Shale oil in-situ thermal cracking reaction experimental device and use method thereof

Abstract

The invention discloses a shale oil in-situ thermal cracking reaction experimental device and a use method thereof, the shale oil in-situ thermal cracking reaction experimental device comprises a continuous gas injection pressurization system and a cracking reactor which are connected in sequence, and further comprises a sample collection system; an electric heating rod is arranged in the cracking reactor; the electric heating rod is an annular heating rod, and a reaction bin is arranged in the electric heating rod; a gas measuring assembly and a liquid measuring assembly are arranged in the sample collecting system. According to the invention, by changing the type and flow of injected gas and carrying out experiments at different heating rates, pyrolysis final temperatures and pyrolysis time, samples are collected and analyzed, the relationship between each reaction parameter and the product structure and yield can be determined, and the designed reaction bin can react with shale oil cores at the highest temperature of 800 DEG C and under the pressure of 20 MPa.

Description

Technical Field

[0001] The invention relates to the technical field of crude oil thermal cracking experimental devices, in particular to an in-situ thermal cracking reaction experimental device for shale oil and a use method thereof. Background Art

[0002] Shale oil resources have great potential. As an important alternative energy source, seeking ways to effectively develop and economically utilize shale oil is of great practical significance to alleviating the contradiction between energy supply and demand. Shale oil is an unconventional oil and gas resource that is difficult to exploit. Its cracking process is complex, and a large amount of experimental research is required to better understand and master the nature and mechanism of its cracking reaction. Compared with traditional oil, shale oil contains more light hydrocarbons that are difficult to separate, so it is more difficult to mine and process. In order to utilize this resource, people have developed many shale oil processing technologies, among which shale oil in-situ thermal cracking technology is a more commonly used method.

[0003] The in-situ thermal cracking technology of shale oil decomposes shale oil into simpler hydrocarbons under high temperature and high pressure conditions, thereby realizing resource utilization. At present, the commonly used shale oil thermal cracking reaction devices mainly include fluidized bed cracking reactors, fixed bed cracking reactors, etc. The heating temperature of the fluidized bed thermal cracking method is usually between 400℃-700℃, and the pressure is between 1-5MPa. Compared with the fluidized bed thermal cracking method, the fixed bed thermal cracking method requires a slightly lower heating temperature. In the fixed bed thermal cracking method, the heating temperature is generally between 300℃-600℃, and the pressure is between 0.1-5MPa.

[0004] Under high temperature and high pressure conditions, the existing shale oil thermal cracking technology still has many defects. The most critical one is that the heating temperature is not enough and the pressure is too low, which is far from the actual formation conditions.

[0005] Publication (Announcement) No.: CN113075247B, discloses a hydrocarbon hydration pyrolysis simulation experimental device and method, the hydrocarbon hydration pyrolysis simulation experimental device comprises an oven and a cooling box, the oven is provided with an autoclave inside, the autoclave is connected to a pressure detector and a weight detector; the cooling box is provided with a gas-liquid separator inside, the gas-liquid separator has an air inlet, an exhaust port and a liquid discharge port, the air inlet is connected to the exhaust valve of the autoclave through a connecting pipe, the exhaust port is connected to a gas chromatograph, and the liquid discharge port is connected to a liquid chromatograph. This prior art can simulate the thermal alteration of crude oil and the migration, desorption and property changes of the produced hydrocarbons of the crude oil under the original water-containing conditions of the shale reservoir.

[0006] This prior art measures the composition of the product, but does not measure the weight or volume of the product.

[0007] Publication (announcement) number: CN116422237A, discloses an experimental pyrolysis furnace and a pyrolysis system, including a main gas tank, a pyrolysis furnace, a fan, a condenser, a gas storage tank and a gas collecting tank; the main gas tank is connected to the gas storage tank through a pipeline, the pyrolysis furnace is connected to the condenser through a pipeline c, the gas storage tank is connected to the pipeline c through a pipeline a, the pyrolysis furnace is connected to the pipeline a through a pipeline b, the condenser is connected to the gas collecting tank through a pipeline d, and the pipeline d is connected to the pipeline a through a pipeline e; the pipeline a is arranged with a first valve, a second valve, a fan and a third valve, and the pipeline b is arranged with a fourth valve; the pipeline c is arranged with a fifth valve and a sixth valve; the pipeline d is installed with a seventh valve; the pipeline e is installed with an eighth valve, and the flow direction of the gas is changed by a three-way valve to enter different equipment to realize three different pyrolysis modes, meet the needs of multiple pyrolysis modes in the research, and greatly simplify the experimental process.

[0008] This prior art has the technical defect that no liquid recovery device is provided.

[0009] Publication (Announcement) No.: CN211500629U, discloses an oil shale in-situ simulated pyrolysis device, belonging to the field of unconventional energy mining, and is composed of a core clamping mechanism, a confining pressure pressurizing mechanism, and a high-temperature and high-pressure sealing mechanism. The core clamping mechanism is composed of a sample sleeve and a clamping gasket, the confining pressure pressurizing mechanism is composed of a pressurizing sleeve and an intermediate sleeve, and the high-temperature and high-pressure sealing mechanism is composed of a first pressure sleeve, a first pressure ring, a second pressure ring, a second pressure sleeve, and a seal. It can apply confining pressure to the oil shale core to simulate the in-situ stress state of the oil shale, and can also inject gas from one end. After passing through the oil shale core, the gas is discharged from the other end to achieve the cracking of the oil shale under high temperature and high confining pressure. The device proposed by the utility model can effectively simulate the real temperature-pressure environment of the underground oil shale layer during the heating process, and obtain the underground in-situ cracking characteristics of the oil shale through experimental research, thereby guiding the actual mining project.

[0010] This prior art has no active heating and is difficult to maintain the experimental temperature.

[0011] In summary, the technical solutions of the above-disclosed technologies, the technical problems to be solved, and the beneficial effects produced are all different from the present invention. Regarding more technical features, technical problems to be solved, and beneficial effects of the present invention, the above-disclosed technical documents do not provide any technical inspiration. Summary of the invention

[0012] In view of the above-mentioned defects in the prior art, the purpose of the present invention is to provide a shale oil in-situ thermal cracking reaction experimental device and a method of using the same, so as to achieve the reaction of shale oil cores at a maximum temperature of 800°C and a pressure of 20MPa, and overcome the above-mentioned deficiencies of the prior art, and can effectively solve the shortcomings of existing thermal cracking chamber experiments under high temperature and high pressure conditions.

[0013] In order to achieve the above object, the present invention adopts the following technical solutions:

[0014] A shale oil in-situ thermal cracking reaction experimental device, comprising a continuous gas injection and pressurization system and a cracking reactor connected in sequence, and also comprising a sample collection system;

[0015] An electric heating rod is arranged in the cracking reactor; the electric heating rod is a ring-shaped heating rod, and the interior is a reaction chamber;

[0016] The sample collection system is provided with a gas measurement component and a liquid measurement component.

[0017] An outer insulation layer is arranged outside the cracking reactor, and an electric heating rod is arranged inside the cracking reactor;

[0018] The reaction chamber is provided with a sample outlet at the bottom of the chamber, and the sample collection system is connected with the sample outlet of the reaction chamber;

[0019] An opening and closing top cover is arranged on the top of the cracking reactor, and a pressure sensor, a temperature sensor and a temperature controller are arranged on the opening and closing top cover.

[0020] The sample collection system comprises a cooling part and a gas-liquid separation part which are connected in sequence; and also comprises a gas measurement component and a liquid measurement component which are respectively connected to the gas-liquid separation part.

[0021] The cooling part includes a gas-liquid mixing tube and a low-temperature condensation tank arranged on the gas-liquid mixing tube, and the gas-liquid mixing tube is respectively provided with a second throttle valve and a third throttle valve in front and rear of the low-temperature condensation tank; the front end of the gas-liquid mixing tube is connected to the sample outlet of the reaction chamber, and the rear end of the gas-liquid mixing tube is connected to the gas-liquid separation part.

[0022] The gas-liquid separation part includes a gas-liquid separator, a liquid outlet pipe is arranged at the bottom of the gas-liquid separator, a gas outlet pipe and a mixture inlet pipe are arranged at the top, the mixture inlet pipe is inserted into the gas-liquid separator, and a fourth throttle valve is arranged on the liquid outlet pipe; the gas-liquid mixing pipe is connected to the mixture inlet pipe.

[0023] The liquid measuring assembly comprises a measuring cylinder and an electronic balance, wherein the electronic balance is below the liquid outlet pipe and the measuring cylinder is on the electronic balance.

[0024] The gas measurement assembly comprises a drying tank, a gas flow meter, and an air bag; the drying tank is arranged at the upper end of the gas outlet pipe, the gas flow meter is arranged at the drying tank outlet, and the air bag is arranged at the gas flow meter outlet.

[0025] The continuous gas injection and pressurization system comprises a gas injection pipe, and a gas source interface, a pressure regulating valve, and a first throttle valve which are sequentially arranged on the gas injection pipe;

[0026] The gas injection pipe is inserted into the cracking reactor.

[0027] A method for using a shale oil in-situ thermal cracking reaction experimental device comprises the following steps:

[0028] S1: Connect the experimental instruments as shown in the figure and place the prepared core into the reaction chamber of the cracking reactor;

[0029] S2: Open the pressure regulating valve and the first throttle valve, and introduce the gas required for the experiment into the reaction chamber through the gas source interface;

[0030] S3: Close the first throttle valve to stop gas injection, heat the reaction chamber to the specified temperature of the experiment and then keep the temperature constant so that the core reacts under the experimental temperature and pressure conditions;

[0031] S4: After the specified pyrolysis reaction time of the core is over, the oil and gas generated by the reaction are separated and collected in the sample collection system; the second throttle valve is opened, and the cracking products are completely entered into the low-temperature condensation tank, and the second throttle valve is closed. After the cracking products are cooled, the third throttle valve is opened to allow the cracking products to enter the gas-liquid separator, and the third throttle valve is closed. The cracking gas is dried in the drying tank, and the gas flow meter measures the cracking gas flow. The gas bag collects the cracking gas. When the gas flow meter remains stable, the fourth throttle valve is opened. When the cracking liquid completely enters the measuring cylinder, the number of scales in the measuring cylinder and the count of the electronic balance are recorded.

[0032] S5: Arrange the experimental instruments, repeat the above steps by changing the experimental conditions, and make comparisons.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] 1. The designed reaction chamber can react shale oil core at a maximum temperature of 800°C and a pressure of 20MPa, solving the blank problem of reaction experiments in shale oil thermal cracking chamber under ultra-high temperature and high pressure conditions;

[0035] 2. The whole set of experimental equipment is simple and easy to operate, occupies a small area and is highly economical;

[0036] 3. The experimental device of the present invention can collect and analyze samples by changing the type and flow rate of injected gas and conducting experiments at different heating rates, pyrolysis final temperatures, and pyrolysis times, and can determine the relationship between various reaction parameters and product structure and yield. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 It is a structural schematic diagram of a shale oil in-situ thermal cracking reaction experimental device of the present invention;

[0038] In the figure: 1. gas source interface; 2. pressure regulating valve; 3. first throttle valve; 4. pressure sensor; 5. temperature sensor; 6. temperature controller; 7. outer insulation layer; 8. electric heating rod; 9. reaction chamber; 10. second throttle valve; 11. low-temperature condensation tank; 12. third throttle valve; 13. air bag; 14. gas flow meter; 15. drying tank; 16. gas-liquid separator; 17. fourth throttle valve; 18. measuring cylinder; 19. electronic balance. DETAILED DESCRIPTION

[0039] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0040] See also Figure 1 The present invention provides a shale oil in-situ thermal cracking reaction experimental device and a method of using the same, comprising a continuous gas injection and pressurization system, a cracking reactor, and a sample collection system connected in sequence;

[0041] The continuous gas injection and pressurization system comprises a gas injection pipe, and a gas source interface 1, a pressure regulating valve 2, and a first throttle valve 3 which are sequentially arranged on the gas injection pipe, and the gas injection pipe is inserted into a cracking reactor.

[0042] The gas source interface 1 is used to connect the gas source to the device to provide the gas required for the experiment.

[0043] The pressure regulating valve 2 ensures that the gas pressure inside the device is within the required range by regulating the gas pressure.

[0044] The first throttle valve 3 acts as a switch to control the gas flow rate and ensure the stability and adjustability of the gas supply during the experiment.

[0045] An outer insulation layer 7 is arranged outside the cleavage reactor, an electric heating rod 8 is arranged inside the cleavage reactor, the electric heating rod 8 is a ring-shaped heating rod, and a reaction chamber 9 is arranged inside. The reaction chamber 9 has a sample outlet arranged at the bottom of the chamber itself, and the sample collection system is connected to the sample outlet of the reaction chamber 9; an opening and closing top cover is arranged on the top of the cleavage reactor, and a pressure sensor 4, a temperature sensor 5, and a temperature controller 6 are arranged on the opening and closing top cover.

[0046] The pressure sensor 4 monitors the pressure change in the cracking reactor and transmits the data to the temperature controller 6 for processing and recording.

[0047] The temperature sensor 5 measures the temperature in the cracking reactor and transmits the data to the temperature controller 6 for temperature control and monitoring.

[0048] The temperature controller 6 controls the power supply of the electric heating rod 8 according to the set temperature requirement, thereby realizing accurate control of the temperature in the cracking reactor.

[0049] The outer thermal insulation layer 7 wraps the cracking reactor, provides a good thermal insulation effect, and ensures the temperature stability in the cracking reactor.

[0050] The electric heating rod 8 is used to heat the cracking reactor.

[0051] The reaction chamber 9 is used for shale sample reaction.

[0052] The sample collection system comprises a cooling part and a gas-liquid separation part which are connected in sequence; and also comprises a gas measurement component and a liquid measurement component which are respectively connected to the gas-liquid separation part.

[0053] The cooling part includes a gas-liquid mixing tube and a low-temperature condensation tank 11 arranged on the gas-liquid mixing tube, and the gas-liquid mixing tube is provided with a second throttle valve 10 and a third throttle valve 12 in front and rear of the low-temperature condensation tank 11, respectively; the front end of the gas-liquid mixing tube is connected to the sample outlet of the reaction chamber 9, and the rear end of the gas-liquid mixing tube is connected to the gas-liquid separation part;

[0054] The gas-liquid separation part includes a gas-liquid separator 16, which has a liquid outlet pipe at the bottom, a gas outlet pipe and a mixture inlet pipe at the top, the mixture inlet pipe is inserted into the gas-liquid separator 16, and a fourth throttle valve 17 is arranged on the liquid outlet pipe; the gas-liquid mixing pipe is connected to the mixture inlet pipe.

[0055] The liquid measuring assembly includes a measuring cylinder 18 and an electronic balance 19, wherein the electronic balance 19 is below the liquid outlet pipe and the measuring cylinder 18 is on the electronic balance 19;

[0056] The gas measurement assembly includes a drying tank 15, a gas flow meter 14, and an air bag 13; the drying tank 15 is arranged at the upper end of the gas outlet pipe, the gas flow meter 14 is arranged at the outlet of the drying tank 15, and the air bag 13 is arranged at the outlet of the gas flow meter 14.

[0057] The low temperature condensation tank 11 is used to cool and liquefy the gas generated by the reaction for further processing and analysis.

[0058] The gas-liquid separator 16 is used to separate gas and liquid samples to ensure the purity of the collected samples.

[0059] The second, third and fourth throttle valves act as switches.

[0060] The air bag 13 is used to collect the generated gas sample and keep its pressure stable.

[0061] The gas flow meter 14 measures the gas flow and records the data of gas generation.

[0062] The drying tank 15 is used to remove moisture from the sample to minimize moisture interference during the experiment.

[0063] The measuring cylinder 18 is used to measure the volume of the liquid produced by the reaction.

[0064] The electronic balance 19 is used to measure the mass of the liquid produced by the reaction.

[0065] The method of using the present invention mainly comprises the following steps:

[0066] S1: Press the experimental instrument Figure 1 As shown, the prepared core is placed in the reaction chamber 9 of the cracking reactor;

[0067] S2: Open the pressure regulating valve 2 and the first throttle valve 3, and introduce the gas required for the experiment into the reaction chamber through the gas source interface 1;

[0068] S3: closing the first throttle valve 3 to stop gas injection, heating the reaction chamber to the specified experimental temperature and then maintaining the constant temperature to allow the core to react under the experimental temperature and pressure conditions;

[0069] S4: After the specified pyrolysis reaction time of the core is over, the oil and gas generated by the reaction are collected and separated. The specific operation is: open the second throttle valve 10, wait for the cracking product to completely enter the low-temperature condensation tank 11, close the second throttle valve 10, wait for the cracking product to cool, open the third throttle valve 12, let the cracking product enter the gas-liquid separator 16, close the third throttle valve 12, the cracking gas passes through the drying tank 15 to dry the gas, the gas flow meter 14 measures the cracking gas flow, the gas bag 15 collects the cracking gas, when the gas flow meter 14 remains stable, open the fourth throttle valve 17, when the cracking liquid completely enters the measuring cylinder 18, record the number of ticks in the measuring cylinder 18 and the count of the electronic balance 19.

[0070] S5: Arrange the experimental instruments, repeat the above steps by changing the experimental conditions, and make comparisons.

[0071] The experimental device of the present invention can perform experiments by changing the type and flow rate of injected gas and at different heating rates, pyrolysis final temperatures, and pyrolysis times, collect and analyze samples, and determine the relationship between each reaction parameter and the product structure and yield.

[0072] All components and connection methods of components not discussed in this application belong to the known technologies in this technical field and can be directly applied without further explanation.

[0073] In the present invention, the term "plurality" refers to two or more than two, unless otherwise clearly defined. The terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; "connected" can be a direct connection or an indirect connection through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to the specific circumstances.

[0074] In the description of the present invention, it is necessary to understand that the directions or positional relationships indicated by terms such as “upper”, “lower”, “left”, “right”, “front” and “back” are based on the directions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or unit referred to must have a specific direction, be constructed and operated in a specific orientation, and therefore, cannot be understood as a limitation on the present invention.

[0075] In the description of this specification, the description of the terms "one embodiment", "some embodiments", "specific embodiments", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0076] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A shale oil in-situ thermal cracking reaction experimental device, comprising a continuous gas injection pressurization system and a cracking reactor connected in sequence, It is characterized in that Also included is a sample collection system; An electric heating rod is arranged in the cracking reactor; the electric heating rod is a ring-shaped heating rod, and the interior is a reaction chamber; The sample collection system is provided with a gas measurement component and a liquid measurement component.

2. A shale oil in-situ thermal cracking reaction experimental device according to claim 1, It is characterized in that An outer insulation layer is arranged outside the cracking reactor, and an electric heating rod is arranged inside the cracking reactor; The reaction chamber is provided with a sample outlet at the bottom of the chamber, and the sample collection system is connected with the sample outlet of the reaction chamber; An opening and closing top cover is arranged on the top of the cracking reactor, and a pressure sensor, a temperature sensor and a temperature controller are arranged on the opening and closing top cover.

3. A shale oil in-situ thermal cracking reaction experimental device according to claim 2, It is characterized in that The sample collection system comprises a cooling part and a gas-liquid separation part which are connected in sequence; and also comprises a gas measurement component and a liquid measurement component which are respectively connected to the gas-liquid separation part.

4. A shale oil in-situ thermal cracking reaction experimental device according to claim 3, It is characterized in that The cooling part includes a gas-liquid mixing tube and a low-temperature condensation tank arranged on the gas-liquid mixing tube, and the gas-liquid mixing tube is respectively provided with a second throttle valve and a third throttle valve in front and rear of the low-temperature condensation tank; the front end of the gas-liquid mixing tube is connected to the sample outlet of the reaction chamber, and the rear end of the gas-liquid mixing tube is connected to the gas-liquid separation part.

5. A shale oil in-situ thermal cracking reaction experimental device according to claim 4, It is characterized in that The gas-liquid separation part includes a gas-liquid separator, a liquid outlet pipe is arranged at the bottom of the gas-liquid separator, a gas outlet pipe and a mixture inlet pipe are arranged at the top, the mixture inlet pipe is inserted into the gas-liquid separator, and a fourth throttle valve is arranged on the liquid outlet pipe; the gas-liquid mixing pipe is connected to the mixture inlet pipe.

6. A shale oil in-situ thermal cracking reaction experimental device according to claim 5, It is characterized in that The liquid measuring assembly comprises a measuring cylinder and an electronic balance, wherein the electronic balance is below the liquid outlet pipe and the measuring cylinder is on the electronic balance.

7. The shale oil in-situ thermal cracking reaction experimental device according to claim 5, It is characterized in that The gas measurement assembly comprises a drying tank, a gas flow meter, and an air bag; the drying tank is arranged at the upper end of the gas outlet pipe, the gas flow meter is arranged at the drying tank outlet, and the air bag is arranged at the gas flow meter outlet.

8. A shale oil in-situ thermal cracking reaction experimental device according to any one of claims 1 to 7, It is characterized in that The continuous gas injection and pressurization system comprises a gas injection pipe, and a gas source interface, a pressure regulating valve, and a first throttle valve which are sequentially arranged on the gas injection pipe; The gas injection pipe is inserted into the cracking reactor.

9. A method for using a shale oil in-situ thermal cracking reaction experimental device, It is characterized in that The following steps are involved: S1: Connect the experimental instruments as shown in the figure and place the prepared core into the reaction chamber of the cracking reactor; S2: Open the pressure regulating valve and the first throttle valve, and introduce the gas required for the experiment into the reaction chamber through the gas source interface; S3: Close the first throttle valve to stop gas injection, heat the reaction chamber to the specified temperature of the experiment and then keep the temperature constant so that the core reacts under the experimental temperature and pressure conditions; S4: After the specified pyrolysis reaction time of the core is completed, the oil and gas generated by the reaction are separated and collected in the sample collection system; S5: Arrange the experimental instruments, repeat the above steps by changing the experimental conditions, and make comparisons.

10. A method for using a shale oil in-situ thermal cracking reaction experimental device according to claim 9, It is characterized in that The steps of collecting and separating the oil and gas generated by the reaction are as follows: opening the second throttle valve, waiting for the cracking product to completely enter the low-temperature condensation tank, closing the second throttle valve, and after the cracking product is cooled, opening the third throttle valve to allow the cracking product to enter the gas-liquid separator, closing the third throttle valve, drying the cracked gas through a drying tank, measuring the cracked gas flow rate with a gas flow meter, collecting the cracked gas with an air bag, opening the fourth throttle valve when the gas flow meter remains stable, and recording the number of ticks on the measuring cylinder and the count of the electronic balance when the cracked liquid completely enters the measuring cylinder.

Images