WO2012139484A1 - 一种钽材质多级蒸馏坩埚和蒸馏工艺 - Google Patents

一种钽材质多级蒸馏坩埚和蒸馏工艺 Download PDF

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WO2012139484A1
WO2012139484A1 PCT/CN2012/073688 CN2012073688W WO2012139484A1 WO 2012139484 A1 WO2012139484 A1 WO 2012139484A1 CN 2012073688 W CN2012073688 W CN 2012073688W WO 2012139484 A1 WO2012139484 A1 WO 2012139484A1
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crucible
pot body
heat insulation
distillation
insulation board
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PCT/CN2012/073688
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English (en)
French (fr)
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袁萍
陶利民
徐秋华
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江西稀有金属钨业控股集团有限公司
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Priority to EP12770997.0A priority Critical patent/EP2698438B1/en
Priority to US14/110,958 priority patent/US9255307B2/en
Priority to AU2012242431A priority patent/AU2012242431B2/en
Priority to JP2014504149A priority patent/JP6144253B2/ja
Priority to KR1020137029261A priority patent/KR20130135388A/ko
Publication of WO2012139484A1 publication Critical patent/WO2012139484A1/zh

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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
    • C22B59/00—Obtaining rare earth metals
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/06—Crucible or pot furnaces heated electrically, e.g. induction crucible furnaces with or without any other source of heat
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details peculiar to crucible or pot furnaces
    • F27B14/10—Crucibles
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details peculiar to crucible or pot furnaces
    • F27B14/14—Arrangements of heating devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details peculiar to crucible or pot furnaces
    • F27B2014/0825—Crucible or pot support
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details peculiar to crucible or pot furnaces
    • F27B14/10—Crucibles
    • F27B2014/102—Form of the crucibles
    • 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

Definitions

  • the invention relates to a multi-stage distillation crucible of bismuth material, which is a special material distillation crucible used in vacuum distillation purification of rare earth metal.
  • multi-stage in this patent specification means that when the height of the crucible is different in the heating element, the temperature difference formed between the upper opening of the crucible and the bottom of the crucible is also different. Since different temperatures are required for the production of different metals, multi-stage distillation is carried out by forming a multi-stage temperature difference.
  • temperature gradient in this patent specification refers to the difference between the temperature of the heat insulating upper portion and the temperature at the bottom of the crucible.
  • the vacuum distillation method is based on the difference of vapor pressure and evaporation rate of rare earth metals and impurity elements at different temperatures to achieve the separation of rare earth metals and impurity elements.
  • the height of the raft buried in the heating element is fixed.
  • the temperature difference formed between the upper outlet of the crucible and the bottom of the crucible is not easily changed, so different crucibles must be used to produce different metals. Therefore, companies must prepare a series of flaws of different sizes.
  • the crucible material is a coffin, and the cost is high; and because the outlet size on the crucible is small, the bulk metal cannot be loaded into the crucible, and it must be broken to perform the distillation operation.
  • the object of the present invention is to provide a multi-stage distillation crucible of bismuth material, the height of which is buried in the heat source can be adjusted, and an appropriate temperature difference during the smelting and purifying process of various rare earth metals can be formed between the upper outlet of the crucible and the bottom of the crucible, so that One crucible can be used to distill a variety of different rare earth metals.
  • a multi-stage distillation crucible of a crucible material comprising a pot body, a heat shield plate, and a receiving cover; the heat insulating plate is sleeved on an upper end of the pot body, The receiving cover is disposed at the top of the pot body and located above the heat insulating board; the pot body is made of enamel, and has a horn-shaped truncated cone shape which is small and large; the heat insulating board is resistant to high temperature and separated
  • a refractory material having good thermal properties characterized in that the heat insulating panel comprises a plurality of heat insulating panels which can be stacked and used; and a plurality of gaskets which can be stacked on the bottom of the crucible are provided in the heating body.
  • the refractory material is a high alumina brick, corundum plate, graphite plate, or coffin.
  • the pot body has a thickness of 2 to 3 mm.
  • the pot body has an upper diameter of 100 to 250 mm, a lower diameter of 300 to 500 mm, and a height of 250 ⁇ 400mm.
  • a distillation process for a multi-stage distillation crucible of a crucible material comprising a pot body, a heat shield, and a receiving cover; the heat insulating plate is sleeved on the upper end of the pot body And a receiving cover is disposed on the top of the pot body and located above the heat insulating board; the pot body is made of enamel, and has a horn-shaped truncated cone shape which is small and large; the heat insulating board is resistant to high temperature and A refractory material having good thermal insulation properties is characterized in that the temperature difference between the heat insulating plate portion and the bottom portion of the crucible is adjusted by adjusting the number of blocks of the heat insulating plate.
  • the height of the crucible in the heating body is further adjusted by increasing or decreasing the spacer to adjust the temperature difference between the upper portion of the insulating panel and the bottom portion of the crucible.
  • the pot body has a thickness of 2 to 3 mm, and the pot body has an upper diameter of 100 to 250 mm, a lower diameter of 300 to 500 mm, and a height of 250 to 400 mm.
  • a distillation process for a multi-stage distillation crucible of a crucible material comprising a pot body, a heat shield, and a receiving cover; the heat insulating plate is sleeved on the upper end of the pot body And a receiving cover is disposed on the top of the pot body and located above the heat insulating board; the pot body is made of enamel, and has a horn-shaped truncated cone shape which is small and large; the heat insulating board is resistant to high temperature and A refractory material having good thermal insulation properties is characterized in that the height of the crucible in the heating body is adjusted by increasing or decreasing the spacer to adjust the temperature difference between the upper portion of the insulating panel and the bottom portion of the crucible.
  • the temperature difference between the heat insulating plate portion and the bottom portion of the crucible is further adjusted by adjusting the number of blocks of the heat insulating plate.
  • the pot body has a thickness of 2 to 3 mm, and the pot body has an upper diameter of 100 to 250 mm, a lower diameter of 300 to 500 mm, and a height of 250 to 400 mm.
  • the multi-stage distillation crucible of the present invention since the rare earth metal has high chemical reactivity at high temperature, it is easy to react with other substances, and the pot body is made of a rare metal crucible having strong chemical stability and corrosion resistance, which can prevent the process of distillation purification. ⁇ Impurities may cause re-contamination of the product.
  • the upper and lower inclined cone structure can block different radiant heat, so that the receiving cover of the top of the crucible and the pot body of the lower part of the heat insulation board form different temperature differences, different distillation metals.
  • the melting point is different, and the receiving temperature requirements in the receiving hood (condensing zone) are also different.
  • the main body is buried in the heating element, and the upper part of the crucible is separated by the refractory material (insulation board) to block the radiation and the conduction heat, so that the condensation zone is formed in the top receiving cover, and the distilled metal is Received in the receiving hood of the top condensing zone.
  • the crucible material multi-stage distillation crucible according to the present invention adjusts the height of the crucible in the heating body by increasing or decreasing the gasket, and/or adjusting the temperature of the condensation receiving zone by adjusting the number of blocks of the heat insulation panel, thereby different melting points Distillation and purification with metals of different vapor pressures.
  • the rare earth metal to be distilled and purified is placed at the bottom of the crucible, and is heated in a heating body, and the rare earth metal having a low melting point and a high vapor pressure is received in the condensation zone.
  • the impurity metal with high melting point and low vapor pressure remains in the crucible.
  • FIG. 1 is a schematic view showing the structure of a multi-stage distillation crucible of cerium according to the present invention.
  • the pot body 1 has a pagoda shape, that is, a horn type truncated cone body that is large and small, and one or more layers of the heat insulation panel 2 are disposed on the upper portion thereof, and the top of the heat insulation panel 2 is provided with a receiving cover 3.
  • the pot body 1 made of coffin, thickness is 2 ⁇ 3mm, the upper diameter is 100 ⁇ 250mm, the lower diameter is 300 ⁇ 500mm, and the height is 250 ⁇ 400mm.
  • the upper and lower slope structure also helps to block different radiant heat, thus forming different temperature gradients. .
  • Distillation crucible is welded to the coffin, and the thickness of the crotch is usually 2 to 3 mm.
  • the crucible body is buried in the heating zone 6, and the upper part of the crucible is isolated by the refractory material to block the radiation and the conduction heat, so that the upper part forms a condensation zone, and the distilled metal is received in the receiving cover of the upper condensation zone.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Crucibles And Fluidized-Bed Furnaces (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Description

一种钽材质多级蒸馏坩埚和蒸馏工艺 技术领域
本发明涉及一种钽材质多级蒸馏坩埚，是稀土金属真空蒸馏提纯时使用的特种材质蒸馏坩埚。
本专利说明书中的术语“多级”是指，当坩埚埋于发热体中的高度不一样时，在坩埚上出口与坩埚底部之间形成的温差也不一样。由于生产不同的金属需采用不同的温差，故通过形成多级温差来进行多级蒸馏。
本专利说明书中的术语“温度梯度”是指，隔热板上部温度与坩埚底部温度之差。
 背景技术
真空蒸馏法是依据稀土金属和杂质元素在不同温度下的蒸汽压及蒸发速度的不同，达到稀土金属与杂质元素分离的目的。
在现有技术中，坩埚埋于发热体中的高度是固定的, 在坩埚上出口与坩埚底部之间形成的温差不容易改变，因此，生产不同的金属就必须采用不同的坩埚。因此，企业必须准备一系列的不同尺寸的坩埚。然而，坩埚材质为钽材，成本较高；而且由于坩埚上的出口尺寸较小，大块状金属无法装入坩埚，必须破碎才能进行蒸馏作业。
 发明内容
本发明的目的是提供一种钽材质多级蒸馏坩埚，其埋于热源的高度可被调节，坩埚的上出口与坩埚的底部之间可形成各种稀土金属熔炼提纯过程中的适当温差，使得一个坩埚可用于蒸馏各种不同的稀土金属。
为此，根据本发明的一个方面，提供了一种钽材质多级蒸馏坩埚，所述蒸馏坩埚包括锅体、隔热板、以及接收罩；所述隔热板套设在锅体的上端，而接收罩设置在所述锅体的顶部，位于隔热板的上方；所述锅体由钽制成，呈上小下大的喇叭型圆台体状；所述隔热板由耐高温且隔热性能好的耐火材料制成，其特征在于，所述隔热板包括可叠置使用的多块隔热板；在发热体内设有多片可在坩埚的底部叠置使用的垫片。
优选地，所述耐火材料为高铝砖、刚玉板、石墨板、或钽材。
优选地，所述锅体的厚度为2～3mm。
优选地，所述锅体的上口径为 100～250mm、下口径为 300～500mm、高为 250～400mm。
根据本发明的另外一个方面，提供了一种钽材质多级蒸馏坩埚的蒸馏工艺，所述蒸馏坩埚包括锅体、隔热板、以及接收罩；所述隔热板套设在锅体的上端，而接收罩设置在所述锅体的顶部，位于隔热板的上方；所述锅体由钽制成，呈上小下大的喇叭型圆台体状；所述隔热板由耐高温且隔热性能好的耐火材料制成，其特征在于，通过调整隔热板的块数来调整隔热板上部与坩埚底部之间的温差。
优选地，进一步通过增加或减少垫片来调节坩埚在发热体内的高度，以调整隔热板上部与坩埚底部之间的温差。
优选地，所述锅体的厚度为2～3mm，所述锅体的上口径为100～250mm、下口径为300～500mm、高为250～400mm。
根据本发明的另外一个方面，提供了一种钽材质多级蒸馏坩埚的蒸馏工艺，所述蒸馏坩埚包括锅体、隔热板、以及接收罩；所述隔热板套设在锅体的上端，而接收罩设置在所述锅体的顶部，位于隔热板的上方；所述锅体由钽制成，呈上小下大的喇叭型圆台体状；所述隔热板由耐高温且隔热性能好的耐火材料制成，其特征在于，通过增加或减少垫片来调节坩埚在发热体内的高度，以调整隔热板上部与坩埚底部之间的温差。
优选地，进一步通过调整隔热板的块数来调整隔热板上部与坩埚底部之间的温差。
优选地，所述锅体的厚度为2～3mm，所述锅体的上口径为100～250mm、下口径为300～500mm、高为250～400mm。
根据本发明的多级蒸馏坩埚，由于稀土金属高温化学活性强，极易与其它物质发生反应，锅体选用化学稳定性强、耐腐蚀的稀有金属钽材制成，能防止在蒸馏提纯过程中坩埚杂质对产品可能造成的再次污染。
根据本发明的多级蒸馏坩埚，其上小下大的斜锥面结构可挡住不同的辐射热量，从而使坩埚顶部的接收罩和隔热板下部的锅体形成不同的温差，不同的蒸馏金属熔点不同，对接收罩（冷凝区）内的接收温度要求也不同。
根据本发明的钽材质多级蒸馏坩埚，主体埋于发热体中，坩埚上部通过耐火材料（隔热板）隔离，挡住辐射和传导热，从而顶部接收罩内形成冷凝区，蒸馏出来的金属在顶部冷凝区的接收罩内接收。
根据本发明的钽材质多级蒸馏坩埚，通过增加或减少垫片来调节坩埚在发热体内的高度，和/或通过调整隔热板的块数来调整冷凝接收区的温度，从而可对不同熔点和不同蒸汽压的金属进行蒸馏提纯。
在根据本发明的钽材质多级蒸馏坩埚，在使用过程中，将欲蒸馏提纯的稀土金属置于坩埚底部，放进发热体内加热，低熔点、高蒸汽压的稀土金属在冷凝区内接收，而高熔点、低蒸汽压的杂质金属则残留在坩埚中。
 附图说明
图1为根据本发明的钽材质多级蒸馏坩埚的结构示意图。
具体实施方式
如图1所示，根据本发明的钽材质多级蒸馏坩埚，包括锅体1、若干层隔热板2、接收罩3。隔热板2设置在锅体1的上端，而接收罩3设置在隔热板2的上方。
该锅体1为宝塔式形状，即呈上小下大的喇叭型圆台体，其上部设置有一层或多层隔热板2，隔热板2的顶部设置有接收罩3。所述锅体 1由钽材制成，厚度为 2～3mm，上口径为100～250mm，下口径为300～500mm，高为250～400mm的圆台体，其上小下大的斜面结构也有助于挡住不同的辐射热量，从而形成不同的温度梯度。
根据本发明的多级蒸馏坩埚，在使用过程中，通过增加或减少垫片5来调节坩埚在发热体6内的高度，可对不同熔点和不同蒸汽压的金属进行不同的蒸馏提纯，通过调整隔热板2的块数来调整冷凝接收区的温度；将蒸馏提纯的稀土金属4置于坩埚底部，放进发热体6中加热，通过本装置后，低熔点、高蒸汽压的稀土金属可通过温度梯度在不同的冷凝区（接收罩3）内接收，而高熔点、低蒸汽压的杂质金属则残留在坩埚中。
本发明通过三种方式使锅体1和冷凝区（接收罩3）之间产生温差：通过坩埚上下之间喇叭型的斜面挡住辐射热量；通过隔热板挡住辐射热量；以及采用耐高温且不易传导热量的耐火材料作为隔热板挡住锅体的辐射热量，使锅体内和接收罩内温度不同。
蒸馏坩埚为钽材焊接而成，钽片厚度通常为2～3mm。坩埚主体埋于加热区6中，坩埚上部通过耐火材料隔离，挡住辐射和传导热，从而使上部形成冷凝区，蒸馏出来的金属在上部冷凝区的接收罩内接收。
坩埚蒸馏不同的熔点和不同蒸汽压的金属时，多级温差调节方法：
A）通过增加或减少垫片，来调节坩埚在发热体内的高度；
B）通过调整隔热板块数来调整冷凝接收区温度。

Claims (10)

  1. 一种钽材质多级蒸馏坩埚，所述蒸馏坩埚包括锅体、隔热板、以及接收罩；所述隔热板套设在锅体的上端，而接收罩设置在所述锅体的顶部，位于隔热板的上方；所述锅体由钽制成，呈上小下大的喇叭型圆台体状；所述隔热板由耐高温且隔热性能好的耐火材料制成，其特征在于，
    所述隔热板包括可叠置使用的多块隔热板；
    在发热体内设有多片可在坩埚的底部叠置使用的垫片。
  2. 如权利要求1所述的钽材质多级蒸馏坩埚，其特征在于，所述耐火材料为高铝砖、刚玉板、石墨板、或钽材。
  3. 如权利要求1所述的钽材质多级蒸馏坩埚，其特征在于，所述锅体的厚度为2～3mm。
  4. 如权利要求1所述的钽材质多级蒸馏坩埚，其特征在于，所述锅体的上口径为100～250mm、下口径为300～500mm、高为250～400mm。
  5. 一种钽材质多级蒸馏坩埚的蒸馏工艺，所述蒸馏坩埚包括锅体、隔热板、以及接收罩；所述隔热板套设在锅体的上端，而接收罩设置在所述锅体的顶部，位于隔热板的上方；所述锅体由钽制成，呈上小下大的喇叭型圆台体状；所述隔热板由耐高温且隔热性能好的耐火材料制成，其特征在于，通过调整隔热板的块数来调整隔热板上部与坩埚底部之间的温差。
  6. 如权利要求5所述的钽材质多级蒸馏坩埚的蒸馏工艺，其特征在于，进一步通过增加或减少垫片来调节坩埚在发热体内的高度，以调整隔热板上部与坩埚底部之间的温差。
  7. 如权利要求5所述的钽材质多级蒸馏坩埚的蒸馏工艺，其特征在于，所述锅体的厚度为2～3mm，所述锅体的上口径为100～250mm、下口径为300～500mm、高为250～400mm。
  8. 一种钽材质多级蒸馏坩埚的蒸馏工艺，所述蒸馏坩埚包括锅体、隔热板、以及接收罩；所述隔热板套设在锅体的上端，而接收罩设置在所述锅体的顶部，位于隔热板的上方；所述锅体由钽制成，呈上小下大的喇叭型圆台体状；所述隔热板由耐高温且隔热性能好的耐火材料制成，其特征在于，通过增加或减少垫片来调节坩埚在发热体内的高度，以调整隔热板上部与坩埚底部之间的温差。
  9. 如权利要求8所述的钽材质多级蒸馏坩埚的蒸馏工艺，其特征在于，进一步通过调整隔热板的块数来调整隔热板上部与坩埚底部之间的温差。
  10. 如权利要求8所述的钽材质多级蒸馏坩埚的蒸馏工艺，其特征在于，所述锅体的厚度为2～3mm，所述锅体的上口径为100～250mm、下口径为300～500mm、高为250～400mm。
PCT/CN2012/073688 2011-04-11 2012-04-10 一种钽材质多级蒸馏坩埚和蒸馏工艺 WO2012139484A1 (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114318012A (zh) * 2022-01-17 2022-04-12 遵义钛业股份有限公司 一种用于生产海绵钛的蒸馏加热炉的炉底

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102181655B (zh) * 2011-04-11 2012-11-07 江西稀有金属钨业控股集团有限公司 一种钽材质多级蒸馏坩埚和蒸馏工艺
CN107916336A (zh) * 2017-12-14 2018-04-17 宁夏太阳镁业有限公司 一种镁合金精炼坩埚
CN110538478A (zh) * 2018-10-29 2019-12-06 天津包钢稀土研究院有限责任公司 一种高品质无水稀土卤化物提纯装置
CN112176206B (zh) * 2020-09-21 2022-08-09 广东先导稀材股份有限公司 精馏提纯装置及利用其通过氟化铍制备铍的方法

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2310302Y (zh) * 1997-07-11 1999-03-10 苏君道 一种陶瓷坩埚
CN2627439Y (zh) * 2003-05-28 2004-07-21 江西南方稀土高技术股份有限公司 高纯金属蒸馏及收集装置
CN1554808A (zh) * 2003-12-24 2004-12-15 山东大学 一种生长具有半导体特性的大直径6H-SiC单晶的装置和方法
CN101027433A (zh) * 2004-08-10 2007-08-29 克里公司 用于大碳化硅单晶的高品质生长的籽晶和籽晶夹持器组合
CA2743543A1 (fr) * 2008-12-19 2010-06-24 Commissariat A L'energie Atomique Et Aux Energies Alternatives Melting-solidification furnace with variable heat exchange via the side walls
CN201538827U (zh) * 2009-09-27 2010-08-04 上海元亮光电科技有限公司 可以调节固液界面温度梯度的坩埚盖板
CN102181655A (zh) * 2011-04-11 2011-09-14 江西稀有金属钨业控股集团有限公司 一种钽材质多级蒸馏坩埚和蒸馏工艺
CN201992981U (zh) * 2011-04-11 2011-09-28 江西稀有金属钨业控股集团有限公司 一种钽材质多级蒸馏坩埚

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB466763A (en) * 1935-09-04 1937-06-04 Harold Alexandre Blackwell An improved process and apparatus for separating magnesium, beryllium, and like metals which sublime from their ores and compounds
JPS60255102A (ja) * 1984-06-01 1985-12-16 Toyota Motor Corp 重合性有機物を含む有機溶剤の回収方法
JPH0436427A (ja) * 1990-06-01 1992-02-06 Nikko Kyodo Co Ltd 希土類金属の製造装置
JPH0885833A (ja) * 1994-09-16 1996-04-02 Shin Etsu Chem Co Ltd 希土類金属の精製方法
JP2001303149A (ja) * 2000-04-24 2001-10-31 Tetsuya Uda 希土類元素の分離方法及び希土類元素分離用組成物
DE10134286C1 (de) * 2001-08-03 2002-12-12 Ald Vacuum Techn Ag Vorrichtung zum Destillieren von Metallschmelzen
JP2003073754A (ja) * 2001-08-30 2003-03-12 Tetsuya Uda 希土類元素の回収方法
US7056383B2 (en) * 2004-02-13 2006-06-06 The Fox Group, Inc. Tantalum based crucible
CN100523315C (zh) * 2007-09-28 2009-08-05 中国科学院物理研究所 分体式钽坩埚及其制造方法
CN102046820B (zh) * 2008-03-26 2013-07-10 财团法人生产技术研究奖励会 稀土元素的回收方法及回收装置

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2310302Y (zh) * 1997-07-11 1999-03-10 苏君道 一种陶瓷坩埚
CN2627439Y (zh) * 2003-05-28 2004-07-21 江西南方稀土高技术股份有限公司 高纯金属蒸馏及收集装置
CN1554808A (zh) * 2003-12-24 2004-12-15 山东大学 一种生长具有半导体特性的大直径6H-SiC单晶的装置和方法
CN101027433A (zh) * 2004-08-10 2007-08-29 克里公司 用于大碳化硅单晶的高品质生长的籽晶和籽晶夹持器组合
CA2743543A1 (fr) * 2008-12-19 2010-06-24 Commissariat A L'energie Atomique Et Aux Energies Alternatives Melting-solidification furnace with variable heat exchange via the side walls
CN201538827U (zh) * 2009-09-27 2010-08-04 上海元亮光电科技有限公司 可以调节固液界面温度梯度的坩埚盖板
CN102181655A (zh) * 2011-04-11 2011-09-14 江西稀有金属钨业控股集团有限公司 一种钽材质多级蒸馏坩埚和蒸馏工艺
CN201992981U (zh) * 2011-04-11 2011-09-28 江西稀有金属钨业控股集团有限公司 一种钽材质多级蒸馏坩埚

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114318012A (zh) * 2022-01-17 2022-04-12 遵义钛业股份有限公司 一种用于生产海绵钛的蒸馏加热炉的炉底

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