CN215640823U - Device for real-time in-situ monitoring and representation of micro-kinetic process of hydrate generation - Google Patents
Device for real-time in-situ monitoring and representation of micro-kinetic process of hydrate generation Download PDFInfo
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Abstract
The utility model provides a device for monitoring and characterizing a hydrate generation micro-dynamics process in real time and in situ, which comprises a reaction kettle system S2, wherein the reaction kettle system S2 is respectively connected with an online infrared spectrum detection system S1, a liquid automatic sampling device S3, a pressure control gas supply system S5, a vacuum system S6 and a data acquisition and processing system S7, and a precooling system S4 is arranged between the reaction kettle system S2 and the pressure control gas supply system S5. The spectrum change of molecules in a system before and after the generation of the hydrate can be monitored in real time and in situ from a molecular level: the probe of the online infrared spectrometer can be inserted into a solution, the change of a molecular infrared absorption peak in the solution is monitored and represented in real time, the understanding of the change of a substance structure and a composition of a guest molecule in the processes of dissolution, induction, nucleation and hydrate generation is deepened on a molecular level, and the influence of an additive on the processes is further improved.
Description
Technical Field
The utility model relates to an in-situ monitoring device, in particular to a device for monitoring and representing a micro-kinetic process of hydrate generation in real time in situ.
Background
The kinetic process of hydrate formation is similar to the crystallization process and is divided into two stages of nucleation and growth. Nucleation of hydrates refers to the process of forming stable hydrate nuclei reaching a critical size, which will enter the stable growth phase of hydrates after reaching the critical size. Because the hydrate needs to be generated and characterized in a low-temperature and high-pressure environment, the research method of the hydrate is limited. Currently, common hydrate characterization methods are XRD, RAMAN and NMR, and all of the methods need to generate hydrates in a reaction kettle and then transfer the hydrates to a low-temperature table for inspection. Due to the change of the surrounding environment in the sampling process, the decomposition of the hydrate or the transformation of the internal structure can be caused, and the in-situ characterization of the microstructure of the hydrate can not be realized. At present, the micro mechanism of the hydrate is researched by directly observing through a perspective window of a reaction kettle, and by using indirect variables such as macroscopic pressure, temperature, resistivity and the like, and by using methods such as computer simulation, theoretical calculation and the like. However, the visible window of the reaction kettle is generally made of resin glass, quartz glass or sapphire, which may mask the structural signal of the hydrate, weaken the laser intensity and the like. The device of the infrared sign gas hydrate of normal position of utility model patent CN 106680239A design generation and decomposition process needs the infrared cell body of normal position that the bilateral symmetry set up the zinc selenide window piece of customization, and is with high costs and operate complicacy. At present, the intuitive monitoring of the microscopic molecular activities of the growth of the hydrate is lacked, and particularly, the real-time and in-situ monitoring of the molecular change behaviors in the processes of guest molecule dissolution, induction, nucleation and hydrate generation is lacked. A Mizaikoff team uses a self-made mid-infrared optical fiber evanescent field absorption spectrum device to monitor a natural gas hydrate system, but the experimental device is complicated and needs to be operated in a dark fume hood so as to reduce fiber degradation caused by light to the maximum extent.
At present, hydrate experimental devices reported at home and abroad rarely work online with modern precise monitoring instruments, and high-precision guest molecule change behaviors are difficult to obtain in real time and in situ. In order to meet the research requirement in the hydrate field, a set of device and analysis method capable of monitoring the micro-kinetic process of the hydrate from a molecular level in real time and in situ is urgently needed.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the defects of the prior art and provide a device for monitoring and characterizing the micro-kinetic process of hydrate generation in real time and in situ. By monitoring the spectral change of system molecules and the change of temperature and pressure along with time in real time through an online infrared spectrum, the understanding of the dissolving, inducing, nucleating and hydrate generating/decomposing process mechanism of guest molecules can be deepened on the molecular level, and the influence mechanism of the additive on the hydrate generating dynamics can be further researched.
The utility model aims to provide a device for monitoring and characterizing the micro-kinetic process of hydrate generation in real time and in situ. The device can be used for monitoring and characterizing the spectrum change, the temperature and the pressure before and after molecules in the solution are converted into hydrates on line.
The utility model adopts a modern precise monitoring instrument, has high accuracy, can be directly combined with a normal-pressure and high-pressure reaction kettle, and does not need to customize a complex reaction kettle with a perspective window.
The utility model is realized by the following technical scheme:
a device for monitoring and representing a micro-kinetic process of hydrate generation in real time and in situ comprises a reaction kettle system S2, wherein the reaction kettle system S2 is respectively connected with an online infrared spectrum detection system S1, a liquid automatic sampling device S3, a precooling system S4, a pressure control gas supply system S5, a vacuum system S6 and a data acquisition and processing system S7, and the data acquisition and processing system S7 is respectively connected with the online infrared spectrum detection system S1 and the precooling system S4.
Further, the reaction kettle system S2 comprises a reaction kettle, a temperature sensor A and a pressure sensor A, wherein the temperature sensor A and the pressure sensor A are matched with the reaction kettle and can detect the temperature of the hydrate in the reaction kettle, and the pressure sensor A is arranged in the reaction kettle.
The reaction kettle adopts a quick-opening structure, the hoops are fastened, the high-pressure sealing requirement can be realized, a water bath jacket is arranged outside the kettle body, and the kettle is connected with a low-temperature constant-temperature water bath control device to control the temperature in the kettle, wherein the temperature range is-20-50 ℃, and the pressure-bearing range is 0-15 MPa. The reaction kettle cover is provided with mechanical stirring to promote the solution to be uniformly stirred and accelerate the generation of hydrate; the temperature sensor in the reaction kettle can accurately measure the temperature in the solution. The temperature sensor in the reaction kettle can accurately measure the temperature in the solution, and the measurement precision is 0.1 ℃. The pressure sensor connected to the reaction kettle measures the pressure in the reaction kettle, and the pressure measurement precision is 0.1 MPa. The top end of the reaction kettle is provided with a sample injection needle valve 18 which can be closed after sample injection is finished and is provided with a detachable bottom detection tube and a filter.
Further, the online infrared spectrum detection system S1 comprises an online infrared spectrometer and an ATR optical fiber probe detector connected with the online infrared spectrometer, wherein the optical fiber probe is made of diamond, the maximum withstand pressure is 69bar, the temperature range is-80-180 ℃, and the pH range is 0-14. The probe of the optical fiber probe detector 2 is connected with the reaction kettle through the adapter, inserted into the reaction kettle and positioned above the stirrer, so that the stirring paddle is prevented from impacting the probe.
Further, the liquid automatic sample feeding device S3 includes a liquid automatic sample feeder, which is disposed on the upper portion of the reaction kettle and is used for feeding liquid into the reaction kettle during high-pressure reaction, so as to prevent the liquid from being drawn out of the reaction kettle during vacuum pumping.
Further, the pressure control gas supply system S5 includes a gas cylinder capable of forming hydrate, and a pressure regulating valve on the gas cylinder, the pressure regulating valve is used for opening and closing the pipeline and regulating the pipeline pressure according to the target pressure, so as to provide stable gas.
Further, precooling system S4 include the cooling balance cauldron, and with the temperature sensor B that can detect the temperature in the cooling balance cauldron and the pressure sensor B who detects pressure that the cooling balance cauldron cooperation was used, the cooling balance cauldron entry end links to each other with the gas cylinder, sets up the needle valve between exit end and the reation kettle.
Furthermore, a water bath jacket A is arranged outside the reaction kettle, a water bath jacket B is arranged outside the cooling balance kettle, and the water bath jacket A and the water bath jacket B are connected with a low-temperature constant-temperature water bath control device.
And a sample precooling system is arranged between the reaction kettle and the gas cylinder and comprises a cooling balance kettle, a temperature sensor B and a pressure sensor B. The inlet end of the cooling balance kettle is connected with a gas cylinder of a pressure control gas supply system, precooled gas is added into the reaction kettle, and gas is prevented from carrying heat to enter the reaction kettle during gas injection, so that ice or hydrate is decomposed and infrared signals are influenced. The outlet end of the sample precooling system is connected with a reaction kettle of the reaction kettle system, and precooled gas is sent into the reaction kettle. The kettle body is externally provided with a water bath jacket B to maintain the low temperature state in the kettle, and a low temperature constant temperature water bath control device connected with the kettle controls the realization of the temperature.
Further, the vacuum system comprises a vacuum pump connected to the pipeline through a tee joint and used for vacuumizing the reaction kettle before reaction, eliminating the influence of impurity gases in the reaction kettle on infrared analysis and quickly exhausting after the reaction is finished.
Furthermore, the data acquisition and processing system is used for acquiring various data of temperature, pressure and infrared spectrum characteristic peaks of the sample on line for analysis.
Has the advantages that:
(1) by using the device, the spectral change of the system substance can be monitored and characterized in real time and in situ from the molecular level: the probe of the on-line infrared spectrometer can be inserted into a solution, the change of a molecular infrared absorption peak in the solution is monitored in real time, the understanding of the change of the material structure and the composition of the processes of guest molecule dissolution, induction, nucleation, hydrate generation/decomposition is deepened on the molecular level, and the influence of additives on the processes is further improved.
(2) The device for monitoring the generation/decomposition process of the hydrate by the online infrared spectrometer has high measurement precision.
(3) The monitoring technology of the utility model has good accuracy.
(4) The method is simple and convenient to operate, can realize on-line infrared continuous microcosmic characterization, does not need to take out a sample for detection, and avoids the defects of difficult sampling and sample transfer decomposition.
(5) The utility model has simple structure, does not need special treatment such as placing darkness and the like, and is convenient to control and maintain.
(6) The utility model has high repeatability.
Drawings
FIG. 1 is a system diagram of an apparatus;
FIG. 2 is a diagram of an apparatus for real-time, in situ monitoring and characterization of the micro-kinetic process of hydrate formation in accordance with the present invention;
in the figure: an online infrared spectrum detection system S1, a reaction kettle system S2, a liquid automatic sample feeding device S3, a precooling system S4, a pressure control gas supply system S5, a vacuum system S6 and a data acquisition and processing system S7;
1. an online infrared spectrometer; 2. a probe detector; 3. a reaction kettle; 4 water bath jacket A; 5. a stirrer; 6. a pressure sensor A; 7. a temperature sensor A; 8. a sampling pipe; 9. a low-temperature constant-temperature water bath control device; 10. a liquid automatic sample introduction device; 11. cooling the balance kettle; 12. a temperature sensor B; 13. a pressure sensor B; 14. a water bath jacket B; 15. a vacuum pump; 16. a pressure regulating valve; 17. a gas cylinder; 18. a needle valve.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A device for monitoring and representing a micro-kinetic process of hydrate generation in real time and in situ comprises a reaction kettle system S2 and is characterized in that the reaction kettle system S2 is respectively connected with an online infrared spectrum detection system S1, a liquid automatic sampling device S3, a precooling system S4, a pressure control gas supply system S5, a vacuum system S6 and a data acquisition and processing system S7, and the data acquisition and processing system S7 is respectively connected with an online infrared spectrum detection system S1 and a precooling system S4.
The reaction kettle system S2 comprises a reaction kettle 3, a temperature sensor A7 and a pressure sensor A6 which are matched with the reaction kettle and can detect the temperature of hydrate in the reaction kettle, and a stirrer 5 arranged in the reaction kettle. The reaction kettle adopts a quick-opening structure, the hoops are fastened, the high-pressure sealing requirement can be realized, a water bath jacket is arranged outside the kettle body, the temperature in the kettle can be controlled by connecting the low-temperature constant-temperature circulating water bath, the temperature range is-20-50 ℃, and the pressure-bearing range is 0-15 MPa. The reaction kettle cover is provided with mechanical stirring to promote the solution to be uniformly stirred and accelerate the generation of hydrate; the temperature sensor in the reaction kettle can accurately measure the temperature in the solution. The temperature sensor in the reaction kettle can accurately measure the temperature in the solution, and the measurement precision is 0.1 ℃. The pressure sensor connected to the reaction kettle measures the pressure in the reaction kettle, and the pressure measurement precision is 0.1 MPa. The top end of the reaction kettle is provided with a sample injection needle valve 18 which can be closed after sample injection is finished and is provided with a detachable bottom detection tube and a filter.
The online infrared spectrum detection system S1 comprises an online infrared spectrometer 1 and an optical fiber probe detector 2 connected with the online infrared spectrometer, wherein an ATR probe of the optical fiber probe detector 2 is connected with a reaction kettle 3 through an adapter, inserted into the reaction kettle and positioned above a stirrer 5, and the stirring paddle is prevented from impacting the probe.
The liquid automatic sample feeding device S3 comprises a liquid automatic sample feeder 10 arranged on the upper part of the reaction kettle 3 and used for adding liquid into the reaction kettle 10 during high-pressure reaction and avoiding the liquid being pumped out of the reaction kettle during vacuum pumping.
The pressure control gas supply system S5 comprises a gas cylinder 17 capable of forming hydrate and a pressure regulating valve 16 on the gas cylinder, wherein the pressure regulating valve is used for opening and closing a pipeline and regulating the pressure of the pipeline according to a target pressure to provide stable gas.
Precooling system S4 include cooling balance cauldron 11, and with cooling balance cauldron cooperation use can detect the temperature sensor B12 of temperature in the cooling balance cauldron and detect pressure sensor B13 of pressure, cooling balance cauldron entry end links to each other with gas cylinder 17, sets up needle valve 18 between exit end and reation kettle 3. The reaction kettle 3 is externally provided with a water bath jacket A4, the cooling balance kettle 11 is externally provided with a water bath jacket B14, and the water bath jacket A and the water bath jacket B are connected with a low-temperature constant-temperature water bath control device 9. The inlet end of the cooling balance kettle 11 is connected with a gas cylinder 17 of a pressure control gas supply system, precooled gas is added into the reaction kettle, and gas is prevented from carrying heat to enter the reaction kettle 3 during gas injection to cause the decomposition of ice or hydrate and influence infrared signals. The outlet end of the sample precooling system is connected with a reaction kettle 3 of the reaction kettle system, and precooled gas is sent into the reaction kettle 3. The kettle body is externally provided with a water bath jacket B to maintain the low temperature state in the kettle, and a low temperature constant temperature water bath control device connected with the kettle controls the realization of the temperature.
The vacuum system S6 comprises a vacuum pump 15 connected to the pipeline by a tee joint and is used for vacuumizing the reaction kettle before reaction, eliminating the influence of impurity gases in the reaction kettle on infrared analysis and quickly exhausting after the reaction is finished.
The data collecting and processing system S7 is used for collecting various data of temperature, pressure and infrared spectrum characteristic peak of the sample on line for analysis, and the collecting system here can be operated by using a computer.
The detection method of the device for monitoring the micro-kinetic process of hydrate generation in real time and in situ comprises the following steps:
take methane hydrate formation and decomposition as an example: the experimental procedure for generation was as follows:
1. firstly, checking whether the connection of all the devices such as pipelines, electrical appliances and the like is normal, and opening the on-line infrared spectrometer and the data acquisition and processing system.
2. Connecting the online infrared spectrometer and the optical fiber probe, and adding liquid nitrogen to cool the probe for 2-4 h.
3. And starting the low-temperature constant-temperature water bath device, starting a needle valve between the precooling system and the reaction kettle, and adjusting the temperature of the reaction kettle to the experimental target temperature.
4. Setting parameters of an online infrared spectrometer, collecting a background, and stably performing standby operation.
5. Before the experiment, the reaction kettle is cleaned and dried for standby.
6. And opening the vacuum pump and the valve, vacuumizing the reaction kettle, and closing the vacuum pump and the valve.
7. Preparing 5.6mol% THF aqueous solution, adding into the reaction kettle, sealing, ensuring the probe to be immersed into the solution, starting stirring to uniformly mix the solution, and stabilizing for 10min to reach the initial temperature.
8. And starting on-line infrared spectrometer monitoring software and a data acquisition and processing system, and recording and acquiring the molecular infrared spectrum, the temperature and the pressure in the generation process of the hydrate in the reaction kettle in real time through a computer.
9. And closing a needle valve at the joint of the precooling system and the reaction kettle, unscrewing a gas cylinder knob in the pressure control gas supply system, adjusting a pressure reducing valve to a target pressure, carrying out gas tightness inspection on each joint part, balancing and stabilizing for a period of time until a digital pressure gauge is stabilized, and precooling the gas to a target temperature.
10. Opening a needle valve of the precooling system, slowly introducing the precooled gas into the reaction kettle for three times until air in the kettle is exhausted, then pressurizing to 50bar, closing an air inlet of the reaction kettle, and reducing the temperature of the constant-temperature circulating water bath to 2 ℃ after the reaction system is stabilized to generate the hydrate.
11. In the hydrate generation process, the online infrared spectrometer collects data every 1 minute, and continuous change information of the molecular infrared absorption peak in the whole hydrate generation process can be obtained. 1041cm-1The peak was ascribed to an asymmetric absorption peak of C-O-C in THF, and the peak was slowly changed to 1040cm-1And 1050 cm-1Acromion, induced and nucleated 1040cm-1The peak absorbance gradually decreased, 1070 cm-1A new peak appeared representing the characteristic peak of THF occupying the large cage of hydrate, with a sudden temperature rise, indicating hydrate formation.
12. After the temperature, the pressure and the absorbance of the infrared absorption peak in the reaction kettle reach stability, the generation of the hydrate is finished, the data acquisition and processing system is closed, and THF-CH is obtained4An online infrared spectrum in the formation process of the mixed hydrate.
13. The temperature is raised by using a program of constant-temperature circulating water bath, the required temperature is set, the hydrate is decomposed, and the change information of the material structure can be obtained by collecting an online infrared spectrogram, temperature and pressure data in the decomposition process.
Claims (4)
1. A device for real-time in-situ monitoring and characterization of a micro-kinetic process of hydrate generation comprises a reaction kettle system S2 and is characterized in that the reaction kettle system S2 is respectively connected with an online infrared spectrum detection system S1, a liquid automatic sampling device S3, a precooling system S4, a pressure control gas supply system S5, a vacuum system S6 and a data acquisition and processing system S7, and the data acquisition and processing system S7 is respectively connected with an online infrared spectrum detection system S1 and a precooling system S4;
the reaction kettle system S2 comprises a reaction kettle (3), a temperature sensor A (7) and a pressure sensor A (6), wherein the temperature sensor A (7) and the pressure sensor A (6) are matched with the reaction kettle and can detect the temperature of hydrate in the reaction kettle, and a stirrer (5) is arranged in the reaction kettle;
the on-line infrared spectrum detection system S1 comprises an on-line infrared spectrometer (1) and an optical fiber probe detector (2) connected with the on-line infrared spectrometer, wherein a probe of the optical fiber probe detector (2) is connected with a reaction kettle (3) through an adapter, inserted into the reaction kettle and positioned above a stirrer (5);
the liquid automatic sample feeding device S3 comprises a liquid automatic sample feeder (10) which is arranged at the upper part of the reaction kettle (3) and is used for feeding liquid into the reaction kettle (3) during high-pressure reaction;
the pressure control gas supply system S5 comprises a gas cylinder (17) capable of forming hydrate and a pressure regulating valve (16) on the gas cylinder;
precooling system S4 include cooling balance cauldron (11), and with temperature sensor B (12) and pressure sensor B (13) of detection pressure that cooling balance cauldron cooperation was used can detect the temperature in the cooling balance cauldron, the cooling balance cauldron entry end links to each other with gas cylinder (17), the exit end links to each other with reation kettle (3).
2. The device for real-time in-situ monitoring and characterization of the micro-kinetic process of hydrate formation according to claim 1, characterized in that the reaction kettle (3) is externally provided with a water bath jacket A (4), the cooling equilibration kettle (11) is externally provided with a water bath jacket B, and the water bath jacket A and the water bath jacket B are connected with a low-temperature constant-temperature water bath control device (9).
3. A device for real-time, in situ monitoring and characterization of hydrate formation micro-kinetics as claimed in claim 1, wherein the vacuum system S6 includes a vacuum pump (15).
4. A device for real-time, in-situ monitoring and characterization of hydrate formation micro-kinetic processes according to claim 1, characterized in that the reaction vessel (3) is provided with a sampling pipe (8).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023279859A1 (en) * | 2021-07-09 | 2023-01-12 | 齐鲁工业大学 | Device for monitoring gas hydrate generation and decomposition process at molecular level in-situ by using online infrared spectrometer, and use method of same |
| CN117213642A (en) * | 2023-10-17 | 2023-12-12 | 江苏大学 | Hydrate nucleation phase transition temperature test system and method based on infrared imaging |
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2021
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023279859A1 (en) * | 2021-07-09 | 2023-01-12 | 齐鲁工业大学 | Device for monitoring gas hydrate generation and decomposition process at molecular level in-situ by using online infrared spectrometer, and use method of same |
| CN117213642A (en) * | 2023-10-17 | 2023-12-12 | 江苏大学 | Hydrate nucleation phase transition temperature test system and method based on infrared imaging |
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