Multi-source monitoring and multi-mode analysis coal body thermal reaction comprehensive testing device and testing method

Abstract

The invention discloses a multi-source monitoring and multi-mode analysis coal thermal reaction comprehensive testing device, which comprises an oil-filled expansion tank and an oil bath reaction chamber, the oil-filled expansion tank and the oil bath reaction chamber form a circulation loop through a pipeline, and a temperature sensor in and a temperature sensor out are respectively arranged in an oil inlet and an oil outlet of the oil bath reaction chamber. The sample bin of the oil bath reaction chamber is also connected with an Air-N2 gas supply device through a gas inlet pipeline, the sample bin is also connected with a mu-GC micro gas chromatographic instrument through a gas outlet pipeline, and the temperature sensor in, the temperature sensor out, the Air-N2 gas supply device and the mu-GC micro gas chromatographic instrument are jointly connected with a programmable logic controller (PLC) through signal cables. The problems that in the prior art, oil temperature stratification is difficult to find, temperature level sampling and continuous temperature rising need to be carried out separately, and the gas flow cannot be adjusted according to needs to maintain the needed low-oxygen seepage condition are solved. The invention further discloses a coal body thermal reaction comprehensive testing method based on multi-source monitoring and multi-mode analysis.

Description

Technical Field

[0001] The present invention belongs to the technical field of coal sample thermal analysis and spontaneous combustion safety testing devices, and relates to a comprehensive coal thermal reaction testing device with multi-source monitoring and multi-mode analysis. The present invention also relates to a comprehensive coal thermal reaction testing method with multi-source monitoring and multi-mode analysis. Background Art

[0002] Coal spontaneous combustion is a serious threat to mine safety, worker health, and environmental safety, while also causing significant losses in coal resources. The coal spontaneous combustion process involves multiple physical and chemical coupling phenomena, including oxygen consumption, heat release, and gas generation.

[0003] Existing equipment for comprehensive coal thermal reaction testing uses a direct heating temperature field with a resistance wire, resulting in uneven heating, inconsistent inlet gas temperature synchronization, and large errors. In devices that use an oil bath for heating, the oil bath temperature is detected by a single probe, making it difficult to detect oil temperature stratification. Existing methods require separate equipment for fixed temperature step sampling and testing: stopping for a period of time at each desired temperature to allow a gas bag to collect gas. However, it is not possible to simultaneously test both continuous heating and gradient heating with the same equipment. These two experiments must either be conducted with separate equipment or separately. Therefore, when continuously feeding the reaction gas flow into the chromatograph to obtain the gas concentration curve during the heating process, it is impossible to maintain a fixed temperature step and accurately correspond to the temperature point. Testing for the shortest spontaneous ignition period of coal samples requires manual sampling with a gas bag at each set temperature step (e.g., a 20°C step) and then injecting it into the chromatograph for offline analysis. This is cumbersome, unable to obtain dynamic data at the second level, and unable to synchronize with the continuously programmed heating curve. The two tests must be conducted separately, which is both time-consuming and fragmented.

[0004] Existing devices are usually designed to deliver air continuously and stably. This constant high flow rate will cause the oxygen concentration in the system to increase rapidly, making it difficult to achieve a hypoxic environment. In addition, there is a lack of precise flow and oxygen concentration control systems, and the air flow cannot be adjusted as needed to maintain the required hypoxic infiltration conditions. Summary of the Invention

[0005] The purpose of the present invention is to provide a comprehensive coal thermal reaction testing device with multi-source monitoring and multi-mode analysis, which solves the problems existing in the prior art such as the difficulty in detecting oil temperature stratification, the need to separate temperature step sampling and continuous heating, and the inability to adjust the gas flow rate as needed to maintain the required low-oxygen seepage conditions.

[0006] Another object of the present invention is to provide a comprehensive test method for coal thermal reaction with multi-source monitoring and multi-mode analysis.

[0007] The technical solution adopted by the present invention is a comprehensive test device for coal thermal reactions with multi-source monitoring and multi-mode analysis, including an oil-filled expansion tank and an oil bath reaction chamber. The oil-filled expansion tank and the oil bath reaction chamber form a circulation loop through a pipeline. A temperature sensor in and a temperature sensor out are respectively provided in the oil inlet and oil outlet of the oil bath reaction chamber. The sample chamber of the oil bath reaction chamber is also connected to an Air-N2 gas supply device through an air inlet pipeline, and the sample chamber is also connected to a μ-GC micro gas chromatograph and an NDIR non-dispersive infrared gas sensor through an air outlet pipeline. The temperature sensor in, the temperature sensor out, the Air-N2 gas supply device, and the μ-GC micro gas chromatograph are commonly connected to a programmable logic controller PLC through a signal cable.

[0008] Preferably, the oil outlet of the oil-filled expansion tank is connected to the oil inlet of the oil bath reaction chamber through a pipeline, the oil outlet of the oil bath reaction chamber is connected to a heater, a gear pump, and a filter device in sequence through a pipeline, and then connected to the oil inlet a of the oil-filled expansion tank, the heater is connected to an SSR solid-state relay through a signal cable, the SSR solid-state relay and the gear pump are respectively connected to a programmable logic controller PLC through signal cables, and a nitrogen bottle is also included, the nitrogen bottle is connected to the air inlet of the oil-filled expansion tank through a pipeline, and a flow meter a, a pressure reducing valve a, and a pressure gauge a are also provided on the pipeline between the nitrogen bottle and the air inlet of the oil-filled expansion tank.

[0009] The grease trap chamber has a plurality of oil drain plugs, and the grease trap chamber has a plurality of oil drain plugs, and the grease trap chamber has a plurality of oil drain plugs.

[0010] Preferably, the Air-N2 gas supply device includes a pump connected to the air inlet pipeline, which is connected to the gas distribution tank and the three-way valve in sequence through the pipeline. The other two ports of the three-way valve are respectively connected to the nitrogen storage tank and the air storage tank through pipelines. The pipeline between the nitrogen storage tank and the three-way valve is also sequentially provided with a pressure gauge c, a pressure reducing valve b, a flow meter b and a mass flow controller MFC from the three-way valve to the nitrogen storage tank. The two mass flow controllers MFC are respectively connected to the programmable logic controller PLC through signal cables.

[0011] Preferably, the end of the gas outlet pipeline facing away from the sample chamber extends out of the furnace body and is connected in sequence to a micro pump, a solenoid valve, and a μ-GC micro gas chromatograph through a pipeline. The solenoid valve and the μ-GC micro gas chromatograph are also connected in parallel with an NDIR non-dispersive infrared gas sensor through a pipeline. The μ-GC micro gas chromatograph and the NDIR non-dispersive infrared gas sensor are also connected to a digital terminal through a signal cable. A temperature sensor is also provided on the gas outlet pipeline. The temperature sensor, micro pump, solenoid valve, and μ-GC micro gas chromatograph are all connected to a programmable logic controller PLC through a signal cable.

[0012] Preferably, IR windows are installed at corresponding positions on the side walls of the furnace body and the sample chamber, the two IR windows are connected by a pipe and the inside of the pipe is a vacuum environment, an IR camera is set at a position outside the furnace body and parallel to the IR window, the lens of the IR camera is arranged facing upward to the IR window, and the IR camera is also connected to the digital terminal through a signal cable.

[0013] Preferably, the IR window is sealed and fixed by an O-ring and a spring-type pressure cover, a top cover is also provided at the upper end of the sample chamber, and a top cover is also installed at the upper end of the furnace body corresponding to the sample chamber removal and loading position; an oil drain valve is also provided at the bottom of the furnace body, and the other end of the oil drain valve is connected to the oil bath chamber, and the μ-GC micro gas chromatograph and the NDIR non-dispersive infrared gas sensor are also connected to an exhaust valve through a pipeline.

[0014] Preferably, the programmable logic controller PLC is embedded with a proportional-integral-differential regulator PID, and the programmable logic controller PLC has two analog output ports: PLC DO and PLC AO, and an analog input port PLC AI. PLCDO is connected to the SSR solid-state relay, micro pump, solenoid valve, and gear pump through signal cables. PLC AO is connected to two mass flow controllers MFC through signal cables; PLC AI is connected to temperature sensor in, temperature sensor out, temperature sensor and μ-GC micro gas chromatography instrument through signal cables.

[0015] The second technical solution adopted by the present invention is a comprehensive test method for coal thermal reaction with multi-source monitoring and multi-mode analysis, which uses the above-mentioned comprehensive test device for coal thermal reaction with multi-source monitoring and multi-mode analysis, specifically: During operation, the temperature sensor in and the temperature sensor out monitor the oil inlet temperature T_in and the oil outlet temperature T_out in real time and transmit them to the programmable logic controller PLC. The programmable logic controller PLC controls the pump speed of the gear pump according to the temperature difference between T_in and T_out. The μ-GC micro gas chromatograph monitors the oil inlet temperature T_in and the oil outlet temperature T_out in real time. concentration, and regularly transmit it to the programmable logic controller PLC, which The concentration-controlled mass flow controller (MFC) maintains low oxygen permeate flow.

[0016] The specific implementation steps are as follows: Step 1: Place the coal sample into the sample bin and level it, lock the top cover of the sample bin, then open the top cover on the furnace body and place the sample bin in through the slide rail, then reset and lock the top cover on the furnace body; Step 2: Add silicone oil to the oil expansion tank until the liquid level reaches 70%, and fill it with 0.05 MPa nitrogen through a nitrogen bottle to make an oil seal; Step 3: Input the ramp command SP(t) = 30°C + 1°C into the proportional-integral-derivative regulator PID of the programmable logic controller (PLC). The end temperature is 300°C, and the flow rates of the two mass flow controllers MFC are set to 100 ; Step 4: Turn on the gear pump to start heating. The programmable logic controller (PLC) controls the SSR solid-state relay to turn on. The heater and gear pump are used together to increase the temperature of the oil bath at a constant speed according to the ramp. During the heating process, the programmable logic controller (PLC) uses the temperature sensor in to monitor the oil inlet temperature T_in in real time and uses it as the measured value of the proportional-integral-differential regulator PID to adjust the power of the gear pump in real time. During the heating process, the temperature sensor in and the temperature sensor out monitor the oil inlet temperature T_in and the oil outlet temperature T_out in real time and transmit them to the programmable logic controller PLC. If the temperature difference is greater than 2°C, the programmable logic controller PLC controls the gear pump to increase the pump speed by 5Hz. If it is less than 1°C, the gear pump speed is controlled to decrease by 5Hz to ensure uniform oil temperature. If the temperature difference is 1 remains unchanged; The temperature sensor monitors the temperature T_coal of the gas outlet pipe in real time and transmits it to the programmable logic controller (PLC). Whenever the temperature T_coal reaches 30 ± 20n°C (n = 1…13), the programmable logic controller (PLC) pauses the ramp constant-rate heating process and then opens the solenoid valve for 30 seconds to inflate the μ-GC micro gas chromatograph for gas component analysis. The solenoid valve is then closed to resume the ramp constant-rate heating process. After the μ-GC micro gas chromatograph is inflated, the μ-GC micro gas chromatograph completes the multi-component full spectrum quantification and The concentration is sent back to the PLC AI port, and the programmable logic controller PLC calculates the concentration based on the concentration sent back by the μ-GC micro gas chromatograph. Concentration, if If the concentration is lower than 5%, the programmable logic controller (PLC) controls the mass flow controller (MFC) of the air tank to increase the flow by 20%. ,like If the concentration is higher than 8%, the flow rate of the mass flow controller MFC controlling the air tank is reduced by 20 , maintain low oxygen permeability; NDIR non-dispersive infrared gas sensor real-time recording and pass the data to the digital terminal; Step 5: When the temperature T_coal of the gas outlet reaches 300°C or the target temperature, the programmable logic controller (PLC) controls the heater to turn off immediately through the SSR solid-state relay, and reduces the pump speed of the gear pump to 20Hz and then cools the pump for 15 minutes before shutting down. Step 6: The digital terminal generates a temperature signal according to the gas-temperature coupling model based on the gas and temperature data of the μ-GC micro gas chromatograph, NDIR non-dispersive infrared gas sensor, and IR camera at the same time. 、Full t Curve, catalytic / inhibitory coefficient and 、CO、 、 、 、 、 、 Gas composition diagram.

[0017] The beneficial effects of the present invention are: 1. The present invention uses "oil bath + preheating coil" to uniformly heat the oil, combined with real-time monitoring of the temperature difference between the oil inlet and outlet, By adjusting the pump speed of the gear pump to achieve closed-loop compensation of the oil flow and dynamic balance of the oil temperature, the oil temperature stratification problem can be discovered in time and adjustments can be made to keep the temperature difference between the oil inlet and outlet less than 2°C.

[0018] 2. The present invention uses a continuous NDIR and valve-controlled μ-GC parallel sampling architecture to detect and analyze gas, with NDIR always open and real-time monitoring in seconds , generating a continuous gas curve corresponding to the whole process of temperature rise, the branch μ-GC is under the control of PLC, triggering the solenoid valve 30s to fill the sampling loop at the target temperature step, and then μ-GC is completed 、CO、 The full spectrum quantification of multiple components such as hydrocarbons can realize continuous gas sampling analysis and specific temperature step gas sampling at the same time, and carry out the next step of analysis at the same time. In one test, a continuous gas release curve and accurate full spectrum data of each temperature step can be obtained at the same time, which not only meets the requirements of programmed temperature rise and step sampling such as the shortest spontaneous combustion period, but also greatly improves the test efficiency and data integrity. During the sampling period, the main NDIR is not interrupted, and the pressure and flow are stable, realizing true non-interference and synchronous operation.

[0019] 3. The present invention can realize the synchronous collection of temperature data and gas data, and then switch between τ_min determination, heat release rate curve, characteristic gas determination, and catalyst / inhibitor screening in the temperature-gas coupling model. When performing catalyst / inhibitor screening, it can quantitatively determine whether a certain additive can significantly extend the shortest spontaneous combustion period of coal or reduce the heat release intensity, thereby providing reliable data support for fire prevention and extinguishing selection, dosage optimization and cost control, avoiding repeated trial and error underground.

[0020] 4. The +20℃ stop sampling strategy of the present invention solves the problems of inaccurate and easy missed points in traditional manual stop. The PLC monitors that the coal temperature crosses the 20℃ step and immediately suspends heating, triggers sampling, and automatically resumes heating after the analysis is completed. The stop is only 30s, which does not affect the integrity of the slope.

[0021] 5. The present invention reads the μ-GC value, the PLC adjusts the MFC-Air voltage to achieve stable low oxygen permeation.

[0022] 6. The present invention monitors the temperature T_coal of the gas outlet pipe to stop heating in case of abnormal over-temperature. Surge nitrogen cutting to ensure the safety of system operation.

[0023] 7. The present invention uses a micro pump with long service life, a valve group with cyclic rotation, an oil bath expansion tank with nitrogen sealing, and the PLC can operate automatically even when the network is disconnected. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a structural schematic diagram of the comprehensive testing device for coal thermal reaction with multi-source monitoring and multi-mode analysis according to the present invention; Figure 2 It is a structural schematic diagram of the oil bath reaction chamber in the comprehensive test device for coal thermal reaction with multi-source monitoring and multi-mode analysis of the present invention; Figure 3 It is a cross-sectional view of the oil bath reaction chamber in the comprehensive test device for coal thermal reaction with multi-source monitoring and multi-mode analysis according to the present invention; Figure 4 The present invention is a flow chart of a comprehensive test method for coal thermal reaction with multi-source monitoring and multi-mode analysis.

[0025] In the figure: 1. Oil expansion tank, 2. Pressure gauge a, 3. Pressure reducing valve a, 4. Flow meter a, 5. Nitrogen cylinder, 6. Filter, 7. Temperature sensor in, 8. Oil inlet, 9. Gear pump, 10. Heater, 11. SSR solid-state relay, 12. Oil outlet, 13. Temperature sensor out, 14. PLC DO, 15. PLC AI, 16. Programmable logic controller PLC, 17. Proportional-integral-derivative controller PID, 18. PLC AO, 19. Top cover, 20. Air inlet pipe, 21. Pressure gauge b, 22. Pump, 23. Gas distribution tank, 24. Three-way valve, 25. Pressure gauge c, 26. Pressure reducing valve b, 27. Flow meter, 28. Mass flow controller (MFC), 29. Nitrogen storage tank, 30. Air storage tank, 31. Air outlet pipe, 32. Temperature sensor, 33. Micropump, 34. NDIR (non-dispersive infrared) gas sensor, 35. Solenoid valve, 36. μ-GC (micro gas chromatograph), 37. Exhaust valve, 38. IR window, 39. O-ring, 40. Circlip-type gland, 41. IR camera, 42. Digital terminal, 43. Oil drain valve, 44. Sample chamber, 45. Oil bath chamber, 46. Furnace, 47. Preheating coil, 48. Slide rail, 49. Distribution main pipe, 50. Distribution branch pipe. DETAILED DESCRIPTION

[0026] The following describes it in detail with reference to specific implementation methods.

[0027] Example 1 The present invention provides a comprehensive test device for coal thermal reaction with multi-source monitoring and multi-mode analysis. The structure is as follows: Figure 1 As shown, it includes an oil-filled expansion tank 1 and an oil bath reaction chamber. The oil-filled expansion tank 1 and the oil bath reaction chamber form a circulation loop through a pipeline. The oil inlet 8 and the oil outlet 12 of the oil bath reaction chamber are respectively provided with a temperature sensor in7 and a temperature sensor out13. The sample chamber 44 of the oil bath reaction chamber is also connected to an Air-N2 gas supply device through an air inlet pipe 22. The sample chamber 44 is also connected to a μ-GC micro gas chromatograph 36 and an NDIR non-dispersive infrared gas sensor 34 through an air outlet pipe 31. The temperature sensor in7, the temperature sensor out13, the Air-N2 gas supply device, and the μ-GC micro gas chromatograph 36 are commonly connected to a programmable logic controller PLC16 through a signal cable.

[0028] The temperature sensor in7 and the temperature sensor out13 of the present invention both adopt platinum temperature sensor PT100.

[0029] The oil outlet of the oil-filled expansion tank 1 is connected to the oil inlet 8 of the oil bath reaction chamber through a pipeline. The oil outlet 12 of the oil bath reaction chamber is connected to the heater 10, the gear pump 9, and the filter device 6 in sequence through a pipeline and then connected to the oil inlet a of the oil-filled expansion tank 1. The heater 10 is connected to the SSR solid-state relay 11 through a signal cable. The SSR solid-state relay 11 and the gear pump 9 are respectively connected to the programmable logic controller PLC16 through signal cables. It also includes a nitrogen bottle 5, and the nitrogen bottle 5 is connected to the air inlet of the oil-filled expansion tank 1 through a pipeline. A flow meter a4, a pressure reducing valve a3, and a pressure gauge a2 are also provided on the pipeline between the nitrogen bottle 5 and the air inlet of the oil-filled expansion tank 1.

[0030] The filter device 6 has 100 built-in Filter element, gear pump 9 uses 6 The gear pump is 2KW, and the heater 10 is a 2KW heater.

[0031] Example 2 On the basis of Example 1, Figure 2-3 As shown, the oil bath reaction chamber includes an outer furnace body 46 made of insulating material, a sample chamber 44 is coaxially arranged in the furnace body 46, an oil bath chamber 45 is used between the outer wall of the sample chamber 44 and the inner wall of the furnace body 46, one end of the oil outlet 12 extends into the oil bath chamber 45, and the other end passes through the furnace body 46 to connect to the oil expansion tank 1, one end of the oil inlet 8 extends into the oil bath chamber 45, and the other end passes through the furnace body 46 to connect to the heater 10, the oil bath chamber 45 is provided with two vertical slide rails 48 at the corresponding ends in the diameter direction, and a slider is provided at the position of the outer wall of the sample chamber 44 corresponding to the slide rail 48, and the sample The bin 44 cooperates with the slide rail 48 and the slider to realize the removal and loading of the sample bin 44 from the furnace body 46. A preheating coil 47 is also provided in the oil bath bin 45 along its height direction. The upper end of the preheating coil 47 is connected to the air intake pipe 20, and the lower end of the preheating coil 47 is connected to the distribution main pipe 49. The distribution main pipe 49 is located below the sample bin 44 and is connected to a plurality of distribution branch pipes 50. The other ends of the plurality of distribution branch pipes 50 lead to the sample bin 44. The oil inlet 8 and the oil outlet 12 of the oil bath reaction chamber are respectively provided with the lower end and the upper end of the side wall of the furnace body 46 and are connected to the oil bath bin 45.

[0032] The preheating coil adopts a spiral coil and the preheating coil is completely immersed in the oil bath.

[0033] Example 3 Based on Example 2, the Air-N2 gas supply device includes a pump 22 connected to the air intake pipe 20, and the pump 22 is connected to the air distribution tank 23 and the three-way valve 24 in sequence through the pipe. The other two ports of the three-way valve 24 are respectively connected to the nitrogen storage tank 29 and the air storage tank 30 through pipes. The pipe between the nitrogen storage tank 29 and the three-way valve 24 is further provided with a pressure gauge c25, a pressure reducing valve b26, a flow meter b27 and a mass flow controller MFC28 in sequence from the three-way valve 24 to the nitrogen storage tank 29. The two mass flow controllers MFC28 are respectively connected to the programmable logic controller PLC16 through signal cables. A pressure gauge b21 is also provided at one end of the air intake pipe 20 near the pump 22.

[0034] Nitrogen and air are first connected to MFC-N2 and MFC-Air respectively, then connected to flow meter 27, connected to pressure reducing valve b26, connected to pressure gauge c25, through three-way valve 24, connected to gas distribution tank 23 for mixing, and pumped into the air intake pipe 20 through pump 22. The mixed gas enters the preheating coil 47 through the air intake pipe 20, passes into the sample chamber 44, and reacts with the coal sample.

[0035] The end of the gas outlet pipe 31 facing away from the sample chamber 44 extends out of the furnace body 46 and is connected to a micro pump 33, a solenoid valve 35, and a μ-GC micro gas chromatograph 36 in sequence through pipelines. The solenoid valve 35 and the μ-GC micro gas chromatograph 36 are also connected in parallel with an NDIR non-dispersive infrared gas sensor 34 through pipelines. The μ-GC micro gas chromatograph 36 and the NDIR non-dispersive infrared gas sensor 34 are also connected to a digital terminal 42 through a signal cable. A temperature sensor 32 is also provided on the gas outlet pipe 31. The temperature sensor 32, the micro pump 33, the solenoid valve 35, and the μ-GC micro gas chromatograph 36 are all connected to the programmable logic controller PLC16 through signal cables.

[0036] The gas after the reaction in the sample chamber 44 passes through the gas outlet pipe 31 and is pumped into the NDIR non-dispersive infrared gas sensor 34 through the micro pump 33 under the control of the programmable logic controller PLC16 for real-time monitoring in seconds. , generate a continuous gas curve, analyze the whole process of programmed temperature rise; under the control of the programmable logic controller PLC16, the solenoid valve 35 is triggered at the target temperature step to extract a part of the gas into the μ-GC micro gas chromatograph 36, sample and detect the gas, and complete the 、CO、 Multi-component full spectrum quantification.

[0037] Example 4 On the basis of Example 3, IR windows 38 are installed at corresponding positions on the side walls of the furnace body 46 and the sample chamber 44. The two IR windows 38 are connected by a pipe and the inside of the pipe is a vacuum environment. An IR camera 41 is provided outside the furnace body 46 at a position parallel to the IR window 38. The lens of the IR camera 41 is arranged facing the IR window 38 upward. The IR camera 41 is also connected to the digital terminal 42 via a signal cable.

[0038] The IR window 38 is a ZnSe window, and the upper end of the IR window 38 located on the sample chamber 44 is tilted 10 degrees into the sample chamber 44 so that the coal powder slides down naturally.

[0039] The IR window 38 is sealed and fixed by an O-ring 39 and a spring-type pressure cover 40. A top cover 19 is also provided at the upper end of the sample chamber 44, and a top cover 19 is also installed at the upper end of the furnace body 46 corresponding to the removal and loading position of the sample chamber 44; an oil drain valve 43 is also provided at the bottom of the furnace body 46, and the other end of the oil drain valve 43 is connected to the oil bath chamber 45. The μ-GC micro gas chromatograph 36 and the NDIR non-dispersive infrared gas sensor 34 are also connected to an exhaust valve 37 through a pipeline to purify the exhaust gas.

[0040] Example 5 On the basis of Example 4, the programmable logic controller PLC16 is embedded with a proportional-integral-differential regulator PID17. The programmable logic controller PLC16 has two analog output ports: PLC DO14 and PLC AO18, and an analog input port PLC AI15. PLC DO14 is connected to the SSR solid-state relay 11, the micro pump 33, the solenoid valve 35, and the gear pump 9 through signal cables. The PLC AO18 is connected to two mass flow controllers MFC28 through signal cables, namely MFC-N2 and MFC-Air, to control the flow of N2 and Air gases, providing a low-oxygen reaction environment in the sample chamber 44.

[0041] The PLC AI15 is connected to the temperature sensor in7, the temperature sensor out13, the temperature sensor 32 and the μ-GC micro gas chromatography instrument 36 through signal cables.

[0042] Example 6 The comprehensive test method for coal thermal reaction with multi-source monitoring and multi-mode analysis of the present invention adopts the comprehensive test device for coal thermal reaction with multi-source monitoring and multi-mode analysis in Example 5, specifically: During operation, the temperature sensor in7 and the temperature sensor out13 monitor the oil inlet temperature T_in and the oil port temperature T_out in real time and transmit them to the programmable logic controller PLC16. The programmable logic controller PLC16 controls the pump speed of the gear pump 9 according to the temperature difference between the temperatures T_in and T_out. The μ-GC micro gas chromatography instrument 36 monitors the O2 concentration in real time and transmits it to the programmable logic controller PLC16 regularly. The programmable logic controller PLC16 controls the mass flow controller MFC28 according to the O2 concentration to maintain low oxygen permeation.

[0043] When conducting the experiment in this embodiment, the sample is first prepared. The coal sample with a particle size of 0.15-0.25 mm is placed in a constant temperature drying oven at 75° C. and dried for 2 hours. Then 200 g of the coal is placed in the metal sample bin 44 and leveled.

[0044] During operation, a circuit self-check is first performed to ensure that the temperature sensor in7 and the temperature sensor out13, MFC, NDIR, and μ-GC are all in communication status, and the oil pump is pre-circulated, that is, the gear pump 9 is first run for 2 minutes to observe whether there is any oil leakage.

[0045] The specific implementation steps are as follows: Figure 4 As shown: Step 1: Place the coal sample into the sample bin 44 and level it, lock the top cover 19 in the sample bin 44, then open the top cover 19 on the furnace body 46 and place the sample bin 44 into the sample bin via the slide rail, then reset and lock the top cover 19 on the furnace body 46; Step 2: Add silicone oil to the oil expansion tank 1 until the liquid level reaches 70%, and fill it with 0.05 MPa nitrogen through the nitrogen bottle 5 to make an oil seal; Step 3: Input the ramp command SP(t) = 30°C + 1°C into the proportional-integral-differential regulator PID17 of the programmable logic controller PLC16. , the end temperature is 300 ° C, and the flow rates of the two mass flow controllers MFC28 are set to 100 mL ; Step 4, the programmable logic controller PLC16 controls to turn on the gear pump 9 and increase the power to 40Hz, starting the temperature rise. The programmable logic controller PLC16 controls to turn on the SSR solid-state relay 11, and uses the heater 10 and the gear pump 9 to heat the oil bath at a constant speed according to the ramp. During the temperature rise process, the programmable logic controller PLC16 uses the temperature sensor in7 to monitor the oil inlet temperature T_in in real time as the measurement value of the proportional-integral-differential regulator PID17 to adjust the power of the gear pump 9 in real time. The power of the heater 10 remains constant during the temperature rise process; Among them, the heater 10 heats the heat transfer oil to a fixed high temperature according to the target oil bath temperature. At each moment, the pump needs to send some hot oil that is higher than the bath temperature into the furnace body, so that the bath temperature rises uniformly according to the set slope. The gear pump determines how much hot oil is sent into the oil bath per second. The faster the pump rotates, the more heat is taken in, and the temperature rises faster; the slower the pump rotates, the less heat is taken in, and the temperature rises slowly or remains constant.

[0046] During the heating process, the temperature sensor in7 and the temperature sensor out13 monitor the oil inlet temperature T_in and the oil outlet temperature T_out in real time and transmit them to the programmable logic controller PLC16. If the temperature difference is greater than 2°C, the programmable logic controller PLC16 controls the pump speed of the gear pump 9 to increase by 5Hz. If it is less than 1°C, the pump speed of the gear pump 9 is controlled to decrease by 5Hz to ensure uniform oil temperature. If the temperature difference is 1 Otherwise, remain unchanged; The temperature sensor 32 monitors the temperature T_coal of the gas outlet pipe 31 in real time and transmits it to the programmable logic controller PLC16. Whenever the temperature T_coal reaches 30+20n°C, where n=1…13, the programmable logic controller PLC16 pauses the ramp uniform heating process, then opens the solenoid valve 35 for 30 seconds to inflate the μ-GC micro gas chromatograph 36 for gas component analysis, and then closes the solenoid valve 35 to resume the ramp uniform heating process. After the μ-GC micro gas chromatograph 36 is inflated, the μ-GC micro gas chromatograph 36 completes the multi-component full spectrum quantification and transmits the O2 concentration back to the PLC AI15 port. The programmable logic controller PLC16 controls the mass flow controller MFC28 of the air tank 30 to increase the flow rate by 20% based on the O2 concentration transmitted back by the μ-GC micro gas chromatograph 36. If the O2 concentration is lower than 5%, the programmable logic controller PLC16 controls the mass flow controller MFC28 of the air tank 30 to increase the flow rate by 20%. If the O2 concentration is higher than 8%, the flow rate of the mass flow controller MFC28 controlling the air tank 30 is reduced by 20%. , maintain low oxygen permeability; After completing the multi-component full spectrum quantification, the μ-GC micro gas chromatograph 36 transmits the data to the digital terminal 42, and the NDIR non-dispersive infrared gas sensor 34 records the data in real time. and transmits the data to the digital terminal 42; Step 5: When the temperature T_coal of the gas outlet pipe 31 reaches 300°C or the target temperature, the programmable logic controller PLC16 controls the heater 10 to be turned off immediately through the SSR solid-state relay 11, and reduces the pump speed of the gear pump 9 to 20Hz and then cools the pump for 15 minutes or the oil temperature reaches 100°C. Shut down after 60°C; Step 6: The digital terminal 42 generates a temperature data according to the gas-temperature coupling model based on the gas and temperature data of the μ-GC micro gas chromatograph 36, the NDIR non-dispersive infrared gas sensor 34, and the IR camera 41 at the same time. 、Full t Curve, catalytic / inhibitory coefficient and 、CO、 、 、 、 、 、 Gas composition diagram.

[0047] After shutdown, drain and filter the oil if necessary, and wipe the external IR window with alcohol.

[0048] Example 7 On the basis of Example 6, when the method of the present invention is used to screen catalysts / inhibitors, typical coal samples are selected, blank controls and catalysts / inhibitors of different types and concentrations are set up and added into the sample bin together with the coal samples.

[0049] Then, a temperature-programmed experiment was conducted according to the method of Example 6. With all other conditions remaining the same, temperature-gas data were collected for a blank control and for the addition of different types and concentrations of catalysts / inhibitors. Based on this temperature-gas data, real-time metrics were calculated: peak heat release and catalytic / inhibitory coefficients. By comparison with the blank control, ineffective / negative formulations were eliminated, and those that met the criteria were retained for further validation.

Claims

1. A comprehensive test device for coal thermal reaction with multi-source monitoring and multi-mode analysis, characterized in that: The invention comprises an oil-filled expansion tank (1) and an oil bath reaction chamber, wherein the oil-filled expansion tank (1) and the oil bath reaction chamber form a circulation loop through a pipeline, wherein the oil inlet (8) and the oil outlet (12) of the oil bath reaction chamber are respectively provided with a temperature sensor in (7) and a temperature sensor out (13), the sample chamber (44) of the oil bath reaction chamber is further connected to an Air-N2 gas supply device through an air inlet pipe (22), the sample chamber (44) is further connected to a μ-GC micro gas chromatograph (36) and an NDIR non-dispersive infrared gas sensor (34) through an air outlet pipe (31), and the temperature sensor in (7), the temperature sensor out (13), the Air-N2 gas supply device, and the μ-GC micro gas chromatograph (36) are connected to a programmable logic controller PLC (16) through a signal cable.

2. The comprehensive coal thermal reaction testing device with multi-source monitoring and multi-mode analysis according to claim 1 is characterized in that: The oil outlet of the oil-filled expansion tank (1) is connected to the oil inlet (8) of the oil bath reaction chamber through a pipeline. The oil outlet (12) of the oil bath reaction chamber is connected to a heater (10), a gear pump (9), and a filter device (6) in sequence through pipelines and then connected to the oil inlet a of the oil-filled expansion tank (1). The heater (10) is connected to an SSR solid-state relay (11) through a signal cable. The SSR solid-state relay (11) and the gear pump (9) are respectively connected to a programmable logic controller (PLC) (16) through signal cables. The invention also includes a nitrogen bottle (5). The nitrogen bottle (5) is connected to the air inlet of the oil-filled expansion tank (1) through a pipeline. A flow meter a (4), a pressure reducing valve a (3), and a pressure gauge a (2) are also provided on the pipeline between the nitrogen bottle (5) and the air inlet of the oil-filled expansion tank (1).

3. The comprehensive test device for coal thermal reaction with multi-source monitoring and multi-mode analysis according to claim 2 is characterized in that: The oil bath reaction chamber includes an outer furnace body (46) made of insulating material, a sample chamber (44) is coaxially arranged in the furnace body (46), and an oil bath chamber (45) is provided between the outer wall of the sample chamber (44) and the inner wall of the furnace body (46). One end of the oil outlet (12) extends into the oil bath chamber (45), and the other end passes through the furnace body (46) to connect to the oil expansion tank (1), and one end of the oil inlet (8) extends into the oil bath chamber (45), and the other end passes through the furnace body (46) to connect to the heater (10). The oil bath chamber (45) is provided with two vertical slide rails (48) at the corresponding two ends in the diameter direction thereof, and a slider is provided at the position of the outer wall of the sample chamber (44) corresponding to the slide rail (48). The bin (44) cooperates with the slide rail (48) and the slider to realize the removal and loading of the sample bin (44) from the furnace body (46). A preheating coil (47) is further provided in the oil bath bin (45) along its height direction. The upper end of the preheating coil (47) is connected to the air inlet pipe (20), and the lower end of the preheating coil (47) is connected to a distribution main pipe (49). The distribution main pipe (49) is located below the sample bin (44) and is connected to a plurality of distribution branches (50). The other ends of the plurality of distribution branches (50) lead to the sample bin (44). The oil inlet (8) and the oil outlet (12) of the oil bath reaction chamber are respectively provided at the lower end and the upper end of the side wall of the furnace body (46) and are connected to the oil bath bin (45).

4. The comprehensive coal thermal reaction testing device with multi-source monitoring and multi-mode analysis according to claim 3 is characterized in that: The Air-N2 gas supply device includes a pump (22) connected to the air inlet pipeline (20), the pump (22) is connected to the gas distribution tank (23) and the three-way valve (24) in sequence through the pipeline, the other two ports of the three-way valve (24) are connected to the nitrogen storage tank (29) and the air storage tank (30) through pipelines, and a pressure gauge c (25), a pressure reducing valve b (26), a flow meter b (27) and a mass flow controller MFC (28) are also sequentially provided on the pipeline between the nitrogen storage tank (29) and the three-way valve (24) from the three-way valve (24) to the nitrogen storage tank (29), and the two mass flow controllers MFC (28) are respectively connected to the programmable logic controller PLC (16) through signal cables.

5. The comprehensive test device for coal thermal reaction with multi-source monitoring and multi-mode analysis according to claim 4 is characterized in that: The end of the gas outlet pipe (31) facing away from the sample chamber (44) extends out of the furnace body (46) and is connected to a micro pump (33), a solenoid valve (35), and a μ-GC micro gas chromatograph (36) in sequence through pipelines. The solenoid valve (35) and the μ-GC micro gas chromatograph (36) are also connected in parallel with an NDIR non-spectroscopy infrared gas sensor (34) through pipelines. The μ-GC micro gas chromatograph (36) and the NDIR non-spectroscopy infrared gas sensor (34) are also connected to a digital terminal (42) through a signal cable. A temperature sensor (32) is also provided on the gas outlet pipe (31). The temperature sensor (32), the micro pump (33), the solenoid valve (35), and the μ-GC micro gas chromatograph (36) are all connected to the programmable logic controller PLC (16) through a signal cable.

6. The comprehensive coal thermal reaction testing device with multi-source monitoring and multi-mode analysis according to claim 5 is characterized in that: IR windows (38) are installed at corresponding positions on the side walls of the furnace body (46) and the sample chamber (44). The two IR windows (38) are connected by a pipe and the inside of the pipe is a vacuum environment. An IR camera (41) is set at a position outside the furnace body (46) parallel to the IR window (38). The lens of the IR camera (41) is arranged facing the IR window (38) upward. The IR camera (41) is also connected to the digital terminal (42) through a signal cable.

7. The comprehensive coal thermal reaction testing device with multi-source monitoring and multi-mode analysis according to claim 6 is characterized in that: The IR window (38) is sealed and fixed by an O-ring (39) and a spring-loaded cover (40); a top cover (19) is also provided at the upper end of the sample chamber (44); a top cover (19) is also installed at the upper end of the furnace body (46) corresponding to the removal and loading position of the sample chamber (44); an oil drain valve (43) is also provided at the bottom of the furnace body (46); the other end of the oil drain valve (43) is connected to the oil bath chamber (45); the μ-GC micro gas chromatograph (36) and the NDIR non-dispersive infrared gas sensor (34) are also connected to an exhaust valve (37) through a pipeline.

8. The comprehensive coal thermal reaction testing device with multi-source monitoring and multi-mode analysis according to claim 7 is characterized in that: The programmable logic controller PLC (16) is embedded with a proportional-integral-differential regulator PID (17). The programmable logic controller PLC (16) has two analog output ports: PLC DO (14) and PLC AO (18), and an analog input port PLC AI (15). The PLC DO (14) is connected to the SSR solid-state relay (11), the micro pump (33), the solenoid valve (35), and the gear pump (9) through signal cables. The PLC AO (18) is connected to the two mass flow controllers MFC (28) via signal cables; The PLC AI (15) is connected to the temperature sensor in (7), the temperature sensor out (13), the temperature sensor (32) and the μ-GC micro gas chromatography instrument (36) through signal cables.

9. A comprehensive test method for coal thermal reaction with multi-source monitoring and multi-mode analysis, characterized in that: The comprehensive coal thermal reaction testing device with multi-source monitoring and multi-mode analysis according to claim 8 is specifically: During operation, the temperature sensor in (7) and the temperature sensor out (13) monitor the oil inlet temperature T_in and the oil outlet temperature T_out in real time and transmit them to the programmable logic controller PLC (16). The programmable logic controller PLC (16) controls the pump speed of the gear pump (9) according to the temperature difference between the temperatures T_in and T_out. The μ-GC micro gas chromatograph (36) monitors the oil inlet temperature T_in and the oil outlet temperature T_out in real time. concentration, and periodically transmits it to the programmable logic controller PLC (16), which then The concentration-controlled mass flow controller MFC (28) maintains the low oxygen permeate flow.

10. The comprehensive test method for coal thermal reaction with multi-source monitoring and multi-mode analysis according to claim 9, characterized in that: The specific implementation steps are as follows: Step 1: Place the coal sample into the sample bin (44) and level it, lock the top cover (19) in the sample bin (44), then open the top cover (19) on the furnace body (46), place the sample bin (44) through the slide rail, and then reset and lock the top cover (19) on the furnace body (46); Step 2: Add silicone oil to the oil expansion tank (1) to a liquid level of 70%, and fill it with 0.05 MPa nitrogen through the nitrogen bottle (5) to make an oil seal; Step 3: Input the ramp command SP(t) = 30°C + 1°C into the proportional-integral-derivative regulator PID (17) of the programmable logic controller PLC (16). , the end temperature is 300°C, and the flow rates of the two mass flow controllers MFC (28) are set to 100 ; Step 4, turning on the gear pump (9) to start heating, the programmable logic controller PLC (16) controls the opening of the SSR solid-state relay (11), and uses the heater (10) and the gear pump (9) to heat the oil bath at a constant speed according to the ramp. During the heating process, the programmable logic controller PLC (16) uses the temperature sensor in (7) to monitor the oil inlet temperature T_in in real time as the measured value of the proportional-integral-differential regulator PID (17) to adjust the power of the gear pump (9) in real time; During the heating process, the temperature sensor in (7) and the temperature sensor out (13) monitor the oil inlet temperature T_in and the oil outlet temperature T_out in real time and transmit them to the programmable logic controller PLC (16). If the temperature difference is greater than 2°C, the programmable logic controller PLC (16) controls the pump speed of the gear pump (9) to increase by 5Hz. If it is less than 1°C, the pump speed of the gear pump (9) is controlled to decrease by 5Hz to ensure uniform oil temperature. If the temperature difference is 1 remains unchanged; The temperature sensor (32) monitors the temperature T_coal of the gas outlet pipe (31) in real time and transmits it to the programmable logic controller PLC (16). Whenever the temperature T_coal is 30+20n°C, n=1…13, the programmable logic controller PLC (16) controls the suspension of the ramp uniform heating, then opens the solenoid valve (35) for 30s to inflate the μ-GC micro gas chromatograph (36) to analyze the gas components, and then closes the solenoid valve (35) to resume the ramp uniform heating. After the μ-GC micro gas chromatograph (36) is filled with gas, the μ-GC micro gas chromatograph (36) completes the multi-component full spectrum quantification and simultaneously The concentration is sent back to the PLC AI (15) port, and the programmable logic controller PLC (16) is based on the μ-GC micro gas chromatography instrument (36) Concentration, if If the concentration is lower than 5%, the programmable logic controller PLC (16) controls the flow rate of the mass flow controller MFC (28) of the air storage tank (30) to increase by 20 ,like If the concentration is higher than 8%, the flow rate of the mass flow controller MFC (28) controlling the air storage tank (30) is reduced by 20%. , maintain low oxygen permeability; NDIR non-dispersive infrared gas sensor (34) real-time recording and pass the data to the digital terminal (42); Step 5: When the temperature T_coal of the outlet pipe (31) reaches 300°C or the target temperature, the programmable logic controller PLC (16) controls the heater (10) to be turned off immediately through the SSR solid-state relay (11), and reduces the pump speed of the gear pump (9) to 20Hz and then cools for 15 minutes or the oil temperature reaches 100°C. Shut down after 60°C; Step 6: The digital terminal (42) generates a temperature data according to the gas-temperature coupling model based on the gas and temperature data of the μ-GC micro gas chromatograph (36), the NDIR non-dispersive infrared gas sensor (34), and the IR camera (41). 、Full t Curve, catalytic / inhibitory coefficient and 、CO、 、 、 、 、 、 Gas composition diagram.

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