CN110836836A - Kerogen elastic modulus testing method - Google Patents
Kerogen elastic modulus testing method Download PDFInfo
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- CN110836836A CN110836836A CN201810938107.9A CN201810938107A CN110836836A CN 110836836 A CN110836836 A CN 110836836A CN 201810938107 A CN201810938107 A CN 201810938107A CN 110836836 A CN110836836 A CN 110836836A
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- 238000012360 testing method Methods 0.000 title claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 22
- 239000003513 alkali Substances 0.000 claims abstract description 16
- 238000011160 research Methods 0.000 claims abstract description 13
- 230000003647 oxidation Effects 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 40
- 238000002360 preparation method Methods 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 9
- 238000010998 test method Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 239000011435 rock Substances 0.000 abstract description 12
- 239000005416 organic matter Substances 0.000 abstract description 9
- 230000000704 physical effect Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 54
- 239000002245 particle Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- 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
- G01N9/36—Analysing materials by measuring the density or specific gravity, e.g. determining quantity of moisture
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- 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
- G01N2009/022—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by measuring weight of a known volume of solids
- G01N2009/024—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by measuring weight of a known volume of solids the volume being determined directly, e.g. by size of container
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The invention relates to a kerogen elastic modulus testing method, relates to the technical field of rock physics research, and is used for solving the technical problem that the physical property of organic rock is difficult to directly measure in the prior art. According to the invention, a chemical separation method is adopted, namely, non-oxidation acid liquor and alkali liquor are added into a shale sample, so that organic matters are separated from the shale sample and prepared into a kerogen sample, namely an artificial rock core, and the elastic modulus of an organic matter enrichment body, namely kerogen, can be obtained through experimental measurement on the kerogen sample, so that a new means is provided for rock physical research of the organic matters.
Description
Technical Field
The invention relates to the technical field of petrophysical research, in particular to a method for testing the elasticity modulus of kerogen.
Background
The content of organic matters in the shale is an important index for evaluating the oil and gas production capacity of the shale, and an organic matter enrichment area is one of important targets of oil and gas reservoir exploration in the oil and gas exploration and development processes. The study of seismic response characteristics for organic matter has also been the primary direction for seismic exploration of hydrocarbon reservoirs. In the field of petrophysics, the research on organic matters is mainly reflected in the research on physical properties of kerogen, including physical properties, mechanics and elastic properties of the kerogen. However, kerogen is an aggregate of organic matters, the form of the kerogen is not fixed, and the kerogen is difficult to be directly used for rock physics research.
Disclosure of Invention
The invention provides a method for testing the elastic modulus of kerogen, which is used for solving the technical problem that the physical property of organic rock is difficult to directly measure in the prior art.
The invention provides a kerogen elastic modulus testing method, which comprises the following steps:
step S10: obtaining a shale sample in a research area, and respectively adding a non-oxidation acid solution and an alkali solution into the shale sample to obtain a mixed solution after the shale sample is fully reacted;
step S20: centrifuging the mixed solution to separate the mixed solution into layers to obtain kerogen;
step S30: putting the kerogen into a sample preparation device for sample preparation, obtaining a kerogen sample,
step S40: and calculating to obtain the elastic modulus of the kerogen according to the longitudinal wave velocity, the transverse wave velocity and the density of the kerogen sample.
In one embodiment, step S30 includes the following sub-steps:
step S31: putting the kerogen into a sample preparation device, and loading pressure at two ends of the sample preparation device;
step S32: keeping the pressure for a certain time, measuring the longitudinal wave velocity and the transverse wave velocity of the kerogen, and if the difference between the longitudinal wave velocity and the transverse wave velocity measured for the nth time and the longitudinal wave velocity and the transverse wave velocity measured for the (n-1) th time is less than 1%, obtaining the ending loading pressure and obtaining the kerogen sample; otherwise, step S31 is repeated.
In one embodiment, the pressure is maintained for at least 1 hour or more in step S32.
In one embodiment, step S10 includes the following sub-steps:
step S11: obtaining a shale sample in a research area, and grinding the shale sample into powder;
step S12: adding non-oxidation acid liquor into the shale sample powder, and reacting to obtain a first intermediate solution;
step S13: washing the first intermediate solution with distilled water to obtain a neutral second intermediate solution;
step S14: adding alkali liquor into the second intermediate solution, and reacting to obtain a third intermediate solution;
step S15: and washing the third intermediate solution with distilled water, and obtaining a neutral mixed solution after reaction.
In one embodiment, the non-oxidizing acid solution is hydrochloric acid having a concentration of 6 mol/L.
In one embodiment, the lye is a sodium hydroxide solution with a concentration of 0.5 mol/L.
In one embodiment, in step S12, the mixing ratio of the shale sample powder to the non-oxidizing acid solution is 1 g: 6 mL.
In one embodiment, in step S12, a non-oxidizing acid solution is added to the shale sample powder for at least 2 h.
In one embodiment, in step S14, lye is added to the second intermediate solution for at least 1h of reaction.
In one embodiment, step S20 includes the following sub-steps:
step S21: centrifuging the mixed solution to layer and removing a solid part;
step S21: and baking the solid part to remove water to obtain the kerogen.
Compared with the prior art, the invention has the advantages that: the method adopts a chemical separation method, namely, non-oxidation acid liquor and alkali liquor are added into a shale sample to separate organic matters from the shale sample, the organic matters are prepared into a kerogen sample, namely an artificial rock core, and the elastic modulus of an organic matter enrichment body, namely kerogen, can be obtained by carrying out experimental measurement on the kerogen sample, so that a new means is provided for the rock physics research of the organic matters.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings.
FIG. 1 is a flow chart of a kerogen modulus of elasticity test method in an embodiment of the invention;
FIG. 2 is a schematic representation of an ultrasonic testing of kerogen in accordance with the present invention.
Detailed Description
The invention will be further explained with reference to the drawings.
As shown in figure 1, the invention provides a kerogen elastic modulus test method, which comprises the following steps:
the first step is as follows: and obtaining a shale sample in a research area, and respectively adding non-oxidation acid liquor and alkali liquor into the shale sample to obtain a mixed solution after the shale sample is fully reacted.
Organic matter in rock generally exists in the form of solid (kerogen), liquid (oil), and gas, and organic matter in the present invention refers to organic matter existing in the form of solid. This organic matter can be extracted from the rock, usually by means of chemical dissolution separation.
Since kerogen is a dispersed organic matter insoluble in alkali, non-oxidizing acids and non-polar organic solvents in sedimentary rock, kerogen can be obtained by reacting a shale sample with non-oxidizing acid and alkali liquids to remove other components in the shale.
Specifically, first, a shale sample is obtained from an area of interest and the shale sample is ground into a powder. Wherein the shale sample is generally cylindrical, for example, a cylindrical structure having a diameter of 25mm and a height of 50 mm. Additionally, the shale samples were ground to 600 mesh powder.
Secondly, adding non-oxidation acid liquor into the shale sample powder, and obtaining a first intermediate solution after reaction.
Preferably, the non-oxidation acid solution is hydrochloric acid with the concentration of 6 mol/L.
Preferably, the mixing ratio of the shale sample powder to the non-oxidation acid solution is 1 g: 6mL, i.e. 6mL of non-oxidizing acid solution per gram of shale sample powder.
In addition, non-oxidation acid liquor is added into the shale sample powder, so that the shale sample reacts with the non-oxidation acid liquor for at least 2 hours or more than 2 hours at the temperature of 65 ℃, and the shale sample is ensured to fully react with the acid liquor.
After the reaction is finished, washing the first intermediate solution with distilled water to obtain a neutral second intermediate solution; and adding alkali liquor into the second intermediate solution, and reacting to obtain a third intermediate solution.
Preferably, the alkali liquor is a sodium hydroxide solution with the concentration of 0.5 mol/L.
In addition, adding alkali liquor into the second intermediate solution to ensure that the second intermediate solution and the alkali liquor react for at least 1h or more than 1h at the temperature of 65 ℃ to ensure that the second intermediate solution and the alkali liquor fully react.
And finally, washing the third intermediate solution with distilled water, and obtaining a neutral mixed solution after reaction.
And secondly, centrifuging the mixed solution to separate layers to obtain the kerogen.
Specifically, first, the mixed solution is centrifuged to separate layers, and then a solid portion is removed.
Next, the solid portion is baked to remove moisture therefrom, thereby obtaining kerogen. For example, the solid part is put into an oven and baked at 60 ℃ for more than 72h to remove the moisture in the solid part.
And thirdly, putting the kerogen into a sample preparation device for sample preparation, and obtaining a kerogen sample.
Specifically, first, the kerogen 3 is put into the sample preparation device 1, and pressure is applied to both ends of the sample preparation device 1 to 10 Mpa.
Secondly, maintaining the pressure for a certain time, preferably, maintaining the pressure for at least more than 1 h; then, the longitudinal wave velocity Vp and the transverse wave velocity Vs of the kerogen are measured by the ultrasonic probe 2 since the ultrasonic probe 2 is embedded in the kerogen 3 already in the sample producing device 1 as shown in fig. 2.
And if the difference between the longitudinal wave velocity and the transverse wave velocity measured at the nth time and the longitudinal wave velocity and the transverse wave velocity measured at the (n-1) th time is less than 1%, the kerogen is considered to be fully compacted, and the kerogen can be used for experimental measurement. Obtaining the end loading pressure and obtaining a kerogen sample; otherwise, repeatedly loading the pressure until the difference is less than 1%.
The difference means that the difference between the longitudinal wave speeds measured in the two previous and next times is less than 1%, and the difference between the transverse wave speeds measured in the two previous and next times is less than 1%.
And fourthly, calculating and obtaining the elastic modulus of the kerogen according to the longitudinal wave velocity, the transverse wave velocity and the density of the kerogen sample.
As shown in FIG. 2, the sample preparation device 1 had a sample preparation inner diameter of 25mm, and the diameter of the kerogen sample was 25mm because the kerogen 3 was placed in the sample preparation device 1 and compacted.
After the kerogen 3 was put into the sample preparation vessel 1, ultrasonic probes 2 were embedded in the kerogen at both ends of the sample preparation vessel 1, respectively, to measure the longitudinal wave velocity and the transverse wave velocity of the kerogen.
And the scale is arranged on the sample preparation device 1, so that the length of the kerogen sample can be obtained according to the scale on the sample preparation device 1, and the volume V of the kerogen sample is obtained.
In addition, the mass m of the kerogen sample can be obtained by weighing, and the density ρ of the kerogen is calculated from V ═ m ρ.
Wherein the Young's modulus E of kerogen satisfies the following defined formula:
the shear modulus μ of kerogen satisfies the following defined formula:
the bulk modulus K of kerogen satisfies the following defined formula:
the Lame constant λ of kerogen satisfies the following defined formula:
the poisson ratio σ of kerogen satisfies the following defined formula:
wherein ρ is the density of kerogen, Vp is the longitudinal wave velocity, and Vs is the transverse wave velocity.
In conclusion, the invention separates out the kerogen particles by a chemical method and prepares the kerogen particles into the artificial core, and the artificial core is used for obtaining the elastic modulus of the kerogen by an experimental measurement method, thereby being used for rock physical modeling of shale and shale seismic attribute research.
While the invention has been described with reference to a preferred embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the technical features mentioned in the embodiments can be combined in any way as long as there is no structural conflict. It is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. A kerogen elastic modulus test method is characterized by comprising the following steps:
step S10: obtaining a shale sample in a research area, and respectively adding a non-oxidation acid solution and an alkali solution into the shale sample to obtain a mixed solution after the shale sample is fully reacted;
step S20: centrifuging the mixed solution to separate the mixed solution into layers to obtain kerogen;
step S30: putting the kerogen into a sample preparation device for sample preparation, obtaining a kerogen sample,
step S40: and calculating to obtain the elastic modulus of the kerogen according to the longitudinal wave velocity, the transverse wave velocity and the density of the kerogen sample.
2. The kerogen modulus of elasticity test method as claimed in claim 1, wherein the step S30 comprises the following sub-steps:
step S31: putting the kerogen into a sample preparation device, and loading pressure at two ends of the sample preparation device;
step S32: keeping the pressure for a certain time, measuring the longitudinal wave velocity and the transverse wave velocity of the kerogen, and if the difference between the longitudinal wave velocity and the transverse wave velocity measured for the nth time and the longitudinal wave velocity and the transverse wave velocity measured for the (n-1) th time is less than 1%, obtaining the ending loading pressure and obtaining the kerogen sample; otherwise, step S31 is repeated.
3. The kerogen modulus of elasticity test method of claim 2, wherein the pressure is maintained for at least 1 hour or more in step S32.
4. The kerogen modulus of elasticity test method according to any one of claims 1 to 3, characterized in that step S10 comprises the following sub-steps:
step S11: obtaining a shale sample in a research area, and grinding the shale sample into powder;
step S12: adding non-oxidation acid liquor into the shale sample powder, and reacting to obtain a first intermediate solution;
step S13: washing the first intermediate solution with distilled water to obtain a neutral second intermediate solution;
step S14: adding alkali liquor into the second intermediate solution, and reacting to obtain a third intermediate solution;
step S15: and washing the third intermediate solution with distilled water, and obtaining a neutral mixed solution after reaction.
5. The kerogen elastic modulus test method according to any one of claims 1 to 3, characterized in that the non-oxidizing acid liquid is hydrochloric acid with a concentration of 6 mol/L.
6. The kerogen elastic modulus test method according to any one of claims 1 to 3, characterized in that the alkali solution is a sodium hydroxide solution with a concentration of 0.5 mol/L.
7. The method for testing elastic modulus of kerogen according to claim 4, wherein in step S12, the mixing ratio of the shale sample powder and the non-oxidizing acid solution is 1 g: 6 mL.
8. The method for testing elastic modulus of kerogen according to claim 4, wherein in step S12, a non-oxidizing acid solution is added to the shale sample powder and reacted for at least 2 hours.
9. The method for testing elastic modulus of kerogen according to claim 4, wherein in step S14, alkali solution is added to the second intermediate solution and reacted for at least 1 h.
10. The kerogen modulus of elasticity test method according to claim 2 or 3, characterized in that step S20 comprises the following sub-steps:
step S21: centrifuging the mixed solution to layer and removing a solid part;
step S21: and baking the solid part to remove water to obtain the kerogen.
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