve 1A and waste liquid valve 3A, outlet end passageways valve 2A and valve 29A, confined pressure interface 18, open temperature control Case 2 and the power supply of computer control part 31, the temperature setting temperature-controlled box 2 is carried out simulated formation temperature, is heated to set mould Intend formation temperature constant temperature no less than 3h；
Step 3: open confined pressure valve 30A, starts confined pressure pump 30, sets confined pressure value 70MPa, constant after reaching setting value No less than 1h；Open vacuum-pumping valve 35A, arrival end channel valve 1A, start vacuum pump 35 evacuation no less than 20min, pass Valve closing door 35A, vacuum pump 34；
Step 4: open piston container 21C or 21D terminal valve 11A and 12A or 13A and 14A equipped with crude oil, Valve 29A and 33A, starts displacement pump 34, sets displacement flow, fracture pressure (if fracture pressure will be enclosed higher than 67MPa, needs Press pump 30 is set as automatic tracing mode, and wherein, automatic tracing mode i.e. follows the tracks of injection pressure (i.e. saturation pressure or displacement pressure Power), to ensure that confined pressure is higher than more than injection pressure 2MPa), inject crude oil volume parameter etc.；Start backpressure pump 33, set back pressure Value (strata pressure residing for the back pressure value of setting and core column sample is consistent)；Starting and inject crude oil, record injects crude oil amount (whereinFor injecting crude oil amount, inject crude oil amountThe displacement flow of (ISCO pump) × injection crude oil time), profit The full passage crude oil amount obtained by step oneWith injection crude oil amountObtain the saturated crude oil amount of realityI.e.Computer control part 31 monitors automaticallyWhenDuring equal to the injection crude oil volume set, calculate Machine controller part 31 automatically controls stopping and injecting crude oil, obtains unconventional tight sand oil Quantitative simulation experiment sample.
After unconventional tight sand oil Quantitative simulation experiment sample making completes, need to close the piston equipped with crude oil and hold Device 21C or 21D terminal valve 11A and 12A or 13A and 14A, opens equipped with CO2Piston container 22C or 22D of gas enters Valve 15A and 16A of outlet or 17A and 18A, waste liquid valve 3A, by arrival end pipeline, the first arrival end passage 19, second Crude oil in the passage of outlet end passageways 110, arrival end channel valve 1A and waste liquid valve 3A blows clean.The purpose of this operation It is to eliminate pipeline Crude Oil to subsequent quantitation test free oil and the impact of absorption oil, when completing to make simulation experiment sample, pipe Road is full of crude oil, if not removing, by subsequent operation CO2Gas drive, for measured as free oil and absorption oil, affects in rock core Free oil and the accurately test of absorption oil.
Step 4) it is used for measuring the dissociate gas drive of oil mass of tight sand and for method of testing is:
Slowly open unconventional tight sand oil quantitative simulation and the intake valve of experimental apparatus for testing free oil displacement portion W 4A, blows clean the crude oil in pipeline with carbon dioxide；Open the turnover valve holding gas piston container 22C and 22D 15A and 17A, 16A and 18A, select constant current or constant voltage mode, input flow rate or force value, and flow is usually set to 2～10mL/ Min, pressure is set smaller than the fracture pressure of this sample, and displacement, until the weight of metrology devices 32 port of export is not further added by, is remembered Record experimental data, terminates experiment, obtains tight sand and dissociates oil mass (mg).
Step 5) tight sand absorption oil extraction method of testing be:
From clamper 1, take out not containing after unconventional tight sand oil simulation experiment sample (through step 4) measures dissociate The laboratory sample of oil), pulverizing is weighed, and puts in extraction kettle 45 or 46；Open carbon dioxide air source 36, condenser parts 39, open Extraction kettle 45,46 and the heater switch (not shown) of separating still 47,48, setting extraction kettle 45,46 and separating still 47,48 Temperature controller (not shown) makes its temperature respectively reach 50 DEG C and 40 DEG C；When condenser parts 39 reaches cryogenic temperature-5 DEG C, Open gas source valve 36A and make CO2Enter filter 37, condenser parts 39 and air accumulator 40, through high-pressure pump 41 or carry agent pump 42 (time if desired), depurator 43, blender 44, enter extraction kettle 45,46, control valve 5A, 6A, 7A, 19A, 10A and extraction Still valve 45A, 46A control the pressure of extraction kettle and separating still and are respectively 20MPa and 10MPa；When supercritical extraction absorption oil When amount is not further added by, opens separating still valve 47A, 48A and obtain extraction oil, recording quality, be tight sand absorption oil mass (mg)；Close condenser parts 39, high-pressure pump 41 and main power, slowly open extraction kettle atmospheric valve 45A or 46A, make extraction kettle pressure Power puts into air accumulator 40, after not having pressure, opens extraction kettle, takes out the tight sand oil simulation experiment sample pulverized.
Two, the specific embodiment of the inventive method
The present invention is described below as a example by middle-shallow layer tight sand exploration activity J341, J28, G616, TX15 well of Daqing exploration area The implementation process of method.
Research background:
Since 2011, Daqing oil field has carried out tight sand oil, tight sandy gravel gas, coal bed gas and mud shale oil comprehensively Deng unconventionaloil pool exploration and on-site development test, deep natural gas deploys DS14, DS15, DS16, SS9H well etc., middle-shallow layer Fine and close oil and mud shale oil deploy QP1, QP2, YX55, YX58, J28 well etc., achieve fine and close oil and tight sandy gravel gas stores up The breakthrough of layer industry production capacity, illustrates great potential and the good prospect of unconventionaloil pool exploration.
The oil of unconventional Sandstone Gas Reservoir mainly has free oil and absorption two kinds of occurrence status of oil, Sandstone Gas Reservoir oil Exploration is general uses conventional coring method, owing to drilling and coring delivery departs from underground primal environment and blood pressure lowering degassing, puts for a long time The free oil putting rock core scatters and disappears, and makes free oil test can not reflect underground situation, lacks the trip of unconventional Sandstone Gas Reservoir at present From oil and absorption oil accurately test experiments technology, it it is the difficult problem being badly in need of capturing.Gather Daqing exploration area middle-shallow layer densification exploration activity The sample of J341, J28, G616, TX15 well, has carried out unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental side Method.The inventive method uses simulated formation temperature and pressure and irreducible water condition to form fine and close oil, and makes rock core be in simulation ground The method testing free oil under lower temperature, pressure and irreducible water state, it is possible to reflection subsurface reservoir free oil and moveable oil situation, A set of laboratory facilities being applicable to unconventional Sandstone Gas Reservoir free oil and absorption oil test are groped, for unconventional fine and close sand The exploration and development research of rock oil provides the foundation.
One) acquisition of laboratory sample and analysis:
Select 17, the core column samples such as Daqing exploration area prospect pit QP1, G616, TX15, J28 well, unconventional according to the present invention The operating procedure of Sandstone Gas Reservoir oiliness and mobility evaluation experimental method carries out simulation experiment, uses step in the present invention 1) method measures face porosity and permeability routinely；Utilize step 2) and 3) method obtain tight sand oil quantitative simulation Laboratory sample；Utilize step 4) method the free oil in unconventional tight sand oil Quantitative simulation experiment sample is carried out point Analysis, it is thus achieved that tight sand dissociates oil mass (mg)；Recycle step 5) method to unconventional tight sand oil Quantitative simulation experiment Absorption oil in sample is analyzed, it is thus achieved that tight sand absorption oil mass (mg)；Finally utilize step 6) method to step 4) With 5) obtain data and calculate, it is thus achieved that tight sand different existence state oil evaluating, the results are shown in Table 1, table 2, table 3.
Two) analysis result and evaluation:
1, the accuracy of Sandstone Gas Reservoir oil quantitative simulation method of testing
The residing stratum actual parameter that the exploration of table 1 core column sample measures
Pound sign Lithology Well depth/m Layer position Strata pressure/MPa Formation temperature/DEG C Permeability/mD Porosity/%
G616 Siltstone 1930.65 q4 19.3 86.9 0.69 9.2
TX15 Containing mud siltstone 2033.56 q4 20.3 91.5 0.18 9.5
J28 Siltstone 2203.6 qn2+3 22.0 99.2 0.22 7.7
J28 Siltstone 2229.9 qn2+3 22.3 100.3 0.21 7.4
QP1 Siltstone 1954.03 qn2+3 19.5 87.9 0.068 8.0
QP1 Containing mud siltstone 1954.88 qn2+3 19.5 88.0 0.046 8.3
According to Song-liao basin densification oil Reservoir Classification standard (I class reservoir porosity 8%～12%, permeability 0.1～1mD, II class reservoir porosity 5%～8%, permeability 0.03～0.1mD, II class following reservoir porosity ＜ 5%, permeability ＜ 0.03mD) seeing with formation data parameter residing for the core column sample exploration mensuration of table 1, G616, J28, TX15 well sample product are I class Reservoir, QP1 well sample product are II class reservoir, and its strata pressure, temperature, physical property (porosity, permeability) parameter have difference.
The parameter of table 2 unconventional tight sand oil Quantitative simulation experiment sample making process and result
In terms of the manufacturing process parameter and result data of the tight sand oil Quantitative simulation experiment sample of table 2, on simulation ground In the case of stressor layer, temperature, simulation makes the reality of the laboratory sample that I class obtains with the II class different oil bearing grade of reservoir core post Crude oil amount is injected on border, is 9.43% to the maximum with setting the relative error injecting crude oil amount when making laboratory sample, minimum 2.91%, show the manufacture method of tight sand oil Quantitative simulation experiment sample accurately and reliably.
The system of unconventional reservoir tight sand oil Quantitative simulation experiment sample of the present invention is specifically illustrated above by example Making the overall process of method, its simulation experiment result accurately and reliably, can be used for unconventional tight sand free oil and absorption oil test And mobility evaluation, unconventionaloil pool exploration and development and research and production.
2, tight sand free oil and absorption oil feature
Table 3 tight sand oil quantitative simulation and test experiments result
From the result (table 3) of unconventional Sandstone Gas Reservoir oil quantitative simulation method of testing experiment, different oil bearing grades There is significant difference, oil immersion free oil content 0～5.93mg/g, free oil rate 0%～53.15%, oil in fine and close oil experimental result Speckle free oil content 0～0.84mg/g, free oil rate 0%～16.05%；Oil immersion absorption oil content 4.01～12.96mg/g, suction Attached oil rate 46.85%～100%, oil mark absorption oil content 4.37～5.32mg/g, absorption oil rate 83.95%～100%；Oil immersion Oil content 8.45～14.81mg/g, oil mark oil content 5.21～5.41mg/g, it is the poorest that different oil bearing grade oiliness exist Not.
As can also be seen from Table 3, there is significant difference in different classification reservoir densification oil test results, I class reservoir (porosity 8%～12%, permeability 0.1～1mD) oil immersion free oil content 4.55～5.93mg/g, its free oil rate 49.77～ 53.15%；II class reservoir (porosity 5%～8%, permeability 0.03～0.1mD) oil immersion free oil content 1.85～4.50mg/ G, its free oil rate 12.50～32.95%, II class reservoir oil mark free oil content 0.09～0.84mg/g, its free oil rate 1.65%-16.05%；The II following reservoir of class (porosity ＜ 5%, permeability ＜ 0.03mD) oil immersion, oil mark free oil content are 0mg/g, its free oil rate are 0%.
From tight sand different existence state oil and reservoir properties relation (Fig. 3, Fig. 4), compact reservoir free oil rate with Permeability positive correlation coefficient is 0.9127 and the positive correlation coefficient of porosity is 0.9137, it is seen then that compact reservoir free oil content Main by reservoir porosity and permeability physical characteristics control.
In sum, different oil bearing grades and different the classification oil content (oiliness) of compact reservoir, free oil content, suction Attached oil content is different, and compact reservoir free oil rate is mainly by reservoir porosity and permeability physical characteristics control, reservoir properties and oil-containing The best moveable oil rate of property is the biggest, and oil recoverable is the highest.But, the good reservoir moveable oil rate of oil content height i.e. oiliness is not necessarily Height, if TX15 well 1974.66m siltstone oil immersion oil content 14.81mg/g in mud is the highest, but free oil content is only 1.85mg/g, its free oil rate are 12.50%, have 87.50% i.e. can not exploit out for non-movable oil.Visible, fine and close oil can Dynamic Journal of Sex Research is most important to fine and close exploration activity exploitation.That fine and close exploration activity is developed it is crucial that there is how many oil energy mined, this The method that invention provides can solve the problem that different oil bearing grade and the different free oils classified in unconventional compact reservoir densification oil and Moveable oil problem, provides New Set and foundation for fine and close oil recoverable reserves and exploration and development.
A kind of unconventional Sandstone Gas Reservoir oiliness of the present invention and mobility evaluation is specifically illustrated above by example The overall process of experimental technique, the evaluation result of the method can be used for fine and close oil oiliness and mobility evaluation and unconventionaloil pool is surveyed Visit exploitation research and production.The present invention has a following feature:
(1) unconventional Sandstone Gas Reservoir oiliness and the experimental technique of mobility evaluation are proposed and establish, it is possible to profit Different oiliness laboratory sample is obtained, in airtight, formation temperature and pressure, the irreducible water condition therapeutic method to keep the adverse QI flowing downwards by Quantitative simulation experiment technology Displacement test free oil, uses supercritical extraction test absorption oil, utilizes free oil content (mg/g), absorption oil content (mg/ G), oil content (mg/g), free oil rate (%), the absorption oil rate evaluating such as (%), reach unconventional reservoir oiliness and The purpose that mobility is evaluated, meets the demand of unconventionaloil pool exploration and development.
(2) this experimental technique is utilized to answer at Daqing exploration area middle-shallow layer tight sand oil prospect pit J341, J28, TX15, G616 well With, tight sand (I class, II class) sets and injects crude oil amount (oil immersion) and experiment test crude oil amount (free oil content and absorption oil Content sum) relative error be 9.43%, minimum 2.91% to the maximum, the accuracy of quantitative simulation and test result is high.Carry Unconventional Sandstone Gas Reservoir different existence state oil experiment analysis results, I class reservoir oil immersion free oil and moveable oil has been supplied to contain Amount 4.55～5.93mg/g (free oil rates 49.77%～53.15%)；II class reservoir oil immersion free oil and moveable oil content 1.85 ～4.50mg/g (free oil rate 12.50%～32.95%), II class reservoir oil mark free oil and moveable oil content 0.09～ 0.84mg/g (free oil rate 1.65%-16.05%；The following reservoir oil immersion of II class, oil mark free oil and mobile oil are all 0；No With oil bearing grade and the different classification oil content (oiliness) of compact reservoir, free oil content, absorption oil content difference, fine and close storage Layer free oil content is mainly by reservoir porosity and permeability physical characteristics control, and the best free oil content of reservoir properties is the highest, oil-containing The reservoir moveable oil rate that amount height i.e. oiliness is good is the highest, provides experiment for unconventional fine and close exploration activity Development and Production and depends on According to.
(3) unconventional cause sandstone reservoir oiliness and mobility evaluation experimental method can be the unconventional fine and close oil in Daqing exploration area Exploration and development provides technical support, has a extensive future.
The above is only the preferred embodiment of the present invention, it is noted that for the common skill of the art For art personnel, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications Also should be regarded as present disclosure.

Claims (10)

1. a unconventional Sandstone Gas Reservoir oiliness and mobility evaluation experimental method, it is characterised in that comprise following step Rapid:
1) rock core drilling through unconventional Sandstone Gas Reservoir makees core column sample, after core column sample washing oil, measures routinely Face porosity and permeability；
2) by step 1) core column sample after washing oil, after scales/electronic balance weighing, obtain core column quality mThe heart, the most wherein Irrigate saturated normal saline solution, obtain saturated normal saline solution core column sample；
3) by step 2) the saturated normal saline solution core column sample that obtains is by unconventional tight sand oil Quantitative simulation experiment sample The preparation method of product, obtains unconventional tight sand oil Quantitative simulation experiment sample；
4) by step 3) the unconventional tight sand oil Quantitative simulation experiment sample that obtains, survey by free Oil and gas displacement method of testing Surely obtain tight sand to dissociate oil mass (mTrip, mg)；
5) by step 4) weigh after tight sand oil simulation experiment sample comminution after the free oil mass of test, obtain rock quality mStone, recycle unconventional tight sand oil quantitative simulation and experimental apparatus for testing, measure by absorption oil extraction method of testing and obtain Tight sand absorption oil mass (mInhale, mg)；
6) by step 4) and 5) tight sand that obtains dissociates oil mass (mg) and absorption oil mass (mg), calculate and obtain tight sand not With occurrence status oil evaluating free oil content (mg/g), absorption oil content (mg/g), oil content (mg/g), free oil Rate (%), absorption oil rate (%)；Free oil content (mg/g) and free oil rate (%) is the biggest, absorption oil content (mg/g) and absorption Oil rate (%) the least explanation unconventional tight sand oil mobility is the best, i.e. oil recoverable is the biggest；Free oil content (mg/g) and Free oil rate (%) is the least, adsorb oil content (mg/g) and absorption oil rate (%) the biggest explanation unconventional tight sand oil mobility The poorest, i.e. oil recoverable is the least；Oil content (mg/g) the biggest explanation unconventional Sandstone Gas Reservoir oiliness is the best, i.e. oil content The highest, the least explanation of oil content unconventional Sandstone Gas Reservoir oiliness is the poorest, i.e. oil content is the lowest.
Unconventional Sandstone Gas Reservoir oiliness the most according to claim 1 and mobility evaluation experimental method, its feature It being, step 4) described free Oil and gas displacement method of testing is:
Slowly open unconventional tight sand oil quantitative simulation and the gas source valve of experimental apparatus for testing, will with carbon dioxide Crude oil in pipeline blows clean；Open the turnover valve holding gas piston container, select constant current or constant voltage mode, input flow rate Or force value, flow is usually set to 2～10mL/min, and it is real that pressure is set smaller than this unconventional tight sand oil quantitative simulation Testing the fracture pressure of sample, displacement, until the weight of the metrology devices port of export is not further added by, obtains tight sand and dissociates oil mass (mg)。
Unconventional Sandstone Gas Reservoir oiliness the most according to claim 1 and 2 and mobility evaluation experimental method, it is special Levy and be, step 5) described absorption oil extraction method of testing is:
Unconventional tight sand oil quantitative simulation put into by tight sand oil simulation experiment sample after pulverizing being weighed and test is real In the extraction kettle of experiment device, open heater switch and the temperature controller of carbon dioxide air source, condenser parts, extraction kettle and separating still； When condenser parts reaches cryogenic temperature-5 DEG C, open gas source valve and make CO2Sequentially enter filter, condenser parts, air accumulator, High-pressure pump and/or carry agent pump, depurator and blender, finally enter extraction kettle, regulation extraction kettle and the pressure of separating still and Temperature is respectively 20MPa, 10MPa and 50 DEG C, 40 DEG C；When oil mass is not further added by, recording quality, it is tight sand absorption oil Amount.
4. according to the unconventional Sandstone Gas Reservoir oiliness described in claim 1 or 2 or 3 and mobility evaluation experimental method, It is characterized in that, described free oil content (mg/g)=mTrip/mThe heart, absorption oil content (mg/g)=mInhale/mStone, oil content (mg/g)= Free oil content (mg/g)+absorption oil content (mg/g), free oil rate (%)=free oil content (mg/g)/oil content (mg/g) × 100%, absorption oil rate (%)=absorption oil content (mg/g)/oil content (mg/g) × 100%.
5. according to the arbitrary described unconventional Sandstone Gas Reservoir oiliness of claim 1-4 and mobility evaluation experimental method, It is characterized in that, step 3) manufacture method of unconventional tight sand oil Quantitative simulation experiment sample, use unconventional fine and close sand Rock oil quantitative simulation and experimental apparatus for testing carry out the making of saturated core post sample, described experimental provision include clamper (1), Temperature-controlled box (2), confined pressure pump (30), backpressure pump (33), displacement pump (34), vacuum pump (35), computer control part (31), piston Container (21C, 21D, 22C, 22D) and multiple valve,
Described manufacture method is characterised by, comprises the following steps:
Step one: stainless steel column is loaded in the lead set (13) of clamper (1), and clamper (1) is put in temperature-controlled box (2), Connect arrival end channel valve (1A) and waste liquid valve (3A), outlet end passageways valve (2A) and the valve of clamper (1) (29A) with confined pressure interface (18), open temperature-controlled box (2) and the power supply of computer control part (31), set the temperature of temperature-controlled box (2) Degree carrys out simulated formation temperature, and the design temperature the constant temperature that are heated to temperature-controlled box (2) are no less than 3h；
Open confined pressure valve (30A), start confined pressure pump (30), set confined pressure value 70MPa, constant 2h after reaching setting value；Open Vacuum-pumping valve (35A), arrival end channel valve (1A), start vacuum pump (35) evacuation 20min, closes valve (35A), true Empty pump (34), open valve (11A, 12A) that the piston container (21C or 21D) equipped with crude oil imports and exports or valve (13A, 14A), valve (29A, 33A), start displacement pump (34), backpressure pump (33), set and inject flow and back pressure value；
Under the control of displacement pump (34), backpressure pump (33), confined pressure pump (30) and computer control part (31), to clamper (1) inject crude oil in, record a certain injection pressure i.e. displacement pressure PiThe crude oil volume of the most full arrival end pipelineIf experiment Displacement pressure P need to be obtainediValue is more than 67MPa'sMore than injection pressure 2MPa can be higher than by setting confined pressure value or confined pressure is set Pump (30) is automatic tracing mode；Repeat said process, use standardizition, record different pressures point PiCorresponding full pipeline is former Oil volumeExperimental provision as described in the orderly close-down contrary with beginning；
Step 2: core column sample is loaded in the lead set (13) of clamper (1), and clamper (1) is put into temperature-controlled box (2) In, connect arrival end channel valve (1A) and waste liquid valve (3A), outlet end passageways valve (2A) and the valve of clamper (1) (29A), confined pressure interface (18), open temperature-controlled box (2) and the power supply of computer control part (31), set the temperature of temperature-controlled box (2) Degree carrys out simulated formation temperature, and the design temperature the constant temperature that are heated to temperature-controlled box (2) are no less than 3h；
Step 3: open confined pressure valve (30A), starts confined pressure pump (30), sets confined pressure value 70MPa, constant after reaching setting value No less than 1h；Open vacuum-pumping valve (35A), arrival end channel valve (1A), start vacuum pump (35) evacuation and be no less than 20min, closes valve (35A), vacuum pump (34)；
Step 4: open valve (11A, 12A) that the piston container (21C or 21D) equipped with crude oil imports and exports or valve (13A, 14A), valve (29A, 33A), start displacement pump (34), set displacement flow, fracture pressure, injection crude oil volume parameter etc.；Open Dynamic backpressure pump (33), sets back pressure value；Starting and inject crude oil, record injects crude oil amountBeing full of of utilizing that step one obtains is logical Road crude oil amountWith injection crude oil amountObtain the saturated crude oil amount of realityI.e.Computer controls Device 31 monitors automaticallyWhenDuring equal to the injection crude oil volume set, computer control part 31 automatically controls stopping note Enter crude oil, obtain unconventional tight sand oil Quantitative simulation experiment sample.
6. according to the arbitrary described unconventional Sandstone Gas Reservoir oiliness of claim 1-5 and mobility evaluation experimental method, It is characterized in that, described unconventional tight sand oil quantitative simulation and experimental apparatus for testing mainly include tight sand oil quantitatively mould Plan and free oil displacement portion and carbon dioxide supercritical fluid extraction adsorb oil test department, be provided with one and can make two between two parts Person's connection or the intake valve of isolation；
Free oil displacement portion includes the model module for simulating oil reservoir, injects crude oil and the injection of displacing medium to model module Module, effluent to model module are acquired and the effluent acquisition testing module that detects and the temperature to model module Degree, pressure carry out the detection control module that detection controls.
Unconventional Sandstone Gas Reservoir oiliness the most according to claim 6 and mobility evaluation experimental method, its feature Being, described model module includes the clamper being placed in temperature-controlled box, and described clamper includes:
Base (11)；
The holder body (12) being fixed on base (11)；
It is placed in the lead set (13) that holder body (12) is internal；
It is installed on the sealing lid (14) at lead set (13) two ends；
It is arranged in and seals the inside and outside inner seal ring of lid (14) and exterior seal ring；
It is fixed on the end cap (16) at holder body (12) two ends；
At two push rods (17) threadeded with end cap (16) in holder body (12) end；
The outwardly directed one end of one end push rod be provided with the first arrival end passage (19) that be connected internal with holder body (12) and Second arrival end passage (110), outwardly directed one end of push rod of the other end is provided be connected with holder body (12) internal First outlet end passageways (111) and the second outlet end passageways (112)；Holder body (12) is provided with confined pressure interface (18), is used for Connect confined pressure pump (30) to control the work confined pressure within clamper；First arrival end passage 19 is by arrival end channel valve (1A) it is connected with injection module, intake valve (4A)；First outlet end passageways (111) is by outlet end passageways valve (2A) and injection Module, intake valve (4A) are connected；Second arrival end passage (110) is connected with waste liquid valve (3A), the second outlet end passageways (112) It is connected with effluent acquisition testing module by valve (29A).
8., according to the unconventional Sandstone Gas Reservoir oiliness described in claim 6 or 7 and mobility evaluation experimental method, it is special Levying and be, described carbon dioxide supercritical fluid extraction absorption oil test department includes carbon dioxide supply and processing module, supercritical two Carbonoxide extraction absorption oil module and Oil-gas Separation module, wherein:
Carbon dioxide supply and processing module include carbon dioxide air source (36) and gas source valve (36A) and lead in its downstream, place Be sequentially connected in series on road in filtering carbon dioxide the filter (37) of impurity, for measuring the carbon dioxide gas scale of construction Effusion meter (38), Filter valve (37A), for cooled carbon dioxide gas condenser system (39), be used for storing titanium dioxide The air accumulator (40) of carbon, for compressing the high-pressure pump (41) of carbon dioxide and carrying agent pump (42), for purifying carbon dioxide Depurator (43) and blender (44).
9. according to the unconventional Sandstone Gas Reservoir oiliness described in claim 6 or 7 or 8 and mobility evaluation experimental method, It is characterized in that, described supercritical carbon dioxide extraction absorption oil module includes extraction kettle (45) and the extraction kettle being connected in parallel (46), the two ends of extraction kettle (45,46) respectively connect a valve, temperature controller, heater element and pressure transducer；
Oil-gas Separation module includes the separating still (47) being sequentially connected in series on the downstream passage that valve (19A) is connected and separates Still (48), is connected by valve (10A) therebetween；
Carbon dioxide supply and processing module are connected to supercritical carbon dioxide extraction absorption oil module by valve (5A), surpass and face Boundary's carbon dioxide abstraction absorption oil module is connected to Oil-gas Separation module by valve (19A)；
Supercritical carbon dioxide extraction absorption oil module is connected to carbon dioxide by valve (8A) and supplies and the gas of processing module Source valve (36A), Oil-gas Separation module forms loop by valve (9A) connecting valve (8A) and gas source valve (36A)；Described Carbon dioxide supply and processing module and supercritical carbon dioxide extraction absorption oil module are connected to cause by valve (4A) respectively Close sandstone oil quantitative simulation and free oil displacement portion thereof.
10. according to the arbitrary described unconventional Sandstone Gas Reservoir oiliness of claim 1 to 9 and mobility evaluation experimental side Method, it is characterised in that described unconventional Sandstone Gas Reservoir refers to packsand, siltstone, shale or contains mud or calcic or containing being situated between The reservoir of bits siltstone.
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