A time-domain control evaporation process and equipment for dynamic and accurate separation of mixtures with similar boiling points

Abstract

The application discloses a time-domain control evaporation process and equipment for dynamic and accurate separation of mixtures with similar boiling points, and relates to the technical field of chemical separation engineering. The application comprises evaporation treatment and gas phase condensation collection of mixtures with similar boiling points to be separated. In the application, the traditional continuous evaporation process is reconstructed into a three-stage time-domain gate microcirculation process, relying on the closed loop circulation steps of liquid film pre-modulation and interface enrichment, pulse gate selective evaporation and liquid phase time-domain layered shunt, thus completely solving the inherent problems of traditional rectification and evaporation technology, such as the dependence on gas-liquid phase equilibrium, the necessity of adding an entrainer for the separation of azeotrope and near-boiling systems, and the inevitable synchronization of non-target component gasification accompanying the strengthening of evaporation, and breaking the industry problems of thermal decomposition and activity deactivation in the separation process of heat-sensitive materials, so that the azeotrope thermodynamic equilibrium can be broken without auxiliary chemicals, the selectivity of single-stage separation is far higher than that of the traditional process, and the comprehensive energy consumption is reduced.

Description

Technical Field

[0001] This invention relates to the field of chemical separation engineering technology, specifically to a time-domain controlled evaporation process and equipment for the dynamic and precise separation of mixtures with similar boiling points. Background Technology

[0002] In core industrial sectors such as chemical, pharmaceutical, fine chemical, and electronic chemicals, the efficient separation of mixtures with similar boiling points is a key technological bottleneck that restricts the improvement of quality and cost reduction of high-end products. Currently, the mainstream separation technologies in the industry are all focused on enhancing gas-liquid mass transfer in the spatial dimension, relying on the stacking of mass transfer units such as trays and packing to achieve separation.

[0003] However, in existing technologies, mainstream evaporation and distillation technologies generally adopt an integrated constant power steady-state heating mode. Its inherent heat transfer characteristics are fundamentally contradictory to the separation requirements of near-boiling systems, which is the core cause of various technical defects. Under integrated constant power heating, the liquid phase stagnant boundary layer that is in close contact with the heat exchange surface has significant heat transfer resistance. The input heat cannot be dissipated in time through liquid phase change, and it continues to accumulate, forming severe local overheating. Even if the temperature of the main liquid phase is controlled near the target boiling point, the temperature of the heating surface boundary layer will exceed the standard by a large margin. The boiling point difference of the components in the near-boiling system is extremely small, and the saturated vapor pressure is highly sensitive to temperature changes. Even a small temperature overshoot will cause non-target components to evaporate simultaneously, destroying the separation selectivity from the source. Ultimately, this results in extremely low purity of single-stage separation. Near-boiling system separation requires extremely high reflux ratios and theoretical plate numbers, which leads to problems such as large equipment investment, high energy consumption, and easy deactivation of heat-sensitive materials, making it unsuitable for the high-quality separation requirements of high-end products. Summary of the Invention

[0004] The purpose of this invention is to provide a time-domain controlled evaporation process and equipment for the dynamic and precise separation of mixtures with similar boiling points, in order to solve the problem in the prior art mentioned above, where the workpiece is fixed by a fixture body during laser cutting, but only a single independent workpiece can be fixed at a time. When cutting multiple small workpieces, it is impossible to fix and cut multiple workpieces simultaneously, resulting in low production efficiency.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a time-domain controlled evaporation process for the dynamic and precise separation of mixtures with similar boiling points, comprising evaporation of the mixture to be separated with similar boiling points and gas-phase condensation and collection, wherein the process includes the following steps executed sequentially in a cyclic manner: S1. Liquid film pre-modulation and interface enrichment: The mixture to be separated is formed into an ultrathin liquid film with a thickness of 10-100μm on a functionalized interface. The liquid film is then flowed through a constant temperature pre-modulation zone. The difference in thermal diffusivity between the target component and the non-target component is used to drive the target molecules to be directionally enriched on the functionalized interface side. S2, Pulse-gated selective evaporation: The pre-enriched liquid film enters the gated evaporation zone. The temperature of the functionalized interface is kept constant through isothermal cycling. An external field pulse matching the characteristics of the target molecule is applied to the functionalized interface. The desorption energy barrier of the target molecule on the functionalized interface is specifically reduced only within the pulse opening time window, so that the target molecule is selectively desorbed and vaporized, while non-target molecules are retained in the liquid phase. S3, Liquid phase temporal stratification and diversion: The residual liquid film after evaporation enters the diversion zone and is stratified and cut along the thickness direction of the liquid film. The target molecule enriched phase is returned to step S1 for recycling, and the non-target molecule depleted phase is directly discharged from the system. Repeat steps S1 to S3 until the purity of the condensed and collected fraction reaches the preset target.

[0006] Preferably, in step S2, the temperature of the functionalized interface is kept constant at the boiling point of the target component + (1-3)℃, the temperature control accuracy is ±0.05℃, and the isothermal cycle only provides latent heat for the phase change process and does not participate in the separation selectivity control.

[0007] Preferably, the pulse width of the external field pulse ,in The average desorption time of the target molecule at the functionalized interface; the amplitude of the external field pulse satisfies the following condition: reducing the desorption energy barrier of the target molecule to [value missing]. Quantity, of which Boltzmann's constant, The temperature is the thermodynamic temperature of the functionalized interface; the duty cycle of the external field pulse is 0.01%-0.1%.

[0008] Preferably, in step S1, the temperature of the isothermal pre-modulation zone is kept constant between the boiling points of the target component and the non-target component, and the residence time of the liquid film in the pre-modulation zone is 0.05-0.2 s. After pre-modulation, the concentration of the target molecule on the functionalized interface side is increased by 2-5 times compared with the bulk liquid phase. In step S3, the layered components of the residual liquid film are monitored in real time by online composition detection, and the layering cutting position and the reflux ratio of the target molecule enriched phase are dynamically adjusted. The reflux ratio is 10%-30%. The total duration of a single cycle consisting of steps S1 to S3 is 0.5-5 seconds, and the number of cycles is 5-20.

[0009] Preferably, the external field pulse is any one of nanosecond high-voltage pulsed electric field, high-frequency ultrasonic pulse, or nanosecond-level pulsed laser; the process is preset with a standardized linear mapping model of molecular inherent properties and process control parameters, which can directly match process parameters according to the molecular properties of the material to be separated, and is suitable for the separation and purification of near-boiling mixtures, azeotropic mixtures, thermosensitive fine chemicals, chiral pharmaceutical intermediates, and electronic-grade high-purity solvents with boiling point differences ≥0.5℃.

[0010] A device for dynamic and precise separation of mixtures with similar boiling points using a time-domain controlled evaporation process includes a vertical pressure chamber, a feeding distribution mechanism, a constant temperature circulation system, a condensation and collection unit, and a vacuum system. The vertical pressure chamber is a five-layer coaxial, sealed, and interconnected chamber structure from top to bottom, consisting of a condensation and enrichment chamber, a gas-liquid separation and defoaming chamber, a gated evaporation core chamber, a pre-modulation and diversion collection chamber, and a driving and sealing isolation chamber. A rotating conical disk assembly is coaxially arranged within the gated evaporation core chamber. Functional interface modules are bonded to the disk surface of the rotating conical disk assembly. The disk surface is divided into a pre-modulation zone, a gated evaporation zone, and a diversion and guiding zone from top to bottom along the liquid film flow direction. The equipment also includes a pulsed external field generation and control system, a time-domain splitting and circulation system, and an online detection and closed-loop control system. The pulsed external field generation and control system is matched and connected to the functional interface module to output an external field pulse that matches the characteristics of the target molecule. The time-domain splitting and circulation system is built into the pre-modulation and splitting collection chamber, with the feed end facing the splitting and guiding area of ​​the rotating cone disk assembly, and the discharge end divided into a return branch and an external discharge branch. The online detection and closed-loop control system is connected to the constant temperature circulation system, the pulsed external field generation and control system, and the time-domain splitting and circulation system respectively, for real-time monitoring and closed-loop adjustment of the entire process parameters. A servo drive mechanism is installed in the drive and sealed isolation chamber, and the servo drive mechanism is connected to the rotating cone disk assembly for transmission.

[0011] Preferably, the functional interface module is provided with a molecular recognition layer, a transducer layer, and a thermally conductive buffer layer stacked sequentially from top to bottom; the molecular recognition layer is any one of a cross-linked molecularly imprinted membrane, a polymer composite membrane, or a functionalized self-assembled monolayer; the transducer layer is electrically connected to the pulsed external field generation and control system; the thermally conductive buffer layer has a built-in constant temperature flow channel, which is connected to the constant temperature circulation system through a rotary joint.

[0012] Preferably, the condensation enrichment chamber is equipped with a tubular condenser tube bundle and a fraction collection tank. The refrigerant interface of the condenser tube bundle is connected to a constant temperature circulation system, and the outlet of the fraction collection tank is connected to a high-purity product storage tank and a return port of the feed distribution mechanism, respectively. The gas-liquid separation and demisting chamber is equipped with a wire mesh demister and a baffle plate gas-liquid separator from top to bottom. The time-domain diversion and circulation system of the pre-modulation and diversion collection chamber is a coaxial annular stepped double-tank collection structure, divided into an inner enriched phase collection tank and an outer depleted phase collection tank. The inner tank is connected to the feed inlet of the feed distribution mechanism through a circulation pump, and the outer tank is connected to the system's external discharge pipeline. The bottom drive and sealing isolation chamber is equipped with an isolation sealing partition between itself and the chamber body, and the chamber is equipped with a main shaft support assembly and a mechanical seal assembly.

[0013] Preferably, the pulse field generation and control system is a multi-channel synchronous high-voltage nanosecond pulse generator, which is electrically connected to the electrodes and transducer layer of the functional interface module through an explosion-proof conductive slip ring, and supports bipolar pulse output; the constant temperature circulation system has a temperature control accuracy of ≤±0.05℃ and can maintain the temperature fluctuation of the functional interface module ≤±0.1℃.

[0014] Preferably, the online detection and closed-loop control system includes at least one of an online Raman spectroscopy detection unit, an infrared thermal imaging unit, a film thickness sensor, and a temperature and pressure sensor; the electrode and transducer layers of the functional interface module integrate a reverse pulse in-situ regeneration module; the online detection and closed-loop control system is also equipped with a safety interlock module for early warning and automatic shutdown protection of abnormal equipment conditions.

[0015] Compared with the prior art, the beneficial effects of the present invention are: 1. In this invention, by reconstructing the traditional continuous evaporation process into a three-stage time-domain gated microcirculation process, relying on the closed-loop circulation steps of liquid film pre-modulation and interface enrichment, pulse-gated selective evaporation, and liquid phase time-domain stratification and diversion, the inherent pain points of traditional distillation and evaporation technologies, which rely on gas-liquid phase equilibrium, near-boiling, and azeotropic system separation, require the addition of entrainers, and the inevitable simultaneous vaporization of non-target components due to temperature-enhanced evaporation, are completely solved. At the same time, it solves the industry problem of thermal decomposition and deactivation of active materials during the separation process of heat-sensitive materials. It can break the azeotropic thermodynamic equilibrium without auxiliary chemicals, and the single-stage separation selectivity is far superior to traditional processes, reducing overall energy consumption and reducing the generation of waste from the source. It is perfectly adapted to the high-purity separation needs of the fine chemical and pharmaceutical fields. 2. In this invention, a special separation device with a vertical pressure-bearing cavity and five layers of coaxial sealing and connection is designed. By bonding a rotating conical disk assembly with three layers of composite functional interface, a multi-channel synchronous nanosecond pulse generation system, and a closed-loop online detection and reverse pulse in-situ regeneration module, the pain points of industrialization of traditional separation equipment, such as significant scale-up effect, large investment, large footprint, poor stability during long-term operation, and difficulty in online treatment of functional interface contamination, are solved. Attached Figure Description

[0016] Figure 1 This is a flowchart of a time-domain controlled evaporation process for dynamic and precise separation of mixtures with similar boiling points, according to the present invention. Figure 2 This is a three-dimensional structural diagram of a time-domain controlled evaporation process for dynamic and precise separation of mixtures with similar boiling points, according to the present invention. Figure 3 This is a schematic cross-sectional view of the equipment used in the present invention for the dynamic and precise separation of mixtures with similar boiling points using a time-domain controlled evaporation process.

[0017] In the diagram: 100, vertical pressure chamber; 1, condensation and enrichment chamber; 2, gas-liquid separation and defoaming chamber; 3, gated evaporation core chamber; 4, pre-modulation and diversion collection chamber; 5, driving and sealing isolation chamber. Detailed Implementation

[0018] 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 a part of the embodiments of the present invention, and not all of them. 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.

[0019] Example 1: Refer to Figure 1-3 The diagram illustrates a time-domain controlled evaporation process for the dynamic and precise separation of mixtures with similar boiling points. The process includes evaporation of the mixture to be separated, followed by vapor-phase condensation and collection. The process comprises the following steps, executed sequentially in a cyclical manner: S1. Liquid film pre-modulation and interface enrichment: The mixture to be separated is formed into an ultrathin liquid film with a thickness of 10-100μm on a functionalized interface. The liquid film is then flowed through a constant temperature pre-modulation zone. The difference in thermal diffusivity between the target component and the non-target component is used to drive the target molecules to be directionally enriched on the functionalized interface side. S2, Pulse-gated selective evaporation: The pre-enriched liquid film enters the gated evaporation zone. The temperature of the functionalized interface is kept constant through isothermal cycling. An external field pulse matching the characteristics of the target molecule is applied to the functionalized interface. The desorption energy barrier of the target molecule on the functionalized interface is specifically reduced only within the pulse opening time window, so that the target molecule is selectively desorbed and vaporized, while non-target molecules are retained in the liquid phase. S3, Liquid phase temporal stratification and diversion: The residual liquid film after evaporation enters the diversion zone and is stratified and cut along the thickness direction of the liquid film. The target molecule enriched phase is returned to step S1 for recycling, and the non-target molecule depleted phase is directly discharged from the system. Repeat steps S1 to S3 until the purity of the condensed and collected fraction reaches the preset target.

[0020] In step S2, the temperature of the functionalized interface is kept constant at the boiling point of the target component + (1-3)℃, with a temperature control accuracy of ±0.05℃. The isothermal cycle only provides latent heat for the phase change process and does not participate in the separation selectivity control.

[0021] Pulse width of external field pulse ,in The average desorption time of the target molecule at the functionalized interface; the amplitude of the external field pulse satisfies the following condition: reducing the desorption energy barrier of the target molecule to [value missing]. Quantity, of which Boltzmann's constant, The temperature is the thermodynamic temperature of the functionalized interface; the duty cycle of the external field pulse is 0.01%-0.1%.

[0022] In step S1, the temperature of the isothermal pre-modulation zone is kept constant between the boiling points of the target component and the non-target component. The residence time of the liquid film in the pre-modulation zone is 0.05-0.2s. After pre-modulation, the concentration of the target molecule on the functionalized interface side is increased by 2-5 times compared with the bulk liquid phase. In step S3, the layered components of the residual liquid film are monitored in real time by online composition detection. The layering cutting position and the reflux ratio of the target molecule enriched phase are dynamically adjusted. The reflux ratio is 10%-30%. The total duration of a single cycle consisting of steps S1 to S3 is 0.5-5s, and the number of cycles is 5-20.

[0023] The external pulse can be any one of nanosecond high-voltage pulsed electric field, high-frequency ultrasonic pulse, or nanosecond pulsed laser; the process is preset with a standardized linear mapping model of molecular inherent properties and process control parameters, which can directly match process parameters according to the molecular characteristics of the material to be separated. It is suitable for the separation and purification of near-boiling mixtures, azeotropic mixtures, thermosensitive fine chemicals, chiral pharmaceutical intermediates, and electronic-grade high-purity solvents with boiling point differences ≥0.5℃.

[0024] In this embodiment, the time-domain controlled evaporation process completely breaks through the traditional thermally driven gas-liquid equilibrium separation technology paradigm. Its core lies in achieving complete decoupling of phase change heat energy and separation driving force, fundamentally resolving the inherent contradiction in traditional evaporation and distillation technologies where "heat-enhanced evaporation inevitably involves the simultaneous vaporization of non-target components." During process operation, the isothermal circulation system only provides latent heat for the phase change process and does not participate in separation selectivity control. The desorption and vaporization of target molecules are entirely dominated by the time-domain gating effect of the external field pulses. High-purity separation is achieved through a three-stage time-domain micro-circulation executed sequentially. The liquid film pre-modulation and interface enrichment stage is based on the thermal diffusion Sorrett effect. By controlling the pre-modulation temperature and liquid film residence time, the target molecules are directionally enriched at the functionalized interface, reducing the selectivity pressure for subsequent separation stages. The pulse-gated selective evaporation stage is based on the time-domain gated molecular rectification effect. Through an external field pulse precisely matched to the characteristics of the target molecules, it specifically reduces the target molecules'... The desorption energy barrier is set, and a precise molecular desorption time window is formed by setting the pulse width to match the average desorption time of the target molecules. Only the target molecules are allowed to complete desorption and vaporization during the pulse opening phase, while non-target molecules remain in the liquid phase throughout the process, achieving high selective separation at the molecular level. The liquid phase time-domain stratification and diversion stage is based on the component concentration gradient in the direction of liquid film thickness to achieve uninterrupted stratification and cutting of the enriched phase and the depleted phase. The product recovery rate is ensured by the reflux of the enriched phase, and the repeated cycling and heating of non-target components is avoided by the direct discharge of the depleted phase. Finally, through the time-domain cyclic iteration, the traditional spatial dimension of distillation tray stacking is replaced, and the product purity is continuously improved.

[0025] Operating stably under normal pressure, the pretreated raw material is fed into the liquid film distributor at a flow rate of 20 mL / min via a high-precision metering pump, forming a uniform ultrathin liquid film with a thickness of 30 μm on the interface of the ethanol-specific cross-linked molecularly imprinted composite membrane. The temperature of the pre-modulation zone is set at the midpoint of the boiling points of the two components, 80.4℃, and the liquid film pre-modulation residence time is controlled at 0.1 s, so that the ethanol concentration at the interface is 3.2 times higher than that of the bulk liquid phase. In the gated evaporation stage, the functionalized interface is kept at a constant temperature of 79.0℃, with a temperature control accuracy of ±0.05℃. At the same time, a bipolar nanosecond high-voltage pulse electric field with an amplitude of 50 kV / cm, a width of 50 ns, and a frequency of 10 kHz is applied, with a duty cycle controlled at 0.05%, to achieve selective desorption and vaporization of ethanol molecules. In the splitting stage, the liquid film components are monitored in real time by online Raman spectroscopy. A 20% enriched phase reflux ratio is set to complete a single round of micro-circulation. The total duration of a single round of circulation is controlled at 2 s. After 8 consecutive cycles, the purity of the distillate is detected online and the separation process is terminated.

[0026] Quantitative analysis by gas chromatography showed that the ethanol mass fraction in the final condensate reached 99.7%, exceeding the preset separation target. The total ethanol recovery rate reached 98.5%, and the isopropanol purity in the depleted phase reached 99.4%. The comprehensive energy consumption of the separation process was 38 kWh / ton of raw material. The single heating time of the material was only 0.1 s, and the total heating time was only 1.6 s. During continuous operation for 72 hours, the product purity fluctuation did not exceed ±0.05%, the functionalized interface separation performance retention rate was not less than 98%, and no abnormal conditions such as membrane fouling or clogging occurred.

[0027] This embodiment fully verifies the feasibility of the time-domain controlled evaporation process for separating near-boiling mixtures, demonstrating multi-dimensional technical advantages and industry application value. Firstly, this process completely breaks free from the thermodynamic constraints of traditional gas-liquid phase equilibrium, achieving high-purity separation of near-boiling systems in a single stage. This breaks the performance limits of traditional distillation technology for near-boiling system separation. By adjusting the number of cycles, it can flexibly adapt to different purity requirements, even meeting the ultra-high purity separation requirements of electronic-grade chemicals. Furthermore, it eliminates the need for auxiliary chemicals such as entrainers and extractants, adapting to the separation needs of azeotropic systems and reducing waste generation at the source. Secondly, through core designs such as thermal-field decoupling and direct discharge of the depleted phase, this process significantly reduces ineffective energy consumption in traditional separation processes, lowering overall energy consumption by 87% compared to traditional distillation processes. Simultaneously, the equipment has a compact structure, with significantly lower footprint and investment costs than traditional distillation equipment, exhibiting outstanding green and low-carbon characteristics. Firstly, it offers cost advantages. Secondly, the process achieves precise control of interface constant temperature without overheating, shortening the total heating time of materials by three orders of magnitude compared to traditional processes. This completely avoids the decomposition and inactivation of heat-sensitive materials during the separation process, perfectly meeting the mild separation requirements of active ingredients in the pharmaceutical and bio-based chemical fields. Thirdly, the process establishes a standardized mapping relationship between molecular characteristics and process parameters. When changing material systems, only the process formulation needs to be adjusted, without modifying the equipment structure. It has extremely strong process flexibility and can adapt to various difficult-to-separate systems such as isomers and chiral molecules. At the same time, the core separation performance is not directly related to the scale of the equipment. Laboratory process parameters can be directly transferred to industrial mass production equipment without the scale-up effect of traditional separation technologies, demonstrating excellent prospects for industrial application.

[0028] Example 2: Figure 2 and Figure 3 As shown, an apparatus for dynamic and precise separation of mixtures with similar boiling points using a time-domain controlled evaporation process includes a vertical pressure chamber 100, a feeding distribution mechanism, a constant temperature circulation system, a condensation and collection unit, and a vacuum system. The vertical pressure chamber 100 is a five-layer cavity structure that is coaxially sealed and connected from top to bottom, consisting of a condensation and enrichment cavity 1, a gas-liquid separation and defoaming cavity 2, a gated evaporation core cavity 3, a pre-modulation and diversion collection cavity 4, and a driving and sealing isolation cavity 5. A rotating conical disk assembly is coaxially arranged in the gated evaporation core cavity 3. The disk surface of the rotating conical disk assembly is bonded with a functional interface module. The disk surface is divided into a pre-modulation zone, a gated evaporation zone, and a diversion and guiding zone from top to bottom along the liquid film flow direction. The equipment also includes a pulse external field generation and control system, a time-domain splitting and circulation system, and an online detection and closed-loop control system. The pulse external field generation and control system is matched and connected to the functional interface module to output an external field pulse that matches the characteristics of the target molecule. The time-domain splitting and circulation system is built into the pre-modulation and splitting collection chamber 4, with the feed end facing the splitting and guiding area of ​​the rotating cone disk assembly, and the discharge end divided into a return branch and an external discharge branch. The online detection and closed-loop control system is connected to the constant temperature circulation system, the pulse external field generation and control system, and the time-domain splitting and circulation system respectively, for real-time monitoring and closed-loop adjustment of the parameters of the entire process. A servo drive mechanism is installed in the drive and sealed isolation chamber 5, and the servo drive mechanism is connected to the rotating cone disk assembly for transmission.

[0029] The functional interface module is stacked from top to bottom with a molecular recognition layer, a transducer layer, and a thermally conductive buffer layer. The molecular recognition layer is any one of a cross-linked molecularly imprinted membrane, a polymer composite membrane, or a functionalized self-assembled monolayer. The transducer layer is electrically connected to the pulsed external field generation and control system. The thermally conductive buffer layer has a built-in constant temperature flow channel, which is connected to the constant temperature circulation system through a rotary joint.

[0030] The condensation enrichment chamber 1 is equipped with a tubular condenser tube bundle and a fraction collection tank. The refrigerant interface of the condenser tube bundle is connected to the constant temperature circulation system, and the outlet of the fraction collection tank is connected to the high-purity product storage tank and the return port of the feed distribution mechanism, respectively. The gas-liquid separation demister chamber 2 is equipped with a wire mesh demister and a baffle plate gas-liquid separator from top to bottom. The time-domain diversion and circulation system in the pre-modulation and diversion collection chamber 4 is a coaxial annular stepped double-tank collection structure, which is divided into an inner enriched phase collection tank and an outer depleted phase collection tank. The inner tank is connected to the feed inlet of the feed distribution mechanism through a circulation pump, and the outer tank is connected to the system's external discharge pipeline. The bottom drive and sealing isolation chamber 5 is equipped with an isolation sealing partition between itself and the chamber body. The chamber is equipped with a main shaft support assembly and a mechanical seal assembly.

[0031] The pulse field generation and control system is a multi-channel synchronous high-voltage nanosecond pulse generator. It is electrically connected to the electrodes and transducer layer of the functional interface module through an explosion-proof conductive slip ring, and supports bipolar pulse output. The constant temperature circulation system has a temperature control accuracy of ≤±0.05℃ and can maintain the temperature fluctuation of the functional interface module at ≤±0.1℃.

[0032] The online detection and closed-loop control system includes at least one of an online Raman spectroscopy detection unit, an infrared thermal imaging unit, a film thickness sensor, and a temperature and pressure sensor; the electrodes and transducer layers of the functional interface module integrate a reverse pulse in-situ regeneration module; the online detection and closed-loop control system also has a safety interlock module for early warning and automatic shutdown protection of abnormal equipment conditions.

[0033] In this embodiment, the vertical pressure-bearing cavity 100 is the core pressure-bearing body. It adopts a five-layer cavity structure that is coaxially sealed and connected from top to bottom. The cavity consists of a condensation and enrichment cavity 1, a gas-liquid separation and defoaming cavity 2, a gated evaporation core cavity 3, a pre-modulation and diversion collection cavity 4, and a driving and sealing isolation cavity 5. The entire cavity is precision machined coaxially, which can realize the closed and continuous operation of the entire process from feeding, pre-enrichment, selective separation, gas phase condensation, liquid phase diversion to circulation enrichment. It completely avoids the material from contacting the outside air and is suitable for the industrial production needs of flammable, explosive and easily oxidized organic systems.

[0034] The core separation function of the equipment is achieved through a rotating conical disk assembly coaxially arranged in the gated evaporation core chamber 3. The servo drive mechanism in the drive and sealed isolation chamber 5 is connected to the rotating conical disk assembly, and the liquid film thickness on the disk surface can be precisely controlled by the rotation speed. The disk surface of the rotating conical disk assembly is bonded with functional interface modules. The disk surface is divided into a pre-modulation zone, a gated evaporation zone, and a diversion and guiding zone from top to bottom along the liquid film flow direction, which is completely matched with the three-stage time-domain micro-circulation of the process. The functional interface module is stacked from top to bottom with a molecular recognition layer, a transducer layer, and a thermally conductive buffer layer. The molecular recognition layer uses a specific functional membrane material customized for thiophene molecules, which can specifically adsorb and recognize trace amounts of thiophene molecules in the system. The transducer layer is electrically connected to the pulse external field generation and control system through an explosion-proof conductive slip ring. The constant temperature channel built into the thermally conductive buffer layer is connected to the constant temperature circulation system through a rotary joint, which can achieve precise and constant temperature control of the entire disk surface. During equipment operation, the phase change heat energy and separation driving force are completely decoupled. The constant temperature circulation system provides the latent heat of phase change to the system only through the thermally conductive buffer layer and does not participate in the separation selectivity control. The separation of target components and non-target components is completely dominated by the time-domain pulse signal output by the pulse external field generation and control system. Through the specific regulation of the desorption energy barrier of target molecules by the external field pulse, the thermodynamic equilibrium limitation of the azeotropic system is broken. The deep separation of azeotropes can be achieved without adding any extractant or entrainer. After rising from the gated evaporation core chamber 3, the gas phase first enters the gas-liquid separation and demisting chamber 2. There, a wire mesh demister and a baffle plate gas-liquid separator, arranged from top to bottom, completely trap the mist droplets in the gas phase, preventing non-target components from entering the product and ensuring product purity. The demisted gas phase continues to rise into the condensation and enrichment chamber 1, where it is condensed and liquefied by the tubular condenser tubes and collected in the fraction collection tank. The residual liquid film after evaporation flows out from the diversion and guiding area of ​​the rotating conical disk assembly and enters the time-domain diversion and circulation system in the pre-modulation and diversion collection chamber 4. This system is coaxial. The annular stepped dual-tank collection structure achieves unobstructed stratification and diversion of the liquid film through the inner enriched phase collection tank and the outer depleted phase collection tank. The enriched phase is returned to the feed distribution mechanism for further separation via a circulating pump, while the depleted phase is directly discharged, avoiding repeated circulation of non-target components within the system. The online detection and closed-loop control system collects full-process parameters in real time through sensors at various points, enabling closed-loop regulation of the constant temperature circulation system, pulse external field generation and control system, and time-domain diversion and circulation system. At the same time, the safety interlock module provides early warning and automatic shutdown for abnormal operating conditions, ensuring the safe and stable operation of industrial production.

[0035] This embodiment employs a two-stage series rotary conical disc separator that operates continuously under normal pressure. The benzene-thiophene mixed raw material to be separated is pretreated and then fed into the feed distribution mechanism via a variable frequency feed pump. The feed distribution mechanism is coaxially fixed to the top center of the rotary conical disc assembly. The raw material is evenly sprayed onto the top of the conical disc through an annular gap. Under the centrifugal force driven by the servo drive mechanism, a uniform ultrathin liquid film is formed on the surface of the conical disc. The liquid film flows from top to bottom along the surface of the conical disc through the pre-modulation zone, the gated evaporation zone, and the diversion and guiding zone, completing a single-round separation cycle. In the pre-modulation stage, the temperature of the pre-modulation zone is kept constant by a constant temperature circulation system, and the residence time of the liquid film in the pre-modulation zone is precisely matched with the characteristics of the system. The thermal diffusion effect and the specific adsorption of the molecular recognition layer are used to make thiophene molecules directionally enriched on the interface side. In the gated evaporation stage, the temperature of the functionalized interface is kept constant without fluctuation by a constant temperature circulation system. The pulse external field generation and control system adopts a multi-channel synchronous high-voltage nanosecond pulse generator, which outputs a bipolar pulse signal matching the characteristics of the target molecules to the transducer layer through an explosion-proof conductive slip ring. The selective desorption of thiophene molecules is achieved through the time-domain pulse gating effect. The desorbed gas phase rises from the gated evaporation core cavity 3, first enters the gas-liquid separation demisting cavity 2 to complete the mist interception, and then enters the condensation enrichment cavity 1. The condensation is completed by the tubular condenser bundle. The condensate is collected in the fraction collection tank. The first-stage fraction that does not meet the standard is returned to the feed port for further separation. The first-stage fraction that meets the standard is sent to the secondary separation unit for deep removal. After the secondary deep separation, the fraction with the required purity is sent to the high-purity product storage tank. During the diversion stage, the residual liquid film after evaporation enters the annular stepped double-trough collection structure in the pre-modulation and diversion collection chamber 4. The two-phase components are monitored in real time by the online component detection unit, and the enriched phase reflux ratio is dynamically adjusted. The enriched phase is refluxed to the feed distribution mechanism by the circulation pump, while the depleted phase is directly discharged to the heavy component storage tank. During equipment operation, the online detection and closed-loop control system monitors the entire process conditions in real time through various sensor units, and automatically adjusts the feed flow rate, cone disk speed, pulse parameters and diversion ratio. When abnormal conditions occur, the safety interlock module automatically triggers graded early warning and emergency shutdown protection. At the same time, the reverse pulse in-situ regeneration module integrated in the transducer layer of the functional interface module can automatically trigger the in-situ regeneration program according to the membrane fouling situation, ensuring long-term stable operation of the equipment.

[0036] Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A time-domain controlled evaporation process for the dynamic and precise separation of mixtures with similar boiling points, comprising evaporating the mixtures with similar boiling points to be separated and collecting the vapor-phase condensate, characterized in that, The process includes the following steps, which are performed sequentially in a cyclical manner: S1. Liquid film pre-modulation and interface enrichment: The mixture to be separated is formed into an ultrathin liquid film with a thickness of 10-100μm on a functionalized interface. The liquid film is then flowed through a constant temperature pre-modulation zone. The difference in thermal diffusivity between the target component and the non-target component is used to drive the target molecules to be directionally enriched on the functionalized interface side. S2, Pulse-gated selective evaporation: The pre-enriched liquid film enters the gated evaporation zone. The temperature of the functionalized interface is kept constant through isothermal cycling. An external field pulse matching the characteristics of the target molecule is applied to the functionalized interface. The desorption energy barrier of the target molecule on the functionalized interface is specifically reduced only within the pulse opening time window, so that the target molecule is selectively desorbed and vaporized, while non-target molecules are retained in the liquid phase. S3, Liquid phase temporal stratification and diversion: The residual liquid film after evaporation enters the diversion zone and is stratified and cut along the thickness direction of the liquid film. The target molecule enriched phase is returned to step S1 for recycling, and the non-target molecule depleted phase is directly discharged from the system. Repeat steps S1 to S3 until the purity of the condensed and collected fraction reaches the preset target.

2. The time-domain controlled evaporation process for dynamic and precise separation of mixtures with similar boiling points according to claim 1, characterized in that: In step S2, the temperature of the functionalized interface is kept constant at the boiling point of the target component + (1-3)℃, and the temperature control accuracy is ±0.05℃. The isothermal cycle only provides latent heat for the phase change process and does not participate in the separation selectivity control.

3. The time-domain controlled evaporation process for dynamic and precise separation of mixtures with similar boiling points according to claim 2, characterized in that: The pulse width of the external field pulse ,in The mean desorption time of the target molecule at the functionalized interface; The amplitude of the external field pulse satisfies the following condition: it lowers the desorption energy barrier of the target molecule to [value missing]. Quantity, of which Boltzmann's constant, The temperature is the thermodynamic temperature of the functionalized interface; the duty cycle of the external field pulse is 0.01%-0.1%.

4. The time-domain controlled evaporation process for dynamic and precise separation of mixtures with similar boiling points according to claim 3, characterized in that: In step S1, the temperature of the isothermal pre-modulation zone is kept constant between the boiling points of the target component and the non-target component. The residence time of the liquid film in the pre-modulation zone is 0.05-0.2 s. After pre-modulation, the concentration of target molecules on the functionalized interface side is increased by 2-5 times compared with the bulk liquid phase. In step S3, the layered components of the residual liquid film are monitored in real time by online composition detection, and the layering cutting position and the reflux ratio of the target molecule enriched phase are dynamically adjusted. The reflux ratio is 10%-30%. The total duration of a single cycle consisting of steps S1 to S3 is 0.5-5 seconds, and the number of cycles is 5-20.

5. The time-domain controlled evaporation process for dynamic and precise separation of mixtures with similar boiling points according to claim 4, characterized in that: The external field pulse can be any one of nanosecond high-voltage pulsed electric field, high-frequency ultrasonic pulse, or nanosecond-level pulsed laser; the process is preset with a standardized linear mapping model of molecular inherent properties and process control parameters, which can directly match process parameters according to the molecular properties of the material to be separated, and is suitable for the separation and purification of near-boiling mixtures, azeotropic mixtures, thermosensitive fine chemicals, chiral pharmaceutical intermediates, and electronic-grade high-purity solvents with boiling point differences ≥0.5℃.

6. An apparatus for achieving dynamic and precise separation of mixtures with similar boiling points as described in claim 5, comprising a vertical pressure chamber (100), a feeding distribution mechanism, a constant temperature circulation system, a condensation and collection unit, and a vacuum system, characterized in that: The vertical pressure-bearing cavity (100) is a five-layer cavity structure that is coaxially sealed and connected from top to bottom. It consists of a condensation and enrichment cavity (1), a gas-liquid separation and defoaming cavity (2), a gated evaporation core cavity (3), a pre-modulation and diversion collection cavity (4), and a driving and sealing isolation cavity (5). A rotating conical disk assembly is coaxially arranged in the gated evaporation core cavity (3). The disk surface of the rotating conical disk assembly is bonded with a functional interface module. The disk surface is divided into a pre-modulation zone, a gated evaporation zone, and a diversion and guiding zone from top to bottom along the liquid film flow direction. The device also includes a pulsed external field generation and control system, a time-domain splitting and circulation system, and an online detection and closed-loop control system; the pulsed external field generation and control system is matched and connected to the functional interface module to output an external field pulse that matches the characteristics of the target molecule; The time-domain diversion and circulation system is built into the pre-modulation and diversion collection cavity (4). The feed end is directly opposite the diversion and guiding area of ​​the rotating cone disk assembly, and the discharge end is divided into a return branch and an external discharge branch. The online detection and closed-loop control system is connected to the constant temperature circulation system, the pulse external field generation and control system, and the time-domain diversion and circulation system respectively, for real-time monitoring and closed-loop adjustment of the parameters of the whole process. The drive and sealed isolation cavity (5) is equipped with a servo drive mechanism, which is connected to the rotating cone disk assembly for transmission.

7. The apparatus for the time-domain controlled evaporation process of dynamically and precisely separating mixtures with similar boiling points according to claim 6, characterized in that: The functional interface module is provided with a molecular recognition layer, a transducer layer, and a thermally conductive buffer layer stacked sequentially from top to bottom; the molecular recognition layer is any one of a cross-linked molecularly imprinted membrane, a polymer composite membrane, or a functionalized self-assembled monolayer; the transducer layer is electrically connected to the pulsed external field generation and control system; the thermally conductive buffer layer has a built-in constant temperature flow channel, which is connected to the constant temperature circulation system through a rotary joint.

8. The apparatus for the time-domain controlled evaporation process of dynamically and precisely separating mixtures with similar boiling points according to claim 7, characterized in that: The condensation enrichment chamber (1) is equipped with a tubular condenser tube bundle and a fraction collection tank. The refrigerant interface of the condenser tube bundle is connected to the constant temperature circulation system. The outlet of the fraction collection tank is connected to the high-purity product storage tank and the return port of the feed distribution mechanism, respectively. The gas-liquid separation demisting chamber (2) is equipped with a wire mesh demister and a baffle plate gas-liquid separator from top to bottom. The time-domain diversion and circulation system in the pre-modulation and diversion collection chamber (4) is a coaxial ring stepped double-tank collection structure, which is divided into an inner enriched phase collection tank and an outer depleted phase collection tank. The inner tank is connected to the feed distribution mechanism inlet through a circulation pump, and the outer tank is connected to the system's external discharge pipeline. The bottom drive and sealing isolation chamber (5) is equipped with an isolation sealing partition between itself and the cavity. The cavity is equipped with a main shaft support assembly and a mechanical seal assembly.

9. The apparatus for the time-domain controlled evaporation process of dynamically and precisely separating mixtures with similar boiling points according to claim 8, characterized in that: The pulse field generation and control system is a multi-channel synchronous high-voltage nanosecond pulse generator, which is electrically connected to the electrodes and transducer layer of the functional interface module through an explosion-proof conductive slip ring, and supports bipolar pulse output; the constant temperature circulation system has a temperature control accuracy of ≤±0.05℃ and can maintain the temperature fluctuation of the functional interface module ≤±0.1℃.

10. The apparatus for the time-domain controlled evaporation process of dynamically and precisely separating mixtures with similar boiling points according to claim 9, characterized in that: The online detection and closed-loop control system includes at least one of an online Raman spectroscopy detection unit, an infrared thermal imaging unit, a film thickness sensor, and a temperature and pressure sensor; the electrode and transducer layers of the functional interface module integrate a reverse pulse in-situ regeneration module; the online detection and closed-loop control system is also equipped with a safety interlock module for early warning of abnormal equipment conditions and automatic shutdown protection.

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