A laboratory rectifying column
By designing a laboratory distillation column and adopting a countercurrent contact design for the reflux pipe and condenser, the problem of vacuum level being affected by traditional distillation methods was solved, achieving efficient component separation and safe sampling.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- SHANGHAI YUANHUAI IND CO LTD
- Filing Date
- 2025-09-03
- Publication Date
- 2026-07-31
AI Technical Summary
Traditional distillation methods, which discharge liquid directly through the discharge port, can affect the vacuum level of the equipment, resulting in poor separation performance.
A laboratory distillation column was designed, including a main frame, a distillation column, a condenser, first and second reflux ratio controllers, a sampling tank, and a liquid distribution assembly. Through the design of the reflux pipe and the condenser, the countercurrent contact of vapor and the diversion of liquid are achieved, avoiding direct discharge that would affect the vacuum level.
It achieves efficient component separation without affecting the vacuum level, improves the separation effect of the distillation column, and enables sample collection without disrupting the vacuum environment, thus avoiding leakage.
Smart Images
Figure CN224573248U_ABST
Abstract
Description
Technical Field
[0001] This application relates to a laboratory distillation column, belonging to the technical field of chemical experimental equipment. Background Technology
[0002] To obtain high-purity materials, it is necessary to utilize the difference in boiling points between substances to separate them and obtain high-purity products. The process of separating a liquid mixture into the desired components by repeatedly partially vaporizing the liquid mixture and simultaneously partially condensing the generated vapor is called distillation. To reduce the separation effect of distillation in industrial processes, small-scale experiments need to be conducted in the laboratory to guide industrial design. In order to save energy, it is possible to use lateral extraction of liquid or gas phases in industrial processes. However, the traditional method is to discharge directly through the discharge port, which will affect the vacuum degree of the equipment when extracting liquid.
[0003] Therefore, a new technical solution is needed to solve the above-mentioned technical problems. Summary of the Invention
[0004] The purpose of this application is to provide a laboratory distillation column that solves the problem that the traditional method of discharging directly through the discharge port affects the vacuum level of the equipment when taking liquid.
[0005] The technical problem to be solved in this application is achieved by the following technical solution: A laboratory distillation column, comprising: Main framework; A distillation column is fixedly connected to the main frame, and a reaction flask is connected to the distillation column. The condenser is connected to the distillation column via a top connection section. A first reflux ratio controller is connected to the bottom of the condenser for reflux extraction, and the first reflux ratio controller is connected to the top connection section of the tower through a reflux pipe; A sampling container is connected to the first reflux ratio controller. The sampling container includes a second reflux ratio controller and a sampler. The sampler is installed on the side wall of the sampling container, and the second reflux ratio controller is installed inside the sampling container. The second reflux ratio controller assists the sampler in sampling. A liquid distribution assembly, connected to the bottom of the sampling tank, is used to receive the sample liquid coming out of the sampling tank.
[0006] Preferably, the return pipe is provided with a U-shaped structure to form a water seal during use, preventing steam from entering the first return ratio controller from the return pipe.
[0007] Preferably, a PTFE glass valve is installed on the top of the condenser for controlling the vacuuming process.
[0008] Preferably, the condenser has an inner layer and an outer layer, and a transition cavity is formed between the inner layer and the outer layer, wherein the inner layer is connected to the PTFE glass valve and the first reflux ratio controller.
[0009] Preferably, the inner layer is provided with a condenser coil, which consists of two sets of spiral tubes arranged in concentric circles, with the inner spiral tubes and the outer spiral tubes intersecting in the axial projection.
[0010] Preferably, the condenser coil further includes a distribution pipe and a collection pipe, both connected to two sets of spiral pipes. The distribution pipe is connected to the condensate inlet, the collection pipe is fixedly connected to the inner layer and connected to the transition cavity, and the outer layer is provided with a condensate outlet, which is connected to the transition cavity.
[0011] Preferably, the top connecting section of the tower is provided with a gas phase outlet, which extends from the middle of the condenser through the outer and inner layers.
[0012] Preferably, the sampler includes: a three-way pipe that penetrates the side wall of the sampling container and extends into the sampling container, with its opening facing upwards; the three-way pipe is provided with an exhaust pipe and a liquid storage pipe, and a discharge valve is installed on the three-way pipe, the discharge valve being used to open or close the passage of the exhaust pipe and the liquid storage pipe; the exhaust pipe is provided with an exhaust port and an exhaust valve; the liquid storage pipe is provided with a drain port and a drain valve.
[0013] Preferably, the liquid distribution assembly includes: a liquid distributor, which is fixedly connected to the main frame via a third steel pipe support, and a first collection bottle and a second collection bottle are connected to the liquid distributor for collecting sample liquids under different working conditions.
[0014] Preferably, the liquid distribution assembly further includes a buffer tank connected to the liquid distributor, and the buffer tank is equipped with a vent valve.
[0015] The beneficial effects of this application are: 1. During operation, the material in the reaction flask is heated in a heating bath. The generated vapor is then distilled through a distillation column and enters a condenser at the top of the column to exchange heat with the cooling medium and condense into liquid. The resulting liquid is split by the first reflux ratio controller. Part of the condensed liquid is returned to the distillation column as reflux liquid through the reflux pipe to come into countercurrent contact with the rising vapor. Component separation is achieved through multiple gas-liquid mass transfers. The other part of the liquid is retained in the sampling tank, and then distributed from the sampling tank to the first collection bottle or... In the second collection bottle, when a sample is needed, first open the discharge valve to introduce the sample liquid from the sampling tank into the three-way pipe through the second reflux ratio controller, and then let it flow into the storage pipe through the three-way pipe. At this time, the sampling tank is still isolated from the outside air and there will be no leakage. Then close the discharge valve to isolate the sampling tank from the exhaust pipe and the storage pipe. Next, open the exhaust valve to restore the air pressure in the exhaust pipe and the storage pipe. Then open the drain valve, and the sample liquid flows smoothly into the sampling container through the drain port. This process will not affect the vacuum degree in the sampling tank. Attached Figure Description
[0016] Figure 1 This is a schematic diagram of the three-dimensional structure of this application. Figure 1 ; Figure 2 This is a schematic diagram of the three-dimensional structure of this application. Figure 2 ; Figure 3 This is a cross-sectional view of this application; Figure 4 This is a cross-sectional structural diagram of the sampler in this application.
[0017] In the diagram: 1. Main frame; 101. Shelf; 102. Casters; 103. First steel pipe support; 104. Second steel pipe support; 105. Third steel pipe support; 2. Reaction flask; 3. Distillation column; 4. Top connection section; 5. Condenser; 501. Outer layer; 502. Inner layer; 503. Transition chamber; 504. Distribution pipe; 505. Condensation coil; 506. Collection pipe; 507. Condensate outlet; 508. Condensate inlet; 509. PTFE glass valve; 6. 7. Reflux ratio controller; 8. Reflux pipe; 9. U-shaped structure; 10. Sampler; 11. Three-way pipe; 12. Exhaust pipe; 13. Exhaust valve; 14. Exhaust port; 15. Discharge valve; 16. Liquid storage pipe; 17. Drain valve; 18. Drain port; 19. Sampling tank; 10. Second reflux ratio controller; 11. Liquid distributor; 12. First collection bottle; 13. Second collection bottle; 14. Buffer tank; 15. Venting valve; 16. Electrical control box; 17. Support pipe. Detailed Implementation
[0018] To facilitate a clear understanding of the technical means, creative features, objectives, and effects of this application, the following description, in conjunction with specific illustrations, further elaborates on this application.
[0019] In the description of this application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the equipment or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this application.
[0020] In this application, unless otherwise expressly specified and limited, the terms "installation," "connection," "joining," "fixing," 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 direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.
[0021] In this application, unless otherwise expressly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature being directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature being directly below or diagonally below the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.
[0022] The following disclosure provides numerous different embodiments or examples for implementing various structures of the embodiments of this application. To simplify the disclosure of the embodiments of this application, specific examples of components and arrangements are described below. Of course, these are merely examples and are not intended to limit the scope of this application. Furthermore, reference numerals and / or reference letters may be repeated in different examples of the embodiments of this application; such repetition is for simplification and clarity and does not in itself indicate a relationship between the various embodiments and / or arrangements discussed. In addition, various specific examples of processes and materials are provided in the embodiments of this application, but those skilled in the art will recognize the application of other processes and / or the use of other materials.
[0023] like Figure 1-4 As shown, a laboratory distillation column includes a main frame 1, a distillation column 3, a condenser 5, a first reflux ratio controller 6, a sampling tank 9, and a liquid distribution assembly.
[0024] Specifically, the main frame 1 is composed of multiple steel pipes connected by pipe joints and screws, a common feature in the market. A shelf 101 is fixedly connected to the bottom of the main frame 1, and the shelf 101 is used to install a heating bath. Universal casters 102 with braking function are installed at each of the four corners of the bottom of the main frame 1. These universal casters 102 are existing technology and readily available in the market. The distillation column 3 is fixedly connected to the main frame 1 via a first steel pipe support 103. The distillation column 3 is connected to a reaction flask 2. During use, the reaction flask 2 is heated by the heating bath. Its main function is to extract as much of the lighter components as possible from the descending liquid, thereby improving the purity of the heavier components (high-boiling-point components) in the distillation column 3. The liquid flowing down from the rectification section comes into countercurrent contact with the hot vapor generated in the stripping section of the reaction flask 2. The hot vapor carries or strips out the light components in the liquid, causing them to vaporize. It should be noted that the rectification column 3 is prior art and not an improvement of this application, so it will not be described in detail here. The reaction flask 2 is also equipped with a feed inlet, a temperature sensor, and a pressure sensor. The condenser 5 is connected to the rectification column 3 through the top connection section 4, and the condenser 5 is fixedly connected to the main frame 1 through the second steel pipe support 104. A PTFE glass valve 509 is installed on the top of the condenser 5. In use, the PTFE glass valve 509 is connected to the vacuum system through a hose to control the vacuum and ensure that a certain vacuum degree is maintained in the condenser 5, so that the vapor from the rectification column can enter the condenser 5. The first reflux ratio controller 6 is connected to the bottom of the condenser 5 for reflux sampling, and the first reflux ratio controller 6 is connected to the top connection section 4 of the tower through the reflux pipe 7; the sampling tank 9 is connected to the first reflux ratio controller 6, and the sampling tank 9 includes a second reflux ratio controller 10 and a sampler 8. The sampler 8 is installed on the side wall of the sampling tank 9, and the second reflux ratio controller 10 is installed inside the sampling tank 9. The second reflux ratio controller 10 assists the sampler 8 in sampling. The sampling tank 9 and the condenser 5 are also connected through a support pipe 17; the liquid distribution assembly is connected to the bottom of the sampling tank 9 for receiving the sample liquid coming out of the sampling tank 9, and the two third steel pipe supports 105 of the liquid distribution assembly are fixedly connected to the main frame 1.
[0025] In a preferred embodiment, a U-shaped structure 701 is provided on the return pipe 7 to form a water seal during use, preventing steam from directly entering the first return ratio controller 6 from the return pipe 7.
[0026] In a preferred embodiment, the condenser 5 has an inner layer 502 and an outer layer 501, with a transition cavity 503 formed between the inner layer 502 and the outer layer 501. The transition cavity 503 facilitates the heat preservation of the condenser 5. The inner layer 502 is connected to the PTFE glass valve 509 and the first reflux ratio controller 6. A condensing coil 505 is installed on the inner layer 502, and the condensing coil 505 consists of two sets of spiral tubes arranged concentrically. The spiral tubes of the inner layer 502 and the spiral tubes of the outer layer 501 are intersected in axial projection. The condensing coil 505 also includes a distribution pipe 504 and a collecting pipe 506, both connected to the two sets of spiral tubes. The distribution pipe 504 is connected to the condensate inlet 508, and the collecting pipe 506 is fixedly connected to the inner layer 502 and connected to the transition cavity 503. A condensate outlet 507 is provided on the outer layer 501, and the condensate outlet 507 is connected to the transition cavity 503. During use, the circulating condensate enters the distribution pipe 504 from the condensate inlet 508, then enters the inner spiral pipe 502 and the outer spiral pipe 501 from the distribution pipe 504, enters the transition chamber 503 through the collecting pipe 506, and then exits from the condensate outlet 507; the tower top connecting section 4 is provided with a gas phase outlet, which passes through the outer layer 501 and the inner layer 502 from the middle of the condenser 5.
[0027] In a preferred embodiment, the sampler 8 includes: a three-way pipe 801, which penetrates the side wall of the sampling tank 9 and extends into the sampling tank 9, with its opening facing upwards to facilitate receiving the sample liquid from the dripping funnel inside the second reflux ratio controller 10; the three-way pipe 801 is provided with an exhaust pipe 802 and a liquid storage pipe 806, and a discharge valve 805 is installed on the three-way pipe 801. The discharge valve 805 is used to open or close the passage between the exhaust pipe 802, the liquid storage pipe 806 and the three-way pipe 801. It should be noted that opening or closing the discharge valve 805 will not affect the flow channel between the exhaust pipe 802 and the liquid storage pipe 806; the exhaust pipe 802 is provided with an exhaust port 804 and an exhaust valve 803; the liquid storage pipe 806 is provided with a drain port 808 and a drain valve 807. When sampling liquid is needed, first open the discharge valve 805 to introduce the sample liquid in the sampling tank 9 into the three-way pipe 801 through the second reflux ratio controller 10, and then flow into the storage pipe 806 through the three-way pipe 801. At this time, the sampling tank 9 is still isolated from the outside air and will not leak. Then close the discharge valve 805 to isolate the sampling tank 9 from the exhaust pipe 802 and the storage pipe 806. Then open the exhaust valve 803 to restore the air pressure in the exhaust pipe 802 and the storage pipe 806. Then open the drain valve 807 and the sample liquid flows smoothly into the sampling container through the drain port 808. This process will not affect the vacuum degree in the sampling tank 9.
[0028] In a preferred embodiment, the liquid distribution assembly includes: a liquid distributor 11, fixedly connected to the main frame 1 via two third steel pipe supports 105; a first collection bottle and a second collection bottle are connected to the liquid distributor 11 for collecting sample liquids under different operating conditions; and a switch valve connected to the first collection bottle 12 and the second collection bottle 13 is installed on the liquid distributor 11. The liquid distribution assembly also includes: a buffer tank 14, connected to the liquid distributor 11; and a venting valve 15 is installed on the buffer tank 14. The buffer tank 14 serves a protective function to prevent a large influx of gas from damaging the equipment during sudden venting at the end; the venting valve 15 is used to break the vacuum and release gas.
[0029] An electrical control box 16 is also installed on the main frame 1. The electrical control box 16 is electrically connected to the vent valve 15, the switching valve, the drain valve 807, the discharge valve 805, the exhaust valve 803, the first reflux ratio controller 6, the second reflux ratio controller 10, and the PTFE glass valve 509. All of the above structures are existing technologies and are readily available on the market. The first reflux ratio controller 6 and the second reflux ratio controller 10 are both magnetic reflux ratio controllers. The first steel pipe support 103, the second steel pipe support 104, and the third steel pipe support 105 have the same structure, all consisting of steel pipes and clamps. One end of the steel pipe is welded with a clamp, which is then connected to the target equipment.
[0030] Principle: During operation, the material in reaction flask 2 is heated in a heating bath. The generated steam is distilled through column 3 and then enters condenser 5 through top connection section 4 to exchange heat with the cooling medium and condense into liquid. The resulting liquid is split by the first reflux ratio controller 6. Part of the condensed liquid is returned to column 3 as reflux liquid through reflux pipe 7 to come into countercurrent contact with the rising steam. Component separation is achieved through multiple gas-liquid mass transfers. The other part of the liquid is retained in sampling tank 9, and then distributed from sampling tank 9 to the first collection bottle 12 or the second collection bottle 13 through liquid distributor 11. When sampling liquid is required... First, the discharge valve 805 is opened to introduce the sample liquid in the sampling tank 9 into the three-way pipe 801 through the second reflux ratio controller 10, and then flows into the storage pipe 806 through the three-way pipe 801. At this time, the sampling tank 9 is still isolated from the outside air and will not leak. Then, the discharge valve 805 is closed, and the sampling tank 9 is isolated from the exhaust pipe 802 and the storage pipe 806. Then, the exhaust valve 803 is opened to restore the air pressure in the exhaust pipe 802 and the storage pipe 806. Then, the drain valve 807 is opened, and the sample liquid flows smoothly into the sampling container through the drain port 808. This process will not affect the vacuum degree in the sampling tank 9.
[0031] The foregoing has shown and described the basic principles, main features, and advantages of this application. Those skilled in the art should understand that this application is not limited to the above embodiments, and various changes and modifications can be made without departing from the spirit and scope of this application; all such changes and modifications fall within the scope of the claims. The scope of protection of this application is defined by the appended claims and their equivalents.
Claims
1. A laboratory rectifying column, characterized in that, include: Main framework; A distillation column is fixedly connected to the main frame, and a reaction flask is connected to the distillation column. The condenser is connected to the distillation column via a top connection section. A first reflux ratio controller is connected to the bottom of the condenser for reflux extraction, and the first reflux ratio controller is connected to the top connection section of the tower through a reflux pipe; A sampling container is connected to the first reflux ratio controller. The sampling container includes a second reflux ratio controller and a sampler. The sampler is installed on the side wall of the sampling container, and the second reflux ratio controller is installed inside the sampling container. The second reflux ratio controller assists the sampler in sampling. A liquid distribution assembly, connected to the bottom of the sampling tank, is used to receive the sample liquid coming out of the sampling tank.
2. A laboratory rectifying column according to claim 1, characterized in that: The return pipe is equipped with a U-shaped structure, which forms a water seal during use to prevent steam from entering the first return ratio controller from the return pipe.
3. A laboratory rectifying column according to claim 2, characterized in that: The top of the condenser is equipped with a PTFE glass valve for controlling the vacuuming process.
4. A laboratory rectifying column according to claim 3, characterized in that: The condenser has an inner layer and an outer layer, and a transition cavity is formed between the inner layer and the outer layer. The inner layer is connected to the PTFE glass valve and the first reflux ratio controller.
5. A laboratory rectifying column according to claim 4, characterized in that: The inner layer is equipped with a condenser coil, which consists of two sets of spiral tubes arranged in concentric circles, with the inner spiral tubes and the outer spiral tubes intersecting in the axial projection.
6. A laboratory rectifying column according to claim 5, characterized in that: The condenser coil also includes a distribution pipe and a collection pipe, both of which are connected to two sets of spiral pipes. The distribution pipe is connected to the condensate inlet, the collection pipe is fixedly connected to the inner layer and is connected to the transition cavity, and the outer layer is provided with a condensate outlet, which is connected to the transition cavity.
7. A laboratory rectifying column according to claim 6, characterized in that: The top connecting section of the tower is provided with a gas phase outlet, which extends from the middle of the condenser through the outer and inner layers.
8. A laboratory rectifying column according to claim 1 or 7, characterized in that: The sampler includes: a three-way pipe that penetrates the side wall of the sampling tank and extends into the sampling tank, with its opening facing upwards; the three-way pipe is provided with an exhaust pipe and a liquid storage pipe, and a discharge valve is installed on the three-way pipe, the discharge valve being used to open or close the passage of the exhaust pipe and the liquid storage pipe; the exhaust pipe is provided with an exhaust port and an exhaust valve; the liquid storage pipe is provided with a drain port and a drain valve.
9. A laboratory rectifying column according to claim 8, characterized in that: The liquid distribution assembly includes a liquid distributor, which is fixedly connected to the main frame via a third steel pipe support. The liquid distributor is connected to a first collection bottle and a second collection bottle for collecting sample liquids under different working conditions.
10. A laboratory rectifying column according to claim 9, characterized in that: The liquid distribution assembly further includes a buffer tank connected to the liquid distributor, and the buffer tank is equipped with a vent valve.