A vacuum rectifying head device for purification of sublimated material

Abstract

The utility model belongs to the technical field of pressure reduction rectification, especially relates to a pressure reduction rectification head device for sublimation material purification, including gas riser, primary condenser pipe, reflux pipe and secondary condenser pipe, the primary condenser pipe is connected between gas riser and reflux pipe, the inner tube of gas riser and the inner tube of primary condenser pipe are communicated, the inner tube of primary condenser pipe and the upper portion of reflux pipe are communicated, the fixed hopper is equipped in reflux pipe, the lower portion of fixed hopper is movably connected magnetic drainage column, the side of magnetic drainage column is equipped with positioning frame, the outer wall of reflux pipe is equipped with electromagnetic controller, the bottom of reflux pipe is connected with the lower portion of gas riser through drain pipe on one side, the other side is equipped with material outlet, the top of reflux pipe is connected secondary condenser pipe through two-way piston, the bottom and top of two-way piston are connected with reflux pipe and secondary condenser pipe through quick -mounting joint clamp respectively, the top of secondary condenser pipe is connected three -way piston. The utility model has high rectification efficiency and good product quality.

Description

Technical Field

[0001] This utility model belongs to the field of vacuum distillation technology, and in particular relates to a vacuum distillation head device for the purification of sublimation materials. Background Technology

[0002] Vacuum distillation is a technique that separates components in a mixture by utilizing the differences in their boiling points at sub-atmospheric pressure. It's a chemical unit operation that achieves efficient separation of liquid mixtures through multiple partial vaporization and condensation processes, simplifying material separation. However, because vacuum distillation requires a vacuum environment, vapor is also removed during the vacuuming process, reducing the yield of the distilled material. In particular, materials containing sublimable substances undergo accelerated sublimation at higher temperatures or lower pressures, resulting in even lower recovery rates and increased separation difficulty. Summary of the Invention

[0003] The technical problem to be solved by this invention is to provide a vacuum distillation head device for the purification of sublimated materials, suitable for the purification of sublimated materials in laboratory-level or industrial production. It can effectively separate sublimated substances from other mixtures.

[0004] To achieve the above objectives, the present invention adopts the following technical solution:

[0005] A vacuum distillation head device for purifying sublimated materials includes a gas riser, a primary condenser, a reflux pipe, and a secondary condenser. The primary condenser connects to the gas riser and the reflux pipe. The inner tube of the gas riser is connected to the inner tube of the primary condenser. The inner tube of the primary condenser is connected to the upper part of the reflux pipe. A fixed funnel is provided inside the reflux pipe. A magnetic guide column is movably connected to the lower part of the fixed funnel. A positioning frame is provided on one side of the magnetic guide column. An electromagnetic controller is provided on the outer wall of the reflux pipe. One side of the bottom of the reflux pipe is connected to the lower part of the gas riser through a drain pipe, and the other side is provided with a material outlet. The top of the reflux pipe is connected to the secondary condenser through a two-way piston. The bottom and top of the two-way piston are connected to the reflux pipe and the secondary condenser through quick-connect couplings, respectively. A three-way piston is connected to the top of the secondary condenser.

[0006] The top of the gas riser is equipped with a temperature sensing element.

[0007] The gas riser pipe is provided with an air inlet at its bottom.

[0008] The lower and upper sides of the primary condenser tube are respectively provided with a cooling water inlet and a cooling water outlet.

[0009] The secondary condenser tube has a serpentine inner tube inside its body, with a cold water outlet at the top and a cold water inlet at the bottom.

[0010] A shut-off valve is provided at the material outlet.

[0011] Compared with existing technologies, the beneficial effects of this utility model are:

[0012] 1. Compared with traditional distillation heads, this device adds a first-stage condenser, where the material vapor is first condensed, effectively separating some easily condensable components and reducing the burden on subsequent condensation.

[0013] 2. The secondary condenser is located above the primary condenser to prevent condensate from dripping and washing away the condensed sublimed material, thus preventing cross-contamination and ensuring the purity of subsequent fractions.

[0014] 3. The secondary condenser can further condense and recover the vapor that failed to be condensed by the primary condenser and was removed by the vacuum system, significantly improving the overall yield of the distillation material.

[0015] 4. The secondary condenser tube is connected by a two-way piston with a quick-connect coupling clamp, which can be disassembled and installed independently, facilitating the removal and collection of sublimated materials and improving operational convenience.

[0016] 5. The secondary condenser adopts a serpentine reflux condensation structure, which not only achieves secondary condensation, but also allows the sublimated vapor to condense into a solid inside, making it easy to collect high-purity sublimation products.

[0017] 6. This utility model has the advantages of high distillation efficiency, good product quality, simple structure and easy cleaning. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the structure of this utility model.

[0019] In the diagram: 1. Gas riser; 2. Temperature sensor; 3. Primary condenser; 4. Cooling water inlet; 5. Cooling water outlet; 6. Return pipe; 7. Fixed funnel; 8. Positioning frame; 9. Magnetic guide column; 10. Electromagnetic controller; 11. Drain pipe; 12. Material outlet; 13. Two-way piston; 14. Quick-connect coupling clamp; 15. Secondary condenser; 16. Three-way piston; 17. Cold water inlet; 18. Cold water outlet; 19. Shut-off valve; 20. Air inlet. Detailed Implementation

[0020] In the description of this utility model, it should be understood that the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Therefore, a feature defined with "first," "second," etc., may explicitly or implicitly include one or more of that feature. In the description of this utility model, unless otherwise stated, "a plurality of" means two or more.

[0021] Unless otherwise expressly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections or electrical connections; they can refer to direct connections or indirect connections through an intermediate medium; and they can refer to the internal connection between two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0022] like Figure 1 A vacuum distillation head device for purifying sublimated materials includes a gas riser 1, a primary condenser 3, a reflux pipe 6, and a secondary condenser 15. The primary condenser 3 is connected between the gas riser 1 and the reflux pipe 6. The inner tube of the gas riser 1 is connected to the inner tube of the primary condenser 3. The inner tube of the primary condenser 3 is connected to the upper part of the reflux pipe 6. A fixed funnel 7 is provided inside the reflux pipe 6. A magnetic guide column 9 is movably connected to the lower part of the fixed funnel 7. A positioning frame 8 is provided on one side of the magnetic guide column 9. An electromagnetic controller 10 is provided on the outer wall of the reflux pipe 6. One side of the bottom of the reflux pipe 6 is connected to the lower part of the gas riser 1 through a drain pipe 11, and the other side is provided with a material outlet 12. The top of the reflux pipe 6 is connected to the secondary condenser 15 through a two-way piston 13. The bottom and top of the two-way piston 13 are connected to the reflux pipe 6 and the secondary condenser 15 respectively through quick-connect coupling clamps 14. The top of the secondary condenser 15 is detachably connected to a three-way piston 16.

[0023] The top of the gas riser pipe 1 is equipped with a temperature measuring element 2.

[0024] The bottom of the gas riser pipe 1 is provided with an air inlet 20.

[0025] The lower and upper sides of the tube body of the primary condenser tube 3 are respectively provided with a cooling water inlet 4 and a cooling water outlet 5.

[0026] The secondary condenser tube 15 has a serpentine inner tube inside its body. The top end of the serpentine inner tube has a cold water outlet 18, and the bottom end of the serpentine inner tube has a cold water inlet 17.

[0027] The material outlet 12 is equipped with a shut-off valve 19.

[0028] Work process:

[0029] 1) One port of the three-way piston 16 at the top of the secondary condenser 15 is connected to a vacuum pump to maintain a vacuum. The mixed vapor containing sublimation substances from the distillation column enters the gas riser 1 through the inlet 20. The condensate condensed by the primary condenser 3 flows into the return pipe 6. The temperature measuring element 2 at the top of the gas riser 1 reflects the vapor temperature in real time.

[0030] 2) When distillation begins, the condensate flows out through the bottom of the fixed funnel in the reflux pipe 6, flows into the drain pipe 11 through the magnetic guide column 9, and returns to the gas riser pipe 1. During this period, the sublimed material rises into the secondary condenser pipe 15 and adheres to the inner wall of the secondary condenser pipe 15.

[0031] 3) As distillation proceeds, once the temperature detected by the temperature measuring element 2 at the top of the gas riser 1 remains constant, the bottom of the magnetic guide column 9 is tilted by the electromagnetic controller 10, so that the boiling point distilled liquid is guided to the material outlet 12.

[0032] 4) When the temperature fluctuates and rises again, repeat steps 2) and 3) until the distillation is complete.

[0033] 5) When the sublimated material needs to be collected during the process, close the two-way piston 13, open the quick-connect coupling clamp 14, turn the three-way piston 16 to the venting state, remove the current secondary condenser tube 15 for subsequent collection, quickly replace the new secondary condenser tube 15, turn the three-way piston 16 to the vacuum state, open the two-way piston 13, and continue the distillation process.

[0034] To make the objectives, technical solutions, and technical effects of this utility model clearer, the technical solutions in the embodiments of this utility model are now described clearly and completely. However, the embodiments described below are only some embodiments of this utility model, not all embodiments. All other embodiments obtained by those skilled in the art in conjunction with the embodiments of this utility model without creative effort are within the scope of protection of this utility model.

[0035] Example

[0036] A vacuum distillation head device for purifying sublimated materials includes a gas riser 1, a primary condenser 3, a reflux pipe 6, and a secondary condenser 15. A temperature sensing element 2 is provided at the top of the gas riser 1. An air inlet 20 is provided at the bottom of the gas riser 1.

[0037] A primary condenser 3 is connected between the gas riser pipe 1 and the return pipe 6. The primary condenser 3 is inclined, with its high end connected to the gas riser pipe 1 and its low end connected to the return pipe 6. Cooling water inlet 4 and cooling water outlet 5 are respectively provided on the lower and upper sides of the primary condenser 3.

[0038] The inner tube of the gas riser 1 is connected to the inner tube of the first-stage condenser 3. The inner tube of the first-stage condenser 3 is connected to the upper part of the return pipe 6. A fixed funnel 7 is provided inside the return pipe 6. A magnetic guide column 9 is movably connected to the lower part of the fixed funnel 7. A positioning frame 8 for supporting the magnetic guide column 9 is connected to the inner wall of the return pipe 6 on one side. An electromagnetic controller 10 is provided on the outer wall of the return pipe 6. One side of the bottom of the return pipe 6 is connected to the lower part of the gas riser 1 through a drain pipe 11. The drain pipe 11 is inclined downwards. A material outlet 12 is provided on the other side. A shut-off valve 19 is provided on the material outlet 12. The top of the return pipe 6 is connected to the second-stage condenser 15 through a two-way piston 13. The body of the second-stage condenser 15 is provided with a serpentine inner tube. A cold water outlet 18 is provided at the top of the serpentine inner tube, and a cold water inlet 17 is provided at the bottom of the serpentine inner tube. The bottom and top of the two-way piston 13 are connected to the return pipe 6 and the secondary condenser pipe 15 respectively via quick-connect coupling clamp 14, and the top port of the secondary condenser pipe 15 is inserted into the three-way piston 16.

[0039] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and basic spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A vacuum distillation head device for purifying sublimated materials, characterized in that, It includes a gas riser, a primary condenser, a reflux pipe, and a secondary condenser. The primary condenser connects to the gas riser and the reflux pipe. The inner tube of the gas riser is connected to the inner tube of the primary condenser. The inner tube of the primary condenser is connected to the upper part of the reflux pipe. A fixed funnel is installed inside the reflux pipe. A magnetic guide column is movably connected to the bottom of the fixed funnel. A positioning frame is installed on one side of the magnetic guide column. An electromagnetic controller is installed on the outer wall of the reflux pipe. One side of the bottom of the reflux pipe is connected to the lower part of the gas riser through a drain pipe, and the other side has a material outlet. The top of the reflux pipe is connected to the secondary condenser through a two-way piston. The bottom and top of the two-way piston are connected to the reflux pipe and the secondary condenser through quick-connect couplings, respectively. A three-way piston is connected to the top of the secondary condenser.

2. The vacuum distillation head apparatus for purifying sublimated materials according to claim 1, characterized in that, The top of the gas riser is equipped with a temperature sensing element.

3. The vacuum distillation head apparatus for purifying sublimated materials according to claim 1, characterized in that, The gas riser pipe is provided with an air inlet at its bottom.

4. The vacuum distillation head apparatus for purifying sublimated materials according to claim 1, characterized in that, The lower and upper sides of the primary condenser tube are respectively provided with a cooling water inlet and a cooling water outlet.

5. A vacuum distillation head apparatus for purifying sublimated materials according to claim 1, characterized in that, The secondary condenser tube has a serpentine inner tube inside its body, with a cold water outlet at the top and a cold water inlet at the bottom.

6. A vacuum distillation head apparatus for purifying sublimated materials according to claim 1, characterized in that, A shut-off valve is provided at the material outlet.

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