CN113945444A - Solvent extraction method for hydrocarbon substances in trace rock sample - Google Patents
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- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 53
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 52
- 239000011435 rock Substances 0.000 title claims abstract description 44
- 239000004215 Carbon black (E152) Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000000126 substance Substances 0.000 title claims abstract description 35
- 238000000638 solvent extraction Methods 0.000 title claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 42
- 239000000284 extract Substances 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 17
- 238000000197 pyrolysis Methods 0.000 claims abstract description 14
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 24
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 230000005284 excitation Effects 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 9
- 238000011156 evaluation Methods 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000003079 shale oil Substances 0.000 abstract description 4
- 238000011002 quantification Methods 0.000 abstract description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 19
- 239000002904 solvent Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 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
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention relates to a solvent extraction method of hydrocarbon substances in trace rock samples, and relates to the technical field of solvent extraction. The solvent extraction method comprises the steps of grinding a trace amount of rock sample, adding an organic solvent, sealing and soaking, performing ultrasonic treatment and centrifuging to obtain an extract liquor, wherein the trace amount is less than 1 g; performing fluorescence quantitative analysis on the extract liquor, and determining the oil concentration; when the oil concentration of the extraction liquid is more than 0.01mg/L, repeating the extraction steps in the steps; otherwise, finishing the extraction to obtain the hydrocarbon substances. The solvent extraction method disclosed by the invention fills the blank of extracting hydrocarbon substances in a trace sample by using an organic solvent, can realize accurate quantification of oil content of shale and analysis of composition of the hydrocarbon substances in the shale by combining extract pyrolysis analysis and extract chromatographic analysis, and strongly supports exploration and evaluation of the shale oil. The method disclosed by the invention is simple to operate, small in time consumption, small in organic solvent consumption and environment-friendly, and can be used for batch treatment.
Description
Technical Field
The invention relates to the technical field of solvent extraction, in particular to a solvent extraction method for hydrocarbon substances in trace rock samples.
Background
Formation rock samples contain varying amounts of petroleum components with important geological information about the source of the hydrocarbons and their characteristics. The method for obtaining the petroleum component in the rock mainly comprises two methods of solvent extraction and heating extraction. The solvent extraction method in the petroleum industry generally adopts normal hexane, dichloromethane or chloroform and the like as solvents to dissolve out hydrocarbon substances in the rock sample, the industrial standard SY/T5118-. The heating extraction method is generally connected with a gas chromatograph or a chromatograph-mass spectrometer on line, and the rock powder sample releases contained hydrocarbon substances under the action of a heating furnace and is blown to on-line connected instrument equipment by carrier gas for detection. The method obtains all volatile hydrocarbon substances in the rock, and the proportion of the components of the volatile hydrocarbon substances is greatly different from that of the components of the actually exploited hydrocarbon, so that the light hydrocarbon fingerprint of the extract is obviously different from that of the crude oil, and the contrast research is influenced.
In the evaluation of oil content in shale, solvent extraction and rock pyrolysis methods (similar to heating extraction, but the experimental temperature is higher than that of heating extraction) are generally adopted to obtain the quality of petroleum contained in a unit shale sample. Solvent extraction methods that require volatilization of the organic solvent at a temperature that results in the concurrent evaporative loss of low molecular weight hydrocarbons are not widely used. Rock pyrolysis methods, combined with wellsite frozen-fracturing, have enabled the detection of oil content in shale samples at the drilling site, and have been widely adopted over the past few years. However, the phenomenon that high molecular weight hydrocarbons and kerogen cracking hydrocarbons volatilize simultaneously exists in the pyrolysis temperature range of 300-450 ℃, so that great errors exist in the evaluation of the content of the shale-bound hydrocarbons. In this case, the organic solvent extraction method can exert an effective effect, and can accurately quantify the content of residual hydrocarbons in the sample after the 300 ℃ pyroelectric analysis.
The existing solvent extraction method (SY/T5118-. Although the heating extraction method is suitable for trace samples, organic matters are cracked to generate new hydrocarbon substances in the heating process, and the possibility of changing the original hydrocarbon information appearance in rock samples exists, so that the current shale oil exploration and evaluation is influenced.
Disclosure of Invention
In order to solve the technical problem, the invention provides a solvent extraction method of hydrocarbon substances in trace rock samples. By extracting trace (<1g) hydrocarbon substance solvent in the shale sample, the chromatographic analysis of the extract can be carried out to know the hydrocarbon composition information in the shale; and carrying out pyrolysis analysis on the extracted rock powder, accurately quantifying the oil content of the shale, and determining the content of the residual hydrocarbon.
The invention aims to provide a solvent extraction method of hydrocarbon substances in trace rock samples, which comprises the following steps,
(1) grinding a trace rock sample, adding an organic solvent, sealing and soaking, performing ultrasonic treatment and centrifuging to obtain an extract liquor, wherein the trace is less than 1 g;
(2) performing fluorescence quantitative analysis on the extraction liquid in the step (1) to determine the oil concentration;
when the oil concentration of the extraction liquid is more than 0.01mg/L, repeating the extraction step in the step (1); otherwise, finishing the extraction to obtain the hydrocarbon substances.
Further, in the step (1), the grinding is to make the rock sample particle size less than 0.18 mm.
Further, in the step (1), the organic solvent is one or more of n-hexane, dichloromethane, methanol and chloroform.
Further, in the step (1), the soaking time is 1-2 h.
Further, in the step (1), the mass ratio of the rock sample to the organic solvent is 1: 10-14.
Further, in the step (2), the fluorescence quantitative analysis is to irradiate the extract liquor by using a wide ultraviolet light source, wherein the excitation wavelength of the ultraviolet light source is 250nm-350 nm.
Further, in step (2), the oil concentration of the extract is determined by the equation Co ═ a × F-b, Co represents the oil concentration, F represents the emission fluorescence intensity of the extract, and a and b are two coefficients.
Further, there are two determination methods for the coefficients a and b. One is to cite the calibration equations disclosed in us patent 4977319, a being 0.7952, b being 1.5101; the other is determined by fitting a correlation curve between the oil concentration and the fluorescence intensity, and particularly by measuring the fluorescence intensity emitted by a plurality of extracts with known oil concentrations, and establishing a correlation equation between the oil concentration and the fluorescence intensity.
Further, the emitted fluorescence intensity is the intensity of the fluorescence emitted by the irradiated extraction liquid at the wavelength of 200nm-400 nm.
Further, the method also comprises the step of volatilizing the organic solvent of the extract liquid after the extraction is finished.
Further, the volatilization temperature is 60-80 ℃.
Further, under the same conditions, the difference between two weighing at 30min intervals was less than 0.2mg, which was regarded as constant weight.
Further, the steps of carrying out chromatographic analysis on the extract liquor and carrying out pyrolytic analysis on the extracted rock powder are also included after the extraction is finished.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the solvent extraction method of the hydrocarbon substances fills the blank of extracting the hydrocarbon substances in a trace sample by the organic solvent, avoids generating new hydrocarbon substances by cracking organic matters by combining extract pyrolysis analysis and extract chromatographic analysis, can realize accurate quantification of oil content of shale and analysis of the composition of the hydrocarbon substances, and strongly supports current shale oil exploration and evaluation.
(2) The solvent extraction method of the hydrocarbon substances uses the sample amount not more than 1g, widens the application range of the solvent extraction method, has simple operation, batch treatment and less time consumption, and improves the working efficiency.
(3) The solvent extraction method of the hydrocarbon substances has the advantages of low organic solvent consumption and environmental friendliness.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the present disclosure taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a flow diagram of a process for solvent extraction of hydrocarbonaceous material according to the invention.
FIG. 2 is a chromatogram of a methylene chloride extract of a shale sample (0.9g) from the Mount-orou group of example 1 according to the present invention.
FIG. 3 is a chromatogram of a methylene chloride extract after 300 ℃ heat release of a shale sample (0.6g) from the Mount Qingshan group of example 2 in accordance with the present invention.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
Referring to fig. 1, a method for extracting hydrocarbon substances from a trace amount of rock sample by using a solvent comprises the following steps:
a sample of shale (0.9g) was ground by hand to a particle size of less than 0.18mm and loaded into a 10mL glass centrifuge tube after grinding.
The tube was centrifuged and organic solvent dichloromethane was added to 8mL mark, then sealed and the rock sample soaked for 2 h.
The centrifuge tube with the rock sample and solvent was transferred to an ultrasonic cleaner, sonicated for 15min, and then centrifuged for 5 min.
And (3) carrying out fluorescence quantitative analysis on the upper layer of extraction liquid, irradiating the extraction liquid by adopting a wide ultraviolet light source with the excitation wavelength of 250nm-350nm, and measuring the emission fluorescence intensity of the extraction liquid with the wavelength of 200nm-400 nm. The fluorescence intensity of the extract was measured to be 2.04, as shown in formula CoThe oil concentration was calculated to be 0.112mg/L, greater than 0.01mg/L at 0.7952 × F-1.5101, and the rock samples required re-extraction.
The upper extract of the tube was transferred to the flask containing the last extract by a pipette.
Repeating the above operations until the oil concentration of the upper layer extractive solution is CoLess than 0.01mg/L, and the extraction is completed.
The chromatographic bottle containing the extract is placed in an environment at 60 ℃ in an open manner, and the solvent is volatilized to dryness. Under the same conditions, the difference between the two weighing times at 30min intervals was 0.1mg, which was regarded as constant weight.
Example 2
Referring to fig. 1, a method for extracting hydrocarbon substances from a trace amount of rock sample by using a solvent comprises the following steps:
selecting four standard solutions with known oil concentrations of 0.01mg/L, 0.5mg/L, 1mg/L and 5mg/L respectively, sequentially irradiating the standard solutions by adopting a wide ultraviolet light source with an excitation wavelength of 250-350 nm, and measuring the emission fluorescence intensities of the standard solutions with the wavelengths of 200-400 nm to be 1.90, 2.55, 3.15 and 8.25 respectively, so that a correction curve C between the oil concentration and the fluorescence intensities is obtainedo＝0.7867*F-1.49。
A sample of shale (0.6g) was ground by hand to a particle size of less than 0.18mm and loaded into a 10mL glass centrifuge tube after grinding.
And adding a mixed solution of 90% dichloromethane and 10% methanol serving as an organic solvent into the centrifugal test tube to 6mL mark, sealing, and soaking the rock sample for 1.5 h.
The centrifuge tube with the rock sample and solvent was transferred to an ultrasonic cleaner, sonicated for 15min, and then centrifuged for 5 min.
And (3) carrying out fluorescence quantitative analysis on the upper layer of extraction liquid, irradiating the extraction liquid by adopting a wide ultraviolet light source with the excitation wavelength of 250nm-350nm, and measuring the emission fluorescence intensity of the extraction liquid with the wavelength of 200nm-400 nm. The fluorescence intensity of the extract was measured to be 1.95, as shown in formula CoThe oil concentration was calculated to be 0.044mg/L, greater than 0.01mg/L at 0.7867F-1.49 and the rock samples required re-extraction.
The upper extract of the tube was transferred to the flask containing the last extract by a pipette.
Repeating the above operations until the oil concentration of the upper layer extractive solution is CoLess than 0.01mg/L, and the extraction is completed.
The chromatographic bottle containing the extract is placed in an environment at 60 ℃ in an open manner, and the solvent is volatilized to dryness. Under the same conditions, the difference between the two weighing times at 30min intervals was 0.15mg, which was regarded as a constant weight.
Example 3
Referring to fig. 1, a method for extracting hydrocarbon substances from a trace amount of rock sample by using a solvent comprises the following steps:
a batch (13 groups) of shale samples of the Qingshan mountain mouth group are taken, and the mass of the samples is between 0.6 and 1.0 g. Each sample was hand ground to a particle size of less than 0.18mm and samples were taken at 0.4-0.6g of ground sample in 10mL glass centrifuge tubes. Taking 0.08g of each sample to perform rock pyrolysis analysis, keeping the pyrolysis program constant at 300 ℃ for 3min, and detecting S1Then raising the temperature to 600 ℃ at a speed of 25 ℃/min for a constant time of 1min, and detecting S2。
And sequentially adding chloroform solvents into the centrifugal test tube to 4.5mL scales, sealing, and soaking the rock sample for 1 h.
The centrifuge tube with the rock sample and solvent was transferred to an ultrasonic cleaner, sonicated for 15min, and then centrifuged for 5 min.
And (3) carrying out fluorescence quantitative analysis on the upper layer of extraction liquid, irradiating the extraction liquid by adopting a wide ultraviolet light source with the excitation wavelength of 250nm-350nm, and measuring the emission fluorescence intensity of the extraction liquid with the wavelength of 200nm-400 nm. The fluorescence intensity of the extract from each sample was measured in turn, according to formula C in the examplesoThe oil concentration of each extract was calculated at 0.7867 × F-1.49 and compared at 0.01mg/L, and rock samples greater than 0.01mg/L were re-extracted until the oil concentration of the extract was less than 0.01mg/L and extraction was complete.
And (4) placing the extracted glass test tube in an open environment at 65 ℃ to volatilize the solvent in the rock sample to be dry. Under the same conditions, the difference between two weighing times at an interval of 30min is less than 0.2mg, and the weight is regarded as constant.
Test example
Referring to FIG. 1, the organic matter extracted from the chromatographic flask of examples 1-2 was redissolved in methylene chloride and analyzed by composition chromatography. The test example adopts Agilent 7890B gas chromatograph, HP-PONA chromatographic column (length 50m, inner diameter 0.2mm, film thickness 0.5 μm), and initial temperature of 40 deg.C and constant temperature of 12min, then the temperature is raised to 310 ℃ at the speed of 3.5 ℃/min, and the temperature is kept for 29 min. FIG. 2 is a chromatogram of 0.9g of original sample of the Qingshan mountain shale for extracting organic matters, and FIG. 3 is a chromatogram of 0.6g of original sample of the Qingshan mountain shale for extracting organic matters after constant temperature heat release for 12min at 300 ℃. FIG. 2 and FIG. 3 show the change of organic solvent extract before and after 300 deg.C heat release of trace shale sample, the content of normal alkane is reduced significantly, and the sample after heat release contains no C20Formerly normal paraffins, small amounts of heavy hydrocarbons remained.
Referring to FIG. 1, rock pyrolysis analysis was performed on the chloroform-extracted shale sample of the Qingshan Kong group of example 3, the pyrolysis procedure was 300 ℃ for 3min, and S was measured1Then raising the temperature to 600 ℃ at a speed of 25 ℃/min for a constant time of 1min, and detecting S2. Wherein S1The value represents the hydrocarbon content per unit of shale measured at 300 ℃, which is generally considered to be the free hydrocarbon content, S, in shale2The values represent the hydrocarbon content per unit of shale detected at 600 ℃ and 300-2Peak height corresponds to pyrolysis temperature.
The pyrolysis parameters of the shale samples before and after chloroform extraction are shown in table 1:
TABLE 1
As can be seen from Table 1, the pyrolysis parameters before and after the extraction of the shale sample of the Qingshan Kou group are obviously changed. Shale sample S after extraction1The value dropped sharply, leaving only sample S before extraction12-7% of value, S2The value likewise produced a significant drop, for sample S before extraction2The value was 53-78%. Due to S2The influence of soluble organic substances is removed, and the Tmax is higher than that of a sample before extraction by 2-7 ℃.
Solvent extraction method for hydrocarbon substances in trace sample in shale oil content evaluationMethod for determining S2S remaining in (1)1Has obvious advantages. S2S remaining in1Mainly hydrocarbons with high molecular weight and hydrocarbons bound by organic matters or minerals, the solvent extraction method can effectively separate the substances, and the kerogen cracking hydrocarbon and S in the pyrolysis temperature range of 300 ℃ and 450 DEG C1Residual hydrocarbons are produced simultaneously, with an overlap effect, which leads to S2Middle S1Residual hydrocarbon evaluation is inaccurate.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (10)
1. A solvent extraction method of hydrocarbon substances in trace rock samples is characterized by comprising the following steps,
(1) grinding a trace rock sample, adding an organic solvent, sealing and soaking, performing ultrasonic treatment and centrifuging to obtain an extract liquor, wherein the trace is less than 1 g;
(2) performing fluorescence quantitative analysis on the extraction liquid in the step (1) to determine the oil concentration;
when the oil concentration of the extraction liquid is more than 0.01mg/L, repeating the extraction step in the step (1); otherwise, finishing the extraction to obtain the hydrocarbon substances.
2. A method for the solvent extraction of trace amounts of hydrocarbon substances from rock samples as claimed in claim 1, wherein in step (1) the grinding is carried out to a particle size of the rock sample of less than 0.18 mm.
3. The method for solvent extraction of hydrocarbon substances in trace rock samples according to claim 1, wherein in the step (1), the organic solvent is one or more of n-hexane, dichloromethane, methanol and chloroform.
4. The method for solvent extraction of hydrocarbon substances in trace rock samples as claimed in claim 1, wherein in step (1), the soaking time is 1-2 h.
5. The method for solvent extraction of hydrocarbon substances in trace rock samples according to claim 1, wherein in the step (2), the fluorescence quantitative analysis is performed by irradiating the extract with a broad ultraviolet light source having an excitation wavelength of 250nm to 350 nm.
6. The method for solvent extraction of hydrocarbon substances in trace rock samples according to claim 1, wherein in step (2), the oil concentration of the extraction liquid is determined by equation Co＝a*F-b，CoRepresenting the oil concentration, F the emitted fluorescence intensity of the extract, and a and b are two coefficients.
7. The method of claim 6, wherein the fluorescence emission intensity is an intensity of a fluorescence emitted from the irradiated extract solution at a wavelength of 200nm to 400 nm.
8. The method of claim 1, further comprising volatilizing the organic solvent from the extracted fluid after the extraction is completed.
9. A method as claimed in claim 8, wherein the temperature of the volatilisation is in the range 60-80 ℃.
10. The method of claim 1, further comprising analyzing the extracted liquid by chromatography and the extracted rock powder by pyrolysis after the extraction.
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| CN114965792A (en) * | 2022-06-14 | 2022-08-30 | 宁夏滨泽新能源科技有限公司 | Analysis method for rapidly detecting content of C4-C22 alkane |
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