WO2011133885A1 - Capacité de stockage totale et porosité totale de supports poreux - Google Patents

Capacité de stockage totale et porosité totale de supports poreux Download PDF

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Publication number
WO2011133885A1
WO2011133885A1 PCT/US2011/033608 US2011033608W WO2011133885A1 WO 2011133885 A1 WO2011133885 A1 WO 2011133885A1 US 2011033608 W US2011033608 W US 2011033608W WO 2011133885 A1 WO2011133885 A1 WO 2011133885A1
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Prior art keywords
pressure
gas
reservoir
valve
core sample
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PCT/US2011/033608
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English (en)
Inventor
Richard F. Sigal
Ibrahim Yucel Akkutlu
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The Board Of Regents Of The University Of Oklahoma
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Publication of WO2011133885A1 publication Critical patent/WO2011133885A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry

Definitions

  • the present invention provides an apparatus for measuring the storage capacity and total porosity of a shale core sample.
  • the apparatus includes a gas source, a pressure vessel suitable for receiving a sample housing which supports a core sample.
  • a reservoir in fluid communication with said pressure vessel receives pressurized gas from the gas source. Control gas flow from the gas source to the reservoir is controlled by a first valve and a second valve controls passage of gas from the reservoir to said pressure vessel.
  • the current invention provides a method for determining the storage capacity of a core sample obtained from a subterranean formation.
  • the method of the current invention utilizes an apparatus comprising a pressure vessel.
  • the pressure vessel is in fluid communication with a high pressure gas reservoir with, fluid flow between the pressure vessel and a high pressure gas reservoir controlled by a first valve.
  • a gas source in fluid communication with the high pressure gas reservoir provides gas for testing of the core sample.
  • the gas source typically includes a pump or other suitable device for providing gas under pressure to the high pressure gas reservoir.
  • a second valve controls flow of gas from said gas source to the high pressure gas reservoir.
  • the first valve is initially closed during positioning of a core sample within said pressure vessel.
  • the initial pressure within the pressure vessel is measured and identified as the first pressure.
  • Pressure within the high pressure gas reservoir is increased to a second pressure.
  • the first valve is opened.
  • Pressure change within the pressure vessel is recorded as a function of time until pressure stabilizes at a third pressure.
  • the change pressure is used to establish a pressure decay curve and to determine transport coefficients.
  • the method determines the volume of the first valve, any fluid communication path, e.g. pipes, between the first valve and the pressure vessel. This volume is defined as the second volume.
  • the first volume corresponds to the high pressure gas reservoir and any fluid communication path between the high pressure gas reservoir and the first valve.
  • the method of the current invention determines the initial moles of gas within the first volume at the first pressure as well as the moles of gas in the second volume at the second pressure. Subsequently, the method determines the increased gas storage capacity of the core sample at the third pressure.
  • Figure 1 depicts a five stage storage measurement performed on an organic shale plug.
  • Figure 2 schematically depicts the apparatus of the present invention.
  • Figure 3 provides a comparison between the measured storage for the sample, lower curve, and methane storage, upper curve.
  • Figure 4 provides a representative NMR T 2 relaxation curve for methane depicting a stress release peak.
  • the current invention provides a measurement of the storage capacity and total porosity as a function of pressure. Additionally, the current invention measures these characteristics using the reservoir gas of interest.
  • the current invention utilizes core samples obtained from the reservoir. These can be old unpreserved samples or samples preserved to be consistent with their in-reservoir condition. However, when determining the liquid porosity, one will preferably use preserved core samples for testing purposes. Additionally, using the apparatus of Figure 2, the current invention permits determination of all storage mechanisms impacting the reservoir in one measurement. Thus, the current invention provides the essential information to characterize the total gas storage as a function of pressure and temperature, and the amount stored by each storage mechanism.
  • the present invention permits determination of the gas production rate as pressure decreases, or in the case of CO 2 sequestration at the injection rate. Simulating the gas production rate is essential for an accurate simulation of the reservoir production.
  • the current invention is suitable for characterizing any reservoir, but is more suitable for reservoirs that include gas stored in an adsorbing state such as shale gas reservoirs, and sequestration of CO 2 in such reservoirs.
  • total porosity is defined as the volume of gas and liquids (not including adsorbed or absorbed gas) contained in the sample.
  • An NMR spectrometry measurement on the gas-free sample is used to determine the water and liquid hydrocarbon volumes within the core sample.
  • the gas storage capacity is separated into the adsorbed/absorbed component and the pore volume component V p .
  • V p will be determined by procedures outlined below.
  • the total porosity is defined as the total volume of liquids in the sample plus the volume available for free gas storage V p divided by the bulk volume of the sample.
  • the bulk volume of the sample is determined by standard procedures.
  • the NMR measurement and storage determination test take place under reservoir confining pressure.
  • V p is a function of both the confining pressure and pore pressure.
  • the current invention provides a multi-step process to measure storage capacity.
  • the desired accuracy of the pressure dependency curve and the data processing method will detennine the exact number of steps.
  • the minimum number of steps necessary is two.
  • One skilled in the art recognizes that a greater number of data points over a wide pressure range provide a better determination of the model parameters that will be fitted to the storage curve.
  • Figure 2 shows the minimum basic components needed to perform the storability measurement.
  • the apparatus will be enclosed in an oven (not shown) to provide a constant temperature environment.
  • the apparatus 100 consists of a pressure vessel 10 suitable for housing a sleeved core sample (not shown) to be tested, valves 20 and 30, gas source 40, high pressure gas reservoir 50, pressure gauges 60 and 70 and piping 22, 24, 26, 28, 32 and 34.
  • Valve 20 separates pressure vessel 10 from high pressure gas reservoir 50.
  • high pressure gas reservoir 50 contains the gas of interest, e.g. methane or carbon dioxide.
  • Valve 30 isolates gas source 40 from high pressure gas reservoir 50.
  • Gas source 40 will also include a pump system (not shown) or other suitable system to ensure adequate operating pressures.
  • Reservoir 50 and piping 26 defines a gas volume designated Volume 1 (Vol- 1).
  • a second gas volume, designated Volume 2 or dead Volume 2 (Vol-2), is defined by the volumes of pipe 28, valve 20 and pressure vessel 10, when the pressure vessel is filled with a zero pore volume sample such as a one inch by one inch solid steel right circular cylinder.
  • the configuration of apparatus 100 provides the ability to maintain pressure vessel 10 and the sample contained therein at a confining pressure that corresponds to the subterranean reservoir confining stress experienced by the formation that provided the sample.
  • the confining pressure must always be kept greater than the pore pressure.
  • the method of the present invention determines the storage capacity of the core sample using a multi-stage measurement. Each stage starts with valve 20 closed. In the first stage, Volume 1, within high pressure gas reservoir 50, is increased to pressure P 1 followed by closing of valve 30. The sample and dead Volume 2 are at an initial starting pressure P 2 . In stage 2, valve 20 opens and pressure change is recorded as a function of time until the pressure within dead Volume 2 has stabilized at new pressure Pf.
  • the pressure decay curve developed by stage 2 can be used to obtain the transport coefficients.
  • the method of the current invention can be run with P 1 less than P 2 or P 1 greater than P 2 .
  • P 1 is less than P 2
  • the method determines the decrease in storability as pressure decreases.
  • P 1 is greater than P 2
  • the method determines the increase in storability under higher pressures.
  • R is the universal gas constant
  • T is the temperature
  • z 1 is the correction factor that accounts for deviation from the ideal gas law.
  • a compressibility factor z 1 compensates for the deviation.
  • the correction factor depends on temperature, pressure and the type of gas. Numerous tables and programs exist that provide accurate values of z 1 .
  • the moles of gas contained in Vol-2 V 2 initially are given by:
  • Mass balance requires that the decrease of moles of gas in Vi, Am, is equal to the increase in moles of gas in V 2 , An 2 , plus the increase in moles of gas stored in the sample ⁇ s .
  • the additional moles of gas ⁇ s stored in the sample provide the increase in storability as a function of the change in pressure.
  • this process is iterated over multiple steps it provides the storability as a function of pressure wherein the total number of moles equals the sum of all ⁇ s .
  • This is the basic information needed to characterize the subterranean reservoir and is an essential input into simulations that model the way gas will be produced from the subterranean reservoir or stored in it, i.e. the total gas storage capacity. It should be noted that as there can be hysteresis in the storability curves both the increasing and decreasing storability cases may need to be measured.
  • V p is a function of the pore pressure and the gas type. It may not be a single valued function. The dependence of V p on pressure needs to be included in the model and will be discussed after the discussion of the adsorption/absorption term.
  • V p2 and V Pf are the pore volumes at pressures P 2 and P f .
  • the amount of gas adsorbed/absorbed by the rock matrix is generally assumed to be described by a Langmuir isotherm.
  • a Langmuir isotherm Those skilled in the art recognize that this is only an approximation and other more exact models could be used to model adsorption/absorption component of the storage component.
  • the Langmuir model all the non-free gas is assumed to be adsorbed.
  • the Langmuir isotherm is parameterized by two parameters, (1) the total moles of adsorbed gas at infinite pore pressure (Samax); and, (2) the Langmuir pressure P L .
  • the pore volume can change as a function of pressure due to both adsorption/absorption and due to pore volume compressibility.
  • Adsorption can affect pore volume both by the adsorbed molecules occupying pore space that otherwise would be occupied by the free gas, or by the adsorbed gas closing off pore throats so gas can not get through to the larger pore.
  • Absorption can cause the matrix to swell, or by swelling close off access to pores. The effects would look very similar for both adsorption and absorption.
  • Using the Langmuir model associates all the pore volume changes with adsorption.
  • the Langmuir model can be used to calculate the pore volume loss due to adsorbed gas.
  • Vamax represents the maximum adsorbed gas volume and V a the adsorbed gas volume at any pressure, then assuming Langmuir adsorption:
  • V p o is the pore volume at zero pore pressure then the decrease in V p at pressure P due to adsorption is given by:
  • the maximum molar density of the adsorbed gas (density at infinite pressure) p ag is related to the maximum adsorbed gas volume by:
  • Vamax Samax/p ag
  • Vamax or p ag could be used as a modeling parameter.
  • the density has been taken as the modeling parameter.
  • Total Porosity ((NMR water porosity) + (V p as a function of pressure))/bulk volume.
  • This model of storability has five parameters to determine, Samax, p ag , P L , V p0 , and C p . They will require a multistage measurement process to determine. For the example given a five-stage measurement process was used with methane as the gas. All the parameters were determined from the five-stage measurement process. When assessing the sequestering capacity of subterranean reservoirs C0 2 would be used. It is also possible to determine some of the parameters by other measurements. Measurements with helium could be used to determine V p0 and C p . If the density of the adsorbed state gas is known, then the measurements would require fewer stages.
  • the measurement apparatus is an improvement over currently available standard pycnometer built to measure pore volume.
  • the current invention differs from a standard system by permitting operations at high pore pressures. As a result, the ideal gas law no longer can be used in the analysis.
  • Figure 1 represents the experimental results of one implementation of a five stage storage measurement on a shale gas reservoir core sample. The data has been fitted to the five parameter model described above. Vp0 is in good agreement with independent measurements on this plug and a companion plug. The Langmuir parameters, Samax and P L are in good agreement with those measured on other samples from this core, and the adsorbed state density is in good agreement with various calculations. [0030] To obtain the data presented in Figure 1, the method of the current invention utilized a cylindrical plug taken from a core sample obtained from the targeted shale formation. The plug was sleeved and placed under confining pressure. With reference to Figure 2, the plug is located within pressure vessel 10
  • Figure 1 shows the total methane storage capacity for a sample at five pore pressures (1316 psi, 2138 psi, 2600 psi, 2965 psi and 3136 psi) These storage capacities were measured using apparatus 100 and a five stage measurement sequence. To start the measurement sequence the sample was placed in the pressure vessel 10 and put under a confining pressure of 5000 psi.
  • valve 20 was closed and valve 30 opened to establish the high-pressure gas reservoir at a pressure, Pi, of 2745 psi.
  • the sample at this time was at a pore pressure P 2 of 14 psi.
  • Valve 30 was then closed and valve 20 was opened. The pressure was allowed to equilibrate.
  • the equilibrium pressure P f was 1316 psi.
  • Stage 2 repeated the procedure starting by closing valve 20, and opening valve 30 setting the gas reservoir to 3243 psi.
  • the sample starting pore pressure was 1316 psi.
  • Stages 3, 4 and 5 followed in the same way. Table 1 summarizes the five stage data, and the total storage at each pressure stage calculated from mass balance.
  • This data was modeled using the five-parameter set of non-linear equations.
  • the parameters determined were: the pore volume at zero pore pressure and 5000 psi confining pressure V p0 , the total amount of methane adsorbed Samax, the Langmuir pressure P L , the pore volume compressibility C p , and the adsorbed state methane density at infinite pore pressure p ag .
  • the modeling was done using a spreadsheet and iteratively changing the parameters until a satisfactory fit was found to the data.
  • Various formal inversion procedures such as those found in standard spreadsheet software can be used to automate the process.
  • Table 2 provides the parameter values found by the iterative modeling. The curve through the data is calculated using the five parameters and the non-linear equations that characterize the storage.
  • Table 1 is a typical data set. From data such as in Table 1 combined with the previously established values for Vol- 1 andVol-2, the mass balance equations provide the moles stored in the sample at each stage. See column 5 in Table 1.
  • the volumes Vol-1 and Vol-2 are found by performing the same procedures as when a sample volume is determined except the procedure uses samples of known volumes such as thick walled hollow steel cylinders where the hole volume is accurately known. In this case VI and V2 are the unknowns. For steel cylinders there is no adsorption, and volume changes can be ignored so the modeling equations simplify.
  • V Pf is the pore volume at the equilibrium pressure P f .
  • V pf is calculated from
  • the left side of the equation is known and the right side can be calculated given values of the five parameters: the pore volume at zero pore pressure and 5000 psi confining pressure V p0 , the total amount of methane adsorbed Samax, the Langmuir pressure P L , the pore volume compressibility C p , and the adsorbed state methane density at infinite pore pressure p ag .
  • the left hand side of the equation is determined by the experimental measurements. For an assumed value of the parameters the right hand side can be calculated. For the example the left hand side of the storage equations is found for each stage in column 5 of Table 1. The values for the pressures for each stage are found in Table 1 column 4.
  • the modeling involves finding a set of values for the five parameters that makes the left side equal to the right for all five stages.
  • One approach to achieve this modeling is to choose an initial set of values and then iteratively change the values until equality is achieved to within the desired specified error.
  • One skilled in the art is familiar with the various approaches for carrying out these iterations.
  • one skilled in the art will use a formal inversion method.
  • Figure 3 represents the estimated methane capacity of the sample used in Example 1 for both the prior art estimation procedures and the current invention's method discussed above.
  • the plots in Figure 3 compare the estimated methane capacity curve (line 90) shown in Figure 1 to a methane storage curve (line 80) calculated according to prior art practices.
  • the plot of line 80 was calculated by adding the adsorbed storage from the Langmuir isotherm to the determined volume of free gas that can be stored in the pore space, i.e. the helium porosity at zero pressure.
  • line 80 is a synthetic curve corresponding to a pore volume based on helium porosity of a crushed sample.
  • Line 90 in Figure 3 represents the methane capacity as calculated in the Example above at various confinement pressures.
  • the present invention further enhances the accuracy of the subsurface storage curve by providing a correction step to account for stress release cracks commonly present in recovered cores.
  • methane gas has an NMR signature.
  • Line 14 in Figure 4 provides a representative NMR T 2 relaxation curve for methane with peak 34 representing the volume corresponding to the stress release cracks within the core sample.
  • the foregoing discussion focused on determining the storage capacity of a reservoir with regard to a gas.
  • the disclosed method may also be adapted to determining the storage capacity for liquids.
  • To determine the hydrocarbon liquid storage capacity one will use the desired hydrocarbon liquid in place of the gas and the appropriate equation of state for the liquid in place of the gas.

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Abstract

L'invention concerne l'évaluation d'un réservoir de gaz ou la capacité d'un réservoir à stocker du CO2, et nécessite la compréhension de la porosité totale et de la capacité de stockage de gaz par unité de volume du matériau poreux constituant le réservoir. De manière générale, la capacité de stockage est fonction des propriétés du matériau poreux, de la pression dans les pores du réservoir et de la température. La porosité totale et la capacité de stockage sont difficiles à caractériser lorsque de multiples mécanismes de stockage sont présents. La présente invention fournit un appareil qui utilise un processus de remplissage par stades multiples combiné à une technique RMN pour déterminer la capacité de stockage totale et la porosité totale en fonction de la pression et de la température. Avantageusement, la présente invention permet de réaliser ces mesures in situ en sous-sol.
PCT/US2011/033608 2010-04-23 2011-04-22 Capacité de stockage totale et porosité totale de supports poreux WO2011133885A1 (fr)

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CN103411872A (zh) * 2013-08-23 2013-11-27 西北农林科技大学 一种散粒体孔隙度就仓测量仪
CN103454198A (zh) * 2013-04-24 2013-12-18 中国石油大学(华东) 一种泥页岩有机孔隙度检测方法
CN104697914A (zh) * 2015-03-18 2015-06-10 中国石油大学(华东) 一种泥页岩不同类型有机孔的预测方法
CN104713803A (zh) * 2015-03-16 2015-06-17 中国石油大学(华东) 一种精确测量甲烷在页岩上吸附相密度的方法
WO2015108880A1 (fr) * 2014-01-14 2015-07-23 Halliburton Energy Services, Inc. Procédé de détermination de pression de formation compacte de gaz
CN106153522A (zh) * 2016-08-23 2016-11-23 重庆泛嘉晟禾工程技术检测有限公司 岩心孔隙度测量装置及测量方法
CN110487664A (zh) * 2019-07-19 2019-11-22 中国矿业大学 基于死空间压力换算的煤层瓦斯参数检测装置及施工方法
CN111007233A (zh) * 2019-12-25 2020-04-14 西南石油大学 一种分析页岩微观孔隙中甲烷-二氧化碳运动行为的方法
US10823331B1 (en) 2015-03-24 2020-11-03 Bimby Power Company, Llc. Big mass battery including manufactured pressure vessel for energy storage
CN112129802A (zh) * 2020-10-22 2020-12-25 重庆科技学院 一种水化页岩不同尺度孔隙体积增量的定量分析方法
CN112129482A (zh) * 2020-08-13 2020-12-25 中国石油天然气股份有限公司 页岩储层基质中页岩气流动能力分析方法及装置
CN113959919A (zh) * 2020-07-21 2022-01-21 中国石油化工股份有限公司 一种页岩层段内有机质孔隙度的计算方法及其应用
CN114062190A (zh) * 2021-11-11 2022-02-18 西安石油大学 表征页岩油微观赋存特征的方法、装置、终端及存储介质
CN114970153A (zh) * 2022-05-25 2022-08-30 重庆科技学院 一种油气藏型地下储气库多周期注采动态库容计算方法
CN116773396A (zh) * 2023-06-07 2023-09-19 中国地质调查局油气资源调查中心 地层温压条件下页岩总含气量获取方法和系统

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CN103454198A (zh) * 2013-04-24 2013-12-18 中国石油大学(华东) 一种泥页岩有机孔隙度检测方法
CN103454198B (zh) * 2013-04-24 2015-06-17 中国石油大学(华东) 一种泥页岩有机孔隙度检测方法
CN103411872A (zh) * 2013-08-23 2013-11-27 西北农林科技大学 一种散粒体孔隙度就仓测量仪
US10301936B2 (en) 2014-01-14 2019-05-28 Halliburton Energy Service, Inc. Tight gas formation pressure determination method
WO2015108880A1 (fr) * 2014-01-14 2015-07-23 Halliburton Energy Services, Inc. Procédé de détermination de pression de formation compacte de gaz
WO2015108884A1 (fr) * 2014-01-14 2015-07-23 Halliburton Energy Services, Inc. Détermination de porosité effective pour formations à faible perméabilité
EP3068972A4 (fr) * 2014-01-14 2017-07-05 Halliburton Energy Services, Inc. Procédé de détermination de pression de formation compacte de gaz
US10174613B2 (en) 2014-01-14 2019-01-08 Halliburton Energy Services, Inc. Effective porosity determination for tight gas formations
CN104713803A (zh) * 2015-03-16 2015-06-17 中国石油大学(华东) 一种精确测量甲烷在页岩上吸附相密度的方法
CN104697914A (zh) * 2015-03-18 2015-06-10 中国石油大学(华东) 一种泥页岩不同类型有机孔的预测方法
CN104697914B (zh) * 2015-03-18 2015-12-02 中国石油大学(华东) 一种泥页岩不同类型有机孔的预测方法
US10823331B1 (en) 2015-03-24 2020-11-03 Bimby Power Company, Llc. Big mass battery including manufactured pressure vessel for energy storage
CN106153522B (zh) * 2016-08-23 2023-05-09 重庆泛嘉晟禾工程技术检测有限公司 岩心孔隙度测量装置及测量方法
CN106153522A (zh) * 2016-08-23 2016-11-23 重庆泛嘉晟禾工程技术检测有限公司 岩心孔隙度测量装置及测量方法
CN110487664B (zh) * 2019-07-19 2024-04-12 中国矿业大学 基于死空间压力换算的煤层瓦斯参数检测装置及施工方法
CN110487664A (zh) * 2019-07-19 2019-11-22 中国矿业大学 基于死空间压力换算的煤层瓦斯参数检测装置及施工方法
CN111007233A (zh) * 2019-12-25 2020-04-14 西南石油大学 一种分析页岩微观孔隙中甲烷-二氧化碳运动行为的方法
CN111007233B (zh) * 2019-12-25 2022-03-11 西南石油大学 一种分析页岩微观孔隙中甲烷-二氧化碳运动行为的方法
CN113959919B (zh) * 2020-07-21 2024-04-09 中国石油化工股份有限公司 一种页岩层段内有机质孔隙度的计算方法及其应用
CN113959919A (zh) * 2020-07-21 2022-01-21 中国石油化工股份有限公司 一种页岩层段内有机质孔隙度的计算方法及其应用
CN112129482A (zh) * 2020-08-13 2020-12-25 中国石油天然气股份有限公司 页岩储层基质中页岩气流动能力分析方法及装置
CN112129802A (zh) * 2020-10-22 2020-12-25 重庆科技学院 一种水化页岩不同尺度孔隙体积增量的定量分析方法
CN112129802B (zh) * 2020-10-22 2023-08-15 重庆科技学院 一种水化页岩不同尺度孔隙体积增量的定量分析方法
CN114062190A (zh) * 2021-11-11 2022-02-18 西安石油大学 表征页岩油微观赋存特征的方法、装置、终端及存储介质
US11874211B2 (en) 2021-11-11 2024-01-16 Xi'an Shiyou University Method and device for obtaining microscopic occurrence characteristics of oil stored in a shale
CN114970153A (zh) * 2022-05-25 2022-08-30 重庆科技学院 一种油气藏型地下储气库多周期注采动态库容计算方法
CN114970153B (zh) * 2022-05-25 2023-07-25 重庆科技学院 一种油气藏型地下储气库多周期注采动态库容计算方法
CN116773396A (zh) * 2023-06-07 2023-09-19 中国地质调查局油气资源调查中心 地层温压条件下页岩总含气量获取方法和系统

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