Energy-saving germanium dioxide preparation rectifying device

Abstract

The application discloses energy-saving germanium dioxide preparation rectification device, including rectification tower, raw material storage tank, overhead condenser, plate heat exchanger, reboiler, tubular heat exchanger and man-machine interaction control cabinet, the top of rectification tower is connected with upper guide pipe, and the one end of upper guide pipe is connected with overhead condenser. Advantage: the application conducts the condensation heat released by overhead condenser to raw material storage tank through plate heat exchanger, preheats germanium dioxide crude liquid to be rectified from normal temperature to 60-70 DEG C, reduces the heating energy consumption of entering rectification tower, heats rectification reflux liquid by using the waste heat of tower kettle reboiler, makes the reflux liquid temperature rise to the vicinity of boiling point before entering tower body, reduces the heating load in tower, is different from the one-way energy loss mode of "heating-condensation" of prior art device, designs the closed loop heat exchange network of raw material preheating-rectification heating-condensation waste heat, realizes the cascade utilization of condensation heat and raw material preheating, reflux liquid heating, and the heat recovery efficiency is improved by more than 40%, so that the rectification energy consumption is significantly reduced.

Description

Technical Field

[0001] This invention relates to the field of germanium dioxide distillation, and more specifically, to an energy-saving germanium dioxide preparation distillation apparatus. Background Technology

[0002] Traditional distillation processes for germanium dioxide production suffer from two major problems: first, low energy utilization, as the heat of condensation released from the top condenser and the waste heat from the reboiler are directly discharged through the cooling system, resulting in approximately 30% of the total energy consumption being wasted; second, unstable mass transfer efficiency, with localized gas-liquid misalignment easily occurring after the feed enters the column due to flow rate fluctuations, affecting the separation accuracy of the packing layer, and traditional methods of manually adjusting the reflux ratio and heating power are slow to respond and difficult to match the dynamic changes in material composition. Furthermore, key components of existing equipment (such as airflow guiding structures and sensors) lack targeted protection designs, and long-term operation is prone to performance degradation due to wear and contamination, increasing maintenance costs. Currently, no effective solutions have been proposed to address these technical problems. Summary of the Invention

[0003] (a) Technical problems to be solved

[0004] To address the shortcomings of existing technologies, this invention provides an energy-saving distillation apparatus for the preparation of germanium dioxide, which has the advantages of cascaded waste heat recovery and utilization, low energy consumption, multi-layer composite packing to enhance the separation of low-concentration components, and dynamic energy consumption adaptation to material state, thereby solving the problems in the background technology mentioned above.

[0005] (II) Technical Solution

[0006] To achieve the advantages of cascaded waste heat recovery and utilization, low energy consumption, multi-layer composite packing for enhanced separation of low-concentration components, and dynamic energy consumption adaptation to material conditions, the specific technical solution adopted in this invention is as follows:

[0007] An energy-saving germanium dioxide preparation distillation apparatus includes a distillation column, a raw material storage tank, a top condenser, a plate heat exchanger, a reboiler, a tubular heat exchanger, and a human-machine interface control cabinet. The top of the distillation column is connected to an upper conduit, one end of which is connected to the top condenser. The condensation heat release end of the top condenser is connected to the plate heat exchanger via a pipe. A feed pipe is connected to the tube-side outlet flange of the plate heat exchanger, and a temperature sensor is installed on the surface of the feed pipe. A feed end is installed on the left side wall of the distillation column, and an airflow guide ring is embedded at the connection between the feed end and the distillation column. A raw material storage tank is located below the top condenser, and a feed pipe is connected to the bottom of the raw material storage tank. A feed pump and a regulating valve are installed sequentially from left to right on the surface of the feed pipe, and one end of the feed pipe is connected to the tube-side feed end of the plate heat exchanger via a flange. The feed pipe is connected to the raw material... One end of the storage tank is connected to the feed end. A lower guide pipe is installed at the bottom of the distillation column, and a reboiler is connected to the surface of the lower guide pipe via a pipe. The steam outlet of the reboiler is connected to the middle and lower part of the distillation column via a pipe. A reflux outlet is provided at the top of the distillation column, and a reflux pipe is connected to the reflux outlet via a flange. A reflux pump, a regulating valve two, and a tubular heat exchanger are installed sequentially on the surface of the reflux pipe. One end of the reflux pipe is connected to the connection position between the stripping section and the rectification section at the top of the distillation column. The waste heat discharge port of the reboiler is connected to the shell-side liquid inlet of the tubular heat exchanger via a pipe. A human-machine interface control cabinet is provided on the side of the distillation column, and a PLC controller is installed inside the human-machine interface control cabinet. The temperature sensor is electrically connected to the PLC controller, and the output terminal of the PLC controller is electrically connected to regulating valve one and regulating valve two.

[0008] Furthermore, a large-pore honeycomb ceramic packing is provided on the lower inner side of the distillation column, and a medium-pore metal corrugated packing is provided above the large-pore honeycomb ceramic packing. A small-pore porous polytetrafluoroethylene packing is provided above the medium-pore metal corrugated packing. The feed end is positioned opposite the large-pore honeycomb ceramic packing of the distillation column, and an airflow guide ring is installed at the connection between the feed end and the distillation column. The airflow guide ring is located on the side of the distillation column body, and the airflow guide ring corresponds to the edge position above the large-pore honeycomb ceramic packing. The inner ring of the airflow guide ring has a fan-shaped opening with a central angle of 30° along the circumferential direction. A servo motor is fixedly installed on the surface of the feed end, and a connecting ring is fixedly installed at the output end of the servo motor. A fan-shaped blade is welded and fixed to the outer ring of the connecting ring, and the fan-shaped blade is positioned corresponding to the fan-shaped opening of the airflow guide ring. The output end of the PLC controller is electrically connected to the servo motor.

[0009] Furthermore, a laser Raman concentration sensor is installed at the connection between the upper conduit and the top of the distillation column, and a column bottom density sensor is installed at the connection between the lower conduit and the bottom of the distillation column. The laser Raman concentration sensor and the column bottom density sensor are electrically connected to the PLC controller of the human-machine interface control cabinet, and the output terminal of the PLC controller is electrically connected to the reflux pump and the reboiler, respectively.

[0010] Furthermore, a rubber sealing ring is installed on the side of the fan-shaped blade facing the airflow guide ring, and the rubber sealing ring is in contact with the airflow guide ring. The surface area of ​​the fan-shaped blade is larger than the surface area of ​​the fan-shaped opening. Furthermore, the human-machine interface control cabinet integrates the core control circuit of the PLC, the power supply circuit, and the core module of the actuator drive circuit. The human-machine interface control cabinet is located 1.5-2 meters to the side of the distillation column, and a human-machine interface panel is embedded in the surface of the control cabinet. Furthermore, the large-pore honeycomb ceramic packing is located in the raw material inlet section of the distillation column, the medium-pore metal corrugated packing is located in the rectification section of the distillation column, and the small-pore porous polytetrafluoroethylene packing is located in the stripping section of the distillation column. Furthermore, the bottom of the raw material storage tank is provided with a germanium dioxide raw material inlet, and a tank cover is sealed at the germanium dioxide raw material inlet. Furthermore, the inner wall of the fan-shaped opening of the airflow guide ring is fitted with a wear-resistant ceramic liner, and the surface of the fan-shaped blades is coated with a polytetrafluoroethylene wear-resistant coating. The gap between the fan-shaped blades and the fan-shaped opening of the airflow guide ring is no greater than 0.5 mm. Furthermore, the interior wall of the distillation column is provided with a heat insulation layer made of aluminum silicate fiber material, with a thickness of 50-80 mm. The outer wall of the distillation column is wrapped with a metal protective shell, and an air insulation layer with a thickness of 10-15 mm is provided between the metal protective shell and the heat insulation layer.

[0011] Furthermore, both the laser Raman concentration sensor and the tower density sensor are equipped with dustproof protective covers. The dustproof protective covers are made of transparent polycarbonate material and have heat dissipation holes. Dustproof meshes are installed inside the heat dissipation holes. A sealing rubber ring is provided between the dustproof protective cover and the sensor mounting base.

[0012] (III) Beneficial Effects

[0013] Compared with the prior art, the present invention provides an energy-saving distillation apparatus for preparing germanium dioxide, which has the following beneficial effects:

[0014] (1) The present invention uses a plate heat exchanger to transfer the condensation heat released by the top condenser to the raw material storage tank, preheating the germanium dioxide crude liquid to be distilled from room temperature to 60-70°C, reducing the heating energy consumption entering the distillation column. The residual heat of the reboiler is used to heat the distillation reflux liquid, so that the reflux liquid is heated to near the boiling point before entering the column, reducing the heating load in the column. Unlike the existing device's "heating-condensation" unidirectional energy loss mode, the present invention designs a closed-loop heat exchange network of raw material preheating-distillation heating-condensation residual heat, realizing the cascade utilization of condensation heat and raw material preheating and reflux liquid heating, improving the heat recovery efficiency by more than 40%, thereby significantly reducing the distillation energy consumption.

[0015] (2) This invention forms a gradient pore composite packing by setting up large-pore honeycomb ceramic packing, medium-pore metal corrugated packing, and small-pore porous polytetrafluoroethylene packing. The large-pore honeycomb ceramic packing set in the lower part of the distillation column (raw material inlet section) is adapted to the higher flow rate of the preheated raw material liquid, reducing the initial flow resistance; the medium-pore metal corrugated packing is used in the middle part of the distillation column (rectification section) to increase the gas-liquid contact area; and the small-pore porous polytetrafluoroethylene packing is used in the upper part of the distillation column (stretching section) to enhance the separation of low-concentration components. At the same time, an airflow guide ring is set on the side of the column body, which automatically adjusts the ring gap opening (0-30°) according to the raw material temperature after preheating according to Scheme 1, avoiding local gas-liquid deviation. The gradient pores and adaptive airflow distribution solve the problem that existing packings with mostly single pore sizes cannot adapt to the flow rate changes after raw material preheating.

[0016] (3) This invention monitors the concentration of GeO2 in the distillate in real time by installing an online laser Raman sensor at the top of the column; and a density sensor is installed in the bottom of the column to detect changes in the density of the residual liquid. After the data is transmitted to the PLC control system, when the concentration is lower than the target value, the amount of waste heat recovery is increased to raise the preheating temperature of the raw material. When the mass transfer efficiency decreases, the opening of the airflow guide ring is expanded by 10-15° to optimize the airflow distribution. By adaptively adjusting the frequency of the reflux pump and the power of the reboiler, the reflux ratio is reduced to 1.5-2 when the concentration reaches the target, while the heating power is reduced. Unlike the existing technology, this invention uses real-time sensing and multi-system linkage to dynamically adapt energy consumption to the material state, thus solving the problem of ineffective energy consumption caused by the "fixed parameter operation" of the existing device. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1This is a schematic diagram of the overall structure of an energy-saving germanium dioxide distillation apparatus according to an embodiment of the present invention;

[0019] Figure 2 This is a schematic diagram of the internal structure of a distillation column;

[0020] Figure 3 This is a schematic diagram of the feed end structure;

[0021] Figure 4 It is a 3D diagram of a fan-shaped blade;

[0022] Figure 5 This is a heat exchange flow diagram of plate heat exchangers and tube heat exchangers;

[0023] Figure 6 This is a circuit block diagram for adjusting the annular gap opening;

[0024] Figure 7 This is a circuit block diagram of a linkage control system.

[0025] In the picture:

[0026] 1. Distillation column; 2. Upper conduit; 3. Lower conduit; 4. Raw material storage tank; 5. Top condenser; 6. Plate heat exchanger; 7. Reboiler; 8. Tubular heat exchanger; 9. Human-machine interface control cabinet; 10. Feed pipe; 11. Feed pump; 12. Reflux pipe; 13. Reflux pump; 14. Laser Raman concentration sensor; 15. Bottom density sensor; 16. Feed end; 17. Servo motor; 18. Feed pipe; 19. Temperature sensor; 20. Airflow guide ring; 21. Fan-shaped blade; 22. Large-pore honeycomb ceramic packing; 23. Medium-pore metal corrugated packing; 24. Small-pore porous polytetrafluoroethylene packing; 25. Reflux outlet; 26. Fan-shaped opening; 27. Rubber sealing ring; 28. Connecting ring; 29. ​​Control valve one; 30. Control valve two; 31. PLC controller. Detailed Implementation

[0027] To further illustrate the various embodiments, the present invention provides accompanying drawings, which are part of the disclosure of the present invention. These drawings are mainly used to illustrate the embodiments and can be used in conjunction with the relevant descriptions in the specification to explain the operating principles of the embodiments. With reference to these drawings, those skilled in the art should be able to understand other possible implementation methods and the advantages of the present invention. The components in the drawings are not drawn to scale, and similar component symbols are generally used to represent similar components.

[0028] According to an embodiment of the present invention, an energy-saving distillation apparatus for preparing germanium dioxide is provided.

[0029] The present invention will now be further described in conjunction with the accompanying drawings and specific embodiments. Please refer to the accompanying drawings for details. Figure 1 , Figure 2 , Figure 5and Figure 6As shown, the energy-saving germanium dioxide preparation distillation apparatus according to an embodiment of the present invention includes a distillation column 1, a raw material storage tank 4, a top condenser 5, a plate heat exchanger 6, a reboiler 7, a tubular heat exchanger 8, and a human-machine interface control cabinet 9. The top of the distillation column 1 is connected to an upper conduit 2, and one end of the upper conduit 2 is connected to the top condenser 5. The condensation heat release end of the top condenser 5 is connected to the plate heat exchanger 6 via a pipe. The tube-side outlet flange of the plate heat exchanger 6 is connected to a feed pipe 18, and a temperature sensor 19 is installed on the surface of the feed pipe 18. A feed end 16 is installed on the left side wall of the distillation column 1, and the feed end 16 communicates with the distillation column 1 at... An airflow guide ring 20 is embedded in the distillation column 1. A raw material storage tank 4 is located below the top condenser 5, and a feed pipe 10 is connected to the bottom of the raw material storage tank 4. A feed pump 11 and a regulating valve 29 are installed sequentially from left to right on the surface of the feed pipe 10. One end of the feed pipe 10 is connected to the tube-side feed end of the plate heat exchanger 6 via a flange, and the end of the feed pipe 18 furthest from the raw material storage tank 4 is connected to the feed end 16. A lower conduit 3 is installed at the bottom of the distillation column 1, and a reboiler 7 is connected to the surface of the lower conduit 3 via a pipe. The steam outlet of the reboiler 7 is connected to the lower middle part of the distillation column 1 via a pipe. A return valve is installed at the top of the distillation column 1. The distillation column 1 has a reflux outlet 25, and a reflux pipe 12 is flanged at the reflux outlet 25. A reflux pump 13, a regulating valve 30, and a tubular heat exchanger 8 are sequentially installed on the surface of the reflux pipe 12. One end of the reflux pipe 12 is connected to the junction of the stripping section and the rectification section at the top of the distillation column 1. The waste heat discharge port of the reboiler 7 is connected to the shell-side inlet of the tubular heat exchanger 8 via a pipe. A human-machine interface control cabinet 9 is installed on the side of the distillation column 1, and a PLC controller 31 is built into the control cabinet 9. A temperature sensor 19 is electrically connected to the PLC controller 31, and the output of the PLC controller 31 is connected to the regulating valve 30. 29 and regulating valve 2 are electrically connected. Raw material storage tank 4 is used to store the crude germanium dioxide liquid to be distilled. Its volume is designed according to the production scale and can generally meet the continuous feeding needs for 8-12 hours. The top condenser 5 adopts a shell-and-tube condensation structure, which can quickly condense the top vapor into liquid. The plate heat exchanger 6 is composed of multiple stainless steel heat exchange plates, which has the characteristics of high heat exchange efficiency and small footprint. The reboiler 7 is a horizontal heating structure, which can provide continuous heating power for the bottom material. The tubular heat exchanger 8 adopts a stainless steel tube bundle design, which is suitable for the recovery and utilization of high-temperature waste heat. The human-machine interface control cabinet 9 is the control center of the entire device. The top of the distillation column 1 is connected to the upper conduit 2, which is made of high-temperature resistant stainless steel. The diameter of the conduit is determined according to the top vapor flow rate. One end of the upper conduit 2 is connected to the top condenser 5, which is used to introduce the germanium dioxide-containing vapor generated at the top of the distillation column 1 into the top condenser 5 for condensation. The condensation heat release end of the condenser 5 at the top of the tower is connected to a plate heat exchanger 6 through a pipe. The outer layer of the pipe is wrapped with an insulation layer to reduce heat loss during the transmission process.The plate heat exchanger 6 has a feed pipe 18 connected to the outlet flange on the tube side. A high-pressure resistant gasket is used at the flange connection to ensure a tight seal. A temperature sensor 19, a PT100 platinum resistance temperature sensor, is installed on the surface of the feed pipe 18. This sensor has a measurement accuracy of ±0.5℃ and can monitor the temperature of the raw material after preheating by the plate heat exchanger 6 in real time. A feed end 16 is installed on the left side wall of the distillation column 1. The feed end 16 adopts a gradually expanding structure, allowing the raw material to enter the distillation column 1 more smoothly. An airflow guide ring 20 is embedded at the connection between the feed end 16 and the distillation column 1 to guide the flow direction of the raw material within the column. Below the top condenser 5, a raw material storage tank 4 is installed. The inner wall of the raw material storage tank 4 is coated with an anti-corrosion coating to prevent the crude germanium dioxide solution from corroding the tank. The bottom of the raw material storage tank 4 is connected to a feed pipe 10. From left to right, a feed pump 11 and a regulating valve 29 are installed on the surface of the feed pipe 10. The feed pump 11 is a stainless steel centrifugal pump with stable flow and moderate head. The regulating valve 29 is an electric regulating ball valve, which can accurately control the feed rate of the raw material through a PLC controller 31. One end of the feed pipe 10 is connected to the tube-side feed end of the plate heat exchanger 6 through a flange, and the end of the feed pipe 18 away from the raw material storage tank 4 is connected to the feed end 16, forming a complete conveying path for the raw material from the storage tank to the distillation column 1. A lower conduit 3 is installed at the bottom of the distillation column 1. The diameter of the lower conduit 3 is larger than that of the upper conduit 2 to meet the conveying requirements of the bottom material. The surface of the lower conduit 3 is connected to a reboiler 7 through a pipe to introduce the material in the bottom of the column into the reboiler 7 for heating. The steam outlet of reboiler 7 is connected to the lower middle part of distillation column 1 via a pipeline, allowing the steam generated by heating to re-enter distillation column 1 to participate in the mass transfer process. A reflux outlet 25 is provided at the top of distillation column 1. The location of the reflux outlet 25 is determined according to the division of the rectification and stripping sections within the column. A reflux pipe 12 is flanged at the reflux outlet 25. A reflux pump 13, a regulating valve 20, and a tubular heat exchanger 8 are sequentially installed on the surface of the reflux pipe 12. The reflux pump 13 is a variable frequency centrifugal pump, which can adjust the reflux flow rate as needed. The regulating valve 20 has the same structure as the regulating valve 29 and is used to precisely control the reflux volume. One end of the reflux pipe 12 is connected to the junction of the stripping and rectification sections at the top of distillation column 1, ensuring that the reflux accurately enters the corresponding packing section. The waste heat discharge port of reboiler 7 is connected to the shell-side inlet of tubular heat exchanger 8 via a pipeline, realizing the recovery and utilization of waste heat. A human-machine interface control cabinet 9 is installed on the side of the distillation column 1, and the human-machine interface control cabinet 9 has a built-in PLC controller 31. This controller adopts a high-performance industrial-grade PLC, which has the characteristics of fast calculation speed and strong anti-interference ability. The temperature sensor 19 is electrically connected to the PLC controller 31, transmitting the monitored temperature signal to the PLC controller 31 in real time. The output terminal of the PLC controller 31 is electrically connected to the regulating valve 29 and the regulating valve 30, and adjusts the valve opening according to the temperature signal and the preset program.

[0030] Please refer to Figure 2 and Figure 6The lower inner side of the distillation column 1 is provided with a large-pore honeycomb ceramic packing 22, and a medium-pore metal corrugated packing 23 is provided above the large-pore honeycomb ceramic packing 22. A small-pore porous polytetrafluoroethylene packing 24 is provided above the medium-pore metal corrugated packing 23. The feed end 16 is positioned opposite the large-pore honeycomb ceramic packing 22 of the distillation column 1, and an airflow guide ring 20 is installed at the connection between the feed end 16 and the distillation column 1. The airflow guide ring 20 is located on the side of the distillation column 1, and the airflow guide ring 20 corresponds to the upper edge position of the large-pore honeycomb ceramic packing 22. The inner ring of the airflow guide ring 20 has a fan-shaped opening 26 with a central angle of 30° along the circumferential direction. A servo motor 17 is fixedly installed on the surface of the feed end 16, and the servo motor 17 outputs... A fixed connecting ring 28 is provided at the outlet. A fan-shaped blade 21 is welded and fixed to the outer ring of the connecting ring 28. The fan-shaped blade 21 is set to correspond to the fan-shaped opening 26 of the airflow guide ring 20. The output end of the PLC controller 31 is electrically connected to the servo motor 17. A large-pore honeycomb ceramic packing 22 is provided in the lower inner part of the distillation column 1. The large-pore honeycomb ceramic packing 22 has the characteristics of high temperature resistance and corrosion resistance. Its pore size is 8-10mm, which can reduce the flow resistance when the raw material enters the column. A medium-pore metal corrugated packing 23 is provided above the large-pore honeycomb ceramic packing 22. The pore size of the medium-pore metal corrugated packing 23 is 4-6mm. It is made of stainless steel sheet and has a corrugated surface, which can increase the gas-liquid contact area and improve the mass transfer efficiency. Above the medium-pore metal corrugated packing 23, a small-pore porous polytetrafluoroethylene (PTFE) packing 24 is arranged. The pore size of the small-pore porous PTFE packing 24 is 2-3 mm, which has good chemical stability and surface non-stickiness, and is suitable for the separation of low-concentration components in the stripping section. The feed end 16 is set to correspond to the large-pore honeycomb ceramic packing 22 of the distillation column 1, so that the raw material can directly enter the packing layer for preliminary separation. An airflow guide ring 20 is installed at the connection between the feed end 16 and the distillation column 1. The airflow guide ring 20 is set on the side of the distillation column 1, and the airflow guide ring 20 corresponds to the edge position above the large-pore honeycomb ceramic packing 22. This ensures that the guided raw material is evenly distributed above the large-pore honeycomb ceramic packing 22. The inner ring of the airflow guide ring 20 has a fan-shaped opening 26 with a central angle of 30° along the circumference. The width of the fan-shaped opening 26 is designed according to the maximum flow rate of the raw material. A servo motor 17 is fixedly mounted on the surface of the feed end 16. The servo motor 17 is a high-precision servo drive motor with a control accuracy of up to 0.1°. The output end of the servo motor 17 is fixedly connected to a connecting ring 28. The connecting ring 28 is made of high-strength alloy material to ensure the stability of the transmission. A fan-shaped blade 21 is welded and fixed to the outer ring of the connecting ring 28. The material of the fan-shaped blade 21 is the same as that of the airflow guide ring 20. The fan-shaped blade 21 is set to correspond to the fan-shaped opening 26 of the airflow guide ring 20. The opening degree of the fan-shaped opening 26 can be adjusted by rotating the fan-shaped blade 21.The output of the PLC controller 31 is electrically connected to the servo motor 17. The PLC controller 31 controls the rotation angle of the servo motor 17 according to the received signal, thereby adjusting the opening of the fan-shaped opening 26.

[0031] Please refer to Figure 1 and Figure 7 A laser Raman concentration sensor 14 is installed at the connection between the upper conduit 2 and the top of the distillation column 1, and a column bottom density sensor 15 is installed at the connection between the lower conduit 3 and the bottom of the distillation column 1. The laser Raman concentration sensor 14 and the column bottom density sensor 15 are electrically connected to the PLC controller 31 of the human-machine interface control cabinet 9. The output terminals of the PLC controller 31 are electrically connected to the reflux pump 13 and the reboiler 7, respectively. The column bottom density sensor 15 is a differential pressure density sensor, which indirectly reflects the content of heavy components by measuring the density of the material in the column bottom, with a measurement accuracy of ±0.001 g / cm³. The laser Raman concentration sensor 14 and the column bottom density sensor 15 are electrically connected to the PLC controller 31 of the human-machine interface control cabinet 9, transmitting the detected concentration and density signals to the PLC controller 31 in real time. The output terminals of the PLC controller 31 are electrically connected to the reflux pump 13 and the reboiler 7, respectively. When the laser Raman concentration sensor 14 detects that the concentration of germanium dioxide in the distillate at the top of the column is lower than the set value, the PLC controller 31 will control the reflux pump 13 to increase the reflux flow rate. When the column bottom density sensor 15 detects that the density of the material in the column bottom exceeds the set range, the PLC controller 31 will adjust the heating power of the reboiler 7 to ensure that the material state in the column bottom is stable.

[0032] Please refer to Figure 2-4 A rubber sealing ring 27 is installed on the side of the fan-shaped blade 21 facing the airflow guide ring 20, and the rubber sealing ring 27 is in contact with the airflow guide ring 20. The surface area of ​​the fan-shaped blade 21 is larger than the surface area of ​​the fan-shaped opening 26. The rubber sealing ring 27 is made of oil-resistant and heat-resistant nitrile rubber, which has good elasticity and sealing performance, and can effectively prevent raw materials from leaking from the gap between the fan-shaped blade 21 and the airflow guide ring 20. In this way, when the fan-shaped blade 21 completely covers the fan-shaped opening 26, the opening can be completely closed, ensuring the sealing effect when raw materials are not needed. At the same time, it also provides sufficient adjustment margin for adjusting the opening degree. The PLC controller 31 converts the raw material preheating temperature (such as 60-70℃) into a fan-shaped blade 21 rotation angle command: for example, for every 1℃ increase in temperature, the corresponding fan-shaped blade 21 rotates 3° (i.e., the opening degree increases by 3°). When the raw material temperature reaches 70℃ (upper limit), the fan-shaped blade 21 rotates to the 30° fully open state; when the temperature drops to 60℃ (lower limit), the fan-shaped blade 21 returns to the 0° fully closed state, forming a linear adjustment relationship of "temperature-angle".

[0033] Please refer to Figure 1The human-machine interface control cabinet 9 integrates the core control circuit of PLC, the power supply circuit, and the core module of the actuator drive circuit. Located 1.5-2 meters to the side of the distillation column 1, the control cabinet 9 features an embedded human-machine interface panel. This integrated design reduces the complexity of circuit connections and improves system reliability. The 1.5-2 meter location ensures convenient operation and observation by operators while preventing the high temperature of the distillation column 1 from affecting the electronic components inside the cabinet. The embedded touchscreen control cabinet allows operators to set various process parameters, such as raw material preheating temperature, reflux ratio, and heating power. The panel also displays real-time operating status parameters of various components, such as temperature, pressure, flow rate, and concentration, facilitating monitoring and management of the system.

[0034] Please refer to Figure 2 Large-pore honeycomb ceramic packing 22 is located in the feed inlet section of distillation column 1, medium-pore metal corrugated packing 23 is located in the rectification section of distillation column 1, and small-pore porous polytetrafluoroethylene packing 24 is located in the stripping section of distillation column 1. The feed inlet section is the initial contact area after the feed enters the distillation column. The large-pore packing structure can adapt to the large flow rate of the feed and the possible impurities, reducing the risk of packing blockage. The rectification section is the key area for the initial separation of germanium dioxide components. The large specific surface area of ​​the medium-pore metal corrugated packing 23 can increase the contact opportunities between the gas and liquid phases and improve the separation efficiency. The stripping section mainly purifies the material separated in the rectification section. The small-pore packing structure can perform more fine separation of low-concentration germanium dioxide components, ensuring the purity of the final product. The three layers of packing are arranged sequentially in height, and a liquid redistributor is set between adjacent layers of packing to ensure that the liquid is evenly distributed to the surface of the lower packing layer, improving the overall mass transfer effect.

[0035] Please refer to Figure 1 The bottom of the raw material storage tank 4 is equipped with a germanium dioxide raw material inlet, and a tank cover is sealed at the germanium dioxide raw material inlet. The diameter of the germanium dioxide raw material inlet pipe is determined according to the outlet pipe diameter of the raw material conveying equipment. A sealing gasket is installed between the tank cover and the inlet to ensure the airtightness of the raw material storage tank 4, preventing the raw material from being contaminated by the outside world during storage, and also avoiding losses caused by raw material volatilization. The tank cover adopts a quick-opening structure, which facilitates the addition of raw materials and the cleaning and maintenance of the storage tank by operators.

[0036] Please refer to Figure 2-4The inner wall of the fan-shaped opening 26 of the airflow guide ring 20 is equipped with a wear-resistant ceramic liner, and the surface of the fan-shaped blade 21 is coated with a polytetrafluoroethylene (PTFE) wear-resistant coating. The gap between the fan-shaped blade 21 and the fan-shaped opening 26 of the airflow guide ring 20 is no greater than 0.5 mm. The wear-resistant ceramic liner and the PTFE wear-resistant coating are not shown in the figure. The wear-resistant ceramic liner is made of alumina ceramic material, which has extremely high hardness and wear resistance, and can withstand the scouring and wear caused by long-term material flow, thus extending the service life of the airflow guide ring 20. The PTFE coating not only has good wear resistance, but also has a low coefficient of friction, which can reduce the frictional resistance between the fan-shaped blade 21 and the airflow guide ring 20, making the blade rotate more smoothly. At the same time, it can also prevent the material from sticking to the blade surface. The gap between the fan-shaped blade 21 and the fan-shaped opening 26 of the airflow guide ring 20 is no greater than 0.5 mm. Such a small gap can ensure the accuracy of airflow guidance and avoid the formation of eddies in the gap, which would affect the guiding effect. The wear-resistant ceramic liner and the PTFE wear-resistant coating are not shown in the figure.

[0037] Please refer to Figure 1 and Figure 2 The distillation column 1 has an internal insulation layer made of aluminum silicate fiber material with a thickness of 50-80mm. The outer wall of the distillation column 1 is covered with a metal protective shell, and an air insulation layer with a thickness of 10-15mm is placed between the metal protective shell and the insulation layer. The insulation layer, metal protective shell, and air insulation layer are not shown in the figure. The insulation layer is made of aluminum silicate fiber material, which has the characteristics of low thermal conductivity and high temperature resistance, which can effectively reduce the heat loss in the distillation column 1 and ensure the stability of the temperature field inside the column. The thickness of the insulation layer is 50-80mm, which can ensure the insulation effect while avoiding the column body being too bulky. The metal protective shell is made of stainless steel, which can protect the internal insulation layer and prevent the insulation layer from being damaged by external impact. An air insulation layer, 10-15mm thick, is installed between the metal protective shell and the insulation layer. Air is a poor conductor of heat, and this air insulation layer further enhances the tower's insulation performance and reduces heat loss through the tower walls. Please refer to [reference needed]. Figure 1Both the laser Raman concentration sensor 14 and the tower density sensor 15 are equipped with dustproof protective covers. These covers are made of transparent polycarbonate material and have heat dissipation holes. Dustproof mesh is installed inside the heat dissipation holes. A sealing ring is provided between the dustproof protective cover and the sensor mounting base. (The dustproof protective cover itself is not shown in the figure.) The transparent polycarbonate material ensures that the sensor's detection optical path is not affected. Simultaneously, polycarbonate material has good mechanical strength and corrosion resistance, effectively protecting the sensor. The number and size of the heat dissipation holes are designed according to the sensor's heat dissipation requirements, effectively dissipating the heat generated during sensor operation and preventing excessive temperature from affecting the sensor's detection accuracy and lifespan. Dustproof mesh, made of metal wire mesh, is installed inside the heat dissipation holes to prevent external dust and impurities from entering the protective cover and contaminating the sensor. A sealing ring is installed between the dustproof protective cover and the sensor mounting base. The sealing ring is made of silicone rubber, which has good sealing performance and aging resistance, and can prevent moisture and dust from entering through the gap between the protective cover and the mounting base.

[0038] Working principle:

[0039] The crude germanium dioxide liquid in the raw material storage tank 4 is transported to the plate heat exchanger 6 by the feed pump 11, where it exchanges heat with the condensation heat of 80-120℃ released by the top condenser 5. After being preheated to 60-70℃, it enters the distillation column 1 through the feed end 16. Meanwhile, the waste heat generated by the reboiler 7 at 150-180℃ is introduced into the shell side of the tubular heat exchanger 8 through a pipeline to preheat the reflux liquid in the reflux liquid pipeline 12 (to near the boiling point), realizing the dual-loop energy recovery of "condensation heat - raw material preheating" and "residual heat in the reboiler - reflux liquid heating", reducing the basic heating load of the reboiler 7. When the raw material enters the tower body through the feed end 16, the airflow guide ring 20 drives the fan-shaped blades 21 to rotate through the servo motor 17. The opening degree of the fan-shaped opening 26 (0-30°) is adjusted according to the real-time data of the raw material inlet temperature sensor 19: when the temperature is too high (the flow rate is fast), the opening degree is increased to guide the material to diffuse evenly to the lower large-diameter honeycomb ceramic packing 22; when the temperature is too low (the flow rate is slow), the opening degree is decreased to avoid excessive airflow dispersion. The three-layer composite packing (large pore size at the bottom, medium pore size in the middle, and small pore size at the top) is adapted to the mass transfer requirements of the raw material inlet section, the rectification section, and the stripping section, respectively. It achieves efficient separation with uniform airflow. The laser Raman concentration sensor 14 at the top of the column monitors the distillate concentration in real time. The PLC controller adjusts the frequency of the reflux pump 13 and the opening of the regulating valve 2 30 according to the concentration deviation to dynamically optimize the reflux ratio. The regulating valve 1 29 can accurately control the feed rate of the raw material through the PLC controller 31. The column bottom density sensor 15 feeds back the residual liquid density and controls the heating power of the reboiler 7 to maintain a stable boiling state in the column bottom. The human-machine interface control cabinet 9 integrates all sensor signals and actuator commands, and realizes parameter setting and status monitoring through the touch screen.

[0040] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "setting," "connection," "fixing," "screw connection," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal connection of two components or the interaction between two components. Unless otherwise explicitly limited, those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0041] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. 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. An energy-saving distillation apparatus for preparing germanium dioxide, characterized in that, The system includes a distillation column (1), a raw material storage tank (4), a top condenser (5), a plate heat exchanger (6), a reboiler (7), a tubular heat exchanger (8), and a human-machine interface control cabinet (9). The top of the distillation column (1) is connected to an upper conduit (2), and one end of the upper conduit (2) is connected to the top condenser (5). The condensation heat release end of the top condenser (5) is connected to the plate heat exchanger (6) through a pipe. The tube side outlet flange of the plate heat exchanger (6) is connected to a feed pipe (18), and a temperature sensor (19) is installed on the surface of the feed pipe (18). The distillation column (1) has a feed end (16) installed on its left side wall, and an airflow guide ring (20) is embedded at the connection between the feed end (16) and the distillation column (1). A raw material storage tank (4) is provided below the top condenser (5), and a feed pipe (10) is connected to the bottom of the raw material storage tank (4). A feed pump (11) and a regulating valve (29) are installed on the surface of the feed pipe (10) from left to right. One end of the feed pipe (10) is connected to the tube side feed end of the plate heat exchanger (6) through a flange, and the feed pipe (18) is far away from the raw material storage tank. 4) One end is connected to the feed end (16). The bottom of the distillation column (1) is equipped with a lower conduit (3), and the surface of the lower conduit (3) is connected to a reboiler (7) through a pipe. The steam outlet of the reboiler (7) is connected to the middle and lower part of the distillation column (1) through a pipe. The upper part of the distillation column (1) is provided with a reflux outlet (25), and a reflux pipe (12) is connected to the reflux outlet (25) by a flange. The surface of the reflux pipe (12) is sequentially equipped with a reflux pump (13), a regulating valve (30), and a tubular heat exchanger (8). One end of the reflux pipe (12) is connected to the connection position between the stripping section and the rectification section of the upper part of the distillation column (1). The waste heat discharge port of the reboiler (7) is connected to the shell side inlet of the tubular heat exchanger (8) through a pipe. A human-machine interaction control cabinet (9) is provided on the side of the distillation column (1), and a PLC controller (31) is installed inside the human-machine interaction control cabinet (9). The temperature sensor (19) is electrically connected to the PLC controller (31). The output end of the PLC controller (31) is electrically connected to the regulating valve one (29) and the regulating valve two (30). The lower inner side of the distillation column (1) is provided with a large-pore honeycomb ceramic packing (22), and a medium-pore metal corrugated packing (23) is provided above the large-pore honeycomb ceramic packing (22). A small-pore porous polytetrafluoroethylene packing (24) is provided above the medium-pore metal corrugated packing (23). The feed end (16) is provided corresponding to the large-pore honeycomb ceramic packing (22) of the distillation column (1), and an airflow guide ring (20) is installed at the connection between the feed end (16) and the distillation column (1). The airflow guide ring (20) is provided on the side of the distillation column (1), and the airflow guide ring ( 20) Corresponding to the edge position above the large-pore honeycomb ceramic filler (22), the inner ring of the airflow guide ring (20) is opened with a fan-shaped opening (26) with a central angle of 30° along the circumferential direction. The surface of the feed end (16) is fixedly installed with a servo motor (17), and the output end of the servo motor (17) is fixedly connected to a connecting ring (28). The outer ring of the connecting ring (28) is welded and fixed with a fan-shaped blade (21), and the fan-shaped blade (21) is set to correspond to the fan-shaped opening (26) of the airflow guide ring (20). The output end of the PLC controller (31) is electrically connected to the servo motor (17). A laser Raman concentration sensor (14) is installed at the connection between the upper conduit (2) and the top of the distillation column (1), and a column bottom density sensor (15) is installed at the connection between the lower conduit (3) and the bottom of the distillation column (1). The laser Raman concentration sensor (14) and the column bottom density sensor (15) are electrically connected to the PLC controller (31) of the human-machine interface control cabinet (9). The output terminal of the PLC controller (31) is electrically connected to the reflux pump (13) and the reboiler (7) respectively. A rubber sealing ring (27) is installed on the side of the fan-shaped blade (21) facing the airflow guide ring (20), and the rubber sealing ring (27) is in contact with the airflow guide ring (20). The surface area of ​​the fan-shaped blade (21) is larger than the surface area of ​​the fan-shaped opening (26). The inner wall of the fan-shaped opening (26) of the airflow guide ring (20) is fitted with a wear-resistant ceramic liner, the surface of the fan-shaped blade (21) is coated with a polytetrafluoroethylene wear-resistant coating, and the gap between the fan-shaped blade (21) and the fan-shaped opening (26) of the airflow guide ring (20) is no greater than 0.5 mm.

2. The energy-saving germanium dioxide preparation distillation apparatus according to claim 1, characterized in that, The human-machine interaction control cabinet (9) integrates the core control circuit of PLC, the power supply circuit and the core module of the actuator drive circuit. The human-machine interaction control cabinet (9) is located 1.5-2 meters to the side of the distillation column (1), and a human-machine interaction panel is embedded in the surface of the human-machine interaction control cabinet (9).

3. The energy-saving germanium dioxide preparation distillation apparatus according to claim 1, characterized in that, The large-pore honeycomb ceramic packing (22) is located in the raw material inlet section of the distillation column (1), the medium-pore metal corrugated packing (23) is located in the rectification section of the distillation column (1), and the small-pore porous polytetrafluoroethylene packing (24) is located in the stripping section of the distillation column (1).

4. The energy-saving germanium dioxide preparation distillation apparatus according to claim 1, characterized in that, The bottom of the raw material storage tank (4) is provided with a germanium dioxide raw material inlet, and a tank cover is sealed at the germanium dioxide raw material inlet.

5. The energy-saving germanium dioxide preparation distillation apparatus according to claim 1, characterized in that, The distillation column (1) has an insulation layer inside its wall. The insulation layer is made of aluminum silicate fiber material and has a thickness of 50-80 mm. The outer wall of the distillation column (1) is wrapped with a metal protective shell. An air insulation layer is provided between the metal protective shell and the insulation layer. The thickness of the air insulation layer is 10-15 mm.

6. The energy-saving germanium dioxide preparation distillation apparatus according to claim 1, characterized in that, Both the laser Raman concentration sensor (14) and the tower density sensor (15) are equipped with dustproof protective covers. The dustproof protective covers are made of transparent polycarbonate material and have heat dissipation holes. Dustproof mesh is installed in the heat dissipation holes. A sealing ring is provided between the dustproof protective cover and the sensor mounting base.

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