Detection device for phenolic resin material element analysis

Abstract

The invention discloses a detection device for phenolic resin material elemental analysis, and belongs to the field of phenolic resin detection equipment, the detection device comprises a cracking furnace, one side of the cracking furnace is communicated with a gas carrying tank through a pipeline; the other end of the cracking furnace is communicated with an oxygen analysis catalytic reaction assembly, and one end of the oxygen analysis catalytic reaction assembly is communicated with a TCD detector; the oxygen analysis catalytic reaction assembly comprises a working barrel, and one side of the working barrel is connected with a main air inlet pipe in a penetrating mode. According to the application, the oxygen analysis catalytic reaction assembly is arranged and has two conditions of standard oxygen mode analysis and sulfur-resistant mode analysis, and corresponding modes can be switched according to the sulfur-containing condition of the phenolic resin pyrolysis gas to be analyzed; further, the problems that the conversion rate attenuation of CO to CO2 in an oxygen mode is greater than 50% and the oxygen content deviation is relatively large due to the fact that a platinum catalyst is irreversibly poisoned by sulfide (SO2) when sulfur-containing phenolic resin is detected through single standard oxygen mode analysis are solved.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of phenolic resin detection equipment, more particularly, to a detection device for elemental analysis of phenolic resin material. BACKGROUND

[0002] For elemental analysis of phenolic resin material, the commonly used detection device is mainly selected according to the type of element to be analyzed, the precision requirement, the sample form, and whether the sample needs to be destroyed, etc. For the scene that needs to comprehensively analyze the major elements, CHNS / O elemental analysis method (EA) is the preferred means.

[0003] CHNS / O elemental analysis method (EA) is the most commonly used and standard method for determining the content of carbon (C), hydrogen (H), nitrogen (N), sulfur (S) and oxygen (O) in organic materials. Its principle is that the sample is pyrolyzed and cracked in an inert gas (helium) at high temperature, the oxygen-containing products (mainly CO) produced are carried by the carrier gas through the carbon catalyst, and are converted into CO2, and then the TCD detection is performed for elemental analysis.

[0004] The traditional CHNS / O elemental analysis method has two technical defects when detecting the oxygen content of sulfur-containing phenolic resin (such as flame-retardant type, rubber modified type): 1. Sulfur poisoning effect: sulfide (SO2) irreversibly poisons the platinum catalyst, resulting in a decay of more than 50% in the conversion rate of CO to CO2 in the oxygen mode, resulting in a large deviation in oxygen content; 2. High maintenance cost: the catalyst needs to be replaced every 20 sulfur-containing samples. Therefore, the existing CHNS / O elemental analysis method (EA) has limitations in elemental analysis and detection of sulfur-containing phenolic resin under the oxygen mode, resulting in high cost and large deviation in detection results, which needs to be further improved. SUMMARY

[0005] In view of the problems in the prior art, the purpose of the present application is to provide a detection device for elemental analysis of phenolic resin material.

[0006] To solve the above problems, the present application adopts the following technical solution.

[0007] A detection device for elemental analysis of phenolic resin material, comprising a cracking furnace, one side of the cracking furnace being connected to a carrier gas tank through a pipeline; the other end of the cracking furnace being connected to an oxygen analysis catalytic reaction assembly, one end of the oxygen analysis catalytic reaction assembly being connected to a TCD detector. The oxygen analysis catalytic reaction component includes a working cylinder, one side of which is penetrated by a main air inlet pipe, on which a sulfur pre-detection sensor is provided and one end of which is connected to a cracking furnace; the other side of the working cylinder is penetrated by a main air outlet pipe, one end of which is connected to a TCD detector; the main air inlet pipe and the main air outlet pipe extend to one end inside the working cylinder and are both fixedly connected to a switching connection component; and the main air inlet pipe and the main air outlet pipe are both movably connected to a rotating base through the switching connection component, one end of the rotating base is fixedly connected to a stepping motor, and the stepping motor is fixedly connected to one side of the working cylinder; an oxygen mode catalytic component and an anti-sulfur catalytic component are symmetrically arranged inside the rotating base, and the oxygen analysis catalytic reaction component also includes a processing unit.

[0008] Furthermore, the switching connection assembly includes a rotating ring body respectively fixed to the lower ends of the main air inlet pipe and the main air outlet pipe, a connecting channel is provided at the middle position of the upper end of the rotating ring body and is connected to the main air inlet pipe and the main air outlet pipe respectively through the connecting channel; graphite sealing rings are provided on both sides of the rotating ring body, and limiting ring grooves are provided on the outer circular surface of the rotating base at positions corresponding to the rotating ring body, and the rotating ring body is rotatably sleeved in the limiting ring groove.

[0009] Furthermore, the oxygen mode catalytic assembly includes a cavity A opened on one side of the rotating base, and two second channels are symmetrically opened on both sides of the rotating base. The outlet positions of the two second channels extend to the limiting ring groove and are located in the same plane as the positions of the two connecting channels in the vertical direction; carbon nanotubes are provided inside the cavity A, sintered metal filters are fixedly connected on both sides of the carbon nanotubes, and the interior of the carbon nanotubes is filled with platinum catalyst particles.

[0010] Furthermore, the sulfur-resistant catalytic assembly includes a cavity B opened on the other side of the rotating base, and the cavity B is symmetrically arranged with respect to the cavity A; two first channels are symmetrically opened on both sides of the cavity B inside the rotating base, and the outlet positions of the two first channels extend to the limiting ring groove, and are located in the same plane as the positions of the two connecting channels in the vertical direction; two supporting skeletons are fixedly connected inside the cavity B, and a CeZr solid solution composite layer and a ZSM-5 molecular sieve composite membrane are provided between the two supporting skeletons, and the CeZr solid solution composite layer and the ZSM-5 molecular sieve composite membrane are in close contact.

[0011] Furthermore, the oxygen analysis catalytic reaction component also includes a regeneration component; the regeneration component includes: a hydrogen-helium mixture tank, which is connected to the main air inlet pipe through a pipeline; it also includes a heating plate and a temperature sensor arranged on the inner wall of the working cylinder, and a thermal mass flow meter is also provided on the main air inlet pipe. The main air outlet pipe is connected to a regeneration gas outlet, and an electrochemical H2S sensor is provided on the regeneration gas outlet; the main air outlet pipe and the regeneration gas outlet are both provided with solenoid valves.

[0012] Further, the processing unit is used for collecting monitoring signals of the sulfur pre-detection sensor in real time to judge the sulfur concentration in the cracking gas and select a working mode; regeneration judgment is made according to the working mode and regeneration execution logic is established; data of the thermal mass flow meter and the sulfur pre-detection sensor are received in real time and a mathematical model is established to calculate the regeneration time; electrochemical H2S sensor data are received in real time to establish regeneration termination judgment logic and control the regeneration termination.

[0013] Further, the monitoring signals of the sulfur pre-detection sensor are collected in real time to judge the sulfur concentration in the cracking gas and select a working mode, which includes two kinds, one is a standard oxygen mode and the other is a sulfur-resistant mode. Standard oxygen mode: when the sulfur pre-detection sensor reading is <10 ppm: the oxygen mode catalytic assembly is cut into the main gas path by the rotating base; Standard oxygen mode: when the sulfur pre-detection sensor reading is ≥10 ppm: the sulfur-resistant catalytic assembly is cut into the main gas path by the rotating base rotating 180°.

[0014] Further, regeneration judgment is made according to the working mode and regeneration execution logic is established, including: After the sulfur concentration in the cracking gas is judged according to the monitoring signals of the sulfur pre-detection sensor and the working mode is selected, the regeneration judgment is determined, if the sulfur-resistant catalytic assembly is used in this analysis, the regeneration needs to be marked, if the sulfur-resistant catalytic assembly is not used, the marking is not needed; regeneration execution logic is established based on the marking result.

[0015] Further, data of the thermal mass flow meter and the sulfur pre-detection sensor are received in real time and a mathematical model is established to calculate the regeneration time, including: The regeneration temperature is limited to 400℃, the hydrogen-helium mixed gas tank is regenerated with 5% H2 / He mixed gas; under this condition, the data of the thermal mass flow meter and the sulfur pre-detection sensor are received in real time and a mathematical model is established to calculate the total sulfur adsorbed by the catalyst before regeneration, and the target regeneration time is calculated according to the total sulfur adsorbed by the catalyst before regeneration.

[0016] Further, electrochemical H2S sensor data are received in real time to establish regeneration termination judgment logic and control the regeneration termination, including: The electrochemical H2S sensor data are received in real time, combined with the target regeneration time, if the actual regeneration time is greater than or equal to the target regeneration time, or the H2S concentration monitored by the electrochemical H2S sensor is ≤2 ppm for 30 seconds, the regeneration termination is controlled, and the regeneration process is completed.

[0017] Compared with the prior art, the present application has the following advantages: (1) The present application sets up an oxygen analysis catalytic reaction component, which has two modes of analysis: standard oxygen mode analysis and anti-sulfur mode analysis. The corresponding mode can be switched according to the sulfur content of the phenolic resin cracking gas to be analyzed, thereby avoiding the problem that the sulfide (SO2) present in the single standard oxygen mode analysis when detecting sulfur-containing phenolic resin irreversibly poisons the platinum catalyst, resulting in a CO→CO2 conversion rate attenuation of more than 50% in the oxygen mode and a large deviation in oxygen content.

[0018] (2) The present application sets a regeneration component. After the anti-sulfur catalytic component is used, the anti-sulfur catalytic component can be reduced in situ in real time through the regeneration component, thereby ensuring the use of the anti-sulfur catalytic component. Compared with the existing technology, the maintenance cost is lower, and there is no need to frequently replace the catalyst, which saves costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic diagram of the overall process structure of the present invention; Figure 2 This is a schematic diagram of the overall structure of the oxygen analysis catalytic reaction assembly of the present invention; Figure 3 For the present invention Figure 2 Schematic diagram of the mid-section structure; Figure 4 For the present invention Figure 2 Schematic diagram of the structure after removing the rotating base and its internal components; Figure 5 This is a schematic structural diagram of the rotating base and its internal components of the present invention.

[0020] Description of the numbers in the figure: 1. Working cylinder; 2. Main air inlet pipe; 3. Thermal mass flowmeter; 4. Sulfur pre-detection sensor; 5. Main air outlet pipe; 6. Stepper motor; 7. Switching connection assembly; 71. Rotating ring; 72. Graphite sealing ring; 73. Connecting channel; 74. Limiting ring groove; 8. Sulfur-resistant catalytic component; 81. First channel; 82. Cavity B; 83. CeZr solid solution composite layer; 84. ZSM-5 molecular sieve composite membrane; 85. Support skeleton; 9. Oxygen mode catalytic component; 91. Cavity A; 92. Second channel; 93. Carbon nanotubes; 94. Sintered metal filter; 10. Rotating base; 11. Regeneration gas outlet; 12. Electrochemical H2S sensor; 13. Solenoid valve; 14. Heating plate; 15. Temperature sensor. DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention; it is obvious that the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0022] See also Figures 1 to 5 , a detection device for elemental analysis of phenolic resin materials, comprising a cracking furnace, one side of which is connected to a carrier gas tank through a pipeline; The other end of the cracking furnace is connected to an oxygen analysis catalytic reaction component, and one end of the oxygen analysis catalytic reaction component is connected to a TCD detector; The oxygen analysis catalytic reaction component includes a working cylinder 1, one side of the working cylinder 1 is penetrated by a main air inlet pipe 2, the main air inlet pipe 2 is provided with a sulfur pre-detection sensor 4 and one end is connected to the cracking furnace; the other side of the working cylinder 1 is penetrated by a main air outlet pipe 5, one end of the main air outlet pipe 5 is connected to a TCD detector; the main air inlet pipe 2 and the main air outlet pipe 5 extend to one end of the interior of the working cylinder 1 and are both fixedly connected to a switching connection component 7; and the main air inlet pipe 2 and the main air outlet pipe 5 are both movably connected to a rotating base 10 through the switching connection component 7, one end of the rotating base 10 is fixedly connected to a stepping motor 6, and the stepping motor 6 is fixedly connected to one side of the working cylinder 1; an oxygen mode catalytic component 9 and an anti-sulfur catalytic component 8 are symmetrically provided inside the rotating base 10, and the oxygen analysis catalytic reaction component also includes a processing unit.

[0023] like Figure 3 and Figure 4 As shown, the switching connection assembly 7 includes a rotating ring body 71 respectively fixed to the lower ends of the main air inlet pipe 2 and the main air outlet pipe 5, and a connecting channel 73 is provided at the middle position of the upper end of the rotating ring body 71 and is connected to the main air inlet pipe 2 and the main air outlet pipe 5 respectively through the connecting channel 73; graphite sealing rings 72 are provided on both sides of the rotating ring body 71, and limiting ring grooves 74 are provided on the outer surface of the rotating base 10 at positions corresponding to the rotating ring body 71, and the rotating ring body 71 is rotatably sleeved in the limiting ring groove 74.

[0024] like Figure 5 As shown, the oxygen mode catalytic component 9 includes a cavity A91 opened on one side of the rotating base 10, and two second channels 92 are symmetrically opened on both sides of the cavity A91 inside the rotating base 10, and the outlet positions of the two second channels 92 extend to the limiting ring groove 74, and are located in the same plane as the positions of the two connecting channels 73 in the vertical direction; carbon nanotubes 93 are provided inside the cavity A91, and sintered metal filter meshes 94 are fixedly connected on both sides of the carbon nanotubes 93, and the interior of the carbon nanotubes 93 is filled with platinum catalyst particles.

[0025] like Figure 5 As shown, the anti-sulfur catalytic component 8 includes a cavity B82 opened on the other side of the rotating base 10, and the cavity B82 is symmetrically arranged with respect to the cavity A91; two first channels 81 are symmetrically opened on both sides of the cavity B82 inside the rotating base 10, and the outlet positions of the two first channels 81 extend to the limiting ring groove 74, and are located in the same plane as the positions of the two connecting channels 73 in the vertical direction; two supporting skeletons 85 are fixedly connected inside the cavity B82, and a CeZr solid solution composite layer 83 and a ZSM-5 molecular sieve composite membrane 84 are provided between the two supporting skeletons 85, and the CeZr solid solution composite layer 83 and the ZSM-5 molecular sieve composite membrane 84 are in close contact.

[0026] When performing elemental analysis, the phenolic resin material to be analyzed is first placed in a cracking furnace for cracking. At the same time, a carrier gas is introduced into the cracking furnace from a carrier gas tank. The carrier gas is usually an inert gas, such as nitrogen. After the carrier gas is introduced, the mixed gas of the cracking gas and the carrier gas passes through the main air inlet pipe 2. At this time, the sulfur concentration in the mixed gas of the cracking gas and the carrier gas is detected by the sulfur pre-detection sensor 4; If the reading of the sulfur pre-detection sensor 4 is less than 10ppm: the rotating base 10 cuts the oxygen mode catalytic component 9 into the main gas path (standard oxygen mode); in the standard oxygen mode, no switching is required (the initial state oxygen mode catalytic component 9 is set to be connected to the main gas path). At this time, the mixed gas enters the oxygen mode catalytic component 9 through the main intake pipe 2 through the connecting channel 73 in the switching connection component 7, specifically first enters the second channel 92, and then enters the cavity A91, passes through the sintered metal filter 94 and enters the platinum catalyst particles in the carbon nanotubes 93. The platinum catalyst particles cooperate with the carbon nanotubes 93 to efficiently catalyze the CO in the mixed gas into CO2. After catalysis, the mixed gas flows into the TCD detector through the main outlet pipe 5 for oxygen element analysis.

[0027] If the reading of the sulfur pre-detection sensor 4 is ≥10ppm: at this time, it is necessary to control the output shaft of the stepper motor 6 to rotate, and drive the rotating base 10 to rotate 180° to cut the anti-sulfur catalytic component 8 into the main gas path (anti-sulfur mode), and switch the connecting component 7 to work. Specifically, first control the output shaft of the stepper motor 6 to rotate, and drive the rotating base 10 to rotate 180°. At this time, due to the existence of the rotating ring body 71 and the graphite sealing ring 72, the gas inside the main intake pipe 2 can be sealed to prevent gas leakage, until the first channel 81 is connected to the main gas path, and the mixed gas enters the first channel 81 through the connecting channel 73; The two first channels 81 are connected to the main gas path and are respectively connected to the main air inlet pipe 2 and the main air outlet pipe 5. At this time, the mixed gas first enters the first channel 81 and enters the cavity B82 from the first channel 81. Then the mixed gas passes through the CeZr solid solution composite layer 83 and the ZSM-5 molecular sieve composite membrane 84 for catalytic oxidation. At this time, SO2 is first captured by the oxygen vacancies on the surface of the CeZr solid solution composite layer 83 to form stable cerium sulfate. Then the remaining mixed gas passes through the ZSM-5 molecular sieve composite membrane 84, and the acidic sites in the pores of the ZSM-5 molecular sieve composite membrane 84 catalyze the oxidation of CO into CO2. After catalysis, the mixed gas flows into the TCD detector through the main air outlet pipe 5 for oxygen element analysis.

[0028] It should be noted that when performing oxidation catalysis, the oxygen analysis catalytic reaction component should be kept in a heated state of 180°C.

[0029] like Figure 1 、 Figure 2 and Figure 4 As shown, the oxygen analysis catalytic reaction component also includes a regeneration component; the regeneration component includes: a hydrogen-helium mixed gas tank, which is connected to the main air inlet pipe 2 through a pipeline; it also includes a heating plate 14 and a temperature sensor 15 arranged on the inner wall of the working cylinder 1, and the main air inlet pipe 2 is also provided with a thermal mass flowmeter 3, the main air outlet pipe 5 is connected to a regeneration gas outlet 11, and the regeneration gas outlet 11 is provided with an electrochemical H2S sensor 12; the main air outlet pipe 5 and the regeneration gas outlet 11 are both provided with a solenoid valve 13.

[0030] After the anti-sulfur catalytic component 8 has been used, it is necessary to regenerate the anti-sulfur catalytic component 8 to ensure its anti-sulfur capability. The regeneration process is as follows: First, the regeneration premise is that the elemental analysis work is stopped and the cracking furnace is no longer working. At the same time, the regeneration condition is 400℃, and the heating is performed by the heating plate 14. The temperature sensor 15 detects the temperature data. The hydrogen-helium mixed gas tank introduces regeneration gas into the main intake pipe 2. The regeneration gas is a 5% H2 / He mixed gas. The gas enters the cavity B82 through the main intake pipe 2. The hydrogen in the regeneration gas reduces cerium sulfate. The specific reaction is as follows: The released H2S and other gases enter the regeneration gas outlet 11 through the main outlet pipe 5 and are captured by the downstream alkaline adsorbent. It should be noted that during regeneration, the solenoid valve 13 on the main outlet pipe 5 is closed, while the solenoid valve 13 on the regeneration gas outlet 11 is open. The reverse operation is performed during oxidation analysis.

[0031] The processing unit is used to collect the monitoring signal of the sulfur pre-detection sensor 4 in real time to judge the sulfur concentration in the cracking gas and select the working mode; make regeneration judgment based on the working mode and establish regeneration execution logic; receive data from the thermal mass flow meter 3 and the sulfur pre-detection sensor 4 in real time and establish a mathematical model to calculate the regeneration time; receive data from the electrochemical H2S sensor 12 in real time, establish regeneration termination judgment logic, and control regeneration termination.

[0032] In some implementations, the monitoring signal of the sulfur pre-detection sensor 4 is collected in real time to determine the sulfur concentration in the cracked gas and select an operating mode, which includes two operating modes: a standard oxygen mode and an anti-sulfur mode; Standard oxygen mode: When the sulfur pre-detection sensor 4 reading is less than 10 ppm: the base 10 is rotated to cut the oxygen mode catalytic component 9 into the main gas path; Anti-sulfur mode: when the sulfur pre-detection sensor 4 reads ≥10 ppm: the rotary base 10 rotates 180° to cut the anti-sulfur catalytic component 8 into the main gas path.

[0033] In some implementations, regeneration determination is performed based on the working mode and regeneration execution logic is established, including: The sulfur concentration in the cracking gas is judged based on the monitoring signal of the sulfur pre-detection sensor 4, and after selecting the working mode, the regeneration judgment is determined. If the anti-sulfur catalyst component 8 is used in this analysis, regeneration needs to be marked. If the anti-sulfur catalyst component 8 is not used, no marking is required; the regeneration execution logic is established based on the marking result.

[0034] By adopting the above technical solution, if the anti-sulfur catalyst assembly 8 is used in this analysis, regeneration is required. The regeneration mark is set to R, 0 means no regeneration is required, and 1 means regeneration is required. The regeneration execution logic is as follows: Among them, A represents the use of the oxygen mode catalytic component 9, B represents the use of the sulfur-resistant catalytic component 8, and M represents the working mode.

[0035] In some implementations, the data from the thermal mass flow meter 3 and the sulfur pre-detection sensor 4 are received in real time and a mathematical model is established to calculate the regeneration time, including: The regeneration temperature is limited to 400°C, and the regeneration gas in the hydrogen-helium mixture tank is a 5% H2 / He mixture. Under this condition, data from the thermal mass flowmeter 3 and the sulfur pre-detection sensor 4 are received in real time and a mathematical model is established to calculate the total amount of sulfur adsorbed on the catalyst before regeneration. A model is also established based on the total amount of sulfur adsorbed on the catalyst before regeneration to calculate the target regeneration time.

[0036] By adopting the above technical solution, under limited conditions, based on the data of the thermal mass flow meter 3 and the sulfur pre-detection sensor 4, a mathematical model is established to calculate the total sulfur adsorbed on the catalyst before regeneration: Wherein, Q0 represents the total amount of sulfur adsorbed by the catalyst before regeneration (unit: mmol); Cso2 represents the SO2 concentration (ppm), which is output in real time by the sulfur pre-detection sensor 4; t1 represents the end time of catalysis, t represents the start time of catalysis; F g represents the carrier gas flow rate (mL / min), which is monitored in real time by the thermal mass flow meter 3; represents the integral over time t.

[0037] After calculating the total amount of sulfur adsorbed on the catalyst before regeneration, calculate the target regeneration time: Among them, t M represents the target regeneration time, K is the basic time for system preheating and gas replacement, which is taken as 3.0 min, and W is the time consumed for removing each millimole of sulfur, which is taken as 12.0 min / mmol.

[0038] In some implementations, real-time data from the electrochemical H2S sensor 12 is received, regeneration termination determination logic is established, and regeneration termination is controlled, including: The data of the electrochemical H2S sensor 12 is received in real time, and combined with the target regeneration time, if the actual regeneration time is greater than or equal to the target regeneration time, or the H2S concentration monitored by the electrochemical H2S sensor 12 is ≤ 2ppm for 30 seconds, the regeneration is controlled to be terminated and the regeneration process is completed.

[0039] The above description is merely a preferred embodiment of the present invention; however, the scope of protection of the present invention is not limited thereto. Any person skilled in the art who, within the technical scope disclosed by the present invention, makes equivalent substitutions or modifications based on the technical solutions and improved concepts of the present invention shall be covered by the scope of protection of the present invention.

Claims

1. A detection device for elemental analysis of phenolic resin materials, comprising a cracking furnace, one side of which is connected to a carrier gas tank via a pipeline; characterized in that: The other end of the cracking furnace is connected to an oxygen analysis catalytic reaction component, and one end of the oxygen analysis catalytic reaction component is connected to a TCD detector; The oxygen analysis catalytic reaction component comprises a working cylinder (1), one side of the working cylinder (1) is connected to the main air inlet pipe (2), the main air inlet pipe (2) is provided with a sulfur pre-detection sensor (4) and one end of the main air inlet pipe (5) is connected to the cracking furnace; the other side of the working cylinder (1) is connected to the main air outlet pipe (5), one end of the main air outlet pipe (5) is connected to the TCD detector; the main air inlet pipe (2) and the main air outlet pipe (5) are both fixedly connected to the switching connection component (7) at one end extending to the inside of the working cylinder (1); and the main air inlet pipe (2) and the main air outlet pipe (5) are both movably connected to the rotating base (10) through the switching connection component (7), one end of the rotating base (10) is fixedly connected to a stepping motor (6), and the stepping motor (6) is fixedly connected to one side of the working cylinder (1); the rotating base (10) is symmetrically provided with an oxygen mode catalytic component (9) and an anti-sulfur catalytic component (8), and the oxygen analysis catalytic reaction component further comprises a processing unit.

2. The detection device for elemental analysis of phenolic resin materials according to claim 1, characterized in that: The switching connection assembly (7) includes a rotating ring body (71) fixedly connected to the lower ends of the main air inlet pipe (2) and the main air outlet pipe (5), respectively. A connecting channel (73) is provided at the middle position of the upper end of the rotating ring body (71) and is connected to the main air inlet pipe (2) and the main air outlet pipe (5) respectively through the connecting channel (73); graphite sealing rings (72) are provided on both sides of the rotating ring body (71), and a limiting ring groove (74) is provided on the outer circumferential surface of the rotating base (10) at a position corresponding to the rotating ring body (71), and the rotating ring body (71) is rotatably sleeved in the limiting ring groove (74).

3. The detection device for elemental analysis of phenolic resin materials according to claim 2, characterized in that: The oxygen mode catalytic component (9) includes a cavity A (91) opened on one side of the interior of a rotating base (10), and two second channels (92) are symmetrically opened on both sides of the interior of the rotating base (10) about the cavity A (91), and the outlet positions of the two second channels (92) extend to the limiting ring groove (74), and are located in the same plane as the positions of the two connecting channels (73) in the vertical direction; a carbon nanotube (93) is provided inside the cavity A (91), and a sintered metal filter (94) is fixedly connected to both sides of the carbon nanotube (93), and the interior of the carbon nanotube (93) is filled with platinum catalyst particles.

4. The detection device for elemental analysis of phenolic resin materials according to claim 3, characterized in that: The anti-sulfur catalytic component (8) includes a cavity B (82) opened on the other side of the rotating base (10), and the cavity B (82) is symmetrically arranged with respect to the cavity A (91); two first channels (81) are symmetrically opened on both sides of the rotating base (10), and the outlet positions of the two first channels (81) extend to the limiting ring groove (74), and are located in the same plane as the positions of the two connecting channels (73) in the vertical direction; two supporting skeletons (85) are fixedly connected inside the cavity B (82), and a CeZr solid solution composite layer (83) and a ZSM-5 molecular sieve composite membrane (84) are provided between the two supporting skeletons (85), and the CeZr solid solution composite layer (83) and the ZSM-5 molecular sieve composite membrane (84) are in close contact.

5. The detection device for elemental analysis of phenolic resin materials according to claim 1, characterized in that: The oxygen analysis catalytic reaction component also includes a regeneration component; the regeneration component includes: a hydrogen-helium mixed gas tank, which is connected to the main air inlet pipe (2) through a pipeline; a heating plate (14) and a temperature sensor (15) arranged on the inner wall of the working cylinder (1); a thermal mass flowmeter (3) is also provided on the main air inlet pipe (2); the main air outlet pipe (5) is connected to a regeneration gas outlet (11), and an electrochemical H2S sensor (12) is provided on the regeneration gas outlet (11); and a solenoid valve (13) is provided on both the main air outlet pipe (5) and the regeneration gas outlet (11).

6. The detection device for elemental analysis of phenolic resin materials according to claim 1, characterized in that: The processing unit is used to collect the monitoring signal of the sulfur pre-detection sensor (4) in real time to judge the sulfur concentration in the cracking gas and select the working mode; make a regeneration judgment according to the working mode and establish a regeneration execution logic; receive the data of the thermal mass flow meter (3) and the sulfur pre-detection sensor (4) in real time and establish a mathematical model to calculate the regeneration time; receive the data of the electrochemical H2S sensor (12) in real time, establish a regeneration termination judgment logic, and control the regeneration termination.

7. The detection device for elemental analysis of phenolic resin materials according to claim 6, characterized in that: It is used to collect the monitoring signal of the sulfur pre-detection sensor (4) in real time to judge the sulfur concentration in the cracking gas and select the working mode, which includes two working modes: one is the standard oxygen mode and the other is the anti-sulfur mode; Standard oxygen mode: When the sulfur pre-detection sensor (4) reading is less than 10 ppm: rotate the base (10) to cut the oxygen mode catalytic component (9) into the main gas path; Anti-sulfur mode: When the sulfur pre-detection sensor (4) reads ≥ 10 ppm: the rotary base (10) rotates 180° to cut the anti-sulfur catalytic component (8) into the main gas path.

8. The detection device for elemental analysis of phenolic resin materials according to claim 7, characterized in that: Make regeneration judgments based on the working mode and establish regeneration execution logic, including: The sulfur concentration in the cracking gas is judged based on the monitoring signal of the sulfur pre-detection sensor (4), and after selecting the working mode, the regeneration judgment is determined. If the anti-sulfur catalytic component (8) is used in this analysis, regeneration needs to be marked. If the anti-sulfur catalytic component (8) is not used, no marking is required; and regeneration execution logic is established based on the marking result.

9. The detection device for elemental analysis of phenolic resin materials according to claim 8, characterized in that: The data from the thermal mass flow meter (3) and the sulfur pre-detection sensor (4) are received in real time and a mathematical model is established to calculate the regeneration time, including: The regeneration temperature is limited to 400°C, and the regeneration gas in the hydrogen-helium mixture tank is a 5% H2 / He mixture. Under this condition, the data from the thermal mass flow meter (3) and the sulfur pre-detection sensor (4) are received in real time and a mathematical model is established to calculate the total amount of sulfur adsorbed on the catalyst before regeneration. The target regeneration time is calculated based on the total amount of sulfur adsorbed on the catalyst before regeneration.

10. The detection device for elemental analysis of phenolic resin materials according to claim 9, characterized in that: Receive data from the electrochemical H2S sensor (12) in real time, establish regeneration termination judgment logic, and control regeneration termination, including: The data of the electrochemical H2S sensor (12) is received in real time, and combined with the target regeneration time, if the actual regeneration time is greater than or equal to the target regeneration time, or the H2S concentration monitored by the electrochemical H2S sensor (12) is continuously ≤2ppm for 30 seconds, the regeneration is controlled to be terminated and the regeneration process is completed.

Images