CN113758957B - Method for rapidly judging crude oil group separation effect by using nuclear magnetic resonance core analysis technology - Google Patents
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Abstract
The invention discloses a method for rapidly judging the separation effect of crude oil components by using nuclear magnetic resonance core analysis technology. The method for judging the separation effect of the crude oil components comprises the following steps: performing nuclear magnetic resonance analysis on each component separated from crude oil to obtain nuclear magnetic resonance characteristics of each component; judging the separation effect by utilizing the nuclear magnetic resonance characteristics; the families include saturated hydrocarbon families, aromatic families, non-hydrocarbon families, and asphaltene families; the nuclear magnetic resonance characteristics include relaxation times and nuclear magnetic resonance response signals. According to the invention, whether the fourth group components of the crude oil are effectively separated can be judged through the difference of the hydrogen atom characteristics of the groups; by detecting the experimental result, the problem of experimental result errors caused by incomplete volatilization of the analysis reagent and incomplete separation of other components can be detected, and experimental data errors caused by human factors are avoided to a large extent, so that the accuracy of analysis and test results is improved, experimental data is more reliable, and correct data support is provided for oilfield geology or engineering analysis.
Description
Technical Field
The invention relates to a method for rapidly judging a crude oil group separation effect by utilizing a nuclear magnetic resonance core analysis technology, and belongs to the technical field of oil and gas exploration.
Background
Crude oil is used as an important energy source in the current society, different kinds of finished oil can be obtained by utilizing different processing means, and in order to evaluate the quality of the crude oil and better utilize the crude oil resources, the crude oil needs to be subjected to group composition analysis. The research of petroleum group components is one of important projects in researches such as organic petroleum geology, petroleum exploration and development, and the like, can quantitatively describe heavy and light organic matters in petroleum, and plays a vital role in the research of petroleum exploitation schemes. Meanwhile, the petroleum group component separation plays an important role in providing experimental samples for subsequent chromatographic analysis, chromatographic-mass spectrometry, infrared spectrometry and isotope analysis, and the petroleum group component analysis has important significance for evaluating the quality of crude oil and better utilizing petroleum resources. In addition, the research of petroleum group components can also provide evidence for the composition, evolution and maturity of crude oil, quantitatively and qualitatively describe petroleum organic matters and provide reliable data support for petroleum exploitation.
The group component is an important index for petroleum evaluation, and different compounds in petroleum have different adsorption and dissolution performances on the adsorbent and the organic solvent due to the difference of molecular structures. Depending on this characteristic, dan Youfen can be divided into four families of saturated hydrocarbons, aromatic hydrocarbons, non-hydrocarbons and asphaltenes by selecting different adsorbents and organic solvents. The percentage of the four groups determines the physical properties of the crude oil, such as density, viscosity and the like, so as to control the quality and the attribute of the crude oil. Such as the viscosity of crude oil increases with increasing aromatic specific gravity, density increases with increasing asphaltene content of high molecular weight, etc. The following are brief descriptions of four family components:
saturated hydrocarbons, also known as aliphatic hydrocarbons, of the formula C n H 2n+2 N-alkanes and isoparaffins and naphthenes are included. The carbon atoms in the molecule are connected by single bonds of carbon and carbon, and the rest bonds are combined with hydrogen, so that the organic compound has low boiling point and low molecular weight and is the simplest organic compound.
Aromatic hydrocarbons are special carbocycle-benzene ring compounds containing six carbon atoms and six hydrogen atoms, and are characterized in that the molecules contain benzene ring structure unsaturated hydrocarbon.
The non-hydrocarbon is complex carbon-containing compound containing sulfur, nitrogen and oxygen, is an oil-soluble, stray, irregular, aromatic hetero-condensed ring macromolecular non-hydrocarbon compound with relative molecular mass and polarity smaller than that of asphaltene, has dark brown to dark brown appearance, is thick and non-flowable liquid or amorphous solid, and is an important component in heavy oil.
The asphaltene has the characteristics of complex components, low volatility and strong adsorptivity, is dissolved in chloroform, but is insoluble in petroleum ether, is different from non-hydrocarbon, has high content of high molecular compounds, has larger relative molecular mass, has a macroscopic structure of asphaltene into colloidal particles under an electron microscope, and has a complex structure composed of condensed ring aromatic hydrocarbon and alkyl chain.
Column chromatography is still the most commonly used separation method at present, firstly, petroleum ether or normal hexane is used for precipitating asphaltene; and then, the adsorption performance between different types of organic substances and adsorbents and the polarity difference of various flushing agents are utilized to achieve the desorption and separation effects on different substances. The group component insoluble in n-hexane or petroleum ether in crude oil is asphaltene, the soluble part is adsorbed by silica gel and alumina, and then saturated hydrocarbon, aromatic hydrocarbon and non-hydrocarbon components are separated from the adsorbent by solvents such as n-hexane or petroleum ether, mixed solution of dichloromethane and n-hexane, mixed solution of absolute ethyl alcohol and chloroform, and the like.
The current commonly used column chromatography experimental method has more problems: (1) Cross-group component problems often occur, such as small amounts of saturated hydrocarbons mixing with asphaltenes during filtration; the saturated hydrocarbon and aromatic hydrocarbon are not thoroughly separated, and the saturated hydrocarbon and aromatic hydrocarbon are mixed with each other; the non-hydrocarbon contains a small amount of aromatic hydrocarbon. (2) Because of inaccurate control of the volatilization time of the experimental reagent, the experimental reagent remains in the separated components, and the experimental error is larger.
The common problems listed above all lead to inaccurate separation effect and weighing result, misjudgment is made on crude oil properties, deviation occurs in geological analysis results, oil source comparison is inaccurate, and incorrect geochemical interpretation is given. The number of samples and the experimental data in the field of oil gas assay analysis are huge, the experiment is greatly influenced by human factors, the accuracy of experimental results can directly influence the judgment and deployment of oil gas development, and how to detect the crossing condition and the separation effect of components obtained by separation is very important.
Disclosure of Invention
The invention aims to provide a method for rapidly judging the separation effect of crude oil components by using nuclear magnetic resonance core analysis technology.
The method utilizes the characteristic that hydrogen nuclei form nuclear magnetic resonance under the action of an external magnetic field, and accordingly, the separation effect of four groups in crude oil can be judged by analyzing relaxation time (the time of a process that a magnetization vector deviates from the original equilibrium state and returns to the equilibrium state when nuclear magnetic resonance is generated under the excitation of an alternating electromagnetic field is called as relaxation time) of each component of crude oil and detection signals of the hydrogen atoms.
The method for judging the separation effect of crude oil components provided by the invention comprises the following steps:
performing nuclear magnetic resonance analysis on each of the fractions separated from the crude oil to obtain nuclear magnetic resonance characteristics of each of the fractions; judging the separation effect by utilizing the nuclear magnetic resonance characteristics;
the families include saturated hydrocarbon families, aromatic families, non-hydrocarbon families, and asphaltene families.
Specifically, if the nuclear magnetic resonance characteristics of each of the groups have the following characteristics, the separation effect is good:
the nuclear magnetic resonance response signals of the saturated hydrocarbon component, the aromatic hydrocarbon component, the non-hydrocarbon component and the asphaltene component become weaker in sequence, and the relaxation time becomes shorter in sequence.
The method is characterized in that a SPEC-PMR-OS instrument is adopted, the main frequency is 14.06MHz, the sampling interval is 2.00us, the relaxation time of the saturated hydrocarbon component is distributed between 70ms and 1060ms, the main peak time is 240ms, and the nuclear magnetic resonance response signal peak value is 34; the normal paraffins inside the saturated hydrocarbon contain a large number of hydrogen atoms, providing a stronger response signal than the other three families;
the relaxation time of the aromatic hydrocarbon component is distributed between 7ms and 120ms, the main peak time is 60ms to 61ms, and the nuclear magnetic resonance response signal peak value is 17; because aromatic hydrocarbon generally contains benzene ring structure and has certain stability, the response signal peak value of hydrogen atoms is generally lower than that of saturated hydrocarbon;
the relaxation time of the non-hydrocarbon component is distributed between 0.2ms and 8ms, the main peak time is between 1.0ms and 1.1ms, and the peak value of the nuclear magnetic resonance response signal is 10; the method has the characteristics of weak response signals and short relaxation time, and is related to macromolecular compounds such as sulfur-containing compounds, nitrogen-containing compounds, oxygen-containing compounds and the like which are contained in a large amount in non-hydrocarbon components;
the relaxation time of the asphaltene group component is distributed between 0.075ms and 0.65ms, the main peak time is between 0.14ms and 0.16ms, and the response signal peak value is 7; asphaltenes, which are the most highly evolved group components of crude oil, are often found in high viscosity crude oils in large quantities and, due to their lower hydrogen atom content, exhibit a characteristic of low relaxation time, weak nuclear magnetic resonance signals, etc., as compared to the nuclear magnetic resonance characteristics of hydrocarbon materials.
In the same crude oil sample, the nuclear magnetic resonance characteristics of different groups of components are greatly different, the nuclear magnetic resonance response signal of saturated hydrocarbon is strongest, and the relaxation time is the longest in all groups; secondly, aromatic hydrocarbon, response signal value and relaxation time are reduced, and then non-hydrocarbon component; finally asphaltenes, with the weakest signal values and the shortest relaxation times.
A SPEC-PMR-OS instrument is adopted, the main frequency is 14.06MHz, the sampling interval is 2.00us, and if the relaxation time of the asphaltene fraction is distributed between 0.07ms and 1050ms, the saturated hydrocarbon fraction is mixed in the asphaltene fraction; because saturated hydrocarbons have a longer relaxation time and a nuclear magnetic resonance signal, asphaltenes have a shorter relaxation time and a weaker signal, and a spectrum with the above characteristics has a common characteristic of asphaltenes and saturated hydrocarbon components, which may be that colorless saturated hydrocarbons in a funnel are easily adsorbed on cotton or glass when the asphaltenes are filtered by the funnel, so that a small amount of saturated hydrocarbons are mixed in the asphaltenes.
If the nuclear magnetic resonance spectrum of the aromatic hydrocarbon component shows bimodal distribution characteristics, the 1 st peak has a relaxation time of 8 ms-300 ms, the nuclear magnetic resonance response signal peak value is 10, the 2 nd peak has a relaxation time of 300 ms-800 ms, and the nuclear magnetic resonance response signal peak value is 2.8, the aromatic hydrocarbon component is mixed with the saturated hydrocarbon component; the first peak is considered to be an aromatic hydrocarbon signal by analysis, and the second peak does not belong to an aromatic hydrocarbon nuclear magnetic resonance signal, but is a nuclear magnetic resonance signal obtained by mixing a saturated hydrocarbon component into an aromatic hydrocarbon. Because the flushing time of crude oil samples with different chemical properties in the process of separating saturated hydrocarbon and aromatic hydrocarbon is different, different laboratory staff control time is different, saturated hydrocarbon is easy to mix in the separated aromatic hydrocarbon, and the saturated hydrocarbon is not completely separated to receive aromatic hydrocarbon components, so that saturated hydrocarbon remains in the aromatic hydrocarbon components.
If the nuclear magnetic resonance spectrum of the non-hydrocarbon group component shows bimodal distribution characteristics, the relaxation time is respectively 0.03 ms-1 ms and 0.6 ms-85 ms, the peak value of nuclear magnetic resonance response signals is 1.7-1.8, and the observation shows that the second peak does not really belong to nuclear magnetic resonance signals of non-hydrocarbon, but is a signal value formed by incomplete separation of the non-hydrocarbon and aromatic hydrocarbon. Because the crude oil samples with different chemical properties have different flushing times in the separation process, different experimenters have different mastering times, and the aromatic hydrocarbon flushing starts to accept the non-hydrocarbon compounds when not finishing, so that the non-hydrocarbon compounds are mixed with aromatic hydrocarbon compounds.
If the nuclear magnetic resonance spectrum of the asphaltene group shows bimodal distribution characteristics, the relaxation time is respectively 0.02 ms-0.2 ms and 0.2 ms-2.5 ms, the nuclear magnetic resonance response signal peak value of the second peak is 10, the second peak is analyzed to be not really the nuclear magnetic resonance signal of the asphaltene, the dichloromethane is difficult to volatilize, and the dichloromethane for dissolving the asphaltene is not volatilized thoroughly to form the peak value.
Because the current experimental method for separating crude oil group components is greatly influenced by human factors, the human experience plays a key role, the oilfield enterprises attach insufficient importance to the geochemical separation experimental effect of oil and gas, and no clear measurement standard and judgment method exists, and in each oilfield unit, huge sample and data quantity also reduce the accuracy of the test result. There is no effective test method or standard for the accuracy of the experimental results of most new practitioners. The invention can judge whether the fourth group component of the crude oil is effectively separated or not through the difference of the hydrogen atom characteristics of each group component. By detecting the experimental result, the problem of experimental result errors caused by incomplete volatilization of the analysis reagent and incomplete separation of other components can be detected, and experimental data errors caused by human factors are avoided to a large extent, so that the accuracy of analysis and test results is improved, experimental data is more reliable, and correct data support is provided for oilfield geology or engineering analysis.
Drawings
FIG. 1 is a nuclear magnetic resonance spectrum of four ethnic groups of components in crude oil.
FIG. 2 is a nuclear magnetic resonance spectrum of asphaltenes containing saturated hydrocarbons.
FIG. 3 is a nuclear magnetic resonance spectrum when aromatic hydrocarbons contain saturated hydrocarbons.
FIG. 4 is a nuclear magnetic resonance spectrum of a non-hydrocarbon aromatic hydrocarbon.
FIG. 5 is a nuclear magnetic resonance spectrum of asphaltenes with methylene chloride.
Detailed Description
The experimental methods used in the following examples are conventional methods unless otherwise specified.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
The following examples were conducted with a SPEC-PMR-OS instrument for nuclear magnetic resonance analysis with a main frequency of 14.06MHz and a sampling interval of 2.00us.
The nuclear magnetic resonance spectrum of four group components in crude oil is shown in figure 1, and at this time, the separation effect of the four group components is good.
As can be seen from FIG. 1, the nuclear magnetic resonance characteristic of the saturated hydrocarbon component is obvious, the relaxation time is distributed between 70ms and 1060ms, the main peak time is 240ms, and the nuclear magnetic resonance response signal value peak value is 34. The normal paraffins within the saturated hydrocarbon contain a large number of hydrogen atoms, providing a stronger response signal than the other three families.
As can be seen from FIG. 1, the relaxation time of the aromatic hydrocarbon component is distributed between 7ms and 120ms, the main peak time is 60ms and 61ms, and the peak value of the nuclear magnetic resonance response signal is 17. Since aromatic hydrocarbons generally contain a benzene ring structure and have a certain stability, the peak value of the response signal of a hydrogen atom is generally lower than that of saturated hydrocarbons.
As can be seen from FIG. 1, the relaxation time of the non-hydrocarbon component is distributed between 0.2ms and 8ms, the main peak time is 1.0ms and 1.1ms, the nuclear magnetic resonance response signal peak value is 10, and the characteristic of weak response signal and short relaxation time is that the relaxation time is related to a large amount of macromolecular compounds such as sulfur-containing compounds, nitrogen-containing compounds and oxygen-containing compounds contained in the non-hydrocarbon component.
As can be seen from FIG. 1, the nuclear magnetic resonance spectrum of asphaltene shows that the relaxation time is distributed between 0.075ms and 0.65ms, the main peak time is between 0.14ms and 0.16ms, and the response signal peak value is 7. Asphaltenes, which are the most highly evolved group components of crude oil, are often found in high viscosity crude oils in large quantities and, due to their lower hydrogen atom content, exhibit a characteristic of low relaxation time, weak nuclear magnetic resonance signals, etc., as compared to the nuclear magnetic resonance characteristics of hydrocarbon materials.
In summary, in the same crude oil sample, the nuclear magnetic resonance characteristics of different groups of components are greatly different, the nuclear magnetic resonance response signal of saturated hydrocarbon is strongest, and the relaxation time is the longest in all groups; the second is aromatic, with a decrease in response signal value and relaxation time, followed by non-hydrocarbon components. Finally asphaltenes, with the weakest signal values and the shortest relaxation times.
According to the change of the nuclear magnetic resonance spectrum of each group of components, the separation effect of each group of components can be judged, and the following groups of components are easy to generate a spectrum of incomplete separation of four groups of components in the crude oil separation process, the two are mixed with each other, the volatilization of the reagent is incomplete, and the spectrum of coexistence of the sample and the reagent is generated.
1. The map of asphaltene mixed with saturated hydrocarbon is shown in figure 2
The asphaltene fraction of crude oil in a certain experiment shows a long relaxation time, as shown in fig. 2. The distribution is 0.07 ms-1050 ms, the spectrum is obviously not the nuclear magnetic resonance response characteristic of asphaltene, the analysis result is that the operation errors occur in the process of crude oil samples, components such as saturated hydrocarbon are mixed in the asphaltene, the saturated hydrocarbon has longer relaxation time and nuclear magnetic resonance signals, the asphaltene has shorter relaxation time and weaker signals, and the spectrum shown in fig. 2 obviously has the common characteristics of the asphaltene and the saturated hydrocarbon. When the funnel is used for filtering the asphaltenes, colorless saturated hydrocarbons in the funnel are easily adsorbed on cotton or glass, so that a small amount of saturated hydrocarbons are mixed in the asphaltenes.
2. The spectrum of the aromatic hydrocarbon mixed with saturated hydrocarbon is shown in FIG. 3
As can be seen from FIG. 3, the aromatic hydrocarbon of the crude oil shows bimodal distribution characteristics in a certain experiment, as shown in FIG. 3, and as can be seen from FIG. 3, the 1 st peak T 2 The delay time is 8 ms-300 ms, the peak value of the nuclear magnetic resonance response signal is about 10, and the 2 nd peak T 2 The relaxation time is 300 ms-800 ms, and the peak value of the nuclear magnetic resonance response signal is about 2.8. By analysis, it is considered that peak 1 is a nuclear magnetic resonance signal of aromatic hydrocarbon, and peak 2 is not a nuclear magnetic resonance signal of aromatic hydrocarbon, but a nuclear magnetic resonance signal of aromatic hydrocarbon mixed with saturated hydrocarbon. Because the flushing time of crude oil samples with different chemical properties in the process of separating saturated hydrocarbon and aromatic hydrocarbon is different, different laboratory staff control time is different, saturated hydrocarbon is easy to mix in the separated aromatic hydrocarbon, and the saturated hydrocarbon is not completely separated to receive aromatic hydrocarbon components, so that saturated hydrocarbon remains in the aromatic hydrocarbon components.
3. The spectrum of the non-hydrocarbon mixed with aromatic hydrocarbon is shown in FIG. 4
The non-hydrocarbons in the crude oil exhibited a bimodal distribution profile in a certain experiment, as shown in fig. 4. As can be seen from FIG. 4, the peak of the nuclear magnetic resonance response signal is between 1.7 and 1.8, with a 1 peak of 0.03ms to 1ms and a 2 peak of 0.6ms to 85 ms. The observation shows that the 2 peak does not really belong to the nuclear magnetic resonance signal of the non-hydrocarbon, but is a signal value formed by incomplete separation of the non-hydrocarbon from the aromatic hydrocarbon. Because the crude oil samples with different chemical properties have different flushing times in the separation process, different experimenters have different mastering times, and the aromatic hydrocarbon flushing starts to accept the non-hydrocarbon compounds when not finishing, so that the non-hydrocarbon compounds are mixed with aromatic hydrocarbon compounds.
4. The graph of the test reagent when it is incompletely volatilized is shown in FIG. 5
As can be seen from FIG. 5, the asphaltene group in crude oil shows a bimodal distribution characteristic in a certain experiment, and as can be seen from FIG. 5, the asphaltene group in crude oil has a 1 peak of 0.02 ms-0.2 ms and a 2 peak of 0.2 ms-2.5 ms, and the nuclear magnetic resonance response signal peak value of No. 2 peak is about 10. Analysis indicated that the 2 peaks do not truly belong to the nuclear magnetic resonance signal of asphaltenes, methylene chloride is difficult to volatilize, and methylene chloride used for dissolving asphaltenes volatilizes incompletely to form peaks.
The analysis of the atlas shows that the nuclear magnetic resonance analysis technology can be used for effectively judging the separation effect of four families, has the characteristics of rapidness and accuracy, solves the problem of incorrect analysis of results caused by incomplete volatilization of experimental reagents and incomplete separation of components, thereby improving the accuracy of analysis and test results and having obvious practical value.
Claims (2)
1. A method for judging the separation effect of crude oil components is characterized by comprising the following steps: the method comprises the following steps:
performing nuclear magnetic resonance analysis on each of the fractions separated from the crude oil to obtain nuclear magnetic resonance characteristics of each of the fractions; judging the separation effect by utilizing the nuclear magnetic resonance characteristics;
the families include saturated hydrocarbon families, aromatic families, non-hydrocarbon families, and asphaltene families;
the nuclear magnetic resonance signature includes a relaxation time and a nuclear magnetic resonance response signal;
if the nuclear magnetic resonance characteristics of each group have the following characteristics, the separation effect is good:
the nuclear magnetic resonance response signals of the saturated hydrocarbon component, the aromatic hydrocarbon component, the non-hydrocarbon component and the asphaltene component are weakened in sequence, and the relaxation time is shortened in sequence;
the relaxation time of the saturated hydrocarbon component is distributed between 70ms and 1060ms, the main peak time is 240ms, and the nuclear magnetic resonance response signal peak value is 34;
the relaxation time of the aromatic hydrocarbon component is distributed between 7ms and 120ms, the main peak time is 60ms to 61ms, and the peak value of the nuclear magnetic resonance response signal is 17;
the relaxation time of the non-hydrocarbon component is distributed between 0.2ms and 8ms, the main peak time is between 1.0ms and 1.1ms, and the peak value of the nuclear magnetic resonance response signal is 10;
the relaxation time of the asphaltene group component is distributed between 0.075ms and 0.65ms, the main peak time is between 0.14ms and 0.16ms, and the response signal peak value is 7;
if the relaxation time of the asphaltene fraction is distributed between 0.07 and 1050ms, the saturated hydrocarbon fraction is mixed in the asphaltene fraction;
if the nuclear magnetic resonance spectrum of the aromatic hydrocarbon component shows bimodal distribution characteristics, the 1 st peak has a relaxation time of 8 ms-300 ms, the nuclear magnetic resonance response signal peak value is 10, the 2 nd peak has a relaxation time of 300 ms-800 ms, and the nuclear magnetic resonance response signal peak value is 2.8, the aromatic hydrocarbon component is mixed with the saturated hydrocarbon component;
if the nuclear magnetic resonance spectrum of the non-hydrocarbon component shows bimodal distribution characteristics, the relaxation time is respectively 0.03 ms-1 ms and 0.6 ms-85 ms, and the nuclear magnetic resonance response signal peak values are 1.7-1.8, the non-hydrocarbon component is mixed with the aromatic hydrocarbon component;
if the nuclear magnetic resonance spectrum of the asphaltene group shows bimodal distribution characteristics, the relaxation time is respectively 0.02 ms-0.2 ms and 0.2 ms-2.5 ms, and the nuclear magnetic resonance response signal peak value of the second peak is 10, the asphaltene group contains an experimental reagent which is not volatilized completely.
2. The method according to claim 1, characterized in that: the experimental reagent is dichloromethane.
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