An organic compound molecular distillation purification device
Patent Information
- Application Number
- CN202611229403.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-13
- Publication Date
- 2026-10-16
AI Technical Summary
[0004]为了解决现有蒸馏纯化设备效率低下的问题,本申请提供一种有机化合物分子蒸馏纯化设备
1.通过设置进料预分布单元,采用一级多孔分布盘、稳流导叶组、二级多孔分布盘、阻尼组件及螺旋导流件的多级结构,实现对物料的逐级分流、稳压、导流,有效消除进料过程中的脉冲流、偏流与涡流,使物料以螺旋状平稳进入蒸发室,结合弹性刮板组件的均匀刮膜作用,在蒸发室内壁形成厚度均匀、连续稳定的超薄液膜,显著提升传热效率与分离稳定性;
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Figure CN122912508A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the technical field of organic compound separation and purification, and in particular to an organic compound molecular distillation purification apparatus. Background Technology
[0002] Molecular distillation is a non-equilibrium distillation separation method performed under high vacuum conditions. Due to its advantages such as low operating temperature, high separation efficiency, and resistance to the decomposition of heat-sensitive substances, it is widely used in fine chemicals, pharmaceutical intermediates, natural product extraction, and the preparation of high-purity organic compounds. However, with the increasing demand for high-purity organic products in modern industry, especially when the boiling point difference between the components to be separated is less than 5°C, traditional molecular distillation equipment has gradually revealed significant shortcomings in terms of separation accuracy and product purity.
[0003] In existing molecular distillation equipment, the feeding system often employs a simple single-stage distribution structure, such as a single distribution disc or a simple inlet channel. This structure struggles to achieve uniform feed distribution when handling materials with fluctuating viscosity or varying flow rates, easily leading to phenomena such as pulsating flow, biased flow, and localized eddies. Uneven material distribution upon entering the evaporation chamber directly results in significant differences in the thickness of the liquid film on the evaporation wall. In some areas, the liquid accumulates, creating an excessively thick liquid film, affecting heat transfer efficiency and vaporization rate. Meanwhile, other areas experience dry wall phenomena, causing localized overheating or coking of the material, severely interfering with the stability and consistency of evaporation. Summary of the Invention
[0004] To address the problem of low efficiency in existing distillation purification equipment, this application provides an organic compound molecular distillation purification device.
[0005] This application provides an organic compound molecular distillation purification device, which adopts the following technical solution: An organic compound molecular distillation purification apparatus, comprising: The feed pre-distribution unit includes a raw material storage tank and a feed distributor. The raw material storage tank is connected to the feed distributor via a feed pipe. The core evaporation unit includes an evaporation chamber, a gradient heating and insulation jacket, and an adjustable speed elastic scraper assembly. The outlet of the feed distributor is connected to the evaporation chamber. The gradient heating and insulation jacket is wrapped around the outer wall of the evaporation chamber, and the elastic scraper assembly is set inside the evaporation chamber and fits against the inner wall of the evaporation chamber. The gradient temperature control condensation unit includes a main condensation section and an auxiliary condensation section installed in the evaporation chamber, with the main condensation section and the auxiliary condensation section forming a temperature gradient from top to bottom. The segmented collection unit includes a heavy component collection chamber, a light component collection chamber 1, and a light component collection chamber 2. The heavy component collection chamber is sealed to the bottom outlet of the evaporation chamber. The light component collection chamber 1 is connected to the bottom outlet of the main condensation section, and the light component collection chamber 2 is connected to the bottom outlet of the auxiliary condensation section. The vacuum temperature control unit is connected to the evaporation chamber, the main condensation section, and the auxiliary condensation section, respectively, and is used to maintain the system vacuum and provide temperature control medium for each unit.
[0006] By adopting the above technical solution, this application integrates feed pre-distribution, evaporation, gradient condensation, segmented collection, and vacuum temperature control modules to form an integrated closed-loop purification process. The feed pre-distribution unit homogenizes the material in multiple stages to eliminate feed disturbance; the evaporation core unit uses an elastic scraper to form an ultra-thin uniform liquid film, combined with gradient heating to improve vaporization efficiency; the gradient temperature control condensation unit achieves stepwise condensation of components with similar boiling points through the temperature difference between the upper and lower sections; the segmented collection unit collects heavy components and light components with different boiling points respectively, effectively avoiding component co-condensation and cross-entrainment, and significantly improving separation purity and yield.
[0007] In some embodiments, the elastic scraper assembly includes a drive source, a rotating spindle, and an elastic scraper. The drive source is installed outside the evaporation chamber and is connected to the rotating spindle via a drive transmission. Multiple sets of elastic scrapers are provided and arranged at intervals along the axial direction of the rotating spindle. Each elastic scraper includes a scraper bracket and a scraper. The scraper is detachably installed on the scraper bracket, and one side of the scraper is in contact with the inner wall of the evaporation chamber.
[0008] In some embodiments, the heating temperature adjustment range of the gradient heating insulation jacket is 50-300℃, the temperature control accuracy is ±0.3℃, and the gradient heating insulation jacket is equipped with multi-segment heating wires with independent temperature control.
[0009] In some implementations, the temperature of the main condensing section is higher than that of the auxiliary condensing section, the temperature difference between the main condensing section and the auxiliary condensing section can be adjusted within a range of 1-5°C, and the temperatures of both the main condensing section and the auxiliary condensing section are lower than the operating temperature of the evaporation chamber.
[0010] In some embodiments, the feed distributor is provided with a primary porous distribution disk and a secondary porous distribution disk. The secondary porous distribution disk is located at the end of the primary porous distribution disk near the evaporation chamber. A flow-stabilizing guide vane assembly is provided between the primary and secondary porous distribution disks. A damping component is provided at the bottom of the secondary porous distribution disk, and a spiral guide component is provided at the bottom of the damping component.
[0011] In some embodiments, the pore diameter of the primary porous distribution plate is 4-5 mm and the opening ratio is 35%-40%, while the pore diameter of the secondary porous distribution plate is 2-3 mm and the opening ratio is 40%-45%.
[0012] In some embodiments, the flow stabilizer guide vane assembly includes a mounting ring and swirl guide vanes. The mounting ring is installed on the inner wall of the feed distributor, and multiple swirl guide vanes are evenly arranged on the inner wall of the mounting ring. The swirl guide vanes have an inclination angle of 20°-40°, and the height of the flow stabilizer guide vane assembly is 10-20mm.
[0013] In some embodiments, the spiral guide is a spiral guide plate or spiral blade with a spiral helix angle of 15°-30°. The top of the spiral guide is fixedly connected to the bottom of the damping plate, and the bottom of the spiral guide extends to the outlet of the feed distributor.
[0014] In some embodiments, the damping assembly includes a damping plate and guide vanes. The damping plate is installed at the bottom of the flow-stabilizing guide vane assembly. The damping plate has guide grooves that are spaced apart circumferentially along the damping plate. The guide vanes are made of elastic material and are located at the bottom of the damping plate. Multiple guide vanes are evenly arranged circumferentially. The guide vanes are used to adaptively adjust their opening and closing angle according to the flow rate.
[0015] In some embodiments, a mounting shaft is provided at the bottom of the damping plate, and multiple guide vanes are mounted on the mounting shaft through a central ring. A torsion spring is provided between the central ring and the mounting shaft. A connecting shaft is provided on the central ring and is arranged perpendicular to the axis of the mounting shaft. The guide vanes are mounted on the connecting shaft, and a torsion spring is provided between the guide vanes and the connecting shaft.
[0016] Compared with the prior art, this application includes at least one of the following beneficial technical effects: 1. By setting up a pre-distribution unit for feeding, and adopting a multi-stage structure of a primary porous distribution disk, a flow-stabilizing guide vane group, a secondary porous distribution disk, a damping component, and a spiral guide component, the material is gradually divided, stabilized, and guided, effectively eliminating pulse flow, deflection flow, and eddies during the feeding process. This allows the material to enter the evaporation chamber smoothly in a spiral shape. Combined with the uniform scraping effect of the elastic scraper component, a uniform, continuous, and stable ultra-thin liquid film is formed on the inner wall of the evaporation chamber, significantly improving heat transfer efficiency and separation stability. 2. By setting a controllable small temperature gradient (1-5℃) between the main condensation section and the auxiliary condensation section, and combining it with the precise control of the vacuum temperature control unit, stepwise condensation of organic components with similar boiling points can be achieved, avoiding the co-condensation and cross-entrainment problems under the traditional single-temperature condensation method. Combined with the segmented collection unit, the separation purity and yield of light and heavy components are significantly improved. 3. This application highly integrates the feed pre-distribution, evaporation film formation, gradient condensation, segmented collection and vacuum temperature control modules to form an integrated closed-loop purification process. The units work together to ensure the long-term stable operation of the equipment under high vacuum and variable operating conditions, meeting the needs of continuous production of high-purity organic compounds. Attached Figure Description
[0017] Figure 1 This is a schematic diagram of the overall structure of the feed distributor in the embodiments of this application.
[0018] Figure 2 This is a cross-sectional view of the internal structure of the feed distributor in an embodiment of this application.
[0019] Figure 3 This is a schematic diagram of the internal structure of the feed distributor in an embodiment of this application.
[0020] Figure 4 This is a top view of the guide vane in an embodiment of this application.
[0021] Figure 5 This is a cross-sectional view of the evaporation chamber in an embodiment of this application.
[0022] In the picture: 1. Raw material storage tank; 2. Feed distributor; 202. Primary porous distribution plate; 203. Flow stabilizer guide vane assembly; 204. Secondary porous distribution plate; 205. Damping plate; 206. Flow guide groove; 207. Flow guide vane; 21. Mounting shaft; 22. Central ring; 23. Connecting shaft; 208. Spiral guide component; 209. Observation window; 3. Evaporation chamber; 4. Elastic scraper assembly; 41. Rotating main shaft; 42. Scraper bracket; 43. Scraper; 5. Gradient heating insulation jacket; 6. Main condensing section; 61. Condensing plate; 62. Liquid collection cup; 7. Auxiliary condensing section; 8. Heavy component collection chamber; 9. Light component collection chamber one; 10. Light component collection chamber two; 11. Vacuum unit; 12. Temperature control system. Detailed Implementation
[0023] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.
[0024] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the term "and / or" in this document merely describes the relationship between related objects in an organic compound molecular distillation purification apparatus, indicating that three relationships can exist. For example, A and / or B can represent: A alone, A and B simultaneously, or B alone. Furthermore, the character " / " in this document, unless otherwise specified, generally indicates that the related objects are in an "or" relationship.
[0025] This application provides an organic compound molecular distillation purification device, including a feed pre-distribution unit, an evaporation core unit, a gradient temperature control condensation unit, a segmented collection unit, and a vacuum temperature control unit.
[0026] Reference Figure 1 and Figure 5The feed pre-distribution unit includes a raw material storage tank 1 and a feed distributor 2. The raw material storage tank 1 is connected to the feed distributor 2 via a feed pipe. The raw material storage tank 1 is used to store raw materials and supply raw materials to the feed distributor 2. The evaporation core unit includes an evaporation chamber 3, a gradient heating and insulation jacket 5, and an adjustable speed elastic scraper assembly 4. The outlet of the feed distributor 2 is connected to the evaporation chamber 3. The gradient heating and insulation jacket 5 is wrapped around the outer wall of the evaporation chamber 3, and the elastic scraper assembly 4 is disposed inside the evaporation chamber 3 and fits against the inner wall of the evaporation chamber 3. The gradient temperature control condensation unit includes a main condensation section 6 and an auxiliary condensation section 7 sealed and connected inside the evaporation chamber 3. The main condensation section 6 and the auxiliary condensation section 7 form a temperature gradient from top to bottom. The segmented collection unit includes a heavy component collection chamber 8, a light component collection chamber one 9, and a light component collection chamber two 10. The heavy component collection chamber 8 is sealed to the bottom outlet of the evaporation chamber 3. The light component collection chamber one 9 is connected to the bottom outlet of the main condensation section 6, and the light component collection chamber two 10 is connected to the bottom outlet of the auxiliary condensation section 7. The vacuum temperature control unit is connected to the evaporation chamber 3, the main condensation section 6, and the auxiliary condensation section 7 respectively, and is used to maintain the system vacuum and provide temperature control medium for each unit. The vacuum temperature control unit includes a vacuum unit 11 and a temperature control system 12. The vacuum unit 11 is connected to the evaporation chamber 3 and is used to evacuate the evaporation chamber 3. The vacuum unit 11 is preferably a Roots-diffusion pump composite unit, which is existing technology and will not be described in detail here. The temperature control system 12 is connected to the gradient temperature control condensation unit through a heat transfer medium pipe, and is connected to the main condensation section and the auxiliary condensation section through independent refrigerant pipes. The temperature control system 12 is also existing technology and will not be described in detail here.
[0027] Through the modular integration and collaborative operation of the above-mentioned units, an integrated continuous purification process from feeding, evaporation, gradient condensation to segmented collection is realized. The feeding pre-distribution unit performs multi-stage homogenization of the raw materials, eliminating pulses and flow deviations during the feeding process; the evaporation core unit forms a uniform ultra-thin liquid film on the inner wall of the evaporation chamber 3 through the adjustable speed elastic scraper assembly 4, and with the precise heating of the gradient heating insulation jacket 5, the vaporization efficiency is improved; the gradient temperature-controlled condensation unit utilizes the temperature difference between the main condensation section 6 and the auxiliary condensation section 7 to condense light components with different boiling points sequentially, avoiding the co-condensation problem caused by traditional single-temperature condensation; the segmented collection unit collects heavy components and light components with different boiling point differences separately, ensuring product purity; the vacuum temperature control unit provides a stable high vacuum environment and precise temperature control for the entire system, ensuring the stability and reliability of the separation process.
[0028] Reference Figures 2 to 4Specifically, the feed distributor 2 is internally equipped with a primary porous distribution disk 202 and a secondary porous distribution disk 204. The secondary porous distribution disk 204 is located at the end of the primary porous distribution disk 202 near the evaporation chamber 3. A flow-stabilizing guide vane assembly 203 is provided between the primary porous distribution disk 202 and the secondary porous distribution disk 204. A damping assembly is provided at the bottom of the secondary porous distribution disk 204, and a spiral guide component 208 is provided at the bottom of the damping assembly.
[0029] Preferably, the primary porous distribution disc 202 has a pore diameter of 4-5 mm and an opening ratio of 35%-40%, while the secondary porous distribution disc 204 has a pore diameter of 2-3 mm and an opening ratio of 40%-45%. This gradient design, combining a primary distribution disc with a large pore diameter and low opening ratio with a secondary distribution disc with a small pore diameter and high opening ratio, allows the primary porous distribution disc 202 to initially divide the concentrated material flow into multiple medium-flow streams, mitigating impact. The secondary porous distribution disc 204 further divides the material flow into finer, more uniform micro-streams. This progressively refined distribution method achieves a smooth transition from concentrated to dispersed flow, and from coarse to fine distribution, improving the initial uniformity of material distribution.
[0030] Furthermore, the flow stabilizing guide vane assembly 203 includes a mounting ring and swirling guide vanes. The mounting ring is installed on the inner wall of the feed distributor 2, and multiple swirling guide vanes are evenly arranged on the inner wall of the mounting ring. The inclination angle of the swirling guide vanes is 20°-40°, preferably 20° in this embodiment. The height of the flow stabilizing guide vane assembly 203 is 10-20mm. When the material flows through the flow stabilizing guide vane assembly 203, a stable tangential swirling flow field is formed under the guidance of the swirling guide vanes with a 20° inclination angle, eliminating pressure fluctuations, pulse flows, and local eddies inside the material. The 10-20mm cavity height provides sufficient swirling pressure equalization space for the material, ensuring the circumferential uniformity of the material flow, transforming the unstable fluctuating material flow into a stable material flow with uniform pressure and stable velocity, and then conveying it to the next stage distribution structure.
[0031] The spiral guide component 208 is a spiral guide plate or spiral blade with a spiral helix angle of 15°-30°. The upper end of the spiral guide component 208 is fixedly connected to the bottom of the damping assembly, and the lower end extends to the outlet of the feed distributor 2. It is used to convert the material flow after being stabilized by the guide plate 207 into a spiral-shaped and stable material flow to be transported to the evaporation chamber 3. After being stabilized by the damping assembly, the material forms a uniform, stable spiral liquid film with a certain tangential kinetic energy under the guidance of the spiral guide component 208 with a spiral helix angle of 15°-30°, and adheres smoothly to the inner wall of the evaporation chamber 3. This spiral feeding method, combined with the subsequent elastic scraper assembly 4, helps to spread an ultra-thin liquid film on the inner wall of the evaporation chamber 3 more quickly and evenly, avoiding splashing and unevenness caused by the material directly impacting the inner wall.
[0032] The damping assembly includes a damping plate 205 and guide vanes 207. The damping plate 205 is installed at the bottom of the flow-stabilizing guide vane assembly 203. Guide grooves 206 are provided on the damping plate 205, spaced apart circumferentially along the damping plate 205. The guide vanes 207 are made of elastic material and are located at the bottom of the damping plate 205. Multiple guide vanes 207 are evenly arranged circumferentially and are used to adaptively adjust their opening and closing angle according to the flow rate. A mounting shaft 21 is provided at the bottom of the damping plate 205. Multiple guide vanes 207 are mounted on the mounting shaft 21 via a central ring 22. A torsion spring is provided between the central ring 22 and the mounting shaft 21. A connecting shaft 23 is provided on the central ring 22, perpendicular to the axis of the mounting shaft 21. The guide vanes 207 are mounted on the connecting shaft 23, and a torsion spring is provided between the guide vanes 207 and the connecting shaft 23. Torsion spring one is used to control the circumferential rotation of the central ring 22 relative to the mounting shaft 21, and torsion spring two is used to control the radial opening and closing of the guide vane 207 relative to the connecting shaft 23. This dual elastic connection method allows the guide vane 207 to make more flexible and precise adaptive adjustments in both the circumferential and radial directions according to the material flow rate and impact angle, further optimizing the pressure stabilization and flow equalization effects, and ensuring that the material flow can be smoothly and evenly transported to the next stage under various working conditions.
[0033] In this embodiment, after the material enters the feed distributor 2 through the feed pipe, it first undergoes preliminary diversion and dispersion through the primary porous distribution plate 202, and then enters the flow stabilizing guide vane group 203 for swirling and pressure equalization, eliminating pulsating flow and local deviation flow. Next, the material undergoes fine diversion through the secondary porous distribution plate 204, and then reaches the damping plate 205. At the damping plate 205, the material squeezes the guide vane 207, and with the elastic force of the torsion spring, the material flow rate is adaptively adjusted, further stabilizing the material flow. Finally, the material is transformed into a spiral-shaped stable material flow through the spiral guide component 208, and is uniformly transported to the evaporation chamber 3. Through this series of multi-stage distribution, pressure stabilization and flow guiding structures, the problems of uneven feeding, deviation flow and eddy currents existing in traditional feeding systems are solved, laying a solid foundation for the subsequent formation of a uniform liquid film.
[0034] Furthermore, the elastic scraper assembly 4 includes a drive source, a rotating spindle 41, and elastic scrapers. The drive source is mounted on the top outside the evaporation chamber 3 and is connected to the rotating spindle 41 via a transmission connection. Multiple sets of elastic scrapers are provided and arranged at intervals along the circumference of the rotating spindle 41. Each elastic scraper includes a scraper support 42 and a scraper 43. The scraper 43 is detachably mounted on the scraper support 42, and one side of the scraper 43 is in contact with the inner wall of the evaporation chamber 3. In this embodiment, the drive source is a servo motor, whose speed can be steplessly adjusted within the range of 50-300 r / min to adapt to materials of different viscosities and flow rates. The elastic scraper 43 is made of a flexible material, and the contact gap between its edge and the inner wall of the evaporation chamber 3 is controlled within 0.1 mm. When the rotating spindle 41 drives the scraper to rotate, the scraper 43 continuously scrapes and extends the material entering the evaporation chamber 3, forming an ultra-thin liquid film of uniform thickness. The flexible nature of the scraper 43 enables it to adaptively compensate for minor processing errors and thermal expansion and contraction deformation of the inner wall of the evaporation chamber 3, ensuring that there is no liquid accumulation on the inner wall and no local dry wall phenomenon, thereby significantly improving heat transfer efficiency and vaporization stability.
[0035] Furthermore, the gradient heating insulation jacket 5 has a heating temperature adjustment range of 50-300℃ and a temperature control accuracy of ±0.3℃. The jacket 5 is internally equipped with multi-segment heating wires with independent temperature control. In this embodiment, the intelligent temperature control system 12 achieves axial temperature gradient control of the evaporation chamber 3 by independently controlling the multi-segment heating wires. For example, the upper temperature can be set slightly higher than the lower temperature to promote preferential vaporization of lighter components. The high-precision temperature control of ±0.3℃ ensures stable evaporation temperature, avoiding uneven vaporization rates and reduced separation efficiency caused by temperature fluctuations, and providing crucial thermodynamic conditions for the accurate separation of components with similar boiling points.
[0036] In this embodiment, the temperature of the main condensing section 6 is higher than that of the auxiliary condensing section 7. The temperature difference between the main condensing section 6 and the auxiliary condensing section 7 is adjustable within a range of 1-5℃, and the temperatures of both the main condensing section 6 and the auxiliary condensing section 7 are lower than the operating temperature of the evaporation chamber 3. The intelligent temperature control system 12 independently regulates the temperatures of the main condensing section 6 and the auxiliary condensing section 7 through branch refrigerant pipes, maintaining a small, controllable temperature difference of 1-5℃ between them.
[0037] Specifically, in this embodiment, the main condensing section 6 and the auxiliary condensing section 7 have the same structure. Taking the main condensing section 6 as an example, the main condensing section 6 includes a condensing plate 61 and a liquid collecting cup 62. The condensing plate 61 is fixed inside the evaporation chamber 3, and a refrigerant channel is provided inside the condensing plate 61. The condensing plate 61 is provided with a refrigerant inlet and a refrigerant outlet, which extend to the outside of the evaporation chamber 3. The liquid collecting cup 62 is located at the bottom of the condensing plate 61 and is fixed at the center of the evaporation chamber 3. There is an annular gap between the liquid collecting cup 62 and the inner wall of the evaporation chamber 3. The liquid collecting cup 62 is conical, and a liquid outlet is provided at the bottom of the liquid collecting cup 62. During operation, lighter components with slightly higher boiling points first move from the inner wall (heating surface) of the evaporation chamber 3 towards the center, liquefying upon impact with the lower-temperature condensing plate 61 (cooling surface). Lighter components with lower boiling points continue to rise with the airflow through the annular gap to the auxiliary condensing section (lower temperature) for condensation. The condensed liquid is drawn to the outlet by gravity and discharged through the outlet. This gradient temperature control design enables precise stepwise condensation of components with similar boiling points, effectively avoiding the co-condensation problem that may occur in a single temperature condensation section, and greatly improving the separation purity.
[0038] The implementation principle of this application embodiment is as follows: The material smoothly enters the evaporation chamber 3 through a uniform feed inlet. Under the action of the elastic scraper assembly 4, a continuous and uniform ultra-thin liquid film is formed on the inner wall of the evaporation chamber 3. At the same time, the gradient heating and insulation jacket 5 on the outer wall of the evaporation chamber 3 delivers heat medium through the intelligent temperature control system 12 to achieve uniform gradient heating of the liquid film. The boiling point of the material is reduced in the high vacuum environment created by the vacuum temperature control unit, so that organic components with similar boiling points vaporize sequentially. The vaporized light component molecules move upward to the gradient temperature control condensation unit. The intelligent temperature control system 12 regulates the main refrigerant through the branch refrigerant pipes. The temperature difference between the condensing section 6 and the auxiliary condensing section 7 enables the stepwise condensation and liquefaction of light components with different boiling points. Due to their high boiling point and large molecular weight, the heavy components cannot vaporize and fall along the inner wall of the evaporation chamber 3, directly entering the heavy component collection chamber 8. The condensed light components fall along the inner walls of the main condensing section 6 and the auxiliary condensing section 7, respectively, and enter the light component collection chamber 1 9 and the light component collection chamber 2 10. The vacuum temperature control unit continuously pumps vacuum to maintain a stable high vacuum inside the evaporation chamber 3 and the condensing unit, and synchronously controls the heating and condensation temperatures in a closed loop to ensure precise and controllable temperature during the separation process.
[0039] The above are all preferred embodiments of this application and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.
Claims
1. An organic compound molecular distillation purification apparatus, characterized in that, include: The feed pre-distribution unit includes a raw material storage tank (1) and a feed distributor (2), wherein the raw material storage tank (1) is connected to the feed distributor (2) through a feed pipe. The evaporation core unit includes an evaporation chamber (3), a gradient heating and insulation jacket (5), and an adjustable speed elastic scraper assembly (4). The outlet of the feed distributor (2) is connected to the evaporation chamber (3). The gradient heating and insulation jacket (5) is wrapped around the outer wall of the evaporation chamber (3). The elastic scraper assembly (4) is set inside the evaporation chamber (3) and fits against the inner wall of the evaporation chamber (3). The gradient temperature control condensation unit includes a main condensation section (6) and an auxiliary condensation section (7) disposed in the evaporation chamber (3), wherein the main condensation section (6) and the auxiliary condensation section (7) form a temperature gradient from top to bottom; The segmented collection unit includes a heavy component collection chamber (8), a light component collection chamber one (9), and a light component collection chamber two (10). The heavy component collection chamber (8) is sealed to the bottom outlet of the evaporation chamber (3). The light component collection chamber one (9) is connected to the bottom outlet of the main condensation section (6), and the light component collection chamber two (10) is connected to the bottom outlet of the auxiliary condensation section (7). The vacuum temperature control unit is connected to the evaporation chamber (3), the main condensation section (6) and the auxiliary condensation section (7) respectively, and is used to maintain the vacuum level of the system and provide temperature control medium for each unit.
2. The organic compound molecular distillation purification equipment according to claim 1, characterized in that: The elastic scraper assembly (4) includes a drive source, a rotating spindle (41) and an elastic scraper. The drive source is installed outside the evaporation chamber (3) and is connected to the rotating spindle (41) for transmission. Multiple sets of elastic scrapers are provided and are arranged at intervals along the axial direction of the rotating spindle (41). The elastic scraper includes a scraper bracket (42) and a scraper (43). The scraper (43) is detachably installed on the scraper bracket (42) and one side of the scraper (43) is in contact with the inner wall of the evaporation chamber (3).
3. The organic compound molecular distillation purification apparatus according to claim 1, characterized in that: The heating temperature adjustment range of the gradient heating insulation jacket (5) is 50-300℃, and the temperature control accuracy is ±0.3℃. The gradient heating insulation jacket (5) is equipped with multi-segment heating wires with independent temperature control.
4. The organic compound molecular distillation purification equipment according to claim 1, characterized in that: The temperature of the main condensing section (6) is higher than that of the auxiliary condensing section (7). The temperature difference between the main condensing section (6) and the auxiliary condensing section (7) can be adjusted within a range of 1-5℃. The temperatures of the main condensing section (6) and the auxiliary condensing section (7) are both lower than the operating temperature of the evaporation chamber (3).
5. The organic compound molecular distillation purification apparatus according to claim 1, characterized in that: The feed distributor (2) is provided with a primary porous distribution disk (202) and a secondary porous distribution disk (204). The secondary porous distribution disk (204) is located at one end of the primary porous distribution disk (202) near the evaporation chamber (3). A flow-stabilizing guide vane assembly (203) is provided between the primary porous distribution disk (202) and the secondary porous distribution disk (204). A damping component is provided at the bottom of the secondary porous distribution disk (204), and a spiral guide component (208) is provided at the bottom of the damping component.
6. The organic compound molecular distillation purification apparatus according to claim 5, characterized in that: The primary porous distribution plate (202) has a pore diameter of 4-5 mm and an opening rate of 35%–40%, while the secondary porous distribution plate (204) has a pore diameter of 2-3 mm and an opening rate of 40%–45%.
7. The organic compound molecular distillation purification apparatus according to claim 5, characterized in that: The flow stabilizer guide vane assembly (203) includes an installation ring and swirl guide vanes. The installation ring is installed on the inner wall of the feed distributor (2). Multiple swirl guide vanes are evenly arranged on the inner wall of the installation ring. The swirl guide vanes have an inclination angle of 20°-40°. The height of the flow stabilizer guide vane assembly (203) is 10-20mm.
8. The organic compound molecular distillation purification apparatus according to claim 5, characterized in that: The spiral guide (208) is a spiral guide plate or spiral blade with a spiral helix angle of 15°-30°. The top of the spiral guide (208) is connected to the bottom of the damping assembly, and the bottom of the spiral guide (208) extends to the outlet of the feed distributor (2).
9. The organic compound molecular distillation purification apparatus according to claim 5, characterized in that: The damping assembly includes a damping plate (205) and a guide vane (207). The damping plate (205) is installed at the bottom of the flow-stabilizing guide vane assembly (203). A guide groove (206) is provided on the damping plate (205). The guide groove (206) is spaced apart along the circumference of the damping plate (205). The guide vane (207) is made of elastic material and is located at the bottom of the damping plate (205). Multiple guide vanes (207) are evenly arranged along the circumference. The guide vane (207) is used to adaptively open and close the angle according to the flow rate.
10. The organic compound molecular distillation purification apparatus according to claim 9, characterized in that: The damping plate (205) has a mounting shaft (21) at its bottom. Multiple guide vanes (207) are mounted on the mounting shaft (21) via a central ring (22). A torsion spring is provided between the central ring (22) and the mounting shaft (21). A connecting shaft (23) is provided on the central ring (22). The connecting shaft (23) is perpendicular to the axis of the mounting shaft (21). The guide vanes (207) are mounted on the connecting shaft (23). A torsion spring is provided between the guide vanes (207) and the connecting shaft (23).