CN103048261A - Device and method for researching rock physical property parameter change under action of acid fluid - Google Patents

Device and method for researching rock physical property parameter change under action of acid fluid Download PDF

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CN103048261A
CN103048261A CN2013100218844A CN201310021884A CN103048261A CN 103048261 A CN103048261 A CN 103048261A CN 2013100218844 A CN2013100218844 A CN 2013100218844A CN 201310021884 A CN201310021884 A CN 201310021884A CN 103048261 A CN103048261 A CN 103048261A
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volume pump
pressure
ball valve
reactor
way
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CN103048261B (en
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李琦
刘学浩
李小春
方志明
王燕
魏宁
王炳郡
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Wuhan Institute of Rock and Soil Mechanics of CAS
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Wuhan Institute of Rock and Soil Mechanics of CAS
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Abstract

The invention discloses a device and a method for researching rock physical property parameter change under the action of an acid fluid. The method comprises the steps of wrapping a cylindrical test sample and a porous gasket by using a sealing material; putting into a reaction kettle; vacuumizing a system; saturating water to the system after being vacuumized; preparing the acid fluid according to demands and sampling and analyzing; keeping a system pipeline at constant temperature; exerting confining pressure and backpressure to the reaction kettle; exerting porous pressure; and measuring permeation coefficients and displacement pressure of the material in real time. The device is excellent in antiseptic property; due to a liquid preparation relay device, the difficulty of preparing a large-capacity acid fluid under high pressure condition is solved, and the contact area of the acid fluid with the device is reduced as much as possible; and a sealing structure of a rock core end part is in a mode that a bandage is adopted to be tightly tied and sealed with a side surface sealing material at a sharp ring of an end part gasket, so that the device is simple and economic, and at the same time, anti-corrosion and sealing are realized.

Description

A kind of device and method of studying petrophysical parameter variation under the acidic fluid effect
Technical field
The present invention relates to the interactional research field of rock type porous media material and outside fluid, more specifically relate to a kind of device that petrophysical parameter changes under the acidic fluid effect of studying, also relate to a kind of method that petrophysical parameter changes under the acidic fluid effect of studying, be applicable to the interaction of rock type porous media material and outside fluid, the impact of the physical parameters such as sandstone infiltration coefficient, replacement pressure being developed such as the carbon dioxide of sandstone and injection and the long chemical reaction of hydrogen sulfide solution.
Background technology
Adopt the exploitation of (ECBM), shale gas, crude oil along with coal-seam gas increases and increase and adopt (EOR), the development of deep part of deep earth heart exploitation Industrial Engineering such as (EGS) and the Requirement and development of safety evaluation project, and in recent years to CO 2The active demand of geological storage (CCS), acid gas re-injection (AGI), nuke rubbish storage, underground energy deposit, landfill disposal equal energy source and discarded object geological storage technology and rapidly development, fluid injects behind the deep formation the risk assessment on this stratum most important thing as the geological storage engineering feasibility study, has attracted numerous researchists and engineering decision person's attention.And the chemical reaction of rock and fluid, becomes and wherein demands one of difficult problem of capturing urgently especially on the impact of rock seepage characteristic and long-term mechanical characteristic evolution the impact of petrophysical parameter.
Inject the expansion of breeding of dissolving, migration and precipitation that fluid and rock interaction can accelerate rock forming mineral and rock interior micro-crack, thereby change the percolation path, integrality of the interior rock of whole storage convering system and long-term mechanical characteristic thereof.The impact of the interaction partners reservoir sandstone of outside fluid and rock, specifically, the variation of seepage characteristic may reduce the stratum property the annotated deterioration that causes because of near the rock permeability coefficient Injection Well, on injecting fluid at the mobile of stratum and moving especially impact greatly; The evolution of rock replacement pressure may cause reservoir and cap rock at the interface replacement pressure gradually less than reservoir pressure with inject fluid (such as supercritical CO 2) buoyancy, can not stop fluid to infiltrate, penetrate cap rock, reservoir loses the residual gas isolating power gradually; Long-term chemical reaction affects the mechanical characteristic of rock, and reservoir pressure also raises because of the continuous injection of fluid, may cause a part of rock failure damage or stratum globality unstability, even bring out earthquake.
Rock and the interaction of injecting fluid, the chemical reaction of its generation changes the micro hole structure of rock, thereby on the impact that seepage characteristic, replacement pressure and the mechanical characteristic of rock develops, is to estimate one of its underground key scientific problems of sealing the engineering success or failure up for safekeeping.Apparatus and method of the present invention are that following China carries out science and technology support and the tachnical storage that the engineering demonstration is badly in need of.
Therefore, the method and apparatus that chemical reaction between this study of rocks and fluid changes physical parameters such as rock permeability coefficient, replacement pressures, can the mobile migration-chemical reaction of convection cell injection stratum process-mechanical response coupling scientific research provide strong experiment to support, can be widely used in carbon dioxide (CO 2) the geological storage field such as geological storage, acid gas re-injection, sour water re-injection, rock gas subsurface reservoir.
Summary of the invention
The objective of the invention is to be the needs for the defective that exists in the prior art and scientific research and engineering, a kind of device that petrophysical parameter changes under the acidic fluid effect of studying is provided, after specifically can measuring the acidic fluid and the long-time circulation of sandstone and chemical reaction that is formed by hydrogen sulfide gas, carbon dioxide and distilled water proportioning, the variation of sandstone infiltration coefficient, replacement pressure.
A kind of method that petrophysical parameter under the acidic fluid effect changes of studying also is provided, can have analyzed chemical reaction between external (acidity) fluid and the rock type porous media material to its material property effect of parameters.
The invention provides a kind of Novel dispensing relay, can realize the jumbo acidic fluid of next time property preparation of condition of high voltage, and reduced substantially the contact area of acidic fluid and device.
The present invention also provides a kind of novel core end seal structure, by the ingenious structure at the arc tip in the middle of the cushion block of end, and brief economically simultaneously realization sealing and anticorrosion.
A kind of device of studying petrophysical parameter variation under the acidic fluid effect comprises reactor, also comprises vacuum pump, vacuum meter, water tank, liquor room, sulfuretted hydrogen gas cylinder and dioxide bottle,
Vacuum pump and vacuum meter are communicated with the first four-way respectively, the first four-way is communicated with the second four-way by the first ball valve, the second four-way is communicated with water tank by the 3rd ball valve, the second four-way is communicated with the 3rd four-way by the 4th ball valve, the second four-way is connected with the liquor room head end by the first volume pump, the 3rd four-way is connected with the 3rd volume pump by the 5th ball valve, the 3rd volume pump is connected with dioxide bottle with the sulfuretted hydrogen gas cylinder respectively, the 3rd four-way is processed part with the first tail washings and is connected, the 3rd four-way is processed part by the 8th ball valve and the second tail washings and is connected, the 3rd four-way is connected with the liquor room tail end and is connected with the reactor head end by the 12 ball valve, the reactor tail end is processed part with the second tail washings respectively by the 14 ball valve and is connected with the 4th volume pump
Also comprise for the first pressure transducer of measuring the first volume pump pressure, be used for measuring the second pressure transducer of the second volume pump pressure, be used for measuring the 3rd pressure transducer of reactor head end pressure, be used for measuring the 4th pressure transducer of reactor tail end pressure, be used for measuring the differential pressure gauge of reactor head end and tail end pressure differential
Also comprise respectively the data collector that is connected with differential pressure gauge with the first volume pump, the second volume pump, the 3rd volume pump, the 4th volume pump, the first pressure transducer, the second pressure transducer, the 3rd pressure transducer, the 4th pressure transducer.
The head end of aforesaid reactor is connected with the tail end of reactor by the first filtrator, the tenth ball valve, differential pressure gauge, the 11 ball valve and the filtrator of being connected successively.
Aforesaid the first tail washings is processed part and is comprised the first tail washings processing mouth that is communicated with the 3rd four-way by the first needle-valve, and the first tail washings is processed part and also comprised the second needle-valve that is connected with the 3rd four-way by the 16 ball valve,
Described the second tail washings is processed part and is comprised the second tail washings processing mouth that is communicated with the 14 ball valve by the 3rd needle-valve, and the second tail washings is processed part and also comprised the 4th needle-valve that is connected with the 14 ball valve by the 19 ball valve.
Aforesaid the first volume pump is imported and exported, the second volume pump is imported and exported, the 3rd volume pump is imported and exported and the import and export of the 4th volume pump are provided with ball valve.
Aforesaid liquor room comprises the liquor room urceolus and is arranged on the interior dosing relay of liquor room urceolus, the dosing relay comprises movable plate, air bag and the fixed head that is successively set on from top to bottom in the urceolus of liquor room, wherein fixed head is fixedly connected with the liquor room urceolus, movable plate is connected with the top of air bag, and movable plate can be along liquor room urceolus extruding gasbag under the effect of pressure.
Aforesaid reactor comprises the reactor urceolus, also comprise the upper end cushion block, upper porous gasket, core, lower porous gasket and the bottom cushion block that are successively set on from top to bottom in the reactor urceolus, upper end cushion block, upper porous gasket, core, lower porous gasket and bottom cushion block adopt encapsulant to wrap, the arc point that circumferentially is provided with at upper end cushion block and bottom cushion block middle part encircles, be wound with elastoplast on the arc point ring, wherein, upper end cushion block, bottom cushion block, encapsulant and elastoplast consist of the core end seal structure.
A kind of method of studying petrophysical parameter variation under the acidic fluid effect may further comprise the steps:
Step 1, measured material is processed into cylindrical core, core is carried out physical property measurement and rock forming mineral constituent analysis;
Step 2, the first volume pump and the 3rd volume pump piston are pushed into the top;
Step 3, startup vacuum pump carry out airtight test to device, and device is vacuumized;
Step 4, to the water tank topping-up, by the first volume pump first to the full water in liquor room again to the pipeline of the whole device water of satisfy, gas and impurity in the eliminating pipeline;
Step 5, open sulfuretted hydrogen gas cylinder and dioxide bottle, the 3rd volume pump is injected into hydrogen sulfide gas and carbon dioxide with the constant flow pattern liquor room of full water, its amount is processed the part sampling by the first tail washings the acidic fluid composition of preparation is analyzed by component requirement preparation acidic fluid;
Step 6, give in the reactor and fill with hydraulic oil, apply predefined confined pressure stress by the second volume pump, the confined pressure stress value is decided according to the actual formation pressure of simulation;
Step 7, device is placed isoperibol, temperature value is decided according to the formation temperature of realistic simulation;
Step 8, the first volume pump be by the pore pressure value of setting, and with constant voltage mode the acidic fluid in liquor room is pressed into reactor, the core of the saturated distilled water of displacement;
Step 9, the 4th volume pump apply constant back pressure stress, keep the reactor tail end, i.e. the force value of core rear end; Until keeping stable, the registration of the 4th pressure transducer no longer rises, record flow and the force value of the first volume pump, the second volume pump, the 3rd volume pump and the 4th volume pump, record the registration of the first pressure transducer, the second pressure transducer, the 3rd pressure transducer, the 4th pressure transducer and differential pressure gauge;
Step 10, utilize the second tail washings to process part the acidic fluid by core is taken a sample, and compare the situation of change of acidic fluid component before and after obtaining testing with the component of acidic fluid in the step 5;
Step 11, process part and the second tail washings at the first tail washings and process part place's emptying acidic fluid and with the distilled water wash mill that circulates, close each ball valve and power supply;
Step 12, the core after the experiment is carried out physical property measurement analysis and rock forming mineral constituent analysis, and compare with petrophysical parameter and mineralogical composition in the step 1, analyze the variation of rock forming mineral composition and acidic fluid component before and after the experiment.
The present invention compared with prior art has the following advantages and effect:
1) the inventive method attempts determining main mineral chemistry reaction by the variation of acidic fluid and rock interaction mineral constituent before and after the test, and analyzes this chemical reaction to the impact of the physical parameter variations such as the infiltration coefficient of rock, replacement pressure.The real-time analysis method of a kind of attainable many field intensity couplings (particularly seepage flow-chemistry-Coupling with Mechanics) is provided, and principle is distinct.
2) apparatus of the present invention antiseptic property is remarkable.Say on the material, the part of the direct contact of device acidic fluid all adopts the Hastelloy material (C276) of ability hydrogen sulfide solution corrosion, such as element and the parts such as liquor room and reactor such as pipe valves.This device has solved the problem of anti-hydrogen sulfide solution corrosion under the condition of high voltage well, reaches the international leading level;
3) apparatus of the present invention structural design has originality and novelty, a kind of Novel dispensing relay that provides such as inside, liquor room, need under the condition of high voltage to guarantee the preparation of the acidic fluid that long-time continuous injects, and reduced substantially the contact area of acidic fluid and device; Such as a kind of novel core end seal structure that reactor inside provides, the brief anticorrosion and sealing problem that solves simultaneously economically the core end.
Description of drawings
Fig. 1 is system architecture schematic diagram of the present invention;
Fig. 2 is the structural representation in liquor room of the present invention;
Fig. 3 is the structural representation of reactor of the present invention.
Among the figure: the 1-water tank; The 2-liquor room; 2a-movable plate (Hastelloy material); The 2b-air bag; 2c-fixed head (Hastelloy sheet material), 2d-liquor room urceolus (stainless steel); 3-sulfuretted hydrogen gas cylinder; The 4-dioxide bottle; The 5-reactor; 5a-1-upper end cushion block, 5a-2-bottom cushion block (adopt the Hastelloy material, middle outstanding certain radian is used for end part seal); The 5b-core; The upper porous gasket of 5c-1-, porous gasket under the 5c-2-(dispersing fluid formation uniform-flow); 5d-encapsulant (the available heat collapsible tube is met thermal shrinkage, the acid resistance flow-induced corrosion); 5e-elastoplast (placing the hydraulic oil in the reactor, from outside tighten heat-shrinkable tube and cushion block prominence, end, enhanced leaktightness effect); 601-the first volume pump; 602-the second volume pump; 603-the 3rd volume pump; 604-the 4th volume pump; 701-the first ball valve; 702-the second ball valve; 703-the 3rd ball valve; 704-the 4th ball valve; 705-the 5th ball valve; 706-the 6th ball valve; 707-the 7th ball valve; 708-the 8th ball valve; 709-the 9th ball valve; 710-the tenth ball valve; 711-the 11 ball valve; 712-the 12 ball valve; 713-the 13 ball valve; 714-the 14 ball valve; 715-the first needle-valve; 716-the 16 ball valve; 717-the second needle-valve; 718-the 3rd needle-valve; 719-the 19 ball valve; 720-the 4th needle-valve; 801-the first pressure transducer; 802-the second pressure transducer; 803-the 3rd pressure transducer; 804-the 4th pressure transducer; 901-the first four-way; 902-the second four-way; 903-the 3rd four-way; The 10-vacuum pump; The 11-vacuum meter; 12-the first filtrator; The 13-differential pressure gauge; 14-the second filtrator; 15-the second tail washings is processed mouth; 16-the first tail washings is processed mouth;
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail:
Embodiment 1:
Shown in Fig. 1 ~ 3, a kind of device of studying petrophysical parameter variation under the acidic fluid effect,
Comprise water tank 1, liquor room 2, sulfuretted hydrogen gas cylinder 3, dioxide bottle 4, reactor 5, volume pump (601-604), valve (701-720), pressure transducer (801-804), four-way (901-903), vacuum pump 10, vacuum meter 11, the first filtrator 12, differential pressure gauge 13, the second filtrator 14, the first tail washings processing mouthful the 15 and second tail washings processing mouth 16.
The 2 regional dosing functions as core take the liquor room, type of attachment is that vacuum pump 10 and vacuum meter 11 are communicated with the first four-way 901 respectively, the first four-way 901 is communicated with the second four-way 902 by the first ball valve 701, and the first four-way 901 is connected with water tank 1 by the second ball valve 702; The second four-way 902 is communicated with the 3rd four-way 903 by the 4th ball valve 704; The 3rd four-way 903 is processed the front end of part by the 8th ball valve 708 accesses the second tail washings, the structure that said elements is constructed can and vacuumize for system's detection of leaks.
The second four-way 902 is communicated with water tank 1 by the 3rd ball valve 703, and the second four-way 902 is connected with the head end in liquor room 2 by the first volume pump 601; The 3rd four-way 903 is connected with the tail end in liquor room 2, and is connected with the 3rd volume pump 603 by the 5th ball valve 705; The 3rd volume pump 603 is connected with dioxide bottle with sulfuretted hydrogen gas cylinder 3 respectively and is connected, the 3rd four-way 903 is processed part with the first tail washings and is connected, and the structure that said elements is constructed can realize preparing in proportion acidic fluid by hydrogen sulfide gas, carbon dioxide and distilled water.
Zone take reactor 5 as core loads and monitoring function, type of attachment is that the first volume pump 601 connects liquor room 2, liquor room 2 is connected to the front end of reactor 5 by the 12 ball valve 712, reactor 5 tail ends are processed part with the second tail washings respectively by the 14 ball valve 714 and are connected with the 4th volume pump 604.This series of elements particularly around a plurality of volume pumps of reactor, has been constructed the value-added tax function of system.
Also comprise for the first pressure transducer 801 of measuring the first volume pump 601 pressure, be used for measuring the second pressure transducer 802 of the second volume pump 602 pressure, be used for measuring the 3rd pressure transducer 803 of reactor 5 head end pressure, be used for measuring the 4th pressure transducer 804 of reactor 5 tail ends, be used for measuring the differential pressure gauge 13 of reactor 5 head ends and tail end pressure differential
Also comprise respectively with the first volume pump 601, the second volume pump 602, the 3rd volume pump 603 and the 4th volume pump 604, the first pressure transducer 801, the second pressure transducer 802, the 3rd pressure transducer 803, the 4th pressure transducer 804 and are connected the data collector that is connected with differential pressure gauge.These pressure transducers and volume pump are connected to computer by data collector, and this series of elements has been constructed the monitoring function of system, and force value and the flow value of system in the loading procedure gathered.
Wherein the branch road connected mode at differential pressure gauge 13 places is that the head end of reactor 5 is connected with the tail end of reactor by the first filtrator 12, the tenth ball valve 710, differential pressure gauge 13, the 11 ball valve 711 and the filtrator 14 of being connected successively.
The first tail washings is processed part and is comprised that the first tail washings processing mouthful 16, the first tail washings processing part that is communicated with the 3rd four-way 903 by the first needle-valve 715 also comprises the second needle-valve 717 that is connected with the 3rd four-way 903 by the 16 ball valve 16.
The second tail washings is processed part and is comprised that the second tail washings processing mouthful 15, the second tail washings processing part that is communicated with the 14 ball valve 714 by the 3rd needle-valve 718 also comprises the 4th needle-valve 720 that is connected with the 14 ball valve 714 by the 19 ball valve 719.
2 inside, liquor room comprise movable plate 2a, air bag 2b, fixed head 2c and liquor room urceolus 2d.Wherein the fixed head 2c of the Embedded air bag 2b in movable plate 2a, middle part of upper end and bottom forms one-piece construction, and air bag 2b internal circulation acidic fluid is distilled water between air bag 2b and the liquor room urceolus 2d.
Liquor room 2 is high pressure vessel (withstand voltage greater than 20MPa), and air bag 2b volume 5L(guarantees once to test the enough amounts of required acidic fluid), liquor room urceolus 2d adopts stainless steel processing; Top in the urceolus 2d of liquor room is provided with movable plate 2a, bottom in the urceolus 2d of liquor room is provided with fixed head 2c, air bag 2b is arranged between movable plate 2a and the fixed head 2c, but the used acidic liquid of test preparation in the air bag 2b, distilled water circulates between air bag 2b and the liquor room urceolus 2d, the first volume pump 601 loads the pressure that causes in the urceolus of liquor room to be increased, thereby cause movable plate 2a extruding gasbag 2b, the pressure of air bag 2b side also can increase simultaneously, further extruding gasbag 2b is so that the acidic liquid in the air bag 2b can flow in the reactor 5.
Reactor 5 comprises the reactor urceolus, also comprises the upper end cushion block 5a-1, upper porous gasket 5c-1, core 5b, lower porous gasket 5c-2 and the bottom cushion block 5a-2 that are successively set on from top to bottom in the reactor urceolus.Upper end cushion block 5a-1, upper porous gasket 5c-1, core 5b, lower porous gasket 5c-2 and bottom cushion block 5a-2 adopt encapsulant 5d to wrap, and adopting elastoplast 5e to tightly wrap in the most advanced and sophisticated place of the arc of upper and lower end parts cushion block (5a-1,5a-2), bottom cushion block 5a-2 is fixed in the reactor urceolus.
Upper and lower end parts cushion block (5a-1,5a-2) the arc point that circumferentially is provided with at middle part encircles, arc point ring can be selected heat-shrinkable tube as encapsulant 5d() structure that seals of side and reactor urceolus, and adopt elastoplast 5e with upper and lower end parts cushion block (5a-1,5a-2) arc point ring and encapsulant 5d(heat-shrinkable tube) twine and tighten, interior outer fluid is at end cushion block (5a-1, the most advanced and sophisticated place of arc 5a-2) realizes dot encapsulation, be the acidic liquid upper porous gasket 5c-1 that only flows through successively, core 5b, lower porous gasket 5c-2, and the oil pressure that the second volume pump 602 produces between encapsulant and reactor urceolus applies confined pressure to core 5b.
Embodiment 2:
As shown in Figure 1, a kind of method of studying petrophysical parameter variation under the acidic fluid effect comprises following steps:
Step 1, measured material is processed into cylindrical core 5b, diameter 50 ± 2mm, length 100 ± 2mm, before the test core 5b is carried out physical property measurement (factor of porosity test, the experiment of true three axles, acoustic emission experiment) and rock forming mineral constituent analysis (scanning electron microscope sem, X-ray diffraction XRD), basic physical properties parameter and the mineralogical composition of (before being chemical reaction) test rock before the circulation reaction experiment.
Step 2, core 5b two ends contact with lower porous gasket 5c-2 with upper porous gasket 5c-1 respectively, and are connected with the device pipeline by upper and lower end parts cushion block (5a-1,5a-2).One-piece construction is made of upper end cushion block 5a-1, upper porous gasket 5c-1, core 5b, lower porous gasket 5c-2 and bottom cushion block 5a-2, this integrally-built side adopts encapsulant 5d to wrap, the bottom is fixed in the reactor 5 by bottom cushion block 5a-2, thus core fixing in the finishing device.The first volume pump 601 and the 3rd volume pump 603 pistons are pushed into the top;
Step 3, startup vacuum pump 10 carry out airtight test to system.System was by the leak detection test when registration Baumer Y91253B59R when the import of vacuum meter 11(Germany) approached-1, then whole system is vacuumized, vacuum meter 11 registrations were closed vacuum pump 10, the first ball valve 701, the second ball valve 702, the 4th ball valve 704 and the 8th ball valve 708 for-1 o'clock, finished thus the processing that vacuumizes to device;
Step 4, to water tank 1 topping-up,,, guarantee not contain gas and impurity in all pipelines of device again to the pipeline of the whole device water of satisfying first to the full water (namely filled by saturated distilled water, do not contain gas) in liquor room 2 by the first volume pump 601;
Step 5, open sulfuretted hydrogen gas cylinder 3 and dioxide bottle 4, the 3rd volume pump 603 is injected into hydrogen sulfide gas and carbon dioxide with the constant flow pattern liquor room 2 of full water, its amount is prepared (during experiment by the component requirement, sulfuretted hydrogen accounts for the 1%-50% of total gas volume in the acid gas, and fully be dissolved in the distilled water), and by the first sampling needle-valve 715 sampling the acidic fluid composition of preparation is analyzed, as not meeting the demands, readjust preparation (on the low side such as component sulfuretted hydrogen, as then the liquor room to be refilled quantitative hydrogen sulfide gas) after calculating the composition of each component.After reaching requirement, record its each component proportion.Finish thus the preparation of acidic fluid;
Step 6, give and to fill with hydraulic oil (the confined pressure Transfer Medium in the reactor) in the reactor 5, apply predefined confined pressure stress by the second volume pump 602, the confined pressure stress value is decided according to the actual formation pressure of simulation, less than 50MPa, by the second pressure transducer 802 record confined pressure stress values;
Step 7, device place isoperibol, and temperature value is decided according to the formation temperature of realistic simulation, less than 100 ℃;
Step 8, the first volume pump 601 be by the pore pressure value (less than 20MPa) of setting, and with constant voltage mode the acidic fluid in liquor room 2 is pressed into reactor 5, the core of the saturated distilled water of displacement;
Step 9, the 4th volume pump 604 apply constant back pressure stress (less than 20MPa), keep reactor 5 tail ends, i.e. the force value of core rear end; Until keeping stable, the registration of the 4th pressure transducer 804 no longer rises, record flow and the force value of the first volume pump 601, the second volume pump 602, the 3rd volume pump 603 and the 4th volume pump 604, record the registration of the first pressure transducer 801, the second pressure transducer 802, the 3rd pressure transducer 803, the 4th pressure transducer 804 and differential pressure gauge 13;
Step 10, in course of reaction, utilize second sampling needle-valve 718 pairs of acidic fluids by core to take a sample, and compare the situation of change of acidic fluid component before and after obtaining testing with the component of acidic fluid in the step 5;
Step 11, process mouthful the 16 and second tail washings at the first tail washings and process mouthful 15 place's emptying device inner acidic fluids and with distilled water circulation washing, close each ball valve and power supply.
Step 12, again the core after the experiment is carried out physical property measurement analysis and rock forming mineral constituent analysis, and compare with petrophysical parameter and mineralogical composition in the step 1.The main chemical reactions that occurs in the variation of rock forming mineral composition and acidic fluid component and then the definite experimentation before and after the analysis experiment;
The infiltration coefficient and the replacement pressure changing value that record by this device, and the additional physical parameter (factor of porosity, mechanical strength, characteristics of Acoustic Emission) of above-mentioned physical property measurement analysis, the variation of petrophysical parameter before and after the analytical chemistry reaction, thereby the coupling analysis of realization seepage flow-chemistry-mechanics.
The concrete steps of wherein surveying the core replacement pressure are:
After the operation above-mentioned steps 1 ~ step 4, device is in full water state, and acidic fluid not yet begins preparation.Valve-off (701,702 and 703) is opened valve (705,712), the 3rd volume pump 603 with the pattern of slow pressurization with the CO in the dioxide bottle 707 2Gas passes into reactor 5, i.e. CO 2The core of the saturated distilled water of gas displacement.And keep the environment temperature that needs by step 7, step 6 pair core applies confined pressure stress, and step 9 pair core tail end applies back pressure stress.
The force value of Real-time Collection the 3rd volume pump 603 and the differential pressure value of differential pressure gauge 13.When differential pressure gauge 13 registration rapid drawdown, show that carbon dioxide broken through core, this moment, the force value of demonstration of the 3rd volume pump 603 was the replacement pressure of core.
The concrete steps of wherein surveying the core infiltration coefficient are:
After the operation above-mentioned steps 1 ~ step 9, the first volume pump 601 is loaded into the pressure that reactor 5, the four volume pumps 604 are kept the core tail end with the pattern of constant flow with the acidic fluid in liquor room 2.(be steady flow in the pipeline) after experiment is stable, record the loading speed V of the first volume pump and the pressure difference of differential pressure gauge (13), find the solution the infiltration coefficient that obtains core by Darcy's law.
Principle of work of the present invention:
1) main chemical reactions of at first definite rock and acidic fluid is by carrying out mineralogical composition analysis (such as scanning electron microscope sem, X-ray diffraction XRD etc.) to rock before and after the test; The acidic fluid composition is carried out the real time sample analysis, and change before and after the contrast, determine main chemical reaction type and reaction rate thereof.
2) the relevant physical parameter of rock changes in next measured test process, in the process of the test rock is carried out real-time testing permeability and replacement pressure test, observes the real-time evolution of this physical parameter, and concrete principle is as follows:
Replacement pressure is the build-in attribute of rock type porous media material, the breakthrough that equals material on the numerical value is pressed, reacted material behavior and interior microscopic pore texture, be defined as in the porous media material and infiltrate phase fluid and begun mutually by non-infiltration to break through/the required minimum critical pressure of displacement.Adopt continuity method to measure the replacement pressure of rock type porous medium herein.Core upstream volume pump slowly carries out pressure-loaded continuously during test, observes the sandstone core of saturated distilled water by CO 2Or H 2During the S gas breakthrough (microbubble flows out, downstream pressure sensor registration become the phenomenon such as large), this moment, the on-load pressure value of upstream volume pump was the replacement pressure value of the saturated distilled water of this material acid gas displacement.
The infiltration coefficient of porous media material adopts two volume pump methods to measure.Keep upstream and downstream volume pump constant pressure differential Δ P(volume pump constant flow pattern to inject, the differential pressure gauge actual measurement obtains the pressure differential at core two ends), the propelling speed V of monitoring upstream volume pump piston, the conversion fluid volume flow adopts Darcy's law to calculate the osmotic coefficient k of material.
Darcy's law: Q = kA h l
The constant loss of flood peak:
In the formula:
Q-unit interval seepage flow advances speed V to convert by volume pump and tries to achieve known quantity;
The A-discharge section area, cylindrical core diameter 50mm, known quantity;
The loss of h-gross head is tried to achieve by conversion formula, and pressure differential Δ P is recorded by differential pressure gauge;
L-percolation path length is core length 100mm herein, known quantity;
ρ g-fluid density and acceleration of gravity, known quantity;
The k-infiltration coefficient, amount to be asked obtains by above-mentioned solving simultaneous equation.
3) rock is carried out the additional testing experiment, as press the mercury experiment to survey factor of porosity, with true triaxial test ergometry intensity and the Cracks Evolution of acoustic emission system, analyse in depth the reaction of rock and fluid chemistry to the impact of its seepage characteristic, mechanical characteristic.
4) analyze experimental data, attempt setting up the stable relation that chemical reaction develops and affects petrophysical parameter in the process of the test, propose to consider under the chemical affect new constitutive relation of rock material saturation degree.
Above-listed detailed description is that this embodiment limits claim of the present invention for the specifying of possible embodiments of the present invention, and the equivalence that all the present invention of disengaging do is implemented or change, all should be contained in the application's the protection domain.

Claims (7)

1. study the device that petrophysical parameter changes under the acidic fluid effect for one kind, comprise reactor (5), it is characterized in that, also comprise vacuum pump (10), vacuum meter (11), water tank (1), liquor room (2), sulfuretted hydrogen gas cylinder (3) and dioxide bottle (4)
Vacuum pump (10) and vacuum meter (11) are communicated with the first four-way (901) respectively, the first four-way (901) is communicated with the second four-way (902) by the first ball valve (701), the second four-way (902) is communicated with water tank (1) by the 3rd ball valve (703), the second four-way (902) is communicated with the 3rd four-way (903) by the 4th ball valve (704), the second four-way (902) is connected with liquor room (2) head end by the first volume pump (601), the 3rd four-way (903) is connected with the 3rd volume pump (603) by the 5th ball valve (705), the 3rd volume pump (603) is connected 4 with sulfuretted hydrogen gas cylinder (3) with dioxide bottle respectively) be connected, the 3rd four-way (903) is processed part with the first tail washings and is connected, the 3rd four-way (903) is processed part by the 8th ball valve (708) and the second tail washings and is connected, the 3rd four-way (903) is connected with liquor room (2) tail end and is connected with reactor (5) head end by the 12 ball valve (712), reactor (5) tail end is processed part with the second tail washings respectively by the 14 ball valve (714) and is connected with the 4th volume pump (604)
Also comprise for the first pressure transducer (801) of measuring the first volume pump (601) pressure, be used for measuring second pressure transducer (802) of the second volume pump (602) pressure, be used for measuring the 3rd pressure transducer (803) of reactor (5) head end pressure, be used for measuring the 4th pressure transducer (804) of reactor (5) tail end pressure, be used for measuring the differential pressure gauge (13) of reactor (5) head end and tail end pressure differential
Also comprise respectively and be connected 13 with the first volume pump (601), the second volume pump (602), the 3rd volume pump (603), the 4th volume pump (604), the first pressure transducer (801), the second pressure transducer (802), the 3rd pressure transducer (803), the 4th pressure transducer (804) with differential pressure gauge) data collector that is connected.
2. a kind of device that petrophysical parameter under the acidic fluid effect changes of studying according to claim 1 is characterized in that:
The head end of described reactor (5) is connected by the first filtrator (12), the tenth ball valve (710), differential pressure gauge (13), the 11 ball valve (711) and the tail end of filtrator (14) with reactor (5) of being connected successively.
A kind of Study of Fluid according to claim 1 and rock interaction partners petrophysical parameter the impact device, it is characterized in that:
Described the first tail washings is processed part and is comprised the first tail washings processing mouthful (16) that is communicated with the 3rd four-way (903) by the first needle-valve (715), the first tail washings is processed part and is also comprised the second needle-valve (717) that is connected with the 3rd four-way (903) by the 16 ball valve (716)
Described the second tail washings is processed part and is comprised the second tail washings processing mouthful (15) that is communicated with the 14 ball valve (714) by the 3rd needle-valve (718), and the second tail washings is processed part and also comprised the 4th needle-valve (720) that is connected with the 14 ball valve (714) by the 19 ball valve (719).
4. a kind of device that petrophysical parameter under the acidic fluid effect changes of studying according to claim 1 is characterized in that:
Described the first volume pump (601) is imported and exported, the second volume pump (602) is imported and exported, the 3rd volume pump (603) is imported and exported and the 4th volume pump (604) import and export are provided with ball valve.
5. a kind of device that petrophysical parameter under the acidic fluid effect changes of studying according to claim 1 is characterized in that:
Described liquor room (2) comprises liquor room urceolus (2d) and is arranged on the interior dosing relay of liquor room urceolus (2d), the dosing relay comprises movable plate (2a), air bag (2b) and the fixed head (2c) that is successively set on from top to bottom in the liquor room urceolus (2d), wherein fixed head (2c) is fixedly connected with liquor room urceolus (2d), movable plate (2a) is connected with the top of air bag (2b), and movable plate (2a) can be along liquor room urceolus (2d) extruding gasbag (2b) under the effect of pressure.
6. a kind of device that petrophysical parameter under the acidic fluid effect changes of studying according to claim 1 is characterized in that:
Described reactor (5) comprises the reactor urceolus, also comprise the upper end cushion block (5a-1) that is successively set on from top to bottom in the reactor urceolus, upper porous gasket (5c-1), core (5b), lower porous gasket (5c-2) and bottom cushion block (5a-2), upper end cushion block (5a-1), upper porous gasket (5c-1), core (5b), lower porous gasket (5c-2) and bottom cushion block (5a-2) adopt encapsulant (5d) to wrap, the arc point that circumferentially is provided with at upper end cushion block (5a-1) and bottom cushion block (5a-2) middle part encircles, be wound with elastoplast (5e) on the arc point ring, wherein, upper end cushion block (5a-1), bottom cushion block (5a-2), encapsulant (5d) and elastoplast (5e) consist of the core end seal structure.
7. one kind is utilized the described device of claim 1 to study the method that petrophysical parameter changes under the acidic fluid effect, it is characterized in that, may further comprise the steps:
Step 1, measured material is processed into cylindrical core (5b), core (5b) is carried out physical property measurement and rock forming mineral constituent analysis;
Step 2, the first volume pump (601) and the 3rd volume pump (603) piston are pushed into the top;
Step 3, startup vacuum pump (10) carry out airtight test to device, and device is vacuumized;
Step 4, to water tank (1) topping-up, by the first volume pump (601) first to liquor room (2) full water again to the pipeline of the whole device water of satisfy, gas and impurity in the eliminating pipeline;
Step 5, open sulfuretted hydrogen gas cylinder (3) and dioxide bottle (4), the 3rd volume pump (603) is injected into hydrogen sulfide gas and carbon dioxide with the constant flow pattern liquor room (2) of full water, its amount is processed the part sampling by the first tail washings the acidic fluid composition of preparation is analyzed by component requirement preparation acidic fluid;
Step 6, give in the reactor (5) and fill with hydraulic oil, apply predefined confined pressure stress by the second volume pump (602), the confined pressure stress value is decided according to the actual formation pressure of simulation;
Step 7, device is placed isoperibol, temperature value is decided according to the formation temperature of realistic simulation;
Step 8, the first volume pump (601) be by the pore pressure value of setting, and with constant voltage mode the acidic fluid of liquor room (2) is pressed into reactor (5), the core of the saturated distilled water of displacement;
Step 9, the 4th volume pump (604) apply constant back pressure stress, keep reactor (5) tail end, i.e. the force value of core rear end; Until keeping stable, the registration of the 4th pressure transducer (804) no longer rises, record flow and the force value of the first volume pump (601), the second volume pump (602), the 3rd volume pump (603) and the 4th volume pump (604), record the registration of the first pressure transducer (801), the second pressure transducer (802), the 3rd pressure transducer (803), the 4th pressure transducer (804) and differential pressure gauge (13);
Step 10, utilize the second tail washings to process part the acidic fluid by core is taken a sample, and compare the situation of change of acidic fluid component before and after obtaining testing with the component of acidic fluid in the step 5;
Step 11, process part and the second tail washings at the first tail washings and process part place's emptying acidic fluid and with the distilled water wash mill that circulates, close each ball valve and power supply;
Step 12, the core after the experiment is carried out physical property measurement analysis and rock forming mineral constituent analysis, and compare with petrophysical parameter and mineralogical composition in the step 1, analyze the variation of rock forming mineral composition and acidic fluid component before and after the experiment.
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CN113738378A (en) * 2021-09-07 2021-12-03 西南交通大学 Chemical rock breaking medium and chemical auxiliary rock breaking method
CN114486701A (en) * 2021-11-16 2022-05-13 华北科技学院(中国煤矿安全技术培训中心) Long-term erosion test method for damaged rock sample

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