CN116223601A - Device and method for gas wash fractionation analysis under high-temperature high-pressure sealing system - Google Patents

Device and method for gas wash fractionation analysis under high-temperature high-pressure sealing system Download PDF

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Publication number
CN116223601A
CN116223601A CN202111476678.3A CN202111476678A CN116223601A CN 116223601 A CN116223601 A CN 116223601A CN 202111476678 A CN202111476678 A CN 202111476678A CN 116223601 A CN116223601 A CN 116223601A
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gas
crude oil
natural gas
analysis
pressure
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翟正
王学军
李祥臣
綦艳丽
鲍燕
林晶
陶军明
王大洋
韩冬梅
王茹
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China Petroleum and Chemical Corp
Exploration and Development Research Institute of Sinopec Shengli Oilfield Co
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China Petroleum and Chemical Corp
Exploration and Development Research Institute of Sinopec Shengli Oilfield Co
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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
    • G01N27/62—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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P90/00—Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
    • Y02P90/70—Combining sequestration of CO2 and exploitation of hydrocarbons by injecting CO2 or carbonated water in oil wells

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Abstract

The invention relates to the technical field of oil and gas exploration, in particular to a gas wash fractional analysis device and method under a high-temperature high-pressure sealing system. The device comprises a gas washing reaction device, a natural gas online collection device, an isotope mass spectrometer, a crude oil online trace rapid sampling device, a crude oil collection device, a carbon dioxide purification device, a valve, a heating sleeve and a liquid nitrogen cold trap. The device provided by the invention realizes real-time detection of raw oil and gas carbon isotopes in the gas washing fractionation process under the high-temperature and high-pressure state, and has the advantages of high analysis speed and high accuracy.

Description

Device and method for gas wash fractionation analysis under high-temperature high-pressure sealing system
Technical Field
The invention relates to the technical field of oil and gas exploration, in particular to a gas wash fractional analysis device and method under a high-temperature high-pressure sealing system.
Background
The oil and gas exploration in partial areas of China reaches a stage of high exploration degree, and deep oil and gas exploration is gradually paid attention to. In deep oil and gas exploration, the common evolution degree of hydrocarbon source rock is high, the stage of natural gas generation is achieved, and the generated natural gas passes through an oil reservoir in the process of migration, and the process of dissolving and carrying part of crude oil components in the oil reservoir is called gas washing. The gas wash changes both the composition of crude oil and natural gas and the characteristics of crude oil and natural gas.
The characteristics of oil gas are identified, the source of the oil gas is clear, and the method has important guiding significance for deep oil gas exploration. The carbon isotope technology of natural gas and crude oil is an important means for identifying deep oil and gas sources, however, the gas washing process can form carbon isotope fractionation of crude oil and natural gas, and change the carbon isotope values of crude oil and natural gas in a primary reservoir. Therefore, the research on the change process of crude oil and natural gas carbon isotopes in the whole gas washing process is an important means for comparing the oil sources in the gas washing process.
Related work has been done by Su-Iris et al in the influence of phase control and gas wash fractionation on the composition of oil and gas components and carbon isotopes. The detection of components and carbon isotopes is carried out by charging excess gas into the crude oil system, collecting the charged gas and crude oil (Su-Iris, zhang Shuichang, long, etc. the effects of phase control and gas wash fractionation on the composition of the oil and gas components [ J. Geochemistry, 2000,29 (6): 7.). In the above process, the collected samples are crude oil under normal pressure in the initial state and the final state of the reaction, and the crude oil presents an overpressure state in the underground oil reservoir, and the method lacks an effective method for the isotope test of the crude oil under the overpressure state. Meanwhile, the gas collecting process is a process of continuously changing pressure, and in the process of changing pressure, gas isotopes generate fractionation effect, and the method lacks an effective means for tracking the gas washing fractionation process.
There is a need for an apparatus and method for performing gas wash fractionation analysis in a high temperature, high pressure containment system.
Disclosure of Invention
The invention mainly aims to provide a device and a method for gas wash fractionation analysis under a high-temperature high-pressure sealing system, and the device provided by the invention realizes real-time detection of raw oil and gas carbon isotopes in the gas wash fractionation process under a high-temperature high-pressure state, and has the advantages of high analysis speed and high accuracy.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a gas wash fractional distillation analysis device under a high-temperature high-pressure sealing system, which comprises a gas wash reaction device, a natural gas online collection device, an isotope mass spectrometer, a crude oil online trace rapid sampling device, a crude oil collection device, a carbon dioxide purification device, a valve, a heating sleeve and a liquid nitrogen cold trap, wherein the gas wash reaction device is connected with the natural gas online collection device; the gas washing reaction device is respectively connected with the natural gas on-line collection device and the crude oil on-line micro rapid sampling device, and is connected with a natural gas source through a valve; the crude oil online trace rapid sampling device is sequentially connected with a crude oil collecting device, a carbon dioxide purifying device and a first isotope mass spectrometer; the natural gas online collection device is connected with a carrier gas source through a valve, and the second isotope mass spectrometer is connected with the natural gas online collection device; the crude oil collecting device is connected with an oxygen source through a valve, and is placed in the first liquid nitrogen cold trap, and the heating jacket surrounds the first liquid nitrogen cold trap; the crude oil on-line micro rapid sampling device is placed in a second liquid nitrogen cold trap.
The natural gas on-line collection device is arranged, so that the real-time tracking of the natural gas carbon isotopes can be realized. The adoption of the crude oil trace rapid sampling device can prevent the fractionation of carbon isotopes in the process of crude oil transmission.
The crude oil micro-rapid sampling device and the crude oil collecting device are respectively arranged in the liquid nitrogen cold trap, so that the transfer of a crude oil sample under the low-temperature condition is realized, the dissipation of dissolved hydrocarbon gas is prevented, and the accuracy of analysis of accurate data is ensured. The natural gas on-line collection device is connected with a carrier gas source, so that the natural gas is completely collected in sample analysis, and the interference of the natural gas carbon isotope fractionation effect on data is eliminated.
Further, the air washing reaction device is also respectively connected with a pressure gauge and a temperature control system. Can realize the selection of samples under different temperature and pressure conditions in the gas washing reaction device.
Further, a valve is arranged on a pipeline between the gas washing reaction device and the crude oil collecting device.
Further, a valve is arranged on a pipeline connected with the natural gas on-line collection device and the second isotope mass spectrometer.
Further, valves are respectively arranged on a pipeline connected with the crude oil collecting device and the carbon dioxide purifying device and a pipeline connected with the carbon dioxide purifying device and the first isotope mass spectrometer.
The invention also provides a gas wash fractional distillation analysis method under the high-temperature high-pressure sealing system, which adopts the gas wash fractional distillation analysis device under the high-temperature high-pressure sealing system for analysis and comprises the following steps:
adding crude oil into a gas washing reaction device, and heating the gas washing reaction device to the temperature required by an experiment; introducing natural gas, and stopping introducing the natural gas after the pressure in the gas washing reaction device is increased to the pressure required by the experiment and reaches a stable state, so as to analyze carbon isotopes in the natural gas and crude oil;
the natural gas carbon isotope analysis steps include: the natural gas online collection device collects the natural gas in the gas washing reaction device, carrier gas is injected into the natural gas online collection device, and the natural gas and the carrier gas enter the second isotope mass spectrometer for online analysis of natural gas carbon isotopes;
the analysis steps of the carbon isotopes in the crude oil comprise: opening a liquid nitrogen cold trap to ensure that the temperatures of the crude oil trace rapid sampling device and the crude oil collecting device cannot cause the loss of dissolved natural gas; taking trace crude oil by a crude oil trace rapid sampling device, and completely transferring the trace crude oil to a crude oil collecting device; closing a liquid nitrogen cold trap, opening an electric heating sleeve to heat the crude oil collecting device, introducing oxygen into the crude oil collecting device, completely burning organic matters in crude oil, purifying carbon dioxide generated by burning, and performing carbon isotope analysis on the purified carbon dioxide.
Further, the carrier gas used in the natural gas carbon isotope analysis step is helium.
Further, in the step of analyzing carbon isotopes in crude oil, the crude oil collecting device is heated to 850-1000 ℃.
Further, the pressure in the gas wash reaction apparatus was increased to the pressure required for the experiment, and the steady state was reached after maintaining the pressure required for the experiment constant for at least 15 min.
Compared with the prior art, the invention has the following advantages:
the device provided by the invention realizes the real-time detection of the raw oil and the gaseous carbon isotopes in the gas wash fractionation process under the high-temperature and high-pressure state, and has the advantages of high analysis speed and high accuracy of the obtained result. The device and the method have important significance for comparing the oil gas sources of the natural gas and the crude oil, and can effectively guide the practical work of exploration.
Drawings
Fig. 1 is a schematic structural diagram of a gas wash fractionation analysis device under a high temperature and high pressure sealing system according to embodiment 1 of the present invention.
The device comprises a gas wash reaction device 1, a temperature control system 2, a pressure gauge 3, a crude oil trace rapid sampling device 4, a crude oil collecting device 5, a carbon dioxide purifying device 6, a first isotope mass spectrometer 7, a natural gas online collecting device 8, a second isotope mass spectrometer 10, a carrier gas source 11, an oxygen source 12, a natural gas source 13, a valve I, a valve II, a valve III, a valve IV, a valve 17, a valve V, a valve 18, a valve six, a valve seven, a valve 20, a first liquid nitrogen cold trap, a second liquid nitrogen cold trap and a heating sleeve 22.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
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 exemplary embodiments according to the present invention. As used herein, the singular forms also are intended to include the plural forms unless the context clearly indicates otherwise, and furthermore, 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, and/or combinations thereof.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present invention, the technical scheme of the present invention will be described in detail with reference to specific embodiments.
Example 1
As shown in fig. 1, the gas wash fractionation analysis device under the high-temperature high-pressure sealing system comprises a gas wash reaction device 1, a natural gas online collection device 8, an isotope mass spectrometer, a crude oil trace rapid sampling device 4, a crude oil collection device 5, a carbon dioxide purification device 6, a valve, a heating jacket 22 and a liquid nitrogen cold trap;
the gas washing reaction device 1 is respectively connected with a natural gas online collection device 8 and a crude oil trace rapid sampling device 4, the gas washing reaction device 1 is connected with a natural gas source 12 through a valve I13, a valve II 14 is arranged on a pipeline connected with the gas washing reaction device 1 and the natural gas online collection device 8, and the gas washing reaction device is also respectively connected with a pressure gauge 3 and a temperature control system 2; the crude oil trace rapid sampling device 4 is sequentially connected with a crude oil collecting device 5, a carbon dioxide purifying device 6 and a first isotope mass spectrometer 7; a valve five 17 is arranged on a pipeline connected with the crude oil collecting device 5 and the carbon dioxide purifying device 6, and a valve six 18 is arranged on a pipeline connected with the carbon dioxide purifying device 6 and the first isotope mass spectrometer 7; the crude oil collecting device 5 is connected with the oxygen source 11 through a valve seven 19, the crude oil collecting device 5 is placed in the first liquid nitrogen cold trap 20, and the heating jacket 22 surrounds the first liquid nitrogen cold trap 20; the crude oil micro-rapid sampling device 4 is placed in a second liquid nitrogen cold trap 21.
The natural gas online collection device 8 is connected with a carrier gas source 10 through a valve IV 16; the second isotope mass spectrometer 9 is connected with the natural gas online collection device 8, and a valve III 15 is arranged on the connecting pipeline.
Example 2
A gas wash fractional analysis method under a high-temperature high-pressure sealing system comprises the following steps: the analysis was performed using the high temperature high pressure closed system gas wash fractionation analysis apparatus described in example 1:
1. natural gas carbon isotope analysis method
(1) Adding crude oil into the gas washing reaction device 1;
(2) Heating the gas wash reaction device 1 to a specified temperature according to experimental requirements;
(3) Closing a valve I13 to enable natural gas to enter the gas washing reaction device 1, and observing the indication of a pressure gauge 3 of the gas washing reaction device 1; when the system pressure begins to increase, indicating that the crude oil in the system has reached a saturated state;
(4) Continuing to introduce natural gas, when the system pressure rises to the experimental specified pressure, opening the valve I13, observing the system pressure, and when the system pressure is constant at the specified pressure for 20min, indicating that the gas washing device 1 has reached a steady state; if the system pressure is reduced, opening a valve I13, and supplementing natural gas to the appointed pressure;
(5) Opening the valve III 15 and the valve IV 16, closing the valve II 14, and diffusing the natural gas in the gas washing reaction device 1 to the natural gas on-line collecting device 8;
(6) Opening the valve II 14, closing the valve IV 16, and injecting carrier gas into the natural gas online collection device 8, wherein the carrier gas is helium;
(7) And closing the valve III 15, and enabling the natural gas and the carrier gas to enter the second isotope mass spectrometer 9 so as to realize the online analysis of the natural gas carbon isotopes.
2. The method for analyzing the crude oil carbon isotopes comprises the following steps:
(1) Adding crude oil into the gas washing reaction device 1;
(2) Heating the gas wash reaction device 1 to a specified temperature according to experimental requirements;
(3) Closing a valve I13 to enable natural gas to enter the gas washing reaction device 1, and observing the indication of a pressure gauge 3 of the gas washing reaction device 1; when the system pressure begins to increase, indicating that the crude oil in the system has reached a saturated state;
(4) Continuing to introduce natural gas, when the system pressure rises to the experimental specified pressure, opening the valve I13, observing the system pressure, and when the system pressure is constant at the specified pressure for 20min, indicating that the gas washing device 1 has reached a steady state; if the system pressure is reduced, opening a valve I13, and supplementing natural gas to the appointed pressure;
(5) Opening the liquid nitrogen cold trap 20 and the liquid nitrogen cold trap 21 to ensure that the temperatures of the crude oil trace rapid sampling device 4 and the crude oil collecting device 5 cannot cause the loss of dissolved natural gas;
(6) The crude oil micro-rapid sampling device 4 is opened, a micro crude oil is taken and transferred to the crude oil collecting device 5, and the dissolved natural gas is ensured not to be lost due to the extremely low internal temperature;
(7) Opening the heating sleeve 22, heating the crude oil collecting device 5 to 900 ℃, closing the valve seven 19, and injecting oxygen 15 into the crude oil collecting device 5; the organic matters in the crude oil are completely burnt and reacted;
(8) Opening a valve seven 19, closing a valve five 17, and enabling gases such as carbon dioxide generated by the reaction to enter a carbon dioxide purifying device 6;
(9) Closing a valve six 18, and detecting the carbon dioxide gas prepared after purification by using a first isotope mass spectrometer 7 to obtain the carbon isotope value in the carbon dioxide gas in the crude oil, namely the carbon isotope value of the crude oil.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (9)

1. The gas washing fractionation analysis device under the high-temperature high-pressure sealing system is characterized by comprising a gas washing reaction device, a natural gas online collection device, an isotope mass spectrometer, a crude oil online trace rapid sampling device, a crude oil collection device, a carbon dioxide purification device, a valve, a heating sleeve and a liquid nitrogen cold trap;
the gas washing reaction device is respectively connected with the natural gas on-line collection device and the crude oil on-line micro rapid sampling device, and is connected with a natural gas source through a valve; the crude oil online trace rapid sampling device is sequentially connected with a crude oil collecting device, a carbon dioxide purifying device and a first isotope mass spectrometer; the natural gas online collection device is connected with a carrier gas source through a valve, and the second isotope mass spectrometer is connected with the natural gas online collection device; the crude oil collecting device is connected with an oxygen source through a valve, and is placed in the first liquid nitrogen cold trap, and the heating jacket surrounds the first liquid nitrogen cold trap; the crude oil on-line micro rapid sampling device is placed in a second liquid nitrogen cold trap.
2. The high-temperature high-pressure closed system gas wash fractionation analysis device according to claim 1, wherein the gas wash reaction device is further connected with a pressure gauge and a temperature control system respectively.
3. The high temperature and high pressure closed system gas wash fractionation analysis device according to claim 1, wherein a valve is provided on a pipeline between the gas wash reaction device and the crude oil collecting device.
4. The high temperature high pressure closed system gas wash fractionation analysis device according to claim 1, wherein a valve is provided on a pipeline connecting the natural gas on-line collection device and the second isotope mass spectrometer.
5. The gas wash fractionation analysis device under a high temperature and high pressure closed system according to claim 1, wherein valves are respectively provided on a pipeline connecting the crude oil collecting device and the carbon dioxide purifying device and a pipeline connecting the carbon dioxide purifying device and the first isotope mass spectrometer.
6. A method for fractional distillation and gas-wash analysis under a high-temperature high-pressure sealing system, characterized in that the method for fractional distillation and gas-wash analysis under a high-temperature high-pressure sealing system is adopted according to any one of claims 1 to 5, and comprises the following steps:
adding crude oil into a gas washing reaction device, and heating the gas washing reaction device to the temperature required by an experiment; introducing natural gas, and stopping introducing the natural gas after the pressure in the gas washing reaction device is increased to the pressure required by the experiment and reaches a stable state, so as to analyze carbon isotopes in the natural gas and crude oil;
the natural gas carbon isotope analysis steps include: the natural gas online collection device collects the natural gas in the gas washing reaction device, carrier gas is injected into the natural gas online collection device, and the natural gas and the carrier gas enter the second isotope mass spectrometer for online analysis of natural gas carbon isotopes;
the analysis steps of the carbon isotopes in the crude oil comprise: opening a liquid nitrogen cold trap to ensure that the temperatures of the crude oil trace rapid sampling device and the crude oil collecting device cannot cause the loss of dissolved natural gas; taking trace crude oil by a crude oil trace rapid sampling device, and completely transferring the trace crude oil to a crude oil collecting device; closing a liquid nitrogen cold trap, opening an electric heating sleeve to heat the crude oil collecting device, introducing oxygen into the crude oil collecting device, completely burning organic matters in crude oil, purifying carbon dioxide generated by burning, and performing carbon isotope analysis on the purified carbon dioxide.
7. The method of claim 6, wherein the carrier gas used in the natural gas carbon isotope analysis step is helium.
8. The method of claim 6, wherein in the step of analyzing the carbon isotopes in the crude oil, the crude oil collecting device is heated to 850-1000 ℃.
9. The method of claim 6, wherein the pressure in the gas wash reaction apparatus is increased to the pressure required for the experiment, and wherein the steady state is achieved after maintaining the pressure required for the experiment for at least 15 minutes.
CN202111476678.3A 2021-12-02 2021-12-02 Device and method for gas wash fractionation analysis under high-temperature high-pressure sealing system Pending CN116223601A (en)

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CN202111476678.3A CN116223601A (en) 2021-12-02 2021-12-02 Device and method for gas wash fractionation analysis under high-temperature high-pressure sealing system

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CN202111476678.3A CN116223601A (en) 2021-12-02 2021-12-02 Device and method for gas wash fractionation analysis under high-temperature high-pressure sealing system

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