CN110763719A - Experimental device and method for thermal cracking of thickened oil into coke in-situ combustion process - Google Patents
Experimental device and method for thermal cracking of thickened oil into coke in-situ combustion process Download PDFInfo
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- 239000000571 coke Substances 0.000 title claims abstract description 59
- 238000004227 thermal cracking Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 21
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 20
- 238000004458 analytical method Methods 0.000 claims abstract description 65
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 56
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- 230000000704 physical effect Effects 0.000 claims abstract description 7
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- 239000007790 solid phase Substances 0.000 claims abstract description 5
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
- 238000002474 experimental method Methods 0.000 claims description 17
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- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
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- 239000012530 fluid Substances 0.000 claims description 6
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
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Abstract
The invention discloses an experimental device for thermal cracking of thickened oil into coke in an in-situ combustion process, which comprises a sample preparation system, a first multifunctional control pump, an experimental model system, a sampling system, a sample analysis system, a cleaning device, a second multifunctional control pump and a computer, wherein the sample preparation system is connected with the first multifunctional control pump; the sampling system comprises a fuel separator and a gas-liquid separator; one end of the sample preparation system is connected with the first multifunctional control pump through a pipeline, the other end of the sample preparation system is connected with the experimental model system through a pipeline, the upper end of the experimental model system is connected with the cleaning device, the second multifunctional control pump and the gas-liquid separator, and the lower end of the experimental model system is connected with the fuel separator; and the gas-liquid separator and the fuel separator are both connected with a sample analysis system. The method can quantitatively represent the reaction rate of thermal cracking of the thick oil under the oil reservoir condition in the nitrogen atmosphere, and quantitatively analyze various chemical reactions, the physical properties and composition changes of gas-liquid phases and the physical and chemical properties of a solid phase in the fuel deposition process of the thermal cracking reaction of the thick oil.
Description
Technical Field
The invention relates to the technical field of experimental devices in the field of tertiary development of petroleum, in particular to an experimental device and method for thermally cracking thickened oil into coke in an in-situ combustion process.
Background
The thickened oil resources in the world are very abundant, and account for a large proportion of the global oil and gas resources. Currently, heavy oil, super heavy oil, oil sands, and bitumen account for approximately 70% of the total amount of global petroleum resources. One report by the U.S. department of energy indicates that the potential reserves of global heavy oil resources are roughly 6 times greater than the reserves of conventional crude oil that have been explored. The thick oil resources are widely distributed all over the world, according to statistics, the global thick oil geological storage is about 8150 hundred million tons, and the annual output of the thick oil is over 127 hundred million tons. China has abundant thick oil resources, and the estimated resource reserves can reach more than 300 hundred million tons. More than 70 heavy oil fields have been discovered, focusing primarily on 12 basins. It can be said that in the present and future period, the development of heavy oil resources will take a great position in the development of global oil and gas resources.
Thermal oil recovery is the most important method for developing heavy oil reservoirs, and compared with the traditional thermal recovery technologies such as steam flooding and the like, the in-situ combustion technology has low CO2High discharge, high temperature, small heat loss, wide action range, capability of modifying crude oil on site and the like, thereby being more suitable for heavy oil resources which are difficult to use, such as super heavy oil, deep heavy oil, water-sensitive heavy oil and the like. At present, over 100 oil fields have developed extensive industrial exploitation tests all over the world, and the recovery rate can reach more than 80 percent at most.
In the process of thick oil fireflood, as the combustion front is the main oxygen consumption and heat generation area in the process of fireflood and serves as a key zone in the process of fireflood, the controllable expansion capability and stability of the combustion front determine the exploitation effect of the fireflood. The coke is used as an important solid fuel of a fire flooding combustion front edge, has stronger activity and lower ignition point, and has important significance for the fire flooding development of the thick oil.
At present, thermal analysis instruments such as TG-DSC and the like are generally adopted at home and abroad to research the mechanism of coke formation by thermal cracking of thick oil and the properties of the coke. In the process of using the thermal analyzer, because the added samples are less, the amount of coke generated by pyrolysis is very limited, and the influence of external conditions and experimental devices is large, the amount of the generated coke is difficult to accurately measure, and the research on the coke property and the pyrolysis coking mechanism is seriously influenced.
At present, for the deposition of the thick oil thermal cracking green coke fuel, no mature and complete experimental device and treatment method for better simulation and analysis of the thermal cracking of the thick oil under the oil reservoir condition exist in China, and the change rule of the heat release property and the activation energy is researched by the aid of a thermal analyzer in the traditional analysis. However, such methods currently have some disadvantages: 1) the amount of the added crude oil is small, the influence of uncontrollable factors such as experimental conditions, devices and the like is large, and the error of experimental measurement is large; 2) when crude oil reacts in a thermal analyzer, the reaction gas pressure is low, and the reaction condition of the crude oil under the oil reservoir condition cannot be well simulated, so the experimental effect is poor, and the experimental result is inaccurate; 3) the coke generated by the reaction is less, and further test analysis cannot be performed on the coke, so that the analysis on the thermal cracking reaction of the thick oil is incomplete, and the economic cost and the experimental error of the experiment can be increased by a repeatability experiment.
Disclosure of Invention
Aiming at the problems, the invention provides an experimental device and method for thermal cracking of thickened oil into coke in an in-situ combustion process, which can quantitatively represent the reaction rate of thermal cracking of the thickened oil in a nitrogen atmosphere under an oil reservoir condition and quantitatively analyze various chemical reactions, the change of physical properties and compositions of gas-liquid phases and the physicochemical properties of a solid phase in the fuel deposition process of the thermal cracking reaction of the thickened oil.
The invention adopts the following technical scheme:
an experimental device for thermal cracking of thickened oil into coke in an in-situ combustion process comprises a sample preparation system, a first multifunctional control pump, an experimental model system, a sampling system, a sample analysis system, a cleaning device, a second multifunctional control pump and a computer;
the sampling system comprises a fuel separator and a gas-liquid separator;
one end of the sample preparation system is connected with the first multifunctional control pump through a pipeline, the other end of the sample preparation system is connected with the experimental model system through a pipeline, the upper end of the experimental model system is connected with the cleaning device, the second multifunctional control pump and the gas-liquid separator, and the lower end of the experimental model system is connected with the fuel separator;
and the gas-liquid separator and the fuel separator are both connected with a sample analysis system.
Preferably, join in marriage a kind system and include the thermostated container and set up container, the middle container of third in the middle of first middle container, second in the middle of the thermostated container, the sample preparation ware in the middle of the third, the left end of container all links to each other with first multi-functional control pump through the pipeline in the middle of first middle container, second, the right-hand member of container is connected and is joined in marriage the sample preparation ware in the middle of first middle container, second, the other end of sample preparation ware and the right-hand member of container in the middle of the third all connect experiment model system.
Preferably, the experimental model system comprises a reaction kettle and a high-temperature heating furnace, and the reaction kettle is arranged in the high-temperature heating furnace.
Preferably, the sample analysis system comprises a gas sample analysis system, a liquid sample analysis system, a solid sample analysis system; the gas sample analysis system is connected with the upper end of the gas-liquid separator through a pipeline, the liquid sample analysis system is respectively connected with the lower end of the gas-liquid separator and the fuel separator through pipelines, and the solid sample analysis system is used for analyzing a solid sample separated by the fuel separator.
Preferably, the gas sample analysis system comprises a gas measuring instrument, a gas storage tank, a gas chromatograph and a mass spectrometer, wherein one end of the gas measuring instrument is connected with the upper end of the gas-liquid separator through a pipeline, the other end of the gas measuring instrument is connected with the gas storage tank, and the gas chromatograph and the mass spectrometer are used for analyzing gas components in the gas storage tank.
Preferably, the liquid sample analysis system comprises a liquid measuring instrument, an oil sample storage tank, an oil phase chromatograph, an infrared spectrometer, a rheometer, a thermogravimetric analyzer, a four-component analysis system and a second element analyzer, wherein one end of the liquid measuring instrument is respectively connected with the gas-liquid separator and the fuel separator through pipelines, the other end of the liquid measuring instrument is connected with the oil sample storage tank, and the oil phase chromatograph, the infrared spectrometer, the rheometer, the thermogravimetric analyzer, the four-component analysis system and the second element analyzer are used for analyzing components of the oil sample in the oil sample storage tank.
Preferably, the solid sample analysis system comprises a solid measuring instrument, a coke storage tank, an electron microscope, a first element analyzer and an infrared spectrometer, wherein one end of the solid measuring instrument is connected with the lower end of the fuel separator, the other end of the solid measuring instrument is connected with the coke storage tank, and the electron microscope, the first element analyzer and the infrared spectrometer are used for analyzing sample components in the coke storage tank.
Preferably, the computer is respectively connected with the first multifunctional control pump, the second multifunctional control pump and the sample preparation device.
The method of utilizing the experimental device for thermal cracking of the thick oil into coke in the in-situ oil burning process comprises the following steps:
s1, preparing the separated gas and the degassed crude oil into fluid under the formation condition according to the target oil reservoir parameters through a sample preparation system, and then uniformly mixing the fluid;
s2, injecting the prepared sample and nitrogen into the experiment model system through a first multifunctional control pump;
s3, starting an experimental model system, and enabling the thick oil to have a cracking reaction in the experimental model system in a nitrogen environment;
s4, respectively sampling the flue gas, the coke residue, the crude oil separation gas and the degassed crude oil generated by the reaction through a sampling system;
and S5, respectively measuring the components and physical properties of the gas phase, the liquid phase and the solid phase through a gas sample analysis system, a liquid sample analysis system and a solid sample analysis system.
Preferably, in step S3, during the cracking reaction of the heavy oil in the experimental model system, the cracking reaction of the crude oil in the porous medium and the interaction with the rock clay mineral are simulated by performing a sand filling experiment in the reaction kettle under the formation conditions.
The invention has the beneficial effects that:
1. according to the invention, the thickened oil can be compounded to the stratum condition, the anaerobic condition of the stratum is simulated by injecting nitrogen, the temperature condition of crude oil reaction is accurately controlled by a heating system, the interaction of crude oil and rock can be simulated by adding rock clay minerals, the thermal cracking reaction condition of crude oil in a porous medium can be simulated by filling sand, and the diversity and reliability of cracking experiments are improved;
2. the method can test and analyze flue gas formed by reaction, associated gas in crude oil, accurate components and physical properties of the crude oil before and after the reaction and physicochemical properties of coke separated by the reaction, and can accurately reflect the change of oil-gas two-phase physicochemical properties before and after cracking, the physicochemical properties of the coke formed by cracking and the influence rule of rock clay minerals on cracking to form coke, thereby providing a theoretical basis for screening the heavy oil reservoir suitable for the in-situ combustion exploitation technology.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below, and it is apparent that the drawings in the following description only relate to some embodiments of the present invention and are not limiting on the present invention.
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a graph comparing the viscosity of the separated oil phase components of the thickened oil of the present invention with the viscosity of crude oil;
FIG. 3 is a schematic diagram showing the mass loss of coke separated from the heavy oil at different temperature rise rates according to the present invention;
FIG. 4 is a DTG diagram of coke separated from heavy oil at different temperature rise rates according to the present invention;
FIG. 5 is a scanning electron microscope image of coke separated by heavy oil cracking according to the present invention;
wherein,
1-a first multifunctional control pump, 2-a first pressure gauge, 8-a first intermediate container, 9-a second intermediate container, 10-a third intermediate container, 13-a sample preparation device, 14-a first valve, 15-a second valve, 17-a reaction kettle, 18-a cleaning device, 19-a third valve, 20-a fuel separator, 21-a solid meter, 22-a coke storage tank, 23-an electron microscope, 24-a first element analyzer, 25-an infrared spectrometer, 26-a fourth valve, 27-a second pressure gauge, 29-a second multifunctional control pump, 30-a fifth valve, 31-a gas-liquid separator, 32-a sixth valve, 33-a liquid meter, 35-an oil sample storage tank, 36-a seventh valve, 37-a gas meter, 38-an eighth valve, 39-a gas storage tank, 40-a ninth valve, 41-a tenth valve, 42-a gas chromatograph, 43-a mass spectrometer, 44-oil phase chromatograph, 45-infrared spectrometer, 46-rheometer, 47-thermogravimetric analyzer, 48-four-component analysis system, 49-second element analyzer, 50-constant temperature box, 51-high temperature heating furnace
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
Unless otherwise defined, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this disclosure belongs. The use of the word "comprising" or "comprises", and the like, in this disclosure is intended to mean that the elements or items listed before that word, include the elements or items listed after that word, and their equivalents, without excluding other elements or items. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
The invention is further illustrated with reference to the following figures and examples.
As shown in fig. 1, an experimental apparatus for thermal cracking of thick oil into coke in an in-situ combustion process includes a sample preparation system, a first multifunctional control pump 1, an experimental model system, a sampling system, a sample analysis system, a cleaning device 18, a second multifunctional control pump 29, and a computer.
The sample preparation system comprises a thermostat 50, and a first middle container 8, a second middle container 9, a third middle container 10, a sample preparation device 13 and the thermostat 50 which are arranged in the thermostat 50, wherein the left ends of the first middle container 8, the second middle container 9 and the third middle container 10 are connected with a first multifunctional control pump 1 through pipelines, the right ends of the first middle container 8 and the second middle container 9 are connected with the sample preparation device 13, and the other end of the sample preparation device 13 and the right end of the third middle container 10 are connected with a reaction kettle 17 in an experiment model system.
The sample preparation device 13 is provided with an electric heating temperature control system and an automatic rotating device, and the electric heating temperature control system can control the internal temperature of the sample preparation device 13 to be in a set target oil deposit temperature range of-20-300 ℃ through a resistance wire. The automatic rotating device is connected to the middle part of a high-temperature high-pressure sample preparation container, so that the sample preparation container can rotate at a constant speed within the range of 360 degrees, and therefore, the separation gas and the stratum thickened oil can be uniformly mixed to a stratum state under the target oil reservoir condition. First multi-functional constant voltage control pump 1 is connected with the sample preparation ware 13 through the computer, and the computer links to each other with the pressure sensor in the sample preparation ware 13 through the RS232 interface, and the first multi-functional constant voltage control pump 1 of computer control makes sample preparation ware 13 internal pressure remain unanimous throughout through advancing the pump and withdrawing the pump.
The experimental model system comprises a high-temperature heating furnace 51 and a reaction kettle 17 arranged in the high-temperature heating furnace 51, wherein the upper end of the reaction kettle 17 is connected with a cleaning device 18, a second multifunctional control pump 29 and a gas-liquid separator 31 through pipelines, and the lower end of the reaction kettle 17 is connected with a fuel separator 20;
the volume of the reaction kettle 17 is 80ml, the reaction kettle can resist temperature of 450 ℃ and resist pressure of 40MPa, so that the process of stratum thick oil cracking reaction can be simulated, the rapid rise of pressure and temperature caused by thick oil cracking reaction can be borne, sand filling experiments can be performed in the reaction kettle in the cracking process, namely, different rock clay minerals are added, and the cracking reaction of crude oil in a porous medium and the interaction of the crude oil and the rock clay minerals under the condition of a target stratum are simulated. The volume of the high-temperature heating furnace 51 is 7L, the temperature range is 0-1000 ℃, different temperature gradients, heating rates, constant temperature time and the like can be set, and important guarantee is provided for reaction conditions of experiments.
The sampling system comprises a fuel separator 20 and a gas-liquid separator 31, wherein the fuel separator 20 comprises a Soxhlet extractor, one interface of the fuel separator 20 is used for collecting coke residues deposited at the bottom of the reaction kettle 17 in the reaction kettle 17, and the other interface is used for collecting an oil sample after reaction in the reaction kettle 17, and further separation and purification are carried out, namely, the Soxhlet extractor and toluene are used for separating and separating the coke residues and the oil sample of the reaction kettle 17; the gas-liquid separator 31 is connected with the second multifunctional constant pressure control pump 29, so that the pressure in the sampling process is ensured, the independent sampling of the gas phase, the separated gas and the separated oil phase after reaction is realized, and the guarantee is provided for calculating important parameters such as crude oil composition, cracking reaction rate and the like.
The gas-liquid separator 31 and the fuel separator 20 are both connected with a sample analysis system.
The sample analysis system comprises a gas sample analysis system, a liquid sample analysis system and a solid sample analysis system; the gas sample analysis system is connected with the upper end of the gas-liquid separator 31 through a pipeline, the liquid sample analysis system is respectively connected with the lower end of the gas-liquid separator 31 and the fuel separator 20 through pipelines, and the solid sample analysis system is used for analyzing a solid sample separated by the fuel separator 20.
The gas sample analysis system comprises a gas meter 37, a gas storage tank 39, a gas chromatograph 42 and a mass spectrum analyzer 43, wherein the gas meter 37 is a gas flow meter, one end of the gas meter 37 is connected with the upper end of the gas-liquid separator 31 through a pipeline, the other end of the gas meter is connected with the gas storage tank 39, and the gas chromatograph 42 and the mass spectrum analyzer 43 are used for analyzing gas components in the gas storage tank 39. The gas sample analysis system is capable of calculating the volume of gas by means of a gas meter 37 and testing the composition and content of the gas by means of a gas chromatograph 42 and a mass spectrometer 43.
The liquid sample analysis system comprises a liquid meter 33, an oil sample storage tank 35, an oil phase chromatograph 44, an infrared spectrometer 45, a rheometer 46, a thermogravimetric analyzer 47, a four-component analysis system 48 and a second element analyzer 49, wherein the liquid meter 33 is a density balance or a specific gravity electronic balance, one end of the liquid meter 33 is respectively connected with the gas-liquid separator 31 and the fuel separator 20 through pipelines, the other end of the liquid meter is connected with the oil sample storage tank 35, the oil phase chromatograph 44, the infrared spectrometer 45, the rheometer 46, the thermogravimetric analyzer 47, the four-component analysis system 48 and the second element analyzer 49 are used for analyzing components of an oil sample in the oil sample storage tank 35, and the four-component analysis system 48 is an automatic petroleum heavy oil family four-component tester.
The liquid sample analysis system is capable of testing the oil phase composition and content by the oil phase chromatograph 44; testing various groups generated by the cracking reaction by an infrared spectrometer 45; the physical property change of the thick oil before and after cracking is tested by a rheometer 46; the element content change of the thick oil before and after cracking is tested by a second element analyzer 49; testing the content change of the heavy oil alkane, aromatic hydrocarbon, colloid and asphaltene before and after cracking by a four-component analysis system 48; finally, the kinetic parameters of the coke deposited after the cracking reaction are measured by a thermogravimetric analyzer 47.
The solid sample analysis system comprises a solid measuring instrument 21, a coke storage tank 22, an electron microscope 23, a first element analyzer 24 and an infrared spectrometer 25, wherein the solid measuring instrument 21 is an analytical balance, one end of the solid measuring instrument 21 is connected with the lower end of the fuel separator 20, the other end of the solid measuring instrument is connected with the coke storage tank 22, and the electron microscope 23, the first element analyzer 24 and the infrared spectrometer 25 are used for analyzing sample components in the coke storage tank 22. The solid sample analysis system can observe the microstructure and the morphological characteristics of the coke through an electron microscope 23, test the elemental composition of the coke through a first elemental analyzer 24, and test the functional groups on the surface of the coke through an infrared spectrometer.
The computer is respectively connected with the first multifunctional control pump 1, the second multifunctional control pump 29 and the sample preparation device 13, and monitors and controls the sample preparation system and the experiment model system, so that various parameters in the experiment process can be recorded more accurately and in detail. And a first pressure gauge 2 and a second pressure gauge 27 are respectively arranged on connecting pipelines between the first multifunctional control pump 1 and the sample preparation system and between the second multifunctional control pump 29 and the experiment model system.
The method of utilizing the experimental device for thermal cracking of the thick oil into coke in the in-situ oil burning process comprises the following steps:
s1, preparing the separated gas and the degassed crude oil into fluid under the formation condition according to the target oil reservoir parameters through a sample preparation system, and then uniformly mixing the fluid;
s2, injecting the prepared sample and nitrogen into the experiment model system through the first multifunctional control pump 1;
s3, starting an experimental model system, and enabling the thick oil to have a cracking reaction in the experimental model system in a nitrogen environment; in the cracking reaction process of the thickened oil in the experimental model system, the cracking reaction of the crude oil in the porous medium and the interaction of the crude oil and rock clay minerals under the formation condition are simulated by carrying out a sand filling experiment in a reaction kettle.
S4, respectively sampling the flue gas, the coke residue, the crude oil separation gas and the degassed crude oil generated by the reaction through a sampling system;
and S5, respectively measuring the components and physical properties of the gas phase, the liquid phase and the solid phase through a gas sample analysis system, a liquid sample analysis system and a solid sample analysis system.
The specific experimental steps are as follows:
connecting all experimental devices, putting the prepared target stratum crude oil into a second intermediate container 9, putting separated gas and nitrogen into a first intermediate container 8 and a third intermediate container 10 respectively, heating to the stratum temperature through a constant temperature box 50, then injecting an oil sample and the separated gas into a sample preparation device 13 through a first multifunctional constant pressure control pump 1 according to the production gas-oil ratio in a target oil reservoir, heating and insulating the sample preparation device 13 (the target stratum temperature), and stirring the sample preparation device 13 for 12 hours under the condition of the target stratum pressure so that the oil sample and the gas sample can be uniformly mixed;
open first valve 14 in proper order, inject into reation kettle 17 with nitrogen gas according to the injection quantity of specific experimental requirement, close first valve 14, open second valve 15, inject into the formation crude oil of corresponding volume according to specific experimental requirement and get into reation kettle 17, close first valve 14 and second valve 15 after the injection is accomplished, heat reation kettle 17 to the experimental temperature through high temperature heating furnace 51, open fourth valve 26, can observe the pressure in reation kettle 17 through second manometer 27, pressure and temperature in the experimentation can be monitored through the computer, after the abundant reaction, sample analysis.
Open fourth valve 26, carry out the pressurize sample to the experimental apparatus through first multifunctional control pump 1 this moment, make the pressure of experimental apparatus among the sampling process all the time be formation pressure, so that the gas that dissolves in crude oil can not isolate along with the reduction of pressure, open fifth valve 30, let in gas-liquid separation appearance 31 with gas-liquid component, the gas that separates gets into in the gas metering appearance 37 through the seventh valve 36 of opening, through the volume of the accurate measurement gas of gas metering appearance 37, open eighth valve 38, collect gas through gas storage tank 39, open ninth valve 40, through mass spectrum analyzer 43 and gas chromatograph 42, the component and the content of the test output gas.
Closing the seventh valve 36, opening the sixth valve 32, accurately measuring the volume of the liquid phase by the liquid measuring instrument 33, collecting an oil sample by the oil sample storage tank 35, opening the tenth valve 41, testing the content of the components in the crude oil by the oil phase chromatography 44, testing the groups contained in the cracked crude oil by the infrared spectrometer 45, and testing the rheological property of the cracked crude oil by the rheometer 46; and the gas-oil ratio of the cracked crude oil is calculated by combining with related parameters such as separation gas, the exothermic property of the cracked crude oil is tested by a thermogravimetric analyzer 47, the content change of colloid and asphaltene of the cracked crude oil is tested by a four-component analysis system 48, and the content change of elements in the cracked crude oil is tested by a second element analyzer 49.
Open third valve 19, separate the coke residue that the schizolysis produced through fuel separator 20, open sixth valve 32, oil to among the gas-liquid separation appearance 31 also can separate through fuel separator 20, accurately meter the weight of solid through solid measurement appearance 21, collect coke storage tank 22 and collect coke, and observe the microstructure and the topography feature of coke with electron microscope 23, test the elemental composition of coke through first elemental analyzer 24, test coke surface functional group through infrared spectrometer 25.
After the experiment is finished, the whole system is cleaned through a cleaning device 18, the cleaning device 18 comprises a beaker and a pump for storing cleaning liquid, and two liquids, namely petroleum ether and distilled water, are filled in the beaker. And (3) performing solvent displacement cleaning on the thickened oil in the system by circularly injecting petroleum ether through a pump, cleaning out asphaltene attached to the pipe wall, and finally cleaning the whole system by pumping distilled water.
As shown in fig. 2, the viscosity of the separated oil phase component is compared with the viscosity of the crude oil after the thermal cracking reaction of the thick oil at 300 ℃,350 ℃ and 400 ℃ is performed in the reaction kettle 17;
fig. 3-4 show thermogravimetric analysis graphs of coke separated after thick oil undergoes a thermal cracking reaction at a set temperature of 400 ℃ in the reaction kettle 17;
FIG. 5 is a scanning electron microscope image of coke separated by heavy oil cracking according to the present invention;
although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. An experimental device for thermal cracking of thick oil into coke in an in-situ combustion process is characterized by comprising a sample preparation system, a first multifunctional control pump (1), an experimental model system, a sampling system, a sample analysis system, a cleaning device (18), a second multifunctional control pump (29) and a computer;
the sampling system comprises a fuel separator (20) and a gas-liquid separator (31);
one end of the sample preparation system is connected with the first multifunctional control pump (1) through a pipeline, the other end of the sample preparation system is connected with the experimental model system through a pipeline, the upper end of the experimental model system is connected with the cleaning device (18), the second multifunctional control pump (29) and the gas-liquid separator (31), and the lower end of the experimental model system is connected with the fuel separator (20);
and the gas-liquid separator (31) and the fuel separator (20) are both connected with a sample analysis system.
2. The experimental device for thermal cracking of thick oil into coke in-situ combustion process according to claim 1, characterized in that the sample preparation system comprises a thermostat (50), and a first intermediate container (8), a second intermediate container (9), a third intermediate container (10) and a sample preparation device (13) which are arranged in the thermostat (50), wherein the left ends of the first intermediate container (8), the second intermediate container (9) and the third intermediate container (10) are all connected with the first multifunctional control pump (1) through pipelines, the right ends of the first intermediate container (8) and the second intermediate container (9) are connected with the sample preparation device (13), and the other end of the sample preparation device (13) and the right end of the third intermediate container (10) are both connected with the experimental model system.
3. The experimental facility for thermal cracking of thick oil into coke in-situ combustion process as claimed in claim 1, wherein the experimental model system comprises a reaction kettle (17) and a high temperature heating furnace (51), and the reaction kettle (17) is disposed in the high temperature heating furnace (51).
4. The experimental facility for thermal cracking of thick oil into coke in an in-situ combustion process as claimed in claim 1, wherein the sample analysis system comprises a gas sample analysis system, a liquid sample analysis system, and a solid sample analysis system; the gas sample analysis system is connected with the upper end of the gas-liquid separator (31) through a pipeline, the liquid sample analysis system is respectively connected with the lower end of the gas-liquid separator (31) and the fuel separator (20) through pipelines, and the solid sample analysis system is used for analyzing a solid sample separated by the fuel separator (20).
5. The experimental device for thick oil thermal cracking into coke in-situ combustion process as claimed in claim 4, characterized in that the gas sample analysis system comprises a gas meter (37), a gas storage tank (39), a gas chromatograph (42) and a mass spectrometer (43), one end of the gas meter (37) is connected with the upper end of the gas-liquid separator (31) through a pipeline, the other end is connected with the gas storage tank (39), and the gas chromatograph (42) and the mass spectrometer (43) are used for analyzing the gas components in the gas storage tank (39).
6. The experimental device for thick oil thermal cracking to coke in-situ combustion process according to claim 4, wherein the liquid sample analysis system comprises a liquid meter (33), an oil sample storage tank (35), an oil phase chromatograph (44), an infrared spectrometer (45), a rheometer (46), a thermogravimetric analyzer (47), a four-component analysis system (48) and a second element analyzer (49), one end of the liquid meter (33) is respectively connected with the gas-liquid separator (31) and the fuel separator (20) through pipelines, the other end of the liquid meter is connected with the oil sample storage tank (35), and the oil phase chromatograph (44), the infrared spectrometer (45), the rheometer (46), the thermogravimetric analyzer (47), the four-component analysis system (48) and the second element analyzer (49) are used for analyzing components of the oil sample in the oil sample storage tank (35).
7. The experimental device for thick oil thermal cracking into coke in-situ combustion process according to claim 4, characterized in that the solid sample analysis system comprises a solid measuring instrument (21), a coke storage tank (22), an electron microscope (23), a first element analyzer (24) and an infrared spectrometer (25), wherein one end of the solid measuring instrument (21) is connected with the lower end of the fuel separator (20), the other end is connected with the coke storage tank (22), and the electron microscope (23), the first element analyzer (24) and the infrared spectrometer (25) are used for analyzing sample components in the coke storage tank (22).
8. The experimental facility for thermal cracking of thick oil into coke in an in-situ combustion process as claimed in any one of claims 1 or 2, wherein said computer is connected to the first multifunctional control pump (1), the second multifunctional control pump (29) and the sample distributor (13).
9. A method for using the experimental apparatus for thermal cracking of thick oil into coke in an in-situ combustion process of claim 1, comprising the steps of:
s1, preparing the separated gas and the degassed crude oil into fluid under the formation condition according to the target oil reservoir parameters through a sample preparation system, and then uniformly mixing the fluid;
s2, injecting the prepared sample and nitrogen into the experiment model system through the first multifunctional control pump (1);
s3, starting an experimental model system, and enabling the thick oil to have a cracking reaction in the experimental model system in a nitrogen environment;
s4, respectively sampling the flue gas, the coke residue, the crude oil separation gas and the degassed crude oil generated by the reaction through a sampling system;
and S5, respectively measuring the components and physical properties of the gas phase, the liquid phase and the solid phase through a gas sample analysis system, a liquid sample analysis system and a solid sample analysis system.
10. The method as claimed in claim 9, wherein in step S3, the cracking reaction of the crude oil in the porous medium and the interaction with the rock clay minerals are simulated by performing sand filling experiments in the reaction kettle during the cracking reaction of the heavy oil in the experimental model system.
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