Cooling receiver and vacuum distillation equipment

Abstract

The utility model discloses a cooling receiver and vacuum distillation equipment. The cooling receiver comprises a cooling cover in a cover shape with a downward opening; the easily-detached part comprises a plate-shaped part and a handle part which are connected into a whole, the plate-shaped part is attached to the inner side surface of the cooling cover in a covering mode, the handle part extends in the direction, pointing to the cooling cover, of the plate-shaped part and penetrates out of the cooling cover, and a through hole allowing the handle part to penetrate out is formed in the cooling cover; the fixing bolt penetrates through the section, exposed out of the cooling cover, of the handle part and makes contact with the outer side surface of the cooling cover, and a through hole for the fixing bolt to penetrate through is formed in the handle part; the receiving lining is separably clung to the surface of one side, back to the cooling cover, of the plate-shaped part in an extrusion manner; the fixing bolts can be taken out from the through holes where the fixing bolts are located, and under the condition that the fixing bolts are taken out, the easily-detached piece can be separated from the cooling cover. Distillation metal separation operation is simple and efficient, and the service life of the receiver is prolonged.

Description

Technical Field

[0001] This utility model relates to a cooling receiver and a vacuum distillation apparatus. Background Technology

[0002] Vacuum distillation is an important method in the field of metal preparation or purification, suitable for preparing or purifying low-boiling-point metals or metals that sublimate before reaching their boiling point. Compared to atmospheric distillation, vacuum distillation features lower distillation temperatures and faster distillation rates. A typical vacuum distillation apparatus consists of a vacuum furnace, a distillation crucible, and a cooling receiver. Inside the vacuum furnace, the sample to be distilled is placed in the distillation crucible, and the cooling receiver is placed on top. After evacuation and heating, metal vapor rises to the surface of the cooling receiver and condenses. The cooling receiver transfers the heat released during condensation to the furnace cavity through thermal radiation. After distillation, the cooling receiver is removed, and the distilled metal covering the inner surface of the cooling receiver is removed using traditional physical methods such as prying or hammering.

[0003] While traditional physical methods for extracting distilled metals can meet basic application requirements, they still have at least the following drawbacks in practical use: low extraction efficiency (taking tens of minutes to extract distilled metals using traditional physical methods), difficulty in collecting distilled metal debris, and pollution such as oxidation of the distilled metal; long-term use of traditional physical methods can reduce the toughness of the receiver, significantly reducing the service life of the cooling receiver. Therefore, we propose a cooling receiver for vacuum distillation to solve the above problems.

[0004] CN111424184B discloses a method for preparing high-purity ytterbium metal using a single continuous reducing distillation, wherein the receiver used is a barrel-shaped device with an open bottom and a closed top. This receiver suffers from the aforementioned problems during the process of removing the distilled metal. Utility Model Content

[0005] This invention provides a cooling receiver and a vacuum distillation apparatus.

[0006] This utility model adopts the following technical solution: a cooling receiver, comprising:

[0007] The cooling cover is shaped like a cover with the opening facing downwards.

[0008] The removable part includes a plate-shaped part and a handle that are integrated together. The plate-shaped part is attached to the inner surface of the cooling cover, and the handle extends along the plate-shaped part in the direction pointing to the cooling cover and passes through the cooling cover. The cooling cover has a through hole for the handle to pass through.

[0009] A fixing bolt passes through the section of the handle that is exposed outside the cooling cover and contacts the outer surface of the cooling cover, wherein the handle has a through hole for the fixing bolt to pass through;

[0010] The receiving liner is detachably and tightly pressed against the side surface of the plate-shaped portion opposite to the cooling cover by compression.

[0011] The fixing bolt can be removed from the through hole, and the removable part can be separated from the cooling cover when the fixing bolt is removed.

[0012] Optionally, the cooling cover defines a cylindrical internal space, the internal space of the cylinder extending in a vertical direction, the plate-like portion being in close contact with the inner top surface of the cooling cover, the receiving liner being a cover with an opening facing downwards, and the receiving liner also being in close contact with the inner circumferential surface of the cooling cover.

[0013] Optionally, the cooling cap defines a cylindrical internal space.

[0014] Optionally, the plate-like portion completely or partially covers the inner surface of the cooling cover.

[0015] Optionally, the plate-shaped portion is flat or divided into multiple plate-shaped regions, which are connected as one unit.

[0016] Optionally, the cooling cover is made of molybdenum, tantalum, or tungsten.

[0017] Optionally, the fixing bolt is made of molybdenum, tantalum, or tungsten.

[0018] Optionally, the removable part is made of stainless steel.

[0019] Optionally, the receiving liner is made of titanium.

[0020] Optionally, the central region of the inner surface of the cooling cover is higher than the edge region.

[0021] Optionally, the bottom section of the cooling cap defines a cylindrical internal space.

[0022] The present invention adopts the following technical solution: a vacuum distillation device, including the above-mentioned cooling receiver.

[0023] After the vacuum distillation process is completed, the cooling receiver is removed from the vacuum distillation equipment, the retaining pin is removed, and the force is evenly distributed on the plate-shaped part by tapping the handle, thereby separating the cooling cover from the removable part and the removable part from the receiving liner. The receiving liner, as a consumable, is separated from the distilled metal adhered to it using machining and scraping processes, thus obtaining high-purity distilled metal. This cooling receiver enables rapid separation of distilled metal from the removable part, improving production efficiency and yield, reducing contamination of the distilled metal, and extending its service life. Attached Figure Description

[0024] Figure 1 This is a cross-sectional view of the cooling receiver of this utility model.

[0025] Figure 2 This is a top view of the cooling receiver of this utility model.

[0026] Figure 3 This is a cross-sectional view of another cooling receiver of this utility model, in which the fixing bolt is omitted.

[0027] Figure 4 This is a cross-sectional view of another cooling receiver of this utility model, in which the fixing bolt is omitted.

[0028] The attached diagram is labeled as follows: 1. Cooling cover; 2. Removable part; 21. Plate-shaped part; 22. Handle; 3. Fixing bolt; 4. Receiving liner. Detailed Implementation

[0029] The present invention will be further described below with reference to specific embodiments, but the scope of protection of the present invention is not limited thereto.

[0030] Note: The vertical positional relationship described in this utility model refers to the spatial positional relationship of the cooling receiver in its usage state.

[0031] refer to Figures 1 to 4 This utility model provides a cooling receiver, comprising:

[0032] Cooling cover 1, which is a cover with the opening facing downwards;

[0033] The easy-to-remove part 2 includes a plate-shaped part 21 and a handle 22 that are integrated together. The plate-shaped part 21 is attached to the inner surface of the cooling cover 1, and the handle 22 extends along the direction of the plate-shaped part 21 toward the cooling cover 1 and passes through the cooling cover 1. The cooling cover 1 has a through hole for the handle 22 to pass through.

[0034] The fixing bolt 3 passes through the section of the handle 22 that is exposed outside the cooling cover 1 and contacts the outer surface of the cooling cover 1. The handle 22 has a through hole for the fixing bolt 3 to pass through.

[0035] The receiving liner 4 is detachably and tightly attached to the side surface of the plate-shaped portion 21 opposite to the cooling cover 1 by compression.

[0036] Among them, the fixing bolt 3 can be removed from the through hole, and the easy-to-remove part 2 can be separated from the cooling cover 1 when the fixing bolt 3 is removed.

[0037] In use, the removable part 2 is placed tightly against the inner surface of the cooling cover 1, and the retaining pin 3 is inserted into the handle 22 of the removable part 2 to secure it. Then, the receiving liner 4 is placed inside the cooling cover 1. The size of the receiving liner 4 is slightly larger than the size of the inner space of the cooling cover 1, and the receiving liner 4 is pressed into the inner space of the cooling cover 1.

[0038] After vacuum distillation, the cooling receiver is removed from the vacuum distillation equipment, the fixing bolt 3 is removed, and the force is evenly distributed on the plate-shaped part 21 by tapping the handle 22, thereby separating the cooling cover 1 from the removable part 2 and the removable part 2 from the receiving liner 4. The receiving liner 4, as a consumable, is separated from the distilled metal adhered to it using processes such as machining and scraping, thus obtaining high-purity distilled metal. This cooling receiver enables rapid separation of distilled metal from the removable part 2, improving production efficiency and yield, reducing contamination of the distilled metal, and extending its service life.

[0039] Optionally, refer to Figure 1 and Figure 2 The cooling cover 1 defines a cylindrical internal space, which extends vertically. The plate-shaped part 21 is in close contact with the inner top surface of the cooling cover 1. The receiving liner 4 is a cover with its opening facing downwards and is also in close contact with the inner circumferential surface of the cooling cover 1.

[0040] Optionally, the cooling cap 1 defines a cylindrical internal space. In other embodiments, the cooling cap 1 defines a polygonal cylindrical internal space.

[0041] Optionally, the plate-shaped portion 21 completely or partially covers the inner surface of the cooling cover 1.

[0042] Figure 1 In the illustrated embodiment, the plate-shaped portion 21 covers the inner top surface of the cooling cover 1. The plate-shaped portion 21 has the same shape and substantially the same size as the inner top surface of the cooling cover 1. To facilitate the removal of the removable part 2, the size of the plate-shaped portion 21 can be slightly smaller than the size of the inner top surface of the cooling cover 1.

[0043] Figure 3 and Figure 4 In the embodiment shown, the plate-shaped portion 21 completely covers the inner surface of the cooling cover 1.

[0044] In other embodiments, the shape of the cooling cover 1 is similar to... Figure 3 The embodiment shown is the same, the plate-shaped part 21 is flat, and the plate-shaped part 21 only covers the inner top surface of the cooling cover 1 (which is a planar area).

[0045] Optionally, refer to Figure 3 and Figure 4 The height of the inner surface of the cooling cover 1 is gradually increased, with the central area being higher than the edge area.

[0046] Figure 1 , Figure 3 and Figure 4 In the illustrated embodiment, the bottom section of the cooling cover 1 defines a cylindrical internal space. The cylindrical internal space extends vertically, facilitating integration with the internal structure of the vacuum distillation equipment.

[0047] Optionally, the plate-shaped portion 21 is flat or divided into multiple plate-shaped regions, which are connected as one unit.

[0048] Figure 1 In the illustrated embodiment, the plate-shaped portion 21 is flat.

[0049] Figure 3 In the embodiment shown, the plate-shaped portion 21 consists of a flat plate region, a first annular plate region (defining a frustum-shaped internal space), and a second annular plate region (defining a cylindrical internal space) from top to bottom.

[0050] Figure 4 In the embodiment shown, the plate-shaped portion 21 consists of a conical plate region (defining a conical internal space) and an annular plate region (defining a cylindrical internal space) from top to bottom.

[0051] refer to Figure 1 The handle 22 is columnar. There is one handle 2, which passes through the middle of the cooling cover 1. In other embodiments, there may be multiple handles 22, which extend in the vertical direction.

[0052] refer to Figure 1 and Figure 2 The retaining bolt 3 is rod-shaped. The cross-section of the retaining bolt 3 can be circular or polygonal. The contact area between the retaining bolt 3 and the outer top surface of the cooling cover 1 is straight or strip-shaped. The function of the retaining bolt 3 is to prevent the cooling cover 1 from separating from the removable part 2 and to ensure that the cooling cover 1 and the removable part 2 are in close contact.

[0053] The cooling cap 1 needs to have a high melting point and high heat exchange efficiency. Optionally, the material of the cooling cap 1 is molybdenum, tantalum or tungsten.

[0054] The fixing bolt 3 needs to have a high melting point and heat exchange efficiency. Optionally, the fixing bolt 3 can be made of molybdenum, tantalum, or tungsten.

[0055] The easy-removable part 2 needs to have a high melting point and heat exchange efficiency, as well as a certain strength and toughness to resist mechanical impact. Optionally, the easy-removable part 2 is made of stainless steel.

[0056] The receiving liner 4 needs to have a high melting point and heat exchange efficiency, and must also have appropriate plasticity to prevent it from breaking when being machined to the shape of the cooling cover 1. Optionally, the material of the receiving liner 4 is titanium.

[0057] The cooling receiver of this invention is suitable for receiving metals including but not limited to rare earth metals such as samarium (Sm), europium (Eu), ytterbium (Yb), thulium (Tm), dysprosium (Dy), terbium (Tb), holmium (Ho), erbium (Er), alkaline earth metals such as sodium (Na) and potassium (K), non-ferrous metals such as magnesium (Mg), zinc (Zn), and cadmium (Cd), ferrous metals such as manganese (Mn), and rare dispersed metals such as selenium (Se) and tellurium (Te).

[0058] Figure 1 In the illustrated embodiment, a suitable gap is left between the plate-shaped portion 21 and the inner circumferential surface of the cooling cover 1. Since the removable part 2 and the cooling cover 1 are made of different materials and have different coefficients of thermal expansion, this gap can prevent damage caused by mutual compression between the removable part 2 and the cooling cover 1.

[0059] This utility model adopts the following technical solution: a vacuum distillation apparatus, including the aforementioned cooling receiver. The structural details of the vacuum distillation apparatus can be designed according to existing technology. Specifically, the cooling receiver has its opening facing downwards, directly opposite the crucible inside the vacuum distillation apparatus.

[0060] The following combination Figure 1 and Figure 2 Here is a practical application example of this utility model.

[0061] (1) Load the industrial-grade metal Tb (melting point 1356℃) block into the purification crucible in the vacuum carbon tube furnace, install the purification crucible and the cooling receiver together, place them together in the vacuum carbon tube furnace, close the furnace cover, turn on the furnace body water cooling pump, start the mechanical pump, open the roughing valve, and turn on the Roots pump after the vacuum degree reaches the requirements of the Roots pump. After the vacuum degree in the furnace reaches 1~10Pa, close the roughing valve, open the main valve, and connect the diffusion pump or molecular pump to continue to increase the vacuum degree of the equipment.

[0062] (2) When the equipment vacuum degree reaches 10 -2 At Pa, the temperature is increased at 20℃ / min by a control program. After reaching 1400~1450℃, the temperature enters the heat preservation stage, which lasts for 500~800min.

[0063] (3) After the distillation stage is completed, disconnect the power to cool the furnace. After the furnace cools to room temperature, turn off the water cooling pump of the furnace body and the water cooling cover, open the furnace cover, remove the cooling receiver from the furnace body, pull out the fixing bolt 3 and physically knock the handle 22 of the easy-removable part 2 to achieve rapid separation of the receiving liner 4 from the cooling cover 1. Then further separate the distilled metal Tb from the receiving liner 4.

[0064] The various embodiments in this utility model are described in a progressive manner. The same or similar parts between the various embodiments can be referred to each other. Each embodiment focuses on describing the differences from other embodiments.

[0065] The scope of protection of this utility model is not limited to the above-described embodiments. Obviously, those skilled in the art can make various modifications and variations to this utility model without departing from its scope and spirit. If these modifications and variations fall within the scope of the claims of this utility model and their equivalents, then the intent of this utility model also includes these modifications and variations.

Claims

1. A cooling receiver, characterized in that, include: The cooling cover is shaped like a cover with the opening facing downwards. The removable part includes a plate-shaped part and a handle that are integrated together. The plate-shaped part is attached to the inner surface of the cooling cover, and the handle extends along the plate-shaped part in the direction pointing to the cooling cover and passes through the cooling cover. The cooling cover has a through hole for the handle to pass through. A fixing bolt passes through the section of the handle that is exposed outside the cooling cover and contacts the outer surface of the cooling cover, wherein the handle has a through hole for the fixing bolt to pass through; The receiving liner is detachably and tightly pressed against the side surface of the plate-shaped portion opposite to the cooling cover by compression. The fixing bolt can be removed from the through hole, and the removable part can be separated from the cooling cover when the fixing bolt is removed.

2. The cooling receiver according to claim 1, characterized in that, The cooling cover defines a cylindrical internal space, the internal space of which extends vertically. The plate-like portion is in close contact with the inner top surface of the cooling cover. The receiving liner is a cover with its opening facing downwards, and the receiving liner is also in close contact with the inner circumferential surface of the cooling cover.

3. The cooling receiver according to claim 2, characterized in that, The cooling cap defines a cylindrical internal space.

4. The cooling receiver according to claim 1, characterized in that, The plate-shaped portion completely covers the inner surface of the cooling cover.

5. The cooling receiver according to claim 1, characterized in that, The plate-shaped portion partially covers the inner surface of the cooling cover.

6. The cooling receiver according to claim 1, characterized in that, The plate-like portion is flat.

7. The cooling receiver according to claim 1, characterized in that, The plate-shaped portion is divided into multiple plate-shaped regions, which are connected as one unit.

8. The cooling receiver according to claim 1, characterized in that, The central region of the inner surface of the cooling cover is higher than the edge region.

9. The cooling receiver according to claim 1, characterized in that, The bottom section of the cooling cap defines a cylindrical internal space.

10. A vacuum distillation apparatus, characterized in that, Includes a cooling receiver according to any one of claims 1 to 9.

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