CN116377250A - Device and method for preparing high-purity magnesium ingot - Google Patents
Device and method for preparing high-purity magnesium ingot Download PDFInfo
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- CN116377250A CN116377250A CN202310264343.8A CN202310264343A CN116377250A CN 116377250 A CN116377250 A CN 116377250A CN 202310264343 A CN202310264343 A CN 202310264343A CN 116377250 A CN116377250 A CN 116377250A
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 65
- 239000011777 magnesium Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 212
- 238000010438 heat treatment Methods 0.000 claims abstract description 130
- 238000004821 distillation Methods 0.000 claims abstract description 112
- 239000012535 impurity Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 229910001338 liquidmetal Inorganic materials 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims 2
- 229910052751 metal Inorganic materials 0.000 abstract description 12
- 229920006395 saturated elastomer Polymers 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 9
- 239000007788 liquid Substances 0.000 description 7
- 238000000746 purification Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000005484 gravity Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
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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
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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
- C22B9/04—Refining by applying a vacuum
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- 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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- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a device and a method for preparing a high-purity magnesium ingot, comprising a distillation unit, a reaction unit and a reaction unit, wherein the distillation unit comprises a distillation crucible; the separation unit is connected with the distillation unit and comprises a plurality of separation chambers which are sequentially arranged along the gas volatilization direction; a collection unit comprising a plurality of collection chambers, each separation chamber being connected to at least one collection chamber; the heating unit comprises a distillation heating body, a plurality of separation chamber heating bodies and a plurality of collection chamber heating bodies, wherein each separation chamber is provided with at least one separation chamber heating body, and each collection chamber is provided with at least one collection chamber heating body; the vacuum unit comprises a vacuum cavity, the vacuum cavity is provided with an air inlet pipe, and the distillation unit, the separation unit and the collection unit are all arranged in the vacuum cavity. The method can directly obtain large-size high-purity magnesium ingots, and can realize the separation of metal impurity elements with different saturated vapor pressures, so that magnesium and other impurity metal elements with higher saturated vapor pressures can be separated, and the purity of distilled magnesium is effectively improved.
Description
Technical Field
The invention relates to the technical field of metal purification, in particular to a device and a method for preparing a high-purity magnesium ingot.
Background
The high-purity magnesium (more than or equal to 99.999%) is widely applied to the high-tech fields of electronic information, aerospace, biomedical and precision instruments and the like. At present, the method for preparing the high-purity magnesium mainly comprises a solvent refining method, a melt purifying method, an electrolytic refining method, a vacuum distillation method and the like. Magnesium has a low boiling point and is volatile, and as the pressure decreases, the vaporization temperature of magnesium can be reduced below the melting point, and the saturated vapor pressure is still higher. Thus, vacuum distillation is considered to be the most efficient method for preparing high purity magnesium (. Gtoreq.99.999%).
In the prior art, researchers have devised different purification devices, and U.S. patent No. 9677151B2 discloses a set of magnesium distillation and collection devices that condense magnesium vapor into a liquid that flows into a crucible to obtain a bulk high purity magnesium ingot. However, in the distillation apparatus disclosed in this patent, the collecting crucible is located in the distillation chamber, and magnesium and other volatile elements (e.g., zn, na, K, etc.) are simultaneously introduced into the collecting crucible during the actual distillation process, but the volatile elements are not completely separated from the magnesium element, and thus, the apparatus cannot be used to achieve the fractional purification of magnesium, and thus it is difficult to obtain a high purity magnesium ingot.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects in the prior art, and provide a device and a method for preparing a high-purity magnesium ingot, which can realize the separation of metal impurity elements with different saturated vapor pressures and can directly obtain the high-purity magnesium ingot.
In order to solve the technical problems, the invention provides a device for preparing a high-purity magnesium ingot, which comprises:
a distillation unit including a distillation crucible;
a separation unit connected to the distillation unit, the separation unit including a plurality of separation chambers sequentially arranged in a gas volatilization direction;
a collection unit comprising a plurality of collection chambers, each of said separation chambers being connected to at least one collection chamber;
the heating unit comprises a distillation heating body, a plurality of separation chamber heating bodies and a plurality of collection chamber heating bodies, wherein the distillation crucible is arranged in the distillation heating body, each separation chamber is provided with at least one separation chamber heating body, and each collection chamber is provided with at least one collection chamber heating body;
the vacuum unit comprises a vacuum cavity, the vacuum cavity is provided with an air inlet pipe, and the distillation unit, the separation unit and the collection unit are all arranged in the vacuum cavity.
Preferably, the temperature control unit comprises a temperature controller and a plurality of temperature measuring elements, the temperature controller is connected with the heating unit, the plurality of temperature measuring elements are respectively connected with the distillation unit, the separation unit and the collection unit, and the temperature controller is connected with the plurality of temperature measuring elements.
Preferably, a first steam outlet is formed in the distillation crucible, a distillation tube is arranged at the first steam outlet, a distillation tube heating body is arranged outside the distillation tube, and the distillation tube heating body is connected with the temperature controller.
Preferably, the separation unit comprises a first separation chamber, a second separation chamber and a third separation chamber which are sequentially arranged along the gas volatilization direction, the first separation chamber, the second separation chamber and the third separation chamber are coaxially arranged along the horizontal direction, the distillation crucible is connected with the air inlet of the first separation chamber through a distillation pipe, the air outlet of the first separation chamber is connected with the air inlet of the second separation chamber, the air outlet of the second separation chamber is connected with the air inlet of the third separation chamber, and the projections of the air inlet of the first separation chamber, the air inlet of the second separation chamber and the air inlet of the third separation chamber along the height direction are not overlapped.
Preferably, the first separation chamber comprises a first separation chamber heating body and a first separation crucible arranged in the first separation chamber heating body, the second separation chamber comprises a second separation chamber heating body and a second separation crucible arranged in the second separation chamber heating body, and the third separation chamber comprises a third separation chamber heating body and a third separation crucible arranged in the third separation chamber heating body.
Preferably, the collecting unit comprises a first collecting chamber connected with the first separating chamber, a second collecting chamber connected with the second separating chamber and a third collecting chamber connected with the third separating chamber, wherein an inlet of the first collecting chamber is positioned right below an outlet of the first separating chamber, an inlet of the second collecting chamber is positioned right below an outlet of the second separating chamber, and an inlet of the third collecting chamber is positioned right below an outlet of the third separating chamber.
Preferably, the first collecting chamber comprises a first collecting chamber heating body and a first collecting crucible arranged in the first collecting chamber heating body, the second collecting chamber comprises a second collecting chamber heating body and a second collecting crucible arranged in the second collecting chamber heating body, and the third collecting chamber comprises a third collecting chamber heating body and a third collecting crucible arranged in the third collecting chamber heating body.
Preferably, the first separating crucible and the first collecting crucible are connected by a first separating tube, the second separating crucible and the second collecting crucible are connected by a second separating tube, and the third separating crucible and the third collecting crucible are connected by a third separating tube.
Preferably, the first separation tube is provided with a first separation tube heating body outside, the second separation tube is provided with a second separation tube heating body outside, the third separation tube is provided with a third separation tube heating body outside, and the first separation tube heating body, the second separation tube heating body and the third separation tube heating body are all connected with a temperature controller.
Preferably, the vacuum unit further comprises a vacuum valve, a vacuum gauge and a vacuum pump unit, wherein the vacuum valve is arranged on the air inlet pipe, the vacuum pump unit comprises a vacuum pump, a first exhaust pipe and a second exhaust pipe, the vacuum pump is connected with the vacuum cavity through the first exhaust pipe, and the vacuum pump is further connected with the second exhaust pipe.
The invention also provides a method for preparing the high-purity magnesium ingot, which is carried out by adopting the device for preparing the high-purity magnesium ingot, and comprises the following steps:
step S1, loading raw materials to be processed into a distillation crucible;
step S2, vacuumizing the vacuum cavity, then filling inert gas into the vacuum cavity, and exhausting air of the vacuum cavity repeatedly in this way;
step S3, heating the distillation crucible, the separation chamber and the collection chamber, and heating the temperatures of the distillation unit, the separation chamber and the collection chamber to the designated temperature;
s4, collecting purified liquid metal through a collecting chamber, and sequentially entering other separating chambers to separate impurity elements;
and S5, after distillation, cooling to obtain the high-purity magnesium ingot.
Compared with the prior art, the technical scheme of the invention has the following advantages:
according to the device and the method for preparing the high-purity magnesium ingot, the distillation unit, the separation unit, the collection unit and the heating unit are arranged, raw materials to be processed are distilled in the distillation crucible of the distillation unit, magnesium vapor generated by distillation volatilizes from the distillation unit and enters the separation chamber to be condensed into liquid, the liquid enters the collection chamber arranged below the separation chamber under the action of gravity, the collection chamber is cooled to form the high-purity magnesium ingot, metal impurity elements with higher saturated vapor pressure volatilize into other separation chambers in sequence, and impurity elements are separated, so that the device can directly obtain the large-size high-purity magnesium ingot, can realize separation of metal impurity elements with different saturated vapor pressures, can separate magnesium from other impurity metal elements with higher saturated vapor pressure, effectively improves the purity of distilled magnesium, and meanwhile, the device provided by the invention adopts a modularized design, is easy to assemble and disassemble, is convenient to sample and clean, can expand according to requirements, and is provided with a plurality of separation chambers and collection chambers, and improves the purification efficiency.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings, in which
Fig. 1 is a schematic structural view of a preferred embodiment of the present invention.
FIG. 2 is a graph showing the results of a GDMS composition test of a high purity magnesium ingot prepared using the apparatus and method of the present invention.
Description of the specification reference numerals: 1. a distillation crucible; 10. a distillation crucible cover; 11. a distillation tube; 12. a distillation heating body; 13. a distillation heating body upper cover; 14. a distillation tube heating body; 2. a vacuum chamber; 21. an air inlet pipe; 22. a vacuum valve; 23. a vacuum gauge; 24. a vacuum pump; 25. a first exhaust pipe; 26. a second exhaust pipe; 3. a temperature controller; 40. a first separation chamber inlet; 41. a first separation chamber heating body; 42. a second separation chamber heating body; 43. a third separation chamber heating body; 50. a second separation chamber inlet; 51. a first separation crucible; 52. a second separation crucible; 53. a third separation crucible; 54. a first separator tube; 55. a second separation tube; 56. a third separation tube; 57. a first separator tube heating body; 58. a second separation tube heating body; 59. a third separator tube heating body; 60. a third separation chamber inlet; 61. a first collection chamber heating body; 62. a second collection chamber heating body; 63. a third collection chamber heating body; 71. a first collection crucible; 72. a second collection crucible; 73. a third collection crucible; 81. a first temperature measuring element; 82. a second temperature measuring element; 83. a third temperature measuring element; 84. a fourth temperature measuring element; 85. a fifth temperature measuring element; 86. a sixth temperature measuring element; 87. and a seventh temperature measuring element.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
Example 1
Referring to fig. 1 and 2, the present invention discloses an apparatus for preparing a high purity magnesium ingot, comprising,
the distillation unit comprises a distillation crucible 1, wherein a distillation crucible cover body 10 is arranged on the distillation crucible, raw materials to be processed are filled into the distillation crucible 1 when the distillation crucible is prepared, a steam outlet is arranged on the side wall of the upper part of the distillation crucible 10, and a distillation pipe 11 is arranged at the steam outlet;
the separation unit is connected with the distillation unit and comprises a plurality of separation chambers which are sequentially arranged along the gas volatilization direction, and the separation chambers are sequentially connected, wherein the separation chamber at the head end is communicated with the distillation crucible 1 through the distillation pipe 11;
a collection unit comprising a plurality of collection chambers, each of said separation chambers being connected to at least one collection chamber, said collection chambers being disposed below the separation chamber;
the heating unit comprises a distillation heating body 12, a plurality of separation chamber heating bodies and a plurality of collection chamber heating bodies, wherein the distillation crucible 1 is arranged in the distillation heating body 12, a distillation heating body upper cover 13 is arranged on the distillation heating body 12, at least one separation chamber heating body is arranged outside each separation chamber, and at least one collection chamber heating body is arranged outside each collection chamber;
the vacuum unit comprises a vacuum cavity 2, the vacuum cavity is provided with an air inlet pipe 21, and the distillation unit, the separation unit and the collection unit are all arranged in the vacuum cavity 2.
According to the device for preparing the high-purity magnesium ingot, which is to be protected by the invention, the distillation unit, the separation unit, the collection unit and the heating unit are arranged, raw materials to be processed are distilled in the distillation crucible of the distillation unit, magnesium vapor generated by distillation volatilizes from the distillation unit and enters the separation chamber to be condensed into liquid, the liquid enters the collection chamber arranged below the separation chamber under the action of gravity, the collection chamber is cooled to form the high-purity magnesium ingot, metal impurity elements with higher saturated vapor pressure volatilize into other separation chambers in sequence, and the impurity elements are separated.
Further, the device of the invention also comprises a temperature control unit, the temperature control unit comprises a temperature controller 3 and a plurality of temperature measuring elements, the temperature controller 3 is connected with the heating unit and controls the heating temperature of the heating unit, and the distillation heating body 12, the plurality of separation chamber heating bodies and the plurality of collection chamber heating bodies are all connected with the temperature controller 3. The temperature measuring elements are respectively connected with the distillation unit, the separation unit and the collection unit, and the temperature controller 3 is connected with the temperature measuring elements through connecting wires.
Further, a distillation tube heating body 14 is arranged outside the distillation tube 11, and the distillation tube heating body 14 is connected with the temperature controller 3.
Specifically, the separation unit comprises a first separation chamber, a second separation chamber and a third separation chamber which are sequentially arranged along the volatilization direction of gas, the first separation chamber, the second separation chamber and the third separation chamber are coaxially arranged along the horizontal direction, the distillation crucible 1 is connected with a first separation chamber air inlet through a distillation pipe 11, a first separation chamber air outlet is connected with a second separation chamber air inlet, and a second separation chamber air outlet is connected with a third separation chamber air inlet.
It should be noted that the projections of the first separation chamber air inlet 40, the second separation chamber air inlet 50 and the third separation chamber air inlet 60 along the height direction do not overlap, so that the volatilization path of the magnesium vapor in the separation unit can be prolonged, and the magnesium vapor can pass through the second separation chamber and the third separation chamber in a zigzag shape, thereby prolonging the volatilization path in the separation unit, and being beneficial to separation and purification.
In detail, the first separation chamber includes a first separation chamber heating body 4 and a first separation crucible 51 disposed in the first separation chamber heating body 41, the second separation chamber includes a second separation chamber heating body 42 and a second separation crucible 52 disposed in the second separation chamber heating body 42, the third separation chamber includes a third separation chamber heating body 43 and a third separation crucible 53 disposed in the third separation chamber heating body 43, and the first separation crucible 51, the second separation crucible 52, and the third separation crucible 53 are each provided with an upper cover.
Furthermore, the collecting unit comprises a first collecting chamber connected with the first separating chamber, a second collecting chamber connected with the second separating chamber, and a third collecting chamber connected with the third separating chamber, and the inlet of the first collecting chamber is positioned under the outlet of the first separating chamber, the inlet of the second collecting chamber is positioned under the outlet of the second separating chamber, and the inlet of the third collecting chamber is positioned under the outlet of the third separating chamber.
Further, the first collecting chamber comprises a first collecting chamber heating body 61 and a first collecting crucible 71 arranged in the first collecting chamber heating body 61, the second collecting chamber comprises a second collecting chamber heating body 62 and a second collecting crucible 72 arranged in the second collecting chamber heating body 62, the third collecting chamber comprises a third collecting chamber heating body 63 and a third collecting crucible 73 arranged in the third collecting chamber heating body 63, and the first collecting crucible 71, the second collecting crucible 72 and the third collecting crucible 73 are all provided with upper covers.
It should be noted that the first separating crucible 51 and the first collecting crucible 71 are connected by the first separating tube 54, the second separating crucible 52 and the second collecting crucible 72 are connected by the second separating tube 55, and the third separating crucible 53 and the third collecting crucible 73 are connected by the third separating tube 56.
Specifically, the first separation tube 54 is provided with a first separation tube heating body 57 at the outside, the second separation tube 55 is provided with a second separation tube heating body 58 at the outside, the third separation tube 56 is provided with a third separation tube heating body 59 at the outside, and the first separation tube heating body 57, the second separation tube heating body 58 and the third separation tube heating body 59 are all connected with the temperature controller 3.
From the detail, the vacuum unit further comprises a vacuum valve 22, a vacuum gauge 23 and a vacuum pump unit, wherein the vacuum valve 22 is arranged on the air inlet pipe 21, the vacuum pump unit comprises a vacuum pump 24, a first exhaust pipe 25 and a second exhaust pipe 26, the vacuum pump 24 is connected with the vacuum cavity 2 through the first exhaust pipe 25, the vacuum pump 24 is also connected with the outside through the second exhaust pipe 26, and the first exhaust pipe 25 adopts a corrugated pipe.
The bottom of the distillation crucible 1 is provided with a first temperature measuring hole, the top of the first separation crucible 51 is provided with a second temperature measuring hole, the top of the second separation crucible 52 is provided with a third temperature measuring hole, the top of the third separation crucible 53 is provided with a fourth temperature measuring hole, the bottom of the first collection crucible 71 is provided with a fifth temperature measuring hole, the bottom of the second collection crucible 72 is provided with a sixth temperature measuring hole, and the bottom of the third collection crucible 73 is provided with a seventh temperature measuring hole.
Further, the plurality of temperature measuring elements include a first temperature measuring element 81 disposed in the first temperature measuring hole, a second temperature measuring element 82 disposed in the second temperature measuring hole, a third temperature measuring element 83 disposed in the third temperature measuring hole, a fourth temperature measuring element 84 disposed in the fourth temperature measuring hole, a fifth temperature measuring element 85 disposed in the fifth temperature measuring hole, a sixth temperature measuring element 86 disposed in the sixth temperature measuring hole, and a seventh temperature measuring element 87 disposed in the seventh temperature measuring hole.
The materials of the distillation crucible 1, the distillation crucible cover 10, the distillation tube 11, the first separation crucible 51, the second separation crucible 52, the third separation crucible 53, the first separation tube 54, the second separation tube 55, the third separation tube 56, the first collection crucible 71, the second collection crucible 72, and the third collection crucible 73 are all high purity graphite, and the graphite ash content is less than 5ppm.
On the other hand, the distillation heating body 12, the distillation tube heating body 14, the first separation chamber heating body 41, the second separation chamber heating body 42, the third separation chamber heating body 43, the first collection chamber heating body 61, the second collection chamber heating body 62, the third collection chamber heating body 63, the first separation tube heating body 57, the second separation tube heating body 58 and the third separation tube heating body 59 are all composed of ceramic tubes wound with resistance wires, wherein the resistance wires comprise but are not limited to Ni-Cr alloy wires and Mo wires, and the ceramic tubes comprise but are not limited to Al 2 O 3 、ZrO 2 。
Example 2
The invention also discloses a method for preparing the high-purity magnesium ingot, which is carried out by adopting the device for preparing the high-purity magnesium ingot, and comprises the following steps:
step S1, loading raw materials to be processed into a distillation crucible;
step S2, vacuumizing the vacuum cavity, then filling inert gas into the vacuum cavity, and exhausting air of the vacuum cavity repeatedly in this way;
step S3, heating the distillation crucible, the separation chamber and the collection chamber, and heating the temperatures of the distillation unit, the separation chamber and the collection chamber to the designated temperature;
s4, collecting purified liquid metal through a collecting chamber, and sequentially entering other separating chambers to separate impurity elements;
and S5, after distillation, cooling to obtain the high-purity magnesium ingot.
Further, in the step S2, the inert gas is argon gas, and after the air in the vacuum cavity is exhausted, the vacuum cavity is evacuated until the air pressure in the vacuum cavity is 0.1pa.
One embodiment of the present invention is as follows:
industrial pure magnesium (purity 99.95%) is used as a raw material, and the device and the method are used for distillation and purification, and the steps are as follows:
step one: the bulk industrial pure magnesium was charged into a distillation crucible.
Step two: vacuum pumping the vacuum cavity to 1×10 -3 Pa, then filling high-purity argon into the vacuum cavity to 1 atmosphere pressure through an air inlet pipe, circulating for 3-5 times, exhausting air in the distillation crucible, and finally vacuumizing to 0.1Pa.
Step three: and starting a temperature controller, and heating the distillation crucible, the distillation tube, the first separation crucible, the second separation crucible, the third separation crucible, the first separation tube, the second separation tube, the third separation tube, the first collection crucible, the second collection crucible and the third collection crucible to a required temperature.
The distillation crucible temperature was set at 700 c, the distillation tube temperature was 700 c, the first separation crucible 51 temperature was 620 c, the first collection crucible 71 temperature was 620 c, and the first separation tube 54 temperature was 620 c. The temperature of the second separating crucible 52 was 500 ℃, the temperature of the second collecting crucible 72 was 500 ℃, and the temperature of the second separating tube 55 was 500 ℃. The temperature of the third separation crucible 53 is 350 ℃, the temperature of the third collection crucible 73 is 350 ℃, and the temperature of the third separation tube 56 is 350 ℃.
The magnesium vapor condenses into liquid metal in the first separating crucible 51, the liquid metal flows into the first collecting crucible 71 through the first separating tube 54, part of the magnesium vapor and impurity metal elements having higher saturated vapor pressures enter the second separating crucible 52, the second collecting crucible 72, the third separating crucible 53, and the third collecting crucible 73.
Step four: after the distillation, the mixture is cooled to room temperature, and the high purity magnesium ingot in the first collection crucible 71 is taken out.
And testing the metal impurity content of the high-purity magnesium ingot, and evaluating the distillation purification effect. FIG. 2 provides GDMS test results (in ppt wt) of a high purity magnesium ingot in the first collection crucible 71, with the metal impurity element content removed and the purity of magnesium 99.9991%.
In summary, the device and the method for preparing the high-purity magnesium ingot to be protected in the invention are characterized in that the distillation unit, the separation unit, the collection unit and the heating unit are arranged, raw materials to be processed are distilled in the distillation crucible of the distillation unit, magnesium vapor generated by distillation volatilizes from the distillation unit and enters the separation chamber to be condensed into liquid, the liquid enters the collection chamber arranged below the separation chamber under the action of gravity, the collection chamber is cooled to form the high-purity magnesium ingot, metal impurity elements with higher saturated vapor pressure volatilize into other separation chambers in sequence, and impurity elements are separated.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (11)
1. The device for preparing the high-purity magnesium ingot is characterized in that: comprising the steps of (a) a step of,
a distillation unit including a distillation crucible;
a separation unit connected to the distillation unit, the separation unit including a plurality of separation chambers sequentially arranged in a gas volatilization direction;
a collection unit comprising a plurality of collection chambers, each of said separation chambers being connected to at least one collection chamber;
the heating unit comprises a distillation heating body, a plurality of separation chamber heating bodies and a plurality of collection chamber heating bodies, wherein the distillation crucible is arranged in the distillation heating body, each separation chamber is provided with at least one separation chamber heating body, and each collection chamber is provided with at least one collection chamber heating body;
the vacuum unit comprises a vacuum cavity, the vacuum cavity is provided with an air inlet pipe, and the distillation unit, the separation unit and the collection unit are all arranged in the vacuum cavity.
2. The apparatus for preparing a high purity magnesium ingot according to claim 1, wherein: the temperature control unit comprises a temperature controller and a plurality of temperature measuring elements, the temperature controller is connected with the heating unit, the plurality of temperature measuring elements are respectively connected with the distillation unit, the separation unit and the collection unit, and the temperature controller is connected with the plurality of temperature measuring elements.
3. An apparatus for preparing a high purity magnesium ingot according to claim 2, wherein: the distillation crucible is provided with a first steam outlet, the first steam outlet is provided with a distillation tube, a distillation tube heating body is arranged outside the distillation tube, and the distillation tube heating body is connected with the temperature controller.
4. A device for preparing high purity magnesium ingot according to claim 3, wherein: the separation unit comprises a first separation chamber, a second separation chamber and a third separation chamber which are sequentially arranged along the gas volatilization direction, the first separation chamber, the second separation chamber and the third separation chamber are coaxially arranged along the horizontal direction, the distillation crucible is connected with a first separation chamber air inlet through a distillation pipe, a first separation chamber air outlet is connected with a second separation chamber air inlet, a second separation chamber air outlet is connected with a third separation chamber air inlet, and the projections of the first separation chamber air inlet, the second separation chamber air inlet and the third separation chamber air inlet along the height direction are not overlapped.
5. The apparatus for preparing a high purity magnesium ingot according to claim 4, wherein: the first separation chamber comprises a first separation chamber heating body and a first separation crucible arranged in the first separation chamber heating body, the second separation chamber comprises a second separation chamber heating body and a second separation crucible arranged in the second separation chamber heating body, and the third separation chamber comprises a third separation chamber heating body and a third separation crucible arranged in the third separation chamber heating body.
6. The apparatus for preparing a high purity magnesium ingot according to claim 5, wherein: the collecting unit comprises a first collecting chamber connected with the first separating chamber, a second collecting chamber connected with the second separating chamber and a third collecting chamber connected with the third separating chamber, wherein an inlet of the first collecting chamber is positioned right below an outlet of the first separating chamber, an inlet of the second collecting chamber is positioned right below an outlet of the second separating chamber, and an inlet of the third collecting chamber is positioned right below an outlet of the third separating chamber.
7. The apparatus for preparing a high purity magnesium ingot according to claim 6, wherein: the first collecting chamber comprises a first collecting chamber heating body and a first collecting crucible arranged in the first collecting chamber heating body, the second collecting chamber comprises a second collecting chamber heating body and a second collecting crucible arranged in the second collecting chamber heating body, and the third collecting chamber comprises a third collecting chamber heating body and a third collecting crucible arranged in the third collecting chamber heating body.
8. The apparatus for preparing a high purity magnesium ingot according to claim 7, wherein: the first separating crucible is connected with the first collecting crucible through a first separating pipe, the second separating crucible is connected with the second collecting crucible through a second separating pipe, and the third separating crucible is connected with the third collecting crucible through a third separating pipe.
9. The apparatus for preparing a high purity magnesium ingot according to claim 8, wherein: the first separation tube is provided with a first separation tube heating body outside, the second separation tube is provided with a second separation tube heating body outside, the third separation tube is provided with a third separation tube heating body outside, and the first separation tube heating body, the second separation tube heating body and the third separation tube heating body are all connected with a temperature controller.
10. The apparatus for preparing a high purity magnesium ingot according to claim 1, wherein: the vacuum unit further comprises a vacuum valve, a vacuum gauge and a vacuum pump unit, wherein the vacuum valve is arranged on the air inlet pipe, the vacuum pump unit comprises a vacuum pump, a first exhaust pipe and a second exhaust pipe, the vacuum pump is connected with the vacuum cavity through the first exhaust pipe, and the vacuum pump is further connected with the second exhaust pipe.
11. A method for preparing a high purity magnesium ingot, which is characterized by comprising the following steps: preparation using the apparatus for preparing a high purity magnesium ingot according to any one of claims 1 to 10, the preparation method comprising:
step S1, loading raw materials to be processed into a distillation crucible;
step S2, vacuumizing the vacuum cavity, then filling inert gas into the vacuum cavity, and exhausting air of the vacuum cavity repeatedly in this way;
step S3, heating the distillation crucible, the separation chamber and the collection chamber, and heating the temperatures of the distillation unit, the separation chamber and the collection chamber to the designated temperature;
s4, collecting purified liquid metal through a collecting chamber, and sequentially entering other separating chambers to separate impurity elements;
and S5, after distillation, cooling to obtain the high-purity magnesium ingot.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310264343.8A CN116377250A (en) | 2023-03-19 | 2023-03-19 | Device and method for preparing high-purity magnesium ingot |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310264343.8A CN116377250A (en) | 2023-03-19 | 2023-03-19 | Device and method for preparing high-purity magnesium ingot |
Publications (1)
| Publication Number | Publication Date |
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| CN116377250A true CN116377250A (en) | 2023-07-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310264343.8A Pending CN116377250A (en) | 2023-03-19 | 2023-03-19 | Device and method for preparing high-purity magnesium ingot |
Country Status (1)
| Country | Link |
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| CN (1) | CN116377250A (en) |
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2023
- 2023-03-19 CN CN202310264343.8A patent/CN116377250A/en active Pending
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