Decompression sublimation device

Abstract

A pressure reduction sublimation device comprises a heating pipe and a condensation crystallization pipe, the upper end of the heating pipe is detachably connected with a pressure reduction buffer pipe, the condensation crystallization pipe is inserted in the pressure reduction buffer pipe, the lower end of the condensation crystallization pipe is adjacent to the connecting position of the heating pipe and the pressure reduction buffer pipe, and the pressure reduction buffer pipe is provided with an air extraction opening which facilitates air extraction and pressure reduction. An inner pipe is arranged in the condensation crystallization pipe, a cooling cavity is formed between the inner pipe and the outer wall of a pipe body of the condensation crystallization pipe, and the pressure reduction buffer pipe and the heating pipe are matched for use, so that the distance between the lower end of the condensation crystallization pipe and the lower end of the heating pipe can be effectively increased, and the capacity of a sample is increased; and the length of the heating pipe can be reduced, so that the heating pipe is completely placed in the hot bath, sublimated gas is prevented from crystallizing on the inner wall of the heating pipe, when crystals need to be taken out, the decompression buffer pipe and the heating pipe are directly detached, and the crystals are prevented from being mixed with residues in the heating pipe.

Description

Technical Field

[0001] The utility model relates to the technical field of sublimation purification, in particular to a reduced pressure sublimation device. Background Art

[0002] The vacuum sublimation tube is an important instrument for separating and purifying substances with sublimation characteristics. It includes two processes: heating sublimation evaporation and cooling condensation crystallization of the crude compound to improve the purity of the compound. It plays a vital role in scientific research and experimental teaching.

[0003] The existing vacuum sublimation tube is generally composed of a heating tube and a condenser. The heating tube is used to place the sample, and the bottom of the condenser is placed in the heating tube for condensation and crystallization of the sublimated gas sample. In the existing vacuum sublimation device, the distance between the bottom of the condenser and the bottom of the heating tube is small, resulting in a small sample capacity available for sublimation, and the condensed product is easily exposed to sample residues and contaminated. In order to increase the sample capacity of the heating tube, the length of the heating tube is generally increased to increase the distance between the bottom of the condenser and the bottom of the heating tube.

[0004] However, increasing the length of the heating tube will cause the sublimated gas sample to crystallize prematurely at the upper part of the tube wall of the heating tube due to the heat exchange between the upper part of the heating tube wall and the air. When the sample crystals are collected after sublimation, they will fall into the sample residue at the bottom of the heating tube. Although the sample crystals and sample residue can be separated by certain methods, it cannot be guaranteed that the impurities can be completely separated. Repeated experiments will consume a lot of manpower, material resources and financial resources, which seriously affects the efficiency of scientific research and experimental teaching. Utility Model Content

[0005] In order to solve the technical problem in the above-mentioned background technology that the existing reduced pressure sublimation device lengthens the heating tube to increase the sample capacity, which causes the gas sample to crystallize prematurely on the wall of the heating tube, and the sample crystals and sample residues are difficult to separate, thus affecting the research or experimental efficiency, the utility model provides a reduced pressure sublimation device.

[0006] The technical solution of this utility model is as follows:

[0007] The utility model provides a reduced pressure sublimation device, comprising: a heating tube and a condensation crystallization tube. The upper end of the heating tube is detachably connected with a reduced pressure buffer tube, the condensation crystallization tube is inserted in the reduced pressure buffer tube, the lower end of the condensation crystallization tube is adjacent to the connection position between the heating tube and the reduced pressure buffer tube, and an exhaust port is provided on the reduced pressure buffer tube, which is convenient for exhausting and reducing pressure, reducing the temperature required for sublimation, and improving efficiency. An inner tube is provided in the condensation crystallization tube, and a cooling chamber is formed between the inner tube and the outer wall of the tube body of the condensation crystallization tube. Through the coordinated use of the reduced pressure buffer tube and the heating tube, the spacing between the lower end of the condensation crystallization tube and the lower end of the heating tube can be effectively increased, and the capacity of the sample can be increased. At the same time, the length of the heating tube can also be reduced, so that the heating tube is completely placed in the hot bath to prevent the sublimated gas from crystallizing on the inner wall of the heating tube. When it is necessary to take out the crystal, the reduced pressure buffer tube and the heating tube can be directly removed to avoid mixing of the crystal with the residue in the heating tube.

[0008] Preferably, the heating tube and the pressure reducing buffer tube, and the pressure reducing buffer tube and the condensation crystallization tube are in contact through frosted surfaces, which effectively ensures the sealing of the connection positions.

[0009] Preferably, the heating tube is an upper open structure, the heating tube includes a first tube body, the lower end of the first tube body is circular, the upper end of the first tube body is fixedly provided with a first frosted portion, the first frosted portion is a variable diameter structure, and the inner wall of the first frosted portion is a frosted surface.

[0010] Preferably, the pressure reducing buffer tube is a structure with openings at both ends, and the pressure reducing buffer tube includes a second tube body, and a second frosted portion with a variable diameter is fixedly provided at the lower end of the second tube body. The outer wall of the second frosted portion is a frosted surface, and the second frosted portion is inserted into the first frosted portion. Through the setting of the frosted surface and the inclined tube wall, the installation position of the pressure reducing buffer tube and the connection sealing with the heating tube can be effectively limited, which is convenient for assembly and use.

[0011] Preferably, a third frosted portion with a variable diameter is fixedly provided on the upper end of the second tube body, the inner wall of the third frosted portion is a frosted surface, and the air exhaust port is located between the second frosted portion and the third frosted portion.

[0012] Preferably, the condensation crystallization tube includes a third tube body, a fourth frosted portion with a variable diameter is provided on the third tube body, the outer wall of the fourth frosted portion is a frosted surface, and the fourth frosted portion is inserted into the third frosted portion. Through the setting of the frosted surface and the inclined tube wall, the installation position of the condensation crystallization tube and the connection sealing with the pressure reducing buffer tube can be effectively limited, which is convenient for assembly and use.

[0013] Preferably, the lower end of the third tube body is circular, the upper end of the third tube body is provided with a water inlet, the water inlet is connected to the inner tube, and the third tube body is also provided with a water outlet, which is close to the upper end of the third tube body.

[0014] Preferably, the inner tube is connected to the third tube body, and there is a distance between the lower end of the inner tube and the lower end of the third tube body, so as to ensure sufficient heat exchange and condensation effect of the condensed water.

[0015] Preferably, the fourth grinding portion is located below the water outlet, thereby avoiding contact and collision between the water outlet and the pressure reducing buffer tube.

[0016] Preferably, the water inlet, the water outlet and the air suction port are all provided with anti-slip grooves to prevent the hose from slipping.

[0017] It can be seen from the above technical solutions that the advantages of the utility model are:

[0018] 1. By using the reduced pressure buffer tube in conjunction with the heating tube, the distance between the lower end of the condensation crystallization tube and the lower end of the heating tube can be effectively increased, thereby increasing the sample capacity. At the same time, the length of the heating tube can be reduced, so that the heating tube can be completely placed in the heat bath to prevent the sublimated gas from condensing and crystallizing on the inner wall of the heating tube, so that the condensation process generated by heat exchange with the air is carried out at the tube wall of the reduced pressure buffer tube. When it is necessary to remove the crystals, the reduced pressure buffer tube and the heating tube can be directly removed, thereby avoiding mixing of the crystals with the residue in the heating tube.

[0019] 2. The heating tube and the pressure reducing buffer tube, as well as the pressure reducing buffer tube and the condensing crystallization tube are connected through the variable diameter frosted part, which can not only effectively limit the installation position, facilitate positioning and disassembly and assembly, and improve the use efficiency, but also ensure the sealing of the connection position and ensure the effective implementation of the vacuum and pressure reduction work. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the technical solution of the utility model, the drawings required for use in the description will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0021] Figure 1 It is a schematic diagram of the overall structure of a vacuum sublimation device according to one or more embodiments of the present invention;

[0022] Figure 2 This is a schematic diagram of the structure of a heating tube according to one or more embodiments of the present invention;

[0023] Figure 3 It is a schematic structural diagram of a pressure reducing buffer tube according to one or more embodiments of the present invention;

[0024] Figure 4 This is a schematic diagram of the structure of a condensation crystallization tube according to one or more embodiments of the present invention;

[0025] The components represented by the reference numerals in the figure are:

[0026] 1. Heating tube; 11. First tube body; 12. First frosting part;

[0027] 2. Decompression buffer tube; 21. Second tube body; 22. Second frosted part; 23. Third frosted part; 24. Air extraction port;

[0028] 3. Condensation crystallization tube; 31. Third tube body; 32. Fourth frosting part; 33. Water inlet; 34. Water outlet; 35. Inner tube. DETAILED DESCRIPTION

[0029] In order to make the purpose, features and advantages of the utility model more obvious and easy to understand, the technical scheme of the utility model will be clearly and completely described below in combination with the drawings in the specific embodiment. Obviously, the embodiments described below are only part of the embodiments of the utility model, not all of them. Based on the embodiments in this patent, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this patent.

[0030] In a typical implementation of the present invention, Figure 1-Figure 4 As shown, a reduced pressure sublimation device is proposed, comprising: a heating tube 1, a reduced pressure buffer tube 2 and a condensation crystallization tube 3, wherein the reduced pressure buffer tube 2 is detachably mounted on the upper end of the heating tube 1, the condensation crystallization tube 3 is inserted into the interior of the reduced pressure buffer tube 2, the lower end of the condensation crystallization tube 3 is adjacent to the connection position between the heating tube 1 and the reduced pressure buffer tube 2, an inner tube 35 is provided inside the condensation crystallization tube 3, the inner tube 35 is used to transport condensed water into the condensation crystallization tube 3, and a cooling chamber is formed between the inner tube 35 and the outer wall of the tube body of the condensation crystallization tube 3.

[0031] By using the reduced pressure buffer tube 2 in conjunction with the heating tube 1, the distance between the lower end of the condensation crystallization tube 3 and the lower end of the heating tube 1 can be effectively increased, thereby increasing the capacity of the sample. At the same time, the length of the heating tube 1 can be reduced so that the heating tube 1 is completely placed in the heat bath to prevent the sublimated gas from crystallizing on the inner wall of the heating tube. Specifically, it can be understood that the traditional extended heating tube is improved into the heating tube 1 and the reduced pressure buffer tube 2 in this embodiment. While the overall length remains unchanged, the length of the heating tube 1 is reduced, thereby increasing the sample capacity and allowing the crystallization produced by heat exchange with the air to occur at the tube wall of the reduced pressure buffer tube 2. When the crystal needs to be removed, the reduced pressure buffer tube 2 and the heating tube 1 can be directly removed to avoid mixing of the crystal with the residue in the heating tube 1.

[0032] like Figure 2As shown, the heating tube 1 includes a first tube body 11 and a first frosted portion 12. The first frosted portion 12 is fixedly arranged at the upper end of the first tube body 11. The lower end of the first tube body 11 is circular, which increases the heating area and improves the sublimation efficiency. The first frosted portion 12 is connected to the interior of the first tube body 11. The first frosted portion 12 is a variable diameter structure. The upper end diameter of the first frosted portion 12 is larger than the lower end thereof, and the inner wall of the first frosted portion 12 is a frosted surface.

[0033] like Figure 3 As shown, the pressure reducing buffer tube 2 includes a second tube body 21, a second frosted portion 22 and a third frosted portion 23, wherein the second tube body 21 is an open structure at both ends, the second frosted portion 22 is fixedly arranged at the lower end of the second tube body 21, and the third frosted portion 23 is fixedly arranged at the upper end of the second tube body 21, and the second frosted portion 22 and the third frosted portion 23 are both variable diameter structures, the diameter of the lower end of the second frosted portion 22 is smaller than that of the upper end, and the diameter of the upper end of the third frosted portion 23 is larger than that of the lower end.

[0034] Among them, the outer wall of the second frosted part 22 is a frosted surface, and the inner wall of the third frosted part 23 is a frosted surface. The pressure reducing buffer tube 2 realizes a detachable connection with the heating tube 1 through the cooperation of the second frosted part 22 and the first frosted part 12. Specifically, the second frosted part 22 is inserted into the first frosted part 12. The setting of the variable diameter structure can effectively control the installation position of the pressure reducing buffer tube 2, facilitate positioning and disassembly, and the tube wall between the pressure reducing buffer tube 2 and the heating tube 1 is inclined and has a frosted surface, which effectively improves the connection sealing between the heating tube 1 and the pressure reducing buffer tube 2.

[0035] like Figure 3 As shown, the second tube body 21 is also provided with an exhaust port 24, which is located between the second frosted portion 22 and the third frosted portion 23, and is used to be connected to an exhaust hose, so that exhaust and decompression operations can be performed during the heating process to reduce the temperature required for sublimation. The exhaust port 24 is a variable diameter structure, and an annular anti-slip pattern is provided on the exhaust port 24 to prevent the exhaust hose from slipping.

[0036] like Figure 4 As shown, the condensation crystallization tube 3 includes a third tube body 31 and a fourth frosted portion 32. The lower end of the third tube body 31 is closed and circular, which increases the contact area and improves the condensation efficiency. A water inlet 33 is provided at the upper end of the third tube body 31, and a water outlet 34 is provided on the side wall of the third tube body 31, and the water outlet 34 is close to the upper end of the third tube body 31. The water inlet 33 is used to connect to the water inlet pipe, and the water outlet 34 is used to connect to the water outlet pipe, so as to facilitate the circulation of condensed water in the third tube body 31. Anti-slip patterns are provided on the water outlet 34 and the water inlet 33.

[0037] An inner tube 35 is provided inside the third tube body 31. Both ends of the inner tube 35 are open. The inner tube 35 extends along the length direction of the third tube body 31. One end of the inner tube 35 is fixedly connected and communicated with the water inlet 33, and the other end of the inner tube 35 is close to the lower end of the third tube body 31. In this embodiment, there is a distance of 1 cm between the lower end of the inner tube 35 and the lower end of the third tube body 31 to ensure sufficient heat exchange and condensation effect of the condensed water.

[0038] The fourth frosted portion 32 is fixedly disposed on the tube body of the third tube body 31, and the fourth frosted portion 32 is close to the upper end of the third tube body 31, and the fourth frosted portion 32 is located below the water outlet 34 to prevent the water outlet 34 from contacting and colliding with the pressure relief buffer tube 2;

[0039] The fourth frosted portion 32 is a variable diameter structure, the diameter of the lower end of the fourth frosted portion 32 is smaller than that of the upper end, the outer wall of the fourth frosted portion 32 is a frosted surface, and the fourth frosted portion 32 is inserted into the third frosted portion 23, so that the installation position of the condensation crystallization tube 3 is fixed and the connection sealing between the condensation crystallization tube 3 and the pressure reducing buffer tube 2 is ensured through the cooperation between the fourth frosted portion 32 and the third frosted portion 23, and the sealing is also achieved by the inclined tube wall cooperating with the frosted surface.

[0040] In this embodiment, the heating tube 1, the pressure reducing buffer tube 2 and the condensation crystallization tube 3 are all made of borosilicate glass and are connected through a ground mouth (i.e., a frosted part), which not only facilitates assembly and disassembly, but also ensures the sealing of the connection position.

[0041] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A vacuum sublimation device, comprising: The heating tube (1) and the condensation crystallization tube (3) are characterized in that the upper end of the heating tube (1) is detachably connected to a pressure reducing buffer tube (2), the condensation crystallization tube (3) is inserted into the pressure reducing buffer tube (2), the lower end of the condensation crystallization tube (3) is adjacent to the connection position between the heating tube (1) and the pressure reducing buffer tube (2), the pressure reducing buffer tube (2) is provided with an exhaust port (24), the condensation crystallization tube (3) is provided with an inner tube (35), and a cooling chamber is formed between the inner tube (35) and the outer wall of the tube body of the condensation crystallization tube (3).

2. A vacuum sublimation device according to claim 1, characterized in that: The heating tube (1) and the pressure reducing buffer tube (2), as well as the pressure reducing buffer tube (2) and the condensation crystallization tube (3) are in contact via frosted surfaces.

3. A vacuum sublimation device according to claim 2, characterized in that: The heating tube (1) is an upper open structure, comprising a first tube body (11), the lower end of the first tube body (11) is circular, a first frosted portion (12) is fixedly provided at the upper end of the first tube body (11), the first frosted portion (12) is a variable diameter structure, and the inner wall of the first frosted portion (12) is a frosted surface.

4. A vacuum sublimation device according to claim 3, characterized in that: The decompression buffer tube (2) is a structure with two ends open. The decompression buffer tube (2) comprises a second tube body (21). A second frosted portion (22) with a variable diameter is fixedly provided at the lower end of the second tube body (21). The outer wall of the second frosted portion (22) is a frosted surface. The second frosted portion (22) is inserted into the first frosted portion (12).

5. A vacuum sublimation device according to claim 3, characterized in that: A third frosted portion (23) with a variable diameter is fixedly provided at the upper end of the second tube body (21); the inner wall of the third frosted portion (23) is a frosted surface; and the air suction port (24) is located between the second frosted portion (22) and the third frosted portion (23).

6. A vacuum sublimation device according to claim 5, characterized in that: The condensation crystallization tube (3) comprises a third tube body (31), and a fourth frosted portion (32) with a variable diameter is provided on the third tube body (31). The outer wall of the fourth frosted portion (32) is a frosted surface, and the fourth frosted portion (32) is inserted into the third frosted portion (23).

7. A vacuum sublimation device according to claim 6, characterized in that: The lower end of the third tube body (31) is circular, the upper end of the third tube body (31) is provided with a water inlet (33), the water inlet (33) is communicated with the inner tube (35), and the third tube body (31) is also provided with a water outlet (34), which is close to the upper end of the third tube body (31).

8. A vacuum sublimation device according to claim 7, characterized in that: The inner tube (35) is communicated with the third tube body (31), and a gap is provided between the lower end of the inner tube (35) and the lower end of the third tube body (31).

9. A vacuum sublimation device according to claim 7, characterized in that: The fourth grinding portion (32) is located below the water outlet (34).

10. A vacuum sublimation device according to claim 7, characterized in that: The water inlet (33), the water outlet (34) and the air suction port (24) are all provided with anti-slip grooves.

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