CN115825286A - Experimental device and method for in-situ thermal cracking of solvent-assisted thickened oil to coke - Google Patents
Experimental device and method for in-situ thermal cracking of solvent-assisted thickened oil to coke Download PDFInfo
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Abstract
The invention discloses an experimental device and method for in-situ thermal cracking of thick oil into coke assisted by a solvent, wherein the device comprises an injection system, an experimental model system, a data monitoring system, a sample acquisition system and a sample analysis system; the injection system is connected with the inlet end of the reaction simulation system; a charging cup and a sand adding cup are arranged in a reaction model in the reaction simulation system; the data monitoring system is used for monitoring the temperature and the pressure at two ends of the reaction model; the sample collection system is connected with the outlet end of the experiment model system; after the reaction is finished, obtaining a coke sample in a charging cup; the invention can complete the deasphalting process of the thick oil, can also carry out the high-temperature oxidation thermal cracking experiment of heavy components such as deposited asphaltene and the like, can further and deeply know the change of physical and chemical properties generated in the thermal cracking reaction process of the heavy components after solvent extraction through the detection of related components, and provides theoretical support for the successive development and process design of oil reservoirs after solvent extraction.
Description
Technical Field
The invention relates to the technical field of oil extraction, in particular to an experimental device and method for in-situ thermal cracking of thickened oil into coke assisted by a solvent.
Background
The heavy oil accounts for about 70% of the global oil reserves and is an important substitute resource of conventional oil and gas. With the strong increase of global energy demand and the high development of thin oil in the future, the strategic position of thick oil will be more and more prominent. The heavy oil contains more heavy components and a small amount of impurities, and the oil product and the fluidity are poor, and the exploitation method comprises thermal exploitation methods such as steam injection, air injection, in-situ combustion and the like, and cold exploitation methods such as solvent extraction, chemical agents, miscible phase flooding and the like.
Steam injection is the most widely applied technology for improving the recovery ratio of the thickened oil so far, but the steam injection economy and adaptability are poor in deep and thin oil reservoirs due to serious heat loss, and the steam in-situ modification effect of the thickened oil is poor under the condition. In fact, only after steam injection is carried out for years, and the reservoir pressure is kept above 7MPa, the upgrading of the heavy oil can be obviously observed, and the investment and maintenance cost of steam injection equipment and steam injection pipeline heat insulation treatment is high, so the application prospect of the heavy oil in-situ upgrading exploitation is poor.
The solvent extraction technology is applied to the exploitation of thick oil, a solvent is injected into a stratum to dissolve part of crude oil components, so that the mobility of the crude oil is enhanced, heavy components such as asphaltene and the like separated by extraction are still retained in the stratum, so that the energy is not fully utilized, and the deposited heavy components such as asphaltene and the like can cause blockage and damage to the reservoir stratum to different degrees. In addition, due to the influence of reservoir geological factors and the physical property difference of crude oil, the exploitation efficiency of the heavy oil and the quality of the produced oil are difficult to accurately predict.
The solvent injection assisted thick oil thermal cracking in-situ modification technology can better improve the recovery ratio of thick oil, the thick oil is extracted by injecting the solvent, light components are extracted, then the deposited heavy components are subjected to high-temperature oxidative cracking, and when the temperature reaches 350-450 ℃, the asphaltene deposited after solvent extraction is cracked to generate coke and volatile products, so that the quality of the produced crude oil is improved, and the recovery ratio is also improved. However, the prior art mostly focuses on analyzing the change of the components of the thick oil before and after solvent extraction by extracting the thick oil with solvent vapor, but does not deeply research the process of secondary modification of heavy components such as deposited asphaltene. For the process technology of replacing the development mode after the heavy oil reservoir is extracted by using the solvent, the process technology is still in an exploration stage at present, and some technical problems still exist, so that the solvent-assisted in-situ thermal cracking of the heavy oil needs to be continuously tested and researched to supplement the technology. However, at present, no complete system can perform better simulation and analysis on the system in China.
Disclosure of Invention
Therefore, based on the above background, the present invention provides an experimental apparatus and method for in-situ thermal cracking of solvent-assisted heavy oil into coke, which can also be used for the research on the thermal cracking process of heavy components deposited after the solvent extraction of the heavy oil, and can realize quantitative analysis of the physical properties of the light components extracted by the solvent, the components of the gases discharged from the deposited heavy components during the high-temperature oxidation process, and the structural and compositional changes of the solid products generated after the reaction is terminated.
The technical scheme provided by the invention is as follows:
an experimental device for in-situ thermal cracking of thick oil into coke assisted by a solvent comprises an injection system, a reaction simulation system, a data monitoring system, a sample collection system and a sample analysis system;
the injection system injects liquid hydrocarbon solvent into the reaction simulation system;
the reaction simulation system comprises a high-temperature heating furnace and a reaction simulator, wherein the reaction simulator is positioned in the high-temperature heating furnace;
a charging cup and a sand adding cup are arranged in the reaction simulator, the charging cup is positioned above the sand adding cup, and the bottoms of the charging cup and the sand adding cup are both in a sieve shape; the charging cup is used for charging oil sand with a pore structure; the sand adding cup is used for filling quartz sand without oil, and the particle size of the quartz sand is smaller than that of the oil sand;
the sample analysis system comprises a rheometer, a crude oil four-component analyzer, an element analyzer, an infrared spectrometer and a micro gas chromatograph;
gas-liquid phase discharge materials in the reaction simulator are conveyed to a micro gas chromatograph of a sample analysis system through a pipeline, and one pipeline is conveyed to a sample collection system;
the data monitoring system monitors the pressure on the feeding pipe and the discharging pipe of the reaction simulator, and the data monitoring system monitors the temperature in the high-temperature heating furnace.
Further, the injection system comprises a solvent tank, and the liquid hydrocarbon solvent in the solvent tank is injected into the reaction simulation system through an injection pump;
a first valve and a first pressure gauge are arranged on a connecting pipeline of the solvent tank and the injection pump;
and a connecting pipeline of the injection pump and the reaction simulation system is provided with a second valve, a liquid meter and a third valve.
Furthermore, the injection system also comprises a nitrogen cylinder, and one end of a nitrogen discharge pipe of the nitrogen cylinder is connected to a connecting pipeline of the injection pump and the reaction simulation system;
a fifth valve and a first gas flowmeter are arranged on the nitrogen discharging pipe;
the junction of the nitrogen discharge pipe and the connecting pipeline of the injection pump and the reaction simulation system is positioned between the third valve and the fourth valve;
and a pressure controller is arranged between the fourth valve and the reaction simulation system on a connecting pipeline of the injection pump and the reaction simulation system.
Further, the reaction simulator is vertically placed in a high-temperature heating furnace, and liquid hydrocarbon solvent from the injection system enters a charging cup through a pipeline;
a first pressure sensor and a sixth valve are arranged on a feed pipeline of the reaction simulator; the first pressure sensor and the sixth valve are positioned in the high-temperature heating furnace;
a discharge pipeline of the reactor is provided with a second pressure sensor, a filter and a seventh valve; the second pressure sensor, the filter and the seventh valve are positioned in the high-temperature heating furnace;
the first pressure sensor and the second pressure sensor are electrically connected with the data monitoring system, and pressure signals collected by the first pressure sensor and the second pressure sensor are transmitted to the data monitoring system.
Furthermore, a thermocouple is arranged in the high-temperature heating furnace, the thermocouple is electrically connected with the data monitoring system through the temperature limiter, and signals collected by the thermocouple are transmitted to the data monitoring system.
Further, the sample collection system comprises an intermediate oil container, a vacuum pump, a liquid storage tank and a condensation system;
the reaction simulator is connected with the intermediate oil container through a pipeline; the intermediate oil container is connected with the storage tank through a pipeline; the vacuum pump is connected with the intermediate oil container;
a fourth pressure gauge and a ninth valve are arranged on a connecting pipeline of the reaction simulator and the intermediate oil container;
a branch pipe is led out from a connecting pipeline of the reaction simulator and the intermediate oil container and is connected with the condensing system;
a third pressure gauge and an eighth valve are arranged on the branch pipe;
the condensing system is connected with a miniature gas chromatograph of the sample analysis system through a pipeline.
The invention also provides a solvent-assisted thick oil in-situ thermal cracking experiment method based on the experiment device, which is characterized by comprising the following steps of:
1) Injecting nitrogen into the system, checking the air tightness, and then injecting a proper amount of liquid hydrocarbon solvent into a reaction simulator in the experimental model system;
2) The injected liquid hydrocarbon solvent is contacted with the oil sand filled in the charging cup under the action of gravity in the vertically arranged reaction simulator;
setting an experiment temperature, standing for 3-4 hours, completing the deasphalting process of the thick oil, extracting light components, and reserving heavy components such as colloid, asphaltene and the like in a charging cup in a reaction model;
3) The high-temperature heating furnace is heated to the experimental temperature at a constant speed, and the high-temperature oxidation thermal cracking experiment of the heavy component deposited after solvent extraction is carried out in the nitrogen atmosphere;
4) Respectively collecting liquid and gas generated in the experimental process through a sample collecting system, wherein a liquid storage tank is used for storing extracted oil extracted by a liquid hydrocarbon solvent, and gas generated in a high-temperature oxidation thermal cracking reaction enters a micro gas chromatograph for analysis after passing through a condensing system;
analyzing the collected liquid and gas for changes in composition and content by a sample analysis system;
5) And (3) keeping the temperature for a period of time after the reaction is finished, cooling, taking out a solid product in the charging cup, and cleaning by using a toluene solvent to obtain a coke sample.
The beneficial effects realized by adopting the invention are as follows:
1. the invention can carry out the experiment of high-temperature oxidative thermal cracking after extracting the thickened oil by a plurality of groups of different single/compound solvents, realizes the conversion of the operating conditions by the switch between the valves, controls the reaction temperature and the related parameters of the experiment according to the experiment requirements and increases the accuracy of the experiment.
2. The invention can utilize the characteristic that each component in the thickened oil has different solubility in hydrocarbon solvent to lead the liquid hydrocarbon solvent to dissolve the light component in the thickened oil, complete the deasphalting process of the thickened oil, test and analyze the components and physical properties of the extracted oil, then carry out the high-temperature oxidation thermal cracking experiment of heavy components such as deposited asphaltene and the like, respectively collect condensable components and non-condensable components in volatile gas by utilizing two groups of containers in a condensing system, further deeply know the change of the physicochemical properties generated in the thermal cracking reaction process of the heavy components after solvent extraction through the analysis of the generated non-condensable gas components, and provide theoretical support for the successive development and process design of oil reservoirs after solvent extraction.
Drawings
FIG. 1 is a schematic structural diagram of the present invention;
FIG. 2 is a schematic diagram of the condensing system;
FIG. 3 is a graph showing the relationship between the viscosity-temperature of the extracted oil and the viscosity-temperature of the crude oil after the thick oil is extracted with n-decane solvent at the target oil layer temperature and pressure in the example of the present invention;
FIG. 4 is the infrared spectrum and crude oil infrared spectrum analysis chart of the oil extracted after extracting thick oil with n-decane solvent at the temperature and pressure of the target oil layer.
The system comprises a solvent tank, a first valve, a first pressure gauge, a 4-injection pump, a second valve, a liquid meter, a third valve, a nitrogen gas cylinder, a 9-second pressure gauge, a fifth valve, a 10-first gas flowmeter, a fourth valve, a pressure controller, a sixth valve, a 15-first pressure sensor, a charging cup, a 17-reaction simulator 17, a sand charging cup, a 19-second pressure sensor, a filter, a seventh valve, a temperature limiter, a data monitoring system, a third pressure gauge, a 25-eighth valve, a 26-ninth valve, a 27-fourth pressure gauge, a 28-high temperature heating furnace, a 29-tenth valve, a middle oil container, a 31-eleventh valve, a 32-liquid storage tank, a 33-crude oil, a 34-rheometer, a 35-four-component analyzer, a 36-element analyzer, a 37-38, a gas phase condensation spectrometer, a micro computer system, a gas phase condensation system and a micro-micro computer.
Detailed Description
Reference will now be made in detail to embodiments of the invention, one or more examples of which are described below. Each example is provided by way of explanation, not limitation, of the invention. Indeed, it will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope or spirit of the invention. For instance, features illustrated or described as part of one embodiment, can be used on another embodiment to yield a still further embodiment.
It is therefore intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents. Other objects, features and aspects of the present invention are disclosed in or are apparent from the following detailed description. It is to be understood by one of ordinary skill in the art that the present discussion is a description of exemplary embodiments only, and is not intended as limiting the broader aspects of the present invention. The present invention will be further described with reference to the following examples.
Example 1: an experimental device for in-situ thermal cracking of thick oil into coke assisted by a solvent comprises an injection system, an experimental model system, a data monitoring system, a sample acquisition system and a sample analysis system.
The injection system comprises a solvent tank 1, and the liquid hydrocarbon solvent in the solvent tank 1 is injected into the reaction simulation system through an injection pump 4;
a first valve 2 and a first pressure gauge 3 are arranged on a connecting pipeline of the solvent tank 1 and the injection pump 4;
and a second valve 5, a liquid meter 6 and a third valve 7 are arranged on a connecting pipeline of the injection pump 1 and the reaction simulation system.
The injection system also comprises a nitrogen bottle 8, and one end of a nitrogen discharge pipe of the nitrogen bottle 8 is connected to a connecting pipeline between the injection pump 1 and the reaction simulation system;
a fifth valve 10 and a first gas flowmeter 11 are arranged on the nitrogen discharging pipe;
the intersection point of the nitrogen discharging pipe and the connecting pipeline of the injection pump 1 and the reaction simulation system is positioned between the third valve 7 and the fourth valve 12;
the connection line between the injection pump 1 and the reaction simulation system is provided with a pressure controller 13 between the fourth valve 12 and the reaction simulation system.
In this example, n-decane was used as the liquid hydrocarbon solvent in the solvent tank 1.
In particular, the liquid meter 6 can precisely measure the amount of the liquid hydrocarbon solvent injected into the reaction simulation system.
The reaction simulation system comprises a high-temperature heating furnace 28 and a reaction simulator 17, wherein the reaction simulator 17 is positioned in a furnace body in the high-temperature heating furnace 28; a charging cup 16 and a sand adding cup 18 are arranged in the reaction simulator 17, the charging cup 16 is positioned above the sand adding cup 18, and the bottoms of the charging cup 16 and the sand adding cup 18 are both in a screen shape; the charging cup 16 is used for charging oil sand with a pore structure; the sand adding cup 18 is used for filling quartz sand without oil mixing, and the particle size of the quartz sand is smaller than that of the oil sand;
the reaction simulator 17 is vertically arranged in a high-temperature heating furnace 28 with high sealing performance, and liquid hydrocarbon solvent from the injection system enters a charging cup 16 through a pipeline;
a first pressure sensor 15 and a sixth valve 14 are arranged on a feed pipeline of the reaction simulator 17; the first pressure sensor 15 and the sixth valve are positioned in the high-temperature heating furnace 28;
a discharge pipe line of the reactor 17 is sequentially provided with a second pressure sensor 19, a filter 20 and a seventh valve 21; the second pressure sensor 19, the filter 20 and the seventh valve 21 are positioned in the high-temperature heating furnace 28;
the first pressure sensor 16 and the second pressure sensor 19 are electrically connected with the data monitoring system, and pressure signals collected by the first pressure sensor 16 and the second pressure sensor 19 are transmitted to the data monitoring system 23.
A thermocouple is arranged in the high-temperature heating furnace 28, the thermocouple is electrically connected with the temperature limiter 22 and the data monitoring system 23, and a signal acquired by the thermocouple is transmitted to the data monitoring system.
In specific implementation, the precision of the thermocouple is +/-1 ℃, the working range is 0-800 ℃, the temperature limiter 22 controls the temperature of the reaction simulation system, and when the temperature of the system exceeds the working range of the thermocouple, the temperature limiter 22 plays a role in protection and cuts off the temperature rise of equipment; the filter 20 is used for removing a small amount of heavy components and particulate impurities such as asphaltene and the like which are settled in the reaction process.
The sample collection system comprises an intermediate oil container 30, a vacuum pump 33, a liquid reservoir tank 32, and a condensing system 40;
the reaction simulator 17 is connected to the intermediate oil container 30 through a pipeline; the intermediate oil container 30 is connected to a liquid reservoir tank 32 through a pipeline; the vacuum pump 33 is connected to the intermediate oil container 30; an eleventh valve 31 is provided on a connection line of the intermediate oil container 30 and the liquid reservoir tank 32.
In specific implementation, the vacuum pump 33 is used for pumping the liquid generated at the outlet end of the reaction simulation 17 and the liquid remained in the pipeline into the intermediate oil container 30, and then flowing into the liquid storage tank 32;
a fourth pressure gauge 27 and a ninth valve 26 are arranged on a connecting pipeline of the reaction simulator 17 and the intermediate oil container 30;
a branch pipe is led out from a connecting pipeline of the reaction simulator 17 and the intermediate oil container 30 and is connected with the condensing system;
a third pressure gauge 24 and an eighth valve 25 are arranged on the branch pipe;
the condensing system is connected by a line to a micro gas chromatograph 39 of the sample analysis system.
As shown in fig. 2, the condensing system 40 is used to condense the gas phase output from the reaction simulator 17 to meet the temperature requirements for detection by the micro gas chromatograph 39.
In one implementation mode, the condensation system consists of two groups of water bath bottles, each group of containers comprises three 100mL water bath bottles, the first group of water bath bottles on the left are sequentially No. 1, no. 2 and No. 3 from left to right, the second group of water bath bottles on the right are sequentially No. 4, no. 5 and No. 6 from left to right, and each water bath bottle is internally provided with 50mL isopropanol reagent, wherein the temperature of the water bath bottles No. 1, no. 2 and No. 3 is 38 ℃, and the temperature of the water bath bottles No. 4, no. 5 and No. 6 is-18 ℃;
the gas phase material that derives from reaction simulator is first through number 1, number 2 water bath bottle in proper order, and the gas phase material through number 2 water bath bottle is through number 4 after condensing, again through number 3 condensation, then after number 5, number 6 condense in proper order, adopts miniature gas chromatograph to its component analysis.
The micro gas chromatograph 39 is connected with the computer 38, and the detection and analysis result of the micro gas chromatograph 39 is displayed on the computer 38; the rheometer 34, the crude oil four-component analyzer 35, the elemental analyzer 36, and the infrared spectrometer 37 are used to analyze the components and properties of the extracted oil in the liquid reservoir tank 32.
The experimental device of the embodiment is adopted to carry out the experiment of solvent-assisted in-situ thermal cracking of thickened oil into coke, and comprises the following steps:
1) Injecting nitrogen into the system, checking the air tightness, and then injecting a proper amount of liquid hydrocarbon solvent into a reaction simulator 17 in the experimental model system;
the specific operation is as follows:
opening a fifth valve 10, a fourth valve 12 and a sixth valve 14, injecting nitrogen in a nitrogen bottle 8 into a charging cup 16 in a reaction model 17, closing the fifth valve 10 and the sixth valve 14 after the injection is finished, detecting the sealing performance of the reaction simulator 17, ensuring that the problem of poor sealing is avoided, then sequentially opening a first valve 2, a second valve 5, a third valve 7 and the sixth valve 14, injecting the liquid hydrocarbon solvent in the solvent tank 1 into the charging cup 16 through an injection pump 4, metering the injection amount of the liquid hydrocarbon solvent required by the experiment through a liquid metering device 6, and sequentially closing the first valve 2, the second valve 5, the third valve 7, the fourth valve 12 and the sixth valve 14 after the injection is finished.
2) The gravity action of the injected liquid hydrocarbon solvent in the vertically placed reaction simulator 17 is utilized to contact with the oil sand filled in the charging cup (16); setting an experiment temperature, standing for 3-4 hours to complete the deasphalting process of the thick oil, extracting light components, and leaving heavy components such as colloid, asphaltene and the like in a charging cup (16) in a reaction model (17);
the specific operation is as follows:
the reaction simulator 17 is vertically placed in the high-temperature heating furnace 28, the upper end of the reaction simulator 17 is an inlet end, the injected liquid hydrocarbon solvent flows from the inlet end direction to the outlet end direction of the reaction simulator 17 by utilizing the gravity action of the liquid hydrocarbon solvent injected into the charging cup 16, the liquid hydrocarbon solvent is fully contacted and mixed with the oil sand filled in the charging cup 16 and flows out through the sand adding cup 18 at the lower part of the reaction simulator 17, and the particle size of the quartz sand in the sand adding cup 18 is slightly smaller than that of the quartz sand in the charging cup 16 at the upper part, so that the sand adding cup 18 at the lower part plays a role in filtering solid particle impurities moved in the reaction process. Setting an experiment temperature, heating the reaction simulator 17 to a formation temperature by a high-temperature heating furnace 28, setting the experiment pressure as a target formation pressure through a pressure controller 13, carrying out well closing (standing) for 3-4 hours, transmitting pressure values to a data monitoring system 23 by a first pressure sensor 15 at the inlet end and a second pressure sensor 19 at the outlet end of the reaction model for monitoring, and finishing the process of solvent-assisted heavy oil deasphalting when the liquid hydrocarbon solvent extracts light components in the heavy oil.
3) The high-temperature heating furnace 28 is heated to the experimental temperature at a constant speed, and the high-temperature oxidation thermal cracking experiment of the heavy component deposited after solvent extraction is carried out in the nitrogen atmosphere;
4) Liquid and gas generated in the experimental process are respectively collected through a sample collecting system, a liquid storage tank (32) is used for storing extracted oil extracted by a liquid hydrocarbon solvent, and gas generated in the high-temperature oxidation thermal cracking reaction enters a micro gas chromatograph (39) for analysis after passing through a condensing system (40);
analyzing the collected liquid and gas for changes in composition and content by a sample analysis system;
5) And (3) keeping the temperature for a period of time after the reaction is finished, cooling, taking out the solid product in the charging cup (16), and cleaning by using a toluene solvent to obtain a coke sample.
The specific operations of steps 3) to 5) are as follows:
and opening a seventh valve 21, a ninth valve 26, a tenth valve 29 and an eleventh valve 31 in sequence, observing the condition of extracting thick oil by the liquid hydrocarbon solvent, enabling the extracted oil to flow into a liquid storage tank 32 through an intermediate oil container 30, and when the liquid hydrocarbon solvent extraction experiment is about to finish, pumping liquid flowing into a pipeline from the outlet end of the reaction model 17 into the intermediate oil container 30 by using a vacuum pump 33, and finally flowing into the liquid storage tank 32 for storage and metering. After the experiment of extracting the thickened oil by the liquid hydrocarbon solvent is finished, the seventh valve 21, the ninth valve 26, the tenth valve 29 and the eleventh valve 31 are closed, the extracted oil in the liquid storage tank 32 is analyzed by the rheometer 34, the crude oil four-component analyzer 35, the element analyzer 36 and the infrared spectrometer 37 in the sample analysis system, the viscosity-temperature relationship of the extracted oil is determined by the rheometer (the result is shown in the attached figure 3), the content changes of the saturates, the aromatics, the colloids and the asphaltins in the extracted oil are determined by the crude oil four-component analyzer, the content of the elements in the extracted oil is determined by the element analyzer, and the functional group changes of the extracted oil are determined by the infrared spectrometer (shown in the attached figure 4).
The asphaltene and other heavy components extracted by the liquid hydrocarbon solvent remain in the charging cup 16 in the reaction simulator 17 for subsequent high-temperature oxidation thermal cracking reaction experiments.
Opening the fifth valve 10, the fourth valve 12 and the sixth valve 14, injecting nitrogen in a nitrogen bottle 8 into a charging cup 16 at a constant injection rate, establishing a nitrogen purging atmosphere, closing the fifth valve 10 and the fourth valve 12 after the injection is completed, heating the reaction simulation 17 to a final experiment temperature (350 ℃ -450 ℃) at a constant temperature by a high-temperature heating furnace 28, wherein the heating rate is 5 ℃/min, the experiment temperature is monitored by a high-precision thermocouple, and is transmitted to a data monitoring system 23 through a temperature limiter 22, the experiment pressure is set through a pressure controller 13, and pressure values are transmitted to the data monitoring system 23 through a first pressure sensor 15 at the inlet end and a second pressure sensor 19 at the outlet end of the reaction simulator 17 for monitoring.
Opening the seventh valve 21 and the eighth valve 25, starting the high-temperature oxidation thermal cracking reaction of the heavy component deposited in the charging cup 16 on the upper portion of the reaction model 17, wherein the particle size of pure quartz sand in the sand adding cup 18 on the lower portion of the reaction model 17 is slightly smaller than that of quartz sand in the charging cup 16 on the upper portion, the sand adding cup 18 on the lower portion plays the same role as the filter 20 at the outlet end of the reaction model 17, filtering solid impurities such as settled asphaltene and the like in the reaction process, and double filtering ensures that the produced gas does not contain solid particle impurities, so that the gas phase generated by the reaction of the heavy component deposited in the charging cup 16 under the high-temperature and high-pressure conditions enters the condensing system 40, and the pressure value is observed through the third pressure gauge 24 at the inlet end of the condensing system 40.
And (3) keeping the temperature for 3 hours after the experiment is finished, cooling, taking out the solid product in the reaction simulator 17 for analysis, cleaning the taken-out solid product by using toluene as the asphaltene is soluble in the toluene and the coke is insoluble, weighing the residual substance after the toluene is dissolved in the solid product to determine the coke content, obtaining a coke sample, and analyzing the obtained coke sample by using instruments such as a scanning electron microscope, an X-ray diffractometer and the like.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
Claims (7)
1. An experimental device for in-situ thermal cracking of solvent-assisted thickened oil into coke is characterized by comprising an injection system, a reaction simulation system, a data monitoring system, a sample collection system and a sample analysis system;
the injection system injects liquid hydrocarbon solvent into the reaction simulation system;
the reaction simulation system comprises a high-temperature heating furnace and a reaction simulator, wherein the reaction simulator is positioned in the high-temperature heating furnace;
a charging cup and a sand adding cup are arranged in the reaction simulator, the charging cup is positioned above the sand adding cup, and the bottoms of the charging cup and the sand adding cup are both in a sieve shape; the charging cup is used for charging oil sand with a pore structure; the sand adding cup is used for filling quartz sand without oil, and the particle size of the quartz sand is smaller than that of the oil sand;
the sample analysis system comprises a rheometer, a crude oil four-component analyzer, an element analyzer, an infrared spectrometer and a micro gas chromatograph;
gas-liquid phase discharge materials in the reaction simulator are conveyed to a micro gas chromatograph of a sample analysis system through a pipeline, and one pipeline is conveyed to a sample collection system;
the data monitoring system monitors the pressure on the feeding pipe and the discharging pipe of the reaction simulator, and the data monitoring system monitors the temperature in the high-temperature heating furnace.
2. The experimental apparatus for in-situ thermal cracking of thick oil into coke assisted by solvent according to claim 1, wherein the injection system comprises a solvent tank, and the liquid hydrocarbon solvent in the solvent tank is injected into the reaction simulation system through an injection pump;
a first valve and a first pressure gauge are arranged on a connecting pipeline of the solvent tank and the injection pump;
and a connecting pipeline of the injection pump and the reaction simulation system is provided with a second valve, a liquid meter and a third valve.
3. The experimental facility for in-situ thermal cracking of thick oil into coke with solvent assistance according to claim 1, wherein the injection system further comprises a nitrogen gas cylinder, one end of a nitrogen gas discharge pipe of the nitrogen gas cylinder is connected to a connecting pipeline between the injection pump and the reaction simulation system;
a fifth valve and a first gas flowmeter are arranged on the nitrogen discharging pipe;
the junction of the nitrogen discharge pipe and the connecting pipeline of the injection pump and the reaction simulation system is positioned between the third valve and the fourth valve;
and a pressure controller is arranged between the fourth valve and the reaction simulation system on a connecting pipeline of the injection pump and the reaction simulation system.
4. The experimental facility for in-situ thermal cracking of thick oil into coke assisted by solvent as claimed in claim 3, wherein the reaction simulator is vertically placed in a high temperature heating furnace, and the liquid hydrocarbon solvent from the injection system enters the charging cup through a pipeline;
a first pressure sensor and a sixth valve are arranged on a feed pipeline of the reaction simulator;
a discharge pipeline of the reactor is provided with a second pressure sensor, a filter and a seventh valve; the second pressure sensor, the filter and the seventh valve are positioned in the high-temperature heating furnace;
the first pressure sensor and the second pressure sensor are electrically connected with the data monitoring system, and pressure signals collected by the first pressure sensor and the second pressure sensor are transmitted to the data monitoring system.
5. The experimental apparatus for in-situ thermal cracking of thick oil into coke assisted by solvent as claimed in claim 4, wherein a thermocouple is disposed in the high temperature heating furnace, the thermocouple is electrically connected to the data monitoring system through a temperature limiter, and the signal collected by the thermocouple is transmitted to the data monitoring system.
6. The apparatus of claim 4, wherein the sample collection system comprises an intermediate oil container, a vacuum pump, a liquid storage tank, and a condensing system;
the reaction simulator is connected with the intermediate oil container through a pipeline; the intermediate oil container is connected with the liquid storage tank through a pipeline; the vacuum pump is connected with the intermediate oil container;
a fourth pressure gauge and a ninth valve are arranged on a connecting pipeline of the reaction simulator and the intermediate oil container;
a branch pipe is led out from a connecting pipeline of the reaction simulator and the intermediate oil container and is connected with the condensing system;
a third pressure gauge and an eighth valve are arranged on the branch pipe;
the condensing system is connected with a miniature gas chromatograph of the sample analysis system through a pipeline.
7. A method for carrying out in-situ thermal cracking coke formation experiment of thick oil by solvent assisted by using the experimental device of any one of claims 1 to 6, which is characterized by comprising the following steps:
1) Injecting nitrogen into the system, checking the air tightness, and then injecting a proper amount of liquid hydrocarbon solvent into a reaction simulator in the experimental model system;
2) The injected liquid hydrocarbon solvent is contacted with the oil sand filled in the charging cup under the action of gravity in the vertically arranged reaction simulator; setting an experiment temperature, standing for 3-4 hours, completing the deasphalting process of the thick oil, extracting light components, and reserving heavy components such as colloid, asphaltene and the like in a charging cup in a reaction model;
3) The high-temperature heating furnace is heated to the experimental temperature at a constant speed, and the high-temperature oxidation thermal cracking experiment of the heavy component deposited after solvent extraction is carried out in the nitrogen atmosphere;
4) Respectively collecting liquid and gas generated in the experimental process through a sample collecting system, wherein a liquid storage tank is used for storing extracted oil extracted by a liquid hydrocarbon solvent, and gas generated in a high-temperature oxidation thermal cracking reaction enters a micro gas chromatograph for analysis after passing through a condensing system;
analyzing the collected liquid and gas for changes in composition and content by a sample analysis system;
5) And (3) after the reaction is finished, keeping the temperature for a period of time, cooling, taking out a solid product in the charging cup, and cleaning by using a toluene solvent to obtain a coke sample.
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