CN117147318B - Shale reservoir multi-scale pore stress sensitivity evaluation method - Google Patents

Shale reservoir multi-scale pore stress sensitivity evaluation method Download PDF

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CN117147318B
CN117147318B CN202311319214.0A CN202311319214A CN117147318B CN 117147318 B CN117147318 B CN 117147318B CN 202311319214 A CN202311319214 A CN 202311319214A CN 117147318 B CN117147318 B CN 117147318B
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杨英
魏建光
赵小青
周晓峰
王安伦
李江涛
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Sanya Offshore Oil And Gas Research Institute Of Northeast Petroleum University
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Abstract

A shale reservoir multi-scale pore stress sensitivity evaluation method comprises the following steps: step one, sample preparation: step two, obtaining a shale pore throat distribution curve; step three, testing the nuclear magnetic signal quantity of the dry sample T 2 spectrum to be NMR 0 by using an online nuclear magnetic resonance system; testing the initial saturated oil T 2 spectrum signal quantity under the reservoir temperature and effective stress as NMR 1; step five, after pore pressure is reduced and effective stress is increased during shale oil exploitation, testing the shale oil T 2 spectrum signal quantity of the core to be NMR 2; step six, testing shale oil T 2 spectrum semaphore when shale oil development effective stress is gradually increased; and step seven, shale multi-scale pore stress sensitivity data processing and analysis are carried out, and shale multi-scale pore stress sensitivity under different effective stress is evaluated. The method solves the problems that the evaluation index is single and the actual production situation of the reservoir cannot be truly reflected, and further improves the accuracy of shale multi-scale pore stress sensitivity evaluation.

Description

Shale reservoir multi-scale pore stress sensitivity evaluation method
Technical Field
The invention relates to the technical field of shale oil gas development, in particular to a shale reservoir multi-scale pore stress sensitivity evaluation method.
Background
With the growing global energy demand, the importance of unconventional oil and gas is increasingly highlighted. Shale oil is taken as an important component of unconventional oil and gas resources, and plays an important role in guaranteeing the energy safety of China. In the shale oil development process, reservoir pressure is continuously reduced, effective stress is continuously increased, and the stress state of shale is changed. Shale is compressed or stretched, and the pore structure and volume of the shale are changed, namely, the porosity and permeability of the shale are changed, so that the seepage capability of oil and gas is affected. Shale reservoir is mainly a micro-nano pore throat, has low matrix permeability, complex pore structure and strong heterogeneity, and is rich in organic matters and clay minerals. The above features exacerbate the complexity of shale reservoir seepage features and stress variations, which are distinguished from conventional reservoirs. The stress sensitivity of the shale reservoir is defined, and the method has important significance for controlling stress sensitive damage in shale oil development and production, improving reservoir seepage capability and keeping long-term stable and high yield of the oil well.
Currently, stress sensitivity of shale reservoirs is evaluated primarily by stress sensitivity experiments. The oil and gas industry standard SY/T5358-2010 reservoir sensitivity flow experiment evaluation method provides a reference method for shale reservoir stress sensitivity evaluation, the experiment method is based on Darcy's law, change of net stress of a rock core is achieved by changing confining pressure or back pressure, corresponding permeability under different net stress effects is calculated, and stress sensitivity is evaluated by using damage degree of permeability of a rock sample. Similar experimental principles and methods are also employed by prior art CN106198338a and CN 112924354A. However, for shale reservoirs, the pores are mostly micro-nano holes, the pore structure is complex, the heterogeneity is strong, the evaluation index of the method is single, namely the overall permeability of the reservoir changes, the distribution of the pore size of the core and the stress sensitivity of the pores with different scales cannot be reflected, and the multi-scale stress sensitivity of the shale reservoir cannot be evaluated truly.
The prior art CN106153662A is a method for measuring the stress sensitivity of the rock core based on nuclear magnetic resonance, and adopts a conventional displacement experiment and a nuclear magnetic resonance test method to measure the stress sensitivity of the rock core. According to the method, the change of the net stress of the rock core is realized by changing confining pressure, the net stress added in the experiment acts on the rock framework first, and the simulation conditions are not consistent with the actual reservoir development conditions; the method uses saturated water as an experimental fluid, is not suitable for shale, and the shale is possibly water-sensitive so as to influence the porosity and the permeability, thereby causing experimental result deviation; the measurement focus of the technology is that the reservoir permeability is not divided by multi-scale pores of the reservoir, the stress sensitivity calculation and evaluation methods of the pores with different sizes are not specifically provided, and the stress sensitivity of the pores with different sizes of shale cannot be truly reflected.
Disclosure of Invention
In order to overcome the defects of the prior art method, the application provides an evaluation method for the multi-scale pore stress sensitivity of a shale reservoir, which can give out the distribution of shale pore diameters and evaluate the stress sensitivity of pores with different scales, and truly reflects the multi-scale pore stress sensitivity of the shale under the actual condition of reservoir production. The application solves the problem of single evaluation index in the prior art, improves the accuracy of page stress sensitivity evaluation, and provides important experimental data support for the design of the field development scheme of the oil field and the optimization of reasonable bottom hole flow pressure. The application aims to provide a shale reservoir multi-scale pore stress sensitivity evaluation method which is used for solving the problems that the evaluation index of the prior art is single, the pore stress sensitivity of different sizes cannot be evaluated, the actual reaction of the shale multi-scale pore stress sensitivity under the actual condition of reservoir production cannot be truly reflected, and the like.
The technical scheme adopted for solving the technical problems is as follows: based on an online nuclear magnetic resonance test technology, the method for evaluating the stress sensitivity of the multi-scale pores of the shale reservoir is provided, and quantitative and accurate evaluation of the effective stress sensitivity of the pores with different sizes under the actual conditions of simulated shale reservoir production is realized.
The shale reservoir multi-scale pore stress sensitivity evaluation method comprises the following steps:
Step one, simulating shale oil preparation and rock sample preparation: the simulated shale oil is prepared by using the ground dehydrated and degassed shale oil and kerosene, so that the simulated shale oil has the same viscosity as the crude oil of the stratum at the reservoir temperature. 1ml of simulated shale oil was tested for nuclear magnetic signal NMR 1ml. Cylindrical cores with the length of 6cm and the diameter of 2.5cm are drilled from shale reservoir full-size coring cores, and the cores are cut into cores with the lengths of 5cm and 1cm, which are respectively marked as 1# rock samples and 2# rock samples. The length L and the diameter D of the 1# rock sample are accurately measured by using a vernier caliper. The No.2 rock sample is used for high-pressure mercury injection test, and the No. 1 rock sample is used for carrying out shale reservoir multi-scale pore stress sensitivity evaluation experiments.
And step two, drying the 1# rock sample and the 2# rock sample to constant weight at the temperature of 110 ℃. And then, carrying out high-pressure mercury testing on the No.2 rock sample to obtain a shale rock sample pore-throat distribution curve.
And thirdly, placing the 1# rock sample in the middle position inside the online nuclear magnetic resonance core holder, connecting the online nuclear magnetic resonance core holder with an online nuclear magnetic resonance core testing system, increasing the confining pressure to 2MPa by using fluorine oil and increasing the temperature of the fluorine oil to the temperature of a shale reservoir. And closing the inlet end and the outlet end of the clamp, vacuumizing the 1# rock sample for 48 hours, then performing a nuclear magnetic T 2 spectrum test in a dry sample state, and recording the nuclear magnetic signal quantity of the dry sample T 2 spectrum as NMR 0.
And step four, the difference value between the shale reservoir overburden pressure P 0 and the reservoir initial pore pressure P p1 is the initial effective stress P to which the shale is subjected. The confining pressure is gradually increased to the initial effective stress by using fluorine oil. In the process of gradually increasing the confining pressure to the overburden pressure P 0, simulated shale oil is simultaneously injected into the inlet end and the outlet end of the clamp to the initial pore pressure P p1 of the reservoir until the flow of the inlet end and the outlet end of the clamp is continuously zero for 4 hours, and the shale core is reduced to the initial conditions of the reservoir temperature and the pressure (the difference value between the confining pressure and the pore pressure is always kept to be the initial effective stress value). And (3) carrying out nuclear magnetic T 2 spectrum test on the saturated oil state of the 1# rock sample under the condition of initial effective stress P 0-Pp1 of the reservoir, and recording the nuclear magnetic signal quantity of the initial saturated oil T 2 spectrum as NMR 1.
Step five, gradually reducing the inlet end and the outlet end of the clamp holder to P p2(Pp2<Pp1), reducing the pore pressure of the rock sample, increasing the effective stress, and then outwards flowing out shale oil in the core to simulate the shale oil exploitation process until the flow of the inlet end and the outlet end of the clamp holder is continuously zero for 4 h. And then, carrying out a nuclear magnetic T 2 spectrum test of the 1# rock sample under the condition of effective stress P 0-Pp2, and recording that the nuclear magnetic signal quantity of shale oil T 2 spectrum in the rock core is NMR 2.
Step six, setting different reservoir pore pressure values Pp3、Pp4、Pp5、Pp6 …(Pp6<Pp5<Pp4<Pp3<Pp2),, repeating step five, respectively simulating a 1# rock sample nuclear magnetic T 2 spectrum test under the condition that effective stress gradually increases P 0-Pp3、P0-Pp4、P0-Pp5、P0-Pp6 … in the shale oil development process, and recording that the shale oil T 2 spectrum nuclear magnetic signal in the core is NMR 3、NMR4、NMR5、NMR6 … at the moment
Step seven, shale multi-scale pore stress sensitivity test data processing and analysis, and the specific method comprises the following steps:
① And drawing shale oil nuclear magnetic signal quantity distribution curves corresponding to different T 2 relaxation times in a semi-logarithmic coordinate system by taking the T 2 relaxation time as a bottom logarithmic abscissa and taking the nuclear magnetic signal quantity of the shale oil saturated into the core as a decimal main ordinate (step four initial saturated oil T 2 spectrum nuclear magnetic signal quantity NMR 1 minus step three dry sample T 2 spectrum nuclear magnetic signal quantity NMR 0).
② Different size pore distribution frequency mercury intrusion test curves (pore radius on top log abscissa and mercury intrusion test pore distribution frequency on decimal minor ordinate) are added in the semi-log coordinate system. And (3) corresponding the maximum T 2 relaxation time of the shale oil nuclear magnetic signal quantity distribution curve to the maximum pore radius of the mercury-pressing test curve, and corresponding the minimum T 2 relaxation time of the shale oil nuclear magnetic signal quantity distribution curve to the minimum pore radius of the mercury-pressing test curve, so as to obtain a space-time conversion relation of one-to-one correspondence of nuclear magnetic resonance T 2 relaxation time and mercury-pressing pore radius. According to the peak distribution characteristics of the nuclear magnetic signal quantity, the shale multi-scale pore can be divided into micro-nano pores, small pores, medium pores and large pores, so that initial nuclear magnetic signal quantities corresponding to the micro-nano pores, the small pores, the medium pores and the large pores are obtained and are NMR N1、NMRS1、NMRM1、NMRL1 respectively, and radius intervals of different pores are determined.
③ Calculating the porosities of pores with different sizes of rock samples under the condition of an initial reservoir: because the pore pressure is much greater than atmospheric pressure at the initial reservoir conditions, fluid compression, shale oil signal volume increases within the same pore volume relative to atmospheric pressure conditions. Therefore, the shale oil nuclear magnetic signal quantity is required to be converted into the saturated oil porosity by utilizing a formula 1 based on the shale oil compression coefficient C O, and then the ① nuclear magnetic signal quantity distribution curve can be converted into the shale multi-scale pore distribution curve under the initial temperature and pressure conditions of the reservoir according to the space-time conversion relation obtained in ②. And then determining the initial total porosity phi 1 of the reservoir layer, the micro-nano pore porosity phi N1, the small pore porosity phi S1, the middle pore porosity phi M1 and the large pore porosity phi L1 according to the formula 1-formula 5 respectively.
④ The porosities of the different size pores of the rock sample under the condition of effective stress P 0-Pp2 are calculated and the stress sensitivity is evaluated: the corresponding initial nuclear magnetic signal quantity of the micro-nano holes, the small holes, the middle holes and the large holes under the condition of obtaining the effective stress P 0-Pp2 by referring to ② is NMR N2、NMRS2、NMRM2、NMRL2. At this time, the pore pressure is reduced, the fluid expands, and the pore volume occupied by shale oil with the same nuclear magnetic signal quantity is increased. Therefore, it is necessary to convert shale oil nuclear magnetic semaphores to saturated oil porosities at corresponding pore pressures using equation 6 based on shale oil compression factor C O. Then, the total porosity Φ 2, the micro-nano pore porosity Φ N2, the small pore porosity Φ S2, the medium pore porosity Φ M2 and the large pore porosity Φ L2 under the condition of effective stress P 0-Pp2 are respectively determined by using a formula 7-a formula 10.
Wherein P p2 is the pore pressure after the first reduction in step five.
⑤ Referring to SY/T5358-2010 reservoir sensitivity flow experiment evaluation method, according to formula 11-formula 15, the change rates of the total pores, the micro-nano pores, the small pores, the medium pores and the large pores are respectively determined to be R 2、RN2、RS2、RM2、RL2, so as to evaluate the multi-scale pore stress sensitivity of the shale.
⑥ The multi-scale pore stress sensitivity of shale under different effective stress P 0-Pp3、P0-Pp4、P0-Pp5、P0-Pp6 conditions was evaluated by repeating ④ and ⑤.
Step two in the scheme, the pore size distribution and the porosity of the solid material are determined according to the standard GB/T21650.1 2008 mercury intrusion method and a gas adsorption method, part 1: performing high-pressure mercury-pressing test on the rock sample by mercury-pressing method to determine pore-throat distribution of the rock core; and step three-step six, performing nuclear magnetic resonance T 2 spectrum test on the rock sample according to SY/T6490-2014 nuclear magnetic resonance parameter laboratory measurement standard, and obtaining shale rock sample nuclear magnetic T 2 spectrum curves under different states.
The invention has the following beneficial effects:
1. The invention relates to a shale reservoir multi-scale pore stress sensitivity evaluation method, which utilizes an online nuclear magnetic resonance technology, and is free from taking out a rock sample and the rock sample is always in a high-temperature and high-pressure state in the test process, so that the interference of human factors is avoided, and the accuracy of a measurement result is high. During testing, firstly, the rock sample is reduced to the initial condition of the reservoir, different effective stresses are applied in a mode of changing the pore pressure by the fixed confining pressure, and the sensitivity of the shale multi-scale pore stress in the actual condition of reservoir production is truly reflected.
2. The method can evaluate the total porosity stress sensitivity under the reservoir condition, and also provides the method for evaluating the pore stress sensitivity of different scales from a microscopic angle, so that the problem of single evaluation index in the prior art is solved, and the accuracy of shale multi-scale pore stress sensitivity evaluation is further improved. In addition, the rock sample can be subjected to continuous nuclear magnetic resonance testing under different effective stress according to the actual field of the oil field, so that the change rule of shale multi-scale pore stress sensitivity along with time and the effective stress is obtained.
3. The shale multi-scale pore stress sensitivity determined by the invention can provide important experimental data support for reasonable bottom hole flow pressure design in an oilfield development site.
Description of the drawings:
FIG. 1 is a schematic diagram of an inventive shale rock sample online nuclear magnetic resonance testing system;
in fig. 1: 1-constant speed constant pressure pump A, 2-valve A, 3-intermediate container, 4-valve B, 5-fluid preheater A, 6-pressure gauge, 7-on-line nuclear magnetic resonance tester, 8-valve C, 9-fluid preheater B, 10-constant speed constant pressure pump B, 11-back pressure valve, 12-valve D, 13-vacuum pump, 14-pipeline, 15-nuclear magnetic control and data acquisition system, 16-1# rock sample, 17-fluorine oil, 18-non-magnetic core holder plug, 19-nuclear magnetic resonance core holder.
Fig. 2 is a graph showing the shale multi-scale pore nuclear magnetic test results and mercury intrusion test pore throat distribution curve pair.
FIG. 3 is a graph showing the multi-scale pore distribution curves of shale under the conditions of 15MPa (initial), 20MPa and 25MPa of effective stress of shale.
The specific embodiment is as follows:
The invention is further illustrated by the following examples in conjunction with the accompanying drawings, which do not in any way limit the scope of the invention.
1-3, The method for evaluating the multi-scale pore stress sensitivity of the shale reservoir based on the online nuclear magnetic resonance testing technology utilizes a shale coring core column with the diameter of 2.5cm, a nuclear magnetic resonance core holder and an online nuclear magnetic resonance tester to realize accurate measurement of the effective stress sensitivity of pores with different sizes under the condition of simulating actual production of the shale reservoir (confining pressure and pore pressure variation), and comprises the following specific steps:
Step one, simulating shale oil preparation and rock sample preparation: preparing simulated shale oil by using ground dehydrated and degassed shale oil and kerosene according to a volume of 1:1, and obtaining the simulated shale oil with the same viscosity (0.64 mPa.s) as the crude oil of the stratum at the reservoir temperature of 110 ℃. Nuclear magnetic signal NMR 1ml for 1ml of simulated shale oil was tested as 1087.8PU. Cylindrical cores with a length of 6cm and a diameter of 2.5cm are drilled from a shale reservoir full-size coring core, and the cores are cut into cores with lengths of 5cm and 1cm, which are respectively marked as a 1# rock sample 16 and a 2# rock sample. The length L and diameter D of the # 1 rock sample 16 were accurately measured by vernier calipers to be 4.988cm and 2.494cm, respectively. The # 2 rock sample was used for high pressure mercury intrusion testing and the # 1 rock sample 16 was used for shale reservoir multiscale pore stress sensitivity evaluation experiments.
Step two, drying the 1# rock sample 16 and the 2# rock sample to constant weight at 110 ℃, wherein the final dry weights of the 1# rock sample 16 and the 2# rock sample are 59.6523g and 11.9204g respectively. And then, carrying out high-pressure mercury injection test on the No. 2 rock sample to obtain a shale rock sample pore-throat distribution curve (shown in figure 2).
And thirdly, placing the 1# rock sample 16 in an online nuclear magnetic resonance core holder 19, fixing the 1# rock sample in an intermediate position by using a non-magnetic core holder plug 18, and connecting the 1# rock sample with the online nuclear magnetic resonance tester 7 by using a pipeline 14. Valve C8 was opened, fluid preheater B9 was opened to increase the temperature of the fluorine oil 17 to 110 ℃ in the shale reservoir, and constant speed constant pressure pump B10 was opened to increase the confining pressure to 2MPa with the fluorine oil 17. Valve B4 is closed, valve D12 is opened, and the shale rock sample is evacuated for 48 hours by vacuum pump 13. Then, a nuclear magnetic control and data acquisition system 15 is used for carrying out a nuclear magnetic T 2 spectrum test in a dry sample state, and the nuclear magnetic signal quantity NMR 0 of the dry sample T 2 spectrum is recorded to be 57.5PU.
And step four, the overlying strata pressure P 0 of the shale reservoir is 45MPa, the initial pore pressure P p1 of the reservoir is 30MPa, and the difference value of the two is that the initial effective stress P of the shale is 15MPa. Valve A2 and valve B4 are opened, and valve D12 is closed. The back pressure valve 11 was set to a pressure of 15MPa. The injection pressure (confining pressure) of the fluorine oil 17 was gradually increased to the initial effective stress of 15MPa by the constant-speed constant-pressure pump B10. The back pressure valve 11 was set to a pressure of 45MPa. Then, in the process of gradually increasing the injection pressure (confining pressure) of the fluorine oil 17 to the overburden pressure of 45MPa (P 0) by using the constant-speed constant-pressure pump B10, the fluid preheater A5 is opened to increase the shale oil temperature to 110 ℃, the constant-speed constant-pressure pump A1 is opened to simultaneously inject the simulated shale oil to the inlet end and the outlet end of the clamp 19 through the intermediate container 3, the injection pressure is gradually increased to 30MPa (P p1) of the initial pore pressure of the reservoir, the pressure is monitored by using the pressure gauge 6 until the flow rate of the inlet end and the outlet end of the clamp 19 is continuously zero for 4h, and the shale core is reduced to the initial condition of the reservoir temperature of 110 ℃ and the pressure of 30MPa (the difference between the confining pressure and the pore pressure is always kept to be 15MPa of the initial effective stress value). And (3) carrying out nuclear magnetic T 2 spectrum test on the saturated oil state of the 1# rock sample under the condition of 15MPa (P 0-Pp1) of initial effective stress of the reservoir by using a nuclear magnetic control and data acquisition system 15, and recording the nuclear magnetic signal quantity NMR 1 of the initial saturated oil T 2 spectrum as 2651.5PU.
Step five, gradually reducing the pressure of the constant-speed constant-pressure pump A1 to 25MPa (P p2), reducing the pore pressure of the rock sample, increasing the effective stress from 15MPa to 20MPa, and at the moment, outwards flowing out shale oil in the core, simulating the shale oil exploitation process until the flow of the inlet end and the outlet end of the clamp 19 is continuously zero for 4 hours. And then, carrying out nuclear magnetic T 2 spectrum test on the 1# rock sample under the condition of effective stress of 20MPa (P 0-Pp2) by using a nuclear magnetic control and data acquisition system 15, and recording that the nuclear magnetic signal quantity of shale oil T 2 spectrum in the core is NMR 2 and 2423.9PU.
And step six, continuously reducing the pressure of the constant-speed constant-pressure pump A1 to 20MPa (P p3)(Pp3<Pp2<Pp1), repeating the step five, developing A1 # rock sample nuclear magnetic T 2 spectrum test under the condition that the effective stress is gradually increased to 25MPa (P 0-Pp3) in the development process of simulated shale oil, and recording that the nuclear magnetic signal quantity of the shale oil T 2 spectrum in the rock core is NMR 3 to be 2253.8PU.
Step seven, shale multi-scale pore stress sensitivity test data processing and analysis, and the specific method comprises the following steps:
① And (3) drawing shale oil nuclear magnetic signal quantity distribution curves corresponding to different T 2 relaxation times in a semi-logarithmic coordinate system by taking the T 2 relaxation time as a bottom logarithmic abscissa and taking the nuclear magnetic signal quantity of the shale oil saturated into the core as a decimal main ordinate (step four initial saturated oil T 2 spectrum nuclear magnetic signal quantity NMR 1 minus step three-dry sample T 2 spectrum nuclear magnetic signal quantity NMR 0;).
② Different size pore distribution frequency mercury intrusion test curves (pore radius on top log abscissa and mercury intrusion test pore distribution frequency on decimal minor ordinate) are added in the semi-log coordinate system. The space-time conversion relation of the one-to-one correspondence of nuclear magnetic resonance T 2 relaxation time and the mercury pressing pore radius can be obtained by corresponding the maximum T 2 relaxation time of the shale oil nuclear magnetic signal quantity distribution curve to 30.2 mu m of the maximum pore radius of the mercury pressing test curve and the minimum T 2 relaxation time of the shale oil nuclear magnetic signal quantity distribution curve to 0.27ms of the minimum pore radius of the mercury pressing test curve to 3.03 mu m (see figure 2). According to the peak distribution characteristics of the nuclear magnetic signal quantity, the shale multi-scale pores can be divided into micro-nano pores, small pores, middle pores and large pores, so that initial nuclear magnetic signal quantities NMR N1、NMRS1、NMRM1、NMRL1 corresponding to the micro-nano pores, the small pores, the middle pores and the large pores are 1072.4, 1359.5, 119.2 and 43.0 PU respectively, and corresponding pore radius intervals and pore occupation ratios of different sizes are determined (see Table 1 for details).
TABLE 1 multiscale pore radius distribution intervals and initial nuclear magnetic semaphores
Pore type Relaxation time interval, ms Pore radius interval, nm Initial nuclear magnetic signal quantity, PU Pore ratio, percent
Micro-nano hole < 0.75 < 15 1072.4 41.3
Small hole 0.75-7.5 15-500 1359.5 52.4
Middle hole 7.5-50.0 500-10000 119.2 4.6
Macropores are formed > 50.0 > 10000 43.0 1.7
③ Calculating the porosities of pores with different sizes of rock samples under the condition of an initial reservoir: based on shale oil compression coefficient 1.4.10 10 -3 MPa-1(CO) converts shale oil nuclear magnetic signal quantity in the multi-scale pore into saturated oil porosity by using a formula 1, and then converts ① nuclear magnetic signal quantity distribution curve into shale multi-scale pore distribution curve under the conditions of initial temperature 110 ℃ of a reservoir, pore pressure 30MPa and effective stress 15MPa according to space-time conversion relation obtained in ② (see figure 3). Further, according to formulas 1-5, the initial total porosity of the reservoir is 1, the micro-nano pore porosity is N1, the small pore porosity is S1, the medium pore porosity is M1, and the large pore porosity is L1 is 9.394, 3.883, 4.923, 0.432, 0.156% (see table 3 for details).
④ The porosities of the different size pores of the rock sample under the condition of effective stress of 20MPa (P 0-Pp2) are calculated and the stress sensitivity is evaluated: the initial nuclear magnetic signal NMR N2、NMRS2、NMRM2、NMRL2 of the micro-nano pore, the small pore, the medium pore and the large pore under the condition of effective stress of 20MPa (P 0-Pp2) obtained by reference ② is 1022.8, 1219.0, 98.2 and 26.5PU respectively. At the moment, the pore pressure is reduced from 30MPa to 25MPa, the fluid expands, and the pore volume occupied by shale oil with the same nuclear magnetic signal quantity is increased. Therefore, it is necessary to convert shale oil nuclear magnetic signal quantity into saturated oil porosity Φ 2 of 8.627% under the condition of corresponding pore pressure of 25MPa using equation 6 based on shale oil compression coefficient of 1.4·10 -3 MPa-1(CO). Reference ③ can convert the nuclear magnetic signal quantity distribution curve under the condition of the effective stress of 15MPa in the fifth step into a shale multi-scale pore distribution curve (see figure 3). Then, the micro-nano pore porosity phi N2, the small pore porosity phi S2, the medium pore porosity phi M2 and the large pore porosity phi L2 under the condition of effective stress of 20MPa (P 0-Pp2) are respectively determined to be 3.728, 4.444, 0.358 and 0.097 by using a formula 7-a formula 10 (see Table 3 for details).
⑤ Referring to sensitivity evaluation indexes (see table 2) of SY/T5358-2010 reservoir sensitivity flow experiment evaluation method, according to the formula 11-formula 15, the change rates R 2、RN2、RS2、RM2、RL2 of the total pore, micro-nano pore, small pore, middle pore and large pore under the condition that the effective stress is increased from 15MPa to 20MPa are respectively 8.2, 4.0, 9.7, 17.1 and 37.8, and then the sensitivity of the shale total pore, micro-nano pore, small pore, middle pore and large pore under the condition that the effective stress is increased from 15MPa to 20MPa is evaluated to be respectively weak sensitivity, insensitive, weak sensitivity and medium weak sensitivity (see table 2).
TABLE 2 sensitivity evaluation index
Rate of change of parameter R% Degree of sensitivity
R≤5 Without any means for
5<R≤30 Weak and weak
30<R≤50 Moderate weakness
50<R≤70 Moderate bias strength
R≥70 Strong strength
⑥ Reference ③ may convert the nuclear magnetic signal profile under the step five effective stress 25MPa (P 0-Pp3) condition to a shale multi-scale pore profile (see fig. 3). The shale multiscale pore stress sensitivity was evaluated under different effective stress conditions of 25MPa by repeating ④ and ⑤ (see table 3 for details).
TABLE 3 Multi-scale pore sensitivity evaluation results under effective stress 20 and 25MPa conditions
According to the method, firstly, the shale multi-scale pore distribution curve is measured under the conditions of the initial temperature, the initial pore pressure and the initial effective stress of the reservoir, and the corresponding porosity and pore diameter distribution intervals of the initial total pores, the micro-nano pores, the small pores, the middle pores and the large pores of the reservoir are determined after the calibration of mercury-pressing data. Then the effective stress of shale is increased by keeping the confining pressure constant and reducing the pore pressure, the shale oil exploitation process is simulated, and the multi-scale pore rate is calculated by measuring the multi-scale pore distribution under different effective stress conditions in real time.
In the implementation process of the method, the core is not required to be taken out, the artificial interference is eliminated, the measurement result accuracy is high, and the condition that the shale multi-scale pores change along with the effective stress under the stratum condition can be truly reflected by a mode of gradually reducing the pore pressure, so that the effective stress sensitivity is evaluated.

Claims (1)

1. A shale reservoir multi-scale pore stress sensitivity evaluation method comprises the following steps:
Step one, simulating shale oil preparation and rock sample preparation: preparing simulated shale oil by using ground dehydrated and degassed shale oil and kerosene, enabling the simulated shale oil to have the same viscosity with stratum crude oil at reservoir temperature, testing nuclear magnetic signal quantity NMR 1ml of 1ml of simulated shale oil, drilling cylindrical cores with the length of 6cm and the diameter of 2.5cm from full-size coring cores of a shale reservoir, cutting the cores into cores with the lengths of 5cm and 1cm, respectively marking the cores as 1# rock sample and 2# rock sample, accurately measuring the length L and the diameter D of the 1# rock sample by using a vernier caliper, and using the 2# rock sample for high-pressure mercury injection test, wherein the 1# rock sample is used for carrying out multi-scale pore stress sensitivity evaluation experiments of the shale reservoir;
Step two, drying the 1# rock sample and the 2# rock sample to constant weight at the temperature of 110 ℃; then, carrying out high-pressure mercury testing on the No.2 rock sample to obtain a shale rock sample pore-throat distribution curve;
step three, placing the 1# rock sample in the middle position inside the online nuclear magnetic resonance core holder, connecting the online nuclear magnetic resonance core testing system, increasing confining pressure to 2MPa by using fluorine oil, increasing the temperature of the fluorine oil to the temperature of a shale reservoir, closing an inlet end and an outlet end of the holder, vacuumizing the 1# rock sample for 48 hours, then carrying out nuclear magnetic T 2 spectrum testing in a dry sample state, and recording that the nuclear magnetic signal quantity of the dry sample T 2 spectrum is NMR 0;
Fourthly, the difference value between the shale reservoir overburden pressure P 0 and the reservoir initial pore pressure P p1 is the initial effective stress P borne by shale, the fluorine oil is utilized to gradually increase the confining pressure to the initial effective stress, in the process of gradually increasing the confining pressure to the overburden pressure P 0, simulated shale oil is simultaneously injected to the reservoir initial pore pressure P p1 at the inlet end and the outlet end of the holder until the flow rate at the inlet end and the outlet end of the holder is continuously zero for 4 hours, the shale core is reduced to the reservoir temperature and the pressure initial condition, the difference value between the confining pressure and the pore pressure is always kept to be the initial effective stress value in the process, the nuclear magnetic T 2 spectrum test of the 1# rock sample saturated oil state under the reservoir initial effective stress P 0-Pp1 condition is developed, and the nuclear magnetic signal quantity of the initial saturated oil T 2 spectrum is recorded as NMR 1;
Gradually reducing the inlet end and the outlet end of the clamp holder to P p2,Pp2 to obtain the pore pressure after the first reduction, wherein P p2<Pp1 is used for reducing the pore pressure of the rock sample and increasing the effective stress, at the moment, shale oil in the rock core flows outwards, simulating the shale oil exploitation process until the flow of the inlet end and the outlet end of the clamp holder is continuously 4h to be zero, then carrying out a 1# rock sample nuclear magnetic T 2 spectrum test under the condition of the effective stress P 0-Pp2, and recording that the nuclear magnetic signal quantity of the shale oil T 2 spectrum in the rock core is NMR 2;
Step six, setting different reservoir pore pressure values Pp3、Pp4、Pp5、Pp6,Pp6<Pp5<Pp4<Pp3<Pp2,, repeating the step five, respectively simulating the gradual increase of effective stress in the shale oil development process, performing nuclear magnetic T 2 spectrum test on a 1# rock sample under the condition of P 0-Pp3、P0-Pp4、P0-Pp5、P0-Pp6, and recording that the nuclear magnetic signal quantity of the shale oil T 2 spectrum in the core is NMR 3、NMR4、NMR5、NMR6;
step seven, shale multi-scale pore stress sensitivity test data processing and analysis are carried out, and shale multi-scale pore stress sensitivity under different effective stress P0-Pp2、P0-Pp3、P0-Pp4、P0-Pp5、P0-Pp6 conditions is evaluated;
The specific method of the step seven is as follows:
① Taking the T 2 relaxation time as a bottom logarithmic abscissa and taking the saturated core shale oil nuclear magnetic signal quantity as a decimal main ordinate in a semi-logarithmic coordinate system, and subtracting the step three dry sample T 2 nuclear magnetic signal quantity NMR 0 from the step four initial saturated oil T 2 spectrum nuclear magnetic signal quantity NMR 1; drawing shale oil nuclear magnetic signal quantity distribution curves corresponding to different T 2 relaxation times;
② Adding different-size pore distribution frequency mercury-pressing test curves in the semi-logarithmic coordinate system, wherein the top logarithmic abscissa is the pore radius, the decimal minor ordinate is the mercury-pressing test pore distribution frequency, the maximum T 2 relaxation time of the shale oil nuclear magnetic signal distribution curve corresponds to the maximum pore radius of the mercury-pressing test curve, the minimum T 2 relaxation time of the shale oil nuclear magnetic signal distribution curve corresponds to the minimum pore radius of the mercury-pressing test curve, so that a space-time conversion relation of one-to-one correspondence of nuclear magnetic resonance T 2 relaxation time and the mercury-pressing pore radius is obtained, the shale multi-scale pores are divided into micro-nano pores, small pores, medium pores and large pores according to the nuclear magnetic signal peak distribution characteristics, and then the corresponding initial nuclear magnetic signal volumes of the micro-nano pores, the small pores, the medium pores and the large pores are NMR N1、NMRS1、NMRM1、NMRL1 respectively, and the radius intervals of different pores are determined;
③ Calculating the porosities of pores with different sizes of rock samples under the condition of an initial reservoir: compared with the atmospheric pressure condition, because the pore pressure is far greater than the atmospheric pressure under the initial reservoir condition, the fluid is compressed, the shale oil signal quantity in the same pore volume is increased, therefore, the shale oil nuclear magnetic signal quantity is required to be converted into saturated oil porosity by utilizing a formula 1 based on a shale oil compression coefficient C O, then the nuclear magnetic signal quantity distribution curve in ① is converted into a shale multi-scale pore distribution curve under the reservoir initial temperature and pressure condition according to the space-time conversion relation obtained in ②, and then the initial total porosity phi 1, the micro-nano pore porosity phi N1, the small pore porosity phi S1, the middle pore porosity phi M1 and the large pore porosity phi L1 are respectively determined according to a formula 1-a formula 5;
④ The porosities of the different size pores of the rock sample under the condition of effective stress P 0-Pp2 are calculated and the stress sensitivity is evaluated: the corresponding initial nuclear magnetic signal quantity of the micro-nano holes, the small holes, the middle holes and the large holes under the condition of obtaining effective stress P 0-Pp2 is NMR N2、NMRS2、NMRM2、NMRL2 respectively by referring to ②; at the moment, the pore pressure is reduced, the fluid expands, and the pore volume occupied by shale oil with the same nuclear magnetic signal quantity is increased; therefore, the shale oil nuclear magnetic signal quantity needs to be converted into saturated oil porosity under the corresponding pore pressure by using a formula 6 based on the shale oil compression coefficient C O, and then the total porosity phi 2, the micro-nano pore porosity phi N2, the small pore porosity phi S2, the middle pore porosity phi M2 and the large pore porosity phi L2 under the condition of effective stress P 0-Pp2 are respectively determined by using a formula 7-a formula 10;
Wherein P p2 is the pore pressure after the first reduction in step five;
⑤ Referring to SY/T5358-2010 reservoir sensitivity flow experiment evaluation method, determining the change rates of total pores, micro-nano pores, small pores, medium pores and large pores to be R 2、RN2、RS2、RM2、RL2 according to formula 11-formula 15 respectively, and further evaluating the multi-scale pore stress sensitivity of shale;
⑥ The multi-scale pore stress sensitivity of shale under different effective stress P 0-Pp3、P0-Pp4、P0-Pp5、P0-Pp6 conditions was evaluated by repeating ④ and ⑤.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104990851A (en) * 2015-06-23 2015-10-21 西南石油大学 Novel experimental research method for shale sensitivity
CN106153662A (en) * 2016-06-17 2016-11-23 北京大学 The measuring method of rock core stress sensitivity
WO2019184429A1 (en) * 2018-03-27 2019-10-03 中国石油大学(华东) Evaluation method for hydrogen containing ingredient, porosity and aperture of shale rich in organic matters
CN112924354A (en) * 2021-01-22 2021-06-08 西南石油大学 Shale reservoir stress sensitivity experiment evaluation method based on gas diffusion coefficient
CN115372398A (en) * 2022-07-19 2022-11-22 东北石油大学 Novel method for quantitatively evaluating sensitivity of shale oil and gas reservoir to foreign fluid
CN115860266A (en) * 2023-02-16 2023-03-28 东北石油大学三亚海洋油气研究院 Shale gas/coal bed gas well productivity evaluation method and system and electronic equipment

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104990851A (en) * 2015-06-23 2015-10-21 西南石油大学 Novel experimental research method for shale sensitivity
CN106153662A (en) * 2016-06-17 2016-11-23 北京大学 The measuring method of rock core stress sensitivity
WO2019184429A1 (en) * 2018-03-27 2019-10-03 中国石油大学(华东) Evaluation method for hydrogen containing ingredient, porosity and aperture of shale rich in organic matters
CN112924354A (en) * 2021-01-22 2021-06-08 西南石油大学 Shale reservoir stress sensitivity experiment evaluation method based on gas diffusion coefficient
CN115372398A (en) * 2022-07-19 2022-11-22 东北石油大学 Novel method for quantitatively evaluating sensitivity of shale oil and gas reservoir to foreign fluid
CN115860266A (en) * 2023-02-16 2023-03-28 东北石油大学三亚海洋油气研究院 Shale gas/coal bed gas well productivity evaluation method and system and electronic equipment

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
致密砂岩孔隙尺度应力敏感分析;丛海龙;吴子森;李虹;杨凯;向洋;张涵之;;科学技术与工程;20190531(第15期);全文 *

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