A germanium tetrachloride short-process rectification and impurity fractional condensation coupled purification device

Abstract

This invention belongs to the field of germanium tetrachloride purification technology and discloses a short-process distillation and impurity fractionation coupled purification device for germanium tetrachloride. The device includes a reactor body, a distillation column body, a regulating valve, a mixing component detachably connected to the inner cavity of the reactor body, a temperature control component detachably connected to the inner cavity of the distillation column body, an atomizing component fixedly connected to the bottom of the temperature control component, and a mixing component detachably connected to the inner cavity of the distillation column body near the top. By coupling the chlorination reaction, distillation separation, and impurity fractionation into one unit, the gaseous product directly enters the middle of the distillation column from the top of the reactor. Within a single column, the vertical temperature gradient formed by the temperature control component and the selective fractionation effect of the atomizing component simultaneously complete distillation purification and the removal of high-boiling-point impurities (such as AsCl3), avoiding the risk of introducing impurities during material transfer and significantly reducing equipment investment costs and plant floor space.

Description

Technical Field

[0001] This invention belongs to the field of germanium tetrachloride purification technology, specifically a short-process distillation and impurity fractionation coupled purification device for germanium tetrachloride. Background Technology

[0002] Germanium tetrachloride (GeCl4) is a colorless liquid with a melting point of -49.5℃ (α-type) or -52℃ (β-type), a boiling point of 84.0℃, a relative density of 1.844330, and a refractive index of 1.464. It decomposes in water to produce germanium dioxide and hydrogen chloride. High-purity germanium tetrachloride is an indispensable key raw material for high-grade quartz-based optical fibers, used as a major dopant to improve the refractive index, reduce optical loss, and thus increase the transmission distance. Since the dopant is incorporated into the fiber core, its content and distribution determine important performance indicators of the fiber, and its quality directly affects whether a high-quality optical fiber can be obtained.

[0003] Patent CN114653085B discloses a germanium tetrachloride production apparatus and method. The apparatus includes: a feeding tank, a distillation mechanism, a rectification column, a discharge head, a first condenser, a second condenser, a pre-distillation tank, a sampling bottle, a third condenser, a product tank, an absorption bottle, a nitrogen distributor, a refrigeration unit, and a controller. The sampling bottle and product tank are connected in parallel, and the pipe connecting the sampling bottle to the discharge head and product tank is a U-shaped pipe. Based on the above apparatus, water in crude germanium tetrachloride is first dissociated, and then air and low-boiling-point impurities in the apparatus are removed to obtain germanium tetrachloride product. The germanium tetrachloride production apparatus and method of this invention are simple in process and convenient in operation. All steps can be completed in one production unit, and it can effectively remove impurities from germanium tetrachloride to obtain a high-purity product.

[0004] Although the purity of germanium tetrachloride can be improved by using multiple condensation stages such as the first condenser, second condenser, and third condenser, as well as multi-stage distillation, the equipment is lengthy, the reaction, condensation, and distillation are independent, the equipment investment is large, the area is large, and the material is transferred between multiple units, which poses risks of leakage, water absorption and hydrolysis, and secondary introduction of impurities. Summary of the Invention

[0005] To address the problems mentioned in the background art, the present invention provides a short-process distillation and impurity fractionation coupled purification device for germanium tetrachloride.

[0006] To achieve the above objectives, the present invention provides the following technical solution: a short-process distillation and impurity fractionation coupled purification device for germanium tetrachloride, comprising a reactor body, a distillation column body, and a regulating valve, wherein the distillation column body and the reactor body are connected by a pipeline, and the regulating valve is detachably connected to the side wall of the pipeline, and further comprising:

[0007] A mixing component, which is detachably connected to the inner cavity of the reactor body;

[0008] Temperature control components are detachably connected to the internal cavity of the distillation column body;

[0009] The atomizing component is fixedly connected to the bottom of the temperature control component;

[0010] A mixing assembly, which is detachably connected to the inner cavity of the distillation column near the top;

[0011] The mixing component includes a stirring assembly, a lifting rod, a connecting ring, a driving component, and a mounting plate. One end of the stirring assembly penetrates the bottom wall of the reactor body. The lifting rod is fixedly connected to the bottom end of the stirring assembly. The connecting ring is fixedly connected to the outer side wall of the lifting rod. The driving component is detachably connected to the connecting ring. The side wall of the driving component is detachably connected to the mounting plate, which is L-shaped.

[0012] Preferably, the stirring assembly includes a drive motor, a connecting rod, a sleeve, and a stirring rod. The drive motor is detachably connected to the top of the reactor body. The connecting rod is fixedly connected to the output end of the drive motor and is inserted into the inner cavity of the reactor body. The sleeve is nested on the outer wall of the connecting rod. The inner wall of the sleeve has multiple sliding grooves. The connecting rod slides relative to the multiple sliding grooves. The stirring rod is rotatably connected to the outer wall of the sleeve.

[0013] Preferably, the driving component includes an eccentric shaft and a second driving motor. One end of the eccentric shaft is fixedly connected to a connecting ring, and the output end of the second driving motor is fixedly connected to the end of the eccentric shaft away from the connecting ring. The second driving motor is detachably connected to the side wall of the mounting plate.

[0014] Preferably, the mixing component includes a fixed plate, a drive motor, and multiple fan blades. The fixed plate is detachably connected to the inner cavity of the distillation column body, and multiple vent holes are provided in the fixed plate. The drive motor is detachably connected to the top of the fixed plate, and the multiple fan blades are fixedly connected to the output end of the drive motor.

[0015] Preferably, the atomizing assembly includes a disassembly plate and multiple atomizing nozzles. The disassembly plate is detachably connected to the inner wall of the distillation column body, and multiple mounting holes are provided in the disassembly plate. The multiple atomizing nozzles are detachably connected to the multiple mounting holes, and the bottom ends of the multiple atomizing nozzles are inserted into the disassembly plate.

[0016] Preferably, the disassembly plate is hollow and has multiple ventilation holes arranged in a circular array with the central axis of the disassembly plate as the reference axis.

[0017] Preferably, the temperature control component includes a gyroscope and a connecting pipe. One end of the gyroscope passes through the side wall of the distillation column body, and the other end of the gyroscope is inserted into the inner cavity of the distillation column body. One end of the connecting pipe is inserted into the inner cavity of the disassembly plate, and the other end of the connecting pipe is fixedly connected to the end of the gyroscope inserted into the inner cavity of the distillation column body.

[0018] Preferably, a water pump is detachably connected to one end of the connecting pipe that extends to the outside of the distillation column body, and a storage tank is detachably connected to the water inlet end of the water pump.

[0019] Preferably, the distillation column body has an air inlet on its side wall, which is located below the disassembly plate, and an air outlet at the top of the distillation column body.

[0020] Preferably, a jacket is fixedly connected to the outer wall of the reactor body, a discharge port is opened on one side of the bottom end of the reactor body and the discharge port passes through the jacket, a water inlet is opened on one side of the jacket near the top of the reactor body, a water outlet is opened at the bottom end of the jacket, and multiple support legs are fixedly connected to the bottom end of the jacket.

[0021] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0022] By coupling the chlorination reaction, distillation separation, and impurity fractionation into a single process, the gaseous product enters directly from the top of the reactor into the middle of the distillation column. Within a single column, the vertical temperature gradient created by the temperature control components and the selective fractionation effect of the atomizing components simultaneously complete distillation purification and the removal of high-boiling-point impurities (such as AsCl3). This "short-process" design eliminates the need for repeated material transfers between multi-stage condensers, pre-distillation tanks, and product tanks, avoiding the risks of leakage, water absorption and hydrolysis, and secondary introduction of impurities due to poor sealing during material transfer. It also significantly reduces equipment investment costs and plant footprint. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of the overall structure of the present invention;

[0024] Figure 2 This is a schematic cross-sectional view of the overall structure of the present invention;

[0025] Figure 3 This is a schematic diagram of the reactor body assembly of the present invention;

[0026] Figure 4 for Figure 3 Enlarged view of point a shown;

[0027] Figure 5 This is a schematic diagram of the internal structure of the distillation column body of the present invention;

[0028] Figure 6 This is a schematic diagram of the atomizing component structure of the present invention;

[0029] Figure 7 This is a schematic diagram of the temperature control component structure of the present invention.

[0030] In the picture:

[0031] 100. Reactor body; 110. Jacket; 120. Discharge port; 130. Inlet; 140. Outlet; 150. Support leg;

[0032] 200. Distillation column body; 210. Gas inlet; 220. Gas outlet;

[0033] 300. Control valve;

[0034] 400. Mixing component; 410. Stirring assembly; 411. Drive motor one; 412. Connecting rod; 413. Sleeve; 414. Stirring rod; 420. Lifting rod; 430. Connecting ring; 440. Drive component; 441. Eccentric shaft; 442. Drive motor two; 450. Mounting plate;

[0035] 500. Temperature control component; 510. Rotary tube; 520. Connecting pipe; 530. Water pump; 540. Storage tank;

[0036] 600. Atomizing assembly; 610. Disassembly plate; 620. Atomizing nozzle;

[0037] 700. Hybrid component; 710. Fixing plate; 720. Drive motor three; 730. Fan blade. Detailed Implementation

[0038] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0039] like Figures 1 to 7 As shown, this invention provides a short-process distillation and impurity fractionation coupled purification device for germanium tetrachloride. The device includes a reactor body 100, a distillation column body 200, and a regulating valve 300. The distillation column body 200 and the reactor body 100 are connected by a pipeline. The regulating valve 300 is detachably connected to the side wall of the pipeline and is used to regulate pressure and temperature. The device also includes:

[0040] The mixing component 400 is detachably connected to the inner cavity of the reactor body 100;

[0041] Temperature control component 500, which is detachably connected to the inner cavity of distillation column body 200;

[0042] Atomizing component 600 is fixedly connected to the bottom of temperature control component 500;

[0043] Mixing component 700 is detachably connected to the inner cavity of distillation column body 200 near the top;

[0044] The mixing component 400 includes a stirring assembly 410, a lifting rod 420, a connecting ring 430, a driving component 440, and a mounting plate 450. One end of the stirring assembly 410 penetrates the bottom wall of the reactor body 100. The lifting rod 420 is fixedly connected to the bottom end of the stirring assembly 410. The connecting ring 430 is fixedly connected to the outer side wall of the lifting rod 420. The driving component 440 is detachably connected to the connecting ring 430. The side wall of the driving component 440 is detachably connected to the mounting plate 450, which is arranged in an "L" shape.

[0045] It should be noted that the mixing component 400 achieves vertical lifting and stirring motion within the reactor body 100 through the linkage of the stirring assembly 410 and the driving component 440. The driving component 440 drives the connecting ring 430 to move up and down via the eccentric shaft 441. The connecting ring 430 is fixedly connected to the lifting rod 420, thereby causing the lifting rod 420 to drive the stirring assembly 410 to move up and down within the reactor; causing the stirring rod 414 to undergo random disturbances on top of its revolution. This composite motion can effectively break the stagnant layer at the gas-liquid-solid three-phase interface in the chlorination reaction, enhance the mass transfer efficiency between chlorine and germanium-containing raw materials, and especially during gradient chlorine pressure switching (transition from the low-pressure section 0.1-0.2MPa to the high-pressure section 0.4-0.6MPa), it can rapidly disperse fresh chlorine to the reaction front, suppress the local over-concentration of AsCl3, and reduce the introduction of impurities into the distillation system from the source.

[0046] like Figure 2 , Figure 3 and Figure 4 As shown, the stirring assembly 410 includes a drive motor 411, a connecting rod 412, a sleeve 413, and a stirring rod 414. The drive motor 411 is detachably connected to the top of the reactor body 100. The connecting rod 412 is fixedly connected to the output end of the drive motor 411 and is inserted into the inner cavity of the reactor body 100. The sleeve 413 is nested in the outer wall of the connecting rod 412. The inner wall of the sleeve 413 is provided with multiple sliding grooves. The connecting rod 412 slides relative to the multiple sliding grooves. The stirring rod 414 is rotatably connected to the outer wall of the sleeve 413.

[0047] It should be noted that multiple grooves on the inner wall of the sleeve 413 form a sliding guide fit with the connecting rod 412, allowing the sleeve 413 and the stirring rod 414 to slide freely along the axial direction of the connecting rod 412 while rotating with it. This sliding freedom is driven by the extension and retraction of the lifting rod 420, enabling continuous lifting and stirring of the stirring rod 414 within the reactor. The stirring rod 414 is rotatably connected to the outer wall of the sleeve 413 and can passively rotate around a horizontal axis during stirring, producing a shear-type dispersion effect. This is particularly suitable for mixing high-viscosity slurries (containing unreacted solid phases), avoiding incomplete chlorination caused by solid settling to the bottom, and reducing the local accumulation of impurities (such as AsCl3) in the stirring dead zone.

[0048] like Figure 2 , Figure 3 and Figure 4 As shown, the drive unit 440 includes an eccentric shaft 441 and a second drive motor 442. One end of the eccentric shaft 441 is fixedly connected to the connecting ring 430. The output end of the second drive motor 442 is fixedly connected to the end of the eccentric shaft 441 away from the connecting ring 430. The second drive motor 442 is detachably connected to the side wall of the mounting plate 450.

[0049] It should be noted that the drive component 440 converts the rotational motion of the drive motor 442 into periodic radial vibration of the connecting ring 430 via the eccentric shaft 441. This vibration frequency is 5-20 Hz, and the amplitude is 2-8 mm. When the vibration is transmitted to the stirring rod 414, the stirring rod 414 generates microscale turbulent pulsations in the liquid phase, significantly enhancing the breaking and redispersing effect of chlorine bubbles, reducing the average bubble diameter from 5-8 mm to 1-2 mm, and increasing the gas-liquid contact area by more than four times. This enhanced mass transfer effect is particularly crucial in the high-pressure section, promoting the deep chlorination conversion of AsCl3 to AsCl5, causing more arsenic impurities to remain at the bottom of the reactor as high-boiling-point residue, and reducing the AsCl3 content in the gas phase entering the distillation column.

[0050] like Figure 5 As shown, the mixing component 700 includes a fixed plate 710, a drive motor 720, and multiple blades 730. The fixed plate 710 is detachably connected to the inner cavity of the distillation column body 200. Multiple vent holes are provided in the fixed plate 710. The drive motor 720 is detachably connected to the top of the fixed plate 710. The multiple blades 730 are fixedly connected to the output end of the drive motor 720.

[0051] It should be noted that the mixing component 700 is located near the top of the distillation column body 200, above the atomizing component 600. Its function is to forcibly mix the rising vapor with part of the reflux liquid from the condensation section, forming sufficient contact between the gas and liquid phases. The drive motor 720 drives the fan blades 730 to rotate (100-300 rpm), generating local negative pressure and turbulence near the vent hole 1 on the fixed plate 710, breaking up any gas-liquid stratification or wall flow phenomena that may occur in the distillation column. This forced mixing effect can effectively increase the number of theoretical plates by 1-2 stages, enabling the rectification section to achieve the separation effect of a traditional 8-10 plate stage with only 4-6 actual plate stages. It is a key auxiliary unit for achieving high-purity purification in a "short process".

[0052] like Figure 6 As shown, the atomizing assembly 600 includes a disassembly plate 610 and multiple atomizing nozzles 620. The disassembly plate 610 is detachably connected to the inner wall of the distillation column body 200, and multiple mounting holes are provided in the disassembly plate 610. The multiple atomizing nozzles 620 are detachably connected to the multiple mounting holes, and the bottom ends of the multiple atomizing nozzles 620 are inserted into the disassembly plate 610.

[0053] It should be noted that the atomizing component 600 is used to spray the cooling medium (ethylene glycol aqueous solution, 50-70℃) from the temperature control component 500 into the inner cavity of the distillation column body 200 in the form of fine droplets. The atomizing nozzle 620 has an orifice diameter of 0.2-0.5mm, an operating pressure of 0.3-0.6MPa, and produces droplet sizes of 50-150μm. Compared with traditional coil or jacket cooling 110, this atomization method has the advantages of large heat exchange area, fast response speed, and uniform temperature distribution. More importantly, the droplets can selectively condense high-boiling-point components (such as AsCl3, boiling point 130.2℃) in the rising vapor, while the condensation efficiency for low-boiling-point GeCl4 (boiling point 83.1℃) is extremely low, thus achieving "selective fractional condensation". The bottom end of the atomizing nozzle 620 is inserted into the disassembly plate 610, which facilitates the uniform acquisition of cooling medium from the cavity of the disassembly plate 610.

[0054] The disassembly plate 610 is hollow, and multiple ventilation holes are provided inside the disassembly plate 610. The multiple ventilation holes are arranged in a circular array with the central axis of the disassembly plate 610 as the reference axis.

[0055] It should be noted that the hollow cavity of the disassembly plate 610 serves as a distribution chamber for the cooling medium, ensuring consistent medium pressure entering each atomizing nozzle 620 and guaranteeing atomization uniformity. Multiple vent holes are arranged in a circumferential array, with their total opening area accounting for 30%-50% of the area of ​​the disassembly plate 610. This ensures that rising steam can smoothly pass through the disassembly plate 610 and contact the atomization zone, while avoiding excessive pressure drop. This structural design allows the atomizing assembly 600 to also function as a gas distributor, uniformly guiding rising steam to the working area of ​​each atomizing nozzle 620, preventing "short-circuit flow" or "deviation flow," and ensuring the stability of the condensation efficiency.

[0056] like Figure 7 As shown, the temperature control assembly 500 includes a gyroscope 510 and a connecting pipe 520. One end of the gyroscope 510 passes through the side wall of the distillation column body 200, and the other end of the gyroscope 510 is inserted into the inner cavity of the distillation column body 200. One end of the connecting pipe 520 is inserted into the inner cavity of the disassembly plate 610, and the other end of the connecting pipe 520 is fixedly connected to the end of the gyroscope 510 inserted into the inner cavity of the distillation column body 200.

[0057] A water pump 530 is detachably connected to one end of the connecting pipe 520 that extends to the outside of the distillation column body 200. A storage tank 540 is detachably connected to the water inlet end of the water pump 530.

[0058] It should be noted that the temperature control component 500 forms a dual-path temperature control loop through the gyroscope 510 and the connecting pipe 520. The gyroscope 510 is coiled around the outside or inner wall of the distillation column body 200, used for overall temperature control of the rectification section (82-85℃). The connecting pipe 520 delivers the temperature-regulated cooling medium to the cavity of the disassembly plate 610, and then sprays it out through the atomizing nozzle 620, achieving localized gradient cooling of the condensation section (50-70℃). The gyroscope 510 and the connecting pipe 520 share the same water pump 530 and storage tank 540, but the flow rate and temperature of the two media can be independently adjusted through the branch flow distribution valve, thereby forming a controllable vertical temperature gradient (colder at the top and hotter at the bottom) within the distillation column. This gradient is the basis for achieving the temperature control of the "distillation-condensation" functional zoning and coordination.

[0059] The distillation column body 200 has an air inlet 210 on its side wall, which is located below the disassembly plate 610. The distillation column body 200 has an air outlet 220 at its top.

[0060] It should be noted that the inlet 210 is located below the disassembly plate 610, that is, below the atomizing component 600 and in the upper middle part of the rectification section. The gaseous product (mainly containing GeCl4, trace amounts of AsCl3 and light components) from the reactor body 100 is depressurized by the regulating valve 300 and then enters the rectification column through the inlet 210. This inlet position is optimized to avoid direct gas impact on the atomizing zone causing liquid entrainment, while ensuring sufficient gas-liquid contact height for the rising vapor in the rectification section. The outlet 220 is located at the top of the column, producing high-purity GeCl4 vapor (purity 6N-7N), which is collected by an external condenser as the product. This "direct gas-phase connection - middle feed - top discharge" process design is one of the core paths of short-process coupled purification.

[0061] A jacket 110 is fixedly connected to the outer wall of the reactor body 100. A discharge port 120 is opened on one side of the bottom end of the reactor body 100 and the discharge port 120 passes through the jacket 110. A water inlet 130 is opened on one side of the jacket 110 near the top of the reactor body 100. A water outlet 140 is opened at the bottom end of the jacket 110. Multiple support legs 150 are fixedly connected to the bottom end of the jacket 110.

[0062] It should be noted that the jacket 110 is used for temperature control of the reactor body 100. Heat transfer oil or hot water (80-100℃) is introduced through the inlet 130 to maintain the suitable temperature (85-95℃) required for the chlorination reaction. The outlet 140 is located at the bottom for easy discharge of condensate or heat transfer medium. The discharge port 120 is installed through the jacket 110 to discharge residues (including unreacted carbon powder, high-boiling-point AsCl5 complexes, metal chlorides, etc.) from the bottom of the reactor. Multiple support legs 150 elevate the entire device for easy discharge operations and maintenance. This jacket 110 structure works in conjunction with the mixing components 400 inside the reactor to provide a stable thermal environment during gradient chlorination pressure switching, ensuring consistent chlorination reaction kinetics and preventing changes in impurity formation behavior due to temperature fluctuations.

[0063] Working principle and usage process of this invention:

[0064] I. Working Principle

[0065] Inside the reactor, the mixing component 400 breaks chlorine bubbles to the micron level through the combined motion of rotation, lifting, and vibration of the stirring rod 414, enhancing the gas-liquid-solid three-phase mass transfer and promoting the deep chlorination of the byproduct AsCl3 into high-boiling-point AsCl5 residue, thus reducing arsenic impurities from entering the gas phase at the source. Subsequently, the gas phase product enters the distillation column, where the temperature gradient formed by the temperature control component 500 (cooler at the top and hotter at the bottom) is combined with the selective condensation of high-boiling-point AsCl3 by the fine droplets sprayed by the atomizing component 600. At the same time, the mixing component 700 forces turbulent contact between the gas and liquid phases to increase the number of theoretical plates, thereby achieving efficient separation and purification of GeCl4 and impurities in a short process within a single column.

[0066] II. Usage Procedure

[0067] Step 1: Preparation

[0068] Check that all components are securely connected and that the regulating valve 300, water pump 530, drive motor 1 411, drive motor 2 442, and drive motor 3 720 are functioning properly.

[0069] Inject sufficient cooling medium (ethylene glycol aqueous solution, 50-70℃) into storage tank 540, turn on water pump 530 and adjust branch flow distribution valve to ensure that medium flows through rotary tube 510 and connecting pipe 520.

[0070] Introduce 80-100℃ heat transfer oil or hot water into the inlet 130 of the jacket 110 to preheat the reactor body to 100-85-95℃.

[0071] Germanium-containing raw materials (mixed with carbon powder in proportion) are loaded into the inner cavity of reactor body 100.

[0072] Step 2: Chlorination reaction and mixing components 400 operation

[0073] Start drive motor 411, which drives sleeve 413 and stirring rod 414 to rotate via connecting rod 412; simultaneously start drive motor 442, which drives sleeve 413 and stirring rod 414 to reciprocate up and down along the axis of connecting rod 412 via connecting ring 430 and lifting rod 420 (frequency 5-20Hz, amplitude 2-8mm). The stirring rod 414 passively rotates in the liquid phase, producing a shear dispersion effect.

[0074] Introduce chlorine gas and operate in a gradient pressurization mode: first maintain the low-pressure section (0.1-0.2 MPa) for 10-20 minutes, then switch to the high-pressure section (0.4-0.6 MPa) and continue the reaction for 20-30 minutes. During this process, chlorine gas bubbles are broken down to 1-2 mm, and AsCl3 is deeply chlorinated and converted into AsCl5 residue.

[0075] The gaseous products generated by the reaction (GeCl4, trace amounts of AsCl3 and light components) gather upwards and enter the distillation column from the top of the reactor after being depressurized by the regulating valve 300.

[0076] Step 3: Coupled purification of distillation and fractionation in the distillation column

[0077] The gaseous products enter through the inlet 210 on the side wall of the distillation column body 200 (inlet 210 is located below the dismantling plate 610). The rising vapor passes through the following in sequence:

[0078] a) Mixing component 700 area: Drive motor 3 720 drives fan blade 730 to rotate (100-300rpm), forcibly mixing rising steam and returning liquid, and enhancing gas-liquid mass transfer.

[0079] b) Remove plate 610 vent hole 2: Steam enters the atomization zone after being evenly dispersed.

[0080] c) Atomizing component 600 area: Atomizing nozzle 620 sprays the cooling medium into 50-150μm droplets, selectively condenses high-boiling-point AsCl3, and the condensate flows back along the inner wall of the column or the packing to the bottom of the rectification section, and is eventually returned to the reactor or collected separately; low-boiling-point GeCl4 vapor continues to rise.

[0081] Temperature control component 500 maintains the temperature gradient inside the column: cyclone tube 510 controls the rectification section at 82-85℃, and the atomized cooling medium keeps the fractionation section at 50-70℃.

[0082] Step 4: Product collection and residue removal

[0083] High-purity GeCl4 vapor (6N-7N) is discharged from the top outlet 220 of the tower, and is collected as a product after being condensed by an external condenser.

[0084] The residue at the bottom of the reactor (containing AsCl5, unreacted solid phase, metal chlorides, etc.) is periodically discharged from the outlet 120 and sent for subsequent processing.

[0085] Based on the product purity test results, parameters such as the frequency of the drive motor 442, the working pressure of the atomizing nozzle 620, and the temperature of the cooling medium can be adjusted to optimize the separation effect.

[0086] Step 5: Shutdown and Maintenance

[0087] Stop the chlorine gas supply, and turn off drive motor 1 (411), drive motor 2 (442), drive motor 3 (720), and water pump 530.

[0088] Drain the heat medium inside the jacket 110. After the device has cooled down, disassemble the mixing component 400, atomizing component 600, and mixing component 700 for cleaning or replacement.

[0089] Check the regulating valve 300 and the pipeline sealing, and record the operating parameters for future use.

[0090] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0091] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A device for purifying germanium tetrachloride by coupling short process rectification with impurity fractional condensation, comprising a reactor body (100), a rectification tower body (200), and an adjusting valve (300), wherein the rectification tower body (200) is connected to the reactor body (100) through a pipeline, and the adjusting valve (300) is detachably connected to the side wall of the pipeline, and characterized in that: Also includes: ​ A mixing component (400) is detachably connected to the inner cavity of the reactor body (100); Temperature control assembly (500), which is detachably connected to the inner cavity of the distillation column body (200); Atomizing component (600) is fixedly connected to the bottom of temperature control component (500); A mixing assembly (700) is detachably connected to the interior of the distillation column body (200) near the top. The mixing component (400) includes a stirring assembly (410), a lifting rod (420), a connecting ring (430), a driving component (440), and a mounting plate (450). One end of the stirring assembly (410) penetrates the bottom wall of the reactor body (100). The lifting rod (420) is fixedly connected to the bottom end of the stirring assembly (410). The connecting ring (430) is fixedly connected to the outer side wall of the lifting rod (420). The driving component (440) is detachably connected to the connecting ring (430). The side wall of the driving component (440) is detachably connected to the mounting plate (450), which is L-shaped.

2. The germanium tetrachloride short-process distillation and impurity fractionation coupled purification device according to claim 1, characterized in that: The stirring assembly (410) includes a drive motor (411), a connecting rod (412), a sleeve (413), and a stirring rod (414). The drive motor (411) is detachably connected to the top of the reactor body (100). The connecting rod (412) is fixedly connected to the output end of the drive motor (411) and is inserted into the inner cavity of the reactor body (100). The sleeve (413) is nested in the outer wall of the connecting rod (412). The inner wall of the sleeve (413) is provided with multiple sliding grooves. The connecting rod (412) slides relative to the multiple sliding grooves. The stirring rod (414) is rotatably connected to the outer wall of the sleeve (413).

3. The germanium tetrachloride short-process distillation and impurity fractionation coupled purification device according to claim 2, characterized in that: The drive unit (440) includes an eccentric shaft (441) and a second drive motor (442). One end of the eccentric shaft (441) is fixedly connected to the connecting ring (430), and the output end of the second drive motor (442) is fixedly connected to the end of the eccentric shaft (441) away from the connecting ring (430). The second drive motor (442) is detachably connected to the side wall of the mounting plate (450).

4. The germanium tetrachloride short-process distillation and impurity fractionation coupled purification device according to claim 3, characterized in that: The mixing component (700) includes a fixed plate (710), a drive motor (720), and multiple fan blades (730). The fixed plate (710) is detachably connected to the inner cavity of the distillation column body (200). Multiple ventilation holes are provided in the fixed plate (710). The drive motor (720) is detachably connected to the top of the fixed plate (710). The multiple fan blades (730) are fixedly connected to the output end of the drive motor (720).

5. The germanium tetrachloride short-process distillation and impurity fractionation coupled purification device according to claim 4, characterized in that: The atomizing assembly (600) includes a disassembly plate (610) and a plurality of atomizing nozzles (620). The disassembly plate (610) is detachably connected to the inner wall of the distillation column body (200), and the disassembly plate (610) has a plurality of mounting holes. The plurality of atomizing nozzles (620) are detachably connected to the plurality of mounting holes, and the bottom ends of the plurality of atomizing nozzles (620) are inserted into the disassembly plate (610).

6. The germanium tetrachloride short-process distillation and impurity fractionation coupled purification apparatus according to claim 5, characterized in that: The disassembly plate (610) is hollow, and multiple ventilation holes are provided inside the disassembly plate (610). The multiple ventilation holes are arranged in a circular array with the central axis of the disassembly plate (610) as the reference axis.

7. The germanium tetrachloride short-process distillation and impurity fractionation coupled purification apparatus according to claim 6, characterized in that: The temperature control assembly (500) includes a gyroscope (510) and a connecting pipe (520). One end of the gyroscope (510) passes through the side wall of the distillation column body (200), and the other end of the gyroscope (510) is inserted into the inner cavity of the distillation column body (200). One end of the connecting pipe (520) is inserted into the inner cavity of the disassembly plate (610), and the other end of the connecting pipe (520) is fixedly connected to the end of the gyroscope (510) inserted into the inner cavity of the distillation column body (200).

8. The germanium tetrachloride short-process distillation and impurity fractionation coupled purification apparatus according to claim 7, characterized in that: The end of the connecting pipe (520) that extends to the outside of the distillation column body (200) is detachably connected to a water pump (530), and the water inlet end of the water pump (530) is detachably connected to a storage tank (540).

9. The germanium tetrachloride short-process distillation and impurity fractionation coupled purification apparatus according to claim 8, characterized in that: The distillation column body (200) has an air inlet (210) on its side wall, which is located below the disassembly plate (610), and an air outlet (220) is provided at the top of the distillation column body (200).

10. The germanium tetrachloride short-process distillation and impurity fractionation coupled purification apparatus according to claim 9, characterized in that: A jacket (110) is fixedly connected to the outer wall of the reactor body (100). A discharge port (120) is opened on one side of the bottom end of the reactor body (100), and the discharge port (120) passes through the jacket (110). A water inlet (130) is opened on one side of the jacket (110) near the top end of the reactor body (100). A water outlet (140) is opened at the bottom end of the jacket (110). Multiple support legs (150) are fixedly connected to the bottom end of the jacket (110).

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