An experimental device for in-situ pyrolysis and online observation of crude oil

Abstract

The present invention discloses an experimental device for in-situ pyrolysis and online observation of crude oil, comprising a base, two groups of top plates arranged side by side are arranged above the base, four groups of limiting mechanisms arranged in a square are installed between the two groups of top plates and the base, a clamping assembly is fixedly installed on the top of the base, the structure of the clamping assembly includes a support seat and a pad, the number of the support seat and the pad are both two groups, the two groups of support seats are fixedly installed on the top of the base side by side, three groups of sample bin assemblies arranged front and back are placed on the top of the two groups of pads, and the structure of the sample bin assembly includes a quartz sealing bin bottom surface, a quartz sealing bin top surface, a sample cavity groove and an injection groove. The sample bin assembly in this device is made of high-purity quartz stone, which can not only withstand the high pressure generated during the pyrolysis of crude oil, but also has the characteristics of no background fluorescence and high light transmittance. The crude oil sample can be pyrolyzed in situ and measured online in this experimental device.

Description

Technical Field

[0001] The invention relates to the technical field of crude oil observation experimental devices, in particular to an experimental device for in-situ pyrolysis and online observation of crude oil. Background Art

[0002] With the rapid development of economy, my country's dependence on foreign crude oil has been increasing, which has caused major hidden dangers to my country's energy security. my country's crude oil resources are unevenly distributed and difficult to explore. It is urgent to expand new exploration areas and formations. At present, deep oil and gas exploration (>4500m) is one of the most important exploration directions in my country. Since deep oil and gas reservoirs usually experience complex burial history, crude oil usually has different degrees of pyrolysis during the accumulation process, which not only restricts the resource potential evaluation of crude oil, but also significantly affects the exploration and development of crude oil. Effectively identifying the degree of pyrolysis of crude oil is a key scientific issue faced by deep crude oil exploration. Since crude oil generally contains polycyclic aromatic hydrocarbons (PHA), crude oil has rich spectral information, including fluorescence spectrum, fluorescence lifetime and infrared spectrum. During the pyrolysis of crude oil, its polycyclic aromatic hydrocarbon components will undergo complex organic chemical reactions, resulting in the evolution of crude oil spectral parameters. The degree of pyrolysis of crude oil can be effectively characterized by measuring the spectral parameters of different pyrolysis oils.

[0003] However, it is difficult to measure the spectroscopic parameters of crude oil online during pyrolysis. There are three main reasons: First, the pyrolysis process of crude oil needs to be heated in a vacuum and oxygen-free environment, and pyrolysis occurs in a high-temperature and high-pressure environment; second, during the spectral test of crude oil, the spectral signal must be transmitted in a material with no background fluorescence and high light transmittance; third, it is necessary to measure the spectral parameters of pyrolysis oil with different pyrolysis degrees under different temperature conditions. Therefore, it is necessary to develop an experimental device that can realize in-situ pyrolysis of crude oil and online observation.

[0004] When pyrolyzing crude oil samples in the prior art, the crude oil samples are usually sealed in glass tubes or gold tubes, and then placed in a muffle furnace for pyrolysis experiments. After reaching the set temperature, the pyrolysis oil in the glass tube or gold tube is taken out, and then processed into optical slice samples for testing in different spectroscopic instruments. During the test process, this method will release the gaseous hydrocarbons and other fluids associated with the pyrolysis oil, change the pressure conditions of the pyrolysis oil, and significantly affect the spectroscopic parameters of the pyrolysis oil; in addition, the crude oil in the oil reservoir is usually in a high-temperature geological environment, and with the evolution of the strata, the temperature is constantly changing. This method is also difficult to achieve spectroscopic testing of pyrolysis oil under different temperature conditions, so it is difficult to apply to actual geological conditions.

[0005] The information disclosed in this background technology section is only intended to deepen the understanding of the overall background technology of the present invention, and should not be regarded as acknowledging or suggesting in any form that the information constitutes the prior art known to those skilled in the art. Summary of the invention

[0006] The purpose of the present invention is to provide an experimental device for in-situ pyrolysis and online observation of crude oil to solve the problems raised in the above background technology.

[0007] To achieve the above-mentioned purpose, the present invention provides the following technical solutions: an experimental device for in-situ pyrolysis and online observation of crude oil, comprising a base, two groups of top plates arranged side by side are arranged above the base, four groups of limiting mechanisms arranged in a square are installed between the two groups of top plates and the base, a clamping assembly is fixedly installed on the top of the base, the structure of the clamping assembly includes a support seat and a pad, the number of the support seat and the pad are both two groups, the two groups of support seats are fixedly installed on the top of the base side by side, the two groups of pads are respectively fixedly installed on the opposite sides of the two groups of support seats, three groups of sample bin assemblies arranged front and back are placed on the top of the two groups of pads, the structure of the sample bin assembly includes a quartz sealing bin bottom surface, a quartz sealing bin top surface, a sample cavity groove and an injection groove, the quartz sealing bin top surface is fixedly installed on the top of the quartz sealing bin bottom surface, the sample cavity groove and the injection groove are both opened on the upper surface of the quartz sealing bin bottom surface, and the injection groove and the sample cavity groove are connected to each other, and a program temperature control mechanism is fixedly installed between the two groups of top plates.

[0008] Preferably, the structure of the snap-on assembly also includes a positioning bar, a limiting bar and a spring, and the number of the springs is multiple groups. The positioning bar is fixedly installed on the top of one group of pads, and the limiting bar is placed on the top of another group of pads. The multiple groups of springs are fixedly connected to the side of the limiting bar away from the positioning bar, and one end of the spring is in contact with the outer surface of one group of support seats.

[0009] Preferably, a controller is fixedly installed on the top of the base, and the controller is electrically connected to the program temperature control mechanism, a puncture needle is fixedly inserted into the back side of the bottom surface of the quartz sealing chamber, and the front end of the puncture needle extends into the space inside the sample cavity groove, and a micro-one-way valve is fixedly connected to the back side of the puncture needle by gluing, and a pressure sensor is inserted into one end of the micro-one-way valve.

[0010] Preferably, the puncture needle is a disposable item, and the pressure sensor is electrically connected to the controller.

[0011] Preferably, two groups of hydraulic cylinders arranged side by side are fixedly installed on the top of the base, and the two groups of hydraulic cylinders are respectively located on opposite sides of the two groups of support seats, the hydraulic cylinders are electrically connected to the controller, the telescopic ends of the two groups of hydraulic cylinders are fixedly connected with threaded columns, the outer surfaces of the threaded columns are connected with combined plates by threaded engagement, and the combined plates are fixedly engaged with the upper surface of the top plate by screws.

[0012] Preferably, the structure of the program temperature control mechanism includes a bending plate, a heating resistance wire, a quartz light-transmitting plate and a thermocouple. The number of the bending plates is two groups, and the two groups of the bending plates are respectively fixedly installed on the opposite sides of the two groups of top plates. The number of the heating resistance wires is multiple groups, and the multiple groups of the heating resistance wires are respectively and evenly embedded in the interior of the two groups of bending plates. The quartz light-transmitting plate is fixedly installed between the two groups of bending plates, and the quartz light-transmitting plate is located above one of the sample chamber assemblies. The thermocouple is installed on the outer surfaces of the two groups of bending plates.

[0013] Preferably, the structure of the limiting mechanism includes a supporting pad, an upright round rod, a square plate and a sliding cylinder, the supporting pad is fixedly installed at the sharp corner of the bottom of the base, the square plate is fixedly installed on the top of the top plate, the upright round rod is fixedly installed on the top of the supporting pad, and the top of the upright round rod is movable through the interior of the square plate, the sliding cylinder is fixedly installed on the bottom of the square plate, and the sliding cylinder is slidably connected to the outer surface of the upright round rod.

[0014] Preferably, the working steps of the experimental device are as follows:

[0015] S1. Insert the needle tip of the syringe loaded with the crude oil sample into the injection tank, squeeze the syringe, and transport the crude oil sample in the space along the injection tank to the space inside the sample cavity tank to complete the injection operation of the crude oil sample;

[0016] S2. Then, a vacuum pump is used to extract the air in the sample chamber assembly. During the vacuuming process, the open end of the injection slot is welded shut to prevent the crude oil sample in the sample chamber assembly from being oxidized by oxygen in the chamber during the pyrolysis process.

[0017] S3, then applying a squeezing force to the limit bar away from the side where the positioning bar is located, causing the multiple groups of springs to contract inward, thereby expanding the distance between the limit bar and the positioning bar, and then placing the multiple groups of sample chamber components on the top of the two groups of pads in turn, and releasing the external force applied to the limit bar;

[0018] S4, by operating two groups of hydraulic cylinders to cause them to retract downward to a set length, the combined plate drives the two groups of top plates to move downward, and then causes the bottom of the program temperature control mechanism to fit the upper surface of the sample chamber assembly, and then directly places the device under a microscope of an optical instrument to perform online measurement of the spectral parameters of the original crude oil sample;

[0019] S5. After the online determination of the spectral parameters of the crude oil sample in step S4 is completed, the hydraulic cylinder is urged to continue to contract downward, driving the bottom of the program temperature control mechanism to pressurize the upper surface of the sample bin assembly, and the pressure sensor is directly subjected to the pressure from above, and the piezoelectric signal is converted into a resistance signal, and fed back to the controller. When the pressure value reaches 50MPa, the pressure is stopped, and the program temperature control mechanism is started, and the heating resistance wire inside the mechanism converts the electrical energy into thermal energy, and transmits it to the sample bin assembly below, and the crude oil therein is subjected to program heating treatment. After reaching the set temperature point, the spectral parameters of the pyrolysis oil at different pyrolysis stages are determined online;

[0020] S6. After the crude oil is subjected to in-situ pyrolysis and online spectroscopy measurement, the quartz sealed chamber is taken out, and the pyrolysis oil at different evolutionary stages is obtained through Soxhlet extraction with organic reagents, and relevant organic geochemical analysis is carried out.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] The present invention places sample bin assemblies of multiple groups of crude oil samples in a snap-on assembly in sequence, and then causes the bottom of a program temperature control mechanism to fit onto the upper surface of the sample bin assembly. The device is then directly placed under a microscope to perform online measurement of spectral parameters of the crude oil samples. In conjunction with the start-up operation of the program temperature control mechanism, the crude oil samples can be conveniently pyrolyzed in situ. After crude oil is injected into the sample bin assembly, the quartz sealed bin can withstand the high pressure during the pyrolysis of crude oil, effectively preventing leakage of pyrolysis oil and its associated gaseous hydrocarbons.

[0023] In the present invention, the high-purity quartz has the characteristics of no background fluorescence and high light transmittance, and can effectively measure the spectral parameters of the pyrolysis oil therein.

[0024] In the present invention, when detecting the internal pressure of the sample chamber assembly, the pressure sensor is electrically connected to the micro-one-way valve and the micro-one-way valve is opened, so that the pressure sensor directly senses the pressure value inside the sample chamber assembly and displays it on its display screen. After the internal pressure measurement of the previous group of sample chamber assemblies is completed, the pressure sensor can be removed and integrated into the micro-one-way valve in the next group of sample chamber assemblies, so that the pressure sensor can be reused. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0026] Figure 2 It is a structural schematic diagram of the clamping assembly of the present invention;

[0027] Figure 3 It is a structural schematic diagram of the limiting mechanism of the present invention;

[0028] Figure 4 It is a schematic diagram of the structure of the limit strip and the spring of the present invention;

[0029] Figure 5 It is a structural schematic diagram of the sample chamber assembly of the present invention;

[0030] Figure 6 It is a structural schematic diagram of the program temperature control mechanism of the present invention;

[0031] Figure 7 It is a schematic structural diagram of the hydraulic cylinder and the threaded column of the present invention.

[0032] In the figure: 1. base; 2. top plate; 3. limit mechanism; 4. snap-on assembly; 5. support seat; 6. pad; 7. sample chamber assembly; 8. bottom surface of quartz sealing chamber; 9. top surface of quartz sealing chamber; 10. sample cavity slot; 11. injection slot; 12. programmed temperature control mechanism; 13. positioning strip; 14. limit strip; 15. spring; 16. puncture needle; 17. micro one-way valve; 18. pressure sensor; 19. hydraulic cylinder; 20. threaded column; 21. combination plate; 22. bending plate; 23. heating resistor wire; 24. quartz transparent plate; 25. thermocouple; 26. support pad; 27. upright round rod; 28. square plate; 29. ​​slide cylinder. DETAILED DESCRIPTION

[0033] 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.

[0034] In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "front end", "rear end", "two ends", "one end", "the other end" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first" and "second" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance.

[0035] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "provided with", "connected", etc. should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0036] See also Figure 1-Figure 7 , an embodiment provided by the present invention:

[0037] An experimental device for in-situ pyrolysis and online observation of crude oil, comprising a base 1, two groups of top plates 2 arranged side by side are arranged above the base 1, four groups of limiting mechanisms 3 arranged in a square are installed between the two groups of top plates 2 and the base 1, a clamping assembly 4 is fixedly installed on the top of the base 1, the structure of the clamping assembly 4 includes a support seat 5 and a pad 6, the number of the support seat 5 and the pad 6 are both two groups, the two groups of support seats 5 are fixedly installed on the top of the base 1 side by side, and the two groups of pads 6 are respectively fixedly installed on the two groups of support seats 5 opposite to each other. On one side, three groups of sample chamber assemblies 7 arranged front and back are placed on the top of the two groups of pads 6. The structure of the sample chamber assembly 7 includes a quartz sealed chamber bottom surface 8, a quartz sealed chamber top surface 9, a sample cavity groove 10 and an injection groove 11. The quartz sealed chamber top surface 9 is fixedly installed on the top of the quartz sealed chamber bottom surface 8. The sample cavity groove 10 and the injection groove 11 are both opened on the upper surface of the quartz sealed chamber bottom surface 8, and the injection groove 11 is connected to the sample cavity groove 10. A program temperature control mechanism 12 is fixedly installed between the two groups of top plates 2.

[0038] In this experimental device, the quartz sealed chamber can effectively replace the crude oil pyrolysis in the glass tube / gold tube. The quartz sealed chamber is made of high-purity quartz, which can not only withstand the high pressure generated during the crude oil pyrolysis process, but also has the characteristics of no background fluorescence and high transmittance. The crude oil sample can be pyrolyzed in situ and measured online in this experimental device.

[0039] Specifically, when using the experimental device, the needle tip of the syringe loaded with the crude oil sample is inserted into the injection groove 11, and the syringe is squeezed to transport the crude oil sample in the space along the injection groove 11 to the space inside the sample cavity groove 10 to complete the injection operation of the crude oil sample. Then, multiple groups of sample bin assemblies 7 injected with crude oil samples are placed in the clamping assembly 4 in sequence, and then the bottom of the program temperature control mechanism 12 is made to fit the upper surface of the sample bin assembly 7. Then, the device is directly placed under a microscope to perform online measurement of the fluorescence spectrum, fluorescence lifetime and infrared spectrum of the crude oil sample. In conjunction with the start-up operation of the program temperature control mechanism 12, the crude oil sample can be conveniently subjected to in-situ pyrolysis operation.

[0040] More specifically, by placing three groups of sample chamber assemblies 7 in the snap-fit ​​assembly 4, the overall efficiency can be effectively improved during subsequent measurements, and the data can be made comparable. The total length of the program temperature control mechanism 12 in the device is consistent with the total front-to-back length of the snap-fit ​​assembly 4, and the same heat can be applied to the three groups of sample chamber assemblies 7 engaged in the snap-fit ​​assembly 4, so that the three groups of sample chamber assemblies 7 are heated more evenly.

[0041] The structure of the clamping assembly 4 also includes a positioning bar 13, a limiting bar 14 and a spring 15. The number of springs 15 is multiple groups. The positioning bar 13 is fixedly installed on the top of one group of pads 6, and the limiting bar 14 is placed on the top of another group of pads 6. The multiple groups of springs 15 are all fixedly connected to the side of the limiting bar 14 away from the positioning bar 13, and one end of the spring 15 is in contact with the outer surface of one group of support seats 5.

[0042] By applying an extrusion force to the limit strip 14 away from the side where the positioning strip 13 is located, the multiple groups of springs 15 are forced to contract inward, thereby expanding the distance between the limit strip 14 and the positioning strip 13, and then placing the multiple groups of sample bin assemblies 7 on top of the two groups of pads 6 in turn, and releasing the external force applied to the limit strip 14. At this time, the position of the sample bin assembly 7 is limited by the positioning strip 13 and the limit strip 14, which can effectively avoid a large positional offset when the sample bin assembly 7 is subsequently pressurized and heated, affecting the pressurization and heating effects. The sample bin assembly 7 is in a state of active fit with the limit strip 14 and the positioning strip 13. Therefore, after a group of crude oil samples under the program temperature control mechanism 12 are measured online, a group of sample bin assemblies 7 at the rear can be pushed forward to facilitate continuous testing as a whole.

[0043] A controller is fixedly installed on the top of the base 1, and the controller is electrically connected to the program temperature control mechanism 12. A puncture needle 16 is fixedly inserted on the back of the bottom surface 8 of the quartz sealing chamber, and the front end of the puncture needle 16 extends into the space inside the sample cavity 10. A micro-one-way valve 17 is fixedly connected to the back of the puncture needle 16 by gluing, and a pressure sensor 18 is inserted at one end of the micro-one-way valve 17. The puncture needle 16 is a disposable item, and the pressure sensor 18 is electrically connected to the controller.

[0044] When the bottom surface 8 of the quartz sealed chamber is produced, the puncture needle 16 is embedded therein, and its ventilation tip is located inside the space of the sample cavity groove 10, so that the two form a set of integral parts. After that, after the top surface 9 of the quartz sealed chamber is welded to the bottom surface 8 of the quartz sealed chamber, the tip of the puncture needle 16 is not sealed, and then the tail end of the puncture needle 16 is connected to a micro-one-way valve 17. By controlling the closing and opening of the micro-one-way valve 17, the puncture needle 16 is adjusted between the unblocked and blocked states. When the micro-one-way valve 17 is closed, the air inside the bottom surface 8 of the quartz sealed chamber cannot flow along the puncture needle 16 to the sample cavity groove 10. The pressure is discharged outside, thereby ensuring the closedness of the system. When detecting the internal pressure of the sample chamber assembly 7, the pressure sensor 18 is electrically connected to the micro-one-way valve 17 and the micro-one-way valve 17 is opened, so that the pressure sensor 18 directly senses the pressure value inside the sample chamber assembly 7 and displays it on its display screen. After the internal pressure measurement of the previous group of sample chamber assemblies 7 is completed, the pressure sensor 18 can be removed and integrated into the micro-one-way valve 17 in the next group of sample chamber assemblies 7, so that the pressure sensor 18 can be reused. The operating principle can refer to the direct measurement method of human intra-abdominal pressure.

[0045] The structure of the program temperature control mechanism 12 includes a bending plate 22, a heating resistance wire 23, a quartz light-transmitting plate 24 and a thermocouple 25. The number of the bending plates 22 is two groups, and the two groups of bending plates 22 are respectively fixedly installed on the opposite sides of the two groups of top plates 2. The number of the heating resistance wires 23 is multiple groups, and the multiple groups of heating resistance wires 23 are respectively and evenly embedded in the inside of the two groups of bending plates 22. The quartz light-transmitting plate 24 is fixedly installed between the two groups of bending plates 22, and the quartz light-transmitting plate 24 is located above one of the groups of sample chamber assemblies 7. The thermocouple 25 is installed on the outer surface of the two groups of bending plates 22.

[0046] The two groups of bending plates 22 provide a more suitable assembly space for the heating resistor wire 23 and the quartz transparent plate 24, and the heating resistor wire 23 is operated by the controller to convert electrical energy into thermal energy and transfer it to the sample chamber assembly 7 below, so as to heat the crude oil therein, so as to facilitate the subsequent online measurement of the spectral parameters of the pyrolysis oil, and the thermocouple 25 can measure the temperature of the outer surface of the bending plate 22 in real time.

[0047] The structure of the limiting mechanism 3 includes a supporting pad 26, an upright round rod 27, a square plate 28 and a slide cylinder 29. The supporting pad 26 is fixedly installed at the sharp corner of the bottom of the base 1, the square plate 28 is fixedly installed on the top of the top plate 2, the upright round rod 27 is fixedly installed on the top of the supporting pad 26, and the top of the upright round rod 27 is movable through the interior of the square plate 28, the slide cylinder 29 is fixedly installed at the bottom of the square plate 28, and the slide cylinder 29 is slidably connected to the outer surface of the upright round rod 27.

[0048] When the hydraulic cylinder 19 is extended and retracted up and down, it can drive the four sets of slide cylinders 29 to move up and down along the outer surface of the upright round rod 27.

[0049] The working steps of the experimental device are as follows:

[0050] S1, inserting the needle tip of the syringe loaded with the crude oil sample into the injection groove 11, and squeezing the syringe, so that the crude oil sample in the space inside the syringe is transported along the injection groove 11 to the space inside the sample cavity groove 10, so as to complete the injection operation of the crude oil sample;

[0051] S2, then use a vacuum pump to extract the air in the sample chamber assembly 7, and weld the open end of the injection slot 11 during the vacuuming process to prevent the crude oil sample inside the sample chamber assembly 7 from being oxidized by the oxygen in the chamber during the pyrolysis process;

[0052] S3, then apply a squeezing force to the limiting strip 14 away from the side where the positioning strip 13 is located, so as to cause the multiple groups of springs 15 to contract inward, thereby expanding the distance between the limiting strip 14 and the positioning strip 13, and then sequentially place the multiple groups of sample chamber assemblies 7 on the two groups of pads 6, and release the external force applied to the limiting strip 14;

[0053] S4, by operating the two groups of hydraulic cylinders 19, causing them to shrink downward to a set length, so that the combined plate 21 drives the two groups of top plates 2 to move downward, and then the bottom of the program temperature control mechanism 12 is made to fit the upper surface of the sample chamber assembly 7, and then the device is directly placed under the microscope of the optical instrument to perform online measurement of the spectral parameters of the original crude oil sample;

[0054] S5. After the online determination of the spectral parameters of the crude oil sample in step S4 is completed, the hydraulic cylinder 19 is urged to continue to contract downward, driving the bottom of the program temperature control mechanism 12 to pressurize the upper surface of the sample chamber assembly 7, and the pressure sensor 18 is directly subjected to the pressure from above, which converts the piezoelectric signal into a resistance signal and feeds it back to the controller. When the pressure value reaches 50MPa, the pressure is stopped, and the program temperature control mechanism 12 is started, and the heating resistor 23 inside it converts the electrical energy into thermal energy and transmits it to the sample chamber assembly 7 below, so as to perform program heating treatment on the crude oil therein. After reaching the set temperature point, the spectral parameters of the pyrolysis oil at different pyrolysis stages are determined online;

[0055] S6. After the crude oil is subjected to in-situ pyrolysis and online spectroscopy measurement, the quartz sealed chamber is taken out, and the pyrolysis oil at different evolutionary stages is obtained through Soxhlet extraction with organic reagents, and relevant organic geochemical analysis is carried out.

[0056] Working principle: by inserting the needle tip of the syringe loaded with crude oil sample into the injection groove 11 and squeezing the syringe, the crude oil sample in its space is transported along the injection groove 11 to the space inside the sample cavity groove 10 to complete the injection operation of the crude oil sample, and then a vacuum pump is used to extract the air in the sample chamber assembly 7, and then multiple groups of sample chamber assemblies 7 are placed on two groups of pads 6, and the two groups of top plates 2 and the program temperature control mechanism 12 are driven downward by the hydraulic cylinder 19 to make the quartz light-transmitting plate 24 in the program temperature control mechanism 12 fit with the top of the sample chamber assembly 7, and then the device is directly placed under a microscope to perform online measurement of the fluorescence spectrum, fluorescence lifetime and infrared spectrum of the crude oil sample. The hydraulic cylinder 19 continuously contracts downward to drive the program temperature control mechanism 12 to squeeze the sample chamber assembly 7 downward, and at the same time cooperate with the program temperature control mechanism 12 to facilitate the in-situ pyrolysis operation of crude oil.

[0057] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.

Claims

1. An experimental device for in-situ pyrolysis and online observation of crude oil, comprising a base (1), characterized in that: Two groups of top plates (2) arranged side by side are provided above the base (1); four groups of limiting mechanisms (3) arranged in a square shape are installed between the two groups of top plates (2) and the base (1); a clamping assembly (4) is fixedly installed on the top of the base (1); the structure of the clamping assembly (4) includes a support seat (5) and a pad (6); the number of the support seat (5) and the pad (6) are both two groups; the two groups of the support seats (5) are fixedly installed side by side on the top of the base (1); the two groups of the pad (6) are fixedly installed on opposite sides of the two groups of the support seats (5); and the two groups of the pad Three groups of sample chamber assemblies (7) arranged in a front-to-rear manner are placed on the top of the quartz sealed chamber (6), the sample chamber assembly (7) comprising a quartz sealed chamber bottom surface (8), a quartz sealed chamber top surface (9), a sample chamber groove (10) and an injection groove (11), the quartz sealed chamber top surface (9) being fixedly mounted on the top of the quartz sealed chamber bottom surface (8), the sample chamber groove (10) and the injection groove (11) being both arranged on the upper surface of the quartz sealed chamber bottom surface (8), and the injection groove (11) and the sample chamber groove (10) being interconnected, and a programmable temperature control mechanism (12) being fixedly mounted between the two groups of top plates (2); The structure of the clamping assembly (4) further includes a positioning bar (13), a limiting bar (14) and a spring (15), wherein the spring (15) is provided in a plurality of groups, wherein the positioning bar (13) is fixedly mounted on the top of one group of pads (6), and the limiting bar (14) is placed on the top of another group of pads (6), and the plurality of groups of springs (15) are fixedly connected to a side of the limiting bar (14) away from the positioning bar (13), and one end of the spring (15) is in contact with the outer surface of one group of support seats (5); A controller is fixedly mounted on the top of the base (1), and the controller is electrically connected to the program temperature control mechanism (12); a puncture needle (16) is fixedly plugged into the back of the bottom surface (8) of the quartz sealing chamber, and the front end of the puncture needle (16) extends into the space inside the sample cavity (10); a micro one-way valve (17) is fixedly connected to the back of the puncture needle (16) by gluing, and a pressure sensor (18) is plugged into one end of the micro one-way valve (17); Two groups of hydraulic cylinders (19) arranged side by side are fixedly mounted on the top of the base (1), and the two groups of hydraulic cylinders (19) are respectively located on opposite sides of the two groups of support seats (5), the hydraulic cylinders (19) are electrically connected to the controller, and the telescopic ends of the two groups of hydraulic cylinders (19) are fixedly connected to threaded columns (20), and the outer surfaces of the threaded columns (20) are connected to the combination plates (21) by threaded engagement, and the combination plates (21) are fixedly engaged with the upper surface of the top plate (2) by screws; The structure of the program temperature control mechanism (12) includes a bending plate (22), a heating resistance wire (23), a quartz light-transmitting plate (24) and a thermocouple (25). The number of the bending plates (22) is two groups, and the two groups of the bending plates (22) are respectively fixedly mounted on opposite sides of the two groups of top plates (2). The number of the heating resistance wires (23) is multiple groups, and the multiple groups of the heating resistance wires (23) are respectively and evenly embedded in the inside of the two groups of bending plates (22). The quartz light-transmitting plate (24) is fixedly mounted between the two groups of bending plates (22), and the quartz light-transmitting plate (24) is located above one group of sample chamber components (7). The thermocouple (25) is mounted on the outer surfaces of the two groups of bending plates (22).

2. The experimental device for in-situ pyrolysis and online observation of crude oil according to claim 1, characterized in that: The puncture needle (16) is a disposable item, and the pressure sensor (18) is electrically connected to the controller.

3. The experimental device for in-situ pyrolysis and online observation of crude oil according to claim 1, characterized in that: The limit mechanism (3) comprises a support pad (26), an upright round rod (27), a square plate (28) and a slide cylinder (29); the support pad (26) is fixedly mounted at the sharp corner of the bottom of the base (1); the square plate (28) is fixedly mounted on the top of the top plate (2); the upright round rod (27) is fixedly mounted on the top of the support pad (26); the top of the upright round rod (27) movably passes through the interior of the square plate (28); the slide cylinder (29) is fixedly mounted on the bottom of the square plate (28); and the slide cylinder (29) is slidably connected to the outer surface of the upright round rod (27).

4. An experimental device for in-situ pyrolysis and online observation of crude oil according to any one of claims 1 to 3, characterized in that: The working steps of the experimental device are as follows: S1, inserting the needle tip of a syringe loaded with a crude oil sample into the interior of the injection groove (11), and squeezing the syringe, so that the crude oil sample in the space inside the syringe is transported along the injection groove (11) to the space inside the sample cavity groove (10), thereby completing the injection operation of the crude oil sample; S2, then using a vacuum pump to extract the air in the sample chamber assembly (7), and in the process of vacuuming, welding the open end of the injection groove (11) to prevent the crude oil sample in the sample chamber assembly (7) from being oxidized by oxygen in the chamber during the pyrolysis process; S3, then applying a squeezing force to the limiting strip (14) away from the side where the positioning strip (13) is located, causing the multiple groups of springs (15) to contract inward, thereby expanding the distance between the limiting strip (14) and the positioning strip (13), and then placing the multiple groups of sample chamber components (7) on top of the two groups of pads (6) in turn, and releasing the external force applied to the limiting strip (14); S4, operating the two groups of hydraulic cylinders (19) to cause them to retract downward to a set length, so that the combined plate (21) drives the two groups of top plates (2) to move downward, and then causes the bottom of the programmable temperature control mechanism (12) to fit the upper surface of the sample chamber assembly (7), and then directly placing the device under a microscope of an optical instrument to perform online measurement of the spectral parameters of the original crude oil sample; S5. After the online determination of the spectral parameters of the crude oil sample in step S4 is completed, the hydraulic cylinder (19) is urged to continue to contract downward, driving the bottom of the program temperature control mechanism (12) to pressurize the upper surface of the sample chamber assembly (7), and the pressure sensor (18) is directly subjected to the pressure from above, converting the piezoelectric signal into a resistance signal and feeding it back to the controller. When the pressure value reaches 50 MPa, the pressure is stopped, and the program temperature control mechanism (12) is started, and the heating resistor (23) inside the mechanism converts the electrical energy into heat energy and transmits it to the sample chamber assembly (7) below, so as to perform a program heating treatment on the crude oil therein. After reaching the set temperature point, the spectral parameters of the pyrolysis oil at different pyrolysis stages are determined online; S6. After the crude oil is subjected to in-situ pyrolysis and online spectroscopy measurement, the quartz sealed chamber is taken out, and the pyrolysis oil at different evolutionary stages is obtained through Soxhlet extraction with organic reagents, and relevant organic geochemical analysis is carried out.

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