Integrated process and device for adsorption and regeneration of tail gas in production of silicone oil silicone resin

Abstract

The application discloses a kind of integrated process and device for adsorbing and regenerating tail gas in silicone oil silicone resin production.The process is sequentially through tail gas pretreatment, electric field pre-polarization, magnetic stable fluidized bed adsorption, pulse heat regeneration, desorption recovery, reset after regeneration, and deep treatment is carried out as needed by membrane separation, and the whole process is realized by process synergistic control adaptive optimization.The supporting device is composed of pretreatment, electric field pre-polarization, magnetic stable fluidized bed adsorption, pulse heat regeneration, condensation recovery, membrane separation concentration and control and switching system, and each unit is cooperatively linked.The process can efficiently remove siloxane, dust and other impurities in tail gas, realize the recycling and regeneration of adsorbent and the recovery of siloxane resources, and the concentration of siloxane after conventional adsorption is ≤50mg / m³, and ≤10mg / m³ after deep treatment, which meets the ultra-low emission requirements, realizes the double goals of environmental protection and resource recycling, adapts to large-scale organic silicon production, has the advantages of high efficiency, energy saving and continuous operation, and is easy to industrialize.

Description

Technical Field

[0001] This invention relates to the field of exhaust gas treatment technology, and more specifically, to an integrated process and apparatus for exhaust gas adsorption and regeneration in the production of silicone oil and organosilicon resin. Background Technology

[0002] The production process of silicone oil and organosilicon resin will generate exhaust gas containing siloxanes, dust, soluble impurities and entrained droplets. Among them, siloxanes are highly stable and difficult to degrade. Direct emission will cause air pollution and harm the ecological environment. At the same time, as a raw material for production, direct emission of siloxanes will lead to resource waste.

[0003] Current exhaust gas treatment technologies mostly employ single adsorption or incineration methods, which have numerous drawbacks: In single adsorption processes, the adsorbent is easily saturated, regeneration is difficult, frequent adsorbent replacement is required, treatment costs are high, and secondary pollution is easily generated; incineration processes are energy-intensive, cannot recover siloxane resources, and may produce harmful byproducts. Furthermore, existing adsorption technologies mostly use fixed-bed adsorption, resulting in low mass transfer efficiency between exhaust gas and adsorbent, poor adsorption performance, and difficulty in reducing the concentration of siloxanes in the exhaust gas to ultra-low emission standards; simultaneously, the switching between adsorption and regeneration processes is cumbersome, making continuous operation impossible, and exhibiting poor adaptability, making it difficult to meet the exhaust gas treatment needs of large-scale organosilicon production.

[0004] Current technologies lack a process that integrates exhaust gas pretreatment, efficient adsorption, adsorbent regeneration, useful component recovery, and deep purification. Furthermore, they cannot achieve dynamic optimization of parameters at each stage through coordinated control, resulting in low exhaust gas treatment efficiency, high energy consumption, and low resource utilization, making it difficult to balance environmental compliance with economic benefits. Therefore, developing a highly efficient, energy-saving, continuously operating, and resource-recoverable integrated exhaust gas adsorption and regeneration process has become an urgent need in the field of organosilicon production exhaust gas treatment. Summary of the Invention

[0005] In order to overcome the problems of low efficiency in treating tail gas from organosilicon production, poor regeneration effect of adsorbent, waste of resources, and difficulty in achieving continuous ultra-low emissions in existing technologies, this invention discloses a correlation analysis method for residual alkali and moisture in cathode materials, which can effectively solve the above-mentioned technical problems.

[0006] To solve the above-mentioned technical problems, the technical solution of the present invention is as follows: An integrated process for adsorption and regeneration of tail gas from silicone oil and organosilicon resin production includes the following steps: S1: Exhaust gas pretreatment, the exhaust gas generated during the production of silicone oil or organosilicon resin is sequentially treated by dust removal, washing and gas-liquid separation to remove solid impurities, soluble components and entrained droplets in the exhaust gas, and control the temperature and moisture content of the exhaust gas to a preset range. S2: Electric field pre-polarization, the pre-treated exhaust gas is introduced into the electric field pre-polarization unit, and the siloxane molecules in the exhaust gas are polarized and oriented under the action of high voltage electric field. At the same time, some refractory siloxanes are pre-oxidized and modified by corona discharge to reduce their molecular weight and further reduce the humidity of the exhaust gas. S3: Magnetic stabilized fluidized bed adsorption. The pre-polarized exhaust gas is passed into the magnetic stabilized fluidized bed adsorption unit. The magnetic composite adsorbent adsorbs the siloxanes in the exhaust gas. The adsorbent is kept in a magnetically stable fluidized state by an external alternating magnetic field, so as to achieve efficient mass transfer between the exhaust gas and the adsorbent and obtain purified exhaust gas. S4: Pulse thermal regeneration. When the adsorbent is close to saturation, the system switches to regeneration mode and uses high-frequency electrothermal pulse coupled with hot nitrogen to enhance the regeneration of the adsorbent. This causes the adsorbed siloxanes to be desorbed by heat and carried out of the adsorption unit with hot nitrogen. S5: Desorbed material recovery. Hot nitrogen carrying desorbed siloxanes is introduced into the condensation recovery system. High-boiling-point and low-boiling-point siloxanes are recovered through two-stage condensation. The recovered siloxanes are returned to the production system for reuse. S6: Reset after regeneration. After regeneration is complete, cold nitrogen gas is introduced to reduce the temperature of the adsorbent bed to the preset range, and the system switches back to adsorption mode to realize continuous cycle of adsorption and regeneration. S7: Membrane separation deep treatment. If the purified exhaust gas needs to meet the ultra-low emission standard, the purified exhaust gas after adsorption is introduced into the membrane separation concentration unit. The residual trace amount of siloxane is enriched and concentrated by the hydrophobic composite membrane module. The enriched gas is returned to the pretreatment unit for recycling treatment. The non-permeable side gas is discharged in compliance with the standard. S8: Process collaborative control, through the automatic control system to monitor key parameters in the process in real time, dynamically adjust electric field strength, magnetic field parameters, adsorption and regeneration switching timing, pulse heating parameters and hot nitrogen parameters, to achieve adaptive optimization control of the process.

[0007] Further, in step S1, the exhaust gas pretreatment specifically includes: first, passing the exhaust gas into a cyclone separator to remove dust particles with a diameter of not less than 5μm; then, passing it into a Venturi scrubber to reduce the exhaust gas temperature to 25~40℃ by spraying circulating cooling water; finally, passing it into a gas-liquid separator with a residence time of not less than 10s, and after separating the entrained droplets, controlling the moisture content of the exhaust gas to not exceed 5%.

[0008] Furthermore, in step S2, the electric field pre-polarization unit adopts a flat high-voltage electric field module, the electric field voltage is controlled at 15~30kV, the electric field spacing is 20~50mm, and the residence time of the exhaust gas in the electric field is controlled at 0.5~2.0s; the corona discharge needle array generates corona discharge to generate active oxygen free radicals, which increases the polarizability of siloxane molecules by 30%~50%, and the relative humidity of the exhaust gas after treatment is controlled below 20%.

[0009] Furthermore, in step S3, the magnetic composite adsorbent uses mesoporous molecular sieve as the matrix, loads nano-magnetic particles, and grafts organosilane coupling agents onto the surface; the external alternating magnetic field is provided by three sets of independent controllable coils (upper, middle, and lower), with the magnetic field strength controlled at 0.1~0.5T and the frequency at 1~50Hz; the residence time of the exhaust gas in the fluidized bed is controlled at 5~15s, and the concentration of siloxane in the exhaust gas after adsorption is reduced to no more than 50mg / m³.

[0010] Further, in step S4, pulse thermal regeneration specifically includes: closing the exhaust gas inlet pipe, opening the hot nitrogen circulation pipe, controlling the hot nitrogen temperature at 180~220℃, the pressure at 0.1~0.3MPa, and the flow rate at 20%~30% of the adsorption working gas volume; simultaneously starting the high-frequency electric heating pulse generator, controlling the frequency at 30~40kHz, and the power at 10~15kW, so that the adsorbent particles can be rapidly self-heated, with a heating rate of 50~100℃ / min.

[0011] Further, in step S5, the secondary condensation specifically involves: the first-stage condensation temperature being controlled at 5~10℃ for the recovery of high-boiling-point siloxanes; the second-stage condensation temperature being controlled at -10~-5℃ for the recovery of low-boiling-point siloxanes; and the collected condensate being returned to the silicone oil or organosilicon resin production system for recycling.

[0012] Furthermore, in step S6, after cold nitrogen is introduced, the temperature of the adsorbent bed is reduced to 40~60℃, the entire regeneration cycle is controlled within 30~60 minutes, and the adsorption capacity recovery rate of the adsorbent after a single regeneration is not less than 90%.

[0013] Furthermore, in step S7, the membrane separation and concentration unit adopts a hydrophobic polydimethylsiloxane-ceramic composite tubular membrane module with a membrane pore size of 0.05~0.2μm; the temperature of the membrane module heating jacket is controlled at 40~80℃, and the pressure on the permeate side is maintained at 10~15kPa; the enriched gas is returned to the front end of the pretreatment unit for further treatment, and the concentration of siloxane in the purified gas on the non-permeate side is reduced to no more than 10mg / m³.

[0014] Furthermore, in step S8, the automatic control system adopts a PLC / DCS control system, and the key parameters monitored include tail gas concentration, adsorbent bed temperature, inlet and outlet pressure difference, and adsorbent temperature distribution; the parameters dynamically adjusted include the voltage intensity of the electric field prepolarization unit, the magnetic field intensity and frequency of the magnetically stabilized fluidized bed, the switching timing of adsorption and regeneration, the power and duty cycle of pulse heating, and the flow rate and temperature of hot nitrogen.

[0015] Furthermore, an integrated process and apparatus for adsorption and regeneration of tail gas from silicone oil and organosilicon resin production is provided. The apparatus includes a pretreatment unit, an electric field prepolarization unit, a magnetically stabilized fluidized bed adsorption unit, a pulsed thermal regeneration unit, a condensation recovery system, a membrane separation and concentration unit, and a control and switching system. The pretreatment unit includes a cyclone separator, a venturi scrubber, and a gas-liquid separator, which are connected in series. The electric field prepolarization unit is connected to the outlet of the pretreatment unit and includes a flat plate high-voltage electric field module, a corona discharge needle array and an insulating dielectric barrier layer. The magnetically stabilized fluidized bed adsorption unit is connected to the outlet of the electric field prepolarization unit and includes a vertical cylindrical adsorption tower, a magnetic composite adsorbent, an external alternating magnetic field coil group, a gas distribution plate, and an internal filter baffle. The pulsed thermal regeneration unit is connected to the magnetically stabilized fluidized bed adsorption unit and includes a high-frequency electrothermal pulse generator, a hot nitrogen circulation pipeline, and a regeneration gas flow regulating valve group. The condensation recovery system is connected to the outlet of the pulse heat regeneration unit and is a two-stage condensation structure. The membrane separation and concentration unit is connected to the top outlet of the magnetically stabilized fluidized bed adsorption unit and includes a hydrophobic composite membrane module, a permeate-side vacuum pump, and a membrane module heating jacket. The control and switching system includes a PLC / DCS automatic control system, multi-parameter online monitoring instruments, and electromagnetic switching valve groups, which are electrically connected to each unit to realize automatic control of the entire process.

[0016] Compared with existing technologies, the beneficial effects of this invention are as follows: This integrated process and device for adsorption and regeneration of exhaust gas from silicone oil and organosilicon resin production effectively solves many drawbacks of existing exhaust gas treatment technologies through the coordinated linkage of various units and the optimized design of the entire process, resulting in significant comprehensive benefits. Specific beneficial effects are as follows: First, high purification efficiency and strong emission compliance. The process adopts a three-stage pretreatment process: pretreatment, electric field prepolarization, and magnetically stabilized fluidized bed adsorption. Pretreatment removes solid impurities and excess moisture; electric field prepolarization polarizes and pre-oxidizes siloxane molecules, improving subsequent adsorption efficiency; and the magnetically stabilized fluidized bed achieves efficient mass transfer between the adsorbent and exhaust gas through an alternating magnetic field. After conventional adsorption, the siloxane concentration is reduced to below 50 mg / m³. Adding membrane separation for further treatment as needed can further reduce the siloxane concentration to below 10 mg / m³, meeting ultra-low emission standards and completely solving the exhaust gas pollution problem. Second, excellent adsorbent regeneration effect and long service life. The regeneration method employs a high-frequency electrothermal pulse coupled with hot nitrogen gas, resulting in rapid and uniform heating of the adsorbent at a rate of 50-100℃ / min. The entire regeneration cycle takes only 30-60 minutes, and the adsorption capacity recovery rate after a single regeneration is no less than 90%. This eliminates the need for frequent adsorbent replacements, significantly reducing tail gas treatment costs. Combined with the highly efficient mass transfer characteristics of the magnetic composite adsorbent, the stability of adsorption and regeneration is further enhanced. Thirdly, it achieves resource recycling and improves economic efficiency. Through a two-stage condensation recovery system, high- and low-boiling-point siloxanes are recovered separately. The recovered products can be directly returned to the production system for reuse, effectively reducing raw material waste and production costs, achieving a win-win situation for environmental governance and resource recovery, aligning with the concept of green production. Fourthly, it can operate continuously and is suitable for large-scale production. Through a PLC / DCS automatic control system, seamless switching between adsorption and regeneration modes is achieved. After regeneration, cold nitrogen gas is introduced for rapid reset without shutdown, allowing for continuous tail gas treatment. This perfectly meets the tail gas treatment needs of large-scale silicone oil and organosilicon resin production, improving production continuity. Fifth, it features low energy consumption, reliable operation, and ease of industrial application. Parameters at each stage are dynamically optimized through an automatic control system. Electric field pre-polarization reduces subsequent adsorption load, and pulsed thermal regeneration is precise and efficient, significantly reducing overall energy consumption. The unit is tightly connected, has a reasonable structure, low failure rate, and is easy to operate, making it widely applicable to tail gas treatment in various organosilicon production enterprises. Attached Figure Description

[0017] To more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are merely exemplary. For those skilled in the art, other embodiments can be derived from the provided drawings without creative effort.

[0018] Figure 1A flowchart of an integrated process for adsorption and regeneration of tail gas from the production of silicone oil and organosilicon resin is provided for embodiments of this application. Figure 2 This is a structural diagram of an integrated device for adsorption and regeneration of tail gas from silicone oil and organosilicon resin production, provided in an embodiment of this application. Detailed Implementation

[0019] The accompanying drawings are for illustrative purposes only and should not be construed as limiting the scope of this patent. To better illustrate this embodiment, some parts in the accompanying drawings may be omitted, enlarged, or reduced, and do not represent the actual product dimensions; It will be understood by those skilled in the art that certain well-known structures and their descriptions may be omitted in the accompanying drawings.

[0020] The embodiments of this application will be further described in detail below with reference to the accompanying drawings and examples.

[0021] It is understood that the specific embodiments described herein are merely illustrative of the embodiments of this application and are not intended to limit the embodiments of this application. Furthermore, it should be noted that, for ease of description, the accompanying drawings only show the parts related to the embodiments of this application, not all structures. Those skilled in the art, after reading this specification, should be able to realize that any combination of technical features can constitute an optional implementation method, provided that the technical features do not contradict each other.

[0022] The terms "first," "second," etc., used in the specification and claims of this application are used to distinguish similar objects and not to describe a specific order or sequence. It should be understood that such use of data can be interchanged where appropriate so that embodiments of this application can be implemented in orders other than those illustrated or described herein, and the objects distinguished by "first," "second," etc., are generally of the same class and the number of objects is not limited; for example, a first object can be one or more. Furthermore, in the specification and claims, "and / or" indicates at least one of the connected objects, and the character " / " generally indicates that the preceding and following objects are in an "or" relationship. In the description of this application, "multiple" means two or more, and "several" means one or more.

[0023] This implementation method takes the siloxane-containing tail gas generated during the production of methyl silicone oil as the specific treatment object, and elaborates on each step of the process, operating parameters, equipment requirements and control logic. At the same time, it clarifies the unit structure, connection relationship and working principle of the supporting equipment to ensure the reproducibility, stability and reliability of the process, and takes into account environmental protection compliance, resource recovery and production efficiency. It solves the technical pain points of low efficiency of tail gas treatment in existing organosilicon production, poor regeneration effect of adsorbent, resource waste, inability to operate continuously and difficulty in achieving ultra-low emissions.

[0024] The core idea of ​​this invention is to achieve efficient removal of siloxanes from exhaust gas, recycling of adsorbents, and recovery of siloxane resources through an integrated design of the entire process from pretreatment to prepolarization, adsorption, regeneration, recovery, and deep treatment, combined with the synergistic effect of electric, magnetic, and thermal fields. At the same time, through automatic collaborative control, the parameters of each process link are optimized and matched to achieve continuous and stable operation, which is suitable for the exhaust gas treatment needs of large-scale organosilicon production.

[0025] Before starting this integrated process, it is necessary to complete the preparation of raw materials, commissioning of supporting equipment, and pretreatment to ensure the smooth operation of subsequent processes and guarantee process stability and treatment effect. The specific preparations are as follows: According to the technical specifications, a magnetic composite adsorbent is prepared. This adsorbent uses a mesoporous molecular sieve (preferably MCM-41 mesoporous molecular sieve) as the matrix and loads nano-magnetic particles (preferably nano-Fe3O4 particles, 5-10 nm in diameter) at a loading amount of 5%-10% of the mass of the mesoporous molecular sieve. After loading, an organosilane coupling agent (preferably γ-aminopropyltriethoxysilane) is grafted onto the surface of the adsorbent at a grafting amount of 2%-5% of the adsorbent mass. The prepared magnetic composite adsorbent needs to be dried at 100-120℃ for 2-3 hours to remove surface moisture and ensure adsorption activity. After drying, it is sealed and stored for later use. This adsorbent possesses good adsorption performance, magnetic responsiveness, and chemical stability. It can achieve stable fluidization under an alternating magnetic field and can efficiently adsorb siloxanes in exhaust gases.

[0026] Auxiliary gas preparation: Prepare nitrogen (purity ≥ 99.99%) as the hot nitrogen carrier during adsorbent regeneration, cold nitrogen for reset after regeneration, and system inert protection; Prepare compressed air (dried and degreased, dew point ≤ -40℃) for purging and cleaning each unit of the device to prevent impurities from accumulating and affecting operation.

[0027] Other auxiliary materials include preparing circulating cooling water (water temperature controlled at 15-20℃) for the exhaust gas washing and cooling of the Venturi scrubber and the cooling of the condensation recovery system; preparing monitoring sensors (temperature, pressure, concentration, humidity sensors, etc.) required for the PLC / DCS control system to ensure that each key parameter can be monitored in real time; and preparing seals, valve grease, etc. for sealing each pipeline and equipment of the device to prevent exhaust gas leakage.

[0028] Please see Figure 2 The supporting equipment for this process includes a pretreatment unit, an electric field prepolarization unit, a magnetically stabilized fluidized bed adsorption unit, a pulsed thermal regeneration unit, a condensation recovery system, a membrane separation and concentration unit, and a control and switching system. These units are connected sequentially and work collaboratively. During commissioning, it is essential to ensure that each unit operates normally and that parameters meet standards. Specific commissioning procedures are as follows: The pretreatment unit includes a cyclone separator, a venturi scrubber, and a gas-liquid separator, connected in series. The cyclone separator is tested by checking the sealing of its inlet and outlet pipes. The fan is started to simulate exhaust gas flow, and the air velocity is adjusted to 15-20 m / s to ensure effective removal of dust particles with a diameter of not less than 5 μm. After testing, the bottom ash hopper of the cyclone separator is cleaned to ensure no dust accumulation. The venturi scrubber is tested by checking the spray system for smooth operation. The circulating cooling water flow rate is controlled at 5-10 m³ / h to ensure uniform spraying and to reduce the exhaust gas temperature to 25-40℃. The scrubbing liquid circulation system is also checked to ensure no leaks or blockages. The gas-liquid separator is tested by checking the liquid level control system inside the tank and adjusting the residence time to 10-15 seconds to ensure effective separation of liquid droplets entrained in the exhaust gas and to control the exhaust gas moisture content to not exceed 5%. After testing, the accumulated liquid at the bottom of the gas-liquid separator is drained, and the inside of the tank is cleaned.

[0029] The electric field pre-polarization unit is connected to the pretreatment unit outlet and includes a flat-plate high-voltage electric field module, a corona discharge needle array, and an insulating dielectric barrier layer. The flat-plate high-voltage electric field module is debugged, adjusting the electric field voltage to 15-30kV adjustable and the electric field spacing to 20-50mm (preferably 30mm) to ensure uniform electric field distribution and no local discharge anomalies. The corona discharge needle array is debugged, checking for integrity and uniform arrangement of the needles. The high-voltage power supply is started to generate corona discharge, ensuring sufficient active oxygen free radicals are generated to increase the polarizability of siloxane molecules by 30%-50%. The insulating dielectric barrier layer is debugged, checking its insulation performance to prevent electric field leakage and ensure operational safety. Simulated exhaust gas is introduced, controlling the residence time of the exhaust gas in the electric field to 0.5-2.0s (preferably 1.0s). The relative humidity of the treated exhaust gas is monitored, ensuring it drops below 20%. After debugging, the high-voltage power supply is turned off and put into standby mode.

[0030] The magnetically stabilized fluidized bed adsorption unit is connected to the outlet of the electric field prepolarization unit and includes a vertical cylindrical adsorption tower, a magnetic composite adsorbent, an external alternating magnetic field coil group, a gas distribution plate, and an internal filter baffle. The prepared magnetic composite adsorbent is loaded into the adsorption tower, with a loading volume of 40%-50% of the effective volume of the tower, ensuring uniform distribution of the adsorbent. The external alternating magnetic field coil group (three independently controllable coils, upper, middle and lower) is adjusted, with the magnetic field strength set to 0.1-0.5T (preferably 0.3T) and the frequency set to 1-50Hz (preferably 10Hz). The magnetic field is then started, and the fluidization state of the adsorbent is observed to ensure that the adsorbent is in a stable fluidized state without clumping or channeling. The gas distribution plate is adjusted to ensure uniform gas distribution and sufficient contact between the exhaust gas and the adsorbent, with the residence time of the exhaust gas in the fluidized bed controlled to be 5-15s (preferably 10s). The built-in filter baffle is adjusted and its filtration effect is checked to prevent adsorbent particles from being carried out by the exhaust gas. After adjustment, nitrogen is introduced to purge the tower to remove internal impurities and air, and it is ready for use.

[0031] The pulsed thermal regeneration unit is connected to the magnetically stabilized fluidized bed adsorption unit and includes a high-frequency electrothermal pulse generator, a hot nitrogen circulation pipeline, and a regeneration gas flow regulating valve group. The high-frequency electrothermal pulse generator is debugged, adjusting the frequency to 30-40kHz (preferably 35kHz) and the power to 10-15kW (preferably 12kW) to ensure stable high-frequency electrothermal pulses are generated, enabling rapid self-heating of the adsorbent particles at a rate of 50-100℃ / min (preferably 80℃ / min). The hot nitrogen circulation pipeline is debugged, checking the pipeline connection seals. The nitrogen heating device is started, controlling the hot nitrogen temperature at 180-220℃ (preferably 200℃), adjusting the pressure to 0.1-0.3MPa (preferably 0.2MPa), and adjusting the flow rate to 20%-30% (preferably 25%) of the adsorption working gas volume. The regeneration gas flow regulating valve group is debugged, ensuring precise and stable flow regulation. After debugging, a no-load test run is performed to check that all components are operating normally, and it is then ready for use.

[0032] The condensation recovery system is connected to the outlet of the pulse heat regeneration unit and is a two-stage condensation structure. The first-stage condenser is debugged, adjusting the condensation temperature to 5-10℃ (preferably 8℃) for the recovery of high-boiling-point siloxanes (such as octamethylcyclotetrasiloxane); the second-stage condenser is debugged, adjusting the condensation temperature to -10 to -5℃ (preferably -8℃) for the recovery of low-boiling-point siloxanes (such as hexamethylcyclotrisiloxane); the condensate collection tank and delivery pipelines are checked to ensure no leaks and that the condensate can be smoothly delivered to the production system for reuse; the refrigeration unit of the condensation system is debugged to ensure stable cooling performance and precise temperature control. After debugging, a no-load test run is performed, and the system is put into standby.

[0033] The membrane separation and concentration unit is connected to the top outlet of the magnetically stabilized fluidized bed adsorption unit and includes a hydrophobic polydimethylsiloxane-ceramic composite tubular membrane module, a permeate-side vacuum pump, and a membrane module heating jacket. The hydrophobic composite membrane module is debugged, and its sealing is checked to ensure no leakage; the membrane pore size is 0.05-0.2 μm (preferably 0.1 μm). The membrane module heating jacket is debugged, and the temperature is adjusted to 40-80℃ (preferably 60℃) to ensure stable membrane module temperature. The permeate-side vacuum pump is debugged, and the permeate-side pressure is maintained at 10-15 kPa (preferably 12 kPa) to ensure membrane separation efficiency. Simulated purified tail gas is introduced, and the siloxane concentration in the non-permeate-side gas is monitored to ensure it can be reduced to no more than 10 mg / m³, and the enriched gas can be smoothly returned to the front end of the pretreatment unit. After debugging, it is ready for use.

[0034] The control and switching system includes a PLC / DCS automatic control system, multi-parameter online monitoring instruments, and an electromagnetic switching valve group, which are electrically connected to each unit respectively. Debug the multi-parameter online monitoring instruments, including tail gas concentration sensors, adsorbent bed temperature sensors, inlet and outlet pressure difference sensors, and adsorbent temperature distribution sensors, to ensure accurate and real-time transmission of the monitoring data of each sensor; debug the electromagnetic switching valve group to ensure flexible valve switching and good sealing, and enable seamless switching between the adsorption and regeneration modes; debug the PLC / DCS control system, input preset parameters (such as adsorption temperature, electric field voltage, magnetic field parameters, regeneration temperature, etc.), set parameter alarm thresholds, and debug the dynamic adjustment function to ensure that the key process parameters can be monitored in real time and the electric field strength, magnetic field parameters, adsorption and regeneration switching timing, pulse heating parameters, and hot nitrogen parameters can be dynamically adjusted to achieve process adaptive optimization control. After debugging, conduct a full-system linkage trial operation to ensure the normal collaborative work of each unit.

[0035] Start the nitrogen purging system to purge the pipelines and each unit equipment of the entire process device for 30 - 60 minutes to remove the air, dust, and impurities in the equipment and pipelines, and avoid impurities affecting the adsorption effect and equipment operation; check the sealing conditions of each unit to ensure no tail gas leakage; start auxiliary equipment such as the circulating cooling water system, refrigeration unit, and heating device, and run them to a stable state to ensure that the parameters of each auxiliary system meet the standards; load the magnetic composite adsorbent into the magnetically stabilized fluidized bed adsorption unit, start the external alternating magnetic field, and make the adsorbent in a stable fluidized state for standby.

[0036] This process operates according to the process flow of S1 tail gas pretreatment → S2 electric field pre-polarization → S3 magnetically stabilized fluidized bed adsorption → S4 pulse thermal regeneration → S5 desorbed matter recovery → S6 reset after regeneration, and performs S7 membrane separation deep treatment as required. The parameter optimization is achieved through S8 process collaborative control throughout the process. The specific implementation steps are as follows: Please refer to Figure 1 , S1: Tail gas pretreatment. The purpose of this step is to remove solid impurities, soluble components, and entrained liquid droplets in the tail gas, control the tail gas temperature and moisture content within the preset range, and lay a foundation for subsequent electric field pre-polarization and adsorption treatment, and avoid impurities affecting the pre-polarization effect and adsorbent performance. The specific operations are as follows: Introduce the siloxane-containing tail gas (temperature 60 - 80°C, moisture content 15% - 20%, siloxane concentration 500 - 1000 mg / m³, containing dust particles with a particle size of 2 - 10 μm and a small amount of soluble organic impurities) generated during the silicone oil production process into the pretreatment unit through an induced draft fan, and sequentially pass through a cyclone separator, a Venturi scrubber, and a gas-liquid separation tank for treatment.

[0037] First, the exhaust gas is introduced into a cyclone separator, and the fan speed is adjusted to 18 m / s. Centrifugal force is used to remove dust particles with a diameter of not less than 5 μm. These dust particles settle into the ash hopper at the bottom of the cyclone separator under centrifugal force. The ash hopper is cleaned regularly (every 2 hours) to prevent excessive dust accumulation from affecting the dust removal efficiency. The dust-removed exhaust gas then enters a Venturi scrubber, where circulating cooling water (18℃, flow rate 8 m³ / h) is sprayed through a spray system. This ensures full contact between the exhaust gas and the cooling water, washing away soluble organic components and lowering the exhaust gas temperature to 25-40℃ (preferably 30℃) to prevent high-temperature exhaust gas from affecting subsequent electric field pre-polarization and adsorption effects.

[0038] After washing, the exhaust gas, carrying some liquid droplets, enters a gas-liquid separator. The residence time of the exhaust gas in the separator is controlled at 12 seconds. Through gravity settling, the liquid droplets entrained in the exhaust gas are separated and settle to the bottom of the separator. These droplets are periodically discharged and subjected to harmless treatment. The exhaust gas after gas-liquid separation is monitored in real time by a moisture content sensor to ensure that the moisture content is controlled to be no more than 5% (preferably 4%) and the temperature is stabilized at around 30°C. The pretreated exhaust gas that meets the requirements proceeds to the next process step. If the moisture content or temperature of the exhaust gas is found to be below the standard, the cooling water flow rate of the Venturi scrubber or the residence time in the gas-liquid separator is adjusted until the standard is met before the gas enters the electric field pre-polarization unit.

[0039] S2: Electric Field Pre-polarization. The purpose of this step is to polarize and orient the siloxane molecules in the exhaust gas, thereby improving their subsequent adsorption performance. Simultaneously, corona discharge is used to pre-oxidize and modify some recalcitrant siloxanes, reducing their molecular weight and further lowering the humidity of the exhaust gas. This provides favorable conditions for magnetically stabilized fluidized bed adsorption. The specific operation is as follows: The pretreated exhaust gas is introduced into the electric field pre-polarization unit, which uses a flat-plate high-voltage electric field module. The electric field voltage is adjusted to 22kV, the electric field spacing is 30mm, and the residence time of the exhaust gas in the electric field is controlled to be 1.0s. The high-voltage power supply is activated, and the flat-plate high-voltage electric field generates a stable high-voltage electric field. Under the action of the high-voltage electric field, the siloxane molecules in the exhaust gas undergo polarization orientation, increasing their molecular polarity and facilitating subsequent adsorption by the magnetic composite adsorbent. Simultaneously, the corona discharge needle array generates corona discharge, producing a large number of active oxygen free radicals (such as ·OH, ·O2⁻). These active oxygen free radicals react with some of the recalcitrant high-molecular-weight siloxanes in the exhaust gas, pre-oxidizing and modifying them, decomposing them into low-molecular-weight siloxanes, reducing their adsorption difficulty, and further removing moisture from the exhaust gas, ensuring that the relative humidity of the treated exhaust gas is controlled below 20% (preferably 15%).

[0040] During the electric field pre-polarization process, the electric field voltage, exhaust gas residence time, exhaust gas relative humidity, and siloxane molecular polarizability are monitored in real time by a PLC / DCS control system. If the monitored polarizability is less than 30%-50% (preferably 40%), the electric field voltage or exhaust gas residence time is adjusted; if the exhaust gas relative humidity exceeds 20%, the corona discharge power is increased to ensure that the pre-polarization effect meets the standard. The exhaust gas after pre-polarization is directly introduced into the magnetically stabilized fluidized bed adsorption unit for the next process step.

[0041] S3: Magnetic Stabilized Fluidized Bed Adsorption. This step is the core of exhaust gas purification. Its purpose is to utilize a magnetic composite adsorbent to efficiently adsorb siloxanes in the exhaust gas. An external alternating magnetic field keeps the adsorbent in a magnetically stable fluidized state, achieving efficient mass transfer between the exhaust gas and the adsorbent, resulting in purified exhaust gas. The specific operation is as follows: The pre-polarized exhaust gas is introduced into the magnetically stabilized fluidized bed adsorption unit. The exhaust gas flow rate is adjusted, and the residence time of the exhaust gas in the fluidized bed is controlled to be 10 seconds to ensure sufficient contact between the exhaust gas and the magnetic composite adsorbent. The external alternating magnetic field coil group is started, and the magnetic field strength is adjusted to 0.3T and the frequency to 10Hz. Under the action of the alternating magnetic field, the magnetic composite adsorbent (with mesoporous molecular sieve as the matrix, loaded with nano-Fe3O4 particles, and grafted with organosilane coupling agent on the surface) is in a magnetically stable fluidized state. This avoids the problem of low mass transfer efficiency in fixed bed adsorption and overcomes the disadvantages of easy adsorbent loss and unstable fluidization in ordinary fluidized bed adsorbents, thus achieving efficient mass transfer between exhaust gas and adsorbent.

[0042] The magnetic composite adsorbent uses its surface active sites to physically and chemically adsorb siloxanes (including pre-oxidized low-molecular-weight siloxanes and unmodified siloxanes) in the exhaust gas. During the adsorption process, the adsorbent bed temperature, the concentration of siloxanes in the inlet and outlet exhaust gas, and the inlet and outlet pressure difference are monitored in real time by a PLC / DCS control system. In the initial adsorption stage, the adsorbent has sufficient adsorption capacity, and the concentration of siloxanes in the outlet exhaust gas decreases rapidly. When the concentration of siloxanes in the outlet exhaust gas drops to no more than 50 mg / m³ (preferably 40 mg / m³), the adsorption reaches a stable state, and the purified exhaust gas can be directly discharged (if ultra-low emission standards are required, it enters the S7 membrane separation deep treatment). When the concentration of siloxanes in the outlet exhaust gas continues to rise, approaching 50 mg / m³, and the inlet and outlet pressure difference reaches the preset threshold (0.05-0.1 MPa), it indicates that the adsorbent adsorption is close to saturation, and the system prepares to switch to regeneration mode.

[0043] If abnormal fluidization state of the adsorbent is detected during adsorption (such as agglomeration or channeling), adjust the intensity and frequency of the external alternating magnetic field to ensure that the adsorbent is in a stable fluidization state. If the adsorption efficiency drops too quickly, check the treatment effect of the pretreatment unit to ensure that the impurity content in the exhaust gas meets the standard and to avoid impurities clogging the active sites of the adsorbent.

[0044] S4: Pulse Thermal Regeneration. When the adsorbent approaches saturation, the system automatically switches to regeneration mode via PLC / DCS control. This step aims to enhance adsorption regeneration by coupling high-frequency electrothermal pulses with hot nitrogen gas, causing the adsorbed siloxanes to desorb upon heating and be carried out of the adsorption unit with the hot nitrogen gas, thus restoring the adsorption capacity of the adsorbent. The specific operation is as follows: First, the exhaust gas inlet pipe is closed by the electromagnetic switching valve group, cutting off the channel for the exhaust gas to enter the magnetically stabilized fluidized bed adsorption unit. At the same time, the hot nitrogen circulation pipe is opened, the nitrogen heating device is started, the hot nitrogen temperature is controlled at 200℃, the pressure is adjusted to 0.2MPa, and the flow rate is adjusted to 25% of the adsorption working gas volume. The hot nitrogen is introduced into the magnetically stabilized fluidized bed adsorption unit in a countercurrent manner to preheat the adsorbent.

[0045] After preheating for 5 minutes, the high-frequency electrothermal pulse generator is started, with the frequency adjusted to 35kHz and the power to 12kW. The high-frequency electrothermal pulse acts on the magnetic composite adsorbent particles, causing the adsorbent particles to rapidly self-heat at a rate of 80℃ / min. The temperature of the adsorbent bed quickly rises to 180-220℃ (matching the temperature of the hot nitrogen). Under high temperature, the siloxanes adsorbed on the surface of the adsorbent are desorbed. The desorbed siloxanes are thoroughly mixed with the hot nitrogen and carried out of the magnetically stabilized fluidized bed adsorption unit along with the hot nitrogen, entering the condensation and recovery system.

[0046] During regeneration, the PLC / DCS control system monitors the adsorbent bed temperature, hot nitrogen temperature, pressure, and flow rate in real time. Simultaneously, it monitors the siloxane concentration at the hot nitrogen outlet. If the adsorbent bed temperature rises too slowly, the power of the high-frequency heating pulse is adjusted. If the siloxane concentration at the hot nitrogen outlet continues to decrease, it indicates that desorption is nearing completion. Throughout the regeneration process, stable hot nitrogen circulation is ensured to prevent temperature and pressure fluctuations from causing poor regeneration results. Additionally, an internal filter baffle prevents adsorbent particles from being carried out by the hot nitrogen, ensuring that the adsorbent remains within the adsorption unit.

[0047] S5: Desorbate Recovery. The purpose of this step is to separate and recover the siloxanes from the hot nitrogen gas carrying the desorbed siloxanes, achieving resource recycling and reducing production costs. The specific operation is as follows: Hot nitrogen gas (temperature 180-220℃, siloxane concentration 300-500mg / m³) carrying desorbed siloxanes is introduced into a condensation recovery system. This system is a two-stage condensation structure, passing through a first-stage condenser and a second-stage condenser to recover high-boiling-point and low-boiling-point siloxanes, respectively.

[0048] The condensing temperature of the first-stage condenser is controlled at 8°C to recover high-boiling-point siloxanes (such as octamethylcyclotetrasiloxane, with a boiling point of 175°C). After hot nitrogen enters the first-stage condenser, its temperature drops rapidly to 8°C, and the high-boiling-point siloxanes condense into liquid and settle to the bottom of the condensate collection tank. The hot nitrogen after the first-stage condensation (at a temperature of around 8°C, still containing low-boiling-point siloxanes) enters the second-stage condenser, where the condensing temperature is controlled at -8°C. The low-boiling-point siloxanes (such as hexamethylcyclotrisiloxane, with a boiling point of 134°C) condense into liquid at the low temperature and settle to the bottom of another condensate collection tank.

[0049] After two-stage condensation, the siloxane liquid in the condensate collection tank (high-boiling and low-boiling points are collected separately) is returned to the silicone oil production system via a pre-set flow rate through a transfer pump for reuse as a production raw material, achieving resource recycling and reducing raw material waste. The condensed nitrogen gas (around -5℃) is heated to 40-60℃ by a heating device and can be recycled as hot nitrogen for subsequent adsorbent regeneration, further reducing energy consumption. If the condensate contains a small amount of impurities, it can be simply filtered before being returned to the production system to ensure that product quality is not affected.

[0050] S6: Reset after regeneration. The purpose of this step is to reduce the temperature of the regenerated adsorbent bed to a preset range, restore the adsorption activity of the adsorbent, and switch the system back to adsorption mode, achieving a continuous cycle of adsorption and regeneration. The specific operation is as follows: When the concentration of siloxane at the hot nitrogen outlet drops below 10 mg / m³, it indicates that the adsorbent regeneration is complete. Turn off the high-frequency electric heating pulse generator, stop the hot nitrogen heating, switch the hot nitrogen circulation pipeline to the cold nitrogen pipeline, and introduce room temperature nitrogen (around 25°C). The cold nitrogen is introduced into the magnetically stabilized fluidized bed adsorption unit in a co-current manner to cool the adsorbent bed.

[0051] The adsorbent bed temperature is monitored in real time by a PLC / DCS control system, and the flow rate of cold nitrogen is controlled to ensure a stable temperature drop and avoid thermal stress caused by excessively rapid cooling, which could lead to adsorbent particle breakage. When the adsorbent bed temperature drops to 40-60℃ (preferably 50℃), the cold nitrogen pipeline is shut off, and nitrogen supply is stopped. At this point, the adsorption capacity recovery rate of the adsorbent is not less than 90% (preferably 95%), and the adsorbent regains its adsorption activity.

[0052] Subsequently, the PLC / DCS control system controls the electromagnetic switching valve group to close the relevant pipelines in the regeneration mode and open the exhaust gas inlet pipeline. The system switches back to adsorption mode, and the pretreated exhaust gas is reintroduced into the magnetically stabilized fluidized bed adsorption unit to begin a new round of adsorption. The entire regeneration cycle is controlled within 30-60 minutes (preferably 45 minutes) to ensure that the regeneration efficiency matches the adsorption efficiency, achieving continuous cycling of adsorption and regeneration without downtime, thus meeting the needs of large-scale production.

[0053] S7: Membrane separation for advanced treatment. If the purified exhaust gas needs to meet ultra-low emission standards (siloxane concentration ≤10mg / m³), then after adsorption in the S3 magnetically stabilized fluidized bed, the purified exhaust gas is introduced into the membrane separation concentration unit for advanced treatment. The specific operation is as follows: The purified tail gas (siloxane concentration ≤50mg / m³) after adsorption by the magnetically stabilized fluidized bed is introduced into the membrane separation concentration unit. This unit uses a hydrophobic polydimethylsiloxane-ceramic composite tubular membrane module with a membrane pore size of 0.1μm. The temperature of the membrane module heating jacket is adjusted to 60℃, and the permeate side vacuum pump is started to maintain the permeate side pressure at 12kPa.

[0054] When the purified exhaust gas passes through the hydrophobic composite membrane module, due to the hydrophobicity and selectivity of the membrane module, trace amounts of siloxane molecules in the exhaust gas can permeate through the membrane module into the permeate side, forming enriched gas (siloxane concentration rises to 200-300 mg / m³). The enriched gas is returned to the front end of the pretreatment unit through pipelines, mixed with fresh exhaust gas, and then pretreated and adsorbed again to achieve cyclic treatment and ensure complete removal of trace amounts of siloxane. The gas on the non-permeate side is the deeply purified exhaust gas, which is monitored in real time by a siloxane concentration sensor to ensure that the siloxane concentration drops to no more than 10 mg / m³ (preferably 8 mg / m³), and is directly discharged after meeting the standard.

[0055] During the membrane separation deep treatment process, the membrane module temperature, permeate side pressure, and non-permeate side tail gas concentration are monitored in real time by the PLC / DCS control system. If the non-permeate side tail gas concentration exceeds 10 mg / m³, the membrane module temperature or permeate side pressure is adjusted to ensure the deep treatment effect. The membrane module is cleaned regularly (every 72 hours) by nitrogen purging combined with organic solvent rinsing to remove residual siloxanes on the membrane surface, prevent membrane clogging, and ensure stable membrane separation efficiency.

[0056] S8: Process Coordination Control. This step is implemented throughout the entire process. Its purpose is to monitor key parameters in the process in real time through the automatic control system, dynamically adjust the parameters of each unit, and achieve adaptive optimization control of the process to ensure stable operation and achieve the required treatment results. The specific operation is as follows: The system employs a PLC / DCS automatic control system, which uses multi-parameter online monitoring instruments to monitor key parameters in the process in real time, including: tail gas concentration (siloxane concentration before and after pretreatment, before and after adsorption, and before and after membrane separation), adsorbent bed temperature, inlet and outlet pressure difference of adsorption unit, adsorbent temperature distribution, electric field voltage, magnetic field strength and frequency, hot nitrogen temperature and pressure, condensation temperature, membrane module temperature and permeate side pressure, etc.

[0057] Based on the monitored parameter changes, the system automatically and dynamically adjusts relevant parameters: when the moisture content of the pretreated exhaust gas exceeds 5% or the temperature exceeds 40℃, the cooling water flow rate of the Venturi scrubber is automatically adjusted; when the polarizability of siloxane molecules is insufficient after electric field pre-polarization, the electric field voltage or exhaust gas residence time is automatically adjusted; when the pressure difference between the inlet and outlet of the magnetically stabilized fluidized bed adsorption unit is too large, the magnetic field parameters or exhaust gas flow rate are automatically adjusted to avoid adsorbent agglomeration; when the adsorbent adsorption is close to saturation, the system automatically switches to regeneration mode; when the adsorbent bed temperature rises too slowly during regeneration, the high-frequency electric heating pulse power or hot nitrogen temperature is automatically adjusted; when the exhaust gas concentration on the non-permeate side of the membrane separation does not meet the standard, the membrane module temperature or permeate side pressure is automatically adjusted.

[0058] Meanwhile, the system sets parameter alarm thresholds. When a critical parameter exceeds the preset range, an alarm signal is automatically issued to remind staff to check and handle the issue promptly, preventing process failures from causing a decrease in processing effectiveness or equipment damage. Through process collaborative control, the system achieves optimized matching of parameters in each process step, ensuring stable and efficient operation of the entire process, reducing manual labor intensity, and improving the automation level and reliability of the process.

[0059] The exhaust gas, after deep treatment by adsorption or membrane separation, meets the emission standards and is discharged through an exhaust stack. Before discharge, online monitoring equipment must be used to monitor indicators such as siloxane concentration and particulate matter concentration in real time to ensure compliance with relevant national and local emission standards. Monitoring data is uploaded to the environmental protection supervision platform in real time. The siloxane condensate collected by the condensation recovery system is returned to the silicone oil or organosilicon resin production system after filtering to remove impurities, and reused as a production raw material. The purity of the recovered siloxane is tested regularly to ensure that it does not affect product quality. If the purity does not meet the standards, it needs to be purified by distillation before reuse. The dust particles collected by the cyclone separator and the liquid discharged from the gas-liquid separator must be treated to render them harmless. The dust particles can be landfilled or incinerated, and the liquid is distilled and discharged in compliance with standards or recycled to avoid secondary pollution.

[0060] Compared with traditional single adsorption processes, this process not only achieves efficient purification of exhaust gas, but also realizes the recycling and regeneration of adsorbent and the recovery and utilization of siloxane resources. At the same time, through automatic coordinated control, it achieves continuous and stable operation, solving many drawbacks of traditional processes and resulting in significant comprehensive benefits.

[0061] The same or similar labels correspond to the same or similar parts; The terms used to describe positional relationships in the accompanying drawings are for illustrative purposes only and should not be construed as limiting this patent. Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the implementation of the present invention. For those skilled in the art, other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all implementation methods here. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the claims of the present invention.

Claims

1. An integrated process for adsorption and regeneration of tail gas from silicone oil and organosilicon resin production, characterized in that, Specifically, the following steps are included: S1: Exhaust gas pretreatment, the exhaust gas generated during the production of silicone oil or organosilicon resin is sequentially treated by dust removal, washing and gas-liquid separation to remove solid impurities, soluble components and entrained droplets in the exhaust gas, and control the temperature and moisture content of the exhaust gas to a preset range. S2: Electric field pre-polarization, the pre-treated exhaust gas is introduced into the electric field pre-polarization unit, and the siloxane molecules in the exhaust gas are polarized and oriented under the action of high voltage electric field. At the same time, some refractory siloxanes are pre-oxidized and modified by corona discharge to reduce their molecular weight and further reduce the humidity of the exhaust gas. S3: Magnetic stabilized fluidized bed adsorption. The pre-polarized exhaust gas is passed into the magnetic stabilized fluidized bed adsorption unit. The magnetic composite adsorbent adsorbs the siloxanes in the exhaust gas. The adsorbent is kept in a magnetically stable fluidized state by an external alternating magnetic field, so as to achieve efficient mass transfer between the exhaust gas and the adsorbent and obtain purified exhaust gas. S4: Pulse thermal regeneration. When the adsorbent is close to saturation, the system switches to regeneration mode and uses high-frequency electrothermal pulse coupled with hot nitrogen to enhance the regeneration of the adsorbent. This causes the adsorbed siloxanes to be desorbed by heat and carried out of the adsorption unit with hot nitrogen. S5: Desorbed material recovery. Hot nitrogen carrying desorbed siloxanes is introduced into the condensation recovery system. High-boiling-point and low-boiling-point siloxanes are recovered through two-stage condensation. The recovered siloxanes are returned to the production system for reuse. S6: Reset after regeneration. After regeneration is complete, cold nitrogen gas is introduced to reduce the temperature of the adsorbent bed to the preset range, and the system switches back to adsorption mode to realize continuous cycle of adsorption and regeneration. S7: Membrane separation deep treatment. If the purified exhaust gas needs to meet the ultra-low emission standard, the purified exhaust gas after adsorption is introduced into the membrane separation concentration unit. The residual trace amount of siloxane is enriched and concentrated by the hydrophobic composite membrane module. The enriched gas is returned to the pretreatment unit for recycling treatment. The non-permeable side gas is discharged in compliance with the standard. S8: Process collaborative control, through the automatic control system to monitor key parameters in the process in real time, dynamically adjust electric field strength, magnetic field parameters, adsorption and regeneration switching timing, pulse heating parameters and hot nitrogen parameters, to achieve adaptive optimization control of the process.

2. The process according to claim 1, characterized in that, In step S1, the exhaust gas pretreatment specifically includes: first, the exhaust gas is introduced into a cyclone separator to remove dust particles with a diameter of not less than 5μm; then it enters a venturi scrubber, where the exhaust gas temperature is reduced to 25~40℃ by spraying circulating cooling water; finally, it enters a gas-liquid separator, where the residence time is not less than 10s, and after separating the entrained droplets, the moisture content of the exhaust gas is controlled to not exceed 5%.

3. The process according to claim 1, characterized in that, In step S2, the electric field prepolarization unit adopts a flat plate high-voltage electric field module, with the electric field voltage controlled at 15~30kV, the electric field spacing at 20~50mm, and the residence time of the exhaust gas in the electric field controlled at 0.5~2.0s; the corona discharge needle array generates corona discharge to generate active oxygen free radicals, which increases the polarizability of siloxane molecules by 30%~50%, and the relative humidity of the exhaust gas after treatment is controlled below 20%.

4. The process according to claim 1, characterized in that, In step S3, the magnetic composite adsorbent uses mesoporous molecular sieve as the matrix, loads nano-magnetic particles, and grafts organosilane coupling agents onto the surface; the external alternating magnetic field is provided by three sets of independent controllable coils (upper, middle, and lower), with the magnetic field strength controlled at 0.1~0.5T and the frequency at 1~50Hz; the residence time of the exhaust gas in the fluidized bed is controlled at 5~15s, and the concentration of siloxane in the exhaust gas after adsorption is reduced to no more than 50mg / m³.

5. The process according to claim 1, characterized in that, In step S4, pulse thermal regeneration specifically includes: closing the exhaust gas inlet pipe, opening the hot nitrogen circulation pipe, controlling the hot nitrogen temperature at 180~220℃, the pressure at 0.1~0.3MPa, and the flow rate at 20%~30% of the adsorption working gas volume; simultaneously starting the high-frequency electric heating pulse generator, controlling the frequency at 30~40kHz, and the power at 10~15kW, so that the adsorbent particles can be rapidly self-heated, with a heating rate of 50~100℃ / min.

6. The process according to claim 1, characterized in that, In step S5, the secondary condensation is specifically as follows: the first-stage condensation temperature is controlled at 5~10℃, which is used to recover high-boiling-point siloxanes; the second-stage condensation temperature is controlled at -10~-5℃, which is used to recover low-boiling-point siloxanes; the condensate is collected and returned to the silicone oil or organosilicon resin production system for recycling.

7. The process according to claim 1, characterized in that, In step S6, after cold nitrogen is introduced, the temperature of the adsorbent bed is reduced to 40~60℃. The entire regeneration cycle is controlled within 30~60 minutes, and the adsorption capacity recovery rate of the adsorbent after a single regeneration is not less than 90%.

8. The process according to claim 1, characterized in that, In step S7, the membrane separation and concentration unit uses a hydrophobic polydimethylsiloxane-ceramic composite tubular membrane module with a membrane pore size of 0.05~0.2μm; the temperature of the membrane module heating jacket is controlled at 40~80℃, and the permeate side pressure is maintained at 10~15kPa. The enriched gas is returned to the front end of the pretreatment unit for further processing, and the concentration of siloxane in the purified gas on the non-permeable side is reduced to no more than 10 mg / m³.

9. The process according to claim 1, characterized in that, In step S8, the automatic control system adopts a PLC / DCS control system. The key parameters monitored include tail gas concentration, adsorbent bed temperature, inlet and outlet pressure difference, and adsorbent temperature distribution. The parameters dynamically adjusted include the voltage intensity of the electric field prepolarization unit, the magnetic field intensity and frequency of the magnetically stabilized fluidized bed, the switching timing of adsorption and regeneration, the power and duty cycle of pulse heating, and the flow rate and temperature of hot nitrogen.

10. An integrated process and apparatus for adsorption and regeneration of tail gas from silicone oil and organosilicon resin production, implementing the process described in any one of claims 1-9, characterized in that, The device includes a pretreatment unit, an electric field prepolarization unit, a magnetically stabilized fluidized bed adsorption unit, a pulsed thermal regeneration unit, a condensation and recovery system, a membrane separation and concentration unit, and a control and switching system. The pretreatment unit includes a cyclone separator, a venturi scrubber, and a gas-liquid separator, which are connected in series. The electric field prepolarization unit is connected to the outlet of the pretreatment unit and includes a flat plate high-voltage electric field module, a corona discharge needle array and an insulating dielectric barrier layer. The magnetically stabilized fluidized bed adsorption unit is connected to the outlet of the electric field prepolarization unit and includes a vertical cylindrical adsorption tower, a magnetic composite adsorbent, an external alternating magnetic field coil group, a gas distribution plate, and an internal filter baffle. The pulsed thermal regeneration unit is connected to the magnetically stabilized fluidized bed adsorption unit and includes a high-frequency electrothermal pulse generator, a hot nitrogen circulation pipeline, and a regeneration gas flow regulating valve group. The condensation recovery system is connected to the outlet of the pulse heat regeneration unit and is a two-stage condensation structure. The membrane separation and concentration unit is connected to the top outlet of the magnetically stabilized fluidized bed adsorption unit and includes a hydrophobic composite membrane module, a permeate-side vacuum pump, and a membrane module heating jacket. The control and switching system includes a PLC / DCS automatic control system, multi-parameter online monitoring instruments, and electromagnetic switching valve groups, which are electrically connected to each unit to realize automatic control of the entire process.

Images