Hydrogen peroxide continuous purification method and device with anti-decomposition safety interlock
By combining digital twin models and proactive optimization commands, the pressure field and stabilizer injection parameters are dynamically adjusted, resolving the contradiction between safety and efficiency in the hydrogen peroxide purification process and achieving high-purity and high-efficiency hydrogen peroxide production.
Patent Information
- Application Number
- CN202511889801.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-15
- Publication Date
- 2026-02-27
AI Technical Summary
Existing technologies for hydrogen peroxide purification lack the ability to predict and proactively intervene in early decomposition risks, resulting in insufficient safety margins and a contradiction between safety and efficiency, making it difficult to achieve high-purity and high-efficiency production.
A digital twin model is used to calculate the decomposition potential energy index in real time. Combined with active optimization commands, the pressure field and stabilizer injection parameters are dynamically adjusted. The entire process decomposition suppression and safety interlock control are achieved by generating self-suppressing reflux liquid in situ.
It achieves full-process decomposition inhibition and safety interlock control in the hydrogen peroxide purification process, improving product purity and yield, reducing energy consumption, and ensuring high safety and efficient production.
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Figure CN121573642A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of inorganic compound purification technology, and in particular to a continuous purification method and apparatus for hydrogen peroxide with an anti-decomposition safety interlock. Background Technology
[0002] Hydrogen peroxide, commonly known as hydrogen peroxide solution, is a key inorganic chemical and ultra-pure reagent used as a core cleaning agent and etching agent in high-tech industries such as semiconductor manufacturing, flat panel displays, and solar photovoltaics. These cutting-edge fields have extremely stringent requirements for the purity of hydrogen peroxide, especially the metal ion content, which must be controlled at the part-in-a-trillion level. Therefore, deep purification of industrial-grade hydrogen peroxide is a crucial step in meeting industry demands.
[0003] Among related technologies, Chinese invention patent CN103204476A discloses an optimized production system and method for concentrating a 27.5% dilute hydrogen peroxide solution into a 50% concentrated hydrogen peroxide solution. The system includes: a 27.5% dilute hydrogen peroxide solution pumped with a dilute hydrogen peroxide concentrate and stabilizer; a 50% hydrogen peroxide product pumped with a hydrogen peroxide stabilizer; and a chemical-grade product tank pumped with a hydrogen peroxide stabilizer. The outputs of all these components are transported to the evaporator pipeline. The gas from the top of the distillation column and the gas extracted from the evaporator shell are mixed and then cooled by a tail gas condenser before entering a vacuum pump unit via a gas-liquid mixing separator. A demineralized water acidity adjustment device and an online pH meter monitoring device are added during the process of sending the demineralized water from the demineralized water station to the reflux tank to ensure safe and controllable system production.
[0004] However, the aforementioned existing technical solutions have the following technical defects: Passive safety response: This solution relies on passive monitoring methods such as online pH meter monitoring, only making delayed adjustments after system parameters exceed limits. It lacks the ability to predict and actively intervene in the risk of hydrogen peroxide decomposition, resulting in insufficient safety margin. Lack of whole-process decomposition inhibition: The stabilizer is added by pre-pumping it into the raw material or product, which is a static addition. It cannot dynamically and in-situ neutralize and inhibit the trace decomposition products newly generated during distillation, resulting in insufficient control over the whole-process decomposition reaction. Efficiency versus safety conflict: To ensure safety, process operating conditions tend to be conservative, limiting further improvements in distillation efficiency and making it difficult to achieve optimal energy consumption control and product yield while ensuring high safety. Summary of the Invention
[0005] To address the aforementioned problems, this invention provides a continuous hydrogen peroxide purification method and apparatus with anti-decomposition safety interlock. It employs a digital twin model to calculate the decomposition potential energy index in real time, and combines this with active optimization commands based on the trend of the index's changes to dynamically adjust the pressure field and stabilizer injection parameters, thereby achieving full-process decomposition suppression and safety interlock control in the hydrogen peroxide purification process.
[0006] The above objectives can be achieved through the following approach:
[0007] A method and apparatus for continuous purification of hydrogen peroxide with anti-decomposition safety interlock includes a pressure fine-tuning unit that dynamically adjusts pressure and temperature parameters at multiple points within the distillation column to establish a non-uniform pressure field for continuous reduced-pressure distillation; reacting the column top vapor with a stabilizer precursor in an in-situ capture reactor containing a catalyst to generate an in-situ stabilizer, forming a self-suppressed reflux liquid that is returned to the distillation column; real-time monitoring of system status parameters and calculation of the decomposition potential energy index, and proactive optimization of pressure regulation logic or stabilizer precursor injection parameters based on its changing trends.
[0008] Optionally, the step of calculating and outputting pressure regulation commands for specific locations based on the current process parameter set includes: identifying regions from the current process parameter set whose temperature parameters exceed a preset first threshold and marking them as sensitive regions; predicting the heat load parameters and vaporization rate parameters of the sensitive regions in a future time period based on the location information of the sensitive regions; and generating pressure regulation commands to increase the local pressure in the sensitive regions based on the heat load parameters and the vaporization rate parameters, wherein the pressure regulation commands cause the dynamic non-uniform pressure field to form local pressure peaks in the sensitive regions.
[0009] Optionally, the reaction to generate the in-situ stabilizer includes: conveying the overhead vapor containing the trace decomposition products to the in-situ capture reactor, the inner wall of the in-situ capture reactor being coated with a nano-catalytic coating; converting the stabilizer precursor into stabilizer precursor vapor and quantitatively injecting it into the inlet section of the in-situ capture reactor; controlling the catalytic reaction between the overhead vapor and the stabilizer precursor vapor as they flow through the surface of the nano-catalytic coating to convert the trace decomposition products into a surface-active stabilizer complex, the stabilizer complex constituting the in-situ stabilizer.
[0010] Optionally, the step of forming a self-suppressing reflux liquid and guiding it back into the distillation column includes: condensing and separating the gas-liquid mixture output from the in-situ capture reactor to obtain a condensate enriched with the stabilizer complex; mixing the condensate with the reflux liquid from the distillation column at an adjustable mixing ratio to generate a self-suppressing reflux liquid; and introducing the self-suppressing reflux liquid into the top reflux distributor of the distillation column, so that it preferentially adsorbs onto the metal surface and the gas-liquid interface during its downward flow within the column.
[0011] Optionally, the reaction efficiency parameters of the in-situ capture reactor include: monitoring the concentration difference of specific reactive oxygen species in the inlet and outlet gas flow of the in-situ capture reactor and calculating the reactive oxygen conversion rate; analyzing the concentration of the in-situ stabilizer in the self-suppressing reflux liquid and obtaining the stabilizer generation concentration; and weighting the reactive oxygen conversion rate and the stabilizer generation concentration to generate the reaction efficiency parameters.
[0012] Optionally, the calculation of the decomposition potential energy index characterizing the overall stability of the system includes: calculating the distance between the current operating point and the theoretical thermal decomposition boundary based on the system state parameter set, generating a real-time distance parameter; acquiring feed impurity information, system operating history, and surface state history parameters; estimating the distribution state of catalytically active impurities in the tower based on the feed impurity information and system operating history, generating a catalytic pressure parameter; and fusing the real-time distance parameter, the catalytic pressure parameter, and the surface state history parameters to calculate the decomposition potential energy index characterizing the overall stability of the system.
[0013] Optionally, generating and executing active optimization instructions based on the changing trend of the decomposition potential energy index includes: determining whether the decomposition potential energy index shows a continuous upward trend and its value is lower than a preset safety threshold; if so, then activating the active optimization mode and generating a first type of active optimization instruction for fine-tuning the amplitude or position of the pressure peak in the dynamic non-uniform pressure field; simultaneously, generating a second type of active optimization instruction for adjusting the injection rate or concentration of the stabilizer precursor.
[0014] Optionally, after activating the active optimization mode, the method further includes: dynamically adjusting the weighting factor used to calculate the catalytic pressure parameter based on the rate of change of the decomposed potential energy index; recalculating the updated decomposed potential energy index based on the adjusted weighting factor; and performing closed-loop correction on the first type of active optimization instruction and the second type of active optimization instruction according to the updated decomposed potential energy index.
[0015] Optionally, the step of continuously reducing pressure to distill the input hydrogen peroxide feedstock under the dynamic non-uniform pressure field to obtain overhead vapor and preliminary purified liquid includes: filtering and preheating the hydrogen peroxide feedstock to obtain purified hydrogen peroxide feedstock liquid; introducing the purified hydrogen peroxide feedstock liquid into the middle of the distillation column, and performing multi-stage equilibrium flash evaporation and mass and heat transfer under the dynamic non-uniform pressure field to separate the overhead vapor and preliminary purified liquid.
[0016] Based on the same inventive concept, this invention also provides a continuous hydrogen peroxide purification device with anti-decomposition safety interlock. The device includes: a parameter acquisition module for acquiring pressure and temperature parameters at multiple locations distributed along the height of the distillation column, generating a current process parameter set; a pressure control module for calculating and outputting pressure adjustment commands for specific locations based on the current process parameter set; a dynamic pressure field establishment module for adjusting multiple pressure fine-tuning units located at corresponding positions in the distillation column in response to the pressure adjustment commands, establishing a dynamic non-uniform pressure field; a continuous vacuum distillation module for continuously vacuum distilling the input hydrogen peroxide feedstock under the dynamic non-uniform pressure field environment to obtain column top vapor and preliminary purified liquid; and an in-situ capture reaction module for reacting the column top vapor with trace amounts of... The stabilizer precursor from the decomposition product reaction is introduced into a pre-designed in-situ capture reactor containing a catalyst to react and generate an in-situ stabilizer. A reflux self-inhibition module is used to mix the in-situ stabilizer with the condensed reflux liquid to form a self-inhibited reflux liquid and guide it back into the distillation column. A monitoring module is used to monitor and acquire a system state parameter set in real time. The system state parameter set includes at least the updated data of the current process parameter set and the reaction efficiency parameters from the in-situ capture reactor. A decomposition calculation module is used to calculate the decomposition potential energy index, which characterizes the overall stability of the system, based on the system state parameter set. An active optimization execution module is used to generate and execute active optimization instructions based on the changing trend of the decomposition potential energy index. The active optimization instructions are used to adjust the generation logic of the pressure regulation instruction or adjust the injection parameters of the stabilizer precursor.
[0017] Compared with the prior art, the present invention has the following advantages:
[0018] This invention fundamentally improves the inherent safety of the continuous hydrogen peroxide purification process by constructing a closed-loop adaptive control system that deeply integrates physical inhibition, chemical self-healing, and intelligent prediction. It abandons the traditional passive monitoring and delayed response mode, actively suppressing decomposition initiation through a dynamic pressure field and continuously repairing weak links in the system using in-situ generated self-suppressing reflux liquid. This achieves source prevention and process suppression of decomposition risks, with a safety level far exceeding existing technologies.
[0019] This invention successfully resolves the technical contradiction between safety and production efficiency in traditional processes, achieving synergistic improvement between the two. Based on the high safety margin provided by predictive safety interlocks, the system can operate stably under process conditions closer to the theoretical optimal point. This not only avoids energy waste caused by conservative operation but also increases the product throughput per unit time, resulting in significant optimization of purification efficiency and energy utilization.
[0020] This invention enables the stable production of higher quality ultrapure products and improves feedstock yield. Under a safe, efficient, and stable continuous operating environment, the mass and heat transfer during the distillation process is more complete and balanced, resulting in more thorough impurity separation. This ensures that the final product achieves and maintains a consistently ultra-high purity level with trace metal ions. Simultaneously, the effective suppression of decomposition reactions minimizes the ineffective loss of hydrogen peroxide in the feedstock, further improving product yield.
[0021] Other features and advantages of the invention will be set forth in the description which follows, and will be apparent in part from the description, or may be learned by practicing the invention. The objects and other advantages of the invention may be realized and obtained by means of the structures pointed out in the description, claims and drawings. Attached Figure Description
[0022] To more clearly illustrate the technical solutions in the embodiments of the present invention or 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 some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0023] Figure 1 This is a schematic flowchart of a continuous hydrogen peroxide purification method with anti-decomposition safety interlock according to an embodiment of the present invention.
[0024] Figure 2 This is a correlation matrix diagram of the efficiency parameters of the in-situ capture reactor in an embodiment of the present invention.
[0025] Figure 3 This is a diagram showing the overall system stability parameters according to an embodiment of the present invention.
[0026] Figure 4 This is a schematic diagram of the structure of a continuous hydrogen peroxide purification device with anti-decomposition safety interlock according to an embodiment of the present invention. Detailed Implementation
[0027] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0028] Reference Figure 1One embodiment of the present invention proposes a continuous hydrogen peroxide purification method with anti-decomposition safety interlock. It uses a digital twin model to calculate the decomposition potential energy index in real time, and combines it with active optimization instructions based on the changing trend of the index to dynamically adjust the pressure field and stabilizer injection parameters, thereby realizing full-process decomposition suppression and safety interlock control of the hydrogen peroxide purification process.
[0029] The method described in this embodiment specifically includes:
[0030] S1. Obtain pressure and temperature parameters at multiple locations along the height of the distillation column to generate the current process parameter set;
[0031] Specifically, suitable sensors need to be installed at multiple specific locations along the height of the distillation column. These sensors include: pressure sensors: used to monitor and acquire pressure parameters at the corresponding locations in real time. High-precision, corrosion-resistant pressure sensors suitable for the reduced-pressure distillation environment should be selected. Temperature sensors, such as thermocouples or resistance temperature detectors (RTDs): used to monitor and acquire temperature parameters at the corresponding locations in real time. Temperature sensors need to have fast response and high accuracy to accurately reflect the temperature distribution within the column. These sensors are arranged in an array along the axial direction (height) inside the distillation column, covering the key area from the bottom to the top of the column to capture the gradient distribution of pressure and temperature parameters. The pressure and temperature parameters acquired by the sensors are used as raw data and are received in real time by the parameter acquisition module through a data acquisition system. The parameter acquisition module then performs data processing on these real-time acquired multi-location pressure and temperature parameters, including but not limited to: data calibration and denoising: eliminating errors caused by sensor drift and environmental interference; timestamp synchronization: ensuring that all acquired pressure and temperature parameters belong to the same process state at the same moment; and data integration: integrating the pressure and temperature parameters from different locations into a structured dataset. Finally, the parameter acquisition module outputs the integrated set of pressure and temperature parameters, which possess time-sensitive and spatial distribution characteristics, as the current process parameter set for subsequent pressure control and system status assessment. The current process parameter set characterizes the operating conditions and thermodynamic state of the distillation column at the current moment.
[0032] S2. Based on the current set of process parameters, calculate and output pressure adjustment commands for certain locations;
[0033] Optionally, calculating and outputting pressure adjustment commands for specific locations based on the current set of process parameters includes:
[0034] Regions whose temperature parameters exceed a preset first threshold are identified from the current process parameter set and marked as sensitive regions.
[0035] Based on the location information of the sensitive area, predict the heat load parameters and vaporization rate parameters of the sensitive area in the future time period;
[0036] Based on the heat load parameters and the vaporization rate parameters, a pressure regulation command is generated to increase the local pressure in the sensitive area. The pressure regulation command causes the dynamic non-uniform pressure field to form a local pressure peak in the sensitive area.
[0037] Specifically, the pressure control module extracts temperature parameters from multiple locations distributed along the column height from the current process parameter set provided by the parameter acquisition module. Then, the temperature parameters at each location are... With the preset first threshold Comparison. First threshold. It is set based on empirical values of the safe decomposition temperature of hydrogen peroxide within the operating pressure range of the distillation column. For example, it can be set to a temperature value that is higher than the target operating temperature by a certain safety margin. If a certain position Temperature parameters satisfy Then the area It is marked as a sensitive area.
[0038] Predicting Heat Load and Vaporization Rate: Once a sensitive area is identified, the pressure control module uses the location information of the sensitive area, along with the real-time temperature and pressure parameters of that area from the current process parameter set, combined with the design parameters of the distillation column, such as tray type, column diameter, heat exchange area, and the thermodynamic properties of the material, to predict the sensitive area in the future. Internal heat load parameters With vaporization rate parameter Heat load parameters : Indicates the sensitive area is The potential heat accumulation or heating power that the area can withstand can be calculated using an energy balance model, for example, based on the flow rate and temperature difference of the heating medium, or estimated according to the heat transfer coefficient and temperature difference of the region. Vaporization rate parameter. This represents the vaporization rate of hydrogen peroxide within the sensitive area. Its value is related to local temperature, pressure, and heat load, and can be obtained by simultaneously solving material balance and mass and heat transfer equations. Higher values indicate higher vaporization rates. and This indicates a higher risk of decomposition.
[0039] Generate pressure regulation command: The pressure regulation module generates the command based on the heat load parameters. With the vaporization rate parameter Calculate the required local pressure increment This generates a pressure regulation command to increase the local pressure in the sensitive area. The goal of this command is to adjust the local pressure in the sensitive area by regulating the pressure fine-tuning unit. achieve ,in This refers to the pressure parameters within the current process parameter set for the sensitive area. Localized pressure increase. It must be sufficient to reduce the boiling point of hydrogen peroxide in this sensitive region. Increase to This suppresses its violent vaporization and decomposition. The pressure regulation command ensures that the dynamically non-uniform pressure field forms localized pressure peaks in the sensitive area. This command is then output to the dynamic pressure field establishment module.
[0040] For example, suppose a distillation column for high-concentration hydrogen peroxide distillation is operating stably, and the current process parameter set obtained by the parameter acquisition module displays a certain tray in the column. Temperature parameters at the location Suddenly rise to The preset first threshold Set as .because The pressure control module marks this area as a sensitive zone. Based on this location information, the pressure control module predicts the following... Within seconds, the heat load parameters of this area Expected to be vaporization rate parameter Expected to be The pressure control module calculates the pressure based on the material characteristics in order to... The boiling point of hydrogen peroxide increases at this time To effectively suppress vaporization, local pressure needs to be increased at this location. Therefore, the pressure regulation module generates pressure to increase the local pressure in the sensitive area. The system receives and outputs pressure regulation commands to the dynamic pressure field establishment module. Upon receiving the commands, the dynamic pressure field establishment module drives the tray... The pressure fine-tuning unit at that location activates, rapidly establishing a local pressure peak higher than the surrounding area, creating a dynamic, non-uniform pressure field, thereby raising the boiling point of the sensitive region to [a higher value]. This ensures the safety and stability of the distillation process.
[0041] S3. In response to the pressure regulation command, adjust multiple pressure fine-tuning units set at the corresponding positions of the distillation column to establish a dynamic non-uniform pressure field;
[0042] Specifically, multiple pressure fine-tuning units need to be pre-installed at several specific locations along the height of the distillation column. These pressure fine-tuning units are actuators used to precisely control the local pressure at their respective locations based on received instructions. They can take the form of high-precision, fast-response micro pneumatic or electric regulating valves, or local gas / vapor injection / suction devices, to achieve real-time, localized, and precise adjustment of pressure parameters in specific areas within the column. The operation process is as follows: Receiving Instructions: The dynamic pressure field establishment module receives pressure regulation instructions output from the pressure control module in real time. Instruction Parsing: The pressure regulation instructions are parsed to determine the corresponding location of the distillation column to be adjusted, i.e., the location of the sensitive area, and the target pressure parameter change, i.e., the amplitude used to increase the local pressure in the sensitive area. Driving Execution: The dynamic pressure field establishment module sends drive signals to the pressure fine-tuning units located at the corresponding positions in the distillation column. For example, if the pressure regulation instruction requires increasing the local pressure in a certain sensitive area, the pressure fine-tuning unit at that location is driven to adjust, possibly by reducing the local vacuum force or injecting a small amount of inert gas, thereby increasing the pressure parameter at that location. Establishing a dynamic non-uniform pressure field: By coordinating and adjusting some or all pressure fine-tuning units in real time, a field with non-uniform pressure parameter distribution is established along the column height of the distillation column. This field is not fixed but changes in real time according to pressure regulation commands, hence the name dynamic non-uniform pressure field. Within the identified sensitive area, after the pressure fine-tuning units are adjusted, the dynamic non-uniform pressure field will form a local pressure peak, making the pressure in that area higher than the surrounding area. Continuous maintenance and updating: Since the current process parameter set is updated in real time, and pressure regulation commands are constantly generated and corrected based on new data, the dynamic pressure field establishment module needs to continuously respond to the pressure regulation commands, constantly adjusting multiple pressure fine-tuning units to maintain or correct the distribution of the dynamic non-uniform pressure field and the amplitude and position of the pressure peak, thereby achieving real-time, dynamic, and safe control of the distillation column operating conditions.
[0043] S4. Under the dynamic non-uniform pressure field, the input hydrogen peroxide feedstock is subjected to continuous vacuum distillation to obtain overhead vapor and preliminary purified liquid.
[0044] Optionally, the continuous vacuum distillation of the input hydrogen peroxide feedstock under the dynamic non-uniform pressure field to obtain overhead vapor and preliminary purified liquid includes:
[0045] The hydrogen peroxide raw material is filtered and preheated to obtain a purified hydrogen peroxide raw material liquid;
[0046] The purified hydrogen peroxide feedstock is introduced into the middle of the distillation column, where it undergoes multi-stage equilibrium flash evaporation and mass and heat transfer under a dynamic non-uniform pressure field to separate the column top vapor and the preliminary purified liquid.
[0047] Specifically, the input hydrogen peroxide feedstock undergoes filtration and preheating to obtain a purified hydrogen peroxide feedstock solution. The filtration process employs a high-precision microporous membrane filtration device to remove solid impurities and catalytically active particles from the feedstock solution that could potentially lead to decomposition, reducing the risk of decomposition at the source. The preheating process involves heating the filtered feedstock solution to near the feed temperature of the distillation column to ensure stable thermal balance and prevent large fluctuations in the temperature field within the column caused by the feed.
[0048] The pretreated and purified hydrogen peroxide feedstock is introduced into the middle of the distillation column. The feed location is usually determined based on material balance calculations to ensure optimal separation efficiency. Mass and heat transfer separation: Inside the distillation column, the material undergoes multi-stage equilibrium flash evaporation and mass and heat transfer under a dynamic non-uniform pressure field. The dynamic non-uniform pressure field is established in real time by a dynamic pressure field establishment module through multiple pressure fine-tuning units. Its function is to form local pressure peaks in potential hot spots, physically inhibiting decomposition. Multi-stage equilibrium flash evaporation refers to the multiple vaporization and condensation of the material as it passes through the trays or packing layer due to pressure reduction and heat transfer, with the gas and liquid phases approaching thermodynamic equilibrium at each stage. Mass and heat transfer is the core process of distillation; components of hydrogen peroxide and water exchange between the gas and liquid phases, achieving high-purity separation. Product separation: After multi-stage equilibrium flash evaporation and mass and heat transfer, high-purity hydrogen peroxide vapor and water vapor rise along the column and are eventually separated to obtain the top vapor. The bottom of the column collects the preliminary purified liquid, which is usually a high-concentration hydrogen peroxide product.
[0049] For example, assume a continuous purification process is performed on a 60% concentration hydrogen peroxide feedstock. Pretreatment: First, the 60% concentration hydrogen peroxide feedstock is passed through a 0.2... A polytetrafluoroethylene (PTFE) membrane is used for filtration to remove catalytic metal particles. Subsequently, the feed solution is preheated to... The purified hydrogen peroxide feedstock is obtained. Distillation: The purified hydrogen peroxide feedstock is introduced into the tenth tray in the middle of the distillation column. Dynamic operation: Inside the distillation column, a dynamic pressure field module maintains the reboiler pressure at 15 kPa and sets a local pressure peak of 20 kPa on the ninth tray, forming a dynamic non-uniform pressure field environment. During the downward flow and vaporization process within the column, the feedstock undergoes efficient multi-stage equilibrium flash evaporation and mass and heat transfer. After the overhead condenser, a condensate of 90% concentrated overhead vapor is collected, while a pre-purified liquid with a concentration of 70% flows out from the reboiler side. This process ensures that the risk of localized thermal decomposition during separation is always physically suppressed by the dynamic non-uniform pressure field.
[0050] S5. The overhead steam and a stabilizer precursor that can react with trace decomposition products in the overhead steam are introduced into a pre-set in-situ capture reactor containing a catalyst to react and generate an in-situ stabilizer.
[0051] Optionally, the reaction to generate the in-situ stabilizer includes:
[0052] The overhead steam containing the trace decomposition products is fed to the in-situ capture reactor, the inner wall of which is coated with a nano-catalytic coating.
[0053] The stabilizer precursor is converted into stabilizer precursor vapor and quantitatively injected into the inlet section of the in-situ capture reactor.
[0054] The vapor at the top of the column and the vapor of the stabilizer precursor are controlled to undergo a catalytic reaction as they flow over the surface of the nano-catalytic coating, converting the trace decomposition products into surface-active stabilizer complexes, which constitute in-situ stabilizers.
[0055] Specifically, the overhead vapor generated by the continuous vacuum distillation module, containing trace decomposition products such as oxygen, water vapor, and low-molecular-weight organic acid vapors, is received by the in-situ capture reaction module. The overhead vapor is then fed to the in-situ capture reactor. The in-situ capture reactor is a specialized reaction device whose inner wall is pre-coated with a nano-catalytic coating. This nano-catalytic coating is a highly efficient heterogeneous catalyst used to promote the reaction between trace decomposition products and stabilizer precursors; its composition typically includes noble metal oxides or complex metal compounds, which possess high specific surface area and selective catalytic activity.
[0056] Pre-prepared stabilizer precursors, such as organophosphonic acid compounds and specific organic amines, can vaporize at high temperatures and react with decomposition products to generate effective stabilizers. Their flow rate is precisely controlled by a metering pump, and they are heated or depressurized to convert them into stabilizer precursor vapor. This stabilizer precursor vapor is then metered into the inlet section of the in-situ capture reactor, ensuring thorough mixing with the incoming overhead vapor.
[0057] Within the in-situ capture reactor, a heterogeneous catalytic reaction occurs as the mixture of overhead vapor and stabilizer precursor vapor flows across the surface of a nano-catalytic coating. The nano-catalytic coating provides highly active reaction sites, accelerating the chemical transformation between trace decomposition products, such as free radicals or reactive oxygen species, and the stabilizer precursor vapor, converting these products into surface-active stabilizer complexes. For example, reactive oxygen species may react with organophosphonic acids to generate stabilizer complexes with better passivation capabilities. These stabilizer complexes constitute the in-situ stabilizer. The resulting gas-liquid mixture containing the in-situ stabilizer is then exited from the outlet of the in-situ capture reactor, ready to enter the subsequent reflux self-inhibition module for condensation and reflux.
[0058] For example, suppose that a distillation column generates trace amounts of oxygen and water vapor, as well as trace amounts of reactive oxygen species as minor decomposition products, during continuous distillation. An in-situ capture reaction module introduces these overhead vapors into an in-situ capture reactor. The inner wall of the in-situ capture reactor is coated with... Nano-catalytic coating. Simultaneously, diethylenetriaminepentamethylenephosphonic acid is used as a stabilizer precursor, which is heated to convert it into stabilizer precursor vapor and quantitatively injected into the inlet section of the in-situ capture reactor. Under the catalytic action of the nano-catalytic coating, diethylenetriaminepentamethylenephosphonic acid in the stabilizer precursor vapor reacts with reactive oxygen free radicals in trace decomposition products to generate phosphonic acid complexes with stronger metal passivation capabilities. For example, this reaction may involve the oxidization or complexation of the hydroxyl or amino groups of diethylenetriaminepentamethylenephosphonic acid by reactive oxygen species, forming new and more stable stabilizer complexes. These complexes constitute in-situ stabilizers and are ultimately output with the gas flow. This process achieves in-situ capture and conversion of harmful trace decomposition products into beneficial stabilizers, completing the in-situ stabilizer generation step.
[0059] S6. Mix the in-situ stabilizer with the refluxed liquid to form a self-suppressing reflux liquid and guide it back into the distillation column;
[0060] Optionally, the process of forming a self-suppressing reflux liquid and guiding it back into the distillation column includes:
[0061] The gas-liquid mixture output from the in-situ capture reactor is condensed and separated to obtain a condensate enriched with the stabilizer complex.
[0062] The condensate is mixed with the reflux condensate from the distillation column at an adjustable mixing ratio to generate a self-suppressing reflux liquid;
[0063] The self-suppressing reflux liquid is introduced into the top reflux distributor of the distillation column, so that it is preferentially adsorbed on the metal surface and gas-liquid interface during the downward flow process in the column.
[0064] Specifically, the gas-liquid mixture containing the in-situ stabilizer, i.e., the stabilizer complex, output from the in-situ capture reactor of the in-situ capture reaction module is conveyed to a condenser for cooling. In the condenser, the gaseous substance is cooled below the dew point and subjected to condensation separation. The condensed liquid then enters a gas-liquid separator to obtain a condensate enriched with the stabilizer complex. Uncondensed gases, such as inert gases and small amounts of unreacted products, are discharged through a vacuum system to ensure stable pressure in the distillation column.
[0065] The resulting condensate enriched with the stabilizer complex is combined with the reflux condensate from the distillation column, specifically a portion of the hydrogen peroxide and aqueous solution condensed from the top condenser of the distillation column. A high-precision metering pump and flow controller are used to achieve an adjustable mixing ratio. Mix to generate a self-suppressing reflux solution. Adjustable mixing ratio. It can be dynamically adjusted based on the reaction efficiency parameters and decomposition risk status within the distillation column obtained in real time by the monitoring module. If... This is the condensate flow rate. The mixing ratio is the reflux condensate flow rate. The mixing ratio can be adjusted by changing the flow rate of any one of the fluids.
[0066] The self-suppressing reflux module introduces the generated self-suppressing reflux liquid into the top reflux distributor of the distillation column via a reflux pump. This top reflux distributor ensures that the liquid is evenly distributed on the trays. As the self-suppressing reflux liquid flows down the column, the surface activity and metal complexing ability of the stabilizer complex itself cause it to preferentially adsorb onto the metal surface and the gas-liquid interface. This preferential adsorption forms a protective film on the inner wall of the column and the surface of the packing, effectively passivating potential catalytic active sites.
[0067] For example, suppose that the concentration of the in-situ stabilizer, i.e., the phosphonic acid complex, in the condensate enriched with the stabilizer complex output from the in-situ capture reactor reaches... The concentration of the in-situ stabilizer in the conventional reflux liquid at the top of the distillation column is considered... The reflux self-suppression module sets an adjustable mixing ratio of 1:9 based on the decomposition risk monitored by the system. A portion of condensate and Mix the reflux condensate. Assume the reflux condensate flow rate is... The reflux condensate flow rate Based on material balance calculations, the final concentration of the in-situ stabilizer in the self-suppressing reflux liquid is: The reflux self-suppression module will ultimately reduce the concentration to [value missing]. The self-suppressing reflux liquid of the in-situ stabilizer is introduced into the distillation column through the top reflux distributor. As the liquid flows downward in the column, the stabilizer complex it contains preferentially covers and passivates the surfaces of all metal equipment and gas-liquid contact interfaces in the column, effectively reducing potential decomposition catalytic activity and enhancing the inherent safety of the system.
[0068] S7. Monitor and acquire the system status parameter set in real time. The system status parameter set includes at least the updated data of the current process parameter set and the reaction efficiency parameters from the in-situ capture reactor.
[0069] Optionally, the reaction efficiency parameters of the in-situ capture reactor include:
[0070] The concentration difference of specific reactive oxygen species in the in-situ capture reactor gas flow is monitored, and the reactive oxygen conversion rate is calculated.
[0071] The concentration of the in-situ stabilizer in the self-suppressing reflux liquid was analyzed to obtain the stabilizer formation concentration;
[0072] The reaction efficiency parameter is generated by weighting the reactive oxygen species conversion rate with the stabilizer generation concentration.
[0073] Specifically, the correlation matrix of efficiency parameters of the in-situ capture reactor is as follows: Figure 2 As shown, high-sensitivity online gas analyzers are installed in the inlet and outlet gas streams of the in-situ capture reactor to monitor the concentration of specific reactive oxygen species in the inlet and outlet gas streams in real time. Specific reactive oxygen species refer to key gaseous products or reactive intermediates produced by the decomposition of hydrogen peroxide. The monitoring module acquires the inlet concentration in real time. and export concentration The reactive oxygen species conversion rate was calculated using the following formula. :
[0074] ,
[0075] in, It is the concentration of a specific reactive oxygen species at the inlet of the in-situ capture reactor, and its value is measured by the inlet gas analyzer; It is the concentration of a specific reactive oxygen species at the outlet of the in-situ capture reactor, and its value is measured by the outlet gas analyzer. The efficiency of the in-situ capture and conversion of trace decomposition products by the reactor was characterized.
[0076] Continuous or periodic samples are extracted from the self-suppressed reflux liquid generated by the reflux self-suppression module. Using high-precision chemical analysis instruments, such as high-performance liquid chromatography (HPLC) or ion chromatography (IGC), the chemical composition of the target in-situ stabilizer (i.e., stabilizer complex) in the samples is quantitatively analyzed to obtain the concentration of the in-situ stabilizer. This concentration value is used as the stabilizer concentration. . It directly reflects the yield of the in-situ capture reactor in converting trace decomposition products into effective in-situ stabilizers.
[0077] The monitoring module will calculate the reactive oxygen species conversion rate. Concentration generated with stabilizer Weighted combinations are performed to generate reaction efficiency parameters. Reaction efficiency parameters The calculation formula is as follows:
[0078] ,
[0079] in, and It is a preset weighting factor, the value of which is determined based on the relative importance of reactive oxygen species conversion rate and stabilizer generation concentration in assessing system safety and decomposition inhibition capability. and All are dimensionless constants, which can be adjusted by... and The proportional relationship ensures that the two terms added in the formula have the same dimensions. For example, it can be expressed as follows: After normalization, ; It is the reactive oxygen species conversion rate calculated in step one; This is the concentration of stabilizer generated obtained from step two analysis. As a comprehensive indicator, it characterizes the effect of the in-situ capture reaction module on reducing and suppressing the risk of decomposition.
[0080] For example, suppose that during a certain monitoring period: the concentration of a specific reactive oxygen species at the inlet of the in-situ capture reactor. Concentration at the outlet Reactive oxygen species conversion rate The calculation is as follows: The concentration of stabilizer generated in situ in the refluxed inhibitor solution Analysis as Preset weighting factors This is used to measure the importance of conversion rate; This is used to measure the importance of the concentration of the product. To ensure dimensional consistency, It needs to be normalized to a dimensionless parameter Assuming the target concentration is... ,but Reaction efficiency parameters The calculation is as follows: ,this This is the reaction efficiency parameter of the in-situ capture reactor at that moment.
[0081] S8. Based on the system state parameter set, calculate the decomposed potential energy index that characterizes the overall stability of the system;
[0082] Optionally, the calculated decomposed potential energy index characterizing the overall stability of the system includes:
[0083] Based on the system state parameter set, the distance between the current operating point and the theoretical thermal decomposition boundary is calculated, and real-time distance parameters are generated.
[0084] Acquire information on feed impurities, system operation history, and historical surface condition parameters;
[0085] Based on the feed impurity information and system operation history, the distribution of catalytically active impurities in the tower is calculated, and catalytic pressure parameters are generated.
[0086] By integrating the real-time distance parameter, the catalytic pressure parameter, and the surface state history parameter, the decomposition potential energy index characterizing the overall stability of the system is calculated.
[0087] Specifically, the decomposition and calculation module extracts the updated current process parameter set, i.e., the pressure parameters at multiple locations within the distillation column, from the system state parameter set. and temperature parameters The decomposition calculation module, based on the system state parameter set, uses a pre-established hydrogen peroxide thermal decomposition kinetic and thermodynamic model to calculate the distance between the current operating point and the theoretical thermal decomposition boundary, generating real-time distance parameters. The theoretical thermal decomposition boundary refers to the critical temperature-pressure combination curve at the current concentration where the thermal decomposition rate of hydrogen peroxide increases sharply. Real-time distance parameters. The safety margin between the operating point and the danger boundary was quantified. Distance It can be defined as:
[0088] ,
[0089] in, It is the highest temperature in the current set of process parameters, i.e., the most dangerous temperature, and its value is obtained through the parameter acquisition module. Is Corresponding pressure The critical decomposition temperature, obtained by solving the thermal decomposition kinetic equation, is calculated using a pre-defined model. It is a dimensionless parameter; the larger its value, the farther away from the decomposition boundary, and the safer the system.
[0090] The decomposition and calculation module obtains feed impurity information. Information on catalysts, such as heavy metal ions and organic matter, can be obtained through online or offline analysis. The decomposition calculation module acquires the system's operating history. Examples include cumulative running time and duration of abnormal operating conditions. The decomposition calculation module obtains historical surface state parameters. Such as the history of cleaning or passivation of the tower's inner wall and packing, and the estimation of the degree of corrosion.
[0091] The decomposition and calculation module is based on the feed impurity information. and system running history By combining material balance and impurity migration models, the distribution of catalytically active impurities within the column, i.e., the catalyst concentration at different locations, is calculated. Based on the calculated impurity distribution and the catalytic effect of impurities on the hydrogen peroxide decomposition rate, the decomposition calculation module generates catalytic pressure parameters. . It is a dimensionless parameter that quantifies the risk of catalytic decomposition, for example, it can be defined as:
[0092] ,
[0093] in, It is the total concentration of catalytically active impurities calculated from the sensitive area. It can be calculated using material balance models and online analyzer data; It is the catalytic decomposition rate constant of impurities, and its value is determined experimentally. The higher the value, the greater the risk of catalytic decomposition.
[0094] The decomposition and calculation module integrates the real-time distance parameters. and the catalytic pressure parameters and the surface state history parameters The decomposition potential energy index characterizing the overall stability of the system was calculated. Decomposition of potential energy index It is a comprehensive, inverse indicator; the higher the value, the more unstable the system and the greater the risk of decomposition. Its calculation formula can be expressed as:
[0095] ,
[0096] in, This is a preset weighting factor, the value of which is determined through system security assessment, used to balance the importance of different risk sources. In the calculation, all parameters must be normalized to ensure that the dimensions of the added items in the formula are consistent, such as all being dimensionless parameters. The overall system stability parameters comprehensively reflect the sum of thermodynamic safety margin, chemical catalytic risk, and equipment condition risk, such as... Figure 3 As shown.
[0097] For example, suppose the decomposition calculation module performs calculations at a certain moment: real-time distance parameters The highest operating temperature inside the tower Critical decomposition temperature under corresponding pressure The real-time distance parameters were calculated. Catalytic pressure parameters Based on feed impurity information and system operating history, the total concentration of catalytically active impurities in the sensitive area is estimated. catalytic decomposition rate constant Catalytic pressure parameters The value is Surface condition history parameters The surface passivation inside the tower was recently completed and is in good condition. Historical surface condition parameters are available. Normalized value Fusion calculation decomposes the potential energy index. Preset weighting factor . The normalized value is Decomposition of potential energy index The calculation is as follows: At this point, the decomposition potential energy index If the preset security threshold is If the system is in a relatively safe state, then vigilance is still necessary.
[0098] S9. Based on the changing trend of the decomposed potential energy index, generate and execute an active optimization instruction, which is used to adjust the generation logic of the pressure regulation instruction or adjust the injection parameters of the stabilizer precursor.
[0099] Optionally, generating and executing active optimization instructions based on the changing trend of the decomposed potential energy exponent includes:
[0100] Determine whether the decomposition potential energy index shows a continuous upward trend and whether its value is lower than a preset safety threshold.
[0101] If so, the active optimization mode is activated to generate a first type of active optimization instruction for fine-tuning the amplitude or position of the pressure peak in the dynamic non-uniform pressure field.
[0102] Simultaneously, a second type of active optimization instruction is generated to adjust the injection rate or concentration of the stabilizer precursor.
[0103] Specifically, the proactive optimization execution module continuously receives and analyzes the decomposition potential energy index output by the decomposition calculation module. The sequence. The module first determines the decomposed potential energy index. Whether it shows a continuous upward trend is usually determined by calculation. The average rate of change over a recent period has been achieved. Subsequently, the module makes a judgment. Is the value lower than the preset safety threshold? Safety threshold It is a critical value that is predetermined by the system security assessment.
[0104] Activating optimization mode and command generation: If decomposing the potential energy index The condition of a continuous upward trend is met, and its value is lower than the preset safety threshold. If the system then activates the active optimization mode, the active optimization execution module simultaneously generates two types of instructions: The first type of active optimization instruction generates instructions for fine-tuning the amplitude or position of pressure peaks in the dynamic non-uniform pressure field. The goal of this instruction is physical intervention, enhancing the suppression of local thermal decomposition risks through refined adjustments to the dynamic non-uniform pressure field. For example, if the increase in the decomposition potential energy index is mainly caused by a decrease in the thermodynamic safety margin, then the amplitude of the pressure peak is increased. This allows for a more effective increase in the local boiling point. The instruction is then sent to the dynamic pressure field establishment module for execution.
[0105] Simultaneously, a second type of active optimization instruction is generated to adjust the injection parameters of the stabilizer precursor. This instruction aims at chemical inhibition by fine-tuning the injection flow rate or concentration of the stabilizer precursor to alter the formation rate of the in-situ stabilizer, thereby enhancing the passivation effect on the catalytic active site. This instruction is then sent to the in-situ capture reaction module and the reflux self-inhibition module for execution. This active optimization execution module achieves closed-loop feedback control of decomposition risk, ensuring the continuous and stable operation of the distillation process through dual coordinated fine-tuning before the risk becomes critical.
[0106] For example, assume that the decomposition potential energy index output by the decomposition calculation module is... in the past A continuous increase within a monitoring period, from Rise to The preset safety threshold Set as Trend Judgment: Decomposing the Potential Energy Index It shows a continuous upward trend. Safety assessment: Below Conclusion: Active optimization mode is triggered. Analysis of the active optimization execution module indicates that this upward trend is mainly due to the catalytic pressure parameter. The slight increase indicates that catalytic activity is accumulating within the column. A first type of active optimization instruction is generated: In response to slight fluctuations in the overall thermodynamics of the system, the module generates an instruction to fine-tune the amplitude of the pressure peak in the dynamic non-uniform pressure field: slightly increasing the amplitude of the current pressure peak based on the original instruction. This instruction is executed by the dynamic pressure field establishment module. A second type of active optimization instruction is generated: in response to an increase in the catalytic pressure parameter, the module generates an instruction to adjust the injection parameters of the stabilizer precursor: increasing the mass flow rate of the stabilizer precursor. This instruction is executed by the in-situ capture reaction module and the reflux self-inhibition module. By simultaneously executing these two types of active optimization instructions, the system actively optimizes its operating conditions through coordinated fine-tuning of physical and chemical means before potential risks materialize, reversing the upward trend of the decomposition potential energy index and keeping the system within a safe and stable range, thus achieving a closed-loop safety interlock for decomposition risks.
[0107] Optionally, after activating the active optimization mode, the method further includes:
[0108] The weighting factor used to calculate the catalytic pressure parameter is dynamically adjusted based on the rate of change of the decomposition potential energy index.
[0109] Based on the adjusted weighting factors, the updated decomposed potential energy index is recalculated.
[0110] Based on the updated decomposed potential energy index, the first type of active optimization instruction and the second type of active optimization instruction are corrected in a closed loop.
[0111] Specifically, the proactive optimization execution module continuously monitors the decomposition potential energy index output by the decomposition calculation module. The core task of this module is to determine... Does the value reach or exceed the preset safety threshold? Safety threshold It is the critical red line for the safe operation of the system, for example .like If this occurs, the emergency safety interlock mechanism will be triggered immediately.
[0112] The active optimization execution module generates an emergency pressure command to significantly increase the amplitude or location of pressure peaks in the dynamic non-uniform pressure field. The goal of this command is to rapidly establish a large local pressure peak in the sensitive area or globally. This pressure regulation is far more aggressive than the fine-tuning of the active optimization mode, aiming to immediately increase the boiling point of hydrogen peroxide in that region, thereby instantly suppressing violent vaporization and thermal decomposition reactions. This command is then sent to the dynamic pressure field establishment module for execution.
[0113] Simultaneously, an emergency stabilizer injection command is generated to initiate the emergency injection mode. This command instructs the in-situ capture reaction module and the reflux self-inhibition module to immediately inject stabilizer precursors or additional inert diluents into the distillation column at the maximum safe flow rate or the preset maximum concentration. This maximizes the generation and reflux of the in-situ stabilizer in the shortest possible time, or directly dilutes the active material in the distillation column, rapidly reducing the risk of decomposition from both chemical and concentration perspectives. As a key interlocking mechanism, the active optimization execution module also generates and executes a command to cut off the reboiler heat source. This command immediately shuts off the heating steam or power supply to the distillation column reboiler, cutting off the system's heat input and eliminating the driving force for decomposition. This is the most important physical interlocking measure to prevent the escalation of decomposition accidents.
[0114] For example, suppose that during the operation of the distillation column, due to sudden changes in feed impurities or localized corrosion of the equipment, the decomposition potential energy index output by the decomposition calculation module is affected. It jumped from 0.55 to 0.70 in a very short time. Meanwhile, the preset safety threshold... Set to 0.65. Critical risk assessment: Exceed The system is in a critical state. An emergency pressure command is generated: the proactive optimization execution module immediately generates an emergency pressure command, requiring the dynamic pressure field establishment module to significantly increase the peak pressure amplitude in the sensitive area compared to the current level. Assume the objective of this operation is to reduce the boiling point of the material in the sensitive zone to [a certain value]. Increase in seconds To ensure the decomposition reaction is rapidly and physically suppressed, an emergency stabilizer injection command is generated. Simultaneously, the module generates an emergency stabilizer injection command, activating a preset emergency injection mode. This requires the in-situ capture reaction module and the reflux self-inhibition module to increase the injection flow rate of the stabilizer precursor to the designed maximum safe flow rate, achieving the maximum intensity of chemical inhibition. The system interlock command is executed: the proactive optimization execution module immediately outputs a command to cut off the reboiler heat source, and the reboiler quickly stops heating. By executing this series of emergency safety interlock commands, when the system detects a critical risk, it immediately takes maximum intervention measures simultaneously from three dimensions: physical, chemical, and heat source, successfully pulling the system away from the decomposition critical point, demonstrating the system's inherent safety interlock capability.
[0115] Based on the same inventive concept, such as Figure 4 As shown, the present invention also provides a continuous hydrogen peroxide purification device with an anti-decomposition safety interlock, the device comprising:
[0116] The parameter acquisition module is used to acquire pressure and temperature parameters at multiple locations along the height of the distillation column and generate the current process parameter set.
[0117] The pressure control module is used to calculate and output pressure adjustment commands for certain locations based on the current set of process parameters.
[0118] The dynamic pressure field establishment module is used to adjust multiple pressure fine-tuning units set at corresponding positions on the distillation column in response to the pressure adjustment command, thereby establishing a dynamic non-uniform pressure field.
[0119] The continuous vacuum distillation module is used to continuously distill the input hydrogen peroxide feedstock under the dynamic non-uniform pressure field to obtain overhead vapor and preliminary purified liquid.
[0120] The in-situ capture reaction module is used to introduce the overhead steam and a stabilizer precursor that can react with trace decomposition products in the overhead steam into a pre-set in-situ capture reactor containing a catalyst to react and generate an in-situ stabilizer.
[0121] The reflux self-inhibition module is used to mix the in-situ stabilizer with the condensed reflux liquid to form a self-inhibition reflux liquid and guide it back into the distillation column;
[0122] The monitoring module is used to monitor and acquire the system status parameter set in real time. The system status parameter set includes at least the updated data of the current process parameter set and the reaction efficiency parameters from the in-situ capture reactor.
[0123] The decomposition calculation module is used to calculate the decomposition potential energy index, which characterizes the overall stability of the system, based on the system state parameter set.
[0124] An active optimization execution module is used to generate and execute active optimization instructions based on the changing trend of the decomposed potential energy index. The active optimization instructions are used to adjust the generation logic of the pressure regulation instructions or adjust the injection parameters of the stabilizer precursor.
[0125] It should be noted that the electrical connections between the various units described above do not necessarily represent direct or indirect connections. Any indirect connection method can be applied to the embodiments of the present invention as long as it achieves the purpose of the present invention. The above descriptions are merely exemplary embodiments of the present invention and should not be construed as limiting the scope of the present invention.
[0126] All equivalent changes and modifications made in accordance with the teachings of this invention are still within the scope of this invention. Those skilled in the art will readily conceive of other embodiments of this invention upon considering the specification and the disclosure of practical truth. This application is intended to cover any variations, uses, or adaptations of this invention that follow the general principles of this invention and include common knowledge or conventional techniques in the art not described herein.
Claims
1. A continuous purification method for hydrogen peroxide with an anti-decomposition safety interlock, characterized in that, The method includes: Obtain pressure and temperature parameters at multiple locations along the height of the distillation column to generate the current process parameter set; Based on the current set of process parameters, calculate and output pressure adjustment commands for certain locations; In response to the pressure regulation command, multiple pressure fine-tuning units located at corresponding positions in the distillation column are adjusted to establish a dynamic non-uniform pressure field; Under the dynamic non-uniform pressure field, the input hydrogen peroxide feedstock is subjected to continuous vacuum distillation to obtain overhead vapor and preliminary purified liquid. The overhead steam and a stabilizer precursor that can react with trace decomposition products in the overhead steam are introduced together into a pre-designed in-situ capture reactor containing a catalyst to react and generate an in-situ stabilizer. The in-situ stabilizer is mixed with the refluxed liquid to form a self-suppressing reflux liquid, which is then returned to the distillation column. The system status parameter set is monitored and acquired in real time. The system status parameter set includes at least the updated data of the current process parameter set and the reaction efficiency parameters from the in-situ capture reactor. Based on the system state parameter set, the decomposed potential energy index characterizing the overall stability of the system is calculated. Based on the changing trend of the decomposed potential energy index, an active optimization instruction is generated and executed. The active optimization instruction is used to adjust the generation logic of the pressure regulation instruction or adjust the injection parameters of the stabilizer precursor.
2. The continuous purification method for hydrogen peroxide with anti-decomposition safety interlock according to claim 1, characterized in that, The step of calculating and outputting pressure adjustment commands for specific locations based on the current process parameter set includes: Regions whose temperature parameters exceed a preset first threshold are identified from the current process parameter set and marked as sensitive regions. Based on the location information of the sensitive area, predict the heat load parameters and vaporization rate parameters of the sensitive area in the future time period; Based on the heat load parameters and the vaporization rate parameters, a pressure regulation command is generated to increase the local pressure in the sensitive area. The pressure regulation command causes the dynamic non-uniform pressure field to form a local pressure peak in the sensitive area.
3. The continuous purification method for hydrogen peroxide with anti-decomposition safety interlock according to claim 1, characterized in that, The process of generating the in-situ stabilizer through reaction includes: The overhead steam containing the trace decomposition products is fed to the in-situ capture reactor, the inner wall of which is coated with a nano-catalytic coating. The stabilizer precursor is converted into stabilizer precursor vapor and quantitatively injected into the inlet section of the in-situ capture reactor. The vapor at the top of the column and the vapor of the stabilizer precursor are controlled to undergo a catalytic reaction when flowing over the surface of the nano-catalytic coating, so as to convert the trace decomposition products into surface-active stabilizer complexes, which constitute in-situ stabilizers.
4. The continuous purification method for hydrogen peroxide with anti-decomposition safety interlock according to claim 3, characterized in that, The process of forming a self-suppressing reflux liquid and guiding it back into the distillation column includes: The gas-liquid mixture output from the in-situ capture reactor is condensed and separated to obtain a condensate enriched with the stabilizer complex. The condensate is mixed with the reflux condensate from the distillation column at an adjustable mixing ratio to generate a self-suppressing reflux liquid; The self-suppressing reflux liquid is introduced into the top reflux distributor of the distillation column, so that it is preferentially adsorbed on the metal surface and gas-liquid interface during the downward flow process in the column.
5. The continuous purification method for hydrogen peroxide with anti-decomposition safety interlock according to claim 1, characterized in that, The reaction efficiency parameters of the in-situ capture reactor include: The concentration difference of specific reactive oxygen species in the in-situ capture reactor gas flow is monitored, and the reactive oxygen conversion rate is calculated. The concentration of the in-situ stabilizer in the self-suppressing reflux liquid was analyzed to obtain the stabilizer formation concentration; The reaction efficiency parameter is generated by weighting the reactive oxygen species conversion rate with the stabilizer generation concentration.
6. The continuous purification method for hydrogen peroxide with anti-decomposition safety interlock according to claim 1, characterized in that, The calculated decomposed potential energy index characterizing the overall stability of the system includes: Based on the system state parameter set, the distance between the current operating point and the theoretical thermal decomposition boundary is calculated, and real-time distance parameters are generated. Acquire information on feed impurities, system operation history, and historical surface condition parameters; Based on the feed impurity information and system operation history, the distribution of catalytically active impurities in the tower is calculated, and catalytic pressure parameters are generated. By integrating the real-time distance parameter, the catalytic pressure parameter, and the surface state history parameter, the decomposition potential energy index characterizing the overall stability of the system is calculated.
7. A continuous purification method for hydrogen peroxide with an anti-decomposition safety interlock according to claim 6, characterized in that, The process of generating and executing active optimization instructions based on the changing trend of the decomposed potential energy index includes: Determine whether the decomposition potential energy index shows a continuous upward trend and whether its value is lower than a preset safety threshold. If so, the active optimization mode is activated to generate a first type of active optimization instruction for fine-tuning the amplitude or position of the pressure peak in the dynamic non-uniform pressure field. Simultaneously, a second type of active optimization instruction is generated to adjust the injection rate or concentration of the stabilizer precursor.
8. The continuous purification method for hydrogen peroxide with anti-decomposition safety interlock according to claim 7, characterized in that, After initiating the active optimization mode, the following also applies: The weighting factor used to calculate the catalytic pressure parameter is dynamically adjusted based on the rate of change of the decomposition potential energy index. Based on the adjusted weighting factors, the updated decomposed potential energy index is recalculated. Based on the updated decomposed potential energy index, closed-loop correction is performed on the first type of active optimization instruction and the second type of active optimization instruction.
9. A continuous purification method for hydrogen peroxide with an anti-decomposition safety interlock according to claim 1, characterized in that, The process of continuously reducing pressure and distilling the input hydrogen peroxide feedstock under the dynamic non-uniform pressure field to obtain overhead vapor and preliminary purified liquid includes: The hydrogen peroxide raw material is filtered and preheated to obtain a purified hydrogen peroxide raw material liquid; The purified hydrogen peroxide feedstock is introduced into the middle of the distillation column, where it undergoes multi-stage equilibrium flash evaporation and mass and heat transfer under a dynamic non-uniform pressure field to separate the column top vapor and the preliminary purified liquid.
10. A continuous hydrogen peroxide purification apparatus with an anti-decomposition safety interlock, applied to the continuous hydrogen peroxide purification method with an anti-decomposition safety interlock as described in any one of claims 1-9, characterized in that, The device includes: The parameter acquisition module is used to acquire pressure and temperature parameters at multiple locations along the height of the distillation column and generate the current process parameter set. The pressure control module is used to calculate and output pressure adjustment commands for certain locations based on the current set of process parameters. The dynamic pressure field establishment module is used to adjust multiple pressure fine-tuning units set at corresponding positions on the distillation column in response to the pressure adjustment command, thereby establishing a dynamic non-uniform pressure field. The continuous vacuum distillation module is used to continuously distill the input hydrogen peroxide feedstock under the dynamic non-uniform pressure field to obtain overhead vapor and preliminary purified liquid. The in-situ capture reaction module is used to introduce the overhead steam and a stabilizer precursor that can react with trace decomposition products in the overhead steam into a pre-set in-situ capture reactor containing a catalyst to react and generate an in-situ stabilizer. The reflux self-inhibition module is used to mix the in-situ stabilizer with the condensed reflux liquid to form a self-inhibition reflux liquid and guide it back into the distillation column; The monitoring module is used to monitor and acquire the system status parameter set in real time. The system status parameter set includes at least the updated data of the current process parameter set and the reaction efficiency parameters from the in-situ capture reactor. The decomposition calculation module is used to calculate the decomposition potential energy index, which characterizes the overall stability of the system, based on the system state parameter set. An active optimization execution module is used to generate and execute active optimization instructions based on the changing trend of the decomposed potential energy index. The active optimization instructions are used to adjust the generation logic of the pressure regulation instructions or adjust the injection parameters of the stabilizer precursor.
Citation Information
Patent Citations
Concentration-rectification optimized production system for concentrating 27.5% hydrogen peroxide dilute solution into 50% hydrogen peroxide thick solution and method thereof
CN103204476A