CN107290204B - Oil washing method for oil-based mud polluted rock debris - Google Patents
Oil washing method for oil-based mud polluted rock debris Download PDFInfo
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Abstract
The invention aims to provide a technology for carrying out oil washing treatment on mud rock debris polluted by oil-based mud, so that organic pollutants such as diesel oil and the like attached to the surface of the rock debris are accurately removed, the organic matter content of the washed mud rock debris is not influenced, and the technology can be used for scientific research in series of experiments of geochemical analysis and testing. The invention also provides a method for evaluating the cleaning effect of the oil-based mud polluted rock debris by using the spectrogram and parameters of the rock pyrolysis analysis, and the method effectively proves the accuracy of extracting the cleaning oil by using the equal-volume mixed liquid of ethanol and benzene, so that the polluted rock debris data can be reused in the geochemical analysis test, and the application range of the rock pyrolysis instrument is widened.
Description
Technical Field
The invention belongs to the field of geochemical analysis sample pretreatment, and particularly relates to an oil washing method for oil-based mud polluted rock debris.
Background
The main organic components of the oil-based mud are diesel oil, sulfonated asphalt, organic soil powder, an emulsifier and the like, and the oil-based mud has the advantages of high temperature resistance, salt and calcium corrosion resistance, contribution to well wall stability, good lubricity, small damage to an oil-gas layer and the like, so that the oil-based mud is more and more widely used in the drilling of easily collapsed wells, highly deviated wells and deep wells.
At present, the oil washing method for oil-based mud polluted rock debris has no current standard, the rock debris sample is mostly subjected to rough washing treatment from the environmental protection perspective, and the sample after oil washing does not meet the requirements of scientific research, test and analysis. The existing cleaning technology for the oil-based mud rock debris belongs to the field of oil-containing waste treatment of oil fields, and the oil-based mud rock debris and crude oil in silt enter a water phase after being fully mixed by directly adding an auxiliary agent into the oil-containing mud, or diesel oil in the oil-based mud is oxidized and removed by adding an oxidizing agent after the oil-based mud rock debris and the water are uniformly mixed. The cleaning technologies are all from the viewpoint of environmental protection, and the cleaned rock debris still has more or less base oil, namely diesel oil and sulfonated asphalt components, remained on the surface of the oil-based mud, and cannot be applied to scientific research in series of experiments of geochemical analysis tests. Therefore, accurate oil washing of cuttings contaminated with oil-based mud by suitable methods is of great importance in geochemical analytical testing.
Disclosure of Invention
The invention aims to provide a technology for carrying out oil washing treatment on mud rock debris polluted by oil-based mud, so that organic pollutants such as diesel oil and the like attached to the surface of the rock debris are accurately removed, and the organic matter content of the washed mud rock debris is less influenced and can be used for scientific research in series of experiments of geochemical analysis and testing.
The inventor of the invention finds that the mixed solvent selected from the conventional reagents can dissolve the oil-based mud pollutants on the surface of the rock debris and can dissolve original organic substances in the rock debris less through a plurality of experiments. The present invention is based on the above findings. The inventor determines that the oil washing effect is best by extracting with mixed liquor of ethanol and benzene with equal volume by analyzing the components of the oil-based mud and repeatedly comparing the oil washing effects of different solvents and different methods, and the combined solvent is firstly used in the method for washing the rock debris polluted by the oil-based mud. On the aspect of evaluating the oil washing effect of the solvent, the method for evaluating the cleaning effect of the oil-based mud polluted rock debris by using a spectrogram and parameters of rock pyrolysis analysis is firstly proposed, the method effectively proves the accuracy of extracting the oil washing by using mixed liquid with equal volume of ethanol and benzene, so that the polluted rock debris data can be reused in the geochemical analysis test, and meanwhile, the application range of the rock pyrolysis instrument is widened.
The invention aims to provide an oil washing method for oil-based mud polluted rock debris, which at least comprises the following steps:
an organic distillation extraction step, namely, a mixed solvent of two solvents is used for carrying out hot extraction on the oil-based mud polluted rock debris, the extraction is carried out at the temperature of 80-90 ℃, the detection is carried out simultaneously, and the cleaning completion is evaluated by combining a judgment method; one of the two solvents is ethanol or chloroform, and the other solvent is carbon tetrachloride or benzene.
Preferably, the cleaning effect judgment method judges according to the pollutant component or organic matter content index of the oil-based mud polluted rock debris; the indexes comprise the color of an extraction solution for mixing the oil-based mud polluted rock debris, the parameters of the pyrolytic analysis of the oil-based mud polluted rock debris and the spectrogram of the pyrolytic analysis of the oil-based mud polluted rock debris.
Preferably, one of the two solvents of the mixed solvent is ethanol, and the other solvent is benzene.
Further preferably, the volume ratio of the ethanol to the benzene is 1:1, and the thermal extraction is carried out at a constant temperature of 85 ℃ for 25 hours.
Still further preferably, the method comprises the following steps:
the pretreatment step, namely wrapping the oil-based mud polluted rock debris by using filter paper extracted by chloroform, and placing the wrapped rock debris into the bottom of a siphon pipe of a Soxhlet extractor; and (3) organic distillation extraction, namely adding a mixed solvent of ethanol and benzene with the volume ratio of 1:1 into the round-bottom flask or the top of a siphon tube of a Soxhlet extractor, connecting the round-bottom flask and the Soxhlet extractor, putting the round-bottom flask into a constant-temperature water bath kettle at 85 ℃, heating and extracting.
Preferably, the method further comprises the following sample selection steps:
and a sample selecting step, namely selecting viscous rock debris polluted by the oil-based mud on the drilling site, and airing for later use.
Preferably, the oil-based mud polluted rock debris is wrapped by filter paper extracted by chloroform, the wrapped oil-based mud polluted rock debris is placed at the bottom of a siphon pipe of a Soxhlet extractor, a mixed solvent of ethanol and benzene with the volume ratio of 1:1 is added into a round-bottom flask or the top of the siphon pipe of the Soxhlet extractor, the round-bottom flask and the Soxhlet extractor are connected, the round-bottom flask is placed into a constant-temperature water bath kettle at the temperature of 85 ℃ for heating and extraction, and oil stains on the surface of the oil-based mud polluted rock debris are cleaned when an extraction liquid in the siphon pipe is changed from colorless to brown yellow and then colorless and.
Preferably, the cleaning effect is evaluated by using the parameters of the pyrolytic analysis of the oil-based mud polluted rock debris; s of two adjacent analyses2、S4、TmaxThe oil stain on the surface of the oil-based mud polluted rock debris is cleaned when the relative double differences and deviations of the hydrocarbon source rock analysis in the rock pyrolysis analysis (GB/T18602-2012) are met.
Preferably, the cleaning effect is evaluated by using a spectrogram of pyrolytic analysis of oil-based mud polluted rock debris; and (3) cleaning oil stains on the surface of the oil-based mud polluted rock debris when no diesel oil characteristic peak exists in a spectrogram of the oil-based mud polluted rock debris pyrolytic analysis.
Preferably, the oil-based mud pollution rock debris is heated by the rock pyrolysis instrument for pyrolysis analysis of the oil-based mud pollution rock debris, the heating is three-stage heating, and S1: keeping the temperature at 300 ℃ for 3 min; s2: the temperature rise rate is 50 ℃/min at 300-600 ℃, and the temperature is kept constant for 1min at 600 ℃; s4: burning at 600 deg.C for 7-13 min; and quantitatively analyzing hydrocarbons and carbon dioxide released by organic matters in the oil-based mud polluted rock debris by using a hydrogen ion flame detector and a thermal conductivity detector to obtain pyrolysis parameters and a pyrolysis analysis spectrogram, wherein the pyrolysis parameters comprise free hydrocarbon S1, pyrolysis hydrocarbon S2, carbon residue S4 and Tmax.
In some embodiments, the technical solution of the present invention is: the oil washing method for the oil-based mud polluted rock debris comprises the following steps: and determining an oil washing device and a solvent. The oil-based mud polluted rock debris washing oil adopts an organic distillation extraction method, the device is a Soxhlet extractor (shown in figures 1 and 2), the solvent is a mixed solvent of ethanol or chloroform and benzene or carbon tetrachloride, and preferably, the solvent is a mixed solvent of absolute ethanol and benzene (the volume ratio is 1: 1): wrapping a rock debris sample polluted by oil-based mud with filter paper extracted by chloroform, placing the wrapped rock debris sample at the bottom of a siphon tube, adding a proper amount of combined solvent into a round-bottom flask, placing a Soxhlet extractor in a water bath kettle for heating, setting the temperature of the water bath kettle to be 85 ℃, extracting and washing oil for a plurality of times, taking out the sample, and airing.
Evaluation of oil washing effect pyrolysis experiments were carried out mainly using the model OGE-II rock pyrolysis apparatus (see FIG. 2) of the institute for oil exploration and development: crushing the dried sample to be below 100 meshes, manually feeding the sample into a pyrolysis instrument for oil-bearing rock analysis, heating the instrument by adopting three-order temperature programming, and quantitatively monitoring and analyzing hydrocarbon and carbon dioxide released by organic matters in the rock sample by a hydrogen ion flame detector (FID) and a thermal conductivity detector to obtain free hydrocarbon S1Pyrolysis of hydrocarbons S2The residual carbon amount S4And (4) waiting for the pyrolysis parameters and the pyrolysis analysis spectrogram, and evaluating the oil washing effect by observing and comparing the pyrolysis spectrogram and the measured values of the pyrolysis parameters of the sample after different extraction oil washing times.
The absolute ethyl alcohol and the benzene are analytically pure, the content of the absolute ethyl alcohol is more than or equal to 99.7 percent, the content of the benzene is more than or equal to 99.5 percent, and the absolute ethyl alcohol and the benzene are uniformly mixed according to the volume ratio of 1:1 and then are added from the top end of a siphon tube or a round-bottom flask.
The specification of the full-automatic Soxhlet extractor is as follows: 150ml serpentine condenser, 250ml siphon, 500ml round bottom flask.
Said third-order temperature-raising program S1: keeping the temperature at 300 ℃ for 3 min; s2300-600 ℃, the heating rate is 50 ℃/min, and the temperature is kept at 600 ℃ for 1 min; s4: burning at 600 deg.C for 7-13min, and the specific program parameters are shown in Table 1.
Table 1: parameter table for temperature programming of rock pyrolysis instrument
The carrier gas of the OGE-II rock pyrolysis instrument is helium, the fuel gas is hydrogen, and the air is combustion-supporting gas. The gas flow is divided into the following values: helium He flow 50ml/min, hydrogen H2 flow 28ml/min, air flow 350-.
In order to prevent improper parameter setting of the pyrolysis instrument and reduce the influence of instrument errors on pyrolysis results, the peak area of the standard sample is corrected by actually measuring the standard sample for multiple times, and the peak areas corresponding to various parameters of the standard sample are shown in table 2.
Table 2: peak area mapping table for standard parameters and correction of pyrolysis instrument
| Parameters of standard sample | Actual measurement result of standard sample | |
| S2 | 4.1 | 239508 |
| S4 | 12.6 | 132132 |
| Tmax | 437 | 425 |
The terms:
in the present invention, the sample, the oil-based mud contaminated sample, and the oil-based mud cuttings have the same meanings, and the remaining terms are preferably explained by the meaning of "rock pyrolysis analysis" (GB/T18602-2012).
The invention has the beneficial effects that:
the existing cleaning technology for the oil-based mud rock debris belongs to the field of oil-containing waste treatment of oil fields, and the oil-based mud rock debris and crude oil in silt enter a water phase after being fully mixed by directly adding an auxiliary agent into the oil-containing mud, or diesel oil in the oil-based mud is oxidized and removed by adding an oxidizing agent after the oil-based mud rock debris and the water are uniformly mixed. The cleaning technologies are all from the viewpoint of environmental protection, and the rock debris after cleaning still has more or less diesel oil components, so the cleaning technologies cannot be applied to scientific research in series of experiments of geochemical analysis and testing. From the angle of organic globalization scientific research, the method evaluates the oil washing effect by testing the mixed solvent and the oil washing mode to obtain the best oil washing effect by extracting the mixed liquid with the same volume of ethanol and benzene.
Drawings
FIG. 1 is a schematic diagram of a Soxhlet extractor;
FIG. 2 is a photograph of a Soxhlet extractor;
FIG. 3-1 is an oil based mud contamination sample;
3-2 are oil based mud contamination samples;
FIG. 4 is a graph of experimental results showing the variation of parameters with extraction time, wherein 4-1, S1；4-2，S2；4-3，S4；4-4，TOC；
FIG. 5 is a thermogram, in which 5-1 is a sample before oil washing and 5-2 is a sample after oil washing;
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
a. Selection of samples
The cuttings polluted by the oil-based mud in the drilling site are generally sticky, the cuttings polluted by the oil-based mud selected in the embodiment are cuttings returned to a core reservoir after being dried in the air in the site, as shown in fig. 3-1 and 3-2, the oil-based mud on the surfaces of the cuttings mainly comprises diesel oil, sulfonated asphalt and a small amount of organic soil, and therefore the cuttings are black solid, the main particle size of the cuttings is about 0.5mm-100mm, and the cuttings have stronger oil smell.
b. Principle of experiment
Through multiple experiments, the isovolumetric mixed liquor of absolute ethyl alcohol with stronger polarity and benzene with weaker polarity and strong non-hydrocarbon dissolving capacity is determined to be selected. Because the sample of the mud rock debris has coarser granularity and low permeability, the mixed liquid can dissolve oil-based mud pollutants on the surface of the debris without permeating into the interior of the debris to dissolve organic substances. Through the full-automatic Soxhlet extractor, the mixed liquid in the round-bottom flask is boiled and evaporated, the gas is liquefied when meeting cold in the snake-shaped condensation pipe at the upper end and flows back to the siphon, the polluted sample in the siphon is soaked by the clean solvent which is evaporated and flows back and does not contain impurities, so that the pollutants on the surface of the sample can be dissolved in the solvent and is taken out through the siphon action, and the effect of removing organic pollutants such as diesel oil and the like in the oil-based mud can be achieved repeatedly.
Principle of oil washing effect evaluation: the evaluation of the oil washing effect can be judged from three aspects, firstly, the qualitative judgment is carried out according to the principle that the higher the contents of non-hydrocarbon and asphaltene in the extract is, the darker the color of the extract is, along with the increase of the oil washing time, the color of the extract solution in the siphon tube can be changed according to the sequence of colorless-brownish yellow-colorless, and if the solvent finally shows colorless, the decontamination oil washing is more thorough; secondly, the content of organic matters in the mud rock debris after the oil is accurately washed is stable, and S is2、S4、TmaxThe value tends to be stable, and the requirements of the relative double differences and deviations of hydrocarbon source rock analysis in rock pyrolysis analysis (GB/T18602-2012) can be met, and after oil washing is incomplete or excessive, S of shale rock debris is unstable due to the content of organic matters in the shale rock debris2、S4、TmaxThe change is large, and the requirements of rock pyrolysis analysis cannot be met. According to this principle, the sample is taken in by a plurality of times at equal time intervalsPerforming pyrolysis experiment, and comparing to obtain pyrolysis parameter S1，S2，S4And the change of TOC can also evaluate the oil washing effect, and the measured value of multiple times of pyrolysis analysis after the same sample is washed away with oil stains tends to be stable within the allowable error range, so that the requirements of relative double differences and deviations can be met. Thirdly, qualitative judgment is carried out through a pyrolysis spectrogram, the main component of the oil-based mud is diesel oil, the temperature of oxidative pyrolysis of the component is 200-350 ℃, and the peak shape of the component appears in the S in the spectrogram of pyrolysis oil-bearing rock analysis2Left side of peak near S2The peak position, the peak shape in the pyrolysis spectrum after the oil is accurately washed, disappears and becomes a smooth curve.
c. Experimental procedure
The experimental operation steps of the embodiment mainly include extraction of the contaminated rock debris sample, sampling and airing, and rock pyrolysis analysis. The materials, instruments and operation steps required for extraction can be described in the national standard 'determination of chloroform bitumen in rock' (SY/T5118-2005) of materials, instruments and equipment, sample package, extraction and other steps, and the difference is two points: firstly, the experiment must ensure that the sample has certain granularity and low permeability, and the sample can not be crushed and the sandstone cuttings can not be extracted; and secondly, replacing the extracted solvent with a mixed solution of absolute ethyl alcohol and benzene in the same volume ratio. Sampling and airing means that sample packets are taken out from a siphon tube at certain intervals, a small amount of rock samples are picked by a clean iron spoon and placed in tin foil paper, and the rock samples are stored after being aired. The operation steps of rock pyrolysis can be referred to the national standard rock pyrolysis analysis (GB/T18602-2012).
d. Results of the experiment
In the extraction process, the extraction liquid in the siphon tube changes from colorless to brown yellow within 0-25h, and the solution is colorless and transparent after extraction for 25 h. From the measured values of pyrolysis (see fig. 4-1, 4-2, 4-3, 4-4, table 3), the parameters of the samples showed a tendency to decrease within 0-25h and the fluctuation amplitude was large, and after 25h, S was analyzed twice after the next 25h2、S4、TmaxThe relative double differences and the deviations meet the requirements of hydrocarbon source rock analysis on the relative double differences and the deviations in rock pyrolysis analysis (GB/T18602-2012), S1Gradually stabilize to be near 0.56S2Stable around 5.65, S4Stabilized at around 9.9 and TOC stabilized at around 1.5. From the pyrolysis spectrum (fig. 5-1, fig. 5-2), the peak shapes of the diesel oil are obviously compared in the spectrum of the sample polluted by the thoroughly washed oil and the mixed oil-based mud. This indicates that the oil stains on the surface of the rock debris sample have been cleaned and the parameters have returned to true values.
Table 3: measured values of pyrolysis parameters of samples extracted by mixed solvent at different times
Note:
deviation | first analysis value — second analysis value |;
relative double differences and deviation requirements S for Source rock pyrolysis analysis2>When 3, the relative difference is less than or equal to 10 percent, 3<S4<When 10, the relative difference is less than or equal to 15 percent, Tmax<At 450 deg.C, the deviation is less than or equal to 2.
Although specific embodiments of the invention have been described in detail, those skilled in the art will appreciate. Various modifications and substitutions of those details may be made in light of the overall teachings of the disclosure, and such changes are intended to be within the scope of the present invention. The full scope of the invention is given by the appended claims and any equivalents thereof.
Claims (8)
1. The oil washing method for the oil-based mud polluted rock debris meeting the requirement of organic geochemical analysis is characterized by at least comprising the following steps of:
organic distillation extraction, namely performing thermal extraction on the oil-based mud polluted rock debris by using a mixed solvent of two solvents at the temperature of 80-90 ℃;
an oil washing effect evaluation step, namely, taking a small amount of samples in the extraction process, drying the samples, performing pyrolysis analysis, and evaluating the completion of cleaning by combining with related indexes;
the indexes comprise the color of an extraction solution for mixing the oil-based mud polluted rock debris, the parameters of the pyrolytic analysis of the oil-based mud polluted rock debris and the spectrogram of the pyrolytic analysis of the oil-based mud polluted rock debris;
one of two solvents of the mixed solvent is ethanol, and the other solvent is benzene.
2. The oil washing method according to claim 1, wherein the volume ratio of the ethanol to the benzene is 1:1, and the thermal extraction is carried out at a constant temperature of 85 ℃ for 25 hours.
3. The oil washing method according to claim 2, comprising the steps of:
the pretreatment step, namely wrapping the oil-based mud polluted rock debris by using filter paper extracted by chloroform, and placing the wrapped rock debris into the bottom of a siphon pipe of a Soxhlet extractor;
and (3) organic distillation extraction, namely adding a mixed solvent of ethanol and benzene with the volume ratio of 1:1 into a round-bottom flask, connecting the round-bottom flask with a Soxhlet extractor, putting the round-bottom flask into a constant-temperature water bath kettle at 85 ℃, heating and extracting.
4. The oil washing method according to claim 3, further comprising a sample selection step of: and a sample selecting step, namely selecting viscous rock debris polluted by the oil-based mud on the drilling site, and airing for later use.
5. The oil washing method as claimed in claim 1, wherein the oil-based mud pollution detritus after air drying is wrapped by filter paper extracted by chloroform, the filter paper is placed at the bottom of a siphon tube of a Soxhlet extractor, a mixed solvent of ethanol and benzene with a volume ratio of 1:1 is added into the round-bottom flask or the top of the siphon tube of the Soxhlet extractor, the round-bottom flask and the Soxhlet extractor are connected, the round-bottom flask is placed into a constant-temperature water bath kettle at 85 ℃ for heating, Soxhlet extraction is carried out, and oil stains on the surface of the oil-based mud pollution detritus are cleaned when the extraction liquid in the siphon tube is changed from colorless to brownish yellow and then colorless and transparent.
6. The oil washing method according to claim 1, wherein a plurality of samples are taken at equal time intervals for pyrolysis experiments, and the cleaning effect is evaluated by using the parameters of pyrolysis analysis of the oil-based mud polluted rock debris; i.e. S of two adjacent analyses2、S4、TmaxThe oil stains on the surfaces of the oil-based mud polluted rock debris are cleaned when the relative double differences and the deviations of the oil-based mud meet the requirements of hydrocarbon source rock analysis in GB/T18602-2012 rock pyrolysis analysis.
7. The oil washing method as claimed in claim 1, wherein, a plurality of times of sampling at equal time intervals are carried out for pyrolysis experiments, and the cleaning effect is evaluated by using a spectrogram of pyrolysis analysis of oil-based mud polluted rock debris; namely, oil stains on the surface of the oil-based mud polluted rock debris are cleaned when no diesel characteristic peak exists in a spectrogram of the oil-based mud polluted rock debris pyrolysis analysis.
8. The oil washing method according to any one of claims 6 or 7, wherein the oil-based mud polluted rock debris is subjected to heating by a rock pyrolysis instrument for pyrolysis analysis of the oil-based mud polluted rock debris, and the heating is three-stage heating S1: keeping the temperature at 300 ℃ for 3 min; s2: the temperature rise rate is 50 ℃/min at 300-600 ℃, and the temperature is kept constant for 1min at 600 ℃; s4: burning at 600 deg.C for 7-13 min; quantitatively analyzing hydrocarbons and carbon dioxide released by organic matters in the oil-based mud polluted rock debris by using a hydrogen ion flame detector and a thermal conductivity detector to obtain pyrolysis parameters and a pyrolysis analysis spectrogram, wherein the pyrolysis parameters comprise free hydrocarbon S1Pyrolysis of hydrocarbons S2Carbon residue S4And Tmax。
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| CN112765765B (en) * | 2020-12-16 | 2022-03-01 | 成都理工大学 | Correction method for pyrolysis result of rock debris of well site oil-based drilling fluid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101397908A (en) * | 2008-11-03 | 2009-04-01 | 大庆油田有限责任公司 | Method for simultaneous removing oil and salt in rock core |
| CN106000478A (en) * | 2016-05-19 | 2016-10-12 | 福州大学化肥催化剂国家工程研究中心 | Recycling method of slurry-bed hydrocracking catalyst for heavy oil |
Family Cites Families (1)
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|---|---|---|---|---|
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-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101397908A (en) * | 2008-11-03 | 2009-04-01 | 大庆油田有限责任公司 | Method for simultaneous removing oil and salt in rock core |
| CN106000478A (en) * | 2016-05-19 | 2016-10-12 | 福州大学化肥催化剂国家工程研究中心 | Recycling method of slurry-bed hydrocracking catalyst for heavy oil |
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| CN107290204A (en) | 2017-10-24 |
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