High-pressure reaction device and Raman analysis device

Abstract

The utility model discloses a high-pressure reaction device and a Raman analysis device. The high-pressure reaction device comprises a reaction kettle, a first sapphire glass window, a temperature control system and a pressure sensor, the reaction kettle comprises a kettle cover and a kettle body, a reaction cavity is formed in the reaction kettle and used for generating hydrates, the kettle cover and the kettle body are detachably connected to open and close the reaction cavity, and the kettle body is rotatably arranged; the first sapphire glass window is arranged on the side wall of the kettle body, and the Raman laser can penetrate through the first sapphire glass window by rotating the kettle body so as to irradiate the hydrate in the reaction cavity; the temperature control system is connected with the reaction kettle so as to control the temperature in the reaction cavity; and the pressure sensor is connected with the reaction kettle so as to measure the pressure in the reaction cavity. The Raman analysis device comprises the high-pressure reaction device. According to the high-pressure reaction device, the distribution characteristic change of hydrates in the longitudinal direction can be observed, the operation is convenient, and the experiment accuracy can be improved. The method is applied to the technical field of Raman analysis.

Description

Technical Field

[0001] This application relates to the field of Raman analysis technology, and particularly relates to a high-pressure reaction device and a Raman analysis device. Background Art

[0002] In the related art, when characterizing hydrates by Raman spectroscopy, generally a reaction kettle is used to generate hydrates. In order to conduct experiments well to obtain accurate experimental data, the use of the reaction kettle (such as operations like opening the kettle and cleaning the reaction kettle) requires researchers with certain operating experience to operate manually, which is time-consuming and laborious, resulting in low experimental efficiency.

[0003] In addition, the observation window of the high-pressure reaction kettle for in-situ observation of laser Raman spectroscopy in the related art is generally set at the top of the reaction kettle, and the high-pressure reaction kettle is generally fixedly arranged. This structure is limited by the working distance of the objective lens of the laser Raman spectrometer and the wall thickness of the device between the objective lens and the sample, making it impossible to collect Raman laser at a position close to the bottom of the reaction kettle. Moreover, the main method for studying hydrates longitudinally in the high-pressure reaction kettle for in-situ observation of laser Raman spectroscopy in the related art is: directly placing the reaction kettle beside the laser confocal Raman spectrometer, reflecting the laser through a light guide mirror, and irradiating it on the viewing window of the reaction kettle to conduct in-situ microscopic structure characterization of hydrates. Among them, the viewing window is generally made of resin glass or quartz glass. The resin structure affects the focusing of the laser on the hydrates, and its Raman signal will mask the structural signal of the hydrates; the quartz glass is too thick and has limited pressure resistance, greatly filtering out the laser intensity and weakening the Raman spectral signal of the hydrates. And the laser is led out from the Raman spectrometer through a light guide mirror, the optical path is lengthened, the laser intensity is weakened, and the laser can only move up and down to find the aggregation point, cannot move left and right to find the aggregation point, and cannot conduct microscopic monitoring on all hydrates inside the reaction kettle. Summary of the Utility Model

[0004] This application aims to solve at least one of the above technical problems in the prior art to a certain extent. For this purpose, this application provides a high-pressure reaction device, which can observe the change of the distribution characteristics of hydrates longitudinally, is convenient to operate, and can improve the accuracy of experiments.

[0005] The high-pressure reaction device provided by the present application includes: a reaction kettle, the reaction kettle includes a kettle cover and a kettle body, a reaction chamber is formed in the reaction kettle, the reaction chamber is used for generating hydrates, the kettle cover and the kettle body are detachably connected to open and close the reaction chamber, and the kettle body is rotatably arranged; a first sapphire glass window, the first sapphire glass window is arranged on the side wall of the kettle body, and the first sapphire glass window is used for allowing Raman laser to pass through and irradiate on the hydrates in the reaction chamber after the kettle body rotates by a preset angle; a temperature control system, the temperature control system is connected to the reaction kettle to control the temperature in the reaction chamber; a pressure sensor, the pressure sensor is connected to the reaction kettle to measure the pressure in the reaction chamber.

[0006] Based on the above technical solution, the high-pressure reaction device provided by the present application has at least the following beneficial effects: In the high-pressure reaction device in the embodiment of the present application, by rotating the kettle body, Raman laser can pass through the first sapphire glass window and irradiate on the hydrates in the reaction chamber, so that the change in the distribution characteristics of hydrates in the longitudinal direction (i.e., along the length direction of the reaction kettle) can be observed. There is no need for a light guide mirror to reflect Raman laser, the operation is convenient, and the experimental accuracy can be improved; the first sapphire glass window has good light transmittance, so that the hydrates in the reaction chamber can receive Raman laser well, ensuring the intensity of the Raman spectrum signal of the hydrates; by setting the temperature control system and the pressure sensor, the temperature and pressure in the reaction chamber can be accurately controlled, which is beneficial to the progress of the experiment.

[0007] According to some embodiments of the present application, the high-pressure reaction device further includes a first driving member, the first driving member is connected to the kettle body to drive the kettle body to rotate.

[0008] According to some embodiments of the present application, the high-pressure reaction device further includes a flushing member and a drying member, the flushing member is used for flushing the reaction kettle, the drying member is used for drying the reaction kettle, and the flushing member and the drying member are both movably arranged on one side of the reaction kettle.

[0009] According to some embodiments of the present application, the high-pressure reaction device further includes a second sapphire glass window, the second sapphire glass window is arranged on the top of the kettle cover.

[0010] According to some embodiments of the present application, the high-pressure reaction device further includes an opening kettle member, the opening kettle member is connected to the kettle cover, and the opening kettle member is used for separating or connecting the kettle cover and the kettle body, so as to open and close the reaction chamber.

[0011] According to some embodiments of the present application, the kettle lid is threadedly connected to the kettle body. The kettle-opening member includes a clamping member and a second driving member. The clamping member is used to clamp the kettle lid. The clamping member is movable in the vertical direction. The second driving member is connected to the clamping member to drive the clamping member to rotate, so as to separate or connect the kettle lid from the kettle body.

[0012] According to some embodiments of the present application, the high-pressure reaction device further includes a vacuum pump, a gas source, and a liquid source. The vacuum pump is communicated with the reaction chamber to evacuate the reaction chamber. The gas source is communicated with the reaction chamber to inject reaction gas into the reaction chamber. The liquid source is communicated with the reaction chamber to inject reaction liquid into the reaction chamber.

[0013] According to some embodiments of the present application, the reaction chamber is communicated with the vacuum pump through a first pipeline. A first connection point is provided on the first pipeline. The first connection point is communicated with the gas source through a second pipeline. A second connection point is provided between the first connection point and the vacuum pump on the first pipeline. The second connection point is communicated with the liquid source through a third pipeline. A first valve is provided between the reaction kettle and the first connection point on the first pipeline. A second valve is provided on the second pipeline. A third valve is provided on the third pipeline. A fourth valve is provided between the second connection point and the vacuum pump on the first pipeline. An electronic flowmeter is provided between the third valve and the second connection point on the third pipeline to measure the volume of the reaction liquid injected into the reaction chamber. A plunger pump is provided between the third valve and the liquid source on the third pipeline.

[0014] According to some embodiments of the present application, the high-pressure reaction device further includes a movable platform. The reaction kettle is placed on the movable platform. The movable platform is used to move the reaction kettle.

[0015] The Raman analysis device provided by the present application includes the above-mentioned high-pressure reaction device.

[0016] Additional aspects and advantages of the present application will be given in part in the following description, become apparent in part from the following description, or be learned through the practice of the present application. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0018] Figure 1It is a schematic structural diagram of the high-pressure reaction device in the embodiment of the present application;

[0019] Figure 2 It is a schematic structural diagram of the reaction kettle when the kettle cover is connected to the kettle body in the embodiment of the present application;

[0020] Figure 3 It is a schematic structural diagram of the first driving member and the connecting member in the embodiment of the present application;

[0021] Figure 4 It is a schematic structural diagram of the reaction kettle when the kettle cover is separated from the kettle body in the embodiment of the present application;

[0022] Figure 5 It is a schematic connection diagram of the first pipeline, the second pipeline and the third pipeline in the embodiment of the present application.

[0023] Reference numerals:

[0024] Reaction kettle 100, kettle body 110, reaction chamber 111, first sapphire glass window 112, kettle cover 120, second sapphire glass window 121, force-bearing member 122, sealing member 130; temperature control system 210, pressure sensor 220; first driving member 310, connecting member 320; flushing member 410, drying member 420, first fixing bracket 430; clamping member 510, second driving member 520; vacuum pump 600; first pipeline 710, first connection point 711, second connection point 712, first valve 713, fourth valve 714, second pipeline 720, second valve 721, third pipeline 730, third valve 731, electronic flowmeter 732; movable platform 800; control unit 900. Detailed implementation manners

[0025] Next, the technical solutions in the embodiments of the present application will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present application without creative efforts shall fall within the protection scope of the present application.

[0026] In the present application, the orientation or positional relationship indicated by terms such as "upper", "lower", "left", "right", "front", "rear", "top", "bottom", "inner", "outer", "middle", "vertical", "horizontal", "lateral", "longitudinal", etc. is the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. These terms are mainly used to better describe the present application and its embodiments, and are not used to limit that the indicated device, element or component must have a specific orientation, or be constructed and operated in a specific orientation.

[0027] Moreover, in addition to being used to represent orientation or positional relationships, some of the above terms may also be used to represent other meanings. For example, the term "upper" may also be used to represent a certain attachment relationship or connection relationship in some cases. For those of ordinary skill in the art, the specific meanings of these terms in this application can be understood according to specific circumstances.

[0028] In addition, the terms "install", "set", "provided with", "connect", "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral structure; it can be a mechanical connection or an electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, or there can be internal communication between two devices, components or parts. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0029] In addition, the terms "first", "second", etc. are mainly used to distinguish different devices, components or parts (the specific types and structures may be the same or different), and are not used to indicate or imply the relative importance and quantity of the indicated devices, components or parts. Unless otherwise specified, the meaning of "a plurality" is two or more.

[0030] The technical solution of this application will be further described below in conjunction with embodiments and drawings.

[0031] See Figure 1 , an embodiment of this application provides a high-pressure reaction device, which can observe the change of the distribution characteristics of hydrates in the longitudinal direction, is convenient to operate, and can improve the accuracy of experiments.

[0032] See Figure 1 and Figure 2 , the high-pressure reaction device includes a reaction kettle 100, a first sapphire glass window 112, a temperature control system 210 and a pressure sensor 220. The reaction kettle 100 includes a kettle lid 120 and a kettle body 110. A reaction chamber 111 is formed in the reaction kettle 100, and the reaction chamber 111 is used to generate hydrates. The kettle lid 120 is detachably connected to the kettle body 110 to open and close the reaction chamber 111, and the kettle body 110 is rotatably arranged; the first sapphire glass window 112 is arranged on the side wall of the kettle body 110, and the first sapphire glass window 112 is used to allow Raman laser to pass through and irradiate on the hydrates in the reaction chamber 11 after the kettle body 110 rotates a preset angle; the temperature control system 210 is connected to the reaction kettle 100 to control the temperature in the reaction chamber 111; the pressure sensor 220 is connected to the reaction kettle 100 to measure the pressure in the reaction chamber 111. Optionally, the reaction kettle 100 is cylindrical.

[0033] In the high-pressure reaction device according to the embodiments of the present application, by rotating the kettle body 110, Raman laser can pass through the first sapphire glass window 112 to irradiate the hydrate in the reaction chamber 111, so that the change in the distribution characteristics of the hydrate in the longitudinal direction (i.e., along the length direction of the reaction kettle 100) can be observed. There is no need for a light guide mirror to reflect the Raman laser, which is convenient to operate and can improve the accuracy of the experiment; the first sapphire glass window 112 has good light transmittance, enabling the hydrate in the reaction chamber 111 to receive the Raman laser well and ensuring the intensity of the Raman spectrum signal of the hydrate; by setting the temperature control system 210 and the pressure sensor 220, the temperature and pressure in the reaction chamber 111 can be accurately controlled, which is beneficial to the progress of the experiment.

[0034] It can be understood that during the synthesis of the hydrate, the kettle body 110 and the kettle lid 120 are connected together. Therefore, when the kettle body 110 rotates, the kettle lid 120 also rotates together with the kettle body 110. Optionally, the kettle body 110 and the kettle lid 120 are connected by covering, jointly defining the reaction chamber 111. That is, a cavity is provided on the kettle body 110, and a cavity is also provided on the kettle lid 120. When the kettle lid 120 and the kettle body 110 are connected, the cavity of the kettle lid 120 communicates with the cavity of the kettle body 110 to jointly define the reaction chamber 111. Of course, the reaction chamber 111 can also be directly provided on the kettle body 110, and no specific limitation is made here. Optionally, by rotating the kettle body 110, the first sapphire glass window 112 can be made to face the Raman laser, that is, the first sapphire glass window 112 is perpendicular to the Raman laser, which can increase the passing amount of the Raman laser on the first sapphire glass window 112 per unit time.

[0035] Optionally, the temperature control system 210 includes a heating element, a cooling element and a temperature sensor (not shown in the drawings). The heating element is used to heat the reaction kettle 100, the cooling element is used to cool the reaction kettle 100, and the temperature sensor is used to detect the temperature in the reaction chamber 111. Both the heating element and the cooling element are electrically connected to the temperature sensor. When the temperature value detected by the temperature sensor is higher than the preset temperature, the cooling element cools to reduce the temperature in the reaction chamber 111 to the preset temperature value; when the temperature value detected by the temperature sensor is lower than the preset temperature, the heating element heats to raise the temperature in the reaction chamber 111 to the preset temperature value. Optionally, the heating element can be a constant temperature water bath, and the constant temperature water bath can be arranged on the outer periphery of the reaction kettle 100. Optionally, the cooling element can be a liquid nitrogen jacket, and the liquid nitrogen jacket can be detachably installed on the outer periphery of the reaction kettle 100.

[0036] Optionally, in some embodiments, the high-pressure reaction device further includes a second sapphire glass window 121, and the second sapphire glass window 121 is arranged on the top of the kettle lid 120. Through the second sapphire glass window 121, the change in the distribution characteristics of the hydrate in the transverse direction (i.e., along the radial direction of the reaction kettle 100) can be observed.

[0037] Optionally, in some embodiments, the high-pressure reaction device further includes a first driving member 310, and the first driving member 310 is connected to the kettle body 110 to drive the kettle body 110 to rotate. Optionally, the first driving member 310 is also a brushless motor. Optionally, referring to Figure 1 and Figure 3 , the first driving member 310 is connected to the kettle body 110 through a connecting member 320 to drive the kettle body 110 to rotate.

[0038] Optionally, in some embodiments, referring to Figure 1 , the high-pressure reaction device further includes a flushing member 410 and a drying member 420. The flushing member 410 is used to flush the reaction kettle 100, and the drying member 420 is used to dry the reaction kettle 100. The flushing member 410 and the drying member 420 are both movably arranged on one side of the reaction kettle 100. By providing the flushing member 410 and the drying member 420, the high-pressure reaction device can complete automatic cleaning and drying without manual operation, saving time and effort and improving the experimental efficiency.

[0039] When the reaction kettle 100 needs to be cleaned, the kettle lid 120 and the kettle body 110 can be separated first (refer to Figure 4 ), then the first driving member 310 is used to drive the kettle body 110 to rotate so that the opening of the kettle body 110 faces downward, and then the flushing member 410 is used to flush the inner cavities of the kettle body 110 and the kettle lid 120, and then the drying member 420 is used to dry the kettle body 110 and the kettle lid 120. After drying, the first driving member 310 can be used to drive the kettle body 110 to rotate in the reverse direction so that the opening of the kettle body 110 faces upward.

[0040] It can be understood that when hydrates are synthesized in the reaction chamber 111, fog will form on the first sapphire glass window 112 and the second sapphire glass window 121. At this time, the drying member 420 can also be used to blow the first sapphire glass window 112 and the second sapphire glass window 121 to remove the fog generated on the surface for clearer in-situ laser Raman spectroscopy observation.

[0041] Optionally, the flushing member 410 is a micro high-pressure water gun. Optionally, the drying member 420 is a temperature-controlled air gun. Optionally, the high-pressure reaction device further includes a first fixing frame 430. The first fixing frame 430 can be arranged on one side of the reaction kettle 100, and the micro high-pressure water gun and the temperature-controlled air gun are both rotatably connected to the first fixing frame 430 for flushing and drying the kettle lid 120 and the kettle body 110.

[0042] Optionally, in some embodiments, the high-pressure reaction device further includes an autoclave opening member, which is connected to the autoclave cover 120 and is used to separate or connect the autoclave cover 120 from the autoclave body 110, thereby opening or closing the reaction chamber 111. By providing the autoclave opening member, the high-pressure reaction device can complete automatic autoclave opening without manual operation, saving time and effort and improving the experimental efficiency.

[0043] Optionally, in some embodiments, referring to Figure 1 and Figure 4 , the autoclave cover 120 is threadedly connected to the autoclave body 110. The autoclave opening member includes a clamping member 510 and a second driving member 520. The clamping member 510 is used to clamp the autoclave cover 120 and is movable in the vertical direction. The second driving member 520 is connected to the clamping member 510 to drive the clamping member 510 to rotate, so as to separate or connect the autoclave cover 120 from the autoclave body 110.

[0044] When opening the autoclave, the clamping member 510 descends and clamps the autoclave cover 120, and then the second driving member 520 drives the clamping member 510 to rotate. At the same time, the clamping member 510 moves upward to screw out the autoclave cover 120 upward, completing the autoclave opening operation. When closing the autoclave, the autoclave cover 120 is aligned with the autoclave body 110. The second driving member 520 drives the clamping member 510 to rotate in the reverse direction. At the same time, the clamping member 510 moves downward to make the autoclave cover 120 be hermetically connected to the autoclave body 110, completing the autoclave closing operation.

[0045] Optionally, the second driving member 520 is movable in the vertical direction, and the clamping member 510 is driven to move up and down by moving the second driving member 520 up and down. Optionally, the second driving member 520 is a brushless motor. Optionally, the high-pressure reaction device further includes a second fixing frame (not shown in the drawings). The second fixing frame can be arranged on one side of the reaction kettle 100. The second driving member 520 can be connected to the second fixing frame through an electric telescopic rod (not shown in the drawings). By telescoping the electric telescopic rod, the second driving member 520 can be controlled to move in the vertical direction, thereby driving the clamping member 510 to move up and down.

[0046] Optionally, in some embodiments, the clamping member 510 includes two calipers. Two force-receiving members 122 are symmetrically arranged on the autoclave cover 120. The two calipers are respectively used to clamp the two force-receiving members 122 to clamp the autoclave cover 120. Optionally, the force-receiving member 122 is a force-receiving rod.

[0047] Optionally, referring to Figure 2 , a sealing member 130 is arranged between the autoclave cover 120 and the autoclave body 110 to enable the autoclave cover 120 to be further hermetically connected to the autoclave body 110 and ensure the tightness of the reaction kettle 100. Optionally, the sealing member 130 is a sealing gasket.

[0048] Optionally, in some embodiments, the high-pressure reaction device further includes a vacuum pump 600, a gas source (not shown in the drawings), and a liquid source (not shown in the drawings). The vacuum pump 600 is connected to the reaction chamber 111 to evacuate the reaction chamber 111. The gas source is connected to the reaction chamber 111 to inject reaction gas into the reaction chamber 111. The liquid source is connected to the reaction chamber 111 to inject reaction liquid into the reaction chamber 111. It can be understood that when injecting reaction gas into the reaction chamber 111, the injection amount of the reaction gas injected into the reaction chamber 111 can be controlled by the pressure sensor 220. Optionally, the vacuum pump 600 is a micro vacuum pump 600, which is beneficial to the miniaturization of the device. By providing the vacuum pump 600, the gas source, and the liquid source, the high-pressure reaction device can complete automatic vacuum pumping, gas injection, and liquid injection without manual operation, saving time and effort and improving the experimental efficiency.

[0049] Optionally, in some embodiments, refer to Figure 1 and Figure 5 , the reaction chamber 111 is connected to the vacuum pump 600 through a first pipeline 710. A first connection point 711 is provided on the first pipeline 710. The first connection point 711 is connected to the gas source through a second pipeline 720. A second connection point 712 is provided on the first pipeline 710 between the first connection point 711 and the vacuum pump 600. The second connection point 712 is connected to the liquid source through a third pipeline 730. A first valve 713 is provided on the first pipeline 710 between the reaction kettle 100 and the first connection point 711. A second valve 721 is provided on the second pipeline 720. A third valve 731 is provided on the third pipeline 730. A fourth valve 714 is provided on the first pipeline 710 between the second connection point 712 and the vacuum pump 600. Optionally, the first valve 713, the second valve 721, the third valve 731, and the fourth valve 714 are all electric high-pressure ball valves.

[0050] By opening the first valve 713 and the fourth valve 714 and closing the second valve 721 and the third valve 731, the passage between the reaction chamber 111 and the vacuum pump 600 can be connected, enabling the vacuum pump 600 to evacuate the reaction chamber 111. By opening the first valve 713 and the second valve 721 and closing the third valve 731 and the fourth valve 714, the passage between the reaction chamber 111 and the gas source can be connected, enabling the gas source to inject reaction gas into the reaction chamber 111. By opening the first valve 713 and the third valve 731 and closing the second valve 721 and the fourth valve 714, the passage between the reaction chamber 111 and the liquid source can be connected, enabling the liquid source to inject reaction liquid into the reaction chamber 111.

[0051] Optionally, refer to Figure 1 and Figure 5, the pressure sensor 220 is connected to the first pipeline 710, and the pressure sensor 220 is disposed between the reaction chamber and the first valve 713 to measure the pressure in the reaction chamber 111. Of course, the pressure sensor 220 can also be directly connected to the reaction kettle 100 to measure the pressure in the reaction chamber 111, and no specific limitation is made here.

[0052] Optionally, in some embodiments, an electronic flowmeter 732 is disposed between the third valve 731 and the second connection point 712 of the third pipeline 730 to measure the volume of the reaction liquid injected into the reaction chamber 111. Optionally, a plunger pump (not shown in the drawings) is disposed between the third valve 731 and the liquid source of the third pipeline 730. The reaction liquid can be pumped into the reaction chamber 111 through the plunger pump. Optionally, a back pressure regulator is installed at the outlet of the plunger pump.

[0053] Optionally, in some embodiments, refer to Figure 1 or Figure 2 , the high-pressure reaction device further includes a movable platform 800, and the reaction kettle 100 is placed on the movable platform 800. The movable platform 800 is used to move the reaction kettle 100 so as to find a better observation site. Optionally, the movable platform 800 can be a six-direction movable platform, that is, the movable platform 800 can move up and down, left and right, and back and forth.

[0054] It can be understood that in order not to affect the pipeline when the reaction kettle 100 moves, the above-mentioned first pipeline 710, second pipeline 720 and third pipeline 730 can adopt flexible hoses. In order not to affect the first driving member 310 when the reaction kettle 100 moves, the above-mentioned first driving member 310 can be fixedly connected to the movable platform 800.

[0055] Optionally, the high-pressure reaction device further includes a control unit 900. Components such as the second driving member 520, the electric telescopic rod, the first driving member 310, the flushing member 410, the drying member 420, the vacuum pump 600, the first valve 713, the second valve 721, the third valve 731, the fourth valve 714, the electronic flowmeter 732, the plunger pump, the movable platform 800, the pressure sensor 220, and the temperature control system 210 are all electrically connected to the control unit 900.

[0056] The working principle of the high-pressure reaction device in the embodiments of this application is as follows: Before conducting an experiment, the high-pressure reaction device automatically completes the steps of opening the kettle, cleaning, and drying the reaction kettle 100. Specifically, the control unit 900 controls the electric telescopic rod to extend so that the second driving member 520 descends, and at the same time drives the clamping member 510 to descend, so that the clamping member 510 clamps the kettle cover 120. Then, the control unit 900 controls the second driving member 520 to drive the clamping member 510 to rotate, and at the same time controls the electric telescopic rod to shorten so that the clamping member 510 screws the kettle cover 120 upward to complete the action of opening the kettle. Next, the control unit 900 controls the first driving member 310 to drive the kettle body 110 to rotate so that the opening of the kettle body 110 faces downward. Then, the control unit 900 controls the flushing member 410 to move to flush the kettle cover 120 and the kettle body 110. It can be understood that in order to ensure the accuracy of the experiment, the flushing member 410 here flushes the kettle cover 120 and the kettle body 110 with deionized water. After flushing, the control unit 900 controls the drying member 420 to move to dry the kettle cover 120 and the kettle body 110. Then, the control unit 900 controls the first driving member 310 to drive the kettle body 110 to rotate in the reverse direction so that the opening of the kettle body 110 faces upward. After the above actions are completed, the device stops running so that the researcher can load the sample for the experiment.

[0057] After the sample loading is completed, the high-pressure reaction device performs the steps of automatic sealing and vacuum pumping. Specifically, the control unit 900 controls the electric telescopic rod to extend so that the second driving member 520 descends, and at the same time drives the clamping member 510 to descend, so that the kettle cover 120 clamped by the clamping member 510 is aligned with the kettle body 110. After alignment, the control unit 900 controls the second driving member 520 to drive the clamping member 510 to rotate in the reverse direction, and at the same time controls the electric telescopic rod to extend so that the kettle cover 120 is hermetically connected to the kettle body 110 to complete the action of closing the kettle. Then, the control unit 900 controls the first valve 713 and the fourth valve 714 to open, and the second valve 721 and the third valve 731 to close to connect the passage between the reaction chamber 111 and the vacuum pump 600. At the same time, the control unit 900 controls the vacuum pump 600 to start to pump the reaction chamber 111 to vacuum, so that the air in the reaction chamber 111 is discharged.

[0058] After the vacuum pumping is completed, the hydrate synthesis step will be carried out. Specifically, the control unit 900 controls the first valve 713 and the second valve 721 to open, and the third valve 731 and the fourth valve 714 to close, so as to connect the passage between the reaction chamber 111 and the gas source (i.e., the gas source passage), thereby injecting reaction gas into the reaction chamber 111. During the injection of the reaction gas, the pressure sensor 220 detects the pressure in the reaction chamber 111 in real time and feeds it back to the control unit 900, so as to accurately control the pressure in the reaction chamber 111 and the injection amount of the reaction gas. If it is necessary to inject reaction liquid, the control unit 900 can control the first valve 713 and the third valve 731 to open, and the second valve 721 and the fourth valve 714 to close, so as to connect the passage between the reaction chamber 111 and the liquid source (i.e., the liquid source passage), and at the same time the control unit 900 controls the plunger pump to open, so as to inject reaction liquid into the reaction chamber 111. During the injection of the reaction liquid, the electronic flowmeter 732 measures the injection amount of the reaction liquid in real time and feeds it back to the control unit 900, so as to accurately control the injection amount of the reaction liquid. Through the pressure sensor 220 and the electronic flowmeter 732, the injection amounts of the reaction gas and the reaction liquid can be accurately controlled, reducing human operation errors and improving the accuracy of experimental results.

[0059] After the gas injection and liquid injection are completed, the control unit 900 controls the temperature control system 210 to turn on, and controls the temperature in the reaction kettle 100 at a preset temperature to carry out the synthesis of hydrates. During the waiting process for the formation of hydrates, the control unit 900 can control the drying part 420 (temperature-controlled air gun) to blow the first sapphire glass window 112 and the second sapphire glass window 121 to remove the fog generated on the surface, so as to perform in-situ Raman spectroscopy observation more clearly. During the observation, the control unit 900 can control the movable platform 800 to move so as to find the best observation site.

[0060] The high-pressure reaction device in the embodiment of the present application can automatically complete some experimental operations in Raman observation through the control unit 900, including: opening the kettle, cleaning, drying, sealing, vacuum pumping, gas injection and liquid injection, which can greatly improve the experimental efficiency and reduce the experimental operation cost.

[0061] The following takes the process of simulating hydrate carbon sequestration by the high-pressure reaction device in the present application as an example for illustration. The specific contents of the high-pressure reaction device automatically completing steps such as opening the kettle, cleaning, drying, and vacuum pumping will not be elaborated here, and can be specifically referred to the content in the working principle of the high-pressure reaction device described above. Of course, the high-pressure reaction device in the present application can also conduct conventional research on the vertical generation and decomposition of hydrates, and no specific restrictions are made here.

[0062] Optionally, the hydrate carbon sequestration process specifically includes the following steps.

[0063] Step S100: Open the autoclave, clean and dry the reaction kettle 100.

[0064] Step S200: Load the porous medium sample saturated with water into the reaction chamber 111 of the reaction kettle 100 and close the autoclave. Use a vacuum pump 600 to evacuate the reaction chamber 111, and inject and release methane gas into the reaction chamber 111 three times through the gas supply path to ensure that there is no residual air in the reaction chamber 111.

[0065] Step S300: Inject methane gas with a pressure of 5 MPa into the reaction chamber 111 through the gas supply path. In other words, when the pressure sensor 220 detects that the pressure in the reaction chamber 111 is 5 MPa, stop injecting methane gas.

[0066] Step S400: Turn on the temperature control system 210, control the temperature in the reaction chamber 111 at 2 °C, and carry out hydrate synthesis. During this process, the reaction kettle 100 can be driven by the first driving member 310 to rotate counterclockwise by 90°, so that the first sapphire glass window 112 on the side wall of the kettle body 110 faces upward, and the distribution characteristic changes of the hydrate in the longitudinal direction (i.e., along the length direction of the reaction kettle 100) can be observed through the first sapphire glass window 112.

[0067] Step S500: After the methane hydrate is completely formed, open the liquid source path, and inject liquid carbon dioxide into the reaction chamber 111 at a preset rate through a plunger pump. When injecting liquid carbon dioxide through the plunger pump, keep the system pressure at 5 Mpa through a back pressure regulator.

[0068] Step S600: Through Raman spectroscopy, the longitudinal distribution characteristics and phase change process of the hydrate after injecting liquid carbon dioxide can be observed in real time. At the same time, gas is collected according to a preset time period, and the stability of carbon dioxide-sequestered hydrate is studied through component detection. Optionally, the effects of different factors on carbon dioxide-sequestered hydrate can also be studied by changing temperature, pressure, injection rate of liquid carbon dioxide, etc.

[0069] It can be understood that the high-pressure reaction device in the present application can be widely applied to the research of the longitudinal growth process of hydrate at the gas-liquid interface, the phase change (formation / decomposition) process of hydrate in the pores of sediments at the sediment-gas, water interface and in the longitudinal direction of sediments, etc. in hydrate and carbon sequestration experiments.

[0070] Other components and operations of the high-pressure reaction device according to the embodiments of the present application are known to those of ordinary skill in the art and will not be described in detail here.

[0071] The embodiment of the present application further provides a Raman analysis device, which includes the above-mentioned high-pressure reaction device and a Raman spectrometer. The Raman laser of the Raman spectrometer can pass through the first sapphire glass window 112 or the second sapphire glass window 121 and irradiate on the hydrate in the reaction chamber 111. The hydrate in the reaction chamber 111 of the high-pressure reaction device can be subjected to in-situ Raman analysis by the Raman spectrometer.

[0072] It can be understood that the Raman analysis device in the embodiment of the present application correspondingly has the beneficial effects provided by the above-mentioned high-pressure reaction device, which will not be elaborated here.

[0073] The other components and operations of the Raman analysis device according to the embodiment of the present application are known to those of ordinary skill in the art and will not be described in detail here.

[0074] The above has described the embodiments of the present application in detail with reference to the drawings. However, the present application is not limited to the above embodiments. Various changes can be made without departing from the spirit of the present application within the scope of knowledge possessed by those of ordinary skill in the art.

Claims

1. A high-pressure reaction device, characterized in that, Comprising: A reaction kettle, the reaction kettle includes a kettle cover and a kettle body, a reaction chamber is formed inside the reaction kettle, the reaction chamber is used to generate hydrates, the kettle cover is detachably connected to the kettle body to open and close the reaction chamber, and the kettle body is rotatably arranged; A first sapphire glass window, the first sapphire glass window is arranged on the side wall of the kettle body, and the first sapphire glass window is used to allow Raman laser to pass through and irradiate on the hydrates in the reaction chamber after the kettle body rotates a preset angle; A temperature control system, the temperature control system is connected to the reaction kettle to control the temperature in the reaction chamber; A pressure sensor, the pressure sensor is connected to the reaction kettle to measure the pressure in the reaction chamber.

2. The high-pressure reaction device according to claim 1, characterized in that: The high-pressure reaction device further includes a first driving member, the first driving member is connected to the kettle body to drive the kettle body to rotate.

3. The high-pressure reaction device according to claim 2, wherein: The high-pressure reaction device further includes a flushing member and a drying member, the flushing member is used to flush the reaction kettle, the drying member is used to dry the reaction kettle, and the flushing member and the drying member are both movably arranged on one side of the reaction kettle.

4. The high-pressure reaction device according to claim 1, wherein: The high-pressure reaction device further includes a second sapphire glass window, the second sapphire glass window is arranged on the top of the kettle cover.

5. The high-pressure reaction device according to claim 1, characterized in that: The high-pressure reaction device further includes an opening kettle member, the opening kettle member is connected to the kettle cover, and the opening kettle member is used to separate or connect the kettle cover and the kettle body, so as to open and close the reaction chamber.

6. The high-pressure reaction device according to claim 5, wherein: The kettle cover is threadedly connected to the kettle body, the opening kettle member includes a clamping member and a second driving member, the clamping member is used to clamp the kettle cover, the clamping member is movable in the vertical direction, and the second driving member is connected to the clamping member to drive the clamping member to rotate, so as to separate or connect the kettle cover and the kettle body.

7. The high-pressure reaction device according to claim 1, characterized in that: The high-pressure reaction device further includes a vacuum pump, a gas source and a liquid source, the vacuum pump is communicated with the reaction chamber to evacuate the reaction chamber, the gas source is communicated with the reaction chamber to inject reaction gas into the reaction chamber, and the liquid source is communicated with the reaction chamber to inject reaction liquid into the reaction chamber.

8. The high-pressure reaction device according to claim 7, wherein: The reaction chamber is communicated with the vacuum pump through a first pipeline, a first connection point is arranged on the first pipeline, the first connection point is communicated with the gas source through a second pipeline, a second connection point is arranged between the first pipeline and the vacuum pump at the first connection point, the second connection point is communicated with the liquid source through a third pipeline, a first valve is arranged between the reaction kettle and the first connection point on the first pipeline, a second valve is arranged on the second pipeline, a third valve is arranged on the third pipeline, a fourth valve is arranged between the second connection point and the vacuum pump on the first pipeline, an electronic flowmeter is arranged between the third valve and the second connection point on the third pipeline to measure the volume of the reaction liquid injected into the reaction chamber, and a plunger pump is arranged between the third valve and the liquid source on the third pipeline.

9. The high-pressure reaction device according to claim 1, wherein: The high-pressure reaction device further includes a movable platform, the reaction kettle is placed on the movable platform, and the movable platform is used to move the reaction kettle.

10. Raman analysis device, characterized in that: Comprising a high-pressure reaction device according to any one of claims 1 to 9.

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