A two-stage rectification purification equipment with staged condensation and reflux

Abstract

The application discloses a kind of hierarchical condensation reflux type two-stage rectification purification equipment, belong to rectification equipment technical field.The equipment includes mounting bracket, primary rectification part, secondary rectification part, condensing part, vacuum negative pressure part and collection device.The condensing part being communicated with primary rectification part is first condensing device, is set at 10 DEG C ~ 20 DEG C first temperature under work;The condensing part being communicated with secondary rectification part is second condensing device, is set at 20 DEG C ~ 30 DEG C second temperature under work, for making product condensation reflux and separating light component.The output end of condensing part being communicated with primary rectification part is communicated with raw material input end of secondary rectification part by special condensate reflux pipeline, and condensate produced by primary rectification is used as the only raw material source of secondary rectification.The application solves the problems of material path confusion, unreasonable condensing structure, temperature control lag and product contamination in the prior art, and has the advantages of high integration, high purification precision, good process flexibility and the like.

Description

Technical Field

[0001] This invention relates to the technical field of staged condensation reflux two-stage distillation purification equipment, specifically to a staged condensation reflux two-stage distillation purification equipment. Background Technology

[0002] Co-based precursors, such as dicobalt hexacarbonyl (CCTBA) (including but not limited to liquid Co precursors like CCTBA and CoDCP), are CVD / ALD precursors used to manufacture important functional layers in equipment and are widely applied in chemical vapor deposition (CVD) or atomic layer deposition (ALD) processes. These compounds, as precursors to cobalt or molybdenum materials, exhibit excellent volatility, enabling efficient deposition of corresponding thin films under relatively mild process conditions, ensuring the uniformity and purity of the deposited layer.

[0003] Currently, most existing distillation equipment adopts a single-stage distillation structure, which has limited purification accuracy and cannot meet the requirements for the preparation of high-purity materials. At the same time, the functional units are scattered, resulting in a large equipment footprint, low integration, and a lack of staged temperature condensation control mechanism. This makes it impossible to accurately separate components with different boiling points, and the absence of independent dedicated collection devices makes cross-contamination during product collection easy. Furthermore, the lack of a unified negative pressure environment construction and temperature control linkage mechanism makes the materials prone to deterioration due to high temperatures during distillation, and the efficiency of vapor phase component condensation and recovery is low. Overall, the continuity and stability of the distillation process are poor. Summary of the Invention

[0004] The present invention aims to solve the problems mentioned in the background art by providing a staged condensation reflux two-stage distillation purification device.

[0005] To address the aforementioned problems, this application proposes a staged reflux two-stage distillation purification device, comprising a mounting frame, a primary distillation unit, a secondary distillation unit, a condenser, and a vacuum negative pressure unit. The mounting frame is fixedly installed on the ground. The primary distillation unit is located on the upper part of the mounting frame and is used for primary distillation of the raw materials. The secondary distillation unit is located on the upper part of the mounting frame and below the primary distillation unit. The condenser has two sets, each connected to the discharge ends of the primary and secondary distillation units respectively. The condenser connected to the primary distillation unit is a first condensation device, set to operate at a first temperature, used to condense and reflux the light components and products formed after processing the raw materials in the primary distillation unit. The condenser connected to the secondary distillation unit is a second condensation device, set to operate at a second temperature, used to condense and reflux the product to the secondary distillation unit. The primary distillation unit allows light components to pass through and enter the tail gas treatment tower. The output end of the condenser, connected to the primary distillation unit, is connected to the raw material input end of the secondary distillation unit via a dedicated condensate reflux pipeline. This condensation process condenses the gaseous light components generated in the primary distillation unit, which then serves as the raw material for the secondary distillation unit. A vacuum negative pressure unit is positioned above the mounting frame, creating a negative pressure environment in both the primary and secondary distillation units. A collection device, located below the mounting frame and independently connected to both the primary and secondary distillation units, includes a collection box containing collection pipelines and collection tanks corresponding to the primary and secondary distillation units. The collection tanks are placed within the collection box, and the collection pipelines connect the collection tanks to the primary and secondary distillation units.

[0006] As a preferred embodiment of the present invention, the first temperature ranges from 10°C to 20°C.

[0007] As a preferred embodiment of the present invention, the second temperature ranges from 20°C to 30°C.

[0008] In a preferred embodiment of the present invention, the primary distillation unit includes a primary reactor and a primary receiving tank, the discharge end of the primary reactor being connected to the inlet end of the primary receiving tank via a first conduit; the secondary distillation unit includes a secondary reactor and a secondary receiving tank, the discharge end of the secondary reactor being connected to the inlet end of the secondary receiving tank via a second conduit; the vacuum negative pressure unit includes a discharge pipe, a vacuum pipe, and a nitrogen pipe disposed above the mounting frame, the primary reactor and the primary receiving tank, and the secondary reactor and the secondary receiving tank being respectively connected to the nitrogen pipe via a first connecting pipe, and the primary reactor and the primary receiving tank, and the secondary reactor and the secondary receiving tank being respectively connected to the discharge pipe via a second connecting pipe, each connecting pipe being independently equipped with an isolation device. The valve enables independent control of the negative pressure environment of each tank. The condenser includes a cooling pipe connected to the gas phase outlet of the primary receiving tank and the secondary receiving tank. The output end of the cooling pipe is connected to the discharge pipe. The middle part of each group of cooling pipes is spirally arranged. The outer circumferential surface of the middle part of each group of cooling pipes is provided with a cooling element for cooling the middle part of the cooling pipe, thereby cooling the light components and products formed after processing raw materials to form a liquid state. The middle part of the first conduit and the second conduit are connected in series with observation pipes. The outer circumferential surface of each group of observation pipes is provided with a sensing control element for monitoring the temperature of the observation pipe and thus controlling the cooling element. The temperature sensing element of the sensing control element is set at the outlet end of the observation pipe or the outlet end of the condenser to improve the real-time performance of temperature feedback.

[0009] As another preferred embodiment of the present invention, a thermometer is connected in series at the input ends of both the first conduit and the second conduit.

[0010] As another preferred embodiment of the present invention, the discharge ends of the primary reactor, the primary receiving tank, the secondary reactor, and the secondary receiving tank are all connected to discharge pipes. The discharge pipe located in the primary receiving tank is only used to discharge the waste liquid of the heavy distillation components and is not connected to the secondary reactor. The condensate generated by the primary distillation is directly sent to the feed end of the secondary reactor through the condensate return pipeline. Sampling ports are connected in series at the output ends of the discharge pipes of the primary reactor and the secondary reactor, as well as in the middle of the discharge pipes of the primary receiving tank and the secondary receiving tank.

[0011] As another preferred embodiment of the present invention, one end of the vacuum tube is connected to a vacuum pump via a connecting pipe, and the output end of the vacuum pump is connected to a discharge pipe.

[0012] As another preferred embodiment of the present invention, the cooling component includes a heat-conducting inner sleeve that is fitted and tightly attached to the outer peripheral surface of the middle part of the cooling pipe. Multiple sets of semiconductor cooling chips are embedded in the outer peripheral surface of the heat-conducting inner sleeve, and the cold surface of the semiconductor cooling chips forms a heat conduction connection with the heat-conducting inner sleeve. The hot surface of each set of semiconductor cooling chips is directly attached to a metal heat sink, and the outer surface of the metal heat sink is provided with heat dissipation fins. A water-cooling circulation sleeve is provided outside the metal heat sink.

[0013] As another preferred embodiment of the present invention, the sensing control component includes a controller and a heat-conducting sleeve fixedly sleeved on one end of the observation tube. A temperature-sensing resistor is embedded on the surface of the heat-conducting sleeve, and thermally conductive adhesive is filled between the heat-conducting sleeve and the observation tube. The signal output terminal of the temperature-sensing resistor is connected to the signal input terminal of the controller through a wire, and the input terminals of the multiple sets of semiconductor cooling chips are connected to the output terminal of the controller through wires.

[0014] As another preferred embodiment of the present invention, a temperature sensor is installed on the metal heat sink, and the signal output terminal of the temperature sensor is connected to the signal input terminal of the controller through a wire.

[0015] As another preferred embodiment of the present invention, the inlet and outlet of the water-cooled circulation jacket are respectively connected to the circulating cooling water source through pipelines, and the pipelines are equipped with solenoid valves controlled by a controller for adjusting the cooling water flow rate.

[0016] As another preferred embodiment of the present invention, a stirring device is fixedly connected to the top of both the primary reactor and the secondary reactor, and the output shaft of the stirring device extends into the corresponding primary reactor and the secondary reactor to stir the materials in the tank.

[0017] The present invention has the following beneficial effects: 1. This invention integrates a two-stage distillation, condensation, and negative pressure system using a mounting frame, resulting in high equipment integration and a compact footprint. It achieves graded and progressive material purification through primary and secondary distillation units, achieving a purification accuracy superior to single-stage distillation. Furthermore, the dual independent condenser units allow for the transfer and reuse of gaseous materials from the primary distillation stage, separate collection of gaseous components from the secondary distillation stage, and full-area linkage of the two-stage distillation structure via vacuum negative pressure units. This unified negative pressure environment adapts to low-temperature negative pressure distillation conditions, reducing material loss due to high-temperature deterioration.

[0018] 2. By setting up a dedicated condensate return pipeline, this invention clarifies the technical path of using primary condensate as the sole raw material source for secondary distillation, thus avoiding raw material confusion. At the same time, it optimizes the structure of the cooling components, allowing the cold side of the semiconductor refrigeration chip to be directly coupled to the cooling pipe, while the hot side is cooled efficiently by a metal heat sink in conjunction with forced air cooling or water cooling, significantly improving cooling efficiency and stability.

[0019] 3. This invention achieves independent control of the negative pressure environment of the multi-stage distillation chamber by independently setting isolation valves on the negative pressure connecting pipelines of each tank, thereby improving process flexibility; and by arranging the temperature sensing element of the sensing and control components at the outlet end of the observation tube or the outlet end of the condenser, the real-time performance of temperature feedback and the accuracy of condensing power adjustment are significantly improved.

[0020] 4. By employing a staged temperature condensation control technology, the first condensation device is set to operate at 10℃~20℃ and the second condensation device is set to operate at 20℃~30℃, which can accurately separate components with different boiling points and improve product purity. At the same time, an independent collection device is set up and connected independently to the two-stage distillation device, which effectively avoids cross-contamination during the product collection process. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the structure of a staged condensation reflux two-stage distillation purification device provided in an embodiment of the present invention; Figure 2 This is a two-dimensional structural schematic diagram of the staged condensation reflux two-stage distillation purification device provided in an embodiment of the present invention; Figure 3 This is a schematic diagram of the sensing and control components of the staged condensation reflux two-stage distillation and purification equipment provided in an embodiment of the present invention; Figure 4 This is a schematic diagram of the cooling component of a staged condensation reflux two-stage distillation purification device provided in an embodiment of the present invention.

[0022] In the attached image: 100. Mounting frame; 101. Primary reactor; 102. Primary receiving tank; 103. Secondary reactor; 104. Secondary receiving tank; 105. Discharge pipe; 106. Sampling port; 107. Thermometer; 108. Liquid outlet pipe; 109. Liquid inlet pipe; 110. First conduit; 111. Second conduit; 112. Stirring device; 200. Discharge pipe; 201. Vacuum pipe; 202. Nitrogen pipe; 203. First connecting pipe; 204. Second connecting pipe; 205. Connecting pipe; 206. Vacuum pump; 300. Sensing and control components; 301. Observation tube; 302. Heat-conducting jacket; 303. Temperature sensing resistor; 400. Cooling component; 401. Cooling pipe; 402. Thermally conductive inner sleeve; 403. Semiconductor cooling chip; 404. Water-cooled circulation sleeve; 405. Temperature sensor; 406. Solenoid valve. Detailed Implementation

[0023] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0024] The accompanying drawings are for illustrative purposes only and are schematic diagrams, not actual images. They should not be construed as limiting the scope of this application. To better illustrate the embodiments of the present invention, some parts in the drawings may be omitted, enlarged, or reduced, and do not represent the actual dimensions of the product. It is understandable to those skilled in the art that some well-known structures and their descriptions may be omitted in the drawings.

[0025] In the accompanying drawings of the embodiments of the present invention, the same or similar reference numerals correspond to the same or similar components. In the description of the present invention, it should be understood that if terms such as "upper," "lower," "left," "right," "inner," and "outer" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, they are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, the terms used to describe positional relationships in the drawings are only for illustrative purposes and should not be construed as limiting the present application. For those skilled in the art, the specific meaning of the above terms can be understood according to the specific circumstances.

[0026] In the description of this invention, unless otherwise explicitly specified and limited, the term "connection" or similar designation indicating a connection between components should be interpreted broadly. For example, it can refer to a fixed connection, a detachable connection, or an integral part; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can refer to the internal communication between two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0027] Please see Figures 1-4 This embodiment provides a staged condenser reflux two-stage distillation purification device, including a mounting frame 100, a primary distillation unit, a secondary distillation unit, a condenser unit, a vacuum negative pressure unit, and a collection device.

[0028] The mounting frame 100 is fixedly installed on the ground; the primary distillation unit is installed on the upper part of the mounting frame 100 for primary distillation of raw materials; the secondary distillation unit is installed on the upper part of the mounting frame 100 and located below the primary distillation unit; the condenser has two sets and is respectively connected to the discharge ends of the primary distillation unit and the secondary distillation unit, wherein the condenser connected to the primary distillation unit is the first condensation device, which is set to operate at a first temperature and is used to condense and reflux the light components and products formed after the primary distillation unit processes the raw materials; the condenser connected to the secondary distillation unit is the second condensation device, which is set to operate at a second temperature and is used to condense the product and reflux it to the secondary distillation unit, and to allow the light components to pass through to enter the tail gas treatment tower; The output end of the condenser connected to the primary distillation unit is connected to the raw material input end of the secondary distillation unit through a dedicated condensate reflux pipeline (not shown in the figure), which is used to condense the light vapor components produced by the primary distillation unit as raw materials for the secondary distillation unit. The vacuum negative pressure unit is set above the mounting frame 100 to create a negative pressure environment in the primary and secondary distillation units. The collection device is located at the lower part of the mounting frame 100 and is independently connected to the primary and secondary distillation units. The collection device includes a collection box, which contains collection pipelines and collection tanks corresponding to the primary and secondary distillation units. The collection tanks are placed in the collection box, and the collection pipelines are used to connect the collection tanks to the primary and secondary distillation units.

[0029] Specifically, the primary distillation unit includes a primary reactor 101 and a primary receiving tank 102. The discharge end of the primary reactor 101 is connected to the feed end of the primary receiving tank 102 through a first conduit 110. The secondary distillation unit includes a secondary reactor 103 and a secondary receiving tank 104. The discharge end of the secondary reactor 103 is connected to the feed end of the secondary receiving tank 104 through a second conduit 111. The vacuum negative pressure unit includes a discharge pipe 200, a vacuum pipe 201, and a nitrogen pipe 202, all located above the mounting frame 100. The primary reactor 101, the primary receiving tank 102, the secondary reactor 103, and the secondary receiving tank 104 are connected to the nitrogen pipe 202 through a first connecting pipe 203. The primary reactor 101, the primary receiving tank 102, the secondary reactor 103, and the secondary receiving tank 104 are connected to the discharge pipe 200 through a second connecting pipe 204. Each connecting pipe is independently equipped with an isolation valve to achieve independent control of the negative pressure environment of each tank.

[0030] The condenser includes a cooling pipe 401 connected to the gas phase outlet of the primary receiving tank 102 and the secondary receiving tank 104. The output end of the cooling pipe 401 is connected to the discharge pipe 200. The middle part of each set of cooling pipes 401 is arranged in a spiral shape. The outer circumferential surface of the middle part of each set of cooling pipes 401 is provided with a cooling element 400 for cooling the middle part of the cooling pipe 401, thereby cooling the light components and products formed after processing raw materials to form a liquid state.

[0031] The cooling component 400 has the following structure: a heat-conducting inner sleeve 402 is fitted and tightly adhered to the outer circumferential surface of the middle part of the cooling pipe 401. Multiple sets of thermoelectric coolers 403 are embedded in the outer circumferential surface of the inner sleeve 402. The cold surfaces of the thermoelectric coolers 403 form a thermal conduction connection with the inner sleeve 402, ensuring efficient transfer of cooling energy to the cooling pipe 401. A metal heat sink (not shown in the figure, made of high thermal conductivity aluminum alloy or copper) is directly attached to the hot surface of each thermoelectric cooler 403. Heat dissipation fins are provided on the outer side of the metal heat sink, and a water-cooled circulation sleeve 404 is provided outside the metal heat sink. A forced-air cooling fan can also be installed outside the heat dissipation fins. The exhaust port of the forced-air cooling fan faces the heat dissipation fins, and the water-cooled circulation sleeve 404 removes heat through circulating cooling water. This design overcomes the poor heat dissipation defects of the original solution, ensuring that the thermoelectric coolers can operate stably for a long time and achieve precise graded temperature control.

[0032] Both the first conduit 110 and the second conduit 111 have observation tubes 301 connected in series at their middle sections. Each observation tube 301 has a sensing control element 300 on its outer circumferential surface for monitoring the temperature of the observation tube 301 and thus controlling the cooling component 400. To improve the real-time performance of temperature feedback, the temperature sensing element (temperature sensing resistor 303) of the sensing control element 300 is preferably located at the outlet end of the observation tube 301 or the outlet end of the condenser, rather than at the feed end, so as to more accurately reflect the true temperature state of the material entering the condensation stage.

[0033] The primary reactor 101 and the secondary reactor 103 are respectively connected to the inlet pipe 109 for connecting the heat source equipment and the outlet pipe 108 for returning the heat source equipment.

[0034] The input ends of both the first conduit 110 and the second conduit 111 are connected in series with a thermometer 107, which allows staff to intuitively monitor the feeding conditions.

[0035] The discharge ends of the primary reactor 101, primary receiving tank 102, secondary reactor 103, and secondary receiving tank 104 are all connected to discharge pipes 105. A key improvement is that the discharge pipe 105 in the primary receiving tank 102 is only used to discharge the heavy distillation waste liquid and is not connected to the secondary reactor 103; the condensate produced by the primary distillation is directly fed into the feed end of the secondary reactor 103 through the condensate reflux pipe, thereby avoiding raw material mixing and ensuring that the secondary distillation is a further purification of the primary distillate. Sampling ports 106 are connected in series at the output ends of the discharge pipes 105 in the primary reactor 101 and secondary reactor 103, and in the middle of the discharge pipes 105 in the primary receiving tank 102 and secondary receiving tank 104. Furthermore, a glove box is installed at each set of sampling ports 106 to allow for real-time sampling at each step. The qualified products from the secondary receiving tank 104 are sent to the corresponding collection tank in the collection device through the corresponding discharge pipe 105 and collection pipeline for storage. The intermediate products of primary distillation and different batches of products from secondary distillation are collected through independent collection pipelines and collection tanks to effectively prevent cross-contamination.

[0036] One end of the vacuum tube 201 is connected to the vacuum pump 206 via the connecting pipe 205. The output end of the vacuum pump 206 is connected to the discharge pipe 200, forming an integrated negative pressure air extraction passage.

[0037] The sensing and control unit 300 includes a controller (such as a Siemens S7-1200) and a heat-conducting sleeve 302 fixedly fitted onto the outlet end of the observation tube 301. A temperature-sensing resistor 303 is embedded in the surface of the heat-conducting sleeve 302, and thermally conductive adhesive is filled between the heat-conducting sleeve 302 and the observation tube 301. The signal output terminal of the temperature-sensing resistor 303 is connected to the signal input terminal of the controller via a wire, and the input terminals of multiple sets of thermoelectric coolers 403 are connected to the output terminal of the controller via wires. Based on the temperature signal collected by the temperature-sensing resistor 303 and a preset liquefaction temperature threshold, the controller adaptively adjusts the power supply current of the thermoelectric coolers 403, so that the first condensing device operates stably within a first temperature range of 10℃ to 20℃, and the second condensing device operates stably within a second temperature range of 20℃ to 30℃.

[0038] Each metal heat sink is equipped with a temperature sensor 405. The signal output of the temperature sensor 405 is connected to the signal input of the controller via a wire to monitor the heat sink temperature and prevent overheating. When the heat sink temperature exceeds a set value (e.g., 45°C), the controller automatically starts the forced air cooling fan or increases the cooling water flow of the water cooling circulation jacket 404. The inlet and outlet of the water cooling circulation jacket 404 are connected to the circulating cooling water source via pipes. A solenoid valve 406, controlled by the controller, is installed on the pipe to regulate the cooling water flow. The forced air cooling fan is also controlled by the controller via a relay. When the system detects an increase in the heat sink temperature, the controller automatically adjusts the cooling intensity to ensure that the hot surface temperature of the semiconductor cooling chip remains below 40°C, thereby achieving long-term reliable operation.

[0039] A stirring device 112 is fixedly connected to the top of both the primary reactor 101 and the secondary reactor 103. The output shaft of the stirring device 112 extends into the corresponding primary reactor 101 and secondary reactor 103 to stir the materials in the tanks and ensure the homogeneity of the materials.

[0040] Typical operating parameter range: Distillation temperature can be controlled between 30℃ and 150℃ depending on the material; system negative pressure is controlled between -0.05MPa and -0.095MPa (gauge pressure); the power supply voltage of the 403 semiconductor refrigeration chip is infinitely adjustable between 0 and 12V, corresponding to a cooling power of 0 to 72W. The operating temperature of the first condenser is stable between 10℃ and 20℃, the operating temperature of the second condenser is stable between 20℃ and 30℃, and the safe threshold for the ambient temperature of the cooling chamber is set between 18℃ and 22℃.

[0041] Furthermore, through the synergistic effect of the aforementioned structure and control methods, this invention achieves the following comprehensive technical effects: ① High integration – The primary distillation unit, secondary distillation unit, condenser, vacuum negative pressure unit, and collection device are compactly integrated using the mounting frame 100, resulting in a neat structure, small footprint, and ease of installation and maintenance; ② High purification accuracy – Two-stage fractional distillation combined with staged temperature condensation (10℃~20℃ and 20℃~30℃), along with a dedicated condensate reflux pipeline, allows the primary distillate to serve as the sole feedstock for secondary distillation, achieving stepwise separation of impurities and significantly higher product purity than single-stage distillation; ③ Good process flexibility – The negative pressure of each tank can be independently controlled, allowing for the setting of distillation pressures according to different material characteristics, and the condensation temperature can be set independently for each stage, adapting to the purification needs of various heat-sensitive materials. Therefore, this invention possesses outstanding comprehensive performance advantages in the field of distillation purification.

[0042] Specifically, in this embodiment, the refrigeration power of the first condensing device and the second condensing device satisfies the following relationship with the vapor load of the corresponding distillation stage: ; in, These represent the first condensing device and the second condensing device, respectively. For the first The total input electrical power of the semiconductor refrigeration unit in the stage condenser, in units of ; For the first The mass flow rate of the gaseous material entering the corresponding condenser from the discharge end of the first distillation unit, in units of... ; For the first The average isobaric specific heat capacity of the gaseous material within the condensation temperature range, in units of ; For the first The measured temperature of the gaseous material before it enters the condenser, in units of... ; For the first The set operating temperature of the stage condenser is in units of ; For the first The latent heat of phase change of a gaseous material at the condensation temperature, in units of... ; For the first The actual cooling efficiency (coefficient of performance) of the semiconductor refrigeration chip is dimensionless. For the first The heat exchange efficiency of the stage condenser is dimensionless. For the first Temperature fluctuation suppression power margin of the stage condenser, in units of Its value is a function of the integral of the temperature deviation within the sampling period of the sensing and control device 300: ; in, , For the first Temperature setpoint of the primary condenser unit The temperature sensing element of the sensing control unit 300 at any time Measured temperature value; , , These are the proportional, integral, and derivative control coefficients, respectively.

[0043] Parameter description table: This equipment is suitable for the distillation and purification of various thermosensitive metal organic or inorganic precursors (including but not limited to the Co precursors mentioned above). The following is a detailed explanation using cobalt hexacarbonyl (CCTBA) as an example.

[0044] Example: Taking the distillation and purification process of a thermosensitive organometallic precursor as an example, the following operating conditions are set: First-stage distillation (primary distillation): Target material: Crude cobalt hexacarbonyl (CCTBA); Temperature of the gas phase before entering the first condenser: (Right now The set temperature of the first condensing unit is: (Right now Gas phase mass flow rate: Average isobaric specific heat capacity of gas phase: Latent heat of phase transition: The cooling efficiency of a semiconductor thermoelectric cooler: ; Heat exchange efficiency of condensing unit: Basic cooling power calculation: .

[0045] Dynamic power margin calculation: Assuming the current measured temperature (Right now ), setting value ,but: Let the adjusted control coefficient be... , , The cumulative value of the integral term is The current value of the derivative term is ,but: Total input power of the thermoelectric cooler: .

[0046] The controller adjusts the input power of the thermoelectric cooler 403 accordingly. This causes the first condenser to return to near the set value; as the measured temperature gradually approaches the set value... Approaching 0, The cooling power is reduced accordingly, and the cooling power is automatically adjusted to the basic power level to achieve precise closed-loop temperature control.

[0047] The operating conditions for second-stage distillation (two-stage distillation) can be deduced similarly, only requiring the corresponding parameters to be replaced with the thermal properties of the secondary material. ( It can be calculated independently.

[0048] This equation and the control logic it relies on bring the following technical benefits to the device: (1) Precise matching of refrigeration power and real-time heat load: The condensation control of traditional distillation equipment mostly adopts simple PID regulation, which lacks a quantitative mapping relationship between refrigeration power and real-time heat load, often resulting in excessive refrigeration power (energy waste) or insufficient refrigeration power (insufficient condensation, light component breakthrough). This equation establishes a quantitative mapping relationship, which enables the refrigeration power to be precisely matched according to the real-time operating conditions, ensuring the condensation effect and avoiding unnecessary energy consumption.

[0049] (2) Significantly improves the real-time performance and control accuracy of temperature feedback: The temperature sensing element of the sensing control component 300 is located at the outlet end of the observation tube 301. At this location, the temperature of the feed liquid is transmitted to the core area, enabling early prediction of material temperature changes before the condensation stage. (The equation...) Based on the real-time temperature signal, the PID calculation enables the two-stage condenser to stably maintain within the preset temperature range for each stage. and The hysteresis effect of temperature control is greatly reduced.

[0050] (3) Achieving precise separation through staged temperature condensation: By applying this equation to the first and second condensing units respectively, the two condensing units can separate the components according to the thermophysical parameters of the materials they process ( , ) and operating temperature ( The required refrigeration power is calculated independently. This allows the light vapor components of the first-stage distillation to be processed in... High-efficiency condensation is used as the sole feedstock for secondary distillation, while the target product of secondary distillation is... The condensation reflux method ensures that the lighter components are not co-processed with the downstream feed, thus achieving precise separation of components with different boiling points.

[0051] (4) Adaptive suppression of operating condition fluctuations and enhanced system robustness: During the distillation process, changes in factors such as feed rate and temperature can lead to changes in gas phase load. and inlet temperature Fluctuations occur. In the equation... This technology enables the control system to automatically adjust the cooling power based on real-time temperature deviations, offsetting the impact of operating condition fluctuations and enhancing the system's robustness and process stability. It is especially suitable for applications where heat-sensitive materials are highly sensitive to temperature fluctuations.

[0052] (5) Optimize energy consumption structure and reduce operating costs: This equation keeps the input power of the thermoelectric cooler at a level close to the minimum required to meet condensation, avoiding the waste of electrical energy caused by excess power in traditional control methods. At the same time, the power margin term only generates additional power when there is a temperature deviation, and approaches zero in steady state, further improving the energy efficiency of the system.

[0053] Workflow: Based on the specific structure of this equipment, the workflow of this equation is as follows: Step 1: Parameter Initialization and Setting: Operators base their decisions on the physical properties of the target material. , Based on the requirements of the distillation process, the operating temperature of the first condenser is set accordingly. ( The operating temperature of the second condensing unit ( ), and the cooling efficiency of the semiconductor refrigeration chip. condensing unit heat exchange efficiency and the PID control coefficients obtained after tuning , , Input controller.

[0054] Step Two: Real-time Data Acquisition During equipment operation, the sensing and control unit 300 performs the following data acquisition tasks: The temperature sensing resistor 303 collects and observes the temperature at the outlet of the observation tube 301 in real time. This temperature is the temperature of the gaseous material before it enters the condenser. Real-time representation; Mass flow meters monitor the mass flow rate of gaseous materials entering each stage of the condensation unit. ; Temperature sensor 405 monitors the temperature of the metal heat sink to prevent overheating.

[0055] Step 3: Calculation of Temperature Deviation and Power Margin: The controller will measure the actual temperature With set temperature Compare and calculate the temperature deviation: Based on this, the power margin is calculated using the PID control law: ; Step 4: Calculation of base power and total power: The controller calculates the total heat power required for the condensation of gaseous materials: Then, combining the cooling efficiency and heat exchange efficiency, calculate the basic cooling power: Finally, the base power and the power margin are added together to obtain the total input power required by the thermoelectric cooler: .

[0056] Step 5: Power Output and Cooling Execution The controller adjusts the supply voltage of the thermoelectric cooler 403 based on the calculation results. (Stepless adjustment), so that the actual input power approaches the value. The cold side of the semiconductor cooling chip 403 cools the cooling pipe 401 through the heat-conducting inner sleeve 402, causing the gaseous material inside the spiral cooling pipe 401 to cool and liquefy; at the same time, the temperature sensor 405 monitors the temperature of the metal heat sink in real time, and when the temperature of the heat sink exceeds... At this time, the cooling fan automatically operates at full load to dissipate heat, ensuring that the temperature of the thermoelectric cooler remains below [temperature value missing]. This ensures its long-term reliable operation.

[0057] Step Six: Closed-Loop Iteration and Dynamic Adjustment Steps two through five are performed in each control cycle (typical value). The internal loop executes, forming a complete closed-loop control system of sensing, calculation, execution, and feedback. When the gas phase load... When it increases, rise, Automatically increases; when the measured temperature When it rises due to fluctuations, Automatically enlarges As the temperature increases synchronously, the controller automatically increases the cooling power. The two-stage condensing units independently execute the above process control, stabilizing within their respective stage temperature ranges, thereby achieving a highly efficient, precise, and stable staged condensation reflux two-stage distillation purification process.

[0058] In summary, the overall working principle of this invention is as follows: After the device is started, vacuum pump 206 draws air from inside vacuum tube 201 through connecting pipe 205, and simultaneously draws air from the discharge pipe 200 and each group of second connecting pipes 204, thereby drawing air from the internal cavities of primary reactor 101, primary receiving tank 102, secondary reactor 103, and secondary receiving tank 104, creating a negative pressure environment suitable for distillation operations within the two-stage distillation chambers. Each independent isolation valve can adjust the negative pressure level of each tank separately, achieving differentiated control.

[0059] The raw materials to be processed are fed into the primary reactor 101 and stirred evenly by the stirring device 112. Then, they are conveyed to the primary receiving tank 102 through the first conduit 110. The material undergoes primary distillation in the primary receiving tank 102, and the resulting gaseous light components enter the corresponding first condensation device (cooling pipe 401). The controller controls the current of the semiconductor cooling chip 403 to stabilize the first condensation device at 10℃~20℃, efficiently condensing the gaseous light components into a liquid. This condensate is directly sent to the secondary reactor 103 through a dedicated condensate return pipeline, serving as the sole feedstock for secondary distillation. The heavy component waste liquid at the bottom of the primary receiving tank 102 is periodically discharged through the discharge pipe 105 and does not enter the secondary distillation system.

[0060] After being stirred, the material in the secondary reactor 103 enters the secondary receiving tank 104 through the second conduit 111 to complete secondary distillation and further purification. The gaseous components produced by the secondary distillation enter the corresponding secondary condenser. The controller controls the current of the semiconductor refrigeration chip 403 to stabilize the secondary condenser at 20℃~30℃, causing the target product to condense and flow back to the secondary distillation unit for further purification. The lighter components with lower boiling points enter the tail gas treatment tower through the secondary condenser for further processing. The final high-purity qualified product is discharged through the discharge pipe 105 at the bottom of the secondary receiving tank 104 and sent to the corresponding collection tank in the collection device for storage via the collection pipeline.

[0061] The temperature-sensing resistor 303 of the sensing and control unit 300 is installed at the outlet end of the observation tube 301 to collect the temperature of the material about to enter the condensation stage in real time. This signal is several seconds to tens of seconds ahead of the temperature signal at the feed end. Based on this, the controller adjusts the power of the semiconductor refrigeration chip 403 in advance, significantly reducing the adjustment lag and ensuring that the two-stage condensation device can be stably maintained within the preset stage temperature range. At the same time, the temperature sensor 405 monitors the temperature of the metal heat sink. Based on this signal, the controller automatically starts or stops the forced air cooling fan or adjusts the cooling water flow of the water cooling circulation jacket 404 to ensure that the hot surface of the semiconductor refrigeration chip is always at a suitable temperature and to avoid overheating damage.

[0062] Through the above improvements, the entire system achieves a closed-loop distillation and purification process with clear material paths, precise staged temperature condensation, independent and pollution-free product collection, timely temperature feedback, independent and controllable negative pressure, and efficient cooling and heat dissipation.

[0063] The above are merely preferred embodiments of the present invention and are not intended to limit the implementation methods and protection scope of the present invention. Those skilled in the art should recognize that any equivalent substitutions and obvious changes made based on the description and illustrations of the present invention should be included within the protection scope of the present invention.

Claims

1. A staged condensation reflux two-stage distillation purification device, characterized in that, include: Mounting bracket (100), which is fixedly installed on the ground; A primary distillation unit is disposed on the upper part of the mounting frame (100), and the primary distillation unit is used for primary distillation of raw materials; A secondary distillation unit is disposed on the upper part of the mounting frame (100) and located below the primary distillation unit; The condenser has two sets of discharge ends connected to the primary distillation unit and the secondary distillation unit, respectively. The condenser connected to the primary distillation unit is a first condensation device, which operates at a first temperature and is used to condense and reflux the light components and products formed after processing the raw materials in the primary distillation unit. The condenser connected to the secondary distillation unit is a second condensation device, which operates at a second temperature and is used to condense the product and reflux it to the secondary distillation unit, and to allow the light components to pass through to enter the tail gas treatment tower. The output end of the condenser connected to the primary distillation unit is connected to the raw material input end of the secondary distillation unit through a dedicated condensate reflux pipeline, which is used to condense the gaseous light components generated in the primary distillation unit as the raw material for the secondary distillation unit. A vacuum negative pressure component is disposed above the mounting bracket (100) and is used to create a negative pressure environment in the primary distillation unit and the secondary distillation unit; A collection device is located at the lower part of the mounting frame (100) and is independently connected to the primary distillation element and the secondary distillation element. The collection device includes a collection box, and the collection box is provided with a collection pipeline and a collection tank corresponding to the primary distillation element and the secondary distillation element. The collection tank is placed in the collection box, and the collection pipeline is used to connect the collection tank to the primary distillation element and the secondary distillation element.

2. The staged condensation reflux two-stage distillation purification equipment according to claim 1, characterized in that, The first temperature ranges from 10°C to 20°C.

3. The staged condensation reflux two-stage distillation purification equipment according to claim 1, characterized in that, The second temperature range is 20°C to 30°C.

4. The staged condensation reflux two-stage distillation purification device according to claim 1, characterized in that, The primary distillation unit includes a primary reaction vessel (101) and a primary receiving tank (102). The discharge end of the primary reaction vessel (101) is connected to the inlet end of the primary receiving tank (102) through a first conduit (110). The secondary distillation unit includes a secondary reactor (103) and a secondary receiving tank (104). The discharge end of the secondary reactor (103) is connected to the inlet end of the secondary receiving tank (104) through a second conduit (111). The vacuum negative pressure component includes a discharge pipe (200) disposed above the mounting bracket (100), a vacuum pipe (201), and a nitrogen pipe (202). The primary reactor (101), the primary receiving tank (102), the secondary reactor (103), and the secondary receiving tank (104) are respectively connected to the nitrogen pipe (202) through the first connecting pipe (203). The primary reactor (101), the primary receiving tank (102), the secondary reactor (103), and the secondary receiving tank (104) are respectively connected to the discharge pipe (200) through the second connecting pipe (204). Each connecting pipe is independently equipped with an isolation valve to achieve independent control of the negative pressure environment of each tank. The condenser includes a cooling pipe (401) connected to the gas phase outlet of the primary receiving tank (102) and the secondary receiving tank (104). The output end of the cooling pipe (401) is connected to the discharge pipe (200). The middle part of each set of cooling pipes (401) is arranged in a spiral shape. The outer circumferential surface of the middle part of each set of cooling pipes (401) is provided with a cooling element (400) for cooling the middle part of the cooling pipe (401) to cool the light components and products formed after processing raw materials to form a liquid state. The cooling component (400) includes a heat-conducting inner sleeve (402) that is fitted and tightly attached to the outer peripheral surface of the middle part of the cooling pipe (401). Multiple sets of semiconductor cooling chips (403) are embedded in the outer peripheral surface of the heat-conducting inner sleeve (402). The cold surface of the semiconductor cooling chip (403) is thermally connected to the heat-conducting inner sleeve (402). The hot surface of each set of semiconductor cooling chips (403) is directly attached to a metal heat sink. The outer surface of the metal heat sink is provided with heat dissipation fins, and a water-cooling circulation sleeve (404) is provided outside the metal heat sink. The first conduit (110) and the second conduit (111) are connected in series with observation tubes (301) in the middle. Each observation tube (301) is provided with a sensing control element (300) on its outer circumferential surface for monitoring the temperature of the observation tube (301) and thus controlling the cooling element (400). The temperature sensing element of the sensing control element (300) is located at the outlet end of the observation tube (301) or the outlet end of the condenser to improve the real-time performance of temperature feedback.

5. The staged condensation reflux two-stage distillation purification device according to claim 4, characterized in that, The input ends of the first conduit (110) and the second conduit (111) are connected in series with a thermometer (107).

6. The staged condensation reflux two-stage distillation purification apparatus according to claim 4, characterized in that, The discharge ends of the primary reactor (101), primary receiving tank (102), secondary reactor (103), and secondary receiving tank (104) are all connected to discharge pipes (105). The discharge pipe (105) located in the primary receiving tank (102) is only used to discharge the waste liquid of the heavy components of distillation and is not connected to the secondary reactor (103). The condensate generated by the primary distillation is directly sent to the feed end of the secondary reactor (103) through the condensate return pipeline. Sampling ports (106) are connected in series at the output ends of the discharge pipes (105) of the primary reactor (101) and the secondary reactor (103) and in the middle of the discharge pipes (105) of the primary receiving tank (102) and the secondary receiving tank (104).

7. The staged condensation reflux two-stage distillation purification device according to claim 4, characterized in that, One end of the vacuum tube (201) is connected to a vacuum pump (206) via a connecting pipe (205), and the output end of the vacuum pump (206) is connected to the discharge pipe (200).

8. The staged condensation reflux two-stage distillation purification device according to claim 4, characterized in that, The sensing control unit (300) includes a controller and a heat-conducting sleeve (302) fixedly sleeved on one end of the observation tube (301). A temperature-sensing resistor (303) is embedded on the surface of the heat-conducting sleeve (302). Thermal conductive adhesive is filled between the heat-conducting sleeve (302) and the observation tube (301). The signal output terminal of the temperature-sensing resistor (303) is connected to the signal input terminal of the controller through a wire. The input terminals of multiple sets of semiconductor cooling chips (403) are connected to the output terminal of the controller through wires.

9. The staged condensation reflux two-stage distillation purification apparatus according to claim 8, characterized in that, A temperature sensor (405) is installed on the metal heat sink, and the signal output terminal of the temperature sensor (405) is connected to the signal input terminal of the controller through a wire.

10. The staged condensation reflux two-stage distillation purification apparatus according to claim 9, characterized in that, The inlet and outlet of the water-cooled circulation sleeve (404) are connected to the circulating cooling water source through pipelines. The pipelines are equipped with solenoid valves (406) controlled by the controller to regulate the cooling water flow. The forced air-cooled fan is controlled by the controller through a relay.

11. The staged condensation reflux two-stage distillation purification apparatus according to claim 4, characterized in that, A stirring device (112) is fixedly connected to the top of both the primary reactor (101) and the secondary reactor (103). The output shaft of the stirring device (112) extends into the corresponding primary reactor (101) and secondary reactor (103) to stir the materials in the tank.

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