A sampling protection device and method for magnetic particles in high-temperature gas-solid two-phase flow

Abstract

The present invention discloses a sampling protection device for high-temperature gas-solid two-phase flow magnetic particles and a method for using the same. The device includes a particle sampling device, an oxygen analysis device, a rapid cooling device, and an inert gas distribution device. The particle sampling probe isolates the atmosphere in the high-temperature reaction environment as much as possible on the one hand, and provides a certain amount of inert gas to dilute the active gas that may exist around the particles on the other hand. The particle rapid cooling device benefits from the high heat exchange efficiency between particles and uses low-temperature bed materials to achieve rapid cooling of the sampled particles, which further reduces the possibility of reaction between the sampled particles and the active gas. This device is different from the traditional simple sampling method and is used for the observation and sampling of ferromagnetic particles in high-temperature multiphase catalytic reactions. It can achieve surface structures and chemical properties of sampled particles that are closer to the actual conditions of the particles during the reaction process.

Description

Technical Field

[0001] The invention relates to a sampling protection device and method for high-temperature gas-solid two-phase flow magnetic particles, belonging to the field of energy and chemical industry. Background Art

[0002] Many reactions in the chemical and combustion fields are different from the external reaction environment and the sampling particles are easy to react with active gases such as oxygen, so it is impossible to correctly measure the surface structure and properties of solid particles in the reaction by directly sampling the particles.

[0003] Metals and their oxides have attracted extensive attention from scientists due to their catalytic effects in chemical production and pollutant removal. Compared with traditional precious metal catalysts, iron and its oxides have good catalytic activity in desulfurization and hydrocarbon activation, and are cheap and environmentally friendly. However, the multiple valence states of iron oxides and their characteristics of reaction with oxygen make it possible for the surface structure and valence state of surface substances to change once the high-temperature iron powder contacts active gases such as oxygen. Therefore, the method of directly taking out the high-temperature ferromagnetic particles from the furnace cannot reflect the true nature of the particles because they are easily oxidized. For multiphase catalytic reactions, the structure and activity of the particle surface largely determine the overall catalytic effect of the particles. In view of this, it is necessary to design a special sampling device to achieve the correct observation of the surface structure and surface valence state of the ferromagnetic particle catalyst. Summary of the invention

[0004] The present invention aims to provide a sampling protection device and sampling method for high-temperature gas-solid two-phase flow magnetic particles, the core content of which is the sampling protection of magnetic particles and the rapid cooling of magnetic particles. The sampled particles of this method can correctly reflect the surface structure and chemical properties of the particles in the reaction environment. The device is suitable for particle sampling in reducing reaction atmosphere and particle sampling in reducing-oxidizing alternating atmosphere.

[0005] The present invention designs a set of particle sampling probes equipped with inert gas and a system and sampling method for rapid particle cooling for magnetic particles in high-temperature gas-solid two-phase flow. On the one hand, the particle sampling probe isolates the atmosphere in the high-temperature reaction environment as much as possible, and on the other hand, provides a certain amount of inert gas to dilute the active gas that may exist around the particles. The particle rapid cooling device benefits from the high heat exchange efficiency between particles. The low-temperature bed material can be used to achieve rapid cooling of the sampled particles, which further reduces the possibility of reaction between iron and its oxide particles and active gases. Different from the traditional simple sampling method, this device is used for the observation and sampling of ferromagnetic particles in high-temperature multiphase catalytic reactions, and can achieve the surface structure and chemical properties of the sampled particles closer to the actual situation of the particles during the reaction process.

[0006] The present invention provides a sampling and protection device for high-temperature gas-solid two-phase flow magnetic particles, comprising a particle sampling device, an oxygen analysis device, a rapid cooling device, and an inert gas distribution device;

[0007] The particle sampling device includes a particle sampling probe, a particle sampling tube, a heat-insulating protective layer, a stainless steel valve and four pressure gauges; a heat-insulating protective layer is provided on the outer layer of the particle sampling tube in a high-temperature environment, including a heat-insulating layer and a steel pipe outside the heat-insulating layer; the inner diameter of the particle sampling tube is 10 to 50 mm, which is adjusted according to the sampling conditions. A first pressure gauge and a second pressure gauge are respectively provided in front of the stainless steel valve and near the rapid cooling device to monitor the flow direction of particles at the rear of the particle sampling tube; a third pressure gauge and a fourth pressure gauge are also provided at the front end of the particle sampling probe and the outer wall of the heat-insulating protective layer to detect the reliability of the first inert gas isolating the reaction atmosphere;

[0008] The particle sampling probe is connected to the first inert gas pipeline and the second inert gas pipeline respectively. The particle sampling probe is located at the front end of the particle sampling tube. The sampled high-temperature particles enter the particle sampling probe and first contact with the second inert gas and then contact with the first inert gas. The second inert gas basically isolates the high-temperature reaction atmosphere. The first inert gas dilutes the active gas near the particles and allows the particles to quickly enter the rapid cooling device.

[0009] The oxygen analysis device includes an oxygen analyzer, a gas sampling tube, a filter screen, a first solenoid valve and a second solenoid valve; the oxygen analyzer is controlled by the opening and closing states of the first solenoid valve and the second solenoid valve to extract gas from different positions for sampling and analysis; the oxygen analyzer uses a trace oxygen analysis device. Furthermore, a paramagnetic oxygen analyzer can be used for places that contain almost no nitrogen oxides; a fuel cell analyzer or an infrared flue gas analyzer can be used for places that contain nitrogen oxides or where sampling requires extremely low oxygen content.

[0010] The rapid cooling device includes a stainless steel barrel, bed material, air distribution plate, a first thermocouple, a second thermocouple, a filter plate, and an eighth pressure gauge; the first thermocouple and the second thermocouple are placed on the side of the stainless steel barrel to monitor the temperature of the bottom particles and the upper airflow respectively. During the sampling process, the temperature of the thermocouples should be lower than 100 ° C to ensure that the ferromagnetic particles sampled in the high temperature environment can be quickly cooled; the stainless steel barrel is built with bed material, and the bed material uses experimental bed material or quartz sand; the filter plate uses a combination of sintered quartz plate and orifice plate, or a combination of multiple screens and orifice plates, and the screen should be selected above 1000 mesh; the particle cooling process is as follows: the high-temperature particles enter the stainless steel barrel under the protection of the first inert gas, and the bed material in the stainless steel barrel is in a fluidized state and the temperature is low. After the high-temperature particles are mixed with the bed material, they are quickly cooled due to the high heat exchange coefficient between the particles. Further, the air distribution plate uses a small hood air distribution plate or a sintered quartz plate. It should be noted that the use of the sintered quartz plate needs to be combined with the orifice plate to ensure its strength. The stainless steel barrel is made of 3101 stainless steel with a wall thickness of 2 to 5 mm; the thermocouple preferably uses a copper-constantan thermocouple (T-type thermocouple) with good low-temperature sensitivity. The container volume of the rapid cooling device is determined according to the total mass of the sampled particles. The total volume of the container is three to four times the volume of the initial bed material, and the initial bed material volume is more than five times the volume of the sampled particles. The mass of the sampled particles can be estimated by the change in the difference between the eighth pressure gauge and the tenth pressure gauge before and after sampling. The change in the difference between the pressure gauges before and after sampling is equal to the weight of the sampled particles divided by the inner cross-sectional area of ​​the stainless steel barrel.

[0011] The inert gas distribution device is a pressure and flow control device for the entire sampling device, which can be described in five ways: the first way is the first inert gas path, the second way is the second inert gas path, the third way is the inert gas flow path, the fourth way is the inert gas purge path, and the non-inert gas path - the fifth way is the tail vacuum path. The first to fourth ways are respectively equipped with a pressure reducing valve, a pressure regulating tank, a pressure gauge and a solenoid valve. Each pipeline component is connected by an inert gas pipeline, and the inner diameter of the inert gas pipeline is 3 to 20 mm.

[0012] Furthermore, the inert gas uses an inert gas with a purity of more than 99.99%. The first inert gas is compressed from an inert gas tank, passes through the tenth solenoid valve, the third flowmeter, the four-way pipe, the ninth solenoid valve, the three-way pipe, the second pressure reducing valve, the second pressure stabilizing tank, the second flowmeter, and the fourth solenoid valve, and finally reaches the first inert gas nozzle. The flow rate of the first inert gas at the air distribution plate of the sampling probe should be maintained at more than 2 m / s. The second inert gas is compressed from an inert gas tank, passes through the tenth solenoid valve, the third flowmeter, the four-way pipe, the ninth solenoid valve, the three-way pipe, the first pressure reducing valve, the first pressure stabilizing tank, the first flowmeter, and the third solenoid valve, and finally reaches the second inert gas outlet. The wind speed of the second inert gas in the thick tube of the No. 2 sampling probe is 0.1 ~ 0.2 m / s, and the wind speed in the thin tubes of the No. 1 sampling probe and the No. 3 sampling probe is 0.5 ~ 1.5 m / s. The inert gas fluidizing air is supplied from the inert gas compression tank, passes through the tenth solenoid valve, the third flow meter, the four-way pipe, the eighth solenoid valve, the fourth pressure reducing valve, the fourth pressure stabilizing tank, and the seventh solenoid valve, and is evenly distributed through the air distribution plate and finally enters the rapid cooling device. The inert gas purge air route consists of a four-way pipe, the sixth solenoid valve, the third pressure reducing valve, the third pressure stabilizing tank, and the fifth solenoid valve. The fifth solenoid valve is opened intermittently to achieve regular removal of the bed material attached to the filter plate. The fifth solenoid valve can be opened once every 15 seconds through the program setting, and the purge time each time is 1 second. The tail vacuum air route quickly removes the gas in the rapid cooling device to maintain the stability of the flow field of the particle sampling system. The tail vacuum air route includes: an exhaust pipeline and a mechanical pump. The exhaust pipeline is connected to a gas sampling tube connected to the flue gas analyzer. The gas in the rapid cooling device enters the exhaust pipe through the filter plate and finally enters the atmosphere through the mechanical pump. In order to avoid the problem of oxygen backflow in the exhaust pipe caused by the thermal motion of air molecules, the air flow in the exhaust pipe needs to maintain an appropriate flow rate. The appropriate flow rate is selected by closing the stainless steel valve, the first solenoid valve, and the ninth solenoid valve, and opening the tenth solenoid valve, the eighth solenoid valve, the seventh solenoid valve, the sixth solenoid valve, the fifth solenoid valve, and the second solenoid valve. The gas flow rate is adjusted to the same as the sampling state, the oxygen analyzer is turned on and the reading is stabilized, and the fluidization wind speed is adjusted to make the oxygen content lower than 100 ppm. At this time, the gas flow rate of the exhaust pipe can meet the requirements.

[0013] The particle sampling probe has three forms, including any of the following structures:

[0014] The No. 1 sampling probe comprises a No. 1 sampling probe thick tube, the two sides of the No. 1 sampling probe thick tube are respectively connected to the two wing thick tubes, the No. 1 sampling probe thick tube elbows are arranged at the ends of the two wing thick tubes, the sampling probe air distribution plates are arranged in the middle of the two wing thick tubes, the No. 1 sampling probe particle inlet pipe is arranged at the bottom of the thick tube, the No. 1 sampling probe thin tube is arranged in the middle of the thick tube, the No. 1 sampling probe thin tube is the second inert gas inlet pipe, the No. 1 sampling probe thin tube is connected to the center of the thick tube, the No. 1 sampling probe thin tube elbow is arranged inside, the bottom outlet of the thin tube is provided with a cone, the cone is supported by the No. 1 sampling probe cone support rod, and the top of the support rod is connected to the thin tube elbow; the thick tube is connected to the first inert gas pipeline, and the thin tube is connected to the second inert gas pipeline;

[0015] The No. 2 sampling probe comprises a first inert gas thick tube of the No. 2 sampling probe and a second inert gas thick tube of the No. 2 sampling probe. Two wing thick tubes are respectively arranged obliquely downward on both sides of the two thick tubes, and the two are butt-jointed and combined into one body. Thick tube elbows are respectively arranged at the ends of the two wing thick tubes, and the elbow of the first inert gas thick tube is arranged downward, and the elbow of the second inert gas thick tube is arranged upward, and the two wing thick tubes at the upper part are staggered with the two wing thick tubes at the lower part; sampling probe air distribution plates are respectively arranged in the middle of the two wing thick tubes, and the structure of the sampling probe air distribution plates is the same as that of the No. 1 sampling probe.

[0016] The No. 3 sampling probe includes an annular wind chamber and a No. 3 sampling probe thick tube. The upper part is the No. 3 sampling probe thick tube. The middle of the sampling probe thick tube is provided with a No. 3 sampling probe thin tube, which is the second inert gas inlet pipe. The No. 3 sampling probe thin tube is provided with a No. 3 sampling probe thin tube elbow at the center of the thick tube. A cone is provided at the bottom of the No. 3 sampling probe thin tube. The cone is connected to the thin tube elbow through the No. 3 sampling probe cone support rod. The bottom of the No. 3 sampling probe thick tube is connected to the No. 3 sampling probe particle inlet pipe; the lower part of the No. 3 sampling probe thick tube is connected to the No. 3 sampling probe annular wind chamber through a sideways inclined tube; the connection between the No. 3 sampling probe thick tube and the inclined tube is provided with a sampling probe air distribution plate, which is made of the same material as the No. 1 sampling probe and arranged in a vertical pipeline; the No. 3 sampling probe annular wind chamber is connected to the No. 3 sampling probe first inert gas inlet pipe.

[0017] Furthermore, the gas flow rate of the first inert gas at the air distribution plate of the sampling probe needs to be greater than 2 m / s, the wind speed of the second inert gas in the thick tube of the No. 2 sampling probe is 0.1 ~ 0.2 m / s, and the wind speed in the thin tubes of the No. 1 sampling probe and the No. 3 sampling probe is 0.5 ~ 1.5 m / s.

[0018] The present invention also provides a method for using the above-mentioned high-temperature gas-solid two-phase flow magnetic particle sampling protection device, and the specific operation process is as follows:

[0019] First pre-experiment: The purpose of this pre-experiment is to find the appropriate fluidization wind speed and the appropriate exhaust pipe diameter: close the stainless steel valve, the first solenoid valve, and the ninth solenoid valve, open the tenth solenoid valve, the eighth solenoid valve, the seventh solenoid valve, the sixth solenoid valve, the fifth solenoid valve, and the second solenoid valve, adjust the gas flow rate to the same as the sampling state, turn on the oxygen analyzer and stabilize the reading, and adjust the fluidization wind speed to make the oxygen content less than 100 ppm. If it is difficult to obtain a suitable flow rate through the above adjustments, it is necessary to change the exhaust pipe diameter and re-adjust the above adjustments.

[0020] Second pre-experiment: In this step, the appropriate gas parameters of the two inert gases at the particle sampling probe are obtained by adjustment. Place the particle sampling probe in the sampling environment, close the second solenoid valve, open all other valves, adjust the inert gas flow path, inert gas purge path and mechanical pump to the appropriate state of the first pre-experiment, and turn on the oxygen analyzer at the same time. Constantly adjust the first pressure reducing valve, the second pressure reducing valve, the third solenoid valve, and the fourth solenoid valve so that the reading of the third pressure gauge is 10~50 Pa higher than that of the fourth pressure gauge, and the reading of the first pressure gauge is 100~500 Pa higher than that of the second pressure gauge. Among them, the third and fourth pressure gauges may have large fluctuations due to their proximity to the reaction area. At this time, the gas parameters should be adjusted with the highest pressure as the reference point. During the adjustment process, pay attention to the reading of the oxygen analyzer, and the oxygen content must be lower than 1000 ppm.

[0021] Precooling of the rapid cooling device: Replace the bed material used in the previous two pre-experiments, set up the particle sampling probe, close the stainless steel valve, the second solenoid valve, and the first solenoid valve, connect the inert gas flow gas path and the inert gas purge gas path, and start the mechanical pump. Observe the first thermocouple and the second thermocouple, and the precooling is considered to be completed when the temperature is below 0°C.

[0022] Sampling starts: First, open the two inert gases at the sampling probe, adjust the gas velocity and pressure to a value higher than the set value, open the stainless steel valve and the first solenoid valve, and preheat the oxygen analyzer; then slowly adjust the first and second inert gases to the set parameters, and sampling officially begins. During the sampling process, ensure that the reading of the third pressure gauge is 10~50 Pa higher than that of the fourth pressure gauge, and the reading of the first pressure gauge is 100~500 Pa higher than that of the second pressure gauge.

[0023] Sampling is finished: when the particle sampling reaches the required mass or the thermocouple temperature is higher than 100 ℃, the sampling is finished. When sampling is finished, first close the stainless steel valve, the ninth solenoid valve and all related inert gases at the sampling probe, keep the remaining pipelines open until the bed material temperature drops to 0 ℃; then close all valves of the sampling device.

[0024] Magnetic particle screening: Take out the bed material mixed with magnetic particles and use a strong magnet or magnetic separator to screen out the magnetic particles.

[0025] Beneficial effects of the present invention:

[0026] (1) All three particle sampling probes can basically isolate the reaction atmosphere around the particles and provide inert gas to protect high-temperature particles.

[0027] (2) Compared with the existing cooling devices, the small fluidized bed cooling device of the present invention can achieve rapid cooling of the sampled particles by means of heat exchange between gas and particles and heat exchange between particles.

[0028] (3) The present invention adopts a method of adjusting the diameter of the exhaust pipe in the pre-experimental stage to eliminate the possible effects of thermal motion of air molecules. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a schematic diagram of the structure of the sampling protection device for high-temperature gas-solid two-phase flow magnetic particles of the present invention.

[0030] Figure 2 This is a stereoscopic image of the particle sampling probe No. 1.

[0031] Figure 3 This is the front view of particle sampling probe No. 1.

[0032] Figure 4 for Figure 3 sectional view of .

[0033] Figure 5 for Figure 3 Right view of .

[0034] Figure 6 for Figure 5 sectional view of .

[0035] Figure 7 This is a stereoscopic image of the No. 2 particle sampling probe.

[0036] Figure 8 This is the front view of the No. 2 particle sampling probe.

[0037] Fig. 9 for Figure 8 sectional view of .

[0038] Fig.10 for Figure 8 Right view of .

[0039] Fig.11 for Fig.10 sectional view of .

[0040] Fig.12 This is a stereoscopic image of the No. 3 particle sampling probe.

[0041] Fig.13 This is the front view of the No. 3 particle sampling probe.

[0042] Fig.14 for Fig.13 sectional view of .

[0043] Fig.15 for Fig.13 Left view of .

[0044] Fig.16 for Fig.15 sectional view of .

[0045] In the figure: 1-first inert gas nozzle; 2-second inert gas nozzle; 3-particle sampling tube; 4-insulation layer; 5-insulation outer steel pipe; 6-first pressure gauge; 7-stainless steel valve; 8-oxygen analyzer; 9-gas sampling tube; 10-first solenoid valve; 11-filter screen; 12-second pressure gauge; 13-second solenoid valve; 14-third pressure gauge; 15-fourth pressure gauge; 16-third solenoid valve; 17-first flow meter; 18-first pressure stabilizing tank; 19-fifth pressure gauge; 20-first pressure reducing valve; 21-fourth solenoid valve; 22-second flow meter; 23-second pressure stabilizing tank; 24-sixth Pressure gauge; 25-second pressure reducing valve; 26-three-way pipe; 27-filter plate; 28-first thermocouple; 29-stainless steel barrel; 30-bed material; 31-second thermocouple; 32-air distribution plate; 33-fifth solenoid valve; 34-third pressure stabilizing tank; 35-seventh pressure gauge; 36-third pressure reducing valve; 37-sixth solenoid valve; 38-eighth pressure gauge; 39-seventh solenoid valve; 40-fourth pressure stabilizing tank; 41-ninth pressure gauge; 42-fourth pressure reducing valve; 43-eighth solenoid valve; 44-inert gas pipeline; 45-ninth solenoid valve; 46-four-way pipe; 47-third flow meter; 48-tenth solenoid valve; 49-inert gas compression tank; 50-exhaust pipe; 51-mechanical pump; 52-the tenth pressure gauge; 53-air distribution plate of sampling probe; 54-cone; 55-thick tube of sampling probe No. 1; 56-thin tube elbow of sampling probe No. 1; 57-thin tube of sampling probe No. 1; 58-cone support rod of sampling probe No. 1; 59-thick tubes on both wings of sampling probe No. 1; 60-thick tube elbow of sampling probe No. 1; 61-particle inlet pipe of sampling probe No. 1; 62-second inert gas inlet pipe of sampling probe No. 1; 63-first inert gas thick tube of sampling probe No. 2; 64-first inert gas thick tubes on both wings of sampling probe No. 2; 65-second 66-the first inert gas thick tube elbow of the No. 2 sampling probe; 67-the second inert gas thick tube of the No. 2 sampling probe; 68-the particle inlet pipe of the No. 2 sampling probe; 69-the second inert gas thick tube elbow of the No. 2 sampling probe; 70-the thick tube of the No. 3 sampling probe; 71-the thin tube elbow of the No. 3 sampling probe; 72-the thin tube of the No. 3 sampling probe; 73-the cone support rod of the No. 3 sampling probe; 74-the annular wind chamber; 75-the first inert gas inlet pipe of the No. 3 sampling probe; 76-the particle inlet pipe of the No. 3 sampling probe; 77-the second inert gas inlet pipe of the No. 3 sampling probe; 78-the inclined tube. A is the particle movement direction, and B is the particle sampling probe. DETAILED DESCRIPTION

[0046] The present invention is further illustrated by the following examples, but is not limited to the following examples.

[0047] Embodiment 1:

[0048] like Figures 1 to 7As shown, a sampling and protection device for high-temperature gas-solid two-phase flow magnetic particles includes a particle sampling device, an oxygen analysis device, a rapid cooling device, and an inert gas distribution device;

[0049] The particle sampling device is a simple reaction atmosphere isolation device, including a particle sampling probe equipped with an inert gas, a particle sampling tube 3, the inert gas includes a first inert gas, a second inert gas and a matching gas path; an inert gas that does not react with particles should be selected. The first inert gas moves in the same direction as the particles to ensure the movement of the particles in the pipeline; the second inert gas flows in the opposite direction to the particle movement to isolate the reaction atmosphere; the particle sampling probe includes any of the following, which is used for different types of particle sampling:

[0050] The No. 1 sampling probe comprises a No. 1 sampling probe thick tube 55, the two sides of the No. 1 sampling probe thick tube 55 are respectively connected to the No. 1 sampling probe two wing thick tubes 59, the No. 1 sampling probe thick tube elbows 60 are arranged at the ends of the No. 1 sampling probe two wing thick tubes 59, the sampling probe air distribution plates 53 are arranged in the middle of the two wing thick tubes, the No. 1 sampling probe particle inlet pipe 61 is arranged at the bottom of the thick tube, the No. 1 sampling probe thin tube 57 (that is, the No. 1 sampling probe second inert gas inlet pipe 62) is arranged in the middle of the thick tube, the No. 1 sampling probe thin tube 57 is connected to the center of the thick tube, the No. 1 sampling probe thin tube elbow 56 is arranged inside, the bottom outlet of the thin tube is provided with a cone 54, the cone is supported by the No. 1 sampling probe cone support rod 58, and the top of the support rod is connected to the thin tube elbow; the thick tube is connected to the first inert gas pipeline, and the thin tube is connected to the second inert gas pipeline.

[0051] The first inert gas of the No. 1 sampling probe enters through the No. 1 sampling probe thick tube elbow 60, which is connected to the inert gas pipeline 44 and controlled by the fourth electromagnetic valve 21; the direction of the first inert gas nozzle is consistent with the direction of particle movement, and the end of the nozzle is provided with a sampling probe air distribution plate 53, which is composed of an air distribution hole plate and a screen, and the screen aperture is 1000 mesh or more; the second inert gas enters through the No. 1 sampling probe second inert gas inlet pipe 62, which is connected to the inert gas pipeline 44 and controlled by the third electromagnetic valve 16; the second inert gas enters through the thin tube, and there is a cone 54 at the second inert gas outlet for dispersing the inert gas. The diameter of the particle sampling probe thick tube and the diameter of the first inert gas nozzle are consistent with the diameter of the particle sampling tube, and the outer diameter of the particle sampling probe thin tube is 1 / 3 to 1 / 4 of the diameter of the sampling probe thick tube.

[0052] The No. 2 sampling probe comprises a first inert gas thick tube 63 of the No. 2 sampling probe and a second inert gas thick tube 67 of the No. 2 sampling probe, and the two are butted up and down to form an integral body. The first inert gas thick tube 63 of the No. 2 sampling probe is provided with a first inert gas two-wing thick tube 64 of the No. 2 sampling probe obliquely downward, and the second inert gas thick tube 67 of the No. 2 sampling probe is provided with a second inert gas two-wing thick tube 66 of the No. 2 sampling probe obliquely upward. Thick tube elbows are respectively provided at the ends of the two-wing thick tubes, and the first inert gas thick tube elbow 65 of the No. 2 sampling probe is arranged downward, and the second inert gas thick tube elbow 69 of the No. 2 sampling probe is arranged upward, and the upper two-wing thick tube 64 is staggered with the lower two-wing thick tube 68; sampling probe air distribution plates 53 are respectively provided in the middle of the two-wing thick tubes, and the structure of the sampling probe air distribution plates is the same as that of the No. 1 sampling probe.

[0053] like Fig. 9 As shown, a first inert gas thick tube 63 of the No. 2 sampling probe is provided above the No. 2 sampling probe, and both sides of the first inert gas thick tube 63 of the No. 2 sampling probe are connected to thick tube elbows through two wing thick tubes obliquely downward, and the bottom of the first inert gas thick tube 63 of the No. 2 sampling probe is connected to the second inert gas thick tube 67 of the No. 2 sampling probe, and the bottom of the second inert gas thick tube 67 of the No. 2 sampling probe is the particle inlet pipe 68 of the No. 2 sampling probe, and second inert gas thick tube elbows 69 of the No. 2 sampling probe are obliquely provided on both sides of the second inert gas thick tube 67 of the No. 2 sampling probe, and the deflection angle between the second inert gas thick tube elbow 69 of the No. 2 sampling probe and the first inert gas thick tube elbow 65 of the No. 2 sampling probe is 90°, and sampling probe air distribution plates 53 are respectively provided in the middle of the thick tube elbows, and the structure of the sampling probe air distribution plates is the same as that of the No. 1 sampling probe.

[0054] The first inert gas of the No. 2 particle sampling probe enters through the first inert gas thick pipe elbow 65 of the No. 2 sampling probe, which is connected to the inert gas pipeline 44 and controlled by the fourth solenoid valve 21; the direction of the first inert gas is consistent with the direction of particle movement, and a wind distribution plate and a screen are arranged at the end of the nozzle, and the screen aperture is 1000 mesh or more; the second inert gas of the No. 2 particle sampling probe enters through the second inert gas thick pipe elbow 69 of the No. 2 sampling probe, which is connected to the inert gas pipeline 44 and controlled by the third solenoid valve 16; the direction of the second inert gas is opposite to the direction of particle movement, and the end of the nozzle is a wind distribution plate and a screen, and the screen aperture is 1000 mesh or more. The diameter of the particle sampling probe thick pipe, the diameter of the first inert gas two-wing thick pipe, and the diameter of the second inert gas two-wing thick pipe are consistent with the diameter of the particle sampling pipe.

[0055] The No. 3 sampling probe includes an annular air chamber 74 and a No. 3 sampling probe thick tube 70, the upper part of which is the No. 3 sampling probe thick tube 70, the middle of which is provided with a No. 3 sampling probe thin tube 72 (i.e., the No. 3 sampling probe second inert gas inlet tube 77), the No. 3 sampling probe thin tube 72 is provided with a No. 3 sampling probe thin tube elbow 71 at the center of the thick tube, the bottom of the No. 3 sampling probe thin tube 72 is provided with a cone 54, the cone is connected to the thin tube elbow through the No. 3 sampling probe cone support rod 73, and the No. 3 sampling probe is connected to the No. 3 sampling probe. The bottom of the sampling probe thick tube is connected to the particle inlet pipe 76 of the No. 3 sampling probe; the bottom of the No. 3 sampling probe thick tube is connected to the No. 3 sampling probe annular air chamber 74 through a sideways inclined tube 78, and a sampling probe air distribution plate is provided in the middle of the inclined tube 78. The sampling probe air distribution plate is made of the same material as the No. 1 sampling probe, and its vertical pipeline layout is different in shape due to different pipelines; the No. 3 sampling probe annular air chamber is connected to the first inert gas inlet pipe of the No. 3 sampling probe, and the thin tube is connected to the second inert gas pipeline.

[0056] The first inert gas of the No. 3 particle sampling probe enters through the first inert gas inlet pipe 75 of the No. 3 sampling probe, which is connected to the inert gas pipeline 44 and controlled by the fourth solenoid valve 21; the direction of the first inert gas of the No. 3 sampling probe is consistent with the direction of particle movement, and the air distribution plate adopts a combination of an air distribution hole plate and a screen, and the screen aperture is 1000 mesh or more; the second inert gas of the No. 3 particle sampling probe enters through the second inert gas inlet pipe 77 of the No. 3 sampling probe, which is connected to the inert gas pipeline 44 and controlled by the third solenoid valve 16; the second inert gas nozzle enters through the thin tube, and there is a cone at the outlet of the thin tube for dispersing the second inert gas. The air inlet area of ​​the first inert gas nozzle is equal to the cross-sectional area of ​​the thick tube of the particle sampling probe, and the outer diameter of the thin tube of the particle sampling probe is 1 / 3 to 1 / 4 of the diameter of the thick tube of the sampling probe.

[0057] The oxygen analysis device includes an oxygen analyzer 8, which is connected to a gas sampling tube 9. The gas sampling tube 9 is respectively connected to a straight section of a particle sampling tube and an exhaust pipe 50. A first solenoid valve 10 and a filter screen 11 are provided on the tube connected to the straight section of the particle sampling tube, and a second solenoid valve 13 is provided on the pipe connected to the exhaust pipe.

[0058] The rapid cooling device includes a stainless steel barrel 29, a bed material 30, an air distribution plate 32, a first thermocouple 28, a second thermocouple 31, a filter plate 27, and an eighth pressure gauge 38. The filter plate 27 is provided on the top of the stainless steel barrel 29, and the first thermocouple 28 and the second thermocouple 31 are connected in the middle. The bed material 30 is built into the stainless steel barrel 29, and an air distribution plate 32 is provided at the bottom of the bed material 30; the bottom of the stainless steel barrel is connected to the inert gas flow gas path, and the top is connected to the inert gas purge gas path. The stainless steel barrel is an integral body from the filter plate 27 to the air distribution plate 32, and a hole is opened on the side thereof, and a thermometer is installed. The bed material is placed on the air distribution plate 32, and the bed material is directly and loosely piled on the air distribution plate, and the bed material plays a cooling role: the inert gas fluidizes the bed material, and the bed material is mixed with the sampled particles to achieve the purpose of rapidly cooling the sampled particles.

[0059] The inert gas distribution device includes five gas paths: the first path is the first inert gas path, the second path is the second inert gas path, the third path is the inert gas flow path, the fourth path is the inert gas purge path, and the fifth path is the tail vacuum gas path; wherein the inert gas distribution device provides inert gas for the first to fourth paths.

[0060] The first inert gas path and the second inert gas path are connected to the particle sampling probe respectively, the third inert gas flow gas path is connected to the bottom of the stainless steel barrel, the fourth inert gas purge gas path is connected to the top of the stainless steel barrel, and the fifth tail vacuum gas path is connected to the top of the stainless steel barrel.

[0061] The present invention provides a sampling protection device for high-temperature gas-solid two-phase flow magnetic particles, which specifically includes the following:

[0062] The particle sampling device comprises a particle sampling probe, a particle sampling tube 3, a heat-insulating protective layer, a stainless steel valve 7 and four pressure gauges (a first pressure gauge 6, a second pressure gauge 12, a third pressure gauge 14 and a fourth pressure gauge 15). The particle sampling probe is connected to the particle sampling tube 3. The particle sampling tube 3 comprises a curved tube section and a straight tube section. The straight tube section is provided with a stainless steel valve 7. The outer curved tube section of the particle sampling tube in a high-temperature environment is provided with a heat-insulating layer 4. The outer side of the heat-insulating layer 4 is provided with a heat-insulating layer outer steel pipe 5. The particle sampling tube, the particle sampling probe and the heat-insulating layer outer steel pipe are made of 3101 stainless steel or high-temperature resistant ceramics. The inner diameter of the particle sampling tube is 10-50 mm, which is adjusted according to the sampling conditions. The stainless steel valve adopts a gate valve or a ball valve, and cannot use a complex structure such as a check valve. The valve state has only two states: fully open and closed. The first pressure gauge 6 and the second pressure gauge 12 are respectively arranged about 10 cm in front of the stainless steel valve and close to the rapid cooling device to monitor the flow direction of particles at the rear of the particle sampling tube. A third pressure gauge and a fourth pressure gauge are also provided at the front end of the particle sampling probe and the outer wall of the thermal insulation protective layer to detect the reliability of the first inert gas isolating the reaction atmosphere. The specific location of the third pressure gauge is 2 to 10 cm from the inlet of the particle sampling tube.

[0063] Specifically, there are three types of particle sampling probes (see the attached figure for their structures). The particle sampling probe is located at the front end of the particle sampling tube. When high-temperature particles enter the particle sampling probe, they first come into contact with the second inert gas and then with the first inert gas. The second inert gas achieves basic isolation from the high-temperature reaction atmosphere. The wind speed of the second inert gas in the thick tube of the No. 2 sampling probe is 0.1 ~ 0.2 m / s, and the wind speed in the thin tubes of the No. 1 sampling probe and the No. 3 sampling probe is 0.5 ~ 1.5 m / s; the first inert gas dilutes the active gas that may exist near the particles and allows the particles to quickly enter the rapid cooling device. The gas flow rate of the first inert gas at the air distribution plate of the sampling probe must be greater than 2 m / s.

[0064] The filter screen 11 of the oxygen analysis device should be a screen with a mesh size of 1000 or more to protect the gas sampling tube and the flue gas analyzer. The oxygen analyzer is controlled by the opening and closing states of the first solenoid valve and the second solenoid valve to extract gas samples for analysis at different locations. The oxygen analyzer uses trace oxygen analysis equipment. For places that contain almost no nitrogen oxides, a paramagnetic oxygen analyzer can be used; for places that contain nitrogen oxides or require extremely low oxygen content for sampling, a fuel cell analyzer or an infrared flue gas analyzer is used.

[0065] The air distribution plate of the rapid cooling device adopts a small hood air distribution plate or a sintered quartz plate. It should be noted that the use of the sintered quartz plate needs to be combined with a perforated plate to ensure its strength. The stainless steel barrel adopts 3101 stainless steel with a wall thickness of 2~5mm. The first thermocouple and the second thermocouple are placed on the side of the stainless steel barrel to monitor the temperature of the bottom particles and the upper airflow respectively. During the sampling process, the temperature of the thermocouple should be lower than 100℃ to ensure that the ferromagnetic particles sampled in the high temperature environment can be quickly cooled. The thermocouple preferably adopts a copper-constantan thermocouple (T-type thermocouple) with good low-temperature sensitivity. The stainless steel barrel has a built-in bed material, which adopts experimental bed material or quartz sand. Note that the experimental bed material needs to remove the ferromagnetic material before use. The container volume of the rapid cooling device is determined according to the total mass of the sampled particles. The total volume of the container is three to four times the volume of the initial bed material, and the volume of the initial bed material is more than five times the volume of the sampled particles. The mass of the sampled particles can be estimated by the change in the difference between the eighth pressure gauge 38 and the tenth pressure gauge 52 before and after sampling. The change in the difference between the pressure gauges before and after sampling is equal to the mass of the sampled particles divided by the inner cross-sectional area of ​​the stainless steel barrel 29. The filter plate adopts a combination of a sintered quartz plate and a perforated plate, or a combination of multiple screens and a perforated plate. The screen should be selected with a mesh size of 1000 or more. The particle cooling process is as follows: the high-temperature particles enter the stainless steel barrel under the protection of the first inert gas. The bed material in the stainless steel barrel is in a fluidized state and has a low temperature. After the high-temperature particles are mixed with the bed material, rapid cooling is achieved due to the high heat transfer coefficient between the particles.

[0066] The inert gas distribution device is a pressure and flow control device for the entire sampling device, which can be described in five ways: the first way is the first inert gas path, the second way is the second inert gas path, the third way is the inert gasification path, the fourth way is the inert gas purge path, and the non-inert gas path - the fifth way is the tail vacuum path. The first to fourth paths are respectively equipped with a pressure reducing valve, a pressure stabilizing tank, a pressure gauge and a solenoid valve. Each pipeline component is connected by an inert gas pipeline 44, and the inner diameter of the inert gas pipeline is 3~20mm. The inert gas uses an inert gas with a purity of more than 99.99%. The first inert gas is compressed by an inert gas tank 49, passes through the tenth solenoid valve 48, the third flowmeter 47, the four-way pipe 46, the ninth solenoid valve 45, the three-way pipe 26, the first pressure reducing valve 20, the first pressure stabilizing tank 18, the first flowmeter 17, and the third solenoid valve 16, and finally reaches the first inert gas nozzle. The speed of the first inert gas outlet should be maintained at about 0.1 m / s. The second inert gas is supplied from the inert gas compression tank 49, passes through the tenth solenoid valve 48, the third flow meter 47, the four-way pipe 46, the ninth solenoid valve 45, the three-way pipe 26, the second pressure reducing valve 25, the second pressure stabilizing tank 23, the second flow meter 22, and the fourth solenoid valve 21, and finally reaches the second inert gas nozzle. The flow rate of the second inert gas outlet should be maintained above 3 m / s. The inert gas fluidizing air is supplied from the inert gas compression tank 49, passes through the tenth solenoid valve 48, the third flow meter 47, the four-way pipe 46, the eighth solenoid valve 43, the fourth pressure reducing valve 42, the fourth pressure stabilizing tank 40, and the seventh solenoid valve 39, and is evenly distributed through the air distribution plate 32 and finally enters the rapid cooling device. The inert gas purge gas route is composed of the four-way pipe 46, the sixth solenoid valve 37, the third pressure reducing valve 36, the third pressure stabilizing tank 34, and the fifth solenoid valve 33. The fifth solenoid valve is opened intermittently to achieve regular removal of the bed material attached to the filter plate 27. The fifth solenoid valve can be set to open once every 15 seconds through the program, and the purge time each time is 1 second. The tail vacuum air circuit quickly removes the gas in the rapid cooling device to maintain the stability of the flow field of the particle sampling system. The tail vacuum air circuit includes: an exhaust pipe 50 and a mechanical pump 49. The exhaust pipe 50 is connected to the gas sampling pipe and is connected to the flue gas analyzer. The gas in the rapid cooling device enters the exhaust pipe 50 through the filter plate 27 and finally enters the atmosphere through the mechanical pump. In order to avoid the problem of oxygen backflow in the exhaust pipe caused by the thermal motion of air molecules, the air flow in the exhaust pipe needs to maintain a suitable flow rate. The suitable flow rate is selected as follows: close the stainless steel valve 7, the first solenoid valve 10, and the ninth solenoid valve 45, open the tenth solenoid valve 48, the eighth solenoid valve 43, the seventh solenoid valve 39, the sixth solenoid valve 37, the fifth solenoid valve 33, and the second solenoid valve 13, adjust the gas flow rate to the same as the sampling state, turn on the oxygen analyzer and stabilize the reading, adjust the fluidization wind speed, so that the oxygen content is lower than 100 ppm, and the gas flow rate of the exhaust pipe can meet the requirements.

[0067] The inert gas flow conditions in the three types of sampling probes are described as follows:

[0068] Sampling probe No. 1: The first inert gas flows from the No. 1 sampling probe thick tube elbow 60, passes through the sampling probe air distribution plate 53, merges with the particles in the No. 1 sampling probe thick tube 55 and enters the particle sampling tube 3. The final flow direction of the first inert gas is the same as the direction of particle movement. The second inert gas flows from the No. 1 sampling probe second inert gas inlet tube 62, passes through the No. 1 sampling probe thin tube elbow 56, the No. 1 sampling probe thin tube 57, and the cone 54, and enters the No. 1 sampling probe particle inlet tube 61. The final flow direction of the second inert gas is opposite to the direction of particle movement.

[0069] Sampling probe No. 2: The first inert gas flows from the first inert gas thick tube elbow 65 of the sampling probe No. 2, passes through the sampling probe air distribution plate 53, merges with the particles in the first inert gas thick tube 63 of the sampling probe No. 2, and then enters the particle sampling tube 3. The final flow direction of the first inert gas is the same as the direction of particle movement; the second inert gas flows from the second inert gas thick tube elbow 69 of the sampling probe No. 2, passes through the sampling probe air distribution plate 53, the second inert gas thick tube 67 of the sampling probe No. 2, and enters the particle inlet tube 68 of the sampling probe No. 2. The final flow direction of the second inert gas is opposite to the direction of particle movement.

[0070] Sampling probe No. 3: The first inert gas and the second inert gas enter through the annular wind chamber 74 and the thin tube 72 of the No. 3 sampling probe respectively. The first inert gas flows from the first inert gas inlet pipe 75 of the No. 3 sampling probe, passes through the annular wind chamber 70 and the sampling probe air distribution plate 53, merges with the particles in the No. 3 sampling probe thick tube 70 and enters the particle sampling tube 3. The final flow direction of the first inert gas is the same as the direction of particle movement. The second inert gas flows from the second inert gas inlet pipe 77 of the No. 3 sampling probe, passes through the thin tube elbow 71 of the No. 3 sampling probe, the thin tube 72 of the No. 3 sampling probe, and the cone 54, and enters the particle inlet pipe 76 of the No. 3 sampling probe. The final flow direction of the second inert gas is opposite to the direction of particle movement.

[0071] The gas flow rate of the first inert gas at the air distribution plate of the sampling probe needs to be greater than 2 m / s, the wind speed of the second inert gas in the No. 2 sampling probe thick tube 64 needs to be maintained at about 0.1 m / s, and the wind speed in the No. 1 sampling probe thin tube 56 and the No. 3 sampling probe thin tube 68 needs to be maintained at about 1 m / s.

[0072] The particle flow in the particle sampling probe is as follows: high-temperature particles enter the particle sampling probe from the particle sampling probe inlet pipe and move upward. After that, the particles first contact with the second inert gas, and the second inert gas moves downward (the second inert gas moves downward, but at a lower speed. The particles have a larger speed in the reaction environment of gas-solid two-phase flow, and they can pass through the second inert gas by relying on the inertia of movement). The particles pass through the second inert gas by relying on the inertia of movement, and then the particles contact with the first inert gas. The movement direction of the first inert gas is the same as that of the particles. Second, the inert gas moves upward at a higher gas speed, carrying the high-temperature particles into the cooling device quickly. The second inert gas achieves basic isolation from the high-temperature reaction atmosphere; the first inert gas dilutes the active gas that may exist near the particles to ensure that the particles quickly enter the rapid cooling device.

[0073] The particle sampling probe and the particle sampling tube 3 can be connected by welding or the like, and the inert gas inlet portion and the inert gas pipeline 44 can also be connected by welding or the like, and the connection needs to ensure the sealing of the connection portion.

[0074] The present invention also provides a method for using the above-mentioned high-temperature gas-solid two-phase flow magnetic particle sampling protection device, and the specific operation process is as follows:

[0075] First pre-experiment: The purpose of this pre-experiment is to find the appropriate fluidization wind speed and the appropriate exhaust pipe diameter: close the stainless steel valve 7, the first solenoid valve 10, and the ninth solenoid valve 45, open the tenth solenoid valve 48, the eighth solenoid valve 43, the seventh solenoid valve 39, the sixth solenoid valve 37, the fifth solenoid valve 33, and the second solenoid valve 13, adjust the gas flow rate to the same as the sampling state, turn on the oxygen analyzer and stabilize the reading, adjust the fluidization wind speed, and make the oxygen content less than 100 ppm. If it is difficult to obtain a suitable flow rate through the above adjustment, it is necessary to change the exhaust pipe diameter and re-adjust the above adjustment.

[0076] Second pre-experiment: In this step, the appropriate gas parameters of the two inert gases at the particle sampling probe are obtained by adjustment. Place the particle sampling probe in the sampling environment, close the second solenoid valve 13, open all other valves, adjust the inert gas flow path, inert gas purge path and mechanical pump to the appropriate state of the first pre-experiment, and turn on the oxygen analyzer at the same time. Continuously adjust the first pressure reducing valve 20, the second pressure reducing valve 25, the third solenoid valve 16, and the fourth solenoid valve 21 so that the reading of the third pressure gauge 14 is 10~50 Pa higher than that of the fourth pressure gauge 15, and the reading of the first pressure gauge 6 is 100~500 Pa higher than that of the second pressure gauge 12. Among them, the third pressure gauge 14 and the fourth pressure gauge 15 may have large fluctuations due to their proximity to the reaction area. At this time, the gas parameters should be adjusted with the highest pressure as the reference point. During the adjustment process, pay attention to the reading of the oxygen analyzer, and the oxygen content must be lower than 1000ppm.

[0077] Precooling of the rapid cooling device: replace the bed materials used in the previous two pre-experiments, set up the particle sampling probe, close the stainless steel valve 7, the second solenoid valve 13, and the first solenoid valve 10, connect the inert gas flow gas path and the inert gas purge gas path, and start the mechanical pump 51. Observe the first thermocouple 28 and the second thermocouple 31, and the precooling is considered to be completed when the temperature is lower than 0°C.

[0078] Sampling starts: First, open the two inert gases at the sampling probe, adjust the gas velocity and pressure to a value higher than the set value, open the stainless steel valve 7 and the first solenoid valve 10, and preheat the oxygen analyzer; then slowly adjust the first and second inert gases to the set parameters, and sampling officially begins. During the sampling process, ensure that the reading of the third pressure gauge 14 is 10~50 Pa higher than that of the fourth pressure gauge 15, and the reading of the first pressure gauge 6 is 100~500 Pa higher than that of the second pressure gauge 12.

[0079] Sampling is finished: when the particle sampling reaches the required mass or the thermocouple temperature is higher than 100 °C, the sampling is finished. When sampling is finished, first close the stainless steel valve 7, the ninth solenoid valve 45 and all related inert gases at the sampling probe, keep the remaining pipelines open until the bed material temperature drops to 0 °C; then close all valves of the sampling device.

[0080] Magnetic particle screening: Take out the bed material mixed with magnetic particles and use a strong magnet or magnetic separator to screen out the magnetic particles.

[0081] Obviously, the described embodiments are only some embodiments of the present invention, but not all. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the protection scope of the present invention.

Claims

1. A sampling protection device for high-temperature gas-solid two-phase flow magnetic particles, characterized in that: It includes a particle sampling device, an oxygen analysis device, a rapid cooling device, and an inert gas distribution device; The particle sampling device is connected to the high-temperature reaction zone, including a particle sampling probe, a particle sampling tube, a heat-insulating protective layer, a stainless steel valve and four pressure gauges; the particle sampling probe is connected to the particle sampling tube, the particle sampling tube includes a curved pipe section and a straight pipe section, the straight pipe section is provided with a stainless steel valve, and the outer layer of the particle sampling tube in the high-temperature environment is provided with a heat-insulating protective layer, including a heat-insulating layer and a steel pipe outside the heat-insulating layer; a first pressure gauge and a second pressure gauge are respectively provided in front of the stainless steel valve and near the rapid cooling device to monitor the flow direction of particles at the rear of the particle sampling tube; the front end of the particle sampling probe A third pressure gauge and a fourth pressure gauge are arranged on the inner side and the outer wall of the heat-insulating protective layer to detect the reliability of the second inert gas isolating the reaction atmosphere; the particle sampling probe is connected to the first inert gas pipeline and the second inert gas pipeline respectively, and the particle sampling probe is located at the front end of the particle sampling tube. The sampled high-temperature particles enter the particle sampling probe and first contact with the second inert gas, and then contact with the first inert gas; the second inert gas realizes the basic isolation of the high-temperature reaction atmosphere, and the first inert gas dilutes the active gas existing near the particles and ensures that the particles quickly enter the rapid cooling device; The oxygen analysis device comprises an oxygen analyzer, a gas sampling tube, a filter screen, a first solenoid valve and a second solenoid valve; the oxygen analyzer is controlled to extract gas from different positions for sampling and analysis by the opening and closing states of the first solenoid valve and the second solenoid valve; the oxygen analyzer uses a trace oxygen analysis device; The rapid cooling device comprises a stainless steel barrel, bed material, an air distribution plate, a first thermocouple, a second thermocouple, a filter plate, and an eighth pressure gauge; the first thermocouple and the second thermocouple are placed on the side of the stainless steel barrel to monitor the temperature of the bottom particles and the upper airflow respectively, and the temperature of the thermocouples during the sampling process should be lower than 100°C to ensure that the ferromagnetic particles sampled in the high temperature environment can be quickly cooled; the stainless steel barrel is built with bed material, and the bed material adopts experimental bed material or quartz sand; the filter plate adopts a combination of a sintered quartz plate and a perforated plate, or a combination of a multi-layer screen and a perforated plate, and the screen should be selected to be above 1000 mesh; the high-temperature particles enter the stainless steel barrel with the first inert gas, and the bed material in the stainless steel barrel is in a fluidized state and has a low temperature. After the high-temperature particles are mixed with the bed material, rapid cooling is achieved due to the high heat exchange coefficient between the particles; The inert gas distribution device is a pressure and flow control device for the entire sampling device, which can be described in five ways: the first way is the first inert gas path, the second way is the second inert gas path, the third way is the inert gas flow path, the fourth way is the inert gas purge path, and the fifth way is the tail vacuum gas path; the first to fourth ways are respectively equipped with a pressure reducing valve, a pressure stabilizing tank, a pressure gauge and a solenoid valve; each pipeline component is connected by an inert gas pipeline, and the inner diameter of the inert gas pipeline is 3 to 20 mm.

2. The sampling protection device for high-temperature gas-solid two-phase flow magnetic particles according to claim 1, characterized in that: The particle sampling probe includes any one of the following structures: The No. 1 sampling probe comprises a No. 1 sampling probe thick tube, the two sides of the No. 1 sampling probe thick tube are respectively connected to the two wing thick tubes, the No. 1 sampling probe thick tube elbows are arranged at the ends of the two wing thick tubes, the sampling probe air distribution plates are arranged in the middle of the two wing thick tubes, the No. 1 sampling probe particle inlet pipe is arranged at the bottom of the thick tube, the No. 1 sampling probe thin tube is arranged in the middle of the thick tube, the No. 1 sampling probe thin tube is the second inert gas inlet pipe, the No. 1 sampling probe thin tube is connected to the center of the thick tube, the No. 1 sampling probe thin tube elbow is arranged inside, the bottom outlet of the thin tube is provided with a cone, the cone is supported by the No. 1 sampling probe cone support rod, and the top of the support rod is connected to the thin tube elbow; the thick tube is connected to the first inert gas pipeline, and the thin tube is connected to the second inert gas pipeline; The No. 2 sampling probe comprises a first inert gas thick tube of the No. 2 sampling probe and a second inert gas thick tube of the No. 2 sampling probe, and the two are butted up and down to form an integral body. The first inert gas thick tube of the No. 2 sampling probe is provided with two wing thick tubes of the first inert gas of the No. 2 sampling probe obliquely downward, and the second inert gas thick tube of the No. 2 sampling probe is provided with two wing thick tubes of the second inert gas of the No. 2 sampling probe obliquely upward. The ends of the two wing thick tubes are respectively provided with thick tube elbows, and the elbow of the first inert gas thick tube is arranged downward, and the elbow of the second inert gas thick tube is arranged upward, and the upper two wing thick tubes are staggered with the lower two wing thick tubes; the sampling probe air distribution plates are respectively provided in the middle of the two wing thick tubes, and the structure of the sampling probe air distribution plates is the same as that of the No. 1 sampling probe; The No. 3 sampling probe includes an annular wind chamber and a No. 3 sampling probe thick tube. The upper part is the No. 3 sampling probe thick tube. The middle of the sampling probe thick tube is provided with a No. 3 sampling probe thin tube, which is the second inert gas inlet pipe. The No. 3 sampling probe thin tube is provided with a No. 3 sampling probe thin tube elbow at the center of the thick tube. A cone is provided at the bottom of the No. 3 sampling probe thin tube. The cone is connected to the thin tube elbow through the No. 3 sampling probe cone support rod. The bottom of the No. 3 sampling probe thick tube is connected to the No. 3 sampling probe particle inlet pipe; the lower part of the No. 3 sampling probe thick tube is connected to the No. 3 sampling probe annular wind chamber through a sideways inclined tube; the connection between the No. 3 sampling probe thick tube and the inclined tube is provided with a sampling probe air distribution plate, which is made of the same material as the No. 1 sampling probe and arranged in a vertical pipeline; the No. 3 sampling probe annular wind chamber is connected to the No. 3 sampling probe first inert gas inlet pipe.

3. The sampling protection device for high-temperature gas-solid two-phase flow magnetic particles according to claim 2, characterized in that: The gas flow rate of the first inert gas at the air distribution plate of the sampling probe must be greater than 2 m / s, the wind speed of the second inert gas in the thick tube of the No. 2 sampling probe is 0.1 ~ 0.2 m / s, and the wind speed in the thin tubes of the No. 1 sampling probe and the No. 3 sampling probe is 0.5 ~ 1.5 m / s.

4. The sampling protection device for high-temperature gas-solid two-phase flow magnetic particles according to claim 1, characterized in that: For places without nitrogen oxides, paramagnetic oxygen analyzers can be used; for places containing nitrogen oxides or where sampling requires extremely low oxygen content, fuel cell analyzers or infrared flue gas analyzers are used.

5. The sampling protection device for high temperature gas-solid two-phase flow magnetic particles according to claim 1, characterized in that: The air distribution plate of the rapid cooling device adopts a small hood air distribution plate or a sintered quartz plate; the stainless steel barrel adopts 3101 stainless steel with a wall thickness of 2~5 mm; the thermocouple adopts a copper-constantan thermocouple with good low-temperature sensitivity.

6. The sampling protection device for high-temperature gas-solid two-phase flow magnetic particles according to claim 1, characterized in that: The volume of the container of the rapid cooling device is determined according to the total mass of the sampled particles. The total volume of the container is three to four times the volume of the initial bed material, and the volume of the initial bed material is more than five times the volume of the sampled particles.

7. The sampling protection device for high temperature gas-solid two-phase flow magnetic particles according to claim 1, characterized in that: The gas in the rapid cooling device enters the exhaust pipe through the filter plate and finally enters the atmosphere through the mechanical pump; the airflow in the exhaust pipe needs to maintain an appropriate flow rate, and the appropriate flow rate is selected by closing the stainless steel valve, the first solenoid valve, and the ninth solenoid valve, and opening the tenth solenoid valve, the eighth solenoid valve, the seventh solenoid valve, the sixth solenoid valve, the fifth solenoid valve, and the second solenoid valve. The gas flow rate is adjusted to the same as the sampling state, the oxygen analyzer is turned on and the reading is stabilized, and the fluidization wind speed is adjusted to make the oxygen content lower than 100 ppm. At this time, the gas flow rate of the exhaust pipe meets the requirement.

8. The sampling protection device for high temperature gas-solid two-phase flow magnetic particles according to claim 1, characterized in that: The inert gas uses an inert gas with a purity of more than 99.99%; the first inert gas is from an inert gas compression tank, through the tenth solenoid valve, the third flow meter, the four-way pipe, the ninth solenoid valve, the three-way pipe, the second pressure reducing valve, the second pressure stabilizing tank, the second flow meter, and the fourth solenoid valve, and finally reaches the first inert gas nozzle; the second inert gas is from an inert gas compression tank, through the tenth solenoid valve, the third flow meter, the four-way pipe, the ninth solenoid valve, the three-way pipe, the first pressure reducing valve, the first pressure stabilizing tank, the first flow meter, and the third solenoid valve, and finally reaches the second inert gas outlet; the inert gas flow gas route is from an inert gas compression tank, through the tenth solenoid valve, the third flow meter, the four-way pipe, the eighth solenoid valve, the fourth pressure reducing valve, the fourth pressure stabilizing tank, the seventh solenoid valve, and finally enters the rapid cooling device after being evenly distributed through the air distribution plate; the inert gas purge gas route is composed of a four-way pipe, a sixth solenoid valve, a third pressure reducing valve, a third pressure stabilizing tank, and a fifth solenoid valve. The fifth solenoid valve is intermittently opened to achieve regular removal of the bed material attached to the filter plate. The fifth solenoid valve is set by the program every 15 s, and the purge time each time is 1 s; the tail vacuum air circuit quickly removes the gas in the rapid cooling device to maintain the stability of the flow field of the particle sampling system. The tail vacuum air circuit includes: an exhaust pipeline and a mechanical pump. The exhaust pipeline is connected to a gas sampling tube by the side and is connected to the flue gas analyzer.

9. A method for using the high-temperature gas-solid two-phase flow magnetic particle sampling protection device according to any one of claims 1 to 8, characterized in that The operation process is as follows: The first preliminary experiment: The purpose is to find the appropriate fluidizing wind speed and the appropriate exhaust pipe diameter: close the stainless steel valve, the first solenoid valve, and the ninth solenoid valve, open the tenth solenoid valve, the eighth solenoid valve, the seventh solenoid valve, the sixth solenoid valve, the fifth solenoid valve, and the second solenoid valve, adjust the gas flow rate to the same as the sampling state, turn on the oxygen analyzer and stabilize the reading, adjust the fluidizing wind speed to make the oxygen content lower than 100 ppm; if it is difficult to obtain a suitable flow rate through the above adjustments, it is necessary to replace the exhaust pipe diameter and re-adjust the above adjustments; Second pre-experiment: Get the appropriate gas parameters of the two inert gases at the particle sampling probe by adjustment: Place the particle sampling probe in the sampling environment, close the second solenoid valve, open all other valves, adjust the inert gas flow path, inert gas purge path and mechanical pump to the appropriate state of the first pre-experiment, and turn on the oxygen analyzer at the same time; continuously adjust the first pressure reducing valve, the second pressure reducing valve, the third solenoid valve and the fourth solenoid valve, so that the reading of the third pressure gauge is 10~50Pa higher than that of the fourth pressure gauge, and the reading of the first pressure gauge is 100~500Pa higher than that of the second pressure gauge; the third and fourth pressure gauges have large fluctuations because they are close to the reaction area, so the gas parameters should be adjusted with the highest pressure as the reference point; during the adjustment process, pay attention to the reading of the oxygen analyzer, and the oxygen content should be lower than 1000 ppm; Precooling of the rapid cooling device: replace the bed materials used in the previous two pre-experiments, set up the particle sampling probe, close the stainless steel valve, the second solenoid valve, and the first solenoid valve, connect the inert gas flow gas path and the inert gas purge gas path, and start the mechanical pump; observe the first thermocouple and the second thermocouple, and determine that the precooling is over when the temperature is lower than 0°C; Sampling starts: First, open the two inert gases at the sampling probe, adjust the gas velocity and pressure to be higher than the set value, open the stainless steel valve and the first solenoid valve, and preheat the oxygen analyzer; then slowly adjust the first and second inert gases to the set parameters, and sampling officially begins; during the sampling process, ensure that the reading of the third pressure gauge is 10~50 Pa higher than that of the fourth pressure gauge, and the reading of the first pressure gauge is 100~500 Pa higher than that of the second pressure gauge; Sampling is finished: when the particle sampling reaches the required mass or the thermocouple temperature is higher than 100 ℃, the sampling is finished; at the end of sampling, first close the stainless steel valve, the ninth solenoid valve and all related inert gases at the sampling probe, and keep the remaining pipelines open until the bed material temperature drops to 0 ℃; then close all valves of the sampling device; Magnetic particle screening: Take out the bed material mixed with magnetic particles and use a strong magnet or magnetic separator to screen out the magnetic particles.

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