CN113504257A - Method for detecting oil content of shale - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000001514 detection method Methods 0.000 claims abstract description 40
- 238000000197 pyrolysis Methods 0.000 claims abstract description 36
- 238000004458 analytical method Methods 0.000 claims abstract description 27
- 239000011435 rock Substances 0.000 claims abstract description 26
- 239000003960 organic solvent Substances 0.000 claims abstract description 24
- 238000000638 solvent extraction Methods 0.000 claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical group ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000010998 test method Methods 0.000 claims 1
- 229930195733 hydrocarbon Natural products 0.000 abstract description 66
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 238000005336 cracking Methods 0.000 abstract description 4
- 230000000717 retained effect Effects 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 47
- 239000004215 Carbon black (E152) Substances 0.000 description 46
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000003079 shale oil Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
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Abstract
The invention discloses a method for detecting oil content of shale, which comprises the following steps: collecting the core by adopting a closed coring method; detecting the oil content of the core at a well site; taking a part of the core sample subjected to oil content detection for pyrolysis analysis; extracting part of the core sample subjected to oil content detection with an organic solvent; carrying out pyrolysis analysis on the core sample subjected to organic solvent extraction; comparing the pre-extraction pyrolysis analysis peak obtained after the step S3 with the post-extraction pyrolysis analysis peak obtained after the step S5; and calculating to obtain the total oil content of the core sample. According to the invention, the loss of hydrocarbons of the sample in the surface process is avoided through closed coring, and the information of low carbon number hydrocarbons in the sample is retained; and the contents of high-carbon-number hydrocarbons and bound hydrocarbons in the sample can be accurately determined by performing pyrolysis analysis on the rock before and after the sample is subjected to organic solvent extraction, so that the problem of overlapping of pyrolysis temperatures of the bound hydrocarbons and kerogen cracking hydrocarbons is solved.
Description
Technical Field
The invention relates to the technical field of oil and gas resource evaluation, in particular to a shale oil content detection method.
Background
From the perspective of global energy structure change, the exploration and evaluation of shale oil and dense oil resources are increasingly important. The shale oil reservoir contains two kinds of organic matters, namely soluble organic matters and kerogen. Kerogen, as a parent hydrocarbon, is an organic compound that is insoluble in organic solvents. When the source rock undergoes deep formation, kerogen thermally cracks to generate soluble organic matter. As the deep-seated effect increases, the organic compounds in the crude oil further crack to produce smaller molecular compounds. The organic substances produced by kerogen are partially dissolved in kerogen, and the rest is discharged into adjacent mineral interparticle pores. Thus, the crude oil in the shale layer system is mainly in three types of occurrence, a kerogen-dissolved phase, a mineral particle adsorption phase and a pore-free phase, which may be combined to be referred to as a bound phase.
Petroleum geochemists generally describe petroleum that can be extracted from hot mature hydrocarbon source rock with an organic solvent, the extracted organic matter being an organic mixture generated from and retained in the hydrocarbon source rock. Therefore, the solvent extraction method is one of the popular methods for obtaining the oil content of the rock, and another commonly adopted method is to use a temperature programmed pyrolysis method to characterize the oil content of the rock by a source rock analyzer or a rock pyrolysis analyzer.
With the exploration of shale oil and tight oil resources, solvent extraction methods and rock pyrolysis methods are being used to evaluate the oiliness of shale or tight sandstone. In order to avoid the great loss of light hydrocarbons during the surface circulation of the core sample, liquid nitrogen freezing is widely adopted. The core sample is frozen with liquid nitrogen at the well site and returned to the laboratory where organic solvent is used to extract all soluble organic matter in the core sample. The loss of hydrocarbons in the extraction process is reduced by adopting a block sample and closed crushing. However, the fatal defect of the method is that the extracted hydrocarbons are not volatilized when the organic solvent is removed by drying, because the organic solvent and the light hydrocarbon in the extract have similar boiling points.
The core sample can be stored in a liquid nitrogen environment (most conditions are stored in a refrigerator) at a well site, then the core sample is sequentially sampled and frozen and crushed in the liquid nitrogen environment, a small amount of powder sample is taken for temperature programming to volatilize or pyrolyze soluble and insoluble organic matters, and the hydrocarbon content generated under different temperature conditions is measured for estimating the oil content of the shale sample. Although the sample is stored and crushed under the low-temperature condition, the volatilization loss of light hydrocarbon substances is still caused by the non-closed environment. A further disadvantage is that the temperature program does not accurately distinguish between the bound and pyrolyzed hydrocarbons because there is an overlap between the two in the temperature range of 300-600 ℃.
Disclosure of Invention
In view of this, the main objective of the present invention is to provide a method for detecting oil content in shale.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the method for detecting the oil quantity of the shale well site comprises the following steps:
s1, collecting a rock core, collecting a sample of the rock core and storing the sample;
step S2, detecting the oil content of the core sample;
step S3, taking a part of the core sample which is subjected to oil content detection to perform pyrolysis analysis;
s4, extracting another part of the core sample subjected to oil content detection with an organic solvent;
step S5, carrying out pyrolysis analysis on the core sample subjected to organic solvent extraction;
step S6, comparing the peak value of the pyrolysis analysis before extraction obtained after the step S3 with the peak value of the pyrolysis analysis after extraction obtained after the step S5;
and step S7, calculating to obtain the total oil content of the core sample.
In one embodiment, the method for collecting the core in step S1 is closed coring, and the core subjected to closed coring is stored in a closed sample tank after sample collection.
In one embodiment, step S2 further includes subjecting the core sample to a crushing process.
In one embodiment, the methods of steps S1 and S2 are performed at the wellsite, with subsequent steps being performed in a laboratory.
In one embodiment, the oil content detection in step S2 employs a temperature programming method.
In one embodiment, the maximum temperature for the oil content test described in step S2 is 300 ℃.
In one embodiment, the oil content detection described in step S2 uses a hydrogen flame ionization detector to determine oil content.
In one embodiment, the organic solvent in step S4 is dichloromethane, methanol, or chloroform.
In one embodiment, step S4 further includes low temperature drying to remove the organic solvent.
According to the method for detecting the oil content of the shale, disclosed by the invention, the fresh core sample well field is processed and detected in a whole closed environment, so that hydrocarbon loss is avoided to the greatest extent, the most real rock free hydrocarbon content is obtained, and the problem of hydrocarbon loss of different degrees in the known method is solved. On the other hand, the rock pyrolysis analysis before and after the organic solvent extraction is carried out on the sample subjected to the oil content analysis of the well site, so that the content of the high-carbon-number hydrocarbon and the content of the bound hydrocarbon in the sample can be accurately determined, and the problem of the overlapping of the pyrolysis temperature of the bound hydrocarbon and the pyrolysis temperature of the kerogen cracking hydrocarbon is solved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a diagram: the invention discloses a flow chart of a method for detecting oil content in shale, which is disclosed by an embodiment of the invention;
FIG. 2 is a diagram of: a wellsite oil content detection profile according to one embodiment of the present disclosure;
FIG. 3 is a diagram of: the pyrolysis profile of the sample after oil content detection before solvent extraction according to one embodiment of the present invention;
FIG. 4 is a diagram of: the pyrolysis profile of the sample after solvent extraction after oil content detection is described in one embodiment of the present invention.
Detailed Description
The method of the present invention will be described in further detail below with reference to the accompanying drawings and embodiments of the invention.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those illustrated or otherwise described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
In this embodiment, a shale oil content detection method is provided by taking the shale of the Qingshan Kou group in the Songliao basin as an example. Fig. 1 is a flowchart of a method for detecting oil content in shale according to the present invention, which includes:
and S1, collecting the rock core, and storing the rock core after the sample is collected.
In one embodiment of the invention, the method for collecting the rock core is closed coring, and the closed coring operation can protect the rock core by using a closed liquid in the formation process of the rock core so as to prevent the rock core from being soaked and polluted by the filtrate of the drilling fluid. In other embodiments of the invention, cores may be collected by conventional coring, but the hydrocarbon loss during tripping may need to be assessed and carried over into the calculations for subsequent steps to achieve the same result.
To avoid loss of hydrocarbons from the core collected, the fresh core from the closed core is collected and weighed and then stored closed in a closed sample tank. The weight of the sample is preferably 1-2 g, so that the sample is not accumulated in the tank to influence the heat release effect of the hydrocarbons, and the sample amount meets the requirement of subsequent analysis on the sample amount.
The core is collected in moderate quantities that would otherwise have an effect on the detection due to the heat release of the hydrocarbon material. In one embodiment of the invention, the core has a collection weight of 1-2 grams, which ensures that the sample is not accumulated in the tank to affect the hydrocarbon heat release effect and also ensures that the sample amount meets the requirements of subsequent analysis on the sample amount.
And step S2, detecting the oil content of the core sample.
In order to improve the heat release effect of hydrocarbons, in one embodiment of the invention, the core sample stored in the closed sample tank is subjected to crushing treatment, which can facilitate oil content detection and further pyrolysis analysis of the core.
In one embodiment of the invention, the oil content of the core sample is detected by a temperature programming method and a hydrogen flame ionization detector. The temperature programming process comprises the following steps: keeping the temperature at 5 ℃ for 3 minutes, increasing the temperature to 90 ℃ at a heating rate of 50 ℃/min, keeping the temperature for 5 minutes, increasing the temperature to 300 ℃ at a heating rate of 50 ℃/min, and keeping the temperatureFor 12 minutes. The maximum detection temperature is 300 ℃. FIG. 2 is a heat release spectrum of a core in a well site, wherein three heat release peaks S are obtained in three temperature stagesg、S0And S1-1In which S isgRepresents the hydrocarbon content per unit mass of shale measured at 5 ℃; s0Represents the hydrocarbon content of the shale with unit mass detected at 5-90 ℃; s1-1Representing the hydrocarbon content per unit mass of shale measured at 90-300 ℃.
To further increase the accuracy of the test, in one embodiment of the invention, the oil content of the core sample is tested in a fully enclosed environment, so that in combination with the closed coring technique, hydrocarbon losses, especially gaseous hydrocarbons and light hydrocarbons, are largely avoided. Further preferably, the fully enclosed inspection environment is located directly at the well site, thus avoiding hydrocarbon loss over long periods of transportation.
In one embodiment of the invention, the oil content of the sample obtained by closed coring in the Qingshan mountain wellsite of Songliao basin is detected, and the detection results are obtained as shown in the following table:
the sample subjected to oil content detection in the well site has no hydrocarbon loss phenomenon, so that the sample can be sent back to a laboratory in a closed environment for continuous detection, and more accurate information on the oil content of the core can be obtained.
And step S3, taking part of the core sample which is subjected to oil content detection to perform pyrolysis analysis.
And taking a certain amount of core samples which are subjected to oil content detection of the well site. In one embodiment of the invention, the core sample for pyrolytic analysis has an amount of 100mg or less, preferably 50 mg.
The rock pyrolysis analysis also adopts a temperature programming method, and adoptsThe hydrogen flame ionization detector measures the oil content. The temperature programming process comprises the following steps: keeping the temperature at 300 ℃ for 3 minutes, and then heating to 600 ℃ at the heating rate of 25 ℃/min and keeping the temperature for 1 minute. The detection spectrum is shown in FIG. 3. Detecting the residual oil content in the rock core sample at the constant temperature of 300 ℃, and detecting the kerogen cracking hydrocarbon content in the rock core sample at the temperature of 300-600 ℃. Since this is the second detection that the same core sample undergoes, the pyrolysis peak is labeled S, respectively1-2And S2-2Denotes S of the second detection1And S2The value is obtained.
And step S4, extracting part of the core sample subjected to oil content detection with an organic solvent.
In order to improve the efficiency of extraction, in one embodiment of the present invention, the organic solvent is dichloromethane, methanol or chloroform because the organic solvent has a stronger polarity and a lower boiling point. The organic matter extracted from the core sample comprises S1-1Residual, high carbon number hydrocarbons and bound hydrocarbons. In one embodiment of the invention, the solvent extraction operation is performed according to SY/T5118-2005 industry standard. Preferably, after extraction is complete, the core sample is dried at 80 ℃ for 2 hours to remove the organic solvent.
And step S5, carrying out pyrolysis analysis on the core sample subjected to organic solvent extraction.
In one embodiment of the present invention, the pyrolytic analysis method is the same as step S3, since this is the third detection that the same core sample undergoes, and thus the pyrolytic peaks are labeled S, respectively1-3And S2-3Denotes S of the third detection1And S2The value is obtained. FIG. 4 shows the pyrolysis spectrum of a core sample after organic solvent extraction.
And step S6, comparing the peak value of the pyrolysis analysis before extraction obtained after the step S3 with the peak value of the pyrolysis analysis after extraction obtained after the step S5.
The sample after solvent extraction is pyrolyzed S due to the removal of high carbon number hydrocarbons and bound hydrocarbons2The peaks reflect only the kerogen-cracked hydrocarbon content. The bound hydrocarbon content of the high carbon number hydrocarbons in the sample can be determined by comparing the pyrolysis peaks of the same sample before and after extraction.
In one practice of the invention, the pyrolysis data of core samples before and after extraction is shown in the following table:
comparing the pyrolysis parameters of the core sample before and after extraction to determine the content of the residual free hydrocarbon in the core sample after the oil content detection of the well site as (S)1-2-S1-3) The content of the high carbon number hydrocarbon and the bound hydrocarbon is (S)2-2-S2-3)。
And step S7, calculating to obtain the total oil content of the core sample.
The main constituent of petroleum is hydrocarbons, so the hydrocarbon content reflects the oil content of shale, i.e., the petroleum content of shale. In one embodiment of the present invention, the total oil content TOY of the core sample can be calculated by the following formula:
TOY＝Sg+S0+S1-1+(S1-2-S1-3)+(S2-2-S2-3)。
wherein S isgRepresents the hydrocarbon content per unit mass of shale measured at 5 ℃, obtained from the first oil content measurement of step S2;
S0represents the hydrocarbon content of the shale with unit mass detected at 5-90 ℃, and is obtained by the first detection of the step S2;
S1-1represents the hydrocarbon content in the shale of unit mass detected at 90-300 ℃, which is obtained by the first detection of the step S2;
S1-2the hydrocarbon content in the shale of unit mass obtained by detecting the unextracted sample at the constant temperature of 300 ℃ after the first oil content detection is shown, and the hydrocarbon content is obtained by the second detection in the step S3;
S2-2the hydrocarbon content in the shale of unit mass obtained by detecting the unextracted sample at 300-600 ℃ after the first oil content detection is shown, and the hydrocarbon content is obtained by the second detection in the step S3;
S1-3shows the sample after solvent extraction after the first oil content measurementDetecting the hydrocarbon content in the shale of unit mass at the constant temperature of 300 ℃, wherein the hydrocarbon content is obtained by the third detection in the step S5;
S2-3which represents the hydrocarbon content per unit mass of shale obtained by testing the sample at 300-600 ℃ after the solvent extraction after the first oil content test, is obtained by the third test in step S5.
According to the method for detecting the oil content of the shale, disclosed by the invention, the fresh core sample well field is processed and detected in a whole closed environment, so that hydrocarbon loss is avoided to the greatest extent, the most real rock free hydrocarbon content is obtained, and the problem of hydrocarbon loss of different degrees in the known method is solved. On the other hand, the rock pyrolysis analysis before and after the organic solvent extraction is carried out on the sample subjected to the oil content analysis of the well site, so that the content of the high-carbon-number hydrocarbon and the content of the bound hydrocarbon in the sample can be accurately determined, and the problem of the overlapping of the pyrolysis temperature of the bound hydrocarbon and the pyrolysis temperature of the kerogen cracking hydrocarbon is solved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (9)
1. The method for detecting the oil content of the shale is characterized by comprising the following steps of:
s1, collecting a rock core, collecting a sample of the rock core and storing the sample;
step S2, detecting the oil content of the core sample;
step S3, taking a part of the core sample which is subjected to oil content detection to perform pyrolysis analysis;
s4, extracting another part of the core sample subjected to oil content detection with an organic solvent;
step S5, carrying out pyrolysis analysis on the core sample subjected to organic solvent extraction;
step S6, comparing the peak value of the pyrolysis analysis before extraction obtained after the step S3 with the peak value of the pyrolysis analysis after extraction obtained after the step S5;
and step S7, calculating to obtain the total oil content of the core sample.
2. The detection method according to claim 1, wherein in the step S1, the core is collected by closed coring, and the closed cored core is collected and stored in a closed sample tank.
3. The method for testing as claimed in claim 1, wherein in step S2, further comprising subjecting the core sample to a crushing process.
4. The method of testing as claimed in claim 1, wherein steps S1 and S2 are performed at a well site.
5. The method of claim 1, wherein the oil content detection of step S2 is performed by a temperature programmed method.
6. The method of claim 1, wherein the maximum temperature of the oil content test of step S2 is 300 ℃.
7. The method of claim 1, wherein the oil content detection of step S2 is performed by a hydrogen flame ionization detector to determine the oil content.
8. The detection method according to claim 1, wherein in the step S4, the organic solvent is dichloromethane, methanol or chloroform.
9. The detection method according to claim 1, wherein the step S4 further comprises low-temperature drying to remove the organic solvent.
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| CN113433202A (en) * | 2021-06-28 | 2021-09-24 | 数皮科技(湖北)有限公司 | Method for calculating oil content of shale oil in drilling field |
| CN113945444A (en) * | 2021-10-28 | 2022-01-18 | 科正检测(苏州)有限公司 | Solvent extraction method for hydrocarbon substances in trace rock sample |
| CN114755256A (en) * | 2022-04-20 | 2022-07-15 | 西南石油大学 | Method for evaluating oil content of shale based on different lithofacies of shale |
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