Method and device for measuring temperature of coal pressurized pyrolysis gasification sample
By using flexible graphite ring sealing and internal direct temperature measurement technology, the problems of sealing failure and inaccurate temperature measurement in high-pressure reactors have been solved, achieving reaction stability and accurate temperature monitoring under high-pressure conditions, and supporting efficient coal pyrolysis/gasification experiments.
Patent Information
- Application Number
- CN202511387850.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-26
- Publication Date
- 2025-12-09
AI Technical Summary
The existing high-pressure reactor sealing structure is prone to failure, leading to media leakage. Furthermore, external temperature measurement methods cannot accurately reflect the internal temperature, affecting the stability and accuracy of coal pyrolysis/gasification reactions.
The system employs flexible graphite ring sealing and internal direct temperature measurement technology. By setting annular grooves at both ends of the reactor and using flexible graphite rings, combined with the stepped surface design of the inlet and outlet plugs, a gapless sealing interface is formed. An independent temperature measurement channel is set in the inlet plug, and the temperature sensor is directly inserted into the center of the sample for real-time monitoring.
It significantly improves sealing reliability and temperature measurement accuracy, reduces the risk of media leakage, enhances reactor safety and temperature monitoring accuracy, and supports efficient coal pyrolysis/gasification experiments.
Smart Images
Figure CN121089918A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of temperature detection in the dry distillation and drying zone of simulated underground coal gasification, and particularly relates to a coal pressurized pyrolysis gasification sample temperature measurement method and device. BACKGROUND
[0002] The energy characteristics of China are "rich in coal, poor in oil, and short of gas", which determines that coal will still account for a large proportion in the energy structure of China for a long time in the future. This is a realistic choice closely related to China's energy resource conditions, industrial development needs, and energy security protection. In the technical system of clean and efficient utilization of coal, coal pyrolysis / gasification is one of the key conversion paths, and its core is to realize the upgrading of coal from "direct combustion" to "high-value conversion" through specific process conditions. Coal pyrolysis / gasification refers to the process of thermal chemical decomposition and conversion reaction of organic matter in coal under controllable temperature, pressure, and oxygen-deficient, oxygen-rich or inert gas atmosphere, breaking the original macromolecular carbon hydrogen structure, and generating small molecule gaseous, liquid or semi-solid products. It is an important bridge connecting coal resources and clean energy, chemical raw materials.
[0003] In the development history of coal pyrolysis / gasification technology, early research mainly focused on pyrolysis reactions under normal pressure, but with the in-depth exploration of underground coal gasification (UCG) technology, the demand for pyrolysis / gasification experiments under high pressure environment has become increasingly prominent. Underground coal gasification is an in-situ conversion technology that realizes the in-situ gasification of coal by injecting gasification agents (such as oxygen and steam) into the coal seam, avoiding ground pollution and resource waste in traditional mining. However, the actual environment of underground coal gasification involves high pressure (usually more than 1 MPa), high temperature (up to more than 1000℃), and complex multiphase reaction systems, which requires laboratory simulation devices to accurately reproduce these conditions. As the core equipment, the high-pressure reactor needs to withstand long-term high-pressure working conditions while ensuring the stability and safety of the internal environment.
[0004] In the prior art, the sealing structure of the high-pressure reactor is mostly designed in a threaded nut fastening mode. This design can meet the requirements under normal pressure or low pressure conditions, but under high pressure conditions, the sealing surface is prone to generate micro gaps due to uneven stress, material fatigue or thermal expansion and contraction, resulting in leakage of high-pressure medium. This not only destroys the pressure balance of the reaction system, affects the continuity of the pyrolysis / gasification reaction and the purity of the product, but also may cause safety accidents such as explosion or toxic gas leakage. In addition, the temperature measurement scheme usually fixes the thermocouple on the outer wall of the reactor. This external temperature measurement method is limited by the thermal resistance and heat conduction delay of the wall, and cannot accurately reflect the real-time temperature of the internal sample. The coal pyrolysis / gasification process involves rapid temperature gradient and phase change reaction, and the hysteresis of external temperature measurement often leads to incorrect judgment of the reaction progress, thereby affecting process optimization and mechanism research. For example, in the dry distillation zone, a slight deviation in temperature may change the volatile release path, affecting the gasification efficiency and product composition.
[0005] Further, these shortcomings of the prior art are due to the limitations of the design concept: the sealing relies on rigid connection, ignoring the dynamic deformation under high pressure; the temperature measurement relies on indirect methods, ignoring the heterogeneous distribution inside the sample. These problems are magnified in industrial applications, restricting the large-scale promotion of coal efficient utilization technology. In view of these pain points, it is urgent to develop a new temperature measurement method that can simultaneously improve the sealing performance and temperature measurement accuracy, and ensure the stability and accuracy of coal pyrolysis / gasification under high pressure conditions. SUMMARY
[0006] Therefore, the purpose of the present application is to solve the problems of sealing failure and inaccurate temperature measurement under high pressure, and to provide a coal pressurized pyrolysis / gasification sample temperature measurement method and device, which ensures the reaction stability and data reliability through flexible sealing and internal direct temperature measurement technology.
[0007] To achieve the above purpose, the present application provides the following technical solutions:
[0008] A coal pressurized pyrolysis / gasification sample temperature measurement method, comprising the following steps:
[0009] S1, preparing a hollow structure reactor, placing a coal sample in the reactor, and providing a ring groove at both ends of the reactor, and placing a flexible sealing ring in the ring groove;
[0010] S2, fixing the gas inlet plug and the gas outlet plug to both ends of the reactor through the connecting piece, and processing a stepped surface on one end of the gas inlet plug and the gas outlet plug to form a sealing interface with the flexible sealing ring;
[0011] S3, a gas passage is provided in the center of the gas inlet plug and the gas outlet plug, and is connected with the gas inlet pipe and the gas outlet pipe respectively; an independent temperature measurement channel is provided in the gas inlet plug, and a temperature sensor probe is inserted into the reactor interior to the sample position, and is connected with an external recorder;
[0012] S4, gas is introduced, pressure is increased, and sample temperature is collected in real time to perform pyrolysis / gasification reaction.
[0013] Further, the reactor is placed in an incubator to maintain stable reaction temperature, and the incubator is fixed by a support.
[0014] Further, the flexible sealing ring is a flexible graphite ring resistant to high temperature and high pressure, and plastic deformation occurs when the connecting piece is fastened, forming a gapless sealing interface.
[0015] Further, the ring groove is coaxially machined on the flange end face of the reactor, with a diameter ranging from 4 to 8 mm and a depth ranging from 2 to 4 mm.
[0016] Further, the gas inlet plug and the gas outlet plug are cylindrical structures, and the outer diameter is in transition fit with the inner diameter of the reactor port, and the step surface is matched with the inner diameter of the ring groove.
[0017] Further, the independent temperature measuring channel is separately arranged from the gas channel to avoid interference of gas flow with temperature measurement.
[0018] Further, the temperature sensor is a thermocouple, the probe is adjusted to be inserted to the center of the sample bed, and an external temperature recorder is connected.
[0019] Further, the method is suitable for simulating temperature detection of a dry distillation drying zone of underground coal gasification, and the pressure range is 1-10 MPa, and the temperature range is 300-1200℃.
[0020] Further, the temperature sensor collects sample temperature in real time, and the recording frequency is at least 1 time per second, meeting the demand of dynamic reaction monitoring.
[0021] A coal pressurized pyrolysis and gasification sample temperature measuring device comprises a reactor, a flexible sealing ring, a gas inlet plug, a gas outlet plug, a connecting piece and a temperature sensor.
[0022] Further, an incubator and a support are further included, the reactor is located in the incubator, and the incubator is fixed and supported by the support.
[0023] Further, the flexible sealing ring is made of a flexible graphite ring, and can resist a temperature of at least 800℃ and a pressure of at least 5 MPa.
[0024] The coal pressurized pyrolysis and gasification sample temperature measuring device has the following beneficial effects:
[0025] Compared with the prior art, the present application has significant advantages in sealing performance, temperature measurement accuracy and operation reliability.
[0026] Firstly, the present application sets a ring groove at both ends of the reactor and inserts a flexible graphite ring, combined with the step surface design of the gas inlet plug and the gas outlet plug. When the connecting piece (such as a nut) is tightened, the flexible graphite ring will plastically deform, forming a gapless sealing interface. This flexible sealing mechanism effectively overcomes the problem of micro-gaps caused by uneven stress or thermal expansion and contraction under high pressure in traditional rigid sealing, significantly reducing the probability of sealing failure. Experiments show that under a high pressure environment of 1-10 MPa, the sealing reliability of the present application is improved by about 30%, effectively preventing high-pressure medium leakage and ensuring the stability of the internal pressure of the reactor. This not only guarantees the continuity of the pressurized pyrolysis / gasification reaction, reduces the reaction interruption and product contamination caused by leakage, but also significantly reduces the safety risks such as explosion or toxic gas leakage, providing higher safety protection for laboratory and industrial applications.
[0027] Secondly, in terms of temperature measurement accuracy, the present application sets up an independent temperature measurement channel in the gas inlet plug, with the thermocouple probe directly inserted into the reactor interior to the center of the sample bed. This avoids the temperature gradient and lag problems caused by the influence of the wall thermal resistance of the traditional external temperature measurement. The thermocouple collects sample temperature in real time, with a recording frequency of at least 1 time per second, which can accurately capture rapid temperature changes during pyrolysis / gasification, such as volatile release or phase transition reaction points. Compared with the temperature measurement deviation of existing technology (often exceeding 50℃), the present application controls the error within ±10℃, significantly improving the accuracy of reaction progress judgment and the precision of process parameter control. This is particularly crucial for temperature detection of the dry distillation drying zone of simulated underground coal gasification, which helps to deeply study the mechanism of coal thermochemical conversion, optimize the gasification agent injection strategy, and improve the product yield and energy conversion efficiency.
[0028] In addition, the method and device of the present application consider both operation convenience and wide applicability. The reactor is placed in a heat preservation box and fixed by a support, ensuring uniform temperature field. The independent temperature measurement channel is designed separately from the gas channel to avoid interference of gas flow with temperature measurement, further improving data reliability. The device structure is simple, the flexible graphite ring can withstand a temperature of ≥800℃ and a pressure of ≥5MPa, which is suitable for extreme working conditions and reduces maintenance costs. By solving the bottlenecks of high-pressure sealing and accurate temperature measurement, the present application enhances experimental efficiency and safety, lays a foundation for the industrialization of clean coal utilization technology, and has significant economic and environmental benefits.
[0029] Other advantages, objects, and features of the present application will be in part apparent and in part pointed out hereinafter. The objects and other advantages of the present application will be realized and attained by the structure particularly pointed out in the specification and claims hereinafter. BRIEF DESCRIPTION OF DRAWINGS
[0030] In order to make the objects, technical solutions and advantages of the present application clearer, the preferred embodiments of the present application will be described in detail below with reference to the drawings, in which:
[0031] Figure 1 Figure 1 is a schematic diagram of a temperature measuring device for a coal pressurized pyrolysis gasification sample in an embodiment of the present application.
[0032] Figure 2 Figure 2 is a schematic diagram of a ring groove at both ends of the reactor.
[0033] Figure 3 Figure 3 is a schematic diagram of a flexible graphite ring installed in the ring groove.
[0034] Figure 4 Figure 4 is a schematic diagram of a nut.
[0035] Figure 5 Figure 5 is a schematic diagram of the structure of a gas outlet plug.
[0036] Figure 6 Figure 6 is a top view of Figure 5 .
[0037] Reference signs: 1 - heat preservation box; 2 - reactor; 3 - gas inlet pipe; 4 - gas outlet pipe; 5 - temperature sensor; 6 - nut; 7 - flexible graphite ring; 8 - gas inlet plug; 9 - gas outlet plug; 10 - support. DETAILED DESCRIPTION
[0038] The present application will be described in greater detail by way of specific embodiments, from which the skilled person will readily appreciate other advantages and functionalities of the present application disclosed in the present specification. The present application can also be implemented or applied by different specific embodiments, and the details in the present specification can be modified or changed based on different views and applications without departing from the spirit of the present application. It should be noted that the drawings provided in the following embodiments only illustrate the basic concept of the present application in a schematic manner, and the following embodiments and features in the embodiments can be combined with each other without conflict.
[0039] The drawings are only used for exemplary illustration, and the representation is only a schematic diagram, not a physical diagram, and should not be understood as a limitation of the present application; in order to better illustrate the embodiments of the present application, some components in the drawings can be omitted, enlarged or reduced, and do not represent the size of the actual product; it can be understood by those skilled in the art that some well-known structures and their descriptions in the drawings can be omitted.
[0040] The same or similar reference numerals in the drawings of the embodiments of the present application correspond to the same or similar components; in the description of the present application, it should be understood that if the orientations or positional relationships indicated by the terms "upper", "lower", "left", "right", "front", "back", etc. are based on the orientations or positional relationships shown in the drawings, they are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, therefore the terms describing the positional relationship in the drawings are only used for exemplary illustration, and cannot be understood as a limitation on the present application, for those skilled in the art, the specific meanings of the above terms can be understood according to the specific circumstances.
[0041] Embodiment 1
[0042] Please refer to Figures 1-6 The present embodiment provides a coal pressurized pyrolysis and gasification sample temperature measurement method, comprising the following steps:
[0043] S1, a hollow structure reactor 2 is prepared, a coal sample is placed in the reactor 2, and a ring groove is arranged at both ends of the reactor 2, a flexible graphite ring 7 is placed in the ring groove, the flexible graphite ring 7 is made of high-temperature and high-pressure resistant graphite, and can resist a temperature of at least 800 DEG C and a pressure of at least 5 MPa; the ring groove is coaxially machined on the flange end face at both ends of the reactor 2, and has a diameter in the range of 4-8 mm and a depth in the range of 2-4 mm;
[0044] S2, the gas inlet plug 8 and the gas outlet plug 9 are fixed to both ends of the reactor 2 through the nut 6, the gas inlet plug 8 and the gas outlet plug 9 are cylindrical structures, the outer diameter is in transition fit with the inner diameter of the reactor 2 port, one end is machined with a stepped surface, which is in close contact with the flexible graphite ring 7, and plastic deformation occurs when the nut 6 is fastened, forming a gapless sealing interface, as shown in Figure 3 ;
[0045] S3, a gas passage is formed in the center of the gas inlet plug 8 and the gas outlet plug 9, and is connected with the gas inlet pipe 3 and the gas outlet pipe 4 respectively; an independent temperature measurement channel is formed in the gas inlet plug 8, the probe of the temperature sensor 5 is inserted into the inside of the reactor 2 to the sample position, and is connected with the external recording instrument; the independent temperature measurement channel is separately arranged with the gas passage to avoid the interference of gas flow with temperature measurement; the temperature sensor 5 is a thermocouple, the probe is adjusted to be inserted into the center of the sample bed layer, and is connected with the external temperature recording instrument;
[0046] S4, the gas is introduced, pressurized and heated, the sample temperature is collected in real time, and the pyrolysis / gasification reaction is carried out; the method is suitable for simulating the temperature detection of the dry distillation drying zone of underground coal gasification, the pressure range is 1-10 MPa, and the temperature range is 300-1200 DEG C; the temperature sensor 5 collects the sample temperature in real time, and the recording frequency is at least 1 time / s, which meets the demand of dynamic reaction monitoring.
[0047] The method also includes placing the reactor 2 in the incubator 1 to maintain the reaction temperature stable, and the incubator 1 is fixed by the support 10 to form stable support.
[0048] In actual operation, first, the reactor 2 is prepared according to step S1, the ring groove is processed, the flexible graphite ring 7 is placed, and the coal sample is loaded; then S2 is executed, the gas inlet plug 8, the gas outlet plug 9 and the nut 6 are assembled to ensure the tightness of the sealing interface; then S3 is executed, the gas inlet pipe 3 and the gas outlet pipe 4 are connected, and the thermocouple probe is inserted into the center of the sample; finally, S4 is executed, the gas such as oxygen or water vapor is introduced, and the temperature change is monitored in real time. The method ensures the stability of the reaction and the accuracy of the temperature data under high pressure environment through flexible sealing and internal direct temperature measurement.
[0049] Embodiment 2
[0050] Please refer to Figures 1-6 , the embodiment provides a coal pressurized pyrolysis gasification sample temperature measuring device for the method in embodiment 1, which comprises a reactor 2, a flexible graphite ring 7, a gas inlet plug 8, a gas outlet plug 9, a nut 6 and a temperature sensor 5; the reactor 2 is a hollow structure, and ring grooves are arranged at both ends of the reactor 2; the flexible graphite ring 7 is arranged in the ring grooves; the gas inlet plug 8 and the gas outlet plug 9 are connected to both ends of the reactor 2 through the nut 6, and the nut 6 is fastened to deform the flexible graphite ring 7 to form a sealing interface; the gas inlet pipe 3 and the gas outlet pipe 4 are respectively connected to the central channels of the gas inlet plug 8 and the gas outlet plug 9; the gas inlet plug 8 is also provided with an independent temperature measuring channel, and the probe of the temperature sensor 5 is inserted into the reactor 2 from the independent temperature measuring channel.
[0051] The device also comprises an incubator 1 and a support 10, and the reactor 2 is placed in the incubator 1 and is fixed and supported by the support 10.
[0052] The flexible graphite ring 7 can resist a temperature of at least 800 DEG C and a pressure of at least 5 MPa, the ring grooves are coaxial flange end faces processed on both ends of the reactor 2, the diameters range from 4 mm to 8 mm, and the depths range from 2 mm to 4 mm; the gas inlet plug 8 and the gas outlet plug 9 are cylindrical structures, the outer diameters are in transition fit with the inner diameters of the reactor 2, and the step surfaces are matched with the inner diameters of the ring grooves, as shown in Figure 3 The independent temperature measuring channel is arranged separately from the gas channel to avoid the interference of gas flow on temperature measurement; the temperature sensor 5 is a thermocouple, the probe is adjusted to be inserted into the center of the sample bed layer, and an external temperature recorder is connected; the device is suitable for simulating temperature detection of a dry distillation dry zone of underground coal gasification, the pressure range is 1-10 MPa, the temperature range is 300-1200 DEG C, and the temperature sensor 5 collects sample temperature in real time, and the recording frequency is at least 1 time per second.
[0053] In actual assembly, firstly, the ring groove of the reactor 2 is processed and the flexible graphite ring 7 is placed; then the gas inlet plug 8 and the gas outlet plug 9 are fixed through the nut 6 to form a seal; the gas inlet pipe 3 and the gas outlet pipe 4 are connected and the thermocouple is inserted; finally, the reactor 2 is placed in the heat preservation box 1 and fixed through the support 10. The device is compact in structure, reliable in sealing, accurate in temperature measurement and suitable for high-pressure pyrolysis / gasification experiments.
[0054] Finally, it should be pointed out that the above examples are only used to illustrate the technical solutions of the present application and are not limiting. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced equivalently without departing from the purpose and scope of the technical solutions, which should be covered in the scope of the claims of the present application.
Claims
1. A method for measuring the temperature of coal samples obtained through pressurized pyrolysis and gasification, characterized in that, Includes the following steps: S1. Prepare a hollow reactor, place a coal sample inside the reactor, and provide annular grooves at both ends of the reactor, with flexible sealing rings placed in the annular grooves; S2. The inlet plug and outlet plug are fixed to both ends of the reactor by connecting parts. One end of the inlet plug and outlet plug is machined with a stepped surface, which fits with the flexible sealing ring to form a sealing interface. S3. Open gas passages in the center of the inlet plug and outlet plug, and connect them to the inlet pipe and outlet pipe respectively; open an independent temperature measurement channel in the inlet plug, insert the temperature sensor probe into the reactor to the sample position, and connect it to an external recorder. S4. Introduce gas, pressurize and heat it, collect sample temperature in real time, and carry out pyrolysis / gasification reaction.
2. The method according to claim 1, characterized in that, It also includes placing the reactor inside an insulated box to maintain a stable reaction temperature, the insulated box being fixed by a bracket.
3. The method according to claim 1, characterized in that, The flexible sealing ring is a high-temperature and high-pressure resistant flexible graphite ring. When it is fastened by the connector, it undergoes plastic deformation to form a gapless sealing interface.
4. The method according to claim 1, characterized in that, The annular groove is coaxially machined on the flange end faces at both ends of the reactor, with a diameter ranging from 4 to 8 mm and a depth ranging from 2 to 4 mm.
5. The method according to claim 1, characterized in that, The inlet and outlet plugs are cylindrical structures with an outer diameter that transitions to the inner diameter of the reactor port, and the stepped surface matches the inner diameter of the annular groove.
6. The method according to claim 1, characterized in that, The independent temperature measurement channel is set separately from the gas path channel to avoid gas flow interfering with temperature measurement.
7. The method according to claim 1, characterized in that, The temperature sensor is a thermocouple, and the probe is adjusted to the center of the sample bed and connected to an external temperature recorder.
8. The method according to claim 1, characterized in that, The method is applicable to temperature detection in simulated underground coal gasification and dry distillation zones, with a pressure range of 1-10 MPa and a temperature range of 300-1200℃.
9. The method according to claim 1, characterized in that, The temperature sensor collects the sample temperature in real time, recording at a frequency of at least once per second, to meet the requirements of dynamic reaction monitoring.
10. An apparatus for the method of claim 1, characterized in that, The reactor includes a flexible sealing ring, an inlet plug, an outlet plug, a connector, and a temperature sensor. The reactor has annular grooves at both ends, and the flexible sealing ring is placed in the annular grooves. The inlet plug and the outlet plug are connected to both ends of the reactor through the connector, and when the connector is fixed, it deforms the flexible sealing ring to form a sealing interface. The inlet pipe and the outlet pipe are respectively connected to the central channels of the inlet plug and the outlet plug. The inlet plug also has an independent temperature measurement channel, through which the temperature sensor probe extends into the reactor.
11. The apparatus according to claim 10, characterized in that, It also includes an insulated box and a support frame, with the reactor located inside the insulated box, which is fixed by the support frame.
12. The apparatus according to claim 10, characterized in that, The flexible sealing ring is made of flexible graphite and can withstand temperatures of at least 800°C and pressures of at least 5 MPa.