CN110538478B - High-quality anhydrous rare earth halide purifying device - Google Patents
High-quality anhydrous rare earth halide purifying device Download PDFInfo
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- CN110538478B CN110538478B CN201811271022.6A CN201811271022A CN110538478B CN 110538478 B CN110538478 B CN 110538478B CN 201811271022 A CN201811271022 A CN 201811271022A CN 110538478 B CN110538478 B CN 110538478B
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 56
- -1 rare earth halide Chemical class 0.000 title claims abstract description 55
- 238000001816 cooling Methods 0.000 claims abstract description 43
- 238000004821 distillation Methods 0.000 claims abstract description 40
- 230000007704 transition Effects 0.000 claims abstract description 40
- 230000005540 biological transmission Effects 0.000 claims abstract description 18
- 230000007246 mechanism Effects 0.000 claims abstract description 18
- 230000007797 corrosion Effects 0.000 claims abstract description 9
- 238000005260 corrosion Methods 0.000 claims abstract description 9
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 38
- 238000000746 purification Methods 0.000 claims description 20
- 239000011449 brick Substances 0.000 claims description 9
- 239000011819 refractory material Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 238000007599 discharging Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000005192 partition Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000010410 layer Substances 0.000 description 10
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- 239000002994 raw material Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000010963 304 stainless steel Substances 0.000 description 3
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 229910000619 316 stainless steel Inorganic materials 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 229910000856 hastalloy Inorganic materials 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 101710150336 Protein Rex Proteins 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
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- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a high-quality anhydrous rare earth halide purifying device, which comprises a vacuum distillation furnace; the vacuum distillation furnace comprises a distillation area and a collection area which are independently arranged and are communicated with each other; the distillation area comprises a furnace body and a furnace cover, and the furnace body is detachably connected with the furnace cover; the furnace cover is communicated with a vacuum system through a pipeline; the collection area comprises a collection cavity and a transition chamber; the collecting cavity is communicated with the furnace body and is connected with the transition chamber through a water-cooling high-vacuum gate valve; a collector is arranged in the transition chamber, and one side, far away from the water-cooling high-vacuum gate valve, of the collector is detachably connected with a transmission mechanism; the collector is movable between the transition chamber and the collection chamber under the influence of the transmission mechanism. The high-quality anhydrous rare earth halide purifying device can realize the purposes of high yield, corrosion resistance, separation of a distillation area and a collection area, partition temperature control, simple material feeding and discharging operation, low cost and large-scale preparation of high-quality anhydrous rare earth halide.
Description
Technical Field
The invention belongs to the field of manufacturing equipment special for new rare earth materials, and particularly relates to a device for preparing high-quality anhydrous rare earth halides through high-temperature purification.
Background
The rare earth halide is widely applied to the preparation of various rare earth compounds, medicines, scintillation crystals and other products. The rare earth halide is a compound formed by rare earth metal cations and halogen anions, and has a general formula of ReX 3, wherein Re represents one or more of La, ce, pr, nd and other rare earth elements, and X represents one or more of F, cl, br, I. Typically, rare earth halides exist in crystalline form containing some crystal water, and other rare earth halides are readily soluble in water, except that rare earth fluoride is insoluble in water. Most rare earth halides are deliquescent and undergo hydrolysis at high temperatures to form oxyhalides. The existing technology for preparing anhydrous rare earth halide generally introduces ammonium halide salt and rare earth oxyhalide into the product, and reduces the quality of the anhydrous rare earth halide.
The halogen element ions in the rare earth halide are very active in chemical property, and are easy to hydrolyze to generate acid mist after being contacted with moisture, so that the acid mist is easy to react with common materials such as various metals, and equipment corrosion is caused, various impurity ions are introduced into the device besides equipment damage, and corrosion resistance of the equipment is required to be considered in the production of anhydrous rare earth halide.
The anhydrous rare earth halide can be further purified by adopting a vacuum high-temperature purification method, and the vacuum high-temperature treatment can increase the difference of volatilizing capacities of different substances in the raw materials, so that the distillation of the anhydrous rare earth halide is accelerated, and the pure high-quality anhydrous rare earth halide is prepared. However, the existing anhydrous rare earth halide purifying device has certain defects: the products can be enriched at the cold end outside the collecting area of the device and even enter a vacuum unit to reduce the yield and corrode equipment; the sectional temperature control of each functional area cannot be performed; raw material impurity removal and product collection are carried out in the same cavity, so that the impurity content in the product is too high; complicated feeding and discharging processes in the production flow, and the like.
Disclosure of Invention
In view of the above, the invention aims to provide a high-quality anhydrous rare earth halide purifying device, which overcomes the defects of the prior art, can realize the purposes of high yield, corrosion resistance, separation of a distillation area and a collection area, partition temperature control, simple material feeding and discharging operation, low cost and large-scale preparation of high-quality anhydrous rare earth halide.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
A high-quality anhydrous rare earth halide purifying device comprises a vacuum distillation furnace; the vacuum distillation furnace comprises a distillation area and a collection area which are independently arranged and are communicated with each other;
The distillation area comprises a furnace body and a furnace cover, and the furnace body is detachably connected with the furnace cover; the furnace cover is communicated with a vacuum system through a pipeline;
the collection area comprises a collection cavity and a transition chamber; the collecting cavity is communicated with the furnace body and is connected with the transition chamber through a water-cooling high-vacuum gate valve; a collector is arranged in the transition chamber, and one side, far away from the water-cooling high-vacuum gate valve, of the collector is detachably connected with a transmission mechanism; when the water-cooling high-vacuum gate valve is opened, the transition chamber is communicated with the collecting cavity, and the collector can move between the transition chamber and the collecting cavity under the action of the transmission mechanism.
Further, the furnace body and the furnace cover are connected through a furnace cover flange; a corrosion-resistant distillation container, a cover plate and a heat shield are arranged in the furnace body; the distillation container is communicated with the collecting cavity; the top of the distillation container is movably connected with a cover plate, and the heat shield is arranged above the cover plate; the heat shield is fixedly connected to the furnace cover.
Further, the heat shield comprises a plurality of layers of heat shield plates which are mutually parallel and are independently positioned on the central shaft; the heat shield is arranged in parallel with the cover plate; and a gap is reserved between the edge of the cover plate and the inner wall of the furnace body.
Further, the vacuum system comprises a vacuum baffle valve, a filter tank and a vacuum pump which are sequentially connected by pipelines; the vacuum baffle valve is communicated with the furnace cover through a pipeline.
Further, a first heating sleeve is sleeved at the upper part outside the furnace body, and a second heating sleeve is sleeved at the lower part; the joint of the first heating sleeve and the second heating sleeve below the collecting cavity is provided with a heat-insulating refractory material layer; the first heating sleeve and the second heating sleeve comprise a refractory brick, and a plurality of electric furnace wires are embedded in the inner wall of the refractory brick at intervals; the first heating sleeve is an openable heating sleeve.
Further, the collecting cavity is a branch pipe arranged on the furnace body; a protection air valve is arranged on the collecting cavity; the outer surface of the collecting cavity is provided with a cooling unit.
Further, the branch pipe is made of metal or ceramic which can withstand high-temperature baking at 1200 ℃ and at least one atmospheric pressure; the cooling unit is a water cooling jacket or an air cooling jacket and other medium circulation cooling jackets or devices.
Further, the collector is detachably connected with the transmission mechanism through one of a fixed hasp, a turnbuckle, an electromagnet, a manipulator and a threaded screw thread; the collector is in sliding connection with the transition chamber and the collection chamber.
Further, the transmission mechanism is one of an air cylinder, a screw rod, a pull rod and a mechanical arm; the collector comprises a cylindrical barrel and a vertical plate; the vertical plate is arranged on the left side of the cylindrical barrel body and is integrally formed with the cylindrical barrel body; the joint of the vertical plate and the cylindrical barrel body is arc-shaped; the outer diameter of the cylindrical barrel is smaller than the inner diameter of the collecting cavity, the diameter difference of the cylindrical barrel and the collecting cavity is smaller than or equal to the inner diameter of the transition chamber, and the diameter difference of the cylindrical barrel and the collecting cavity is smaller than or equal to 10 mm; the cylindrical barrel body is connected with the transition chamber and the collecting cavity in a sliding way.
Furthermore, a flange blind plate is arranged at one end of the transition chamber, which is far away from the water-cooling high-vacuum gate valve, through a vacuum flange, and the flange blind plate can be opened and assembled and disassembled in the working state of the furnace body; the transmission mechanism passes through the flange blind plate and is connected with the collector; the transition chamber is provided with an air inlet for introducing the shielding gas and an air outlet for extracting the shielding gas.
Compared with the prior art, the high-quality anhydrous rare earth halide purifying device has the following advantages:
according to the high-quality anhydrous rare earth halide purifying device, the distillation area and the collection area are placed in different cabin bodies, so that the pollution of products can be prevented; the collection area is subjected to forced cooling, so that the collection efficiency can be ensured; the position of the collector is controlled through the transmission mechanism, so that the collector is isolated from evaporated impurities, the vacuum baffle valve is opened again to push the collector to the collecting cavity to collect products in the distillation process, the collector can be pulled back to the transition chamber after the collection is finished, the purpose that the collector can be independently replaced from the transition chamber on the premise of not cooling the furnace body and filling protective gas is achieved, the continuity of operation is improved, the saving time is suitable for batch production; the corrosion-resistant distillation container can be used for feeding a large amount of materials at one time; the temperature difference of the furnace body can be controlled by sectionally arranging the first heating sleeve and the second heating sleeve which can be opened and closed and arranging the cooling unit.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 is a schematic diagram of a front view of a high quality anhydrous rare earth halide purification apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram showing the front view of the heat insulation screen of the high-quality anhydrous rare earth halide purifying device according to the embodiment of the invention;
FIG. 3 is a top view of a single insulating baffle in a heat shield;
FIG. 4 is a schematic diagram showing the front view of the cover plate in the high-quality anhydrous rare earth halide purifying apparatus according to the embodiment of the present invention;
FIG. 5 is a schematic diagram showing the front view of a collector in a high quality anhydrous rare earth halide purification device according to an embodiment of the present invention;
FIG. 6 is a schematic side view of a vacuum valve plate in a high quality anhydrous rare earth halide purification device according to an embodiment of the present invention;
FIG. 7 is a schematic diagram showing the relative positions of a first heating jacket, a heat insulating refractory layer and a second heating jacket in a high quality anhydrous rare earth halide purification apparatus according to an embodiment of the present invention;
FIG. 8 is a cross-sectional view of a first heating mantle in a high quality anhydrous rare earth halide purification apparatus according to an embodiment of the present invention;
FIG. 9 is a cross-sectional view of a heat insulating refractory layer of a high quality anhydrous rare earth halide purification apparatus according to an embodiment of the present invention;
fig. 10 is a cross-sectional view of a second heating mantle in a high quality anhydrous rare earth halide purification apparatus according to an embodiment of the present invention.
Reference numerals illustrate:
1-a transmission mechanism; 2-fixing a hasp; 3-a collector; 301-a cylindrical barrel; 302-risers; 4-a cooling unit; 5-a furnace cover flange; 6-furnace cover; 7-vacuum flapper valve; 8-a vacuum pump; 9-a filter tank; 10-heat shield; 101-a heat insulation baffle; 102-a central axis; 103-fixing the nut; 11-cover plate; 12-a distillation vessel; 13-a furnace body; 14-a layer of heat insulating refractory material; 15-electric stove wires; 16-water-cooling high vacuum gate valve; 17-transition chamber; 18-a flange blind plate; 19-a protection air valve; 20-collecting cavity; 21-a first heating mantle; 2101-semicircular openings; 22-branch pipes; 23-a second heating mantle.
Detailed Description
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first", "a second", etc. may explicitly or implicitly include one or more such feature. In the description of the present invention, unless otherwise indicated, the meaning of "a plurality" is two or more.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art in a specific case.
The invention will be described in detail below with reference to the drawings in connection with embodiments.
As shown in fig. 1, a high quality anhydrous rare earth halide purification apparatus includes a vacuum distillation furnace; the vacuum distillation furnace comprises a furnace body 13, wherein the furnace body 13 can provide a sealed vacuum environment, a distillation area is arranged in the vertical direction in the vacuum environment, and a collection area is formed by a collection cavity 20 welded on the side part of the furnace body 13. The collecting cavity 20 is a branch pipe 22 welded on the side part of the furnace body 13, and the collecting cavity 20 is provided with a protection air valve 19. The branch pipe 22 is made of metal or ceramic which can withstand high temperature baking at 1200 ℃ and at least one atmospheric pressure, and is used for providing vacuum environment; the metal can be 304 stainless steel, 316 stainless steel, hastelloy, tungsten, molybdenum or other metal or alloy, and the ceramic can be quartz, corundum, zirconia, silicon carbide or other ceramic materials. Silicon carbide is preferred in this embodiment.
The distillation area comprises a distillation container 12, a cover plate 11, a heat shield 10 fixed on the furnace cover 6 by bolts and a furnace cover flange 5 connected with the furnace cover 6 in the furnace body 13 besides the furnace body 13. The distillation container 12 is a cylinder with a bottom and a branch pipe on the side wall, so that the distillation container 12 can be communicated with the collecting cavity 20; the top of the distillation vessel 12 is covered with a non-sealing cover plate 11, said cover plate 11 providing a guide for the steam while not affecting the vacuum evacuation, increasing the collection efficiency. A heat shield 10 fixed on the furnace cover 6 is arranged between the distillation container 12 and the furnace cover 6, the heat shield 10 is used for isolating heat radiation, the working temperature of the sealing gasket of the furnace cover flange 5 is ensured to be lower than the long-term use temperature, the service life of a sealing element is prolonged, and the vacuum environment can be maintained in a high vacuum state during working.
In this embodiment, as shown in fig. 2 and 3, the heat shield 10 includes 7 layers of heat shield plates 101 which are parallel to each other and are independently positioned on a central shaft 102, the central shaft 102 is a screw rod, and the heat shield plates 101 are fixed on the central shaft 102 by fixing nuts 103; the heat shield 10 is arranged in parallel with the cover plate 11; a gap is reserved between the edge of the cover plate 11 and the inner wall of the furnace body 13. As shown in fig. 4, the cover plate 11 is a circular flat plate with a handle, and directly covers the upper opening of the distillation container 12, gas is pumped out from the gap when the vacuum is pumped, and gravity causes the cover to semi-seal the distillation container 12 when the vacuum state is reached. The distillation container 12 can be used for containing raw materials or raw material containers, when the purification device is used, the furnace cover 6 and the cover plate 11 are opened, raw materials or raw material containers are added into the distillation container 12, and then the furnace cover 6 is covered, so that the purification device can start to work.
The furnace cover 6 is connected with a vacuum system through a vacuum pipeline, the vacuum system comprises a vacuum baffle valve 7, a filtering tank 9 and a vacuum pump 8, and the vacuum system can provide a high vacuum environment for the preferred embodiment of the invention and collect impurities and wastes generated by distillation.
In addition, as shown in fig. 1 and 7-10, an annular heat-insulating refractory material layer 14 with the thickness of 20mm is wrapped outside the furnace body 13 below the collecting cavity 20 and close to the collecting cavity 20, and refractory bricks are selected as the heat-insulating refractory material layer 14; a first heating sleeve 21 is arranged at a position of the furnace body 13 above the heat-insulating refractory material layer 14, a second heating sleeve 23 is arranged at a position of the furnace body 13 below the heat-insulating refractory material layer 14, and the first heating sleeve 21 and the second heating sleeve 23 are composed of a refractory brick and 8 electric furnace wires 15 which are arranged in grooves on the inner wall of the refractory brick at intervals; the temperature rise limit of the wire 15 is 1200 ℃. The refractory bricks and the electric furnace wires 15 form a heat supply structure of the preferred embodiment of the invention, and the first heating sleeve 21 and the second heating sleeve 23 are connected in series up and down and can independently control the temperature; the first heating jacket is an openable heating jacket, specifically, is composed of two semi-cylindrical heating jackets with semicircular openings 2101 at one ends, and can be separated to strengthen heat dissipation when heat dissipation is insufficient, so that the furnace body 13 is rapidly cooled when necessary, and further, the sectional temperature control process of distilling anhydrous rare earth halide is realized.
The refractory package constituting the first heating jacket 21 and the second heating jacket 23 may be replaced with a refractory fiber brick or a mixed refractory fiber product.
In addition, the collecting area includes, in addition to the side collecting chamber 20 of the furnace body 13, a water-cooled high vacuum gate valve 16 (the water-cooled interlayer is shown in the dotted line of the water-cooled high vacuum gate valve 16 in fig. 1) connected to the other end of the side collecting chamber 20, and a transition chamber 17 connected to the water-cooled high vacuum gate valve 16. The collecting cavity 20 is wrapped with a cooling unit 4, in this embodiment, the cooling unit 4 selects a water cooling jacket, and the water cooling jacket and the water cooling high vacuum gate valve 16 jointly reduce the temperature in the collecting area, so as to provide a large low-temperature difference for condensing anhydrous rare earth halide steam, accelerate the condensing rate, and improve the collecting efficiency. The water-cooling high vacuum gate valve 16 is commercially available, the inner gate can be controlled to lift by a knob to indirectly control the opening and closing of the valve, and the structure of the water-cooling high vacuum gate valve 16 is shown in fig. 6.
The water cooling jacket and the water cooling high vacuum gate valve 16 respectively comprise a water inlet and a water outlet for cooling circulating water, and the water inlet is connected with a water chiller to ensure cooling efficiency.
One end of the transition chamber 17, which is far away from the water-cooling high vacuum gate valve 16, is provided with a vacuum flange, the vacuum flange is connected with a flange blind plate 18, and the flange blind plate 18 can be opened and assembled and disassembled with the collector 3 in the working state of the furnace body 13. The flange blind plate 18 is provided with an interface, and is fixedly connected with a transmission mechanism 1, and the transmission mechanism 1 of the embodiment adopts a vacuum cylinder; the vacuum cylinder is connected via a vacuum dynamic seal to the collector 3 (the structure of the collector is shown in fig. 5) mounted in the transition chamber 17 via a fixed snap 2 inserted into the flange blind 18. When the water-cooled high vacuum gate valve 16 is opened, the transmission mechanism 1 (i.e. the vacuum cylinder) can enable the collector 3 to move between the transition chamber 17 and the collecting cavity 20, and can disconnect or restore the connection with the collector 3 at any time through the fixed buckle 2. Collector 3 is slidingly connected with transition chamber 17 and collection chamber 20. As shown in fig. 5, the collector 3 includes a cylindrical body 301 and a riser 302; the vertical plate 302 is arranged on the left side of the cylindrical barrel 301 and is integrally formed with the cylindrical barrel 301; the joint of the vertical plate 302 and the cylindrical barrel 301 is arc-shaped; the outer diameter of the cylindrical barrel 301 is smaller than the inner diameter of the collecting cavity 20, the diameter difference between the two is 5mm, and the inner diameter of the collecting cavity 20 is equal to the inner diameter of the transition chamber 17; the cylindrical body 301 is slidingly connected with the transition chamber 17 and the collection chamber 20. The transition chamber 17 is provided with an air inlet for introducing the shielding gas and an air outlet for extracting the shielding gas.
In the use process, the water-cooling high vacuum gate valve 16 can be used for controlling the on-off of the transition chamber 17 and the collecting cavity 20 besides connecting and fixing the transition chamber 17 and the collecting cavity 20, and when the water-cooling high vacuum gate valve 16 is used for disconnecting the transition chamber 17 and the collecting cavity 20, the gas pressure in the transition chamber 17 and the furnace body can be independently controlled through the protection gas valve 19. The water-cooling high vacuum gate valve 16 can be closed and the vacuum flange can be opened to replace the collector 3 when the high vacuum is achieved in the distillation area, so that the production process can be continuously carried out after a large amount of material is fed at one time, and the collector 3 is replaced without frequent operations such as pumping out, heating and cooling the distillation area.
In addition, when the raw materials of anhydrous rare earth halide are subjected to high-temperature impurity removal, the collector 3 can be sealed in the transition chamber 17 by using a water-cooling high-vacuum gate valve 16 and is physically isolated from impurity steam generated in the distillation container 12; when the anhydrous rare earth halide is distilled and purified, the water-cooling high-vacuum gate valve 16 can be opened again to push the collector 3 to the collecting cavity 20 through the transmission mechanism 1 (namely the vacuum cylinder), the water-cooling high-vacuum gate valve 16 is closed after the fixed buckle 2 is disconnected to retract to the vacuum cylinder, and the collector 3 is positioned in the cold end collecting cavity 20 of the distillation device in the preferred embodiment of the invention, so that the highest condensation efficiency is achieved, and the collecting yield of distilled products is ensured.
The furnace cover 6, the furnace body 13, the corrosion-resistant distillation container 12 and the cover plate 11 are made of one or more of 304 stainless steel, 316 stainless steel, hastelloy, quartz, tungsten and molybdenum; in this embodiment, 304 stainless steel is preferable.
In summary, the present invention separates impurities from products by vacuum high-temperature heat treatment of raw materials of anhydrous rare earth halide and then stage heat treatment of generated steam, and the collector 3 enters the high-efficiency collection chamber 20 with the cooling unit 4 only in the collection stage by separating the collection region from the distillation region, thereby being physically isolated from impurities. Finally, the collector 3 is handled separately in the transition chamber 17 without affecting the distillation. The problems that the existing anhydrous rare earth halide preparation device has dispersed products, no sectional temperature control, overlapping distillation and collection areas and complicated feeding and discharging operations are solved, the high-yield corrosion-resistant device is provided, the distillation and collection areas are separated and can be used for regional temperature control, the feeding and discharging operation is simple, and the high-quality anhydrous rare earth halide can be prepared in a low-cost and large-scale manner.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (9)
1. A high-quality anhydrous rare earth halide purifying device is characterized in that: comprises a vacuum distillation furnace; the vacuum distillation furnace comprises a distillation area and a collection area which are independently arranged and are communicated with each other;
The distillation area comprises a furnace body (13) and a furnace cover (6), and the furnace body (13) is detachably connected with the furnace cover (6); the furnace cover (6) is communicated with a vacuum system through a pipeline;
The collecting area comprises a collecting cavity (20) and a transition chamber (17); the collecting cavity (20) is communicated with the furnace body (13), and the collecting cavity (20) is connected with the transition chamber (17) through a water-cooling high-vacuum gate valve (16); a collector (3) is arranged in the transition chamber (17), and one side, far away from the water-cooling high-vacuum gate valve (16), of the collector (3) is detachably connected with a transmission mechanism (1); when the water-cooling high-vacuum gate valve (16) is opened, the transition chamber (17) is communicated with the collecting cavity (20), and the collector (3) can move between the transition chamber (17) and the collecting cavity (20) under the action of the transmission mechanism (1);
the collecting cavity (20) is a branch pipe (22) arranged on the furnace body (13); a protection air valve (19) is arranged on the collecting cavity (20); the outer surface of the collecting cavity (20) is provided with a cooling unit (4).
2. The high quality anhydrous rare earth halide purification device of claim 1, wherein: the furnace body (13) is connected with the furnace cover (6) through a furnace cover flange (5); a corrosion-resistant distillation container (12), a cover plate (11) and a heat shield (10) are arranged in the furnace body (13); the distillation vessel (12) is in communication with a collection chamber (20); a cover plate (11) is movably connected to the top of the distillation container (12), and the heat shield (10) is arranged above the cover plate (11); the heat shield (10) is fixedly connected to the furnace cover (6).
3. The high quality anhydrous rare earth halide purification device of claim 2, wherein: the heat shield (10) comprises a plurality of layers of heat shield plates (101) which are parallel to each other and are independently positioned on a central shaft (102); the heat shield (10) is arranged in parallel with the cover plate (11); a gap is reserved between the edge of the cover plate (11) and the inner wall of the furnace body (13).
4. The high quality anhydrous rare earth halide purification device of claim 2, wherein: the vacuum system comprises a vacuum baffle valve (7), a filtering tank (9) and a vacuum pump (8) which are sequentially connected by pipelines; the vacuum baffle valve (7) is communicated with the furnace cover (6) through a pipeline.
5. The high quality anhydrous rare earth halide purification device of claim 1, wherein: the upper part of the furnace body (13) is sleeved with a first heating sleeve (21), and the lower part is sleeved with a second heating sleeve (23); the joint of the first heating sleeve (21) and the second heating sleeve (23) below the collecting cavity (20) is provided with a heat-insulating refractory material layer (14); the first heating sleeve (21) and the second heating sleeve (23) comprise refractory bricks, and a plurality of electric furnace wires (15) are embedded in the inner walls of the refractory bricks at intervals; the first heating jacket (21) is an openable heating jacket.
6. The high quality anhydrous rare earth halide purification device of claim 1, wherein: the branch pipe (22) is made of metal or ceramic which can withstand high-temperature baking at 1200 ℃ and at least one atmospheric pressure; the cooling unit (4) is a medium circulation cooling sleeve.
7. The high quality anhydrous rare earth halide purification device of claim 1, wherein: the collector (3) is detachably connected with the transmission mechanism (1) through one of a fixed hasp (2), a turnbuckle, an electromagnet, a manipulator and a threaded screw thread; the collector (3) is slidingly connected with the transition chamber (17) and the collection chamber (20).
8. The high quality anhydrous rare earth halide purification device of claim 6, wherein: the transmission mechanism (1) is one of an air cylinder, a screw rod, a pull rod and a mechanical arm; the collector (3) comprises a cylindrical body (301) and a riser (302); the vertical plate (302) is arranged on the left side of the cylindrical barrel (301) and is integrally formed with the cylindrical barrel; the joint of the vertical plate (302) and the cylindrical barrel (301) is arc-shaped; the outer diameter of the cylindrical barrel body (301) is smaller than the inner diameter of the collecting cavity (20), the diameter difference of the two is smaller than 10mm, and the inner diameter of the collecting cavity (20) is smaller than or equal to the inner diameter of the transition chamber (17); the cylindrical body (301) is in sliding connection with the transition chamber (17) and the collecting chamber (20).
9. The high quality anhydrous rare earth halide purification device of claim 1, wherein: one end of the transition chamber (17) far away from the water-cooling high-vacuum gate valve (16) is provided with a flange blind plate (18) through a vacuum flange, and the flange blind plate (18) can be opened and assembled and disassembled with the collector (3) in the working state of the furnace body (13); the transmission mechanism (1) passes through the flange blind plate (18) to be connected with the collector (3); the transition chamber (17) is provided with an air inlet for introducing the shielding gas and an air outlet for extracting the shielding gas.
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| CN113893773B (en) * | 2021-10-11 | 2023-07-25 | 天津包钢稀土研究院有限责任公司 | Method for granulating high-purity anhydrous rare earth halide |
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