Visual CO2 hydrate reaction kettle for in-situ Raman test

Abstract

The utility model discloses a visual CO2 hydrate reaction kettle for in-situ Raman test, which comprises a kettle body, a jacket wall is arranged on the outer wall of the kettle body, a temperature control cavity is formed between the jacket wall and the kettle body, a transparent window is arranged on the outer wall of the kettle body, and a sealing sleeve extending to the transparent window is arranged on the jacket wall. A connecting plug is detachably installed at the end, located outside the jacket wall, of the sealing sleeve, and a through hole used for installing a detection probe is formed in the center of the connecting plug. The utility model has the beneficial effects that the sealing sleeve is matched with the transparent window, the detection probe is arranged on the connecting plug in a penetrating manner, and the connecting plug is clamped into the outer end of the sealing sleeve, so that the detection probe is closer to the transparent window to carry out laser emission and scattered laser absorption; and the detection probe transmits the generated signal to the Raman detection device for spectral analysis so as to determine the composition of the hydrate and the type and occupancy rate of the object cavity, and carry out hydrate dynamics experiment research.

Description

Technical Field

[0001] The utility model relates to the technical field of reaction kettles, in particular to a visual CO2 hydrate reaction kettle for in-situ Raman testing. Background Technique

[0002] As one of the main components of greenhouse gases, it is urgent to reduce the emissions of CO2. Hydrates are non-stoichiometric clathrate compounds formed by some small molecule gases and water under high pressure and low temperature conditions, and their appearance is similar to ice. Gases have selectivity during the formation of hydrates, and different gases have different temperatures and pressures during the formation of hydrates. By controlling the temperature and pressure changes during the formation of hydrates, the gases that are prone to form hydrates can be enriched in the hydrate phase, thereby achieving the purpose of separation. Compared with traditional separation methods, the separation principle and process of the hydrate method are relatively simple and the cost is low. And the reaction conditions required for the hydrate separation process are relatively mild, and the pressure and temperature are relatively easy to achieve and control the energy consumption during the chemical reaction process. The hydrate separation process will not produce secondary pollution. The formation and separation processes of hydrates only require gas and water, and will not produce waste and material losses like traditional separation processes.

[0003] At present, the phase equilibrium and the growth process of hydrates during formation are often studied from the perspectives of thermodynamics and kinetics. Laser Raman spectroscopy is usually used to detect the basic information of the hydrate structure. However, it is difficult to fix the detection probe with the existing reaction kettles, and the operator needs to hold the probe for detection, which is rather inconvenient. Content of the Utility Model

[0004] The purpose of the utility model is to provide a visual CO2 hydrate reaction kettle for in-situ Raman testing, and solve the problem that it is difficult to fix the detection probe with the existing reaction kettles and the operator needs to hold the probe for detection.

[0005] The purpose of the utility model is achieved through the following technical solutions:

[0006] A visual CO2 hydrate reaction kettle for in-situ Raman testing includes a kettle body. A jacket wall is provided on the outer wall of the kettle body. A temperature control cavity is formed between the jacket wall and the kettle body. A transparent window is provided on the outer wall of the kettle body. A sealing sleeve extending to the position of the transparent window is provided on the jacket wall. A connection plug is detachably installed at one end of the sealing sleeve located outside the jacket wall. A through hole for installing a detection probe is opened at the center of the connection plug.

[0007] Furthermore, symmetrically arranged centering reeds with gradually decreasing sizes are provided inside the sealing sleeve. An arc-shaped support piece for supporting the detection probe is provided at the end of the centering reed.

[0008] Further, a liquid inlet and a liquid outlet communicating with the temperature control chamber are provided on the jacket wall.

[0009] Further, a kettle cover is installed on the upper end of the kettle body through a buckle. A stirring mechanism extending into the kettle body is provided on the kettle cover, and mounting fixing holes are provided on the kettle cover.

[0010] Further, a snap - on upper positioning ring plate is provided at the upper end of the buckle, and a snap - on lower positioning ring plate is provided at the lower end. A positioning cavity is formed by the snap - on upper positioning ring plate, the buckle, and the snap - on lower positioning ring plate. The lower end of the kettle cover extends into the positioning cavity and is provided with a kettle - cover hanging plate adapted to the snap - on upper positioning ring plate. The upper end of the kettle body extends into the positioning cavity and is provided with a kettle - body hanging plate adapted to the snap - on lower positioning ring plate. The sizes of the kettle - cover hanging plate and the kettle - body hanging plate are mutually adapted, and a locking screw hole for pressing the kettle - cover hanging plate is formed on the snap - on upper positioning ring plate.

[0011] Further, a snap ring gasket is provided between the snap - on upper positioning ring plate and the kettle - cover hanging plate.

[0012] Further, an air inlet, an exhaust port, a gas - phase temperature measuring port, a liquid - phase temperature measuring port, and a rupture disk port are provided on the kettle cover. The air inlet is connected with an air inlet needle valve, the exhaust port is connected with an exhaust needle valve, the gas - phase temperature measuring port and the liquid - phase temperature measuring port are connected with thermocouples, and the rupture disk port is connected with a rupture disk.

[0013] The present utility model has the following advantages:

[0014] By using the provided sealing sleeve and the transparent window in cooperation, the detection probe is inserted through the connecting plug. The connecting plug is snapped into the outer end of the sealing sleeve, so that the detection probe is closer to the position of the transparent window for laser emission and scattered laser absorption. The detection probe transmits the generated signal to the Raman detection device for spectral analysis to determine the composition of the hydrate, the type of guest cavities, and the occupancy rate, and to conduct experimental research on hydrate kinetics. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 is a schematic structural diagram of the present utility model.

[0016] Figure 2 is a schematic top - view structure diagram of the kettle cover.

[0017] In the figure, 1 - kettle body, 2 - jacket wall, 3 - temperature controller chamber, 4 - transparent viewing window, 5 - sealing sleeve, 6 - connecting plug, 7 - detection probe, 8 - through hole, 9 - centering reed, 10 - arc-shaped support piece, 11 - liquid inlet, 12 - liquid outlet, 13 - buckle, 14 - kettle cover, 15 - stirring mechanism, 16 - installation and fixing hole, 17 - upper positioning ring plate of the buckle, 18 - lower positioning ring plate of the buckle, 19 - hanging plate of the kettle cover, 20 - hanging plate of the kettle body, 21 - locking screw hole, 22 - air inlet, 23 - exhaust port, 24 - gas-phase temperature measurement port, 25 - liquid-phase temperature measurement port, 26 - bursting disc port, 27 - snap ring gasket, 28 - sealing gasket. Detailed implementation manners

[0018] To make the purpose, technical solutions and advantages of the embodiments of the present utility model clearer, the technical solutions in the embodiments of the present utility model will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present utility model. Obviously, the described embodiments are some but not all of the embodiments of the present utility model. Usually, the components of the embodiments of the present utility model described and shown in the accompanying drawings here can be arranged and designed in various different configurations.

[0019] Therefore, the following detailed description of the embodiments of the present utility model provided in the accompanying drawings is not intended to limit the scope of the claimed present utility model, but merely represents the selected embodiments of the present utility model. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present utility model without making creative efforts fall within the scope of protection of the present utility model.

[0020] It should be noted that, without conflict, the embodiments in the present utility model and the features in the embodiments can be combined with each other.

[0021] It should be noted that like reference numerals and letters denote like items in the following drawings, and thus, once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings.

[0022] In the description of the present utility model, it should be noted that the orientation or positional relationship indicated by terms such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings, or the orientation or positional relationship in which the product of the present utility model is customarily placed during use, or the orientation or positional relationship commonly understood by those skilled in the art. It is only for the convenience of describing the present utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as a limitation to the present utility model. In addition, terms such as "first", "second", etc. are only used for distinguishing descriptions and cannot be understood as indicating or implying relative importance.

[0023] In the description of the present utility model, it should also be noted that unless otherwise clearly specified and defined, the terms "set", "installed", "connected", "coupled" should be understood in a broad sense. For example, it 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 directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present utility model can be understood according to specific circumstances.

[0024] Refer to Figure 1 As shown, an embodiment of the present utility model is:

[0025] A visualization CO2 hydrate reactor for in-situ Raman testing, comprising a reactor body 1, an outer wall of the reactor body 1 is provided with a jacket wall 2, a temperature control chamber 3 is formed between the jacket wall 2 and the reactor body 1, a transparent window 4 is provided on the outer wall of the reactor body 1, a sealing sleeve 5 extending to the position of the transparent window 4 is provided on the jacket wall 2, a connection plug 6 is detachably installed at one end of the sealing sleeve 5 outside the jacket wall 2, and a through hole 8 for installing a detection probe 7 is opened at the center of the connection plug 6.

[0026] The internal situation of the reactor can be conveniently observed through the provided transparent window 4, including the state of the reactants, the reaction process, the temperature change, and the mixing effect, so as to adjust the reaction conditions in a timely manner according to the reaction process. The provided sealing sleeve 5 cooperates with the transparent window 4, and the detection probe is inserted through the connecting plug 6. The connecting plug 6 is snapped into the outer end of the sealing sleeve 5, making the detection probe closer to the transparent window for laser emission and scattered laser absorption. After raising the temperature of the reactor, solid carbon dioxide hydrate can be decomposed to obtain high-purity carbon dioxide gas. The detection probe transmits the generated signal to the Raman detection device for spectral analysis to determine the composition of the hydrate, the type and occupancy rate of the guest cavities, and conduct kinetic experiments on the hydrate. The detection process is fast and direct, without offline sampling, the static / dynamic generation kinetic process of the hydrate is not restricted, the operation process is simple, and the monitoring process does not require pressure maintenance.

[0027] Specifically, for the convenience of installation, a connecting sleeve with an enlarged diameter is integrally formed at the outer end of the sealing sleeve 5 to facilitate the setting of a larger-sized connecting plug 6, which is convenient for operation and the installation of the detection probe.

[0028] Furthermore, to facilitate stabilizing the position of the detection probe 7 in the sealing sleeve 5, symmetrically arranged centering reeds 9 with gradually decreasing dimensions are provided inside the sealing sleeve 5, and arc-shaped support pieces 10 for supporting the detection probe 7 are provided at the ends of the centering reeds 9.

[0029] An inlet 11 and an outlet 12 communicating with the temperature control chamber 3 are provided on the jacket wall 2.

[0030] During operation, a medium (such as ethylene glycol, liquid nitrogen) can be introduced into the temperature control chamber 3, and the temperature of the reactor can be lowered or raised by using the circulation of the medium. To reduce energy consumption, the outer wall of the jacket is also coated with a heat-insulating material.

[0031] In this embodiment, the upper end of the kettle body 1 is installed with a kettle cover 14 through a buckle 13. A stirring mechanism 15 extending into the kettle body 1 is provided on the kettle cover 14, and an installation fixing hole 16 is provided on the kettle cover 14.

[0032] Specifically, the stirring mechanism 15 includes a stirring blade, a stirring rod, and an external driving motor.

[0033] The upper end of the buckle 13 is provided with an upper positioning ring plate 17 of the buckle, and the lower end is provided with a lower positioning ring plate 18 of the buckle. The upper positioning ring plate 17 of the buckle, the buckle 13 and the lower positioning ring plate 18 of the buckle enclose a positioning cavity. The lower end of the kettle cover 14 extends into the positioning cavity and is provided with a hanging plate 19 of the kettle cover adapted to the upper positioning ring plate 17 of the buckle. The upper end of the kettle body 1 extends into the positioning cavity and is provided with a hanging plate 20 of the kettle body adapted to the lower positioning ring plate 18 of the buckle. The sizes of the hanging plate 19 of the kettle cover and the hanging plate 20 of the kettle body are mutually adapted. The upper positioning ring plate 17 of the buckle is provided with a locking screw hole 21 for pressing the hanging plate 19 of the kettle cover, and a locking screw is provided on the locking screw hole 21.

[0034] Furthermore, a clamping ring gasket 27 is arranged between the upper positioning ring plate 17 of the buckle and the hanging plate 19 of the kettle cover. When connecting the kettle body 1 and the kettle cover 14, screw the locking screw into the locking screw hole 21 to press the clamping ring gasket 27, the hanging plate 19 of the kettle cover, the hanging plate 20 of the kettle body and the lower positioning ring plate 18 of the buckle, so that the whole structure can be kept stable; the installation fixing hole 16 is used to install and fix the kettle cover 14 with an external fixing plate, improve the stability of the kettle cover 14, reduce the influence of the operation vibration of the stirring mechanism 15 on the kettle cover 14, and then ensure the temperature of the internal environment of the reaction kettle and the gas storage effect of the reaction kettle. At the same time, an annular sealing groove is arranged at the lower end of the kettle cover 14, and a sealing gasket 28 is arranged in the sealing groove.

[0035] In this embodiment, the kettle cover 14 is provided with an air inlet 22, an exhaust port 23, a gas-phase temperature measuring port 24, a liquid-phase temperature measuring port 25 and a bursting disc port 26. The air inlet 22 is connected with an air inlet needle valve, the exhaust port 23 is connected with an exhaust needle valve, the gas-phase temperature measuring port 24 and the liquid-phase temperature measuring port 25 are connected with thermocouples, and the bursting disc port 26 is connected with a bursting disc.

[0036] The air inlet 22 is used to introduce a carbon dioxide mixed gas. In the high-pressure and low-temperature environment of the reaction kettle, the gas reacts with the solution by hydration. According to the phase equilibrium difference of different hydrates, carbon dioxide will form solid hydrates, and the remaining gas remains stable and is then discharged to achieve gas-solid separation. The exhaust port 23 is used to discharge impurity gases and purified carbon dioxide. Specifically, the exhaust port 23 can be connected to two exhaust pipes through a three-way valve. One exhaust pipe is used to discharge impurities, and the other exhaust pipe discharges purified carbon dioxide. The gas-phase temperature measuring port 24 and the liquid-phase temperature measuring port 25 are connected with thermocouples to detect the gas-phase and liquid-phase temperatures in the reaction kettle, so as to accurately control the temperature. A pressure gauge and a pressure sensor are also arranged on the kettle cover 14 to detect the pressure inside the reaction kettle and make the pressure meet the requirements of the hydration reaction. When the pressure in the reaction kettle rises to the set value, the bursting disc automatically breaks or falls off to relieve pressure and ensure the safety of the reaction kettle.

[0037] Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some of the technical features. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present utility model shall be included within the protection scope of the present utility model.

Claims

1. A visualization CO2 hydrate reactor for in-situ Raman testing, characterized in that: It includes a kettle body, an outer wall of the kettle body is provided with a jacket wall, a temperature control chamber is formed between the jacket wall and the kettle body, a transparent window is provided on the outer wall of the kettle body, a sealing sleeve extending to the position of the transparent window is provided on the jacket wall, a connection plug is detachably installed at one end of the sealing sleeve located outside the jacket wall, and a through hole for installing a detection probe is opened at the center of the connection plug.

2. The visual CO2 hydrate reactor for in-situ Raman testing according to claim 1, characterized in that: Centering reeds with gradually decreasing sizes are symmetrically arranged in the sealing sleeve, and arc-shaped support pieces for supporting the detection probe are provided at the ends of the centering reeds.

3. The visualized CO2 hydrate reactor for in-situ Raman testing according to claim 1, wherein: The jacket wall is provided with a liquid inlet and a liquid outlet communicating with the temperature control chamber.

4. A visualization CO2 hydrate reactor for in-situ Raman testing according to claim 1, characterized in that: The upper end of the kettle body is installed with a kettle cover through a buckle, a stirring mechanism extending into the kettle body is provided on the kettle cover, and installation fixing holes are provided on the kettle cover.

5. The visualized CO2 hydrate reactor for in-situ Raman testing according to claim 4, characterized in that: The upper end of the buckle is provided with an upper positioning ring plate of the buckle, and the lower end is provided with a lower positioning ring plate of the buckle. The upper positioning ring plate of the buckle, the buckle and the lower positioning ring plate of the buckle enclose a positioning chamber. The lower end of the kettle cover extends into the positioning chamber and is provided with a kettle cover hanging plate adapted to the upper positioning ring plate of the buckle. The upper end of the kettle body extends into the positioning chamber and is provided with a kettle body hanging plate adapted to the lower positioning ring plate of the buckle. The sizes of the kettle cover hanging plate and the kettle body hanging plate are mutually adapted, and a locking screw hole for pressing the kettle cover hanging plate is opened on the upper positioning ring plate of the buckle.

6. The visualized CO2 hydrate reactor for in-situ Raman testing according to claim 5, characterized in that: A snap ring gasket is arranged between the upper positioning ring plate of the buckle and the kettle cover hanging plate.

7. A visualization CO2 hydrate reactor for in-situ Raman testing according to claim 4, characterized in that: An air inlet, an exhaust port, a gas-phase temperature measurement port, a liquid-phase temperature measurement port and a rupture disk port are provided on the kettle cover. The air inlet is connected with an air inlet needle valve, the exhaust port is connected with an exhaust needle valve, the gas-phase temperature measurement port and the liquid-phase temperature measurement port are connected with thermocouples, and the rupture disk port is connected with a rupture disk.

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