CN110146409B - Method for determining shale gas saturation based on density - Google Patents

Method for determining shale gas saturation based on density Download PDF

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CN110146409B
CN110146409B CN201910384487.0A CN201910384487A CN110146409B CN 110146409 B CN110146409 B CN 110146409B CN 201910384487 A CN201910384487 A CN 201910384487A CN 110146409 B CN110146409 B CN 110146409B
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覃泽健
郭小文
陈家旭
杨毅
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China University of Geosciences
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    • G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
    • G01N9/02—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by measuring weight of a known volume
    • G—PHYSICS
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
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Abstract

The invention relates to a method for determining shale gas saturation based on density, and belongs to the field of oil and gas geology. The method comprises the following steps: s1, taking a shale sample to be tested, carrying out wax sealing treatment on the surface of the shale sample to be tested, and then measuring the bulk apparent density rho of the shale sample by adopting a drainage methodVision(ii) a S2, taking another shale sample to be tested, and measuring the water-containing skeleton density rho of the shale sample when the skeleton contains waterWater-containing skeleton(ii) a After heating to remove water in the shale sample skeleton, measuring the skeleton density rho of the shale sampleBone(ii) a S3, calculating the gas saturation S of the shale sample according to the following formulag：Sg＝((1/ρVision‑1/ρWater-containing skeleton)/(1/ρVision‑1/ρBone) × 100%, the measuring method has simple principle, rapid and efficient experimental process and accurate and considerable calculation result.

Description

Method for determining shale gas saturation based on density
Technical Field
The invention relates to the field of oil and gas geology, in particular to a method for determining shale gas saturation based on density.
Background
Shale gas saturation refers to the volume of natural gas as a percentage of the pore volume of the reservoir under formation pressure conditions. In the exploration and development process of shale oil and gas, the gas saturation is one of important parameters for evaluating the shale resource amount and the gas content.
In the prior art, methods such as well logging, geophysical method, numerical simulation method and the like are commonly adopted to determine the gas saturation of shale. However, the logging method is influenced by complex geological conditions and is difficult to accurately determine the gas saturation of the shale, and the accuracy of the geophysical and numerical simulation method depends on the selection of geological parameters and the reliability of a calculation model.
In the exploration research of shale, the shale reservoir stratum has the characteristics of complex geological conditions, strong heterogeneity and low porosity and low permeability, and the gas saturation of the shale reservoir stratum cannot be accurately measured by adopting the conventional testing technology. The gas saturation of the shale is one of key indexes for evaluating shale free gas, and has important significance for evaluating the gas saturation of the shale gas. Most of the existing methods for measuring the gas saturation of shale in a laboratory are complex in principle and complex in experimental process, so that a method which can be used for simply, quickly, accurately and efficiently measuring the gas saturation of shale is needed.
Disclosure of Invention
In view of this, the invention provides a method capable of accurately and conveniently measuring the shale gas saturation.
The invention provides a method for determining shale gas saturation based on density, which comprises the following steps:
s1, taking a shale sample to be tested, carrying out wax sealing treatment on the surface of the shale sample to be tested, and then measuring the bulk apparent density rho of the shale sample by adopting a drainage methodVision；
S2, taking another shale sample to be tested, and testing the water-containing skeleton density rho of the shale sample when the skeleton contains waterWater-containing skeleton(ii) a After heating to remove water in the shale sample skeleton, measuring the skeleton density rho of the shale sampleBone；
S3, calculating the gas saturation S of the shale sample according to the following formulag：
Sg＝((1/ρVision-1/ρWater-containing skeleton)/(1/ρVision-1/ρBone))×100％
In the formula: sgIs the gas saturation of the shale sample, and the unit is%; rhoVisionIs the bulk apparent density of the shale sample in g/cm3；ρWater-containing skeletonIs the density of the hydrated skeleton of the shale sample, and the unit is g/cm3；ρBoneIs the skeletal density of the shale sample, in g/cm3。
Further, the step S1 is specifically:
s1.1, taking a shale sample to be detected, making the shale sample into a regular shape, flattening edges and corners, brushing off surface attachments, and removing easily-dropped rock debris;
s1.2, weighing the shale sample obtained in the step S1.1 in the air to obtain the mass M of the shale sample in the air4；
S1.3, putting the shale sample into melted paraffin to form a bubble-free wax film on the surface of the shale sample; taking out the cooled and wax-sealed shale sample, weighing in the air, and measuring the mass M of the wax-sealed shale sample in the air5；
S1.4, putting the shale sample after wax sealing into a tray filled with water, and measuring the gravity M of the shale sample after wax sealing in the water6g；
S1.5, obtaining the bulk apparent density rho of the shale sample according to the following formulaVision：
ρVision＝M4/(((M5-M6)/ρWater (W))-((M5-M4)/ρWax))
In the formula: rhoVisionIs the bulk apparent density of the shale sample in g/cm3；M4The mass of the shale sample in the air is g; m5The mass of the shale sample after wax sealing in the air is g; m6Putting the shale sample after wax sealing into a tray filled with water, and measuring the mass of the shale sample after wax sealing in water by gravity conversion, wherein the unit is g; rhoWater (W)Is the density of water in g/cm3；ρWaxIs the density of the paraffin wax in g/cm3。
Further, in steps S1.2, S1.3 and S1.4, the instrument used for weighing is a high precision electron densitometer.
Further, step S2 is specifically:
s2.1, crushing a shale sample to be detected, putting the crushed shale sample into a Rubotherm magnetic suspension balance high-pressure isothermal adsorption instrument, and directly carrying out Buoyancy MeasurTesting the element, namely measuring the water-containing skeleton density rho of the shale sample under the condition that the skeleton contains waterWater-containing skeleton；
S2.2, heating the shale sample by using a Rubotherm magnetic suspension balance high-pressure isothermal adsorption instrument to remove water in the pores of the shale sample skeleton, and then performing Buoyancy Measurement test to measure the skeleton density rho under the condition that the shale sample skeleton does not contain waterBone。
Compared with the prior art, the technical scheme of the invention has the following beneficial effects: the invention adopts the apparent density rho of the shale blockVisionDensity of hydrous skeleton rhoWater-containing skeletonAnd skeleton density ρBoneThe shale gas saturation is accurately calculated, the principle is simple, and the experiment is efficient and rapid. The high-precision electronic densitometer and the German Rubotherm magnetic suspension balance high-pressure isothermal adsorption instrument used in the invention have high instrument precision and accurate and reliable calculation results.
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The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention.
FIG. 1 is a schematic flow chart of a method for measuring shale gas saturation in an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, an embodiment of the present invention provides a method for determining shale gas saturation based on density, which specifically includes the following steps:
step 1: putting paraffin into a beaker, heating and melting the paraffin, slightly vibrating the paraffin to drive out bubbles in the paraffin, and then keeping the beaker static to cool the paraffin; after the paraffin was completely cooled, a paraffin block of 1 cubic centimeter was taken.
Step 2: putting the paraffin block obtained in the step 1 on a high-precision electronic density instrument for weighing, and measuring the mass M of the paraffin block in the air1。
And step 3: putting a U-shaped metal block in a high-precision electronic sealDischarging water with corresponding volume in a tray filled with water of the gradiometer, and measuring the mass M of U-shaped metal blocks and residual water in the tray2(ii) a Slowly putting the paraffin blocks obtained in the step 2 on the same tray by using tweezers, discharging corresponding volume of water, and measuring the mass M of the U-shaped metal blocks, the paraffin blocks and the residual water in the tray at the moment3。
And 4, step 4: by the formula of calculation pWax＝(M1×ρWater (W))/(M1-(M3-M2) Paraffin density was measured.
In the formula: rhoWaxIs the density of the paraffin wax in g/cm3；M1The mass of the paraffin block in the air is g; rhoWater (W)Is the density of water in g/cm3；M2The mass of the U-shaped metal block and the residual water in the tray is g; m3Is the mass M of the U-shaped metal block, the paraffin block and the residual water in the tray3In units of g.
Repeating the steps 2, 3 and 4 three times, taking the arithmetic mean value, and determining rho three timesWaxShould not exceed 0.01g/cm3Otherwise, repeating steps 2, 3 and 4.
And 5: taking a shale sample to be detected, and dividing the shale sample into two parts: cutting a first sample into an approximate cube with the side length of about 2cm, flattening edges and corners, brushing off surface attachments, and removing easily falling rock debris; the second sample was ground to 60-80 mesh powder, weighing about 5 g.
Step 6: weighing the first shale sample in the step 5 on a sample tray of a high-precision electronic density instrument, and measuring the mass M of the first shale sample in the air4；
And 7: heating and melting the paraffin block with the known density, putting the first shale sample in the step 6 into the melted paraffin for 1-2s, taking out, forming a wax film with the thickness of about 1mm on the surface of the first shale sample, checking whether the paraffin film on the first shale sample has bubbles, and putting the first shale sample into the melted paraffin again if the paraffin film has the bubbles;
placing the first shale sample after being taken out, cooled and wax-sealed in a sample holder of a high-precision electron densitometerWeighing on a disc, and measuring the mass M of the first shale sample in the air after wax sealing5；
And 8: putting the first shale sample sealed with wax in the step 7 into a sample tray of a high-precision electronic densitometer filled with water, and measuring the gravity M of the first shale sample sealed with wax on the sample tray in water6g；
And step 9: calculating the bulk apparent density rho of the shale sample according to the following formulaVision：
ρVision＝M4/(((M5-M6)/ρWater (W))-((M5-M4)/ρWax))
In the formula: rhoVisionIs the bulk apparent density of the shale sample in g/cm3；M4The mass of the first shale sample in air is given in g; m5The mass of the first shale sample after wax sealing in the air is g; m6The mass of the first shale sample after wax sealing on the tray is obtained by converting the gravity of the first shale sample in water, and the unit is g; rhoWater (W)Is the density of water in g/cm3；ρWaxThe density of the paraffin calculated for step 4 in g/cm3。
Step 10: putting the second shale sample obtained in the step 5 into a Rubotherm magnetic suspension balance high-pressure isothermal adsorption instrument, directly carrying out Buoyancy Measurement test, and measuring the shale water-containing skeleton density rho of the second shale sample skeleton under the water-containing conditionWater-containing skeleton。
Step 11: heating the sample for 24 hours under the vacuum condition of 110 ℃ by using a Rubotherm magnetic suspension balance high-pressure isothermal adsorption instrument to remove the water in the pores of the second shale sample skeleton; and after heating, carrying out BuoyancyMeasurement test to obtain the skeleton density rho of the second shale sample in the absence of waterBone。
Step 12: bulk apparent density ρ through shale samplesVisionDensity of hydrous skeleton rhoWater-containing skeletonAnd skeleton density ρBoneCalculating the gas saturation S of the shale samplegThe calculation formula is as follows:
Sg＝((1/ρvision-1/ρWater-containing skeleton)/(1/ρVision-1/ρBone))×100％
In the formula: sgIs the gas saturation of the shale sample, and the unit is%; rhoVisionIs the bulk apparent density of the shale sample in g/cm3；ρWater-containing skeletonIs the density of the hydrated skeleton of the shale sample, and the unit is g/cm3；ρBoneIs the skeletal density of the shale sample, in g/cm3。
Taking a shale sample of the Longmaxi group in the region of the Jobi Jordan rock dam in the Sichuan basin as an example, the apparent density rho of the shale sample block is calculated according to the methodVisionDensity of hydrous skeleton rhoWater-containing skeletonSkeleton density ρBoneAnd the calculated gas saturation S of the shale samplegAs shown in table 1 below:
table 1 shale sample calculation data
Figure GDA0002443172710000061
As can be seen from Table 1, the gas saturation S of the shale sample calculated according to the method described above in the examples of the present inventiongThe gas saturation of the shale sample obtained by the nuclear magnetic resonance method has small difference, and the determination method of the embodiment of the invention is accurate and convenient.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict. The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (4)

1. A method for determining shale gas saturation based on density is characterized by comprising the following steps:
s1, taking a shale sample to be tested, carrying out wax sealing treatment on the surface of the shale sample to be tested, and then testing the apparent density of the block of the shale sample by adopting a drainage methodDegree rhoVision；
S2, taking another shale sample to be tested, and testing the water-containing skeleton density rho of the shale sample when the skeleton contains waterWater-containing skeleton(ii) a After heating to remove water in the shale sample skeleton, measuring the skeleton density rho of the shale sampleBone；
S3, calculating the gas saturation S of the shale sample according to the following formulag：
Sg＝((1/ρVision-1/ρWater-containing skeleton)/(1/ρVision-1/ρBone))×100％
In the formula: sgIs the gas saturation of the shale sample, and the unit is%; rhoVisionIs the bulk apparent density of the shale sample in g/cm3；ρWater-containing skeletonIs the density of the hydrated skeleton of the shale sample, and the unit is g/cm3；ρBoneIs the skeletal density of the shale sample, in g/cm3。
2. The method for determining shale gas saturation based on density as claimed in claim 1, wherein the step S1 is specifically:
s1.1, taking a shale sample to be detected, making the shale sample into a regular shape, flattening edges and corners, brushing off surface attachments, and removing easily-dropped rock debris;
s1.2, weighing the shale sample obtained in the step S1.1 in the air to obtain the mass M of the shale sample in the air4；
S1.3, putting the shale sample into melted paraffin to form a bubble-free wax film on the surface of the shale sample; taking out the cooled and wax-sealed shale sample, weighing in the air to obtain the mass M of the wax-sealed shale sample in the air5；
S1.4, putting the shale sample after wax sealing into a tray filled with water, and measuring the gravity M of the shale sample after wax sealing in the water6g；
S1.5, obtaining the bulk apparent density rho of the shale sample according to the following formulaVision：
ρVision＝M4/(((M5-M6)/ρWater (W))-((M5-M4)/ρWax))
In the formula: rhoVisionIs the bulk apparent density of the shale sample in g/cm3；M4The mass of the shale sample in the air is g; m5The mass of the shale sample after wax sealing in the air is g; m6Putting the shale sample after wax sealing into a tray filled with water, and measuring the mass of the shale sample after wax sealing in water by gravity conversion, wherein the unit is g; rhoWater (W)Is the density of water in g/cm3；ρWaxIs the density of the paraffin wax in g/cm3。
3. The method for determining shale gas saturation based on density as claimed in claim 2, wherein in steps S1.2, S1.3 and S1.4, the instrument used for weighing is a high precision electron densitometer.
4. The method for determining shale gas saturation based on density as claimed in claim 1, wherein the step S2 is specifically:
s2.1, crushing a shale sample to be tested, putting the crushed shale sample into a Rubotherm magnetic suspension balance high-pressure isothermal adsorption instrument, directly carrying out Buoyancy Measurement test, and measuring the water-containing skeleton density rho of the shale sample under the condition that the skeleton contains waterWater-containing skeleton；
S2.2, heating the shale sample by using a Rubotherm magnetic suspension balance high-pressure isothermal adsorption instrument to remove water in the pores of the shale sample skeleton, and then performing Buoyancy Measurement test to measure the skeleton density rho under the condition that the shale sample skeleton does not contain waterBone。
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