Coal thermal conversion process in-situ detection system and detection method

Abstract

The invention discloses a coal thermal conversion process in-situ detection system and a detection method.The coal thermal conversion process in-situ detection system comprises a gas distribution module, a feeding module, a reaction module, a gas-solid product separation and collection module and an in-situ analysis and detection module; the reaction module comprises a reaction device and a reaction cavity arranged in the reaction device, the side wall of the reaction device is provided with a first visible window and a second visible window, and the side wall of the reaction cavity is provided with a third visible window and a fourth visible window; the in-situ analysis and detection module comprises a planar laser-induced fluorescence measurement system and the like. According to the application, the planar laser-induced fluorescence measurement system is combined with the reaction device with the visual window and the like, so that in-situ detection of form changes of gas-phase products, intermediate reaction free radicals and solid-phase products generated in coal pyrolysis, coal gasification and coal combustion processes is realized for the first time; and a new means is provided for explaining the intrinsic reaction mechanism of the coal thermal conversion process.

Description

Technical Field

[0001] This application belongs to the field of in-situ detection systems for coal thermal conversion processes, specifically relating to an in-situ detection system and method for coal thermal conversion processes. Background Technology

[0002] The thermal conversion of coal mainly includes processes such as pyrolysis, gasification, and combustion. Most existing research on coal thermal conversion is based on kinetic inferences and modeling based on macroscopic temperature, pressure, and products. The established thermal conversion process mechanisms and operating strategies lack in-depth and specific process theory support, and lack the detection, prediction, and process reconstruction of fine intermediate products in the reaction process.

[0003] Currently, research on the precise and controllable thermal conversion process of coal has become a key direction in the field of energy science and engineering. In-depth research into the intrinsic reaction mechanisms of coal thermal conversion processes helps to achieve precise control over processes such as coal pyrolysis, gasification, and combustion. This can improve energy utilization efficiency, reduce pollutant emissions, and better promote the efficient and clean utilization of coal. However, currently, there are no reports on in-situ detection systems suitable for explaining the intrinsic reaction mechanisms of coal thermal conversion processes. Summary of the Invention

[0004] This application aims to at least partially address one of the technical problems in related technologies. Therefore, the purpose of this application is to propose an in-situ detection system and method for coal thermal conversion processes. This in-situ detection system for coal thermal conversion processes accurately detects intermediate products in different reaction processes (pyrolysis, gasification, and combustion) during coal thermal conversion, thereby establishing a detailed and intrinsic reaction mechanism, reconstructing and predicting the evolution of products during coal thermal conversion. By combining a planar laser-induced fluorescence measurement system with a reaction device featuring a viewing window, this system achieves, for the first time, in-situ detection of the morphological changes of gaseous products, intermediate reaction free radicals, and solid products generated during coal pyrolysis, coal gasification, and coal combustion. This provides a new means for explaining the intrinsic reaction mechanism of coal thermal conversion processes and has broad application prospects.

[0005] The first aspect of this application discloses an in-situ detection system for coal thermal conversion processes. According to an embodiment of this application, the in-situ detection system for coal thermal conversion processes includes a gas distribution module, a feeding module, a reaction module, a gas-solid product separation and collection module, and an in-situ analysis and detection module; The reaction module includes a reaction device and a reaction chamber disposed inside the reaction device. A first viewing window and a second viewing window are provided on the side wall of the reaction device, and a third viewing window and a fourth viewing window are provided on the side wall of the reaction chamber. The in-situ analysis and detection module includes a planar laser-induced fluorescence measurement system and an image acquisition device connected to the planar laser-induced fluorescence measurement system. The planar laser-induced fluorescence measurement system includes a laser. The emitted light of the laser passes through the first viewing window and the third viewing window in sequence to induce the luminescence imaging of intermediate reactant species in the reaction chamber. The image acquisition device captures the luminescence image of the intermediate reactant species through the second viewing window and the fourth viewing window. The gas distribution module and the feeding module are both connected to the inlet end of the reaction device, and the gas-solid product separation and collection module is connected to the outlet end of the reaction device.

[0006] The in-situ detection system for coal thermal conversion processes described in the above embodiments of this application enables precise in-situ detection of intermediate products during different reaction processes (pyrolysis, gasification, and combustion) of coal thermal conversion. This allows for the establishment of detailed and intrinsic reaction mechanisms, the reconstruction and prediction of product evolution during coal thermal conversion, and the first-ever in-situ detection of morphological changes in gaseous products, intermediate reaction free radicals, and solid products generated during coal pyrolysis, coal gasification, and coal combustion. This provides a new means for explaining the intrinsic reaction mechanisms of coal thermal conversion processes and has broad application prospects.

[0007] In addition, the in-situ detection system for the coal thermal conversion process according to the above embodiments of this application may also have the following additional technical features: In some embodiments of this application, the first and second view windows are both circular in shape, and the third and fourth view windows are both rectangular in shape. The length of the short side of the rectangle is not less than the diameter of the circle, and the length of the long side of the rectangle is 2 to 3 times the diameter of the circle.

[0008] In some embodiments of this application, the first view window, the second view window, the third view window, and the fourth view window located at the same vertical height are regarded as a group of view window units, and the number of groups of view window units is not less than 2 groups, and the vertical spacing between adjacent view window units on the sidewall is equal.

[0009] In some embodiments of this application, the reaction apparatus includes a settling furnace connected to a temperature control device. The length of the constant temperature zone of the settling furnace in the vertical direction is equal to the length of the viewing window unit in the vertical direction. The length of the constant temperature zone is 1000~1200 mm, and the operating temperature of the settling furnace is ≤1600℃. The reaction chamber includes a circular tube, and the viewing window on the circular tube is provided with sapphire tube sealing sections on its surrounding side walls.

[0010] In some embodiments of this application, the gas distribution module includes a gas source delivery pipeline and a pressure reducing valve and a mass flow meter disposed on the gas source delivery pipeline; The gas source delivery pipeline includes a first inert gas delivery pipeline, a second inert gas delivery pipeline, an oxygen / hydrogen delivery pipeline, and a carbon dioxide / carbon monoxide delivery pipeline. The second inert gas delivery pipeline, the oxygen / hydrogen delivery pipeline, and the carbon dioxide / carbon monoxide delivery pipeline are sequentially connected to a gas mixing device and a steam generator. The steam generator is connected to the inlet of the reaction device via a constant temperature pipeline, and the steam generator is also connected to a water tank via a pump.

[0011] In some embodiments of this application, the feeding module includes a powder feeding device, which is connected to the inlet end of the reaction device via a feeding pipe. The feeding pipe is also connected to the first inert gas conveying pipe, and the feeding pipe is provided with a first cooling water inlet and a first cooling water outlet.

[0012] In some embodiments of this application, the gas-solid product separation and collection module includes a sampling tube, the two ends of which are connected to the reaction chamber and the solid product collection device, respectively. The solid product collector is connected in sequence to a filtration device and a vacuum device. The sampling tube is provided with a second cooling water inlet and a second cooling water outlet. The length of the sampling tube is 1000-1500 mm. The reaction chamber is formed by assembling a corundum tube and a sapphire.

[0013] In some embodiments of this application, the in-situ analysis and detection module further includes an online gas analysis device and a central control device. The online gas analysis device is connected to the exhaust outlet of the gas extraction device, and the central control device is connected to the online gas analysis device and the image acquisition device.

[0014] The second aspect of this application proposes an in-situ detection method for coal thermal conversion processes. According to embodiments of this application, the in-situ detection method employs the coal thermal conversion process in-situ detection system described in any one of the first aspects above. Therefore, this detection method can accurately detect the intermediate products of different reaction processes in coal thermal conversion (pyrolysis, gasification, combustion processes) in situ, thereby establishing a detailed and intrinsic reaction mechanism, and reconstructing and predicting the evolution of products during coal thermal conversion.

[0015] In addition, the in-situ detection method for the coal thermal conversion process according to the above embodiments of this application may also have the following additional technical features: In some embodiments of this application, the detection targets include continuous online detection of gaseous products generated during coal pyrolysis, coal gasification, and coal combustion processes, continuous online detection of intermediate reaction free radicals, and continuous online detection of changes in the morphology of solid products.

[0016] Additional aspects and advantages of this application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of this application. Attached Figure Description

[0017] The above and / or additional aspects and advantages of this application will become apparent and readily understood from the description of the embodiments taken in conjunction with the following drawings, in which: Figure 1 This is a schematic diagram of the in-situ detection system for the coal thermal conversion process in an embodiment of this application.

[0018] Figure 2 This is a partial structural schematic diagram of the reaction device in the in-situ detection system for the coal thermal conversion process in the embodiments of this application.

[0019] Figure 3 This is a partial structural diagram of the reaction chamber in the in-situ detection system for the coal thermal conversion process in this embodiment of the application.

[0020] Figure label: 1-First inert gas conveying pipeline, 2-Second inert gas conveying pipeline, 3-Oxygen / hydrogen conveying pipeline, 4-Carbon dioxide / carbon monoxide conveying pipeline, 5-Pressure reducing valve, 6-Mass flow meter, 7-Gas mixing device, 8-Steam generator, 9-Pump, 10-Water tank, 11-Thermostatic pipeline, 12-Powder feeding device, 13-Feeding pipe, 14-First cooling water inlet, 15-First cooling water outlet, 16-Reaction device, 17-Reaction chamber, 18-Temperature control device 19-Sampling tube, 20-Second cooling water inlet, 21-Second cooling water outlet, 22-Solid phase product collection device, 23-Filter device, 24-Gas extraction device, 25-Exhaust outlet, 26-Online gas analysis device, 27-Image acquisition device, 28-Planar laser-induced fluorescence measurement system, 29-Central control device, 30-First viewing window, 31-Second viewing window, 32-Third viewing window, 33-Fourth viewing window, 34-Sapphire tube sealing section. Detailed Implementation

[0021] The embodiments of this application are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and intended to explain this application, and should not be construed as limiting this application.

[0022] The first aspect of this application discloses an in-situ detection system for coal thermal conversion processes. According to embodiments of this application, such as... Figure 1 , Figure 2 and Figure 3 As shown, the in-situ detection system for the coal thermal conversion process includes a gas distribution module, a feeding module, a reaction module, a gas-solid product separation and collection module, and an in-situ analysis and detection module. The reaction module includes a reaction device 16 and a reaction chamber 17 disposed inside the reaction device 16. A first viewing window 30 and a second viewing window 31 are provided on the side wall of the reaction device 16, and a third viewing window 32 and a fourth viewing window 33 are provided on the side wall of the reaction chamber 17. The in-situ analysis and detection module includes a planar laser-induced fluorescence measurement system 28 and an image acquisition device 27 connected to the planar laser-induced fluorescence measurement system 28. The planar laser-induced fluorescence measurement system 28 includes a laser (the laser is a component of the planar laser-induced fluorescence measurement system 28 and is not shown in the figure). The emitted light of the laser passes through the first viewing window 30 and the third viewing window 32 in sequence to induce the intermediate reaction species (such as free groups such as OH and CH) in the reaction chamber 17 to emit light and form images. The image acquisition device 27 captures the emission images of the intermediate reaction species through the second viewing window 31 and the fourth viewing window 33. The gas distribution module and the feeding module are both connected to the inlet end of the reaction device 16, and the gas-solid product separation and collection module is connected to the outlet end of the reaction device 16.

[0023] Currently, the coal thermal conversion process is like a "black box" waiting to be opened. Under the existing technological framework, the coal thermal conversion process mainly relies on inputting specific parameters to obtain corresponding output results. However, how this process evolves step by step, that is, how the intermediate processes occur, has not yet been fully revealed.

[0024] Current online detection of coal thermal conversion mainly relies on online mass spectrometry, which infers molecular structure by detecting molecular weight, thereby predicting the formation of intermediate products during the reaction. However, most existing research focuses on fixed-bed reactors, where the reaction process employs programmed temperature increases. This approach deviates to some extent from the actual coal thermal conversion process and cannot accurately reflect the true situation during coal thermal conversion.

[0025] The in-situ detection system for coal thermal conversion processes described in the above embodiments of this application enables precise in-situ detection of intermediate products during different reaction processes (pyrolysis, gasification, and combustion) of coal thermal conversion. Based on this, a detailed and intrinsic reaction mechanism is established, and the evolution of products during coal thermal conversion is reconstructed and predicted. By combining a planar laser-induced fluorescence measurement system with a reaction device featuring a viewing window, this system achieves, for the first time, in-situ detection of the morphological changes of gaseous products, intermediate reaction free radicals, and solid products generated during coal pyrolysis, coal gasification, and coal combustion. This provides a new means for explaining the intrinsic reaction mechanism of coal thermal conversion processes and has broad application prospects.

[0026] Furthermore, the aforementioned gas distribution module can be used to provide different gas atmospheres, such as oxidizing atmospheres, reducing atmospheres, and inert atmospheres, according to the actual gas atmosphere required in the coal thermal conversion process; the aforementioned feeding module can provide continuous, stable, and precise feeding according to the actual material required in the coal thermal conversion process; the aforementioned reaction module provides the reaction site for the coal thermal conversion process, realizing the coal thermal conversion of the material conveyed by the feeding module under the gas atmosphere provided by the gas distribution module, and realizing the separation of gas and solid products through the gas-solid product separation and collection module, and in-situ detection and analysis through the in-situ analysis and detection module.

[0027] In an embodiment of the present application, the above-mentioned planar laser-induced fluorescence measurement system (abbreviated as PLIF system) is an analytical instrument based on the principle of laser-induced fluorescence. Existing devices such as ZOLIX / Zhuoli Hanguang, WK-OPTICS / WK-OPTICSPLIF-80, etc. can be directly used. The laser emits high-frequency laser, which passes through the visual windows on the same side of the reaction device and the reaction chamber to induce the luminescence imaging of free radical groups such as OH and CH in the reaction atmosphere in the reaction chamber. In addition, the image acquisition device can use existing devices such as existing high-speed and high-resolution cameras (or the image acquisition device自带的图像采集装置 in the planar laser-induced fluorescence measurement system) to take PLIF images through the visual window, analyze the PLIF images at different reaction positions, and obtain the evolution law of relevant reactions at different reaction times. In addition, when setting the visual windows (including the third visual window 32 and the fourth visual window 33) on the side wall of the reaction chamber 17, corresponding openings can be set according to the visual windows (including the first visual window 30 and the second visual window 31) on the side wall of the reaction device 16, ensuring that the emitted light of the laser can sequentially pass through the first visual window 30 and the third visual window 32 to induce the luminescence imaging of intermediate reaction species in the reaction chamber 17 and at the same time enabling the image acquisition device 27 to take the luminescence images of the intermediate reaction species through the second visual window 31 and the fourth visual window 33. For example, the first visual window 30 and the third visual window 31 can be set at 90° on the side wall of the reaction device 16. Correspondingly, the third visual window 32 and the fourth visual window 33 are also set at 90° on the side wall of the reaction chamber 17, and when the first visual window 30 and the third visual window 32 approach each other in the horizontal direction, they at least partially overlap or completely overlap, and when the second visual window 31 and the fourth visual window 33 approach each other in the horizontal direction, they also at least partially overlap or completely overlap.

[0028] It should be noted that the part "自带的图像采集装置" in the original text seems to be an incorrect expression. I translated it as "自带的图像采集装置" for the purpose of keeping the translation consistent with the original text as much as possible. It might need to be corrected in the original content.According to some specific embodiments of this application, the first viewing window 30 and the second viewing window 31 are both circular (or square, for example, the diameter of the circular opening or the side length of the square opening is 30-50 mm, and the height is 1000-1200 mm). The third viewing window 32 and the fourth viewing window 33 are both rectangular (for example, a rectangular strip with a width of 30-50 mm and a height of 1000-1200 mm). The length of the short side of the rectangle is not less than the diameter of the circle, and the length of the long side of the rectangle is 2-3 times the diameter of the circle. This allows the viewing windows (including the third viewing window 32 and the fourth viewing window 33) on the side wall of the reaction chamber 17 to completely cover the viewing windows (including the first viewing window 30 and the second viewing window 31) on the side wall of the reaction device 16. At the same time, it avoids the problem that the viewing windows of the reaction device 16 and the reaction chamber 17 cannot correspond due to the thermal expansion of the reaction chamber 17 during the heating process. This is beneficial for the image acquisition device to more easily capture PLIF images (i.e., real-time emission images of free radicals) through the other viewing window when using a planar laser-induced fluorescence measurement system to induce the emission of free radicals such as OH and CH in the reaction atmosphere of the reaction chamber through the viewing window on one side.

[0029] According to some specific embodiments of this application, the first view window 30, the second view window 31, the third view window 32, and the fourth view window 33, located at the same vertical height, are considered as a group of view window units, and the number of groups of view window units is not less than 2 (e.g., Figure 2 and Figure 3 (The diagram shows 4 groups, evenly spaced from top to bottom), and the vertical spacing between adjacent view window units on the sidewall is equal.

[0030] According to some specific embodiments of this application, the reaction apparatus 16 includes a settling furnace connected to a temperature control device 18. The length of the constant temperature zone of the settling furnace in the vertical direction is equal to the length of the viewing window unit in the vertical direction. The length of the constant temperature zone is 1000~1200 mm, and the operating temperature of the settling furnace is ≤1600℃. The reaction chamber includes a circular tube (e.g., a corundum tube). The viewing window on the circular tube is provided with sapphire tube sealing sections 34 on its surrounding sidewalls (similarly, the viewing window of the settling furnace body can be sealed with a transparent quartz sheet to ensure the sealing of the reaction). Thus, the position and height range of the viewing window correspond to the position and length of the effective constant temperature zone of the reaction apparatus such as the settling furnace. At the same time, the detection system provided by this application can realize in-situ detection of thermal conversion processes (pyrolysis, gasification, combustion) at reaction temperatures of 1600℃ and below, including continuous online detection of gaseous products, detection of intermediate reaction free radicals, and morphological changes of solid products. Specifically, the aforementioned settling furnace can directly adopt existing settling furnaces with viewing windows, such as AZ-GWL-105 and STGLC-60-17.

[0031] According to some specific embodiments of this application, the gas distribution module includes a gas source delivery pipeline and a pressure reducing valve 5 and a mass flow meter 6 disposed on the gas source delivery pipeline; The gas source delivery pipeline includes a first inert gas delivery pipeline 1, a second inert gas delivery pipeline 2, an oxygen / hydrogen delivery pipeline 3, and a carbon dioxide / carbon monoxide delivery pipeline 4. The second inert gas delivery pipeline 2, the oxygen / hydrogen delivery pipeline 3, and the carbon dioxide / carbon monoxide delivery pipeline 4 are sequentially connected to a gas mixing device 7 and a steam generator 8. The steam generator 8 is connected to the inlet of the reaction device 16 via a constant temperature pipeline 11, and is also connected to a water tank 10 via a pump 9. Thus, the gas distribution module, through the gas source, pressure reducing valve 5, mass flow meter 6, and steam generator 8, can configure oxidizing atmospheres, reducing atmospheres, and inert atmospheres of different gas combinations and concentrations according to the gas combination used and the adjustment of each mass flow meter. At the same time, the steam generator 8 in the gas distribution module can provide steam at different flow rates for gas distribution.

[0032] According to some specific embodiments of this application, the feeding module includes a powder feeding device 12, which is connected to the inlet end of the reaction device 16 via a feeding pipe 13. The feeding pipe 13 is also connected to the first inert gas conveying pipe 1, and the feeding pipe 13 is provided with a first cooling water inlet 14 and a first cooling water outlet 15. Thus, the feeding module, through the powder feeding device 12, feeding pipe 13, etc., can achieve continuous, stable, and precise feeding of 0.5 ~ 10 g / min. The fed material is mixed with the gas through the cold feeding pipe 13 and enters the reaction device such as a settling furnace with a viewing window. The feeding pipe 13 can be an existing water / oil-cooled feeding pipe, etc., and the powder feeding device can be existing equipment such as a micro-powder feeder.

[0033] According to some specific embodiments of this application, the gas-solid product separation and collection module includes a sampling tube 19, with both ends of the sampling tube 19 connected to the reaction chamber 17 and the solid product collection device 22, respectively. The solid product collector is sequentially connected to a filter device 23 and a vacuum pump 24. The sampling tube 19 is provided with a second cooling water inlet 20 and a second cooling water outlet 21. The length of the sampling tube 19 is 1000-1500 mm. The reaction chamber 17 is formed by assembling a corundum tube and a sapphire. Thus, the gas-solid separation and collection module realizes the separation and collection of gas-solid products through the arrangement of the sampling tube 19 (such as a water / oil-cooled sampling tube), the solid product collection device 22, the filter device 23, and the vacuum pump 24 (such as a vacuum pump). The water / oil-cooled sampling tube is 1000-1500 mm long and can be used for a long time at temperatures of 1600 ℃ and below. The water / oil-cooled sampling tube is inserted into the bottom of the corundum tube and sapphire assembled reactor with a viewing window. The effective reaction zone in the isothermal reaction zone can be adjusted according to the insertion depth. The adjustable range of the effective reaction zone is 100-1200 mm. The solid phase collector, filter, and vacuum pump are all common existing experimental equipment.

[0034] According to some specific embodiments of this application, the in-situ analysis and detection module further includes an online gas analysis device 26 and a central control device 29, such as a computer. The online gas analysis device 26 is connected to the exhaust outlet 25 of the gas extraction device 24, and the central control device 29 is connected to the online gas analysis device 26 and the image acquisition device 27. Thus, the in-situ analysis and testing module includes an online gas analysis device 26, a planar laser-induced fluorescence (PLIF) testing system 28, etc., wherein the online gas analysis mass spectrometer is connected to the water / oil-cooled sampling tube in the gas-solid separation and collection module, and can directly and continuously test the gas composition and concentration at different reaction times in the isothermal reaction zone online. PLIF is a non-contact optical measurement and diagnostic method that uses a high-frequency laser to induce the emission of free radicals such as OH and CH in the reaction atmosphere within the reactor through a viewing window on the same side of the furnace and reactor. Simultaneously, a high-speed, high-resolution camera captures PLIF images through a viewing window on the other side, and by analyzing PLIF images at different reaction locations, the evolution patterns of the relevant reactions at different reaction times can be obtained.

[0035] The second aspect of this application proposes an in-situ detection method for coal thermal conversion processes. According to embodiments of this application, the in-situ detection method employs the coal thermal conversion process in-situ detection system described in any one of the first aspects above. Therefore, this detection method can accurately detect the intermediate products of different reaction processes in coal thermal conversion (pyrolysis, gasification, combustion processes) in situ, thereby establishing a detailed and intrinsic reaction mechanism, and reconstructing and predicting the evolution of products during coal thermal conversion.

[0036] According to some further specific embodiments of this application, the in-situ detection system for the coal thermal conversion process according to the above embodiments of this application may also have the following additional technical features: According to some specific embodiments of this application, the detection targets include continuous online detection of gaseous products generated during coal pyrolysis, coal gasification, and coal combustion processes, continuous online detection of intermediate reaction free radicals, and continuous online detection of changes in the morphology of solid products.

[0037] According to some specific embodiments of this application, when operating the in-situ detection system for the coal thermal conversion process described in any one of the first aspects above, the following steps are included: 1) Start the cooling water / oil system, including the water / oil cooled feed pipe and the water / oil cooled sampling pipe.

[0038] 2) Start the electric furnace and heat it up to the required reaction temperature according to the program.

[0039] 3) When the furnace temperature reaches the required reaction temperature, turn on the gas distribution system and adjust the gas combination and mass flow meter opening of the gas distribution system to achieve the reaction gas atmosphere required for the specific experiment.

[0040] 4) Once the reaction temperature and reaction atmosphere meet the experimental requirements, after stabilizing for 3 to 5 minutes, turn on the feeding system. By adjusting the speed of the micro-feeder, different feeding amounts can be achieved.

[0041] 5) After the feeding has stabilized for 3 to 5 minutes, the experimental conditions are basically stable, and the corresponding in-situ detection begins.

[0042] Furthermore, the in-situ detection includes an online gas analysis mass spectrometer and a planar laser-induced fluorescence (PLIF) testing system. The online gas analysis mass spectrometer is connected to a water / oil-cooled sampling tube. By adjusting the insertion depth of the water / oil-cooled sampling tube, the distribution and changes of gaseous products at different reaction times can be continuously detected online. Simultaneously, according to the arrangement of the viewing window, during the stable experimental conditions, the incident high-frequency laser on one side and the high-resolution camera on the other side are adjusted synchronously from top to bottom to continuously detect the distribution and changes of free radicals such as OH and CH at different reaction times online.

[0043] Furthermore, the electric furnace has an adjustable reaction temperature range from room temperature to 1600 °C.

[0044] Furthermore, the gas distribution system can achieve a combination of one or more gases, including but not limited to: nitrogen, oxygen, argon, hydrogen, carbon dioxide, carbon monoxide, and water vapor.

[0045] Furthermore, the gas flow rate of the gas distribution system is 0 ~ 5 L / min for a single channel and 0 ~ 20 L / min for the total gas flow rate.

[0046] The embodiments of this application are described in detail below. It should be noted that the embodiments described below are exemplary and are only used to explain this application, and should not be construed as limiting this application. In addition, unless otherwise specified, all reagents used in the following embodiments are commercially available or can be synthesized according to the methods described herein or known methods. For reaction conditions not listed, they are also readily available to those skilled in the art.

[0047] Example This embodiment provides an in-situ detection system for the thermal conversion process of coal, such as... Figure 1 , Figure 2 and Figure 3As shown, it mainly includes a gas distribution module (such as a first inert gas conveying pipeline 1, a second inert gas conveying pipeline 2, such as nitrogen, an oxygen / hydrogen conveying pipeline 3, and a carbon dioxide / carbon monoxide conveying pipeline 4, a pressure reducing valve 5, a mass flow meter 6, a gas mixing device 7, a steam generator 8, a pump such as a peristaltic pump 9, a water tank 10, and a constant temperature pipeline 11), a feeding module (such as a micro-feeder and a feeding pipe such as a water / oil-cooled feeding pipe 13), and a settling furnace with a viewing window. The system comprises a reaction module (consisting of a reaction device 16 such as a settling furnace with a viewing window, a reaction chamber 17 such as a corundum tube and sapphire assembled reactor with a viewing window, and a temperature control device 18 such as a temperature control box), a gas-solid separation and collection module (including a sampling tube 19 such as a water / oil-cooled sampling tube, a solid product collection device 22, a filtration device 23, and a gas extraction device 24 such as a gas pump), and an in-situ analysis and testing module (including an online gas analysis device 26, an image acquisition device 27, and a planar laser-induced fluorescence measurement system 28).

[0048] Specifically, the reaction module includes a reaction device 16 and a reaction chamber 17 disposed inside the reaction device 16. A first viewing window 30 and a second viewing window 31 are provided on the side wall of the reaction device 16, and a third viewing window 32 and a fourth viewing window 33 are provided on the side wall of the reaction chamber 17. The in-situ analysis and detection module includes a planar laser-induced fluorescence measurement system 28 and an image acquisition device 27 connected to the planar laser-induced fluorescence measurement system 28. The planar laser-induced fluorescence measurement system 28 includes a laser. The emitted light of the laser passes through the first viewing window 30 and the third viewing window 32 in sequence to induce the intermediate reaction species (such as free groups such as OH and CH) in the reaction chamber 17 to emit light and form images. The image acquisition device 27 captures the emission images of the intermediate reaction species through the second viewing window 31 and the fourth viewing window 33. The gas distribution module and the feeding module are both connected to the inlet end of the reaction device 16, and the gas-solid product separation and collection module is connected to the outlet end of the reaction device 16.

[0049] Furthermore, the first viewport 30 and the second viewport 31 are both circular in shape, and the third viewport 32 and the fourth viewport 33 are both rectangular in shape. The shorter side of the rectangle is not less than the diameter of the circle, and the longer side of the rectangle is 2 to 3 times the diameter of the circle. The first viewport 30, the second viewport 31, the third viewport 32, and the fourth viewport 33 located at the same vertical height are considered as a group of viewport units, and the number of viewport units is not less than 2 groups (e.g., ...). Figure 2 and Figure 3The diagram shows four groups, evenly spaced from top to bottom. The vertical spacing between adjacent viewing window units on the side wall is equal. The first viewing window 30, the second viewing window 31, the third viewing window 32, and the fourth viewing window 33 in the same group are all distributed at 90° on the side wall (i.e., the side wall of the reaction device 16 or the side wall of the reaction chamber 17).

[0050] Furthermore, the reaction apparatus 16 includes a settling furnace connected to a temperature control device 18. The length of the constant temperature zone of the settling furnace in the vertical direction is equal to the length of the viewing window unit in the vertical direction. The length of the constant temperature zone is 1000~1200 mm, and the operating temperature of the settling furnace is ≤1600℃. The reaction chamber 17 includes a circular tube (e.g., a corundum tube). The viewing window on the circular tube is provided with sapphire tube sealing sections 34 on its surrounding side walls (similarly, the viewing window of the settling furnace body can be sealed with a transparent quartz sheet to ensure the airtightness of the reaction).

[0051] Furthermore, the gas distribution module includes a gas source delivery pipeline and a pressure reducing valve 5 and a mass flow meter 6 installed on the gas source delivery pipeline; the gas source delivery pipeline includes a first inert gas delivery pipeline 1, a second inert gas delivery pipeline 2, an oxygen / hydrogen delivery pipeline 3, and a carbon dioxide / carbon monoxide delivery pipeline 4, which are connected in sequence to a gas mixing device 7 and a steam generator 8; the steam generator 8 is connected to the inlet end of the reaction device 16 through a constant temperature pipeline 11, and the steam generator 8 is also connected to a water tank 10 through a pump 9.

[0052] Furthermore, the feeding module includes a powder feeding device 12, which is connected to the inlet end of the reaction device 16 via a feeding pipe 13. The feeding pipe 13 is also connected to the first inert gas conveying pipe 1, and the feeding pipe 13 is provided with a first cooling water inlet 14 and a first cooling water outlet 15.

[0053] Furthermore, the gas-solid product separation and collection module includes a sampling tube 19, with both ends of the sampling tube 19 connected to the reaction chamber 17 and the solid product collection device 22, respectively. The solid product collector is connected in sequence to the filter device 23 and the pumping device 24. The sampling tube 19 is provided with a second cooling water inlet 20 and a second cooling water outlet 21. The length of the sampling tube 19 is 1000~1500 mm. The reaction chamber 17 is formed by assembling a corundum tube and a sapphire.

[0054] Furthermore, the in-situ analysis and detection module also includes an online gas analyzer 26 and a central control unit 29. The online gas analyzer 26 is connected to the exhaust outlet 25 of the gas extraction device 24, and the central control unit 29 is connected to the online gas analyzer 26 and the image acquisition device 27.

[0055] This embodiment also provides a method for in-situ detection of the coal thermal conversion process using the above-mentioned detection system, including the following steps: 1) Start the circulating cooling circuit of water / oil cooled feed pipe 13 and water / oil cooled sampling pipe 19.

[0056] 2) Start the settling furnace 16 with a viewing window and heat it up to the required reaction temperature according to the program.

[0057] 3) When the furnace temperature reaches the required reaction temperature, turn on the gas distribution system and adjust the gas combination and mass flow meter opening of the gas distribution system to achieve the reaction gas atmosphere required for the specific experiment.

[0058] 4) When the reaction temperature and reaction atmosphere meet the experimental requirements, after stabilizing for 3 to 5 minutes, turn on the feeding system. By adjusting the speed of the micro-feeder 12, different feeding amounts can be achieved.

[0059] 5) After the feeding has stabilized for 3 to 5 minutes, the experimental conditions are basically stable, and the corresponding in-situ detection begins.

[0060] Therefore, this application, by combining a planar laser-induced fluorescence measurement system with a reaction device with a viewing window, has for the first time achieved in-situ detection of the morphological changes of gaseous products, intermediate reaction free radicals and solid products generated during coal pyrolysis, coal gasification and coal combustion, providing a new means to explain the intrinsic reaction mechanism of coal thermal conversion process.

[0061] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0062] Although embodiments of this application have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting this application. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of this application.

Claims

1. An in-situ detection system for coal thermal conversion process, characterized in that, It includes a gas distribution module, a feeding module, a reaction module, a gas-solid product separation and collection module, and an in-situ analysis and detection module; The reaction module includes a reaction device and a reaction chamber disposed inside the reaction device. A first viewing window and a second viewing window are provided on the side wall of the reaction device, and a third viewing window and a fourth viewing window are provided on the side wall of the reaction chamber. The in-situ analysis and detection module includes a planar laser-induced fluorescence measurement system and an image acquisition device connected to the planar laser-induced fluorescence measurement system. The planar laser-induced fluorescence measurement system includes a laser. The emitted light of the laser passes through the first viewing window and the third viewing window in sequence to induce the luminescence imaging of intermediate reactant species in the reaction chamber. The image acquisition device captures the luminescence image of the intermediate reactant species through the second viewing window and the fourth viewing window. The gas distribution module and the feeding module are both connected to the inlet end of the reaction device, and the gas-solid product separation and collection module is connected to the outlet end of the reaction device.

2. The in-situ detection system for coal thermal conversion process according to claim 1, characterized in that, The first and second view windows are both circular in shape, and the third and fourth view windows are both rectangular in shape. The length of the short side of the rectangle is not less than the diameter of the circle, and the length of the long side of the rectangle is 2 to 3 times the diameter of the circle.

3. The in-situ detection system for coal thermal conversion process according to claim 1, characterized in that, The first, second, third, and fourth view windows located at the same vertical height are considered as a group of view window units. The number of groups of view window units is not less than 2, and the vertical spacing between adjacent view window units on the sidewall is equal.

4. The in-situ detection system for coal thermal conversion process according to claim 3, characterized in that, The reaction apparatus includes a settling furnace, which is connected to a temperature control device. The length of the constant temperature zone of the settling furnace in the vertical direction is equal to the length of the viewing window unit in the vertical direction. The length of the constant temperature zone is 1000~1200 mm, and the operating temperature of the settling furnace is ≤1600℃. The reaction chamber includes a circular tube, and the viewing window on the circular tube is provided with sapphire tube sealing sections on its surrounding side walls.

5. The in-situ detection system for coal thermal conversion process according to any one of claims 1 to 4, characterized in that, The gas distribution module includes a gas source delivery pipeline and a pressure reducing valve and a mass flow meter installed on the gas source delivery pipeline; The gas source delivery pipeline includes a first inert gas delivery pipeline, a second inert gas delivery pipeline, an oxygen / hydrogen delivery pipeline, and a carbon dioxide / carbon monoxide delivery pipeline. The second inert gas delivery pipeline, the oxygen / hydrogen delivery pipeline, and the carbon dioxide / carbon monoxide delivery pipeline are sequentially connected to a gas mixing device and a steam generator. The steam generator is connected to the inlet of the reaction device via a constant temperature pipeline, and the steam generator is also connected to a water tank via a pump.

6. The in-situ detection system for coal thermal conversion process according to claim 5, characterized in that, The feeding module includes a powder feeding device, which is connected to the inlet end of the reaction device via a feeding pipe. The feeding pipe is also connected to the first inert gas conveying pipe, and the feeding pipe is provided with a first cooling water inlet and a first cooling water outlet.

7. The in-situ detection system for coal thermal conversion process according to claim 6, characterized in that, The gas-solid product separation and collection module includes a sampling tube, the two ends of which are connected to the reaction chamber and the solid product collection device, respectively. The solid product collector is connected to a filter device and a vacuum device in sequence. The sampling tube is provided with a second cooling water inlet and a second cooling water outlet. The length of the sampling tube is 1000-1500 mm. The reaction chamber is formed by assembling a corundum tube and a sapphire.

8. The in-situ detection system for coal thermal conversion process according to claim 7, characterized in that, The in-situ analysis and detection module also includes an online gas analysis device and a central control device. The online gas analysis device is connected to the exhaust outlet of the gas extraction device, and the central control device is connected to the online gas analysis device and the image acquisition device.

9. An in-situ detection method for the thermal conversion process of coal, characterized in that, The in-situ detection method for the coal thermal conversion process adopts the in-situ detection system for the coal thermal conversion process as described in any one of claims 1 to 8.

10. The in-situ detection method for coal thermal conversion process according to claim 9, characterized in that, The detection targets include continuous online detection of gaseous products generated during coal pyrolysis, coal gasification, and coal combustion, continuous online detection of intermediate reaction free radicals, and continuous online detection of changes in the morphology of solid products.

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