CN112626349B - Continuous crystallization and purification device and crystallization and purification method for scattered metal - Google Patents
Continuous crystallization and purification device and crystallization and purification method for scattered metal Download PDFInfo
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 246
- 230000008025 crystallization Effects 0.000 title claims abstract description 246
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 74
- 239000002184 metal Substances 0.000 title claims abstract description 74
- 238000000746 purification Methods 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000001816 cooling Methods 0.000 claims abstract description 124
- 239000000110 cooling liquid Substances 0.000 claims abstract description 36
- 150000002739 metals Chemical class 0.000 claims abstract description 16
- 238000002844 melting Methods 0.000 claims abstract description 13
- 230000008018 melting Effects 0.000 claims abstract description 12
- 238000007790 scraping Methods 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 28
- 238000003860 storage Methods 0.000 claims description 20
- 238000009413 insulation Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 230000020169 heat generation Effects 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims 2
- 150000002910 rare earth metals Chemical class 0.000 claims 2
- 239000013078 crystal Substances 0.000 description 34
- 239000012452 mother liquor Substances 0.000 description 20
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 14
- 239000002826 coolant Substances 0.000 description 14
- 229910052733 gallium Inorganic materials 0.000 description 14
- 229910052738 indium Inorganic materials 0.000 description 11
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004857 zone melting Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000004781 supercooling Methods 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
本发明公开了一种稀散金属连续结晶提纯装置，包括冷却结晶系统，所述冷却结晶系统包括结晶单元与冷却单元；所述结晶单元包括结晶槽与旋转冷却器，所述旋转冷却器包括转盘和用于带动所述转盘转动的转轴，所述转盘的外缘上开设有结晶凹槽，所述转盘的下部浸入所述结晶槽内；所述冷却单元包括设于所述转盘外缘处并用于给转盘外缘提供结晶环境的冷却套和用于向冷却套内提供冷却液的冷却液供给系统。本发明还提供一种利用上述的稀散金属连续结晶提纯装置的结晶提纯方法。本发明的稀散金属连续结晶提纯装置结构简单，结晶提纯方法使用方便，可以实现低熔点稀散金属的高效、高纯度冷却结晶提纯。
The invention discloses a continuous crystallization and purification device for scattered metals, comprising a cooling and crystallization system, wherein the cooling and crystallization system includes a crystallization unit and a cooling unit; the crystallization unit includes a crystallization tank and a rotary cooler, and the rotary cooler includes a turntable and A rotating shaft for driving the turntable to rotate, a crystallization groove is formed on the outer edge of the turntable, and the lower part of the turntable is immersed in the crystallization groove; A cooling jacket for providing a crystallization environment to the outer edge of the turntable and a cooling liquid supply system for supplying cooling liquid into the cooling jacket. The present invention also provides a crystallization purification method utilizing the above-mentioned scattered metal continuous crystallization purification device. The continuous crystallization and purification device for scattered metals of the invention has a simple structure, and the crystallization purification method is convenient to use, and can realize high-efficiency and high-purity cooling crystallization purification of the scattered metals with low melting point.
Description
Technical Field
The invention belongs to the field of metal purification, and particularly relates to a crystallization purification device and a crystallization purification method.
Background
With the development of technology, the demand for high purity metals is increasing. Particularly, the demand of the market for the high-purity rare metal is further increased because the high-purity rare metal has irreplaceable effects in the high-tech field of modern equipment manufacturing such as chemical industry, solar photovoltaic, national defense, aerospace, signal image processing, catalysis, automobile industry and the like.
At present, the high-purity preparation of the rare metal becomes a hot spot of controversy layout of high and new technology enterprises and a key point of research and development of vast technologists. The existing research on the high-purity preparation of the rare metal mainly focuses on two aspects of equipment research and development and impurity behavior control. At present, the high purification preparation of the rare metal is mostly realized by adopting the modes of distillation, volatilization, monocrystal pulling, electrolysis, crystallization, zone melting, chemical purification or combination thereof and the like. For example, patent publication No. CN1619018A proposes a method for preparing ultra-pure gallium metal, which includes two processes of low-temperature electrolytic purification and zone melting purification. For example, patent publication No. CN102618734A proposes a mass production method for preparing high purity gallium, which cools the bottom of the crystallization vessel to obtain high purity gallium. As disclosed in patent publication No. CN107858523A, zone melting and directional solidification are simultaneously achieved by arranging several resistance heaters in sequence in a horizontal direction outside a quartz tube. For example, patent publication No. CN209052802U discloses a quartz boat for purifying and growing ultra-high purity germanium single crystal by horizontal zone melting method. For example, patent publication No. CN209039630U discloses a single crystal growth furnace for growing a high purity germanium single crystal by the Czochralski method. For example, patent publication No. CN103172038A provides a high-purity selenium preparation apparatus and method, wherein the preparation apparatus includes a rectification device, a temperature control device, a vacuum system, and a quartz ring.
The existing high-purification preparation process and device for the scattered metal have the main problems that: the solid-liquid separation of the crystallized crystals and the crystallization mother liquor is difficult and incomplete, the crystallization mother liquor is polluted by high-purity crystals due to the enrichment of a large amount of impurities, and the crystals are slow in purification speed, low in efficiency, low in yield, difficult to continuously carry out, further not beneficial to mechanical control and difficult to apply to mass production.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming the defects and shortcomings in the background technology and providing a scattered metal continuous crystallization purification device and a scattered metal continuous crystallization purification method which have the advantages of thorough separation of crystallized metal and mother liquor, high purity of crystallized metal, high purification efficiency and easy mechanical automatic production. In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a scattered metal continuous crystallization purification device comprises a cooling crystallization system, wherein the cooling crystallization system comprises a crystallization unit and a cooling unit; the crystallization unit comprises a crystallization tank and a rotary cooler, the rotary cooler comprises a rotary table and a rotating shaft for driving the rotary table to rotate, a crystallization groove is formed in the outer edge of the rotary table, and the lower part of the rotary table is immersed in the crystallization tank; the cooling unit comprises a cooling jacket arranged at the outer edge of the rotary disk and used for providing a crystallization environment for the outer edge of the rotary disk (namely used for cooling the outer edge of the rotary disk) and a cooling liquid supply system used for providing cooling liquid for the cooling jacket.
In the above continuous crystallization and purification device for scattered metals, preferably, the cooling jacket includes an inner cooling jacket and an outer cooling jacket, the outer edge of the turntable is clamped between the inner cooling jacket and the outer cooling jacket, and the installation positions of the inner cooling jacket and the outer cooling jacket are both higher than the liquid level in the crystallization tank. The cooling jacket is used for providing a cooling environment, and the cooling environment required by the rotary cooler can be ensured more stably by adopting a mode of wrapping the inner cooling jacket and the outer cooling jacket. The outer cooling sleeve directly covers the rotary table, and the rotary table can be hollowed out to be used for installing the inner cooling sleeve.
In the above continuous crystallization purification device for scattered metals, preferably, the device further comprises a scraping system, wherein the scraping system comprises a front scraper and a rear scraper, the front scraper is arranged on one side of the turntable, which leaves the crystallization tank and enters the cooling jacket, and the scraping end of the front scraper is positioned on steps on two sides of the crystallization groove; the rear scraper is arranged on one side, away from the cooling sleeve, of the rotary disc and entering the crystallization groove, the shape of the scraping end of the rear scraper is matched with that of the crystallization groove, and the scraping end of the rear scraper is arranged in the crystallization groove. The temperature of the outer edge of the rotary plate of the rotary cooler is lower when the outer edge of the rotary plate enters the crystallization tank, crystallization mother liquor in the crystallization tank can be crystallized on the rotary plate, the rotary plate further crystallizes after entering the cooling jacket, and considering that the gap between the outer cooling jacket and the rotary plate is smaller, if a front scraper is not arranged, crystalline substances on the steps on two sides of the crystallization groove can be attached to the outer cooling jacket, and the crystalline substances on the steps on two sides of the crystallization groove can be scraped off to enter the crystallization tank by arranging the front scraper, so that the problems can be well solved; in addition, the front scraper can also scrape the crystallization mother liquor brought up by the outer edge of the turntable, so that the crystallization mother liquor is prevented from entering the cooling jacket for crystallization. The crystallized material in the crystallization groove is a product required by people, and the crystallized product in the crystallization groove can be collected by controlling the shape of the rear scraper blade to be matched with the shape of the crystallization groove and then enters the next cooling crystallization system or the subsequent material receiving system. One or more crystallization grooves can be arranged, and when the crystallization grooves are arranged, the shape of the rear scraper blade is correspondingly changed to be matched with the shape of each crystallization groove.
In the above apparatus for continuously crystallizing and purifying a scattered metal, preferably, a plurality of pits are formed on a wall of the crystallization groove. The crystallization process generally needs seed crystals to promote the crystallization process and control the crystal form of the product, and the seed crystals need to be added into the crystallization groove when the crystallization purification device provided by the invention is used for the first time. According to the invention, the pits are formed in the inner wall of the crystallization groove, and a small part of crystallized crystals can be remained in the pits to serve as seed crystals for subsequent crystallization when the rear scraper scrapes materials, so that more products with better crystal forms can be obtained by rotating and crystallizing the rotary cooler every time. The quantity and the distribution mode of the pits are not limited, and the residual seed crystals in the crystallization groove after the scraping of the rear scraper can be ensured.
In the above continuous crystallization and purification device for scattered metals, preferably, the device further comprises a feeding system, wherein the feeding system comprises a storage tank, a heat insulation sleeve and a discharging chute, the heat insulation sleeve is arranged on the outer surface of the storage tank, and the storage tank is connected with the crystallization tank through the discharging chute. The insulation sleeve is used for keeping the temperature of the storage chute, and the discharging chute is provided with a discharging valve.
In the above continuous crystallization and purification device for scattered metals, preferably, the device further comprises a material receiving system, wherein the material receiving system comprises a remelting chute and a material receiving groove, an inlet end of the remelting chute is connected with an outlet of the cooling crystallization system, and an outlet end of the remelting chute is connected with the material receiving groove; and a first heater and a first temperature control system for sensing the temperature in the remelting chute and controlling the heat productivity of the first heater are arranged on the remelting chute. The product after crystallization is remelted by the remelting chute, so that the crystallized product can be remelted, and the fluidity is improved, so that the crystallized product can conveniently enter a next cooling crystallization system or enter a material receiving tank. The first heater and the first temperature control system can realize temperature control in the remelting chute.
In the above apparatus for purifying scattered metal by continuous crystallization, preferably, a second heater and a second temperature control system for sensing the temperature in the crystallization tank and controlling the heat generation of the second heater are disposed at the bottom of the crystallization tank. The second heater and the second temperature control system can realize temperature control in the crystallization tank, so that the crystallization material has certain fluidity in the crystallization tank.
In the above apparatus for continuously crystallizing and purifying scattered metals, preferably, the coolant supply system includes a coolant storage tank, a coolant inlet pipe, a coolant outlet pipe, a refrigerator, and a third temperature control system for sensing a temperature in the coolant storage tank and controlling a refrigerating capacity of the refrigerator, wherein an inlet of the coolant inlet pipe is connected to the coolant storage tank, an outlet of the coolant inlet pipe is connected to the cooling jacket, an inlet of the coolant outlet pipe is connected to the cooling jacket, and an outlet of the coolant outlet pipe is connected to the coolant storage tank. The cooling liquid supply system can realize the real-time control of the temperature of the cooling liquid so as to ensure the temperature in the cooling jacket and ensure the smooth proceeding of the crystallization process.
In the above continuous crystallization and purification apparatus for scattered metals, preferably, the cooling crystallization systems are connected in series and/or in parallel with a plurality of sets, and two adjacent cooling crystallization systems connected in series are connected by a remelting chute. The purity of the crystallized product can be further improved by adopting a plurality of cooling crystallization systems connected in series. The cooling crystallization system can realize continuous and multistage crystallization purification in series or in parallel or in series-parallel connection, and is beneficial to automatic control of the scattered metal crystallization purification process and continuous production of high-purity products.
In the above continuous crystallization and purification device for scattered metals, preferably, the device further comprises a closed protection box, and the cooling crystallization system and the material receiving system are both arranged in the closed protection box of the system. The function of the closed protection box is to provide an inert atmosphere or vacuum environment for crystallization.
As a general technical concept, the present invention also provides a crystallization purification method using the above scattered metal continuous crystallization purification apparatus, comprising the steps of:
s1: the temperature of each part reaches a preset value by adjusting each heater, each refrigerator and each temperature control system;
s2: starting a heat preservation program of a feeding system, feeding molten to-be-crystallized scattered metal into the crystallization tank through the feeding system, controlling the temperature in the crystallization tank to be 0-30 ℃ higher than the melting point of the to-be-crystallized scattered metal, starting the cooling unit after a crystallization mother liquor occupies a certain volume of the crystallization tank (such as 1/3-4/5 of the volume of the crystallization tank), and controlling the temperature in the cooling jacket to be 10-50 ℃ lower than the melting point of the to-be-crystallized scattered metal;
s3: and when the temperature of the outer edge of the rotary disc of the rotary cooler is 10-50 ℃ lower than the melting point of the to-be-crystallized scattered metal, starting the rotary cooler, starting the scraping system, enabling the rotary cooler to rotate at a certain speed (the rotating speed is 0.05-2r/min), scraping the to-be-crystallized scattered metal positioned in the crystallization groove, and enabling the to-be-crystallized scattered metal to enter a material receiving system, thus finishing the crystallization purification of the to-be-crystallized scattered metal. If a plurality of cooling crystallization systems are adopted, the crystallized scattered metal in the crystallization groove in the first cooling crystallization system is scraped and enters the next cooling crystallization system or systems through a remelting chute (the temperature of the remelting chute is 0-30 ℃ higher than the melting point of the scattered metal to be crystallized), and finally enters a material receiving groove.
The continuous crystallization and purification device and the crystallization and purification method for the scattered metals are mainly applied to the cooling crystallization and purification of the scattered metals with low melting points, such as gallium, indium and the like. According to the invention, by utilizing the temperature difference between the rotary cooler and the crystallization tank, when the rotary cooler is transferred into the crystallization tank, the feed liquid (namely the crystallization mother liquor) around the rotary cooler forms a certain supercooling degree, so that the feed liquid is crystallized on the rotary cooler, the crystals of the rotary cooler are separated from the rotary cooler through the scraping system and enter the next equipment unit or the receiving system, the continuous and automatic operation of the crystallization process can be realized, the problem of separation of the crystallized crystals and the crystallization mother liquor is avoided, the purity of the crystallized crystals is higher, and the purification efficiency is higher.
Compared with the prior art, the invention has the advantages that:
1. the scattered metal continuous crystallization and purification device provided by the invention utilizes the temperature difference between the rotary cooler and the crystallization tank, and when the rotary cooler is rotated into the crystallization tank, the crystallization mother liquor around the rotary cooler forms a certain supercooling degree, so that the crystallization mother liquor is crystallized on the rotary cooler, the continuous and automatic operation of the crystallization process can be realized, the speed is high, the purification efficiency is high, the yield is high, the problem of separation of the crystallization crystal and the crystallization mother liquor is not needed, and the purity of the crystallization crystal is higher.
2. The scattered metal continuous crystallization and purification device disclosed by the invention is simple in structure, the crystallization and purification method is convenient to use, and the high-efficiency and high-purity cooling, crystallization and purification of low-melting scattered metal can be realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a scattered metal continuous crystallization purification device in an embodiment (two cooling crystallization systems are adopted).
FIG. 2 is a front view (with scraper system) of a crystallizing unit of the apparatus for continuous crystallization and purification of scattered metal in the example.
FIG. 3 is a top view (with scraper system) of the crystallizing unit of the continuous crystallizing purification apparatus for scattered metal in the example.
Illustration of the drawings:
1. a crystallization tank; 2. a rotary cooler; 3. a turntable; 4. a rotating shaft; 5. a crystallization groove; 6. a cooling jacket; 61. cooling the sleeve in the inner mode; 62. an outer cooling jacket; 7. a front squeegee; 8. a rear squeegee; 9. a step; 10. a pit; 11. a storage tank; 12. a thermal insulation sleeve; 13. a discharge chute; 14. remelting a chute; 15. a material receiving groove; 16. a first heater; 17. a first temperature control system; 18. a second heater; 19. a second temperature control system; 20. a coolant reservoir; 21. a coolant inlet pipe; 22. a coolant outlet pipe; 23. a refrigerator; 24. a third temperature control system; 25. and (5) sealing the protection box.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The apparatus for purifying scattered metal by continuous crystallization in the following examples 1 to 4, as shown in fig. 1 to 3, comprises one or more cooling crystallization systems, each of which comprises a crystallization unit and a cooling unit; the crystallization unit comprises a crystallization tank 1 and a rotary cooler 2, the rotary cooler 2 comprises a rotary table 3 and a rotating shaft 4 for driving the rotary table 3 to rotate, a crystallization groove 5 is formed in the outer edge of the rotary table 3, and the lower part of the rotary table 3 is immersed in the crystallization tank 1; the cooling unit comprises a cooling jacket 6 arranged at the outer edge of the rotating disc 3 and used for providing a crystallization environment for the outer edge of the rotating disc 3 and a cooling liquid supply system used for supplying cooling liquid into the cooling jacket 6.
In this embodiment, the cooling jacket 6 includes an inner cooling jacket 61 and an outer cooling jacket 62, the outer edge of the turntable 3 is sandwiched between the inner cooling jacket 61 and the outer cooling jacket 62, and the installation positions of the inner cooling jacket 61 and the outer cooling jacket 62 are both higher than the liquid level in the crystallization tank 1.
As shown in fig. 3, in this embodiment, the apparatus further comprises a scraping system, the scraping system comprises a front scraper 7 and a rear scraper 8, the front scraper 7 is disposed on one side of the rotary table 3 away from the crystallization tank 1 and entering the cooling jacket 6, and a scraping end of the front scraper 7 is located on steps 9 on two sides of the crystallization tank 5; the rear scraper 8 is arranged on one side of the rotary disc 3, which is away from the cooling jacket 6 and enters the crystallization tank 1, the shape of the scraping end of the rear scraper 8 is matched with that of the crystallization groove 5, and the scraping end of the rear scraper 8 is arranged in the crystallization groove 5. The arrangement of the front screed 7 and the rear screed 8 shown in fig. 3 is only one preferred arrangement in the present embodiment, and only the requirements of the present embodiment can be met.
In this embodiment, a plurality of pits 10 are provided on the wall of the crystallization groove 5.
In this embodiment, still include charging system, charging system includes stock chest 11, insulation cover 12 and blowing chute 13, and 11 surfaces of stock chest are located to insulation cover 12, and stock chest 11 passes through blowing chute 13 and links to each other with crystallizer 1.
In the embodiment, the material receiving system comprises a remelting chute 14 and a material receiving groove 15, wherein the inlet end of the remelting chute 14 is connected with the outlet of the cooling crystallization system, and the outlet end of the remelting chute 14 is connected with the material receiving groove 15; the remelting chute 14 is provided with a first heater 16 and a first temperature control system 17 for sensing the temperature in the remelting chute 14 and controlling the heat generation of the first heater 16.
In this embodiment, the bottom of the crystallization tank 1 is provided with a second heater 18 and a second temperature control system 19 for sensing the temperature in the crystallization tank 1 and controlling the heat generation of the second heater 18.
In the present embodiment, the cooling liquid supply system includes a cooling liquid storage tank 20, a cooling liquid inlet pipe 21, a cooling liquid outlet pipe 22, a refrigerator 23, and a third temperature control system 24 for sensing the temperature in the cooling liquid storage tank 20 and controlling the refrigerating capacity of the refrigerator 23, the inlet end of the cooling liquid inlet pipe 21 is connected to the cooling liquid storage tank 20, the outlet end of the cooling liquid inlet pipe 21 is connected to the cooling jacket 6, the inlet end of the cooling liquid outlet pipe 22 is connected to the cooling jacket 6, and the outlet end of the cooling liquid outlet pipe 22 is connected to the cooling liquid storage tank 20.
In this embodiment, two cooling crystallization systems (optionally, a plurality of cooling crystallization systems) are connected in series, and two adjacent cooling crystallization systems are connected through the remelting chute 14.
In this embodiment, the system further comprises a closed protection box 25, and the cooling crystallization system and the material receiving system are both arranged in the closed protection box 25 of the system.
The crystallization purification method using the above apparatus for continuous crystallization purification of scattered metals of the present embodiment includes the following steps:
s1: adding molten to-be-crystallized scattered metal into a crystallization tank 1 through a feeding system, controlling the temperature in the crystallization tank 1 to be higher than the melting point of the to-be-crystallized scattered metal by 0-30 ℃, starting a cooling unit, and controlling the temperature in a cooling jacket 6 to be lower than the melting point of the to-be-crystallized scattered metal by 10-50 ℃;
s2: and when the temperature of the outer edge of the rotary disc 3 of the rotary cooler 2 is 10-50 ℃ lower than the melting point of the scattered metal to be crystallized, starting the rotary cooler 2, starting the scraping system, scraping the scattered metal to be crystallized in the crystallization groove 5, and enabling the scattered metal to enter the material receiving system, thus finishing the crystallization and purification of the scattered metal to be crystallized.
Example 1:
the crystallization purification method using the scattered metal continuous crystallization purification device (using two-stage cooling crystallization systems connected in series) shown in fig. 1 comprises the following steps:
(1) introducing ultra-high purity argon into the closed protection box 25;
(2) coating a layer of high-purity gallium with the purity of 7N on the crystallization groove 5 of each rotary cooler 2, and cooling, solidifying and adsorbing the gallium on the crystallization groove 5;
(3) controlling the temperature of cooling liquid in the cooling jacket 6 to be 10 ℃, controlling the temperature of the crystallization tank 1 to be 35 ℃ and controlling the temperature of the remelting chute 14 to be 45 ℃ through various temperature control systems;
(4) starting a feeding system, adding gallium crystallization mother liquor with the purity of 4N, starting a cooling unit when the volume of the gallium crystallization mother liquor is 2/3 of the volume of the crystallization tank 1, and rotating the rotary cooler 2 at 0.5r/min when the temperature of the rotary cooler 2 to be measured is stabilized at 10 ℃;
(5) starting the front scraper 7 and the rear scraper 8, scraping the crystal outside the crystallization groove 5 (namely on the step 9) by the front scraper 7 to return to the crystallization groove 1, and scraping the crystal in the crystallization groove 5 by the rear scraper 8 to enter a next cooling crystallization system through the remelting chute 14;
(6) and after the crystal in the next cooling crystallization system is scraped by the rear scraper 8, the crystal finally enters the material receiving tank 15 through the remelting chute 14 to obtain a crystallized product, and the purity of the crystallized product is measured to be 6N gallium.
Example 2:
the crystallization purification method using the scattered metal continuous crystallization purification device (but using a three-stage cooling crystallization system connected in series) as shown in fig. 1 comprises the following steps:
(1) introducing ultra-high purity argon into the closed protection box 25;
(2) coating a layer of high-purity gallium with the purity of 7N on the crystallization groove 5 of each rotary cooler 2, and cooling, solidifying and adsorbing the gallium on the crystallization groove 5;
(3) controlling the temperature of cooling liquid in the cooling jacket 6 to be 10 ℃, controlling the temperature of the crystallization tank 1 to be 35 ℃ and controlling the temperature of the remelting chute 14 to be 45 ℃ through various temperature control systems;
(4) starting a feeding system, adding gallium crystallization mother liquor with the purity of 4N, starting a cooling unit when the volume of the gallium crystallization mother liquor is 2/3 of the volume of the crystallization tank 1, and rotating the rotary cooler 2 at 0.5r/min when the temperature of the rotary cooler 2 to be measured is stabilized at 10 ℃;
(5) starting the front scraper 7 and the rear scraper 8, scraping the crystal outside the crystallization groove 5 (namely on the step 9) by the front scraper 7 to return to the crystallization groove 1, and scraping the crystal in the crystallization groove 5 by the rear scraper 8 to enter a next cooling crystallization system through the remelting chute 14;
(6) and after the crystal in the next cooling crystallization system is scraped by the rear scraper 8, the crystal finally enters the material receiving tank 15 through the remelting chute 14 to obtain a crystallized product, and the purity of the crystallized product is measured to be 7N gallium.
Example 3:
the crystallization purification method using the scattered metal continuous crystallization purification device (using two-stage cooling crystallization systems connected in series) shown in fig. 1 comprises the following steps:
(1) introducing ultra-high purity argon into the closed protection box 25;
(2) coating a layer of high-purity indium with the purity of 6N on the crystallization groove 5 of each rotary cooler 2, and cooling, solidifying and adsorbing the high-purity indium on the crystallization groove 5;
(3) controlling the temperature of cooling liquid in the cooling jacket 6 to be 25 ℃, controlling the temperature of the crystallization tank 1 to be 180 ℃ and controlling the temperature of the remelting chute 14 to be 170 ℃ through various temperature control systems;
(4) starting a feeding system, adding indium crystallization mother liquor with the purity of 4N, starting a cooling unit when the volume of the indium crystallization mother liquor is 2/3 of the volume of the crystallization tank 1, and enabling the rotary cooler 2 to rotate at the speed of 1r/min when the temperature of the rotary cooler 2 to be measured is stabilized at 25 ℃;
(5) starting the front scraper 7 and the rear scraper 8, scraping the crystal outside the crystallization groove 5 (namely on the step 9) by the front scraper 7 to return to the crystallization groove 1, and scraping the crystal in the crystallization groove 5 by the rear scraper 8 to enter a next cooling crystallization system through the remelting chute 14;
(6) and after the crystal in the next cooling crystallization system is scraped by the rear scraper 8, the crystal finally enters the material receiving groove 15 through the remelting chute 14 to obtain a crystallized product, and the purity of the crystallized product is measured to be 6N indium.
Example 4:
the crystallization purification method using the scattered metal continuous crystallization purification device (using two-stage cooling crystallization systems connected in series) shown in fig. 1 comprises the following steps:
(1) introducing ultra-high purity argon into the closed protection box 25;
(2) coating a layer of high-purity indium with the purity of 6N on the crystallization groove 5 of each rotary cooler 2, and cooling, solidifying and adsorbing the high-purity indium on the crystallization groove 5;
(3) controlling the temperature of cooling liquid in the cooling jacket 6 to be 5 ℃, controlling the temperature of the crystallization tank 1 to be 180 ℃ and controlling the temperature of the remelting chute 14 to be 170 ℃ through various temperature control systems;
(4) starting a feeding system, adding indium crystallization mother liquor with the purity of 4N, starting a cooling unit when the volume of the indium crystallization mother liquor is 2/3 of the volume of the crystallization tank 1, and enabling the rotary cooler 2 to rotate at 2r/min when the temperature of the rotary cooler 2 to be measured is stabilized at 5 ℃;
(5) starting the front scraper 7 and the rear scraper 8, scraping the crystal outside the crystallization groove 5 (namely the step 9) by the front scraper 7 to return to the crystallization groove 1, and scraping the crystal in the crystallization groove 5 by the rear scraper 8 to enter a next cooling crystallization system through the remelting chute 14;
(6) and after the crystal in the next cooling crystallization system is scraped by the rear scraper 8, the crystal finally enters the material receiving groove 15 through the remelting chute 14 to obtain a crystallized product, and the purity of the crystallized product is measured to be 6N indium.
Claims (9)
1. The continuous crystallization and purification device for the scattered metal is characterized by comprising a cooling crystallization system and a scraping system, wherein the cooling crystallization system comprises a crystallization unit and a cooling unit; the crystallization unit comprises a crystallization tank (1) and a rotary cooler (2), the rotary cooler (2) comprises a rotary table (3) and a rotating shaft (4) for driving the rotary table (3) to rotate, a crystallization groove (5) is formed in the outer edge of the rotary table (3), and the lower part of the rotary table (3) is immersed in the crystallization tank (1); the cooling unit comprises a cooling jacket (6) arranged at the outer edge of the rotary disc (3) and a cooling liquid supply system used for supplying cooling liquid into the cooling jacket (6);
the scraping system comprises a front scraper (7) and a rear scraper (8), the front scraper (7) is arranged on one side, away from the crystallization groove (1), of the rotary table (3) and entering the cooling jacket (6), and the scraping end of the front scraper (7) is positioned on steps (9) on two sides of the crystallization groove (5); rear scraper blade (8) are located carousel (3) leave cooling jacket (6), get into one side of crystallization groove (1), just the shape of the material end of scraping of rear scraper blade (8) with the shape phase-match of crystallization recess (5), the material end of scraping of rear scraper blade (8) is located in crystallization recess (5).
2. The continuous crystallization and purification device for rare metals according to claim 1, wherein the cooling jacket (6) comprises an inner cooling jacket (61) and an outer cooling jacket (62), the outer edge of the rotating disc (3) is clamped between the inner cooling jacket (61) and the outer cooling jacket (62), and the inner cooling jacket (61) and the outer cooling jacket (62) are both arranged at a position higher than the liquid level in the crystallization tank (1).
3. The continuous crystallization and purification device for scattered metal according to claim 1, wherein a plurality of pits (10) are formed on the wall of the crystallization groove (5).
4. The continuous crystallization and purification device for rare metals according to claim 1, further comprising a feeding system, wherein the feeding system comprises a storage tank (11), a heat insulation sleeve (12) and a discharge chute (13), the heat insulation sleeve (12) is arranged on the outer surface of the storage tank (11), and the storage tank (11) is connected with the crystallization tank (1) through the discharge chute (13).
5. The continuous crystallization and purification device for scattered metal as claimed in claim 1, further comprising a material receiving system, wherein the material receiving system comprises a remelting chute (14) and a material receiving tank (15), the inlet end of the remelting chute (14) is connected with the outlet of the cooling crystallization system, and the outlet end of the remelting chute (14) is connected with the material receiving tank (15); the remelting chute (14) is provided with a first heater (16) and a first temperature control system (17) for sensing the temperature in the remelting chute (14) and controlling the heat productivity of the first heater (16).
6. The continuous crystallization and purification device for rare earth metal as claimed in any one of claims 1-5, characterized in that the bottom of the crystallization tank (1) is provided with a second heater (18) and a second temperature control system (19) for sensing the temperature in the crystallization tank (1) and controlling the heat generation of the second heater (18).
7. The scattered metal continuous crystallization purification apparatus according to any one of claims 1 to 5, wherein the cooling liquid supply system comprises a cooling liquid storage tank (20), a cooling liquid inlet pipe (21), a cooling liquid outlet pipe (22), a refrigerator (23), and a third temperature control system (24) for sensing the temperature in the cooling liquid storage tank (20) and controlling the refrigerating capacity of the refrigerator (23), wherein the inlet end of the cooling liquid inlet pipe (21) is connected to the cooling liquid storage tank (20), the outlet end of the cooling liquid inlet pipe (21) is connected to the cooling jacket (6), the inlet end of the cooling liquid outlet pipe (22) is connected to the cooling jacket (6), and the outlet end of the cooling liquid outlet pipe (22) is connected to the cooling liquid storage tank (20).
8. The continuous crystallization and purification device for rare earth metal as claimed in any one of claims 1-5, wherein a plurality of cooling crystallization systems are arranged in series and/or in parallel, and two adjacent cooling crystallization systems in series are connected through a remelting chute (14).
9. A crystallization purification method using the scattered metal continuous crystallization purification apparatus according to any one of claims 1 to 8, characterized by comprising the steps of:
s1: adding molten to-be-crystallized scattered metal into the crystallization tank (1) through a feeding system, controlling the temperature in the crystallization tank (1) to be higher than the melting point of the to-be-crystallized scattered metal, starting the cooling unit, and controlling the temperature in the cooling jacket (6) to be lower than the melting point of the to-be-crystallized scattered metal;
s2: and when the temperature of the outer edge of the rotary disc (3) of the rotary cooler (2) is lower than the melting point of the to-be-crystallized scattered metal, the rotary cooler (2) is opened, the scraping system is started, the to-be-crystallized scattered metal in the crystallization groove (5) is scraped down and enters the receiving system, and then the crystallization and purification of the to-be-crystallized scattered metal are completed.
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