In-situ detection device for separating carbon dioxide by hydrate method

Abstract

The utility model discloses an in-situ detection device for separating carbon dioxide by a hydrate method, which comprises a Raman reaction kettle, the Raman reaction kettle is provided with a liquid inlet, a gas inlet and a gas outlet, the gas outlet is connected with a vacuum system, the gas inlet is connected with a gas supply system, and the Raman reaction kettle is further connected with a temperature control system and a monitoring system. Window glass is arranged on an inner kettle body of the Raman reaction kettle, a glass pressing plate is arranged on the window glass, an opening matched with the window glass is formed in the center of the glass pressing plate, a fixing piece is arranged on the glass pressing plate and located on the outer side of the opening, and a monitoring camera is arranged on the fixing piece. According to the method, the hydrate dissolution-induced nucleation and growth period kinetic curve can be intuitively analyzed, online microstructure monitoring and in-situ decomposition observation are simultaneously carried out in the hydrate generation process, important information is provided for carbon dioxide separation dynamics and microstructures, the detection process is rapid and direct, off-line sampling is not needed, and the detection efficiency is high. And the dynamic process of hydrate static / dynamic generation is not limited.

Description

TECHNICAL FIELD

[0001] The utility model relates to reaction kettle technical field, especially a hydrate method separates carbon dioxide in situ detection device. BACKGROUND

[0002] Hydrate is a non-stoichiometric, ice-like envelope compound formed by some small molecule gas and water under high pressure and low temperature. Gas hydrate has selectivity to gas in the generation process, and different gases have different temperature and pressure when generating hydrate. By controlling the temperature and pressure change in the hydrate generation process, the gas that is easy to generate hydrate is enriched in the hydrate phase, so as to achieve the purpose of separation.

[0003] With the increasing attention to climate change and environmental protection problems in the world, carbon dioxide capture, separation and storage technology has become a research hotspot. As an effective carbon dioxide capture and separation technology, hydrate method has attracted much attention due to its low energy consumption, simple operation and environmental friendliness. In-situ detection is a key link in this technology, which can realize real-time monitoring and analysis of the carbon dioxide hydrate generation process, and provide important basis for optimizing process conditions and improving separation efficiency

[0004] At present, the phase equilibrium and hydrate growth process of hydrate generation are often studied from the thermodynamic and kinetic points of view, and laser Raman spectrum is usually used to detect the basic information of hydrate structure. At present, when laser Raman spectrum is used to detect hydrate, the first method is to take sample off-line monitoring after hydrate is generated in the reaction kettle, which cannot realize in-situ monitoring of hydrate generation and decomposition; the second method is to use pressure maintaining system and isotope gas replacement method to detect hydrate structure after hydrate is generated in the reaction kettle, which has complex operation process and high energy consumption and cost; the third method is to generate hydrate directly in a micro in-situ reaction device and monitor the growth process of hydrate in-situ, on the one hand, the generation of hydrate is limited to static reaction, on the other hand, it cannot meet the experimental requirements of gas separation kinetics. UTILITY MODEL CONTENT

[0005] The utility model aims at providing a hydrate method separates carbon dioxide in situ detection device, realizes that the hydrate generation process carries out online microstructure monitoring and in-situ decomposition observation simultaneously, realizes the kinetic experiment and hydrate continuous online microstructure observation research of hydrate method carbon dioxide separation under the condition of low energy consumption and simple operation.

[0006] The utility model realizes the purpose by the following technical scheme:

[0007] A hydrate method separates carbon dioxide in-situ detection device, including raman reactor, the raman reactor is equipped with liquid inlet, gas inlet, gas outlet, the gas outlet is connected with vacuum system, the gas inlet is connected with gas supply system, the raman reactor is also connected with temperature control system, monitoring system, the inner pot of the raman reactor is equipped with window glass, the window glass is equipped with glass pressing plate, the center of the glass pressing plate is equipped with the opening of the window glass, the raman reactor is equipped with the upper cover plate of the glass pressing plate, the glass pressing plate is equipped with fixing piece outside the opening, the fixing piece is equipped with monitoring camera, the monitoring camera is connected with the monitoring system.

[0008] Further, the gas supply system includes CH4 gas cylinder, CO2 gas cylinder, N2 gas cylinder, the CH4 gas cylinder, CO2 gas cylinder, N2 gas cylinder are connected with the gas inlet through branch pipeline connected main pipeline, the branch pipeline is equipped with branch regulating valve and pressure gauge.

[0009] Further, the vacuum system includes vacuum tank and vacuum pump connected with the gas outlet through pipeline.

[0010] Further, the fixing piece includes connection sleeve, expansion frame and support sleeve arranged from bottom to top, the connection sleeve is threadedly connected with the glass pressing plate, the size of the expansion frame gradually increases from the connection sleeve to the support sleeve, and the support sleeve is provided with a non-slip pad.

[0011] Further, the temperature control system includes high-low temperature constant temperature tank, and the high-low temperature constant temperature tank is connected with the jacket cavity of the raman reactor.

[0012] Further, the gas inlet is provided with a total regulating valve, the gas outlet is provided with an outlet valve, and the raman reactor is further connected with a temperature sensor.

[0013] Further, the raman reactor is relatively provided with an electric conductivity probe, and the probe of the electric conductivity probe is connected with the monitoring system through a time domain reflectometer.

[0014] The utility model has the following advantages:

[0015] The device can intuitively analyze hydrate dissolution-inducing nucleation and growth period kinetics curve, realize online microstructure monitoring and in-situ decomposition observation during hydrate generation process, provide important information for carbon dioxide separation kinetics and microstructure, the detection process is fast and direct, without offline sampling, and the hydrate static / dynamic generation kinetics process is not limited. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 It is the structural schematic diagram of the utility model.

[0017] Figure 2 For Figure 1 Partial sectional view of A-A plane.

[0018] In the figure, 1-Raman reactor, 2-liquid inlet, 3-gas inlet, 4-gas outlet, 5-monitoring system, 6-viewing glass, 7-glass pressing plate, 8-opening, 9-upper cover plate, 10-monitoring camera, 11-CH4 gas cylinder, 12-CO2 gas cylinder, 13-N2 gas cylinder, 14-vacuum tank, 15-vacuum pump, 16-high and low temperature constant temperature tank, 17-outlet valve, 18-temperature sensor, 19-connection sleeve, 20-expansion frame, 21-supporting sleeve, 22-conductivity probe, 23-time domain reflectometer. DETAILED DESCRIPTION

[0019] In order to make the purpose, technical scheme and advantages of the embodiments of the present application more clear, the technical scheme in the embodiments of the present application will be described clearly and completely below in combination with the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments of the present application. The components of the embodiments of the present application described and shown in the drawings herein can be arranged and designed in various different configurations.

[0020] Therefore, the following detailed description of the embodiments of the present application provided in the drawings is not intended to limit the scope of the claimed present application, but only represents selected embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without making creative efforts fall within the scope of protection of the present application.

[0021] It should be noted that the embodiments in the present application and the features in the embodiments can be combined with each other without conflict.

[0022] It should be noted that: similar reference numerals and letters represent similar items in the following drawings, therefore, once an item is defined in one drawing, it does not need to be further defined and explained in the subsequent drawings.

[0023] In the description of the utility model, it needs to explain that, the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, or the orientation or positional relationship commonly placed when the utility model product is used, or the orientation or positional relationship commonly understood by those skilled in the art, and is only for the convenience of describing the utility model and simplifying the description, and therefore cannot be understood as indicating or implying that the indicated device or element must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the utility model. In addition, the terms "first", "second" and the like are only used for differentiation in description and cannot be understood as indicating or implying relative importance.

[0024] In the description of the utility model, it also needs to explain that, unless otherwise explicitly specified and limited, the terms "arrangement", "installation", "connection", "connection" should be broadly understood, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected, it can be mechanically connected, or it can be electrically connected, it can be directly connected, or it can be indirectly connected through an intermediate medium, it can be the communication inside two elements. For ordinary skilled in the art, the specific meaning of the above terms in the utility model can be understood according to the specific circumstances.

[0025] Reference Figure 1 , 2 is shown, an embodiment of the utility model is:

[0026] A hydrate method separates carbon dioxide in-situ detection device, including raman reactor 1, the raman reactor is equipped with liquid inlet 2, gas inlet 3, gas outlet 4, the gas outlet 4 is connected with vacuum system, the gas inlet 3 is connected with gas supply system, the raman reactor 1 is also connected with temperature control system, monitoring system 5, the inner kettle body of the raman reactor 1 is equipped with window glass 6, the window glass 6 is equipped with glass pressing plate 7, the center of glass pressing plate 7 is equipped with the opening 8 of adaptation window glass, the raman reactor 1 is equipped with the upper cover plate 9 of adaptation glass pressing plate 7, the outside of opening 8 on glass pressing plate 7 is equipped with fixing piece, the monitoring camera 10 is equipped on the fixing piece, the monitoring camera 10 is connected with monitoring system 5.

[0027] Specifically, the upper cover plate 9 is clamped on the outside of the glass pressing plate 7 and is threadedly connected with the kettle body support, and, to ensure that the window glass is damaged under pressure, the upper and lower contact surfaces thereof are provided with buffer pads; in liquid delivery, a horizontal pump is used as a liquid delivery pump to realize accurate control of the suction amount, flow rate and other parameters of the reaction liquid, ensure that the reaction liquid enters the reaction pool at a constant rate and amount, and study the influence of liquid flow on the formation and dissociation process of hydrate.

[0028] The gas supply system comprises a CH4 gas cylinder 11, a CO2 gas cylinder 12, and a N2 gas cylinder 13, which are connected to the gas inlet through a branch pipe and a main pipe.

[0029] The vacuum system comprises a vacuum tank 14 and a vacuum pump 15 connected to the gas outlet 4 through a pipe.

[0030] The vacuum tank 14 and the vacuum pump 15 cooperate to extract gas from the system to achieve the required operation adjustment. In use, the vacuum state is extracted through the vacuum system to remove the non-condensable gas and moisture in the system, ensuring a pure environment for subsequent experiments. Subsequently, the CH4 gas cylinder, CO2 gas cylinder, N2 gas cylinder, and valve assembly are used to adjust the type and concentration of the gas into the system to meet the requirements of the experimental conditions.

[0031] The temperature control system comprises a high-low temperature constant-temperature tank 16 connected to the jacket cavity of the Raman reaction kettle 1.

[0032] The high-low temperature constant-temperature tank 16 stably maintains the temperature of the sample or system under different environments, ensuring that the reaction is carried out under constant temperature conditions, which is crucial for studying the influence of temperature on the formation and dissociation process of hydrates.

[0033] The gas inlet 3 is provided with a total adjusting valve, the gas outlet 4 is provided with an outlet valve 17, and the Raman reaction kettle 1 is further connected with a temperature sensor 18.

[0034] The total adjusting valve of the other inlet serves as a gas pressure measuring point of the system. By controlling and adjusting the gas flow and then introducing it into the reaction kettle, a high-pressure or low-pressure environment required for the experiment is realized, so as to study and analyze the influence of pressure on the formation and dissociation process of hydrates. The temperature sensor 18 is used to monitor the temperature of the system, providing a guarantee for the accuracy and reliability of experimental data and ensuring that the reaction operates within a safe range.

[0035] The monitoring camera is used to capture the transient process of hydrate formation and dissociation in the kettle, so as to analyze and adjust the operating state of the system.

[0036] The mixed gas is separated by the reaction kettle through continuous kinetics, and through the connection of a Raman spectrometer, a system, etc., the hydrate dissolution-induction nucleation and growth period kinetics curve is analyzed intuitively, the hydrate generation process is monitored online, and the in-situ decomposition observation is realized, which provides important information for the separation kinetics and microstructure of carbon dioxide. The detection process is fast and direct, without the need for offline sampling, and the static / dynamic generation kinetics process of hydrates is not limited.

[0037] Further, to ensure that the monitoring camera can stably capture image data of the reaction process during the reaction, the fixing member comprises a connecting sleeve 19, an expansion frame 20 and a supporting sleeve 21 arranged from bottom to top, the connecting sleeve 19 is threadedly connected with the glass pressing plate 7, the expansion frame 20 gradually increases in size from the connecting sleeve 19 to the supporting sleeve 21, and the supporting sleeve 21 is provided with an antiskid pad.

[0038] The expansion frame 20 is specifically a net frame plastic frame arranged oppositely, so as to facilitate adjustment of the monitoring visual angle of the camera.

[0039] In the embodiment, the Raman reaction kettle 1 is oppositely provided with a conductance probe 22, and a probe of the conductance probe 22 is connected with the monitoring system 5 through a time domain reflectometer 23.

[0040] When the hydrate is generated, thickened, or decomposed and thinned between the conductance probes 22, the resistance between the probes changes, the output signal collected also changes, the time domain reflectometer can judge the time experienced by the THF aqueous solution during the generation of the hydrate, and the change of the dielectric constant can be used to monitor the change of the water content in the THF aqueous solution during the generation of the hydrate in real time, and then the change of the hydrate saturation degree is calculated.

[0041] Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement to part of the technical features, and any modification, equivalent replacement, improvement, etc. within the spirit and principles of the utility model should be included in the protection scope of the utility model.

Claims

1. A hydrate process for separating carbon dioxide in situ detection device, characterized in that: The application relates to a Raman reactor, which comprises a Raman reactor, a liquid inlet, a gas inlet, a gas outlet, a vacuum system connected to the gas outlet, a gas supply system connected to the gas inlet, a temperature control system, a monitoring system, a window glass arranged on the inner reactor body of the Raman reactor, a glass pressing plate arranged on the window glass, an opening arranged in the center of the glass pressing plate and matched with the window glass, an upper cover plate arranged on the Raman reactor and matched with the glass pressing plate, a fixing member arranged on the glass pressing plate outside the opening, a monitoring camera arranged on the fixing member, and the monitoring camera being connected with the monitoring system.

2. The device for in-situ detection of carbon dioxide separated by a hydrate method according to claim 1, characterized in that: The gas supply system comprises a CH4 gas cylinder, a CO2 gas cylinder and an N2 gas cylinder, the CH4 gas cylinder, the CO2 gas cylinder and the N2 gas cylinder are connected with the gas inlet through a branch pipeline and a main pipeline, and branch regulating valves and pressure gauges are arranged on the branch pipeline.

3. The device for in-situ detection of carbon dioxide separated by a hydrate method according to claim 1, characterized in that: The vacuum system comprises a vacuum tank and a vacuum pump connected with the gas outlet through a pipeline.

4. The device for in-situ detection of carbon dioxide separated by a hydrate method according to claim 1, characterized in that: The fixing member comprises a connecting sleeve, an expansion frame and a supporting sleeve arranged from bottom to top, the connecting sleeve is threadedly connected with the glass pressing plate, the size of the expansion frame gradually increases from the connecting sleeve to the supporting sleeve, and an antiskid pad is arranged on the supporting sleeve.

5. The hydrate method in-situ detection device for separating carbon dioxide according to claim 1, characterized in that: The temperature control system comprises a high-low temperature constant temperature tank connected with the jacket cavity of the Raman reactor.

6. The hydrate method separation of carbon dioxide in-situ detection device according to claim 1, characterized in that: The gas inlet is provided with a total regulating valve, the gas outlet is provided with an outlet valve, and the Raman reactor is further provided with a temperature sensor.

7. The hydrate method separation of carbon dioxide in-situ detection device according to claim 1, characterized in that: An electric conductivity probe is oppositely arranged in the Raman reactor, and the probe head of the electric conductivity probe is connected with the monitoring system through a time domain reflectometer.

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