WO2015019434A1 - Appareil de séparation et de récupération de terres rares - Google Patents

Appareil de séparation et de récupération de terres rares Download PDF

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Publication number
WO2015019434A1
WO2015019434A1 PCT/JP2013/071312 JP2013071312W WO2015019434A1 WO 2015019434 A1 WO2015019434 A1 WO 2015019434A1 JP 2013071312 W JP2013071312 W JP 2013071312W WO 2015019434 A1 WO2015019434 A1 WO 2015019434A1
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WO
WIPO (PCT)
Prior art keywords
rare earth
heating furnace
ammonium chloride
recovery
buffer
Prior art date
Application number
PCT/JP2013/071312
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English (en)
Japanese (ja)
Inventor
宮田　素之
山本　浩貴
元 村上
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株式会社日立製作所
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Priority to JP2015530599A priority Critical patent/JPWO2015019434A1/ja
Priority to PCT/JP2013/071312 priority patent/WO2015019434A1/fr
Publication of WO2015019434A1 publication Critical patent/WO2015019434A1/fr

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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
    • C22B59/00—Obtaining rare earth metals
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • 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 present invention relates to an apparatus for separating and collecting a rare earth composition.
  • Rare earth elements are used in motors for hybrid automobiles and magnetic disk devices (so-called rare earth magnets), phosphors used in displays and lighting equipment, abrasives used for polishing glass, and amplifiers in optical communication equipment. The demand is expected to increase further in the future. On the other hand, in recent years, the price of rare earth materials has risen due to the uneven distribution of rare earth resources, and as a resource risk hedge, the use of rare earths, development of alternative materials, and separation and recovery of rare earth elements from products The method to do is examined.
  • Patent Document 1 describes separation using the solubility difference of Re sulfate.
  • Patent Document 1 uses a very high concentration of strong acid or highly volatile solvent, and thus has a problem of having a significant impact on the environment.
  • the present invention is an object to reduce the influence on the environment when the rare earth component is separated and recovered.
  • the present invention provides an apparatus for separating and recovering a plurality of types of rare earth elements, a first heating furnace for chlorinating a rare earth material containing a plurality of types of rare earth elements, and the chlorinated rare earth material.
  • a second heating furnace that heats in an oxygen atmosphere; and a solid-liquid separation unit that mixes the rare earth material heated in an oxygen atmosphere with a solvent to separate the plurality of rare earth elements from each other in a solid-liquid manner.
  • the heating furnace and the second heating furnace include a device for switching an atmosphere between an inlet and an outlet of the rare earth material.
  • the influence on the environment can be reduced during the separation and recovery of rare earth components.
  • Fig. 1 shows the block diagram of the separation device.
  • the present embodiment is an apparatus for separating and recovering rare earth elements from a raw material containing a plurality of types of rare earth elements, and includes an apparatus for performing at least three steps of a raw material adjustment step 10, a heat treatment step 20, and a separation step 30. .
  • the raw material adjustment step 10 includes devices such as a rare earth raw material supply unit 110, an ammonium chloride supply unit 120, a solvent supply unit 130, a mixing and grinding unit 140, a drying unit 150, and a molding unit 160.
  • the heat treatment step 20 includes devices such as a gas supply unit 210, a heat treatment unit 220, an ammonium chloride recovery unit 230, a gas abatement unit 240, an ammonium chloride measurement unit 250, and an ammonium chloride recovery pipe 260.
  • the separation step 30 includes devices such as a solvent supply unit 310, a solid-liquid separation unit 320, and a solid recovery unit 330.
  • each rare earth element When a powder containing a mixture of a raw material containing multiple types of rare earth elements and ammonium chloride is heated, each rare earth element generates a chloride. Thereafter, when the chloride is oxidized, an acid chloride is generated depending on the type of rare earth chloride.
  • a solvent such as water
  • it is divided into rare earth chloride that is easily soluble in the solvent and rare earth acid chloride that is hardly soluble in the solvent and easily precipitates. Separate and recover seed rare earth elements.
  • the raw material and ammonium chloride are mixed in the raw material adjustment step 10, the mixed powder is heated in the heat treatment step 20, and the rare earth chloride mixture is solid-liquid separated using a solvent in the separation step 30. According to this, rare earth elements can be separated and recovered without using a solvent with a large environmental load.
  • FIG. 2 shows a schematic diagram of an apparatus of the heat treatment unit 220.
  • 210 is a gas supply unit
  • 221 is a buffer
  • 222 is a shutter
  • 223 is an evacuation device
  • 224 is a heating furnace
  • 225 is a transfer machine
  • 226 is a furnace body
  • 227 is a heating furnace
  • 228 is a heating furnace
  • 230 is an ammonium chloride recovery section
  • 231 is a solvent supply section
  • 240 is a gas abatement section
  • 260 is an ammonium chloride recovery pipe.
  • the sample (mixed powder) supplied from the raw material adjustment step 10 is conveyed to the heating furnace 224 through the buffer 221.
  • chlorination with ammonium chloride which is the first step of heat treatment
  • the sample after the chlorination treatment is transported to the heating furnace 227 via the buffer 221 installed between the heating furnace 224 and the heating furnace 227.
  • ammonium chloride removal which is the second step of heat treatment
  • the sample after the ammonium dechlorination treatment is transported to the heating furnace 228 via a buffer 221 installed between the heating furnace 227 and the heating furnace 228.
  • oxidation (acidification) treatment which is a third step of heat treatment, is performed.
  • the sample after the oxidation treatment is supplied to the separation step 30 via the buffer 221.
  • the buffer 221 is provided with shutters 222 at both ends (inlet side and outlet side). Further, the vacuum exhaust device 223 and the gas supply unit 210 are connected. Although it is necessary to change the atmosphere in the raw material adjustment process 10 and the heat treatment process 20, the atmosphere in the buffer can be controlled by the vacuum exhaust device 223, the gas supply unit 210, and the shutter 222. Further, by installing a heater in the buffer, the temperature in the buffer can be controlled together with the atmosphere. Furthermore, the moisture content in the atmosphere can be controlled by installing a dew point control device.
  • Examples of the structure of the heating furnace include a batch furnace method in which the sample is allowed to stand, a rotary kiln furnace method in which the sample is flowed and stirred, a fluidized bed furnace method, a tunnel furnace method having a mechanism for transporting the stationary sample, and the like. It can be appropriately selected according to the shape of the sample, the amount of sample treatment, the heat treatment conditions, the size, shape, mechanism, etc. of the heating furnace. The arrangement of the heating furnaces may not be alternately up and down.
  • a batch furnace method or a method of standing a sample such as a tunnel furnace method is preferable.
  • the reaction is accelerated if the solid is agitated to increase the chance of contact with the gas.
  • a method of flowing and stirring a sample such as a rotary kiln furnace method or a fluidized bed furnace method. preferable.
  • a transporter 225 for transporting the sample is installed in the heating furnace.
  • the heating source of the heating furnace includes electricity, LP gas, heavy oil, etc., which can be appropriately selected according to the sample processing amount, processing cost, environmental conditions (such as legal regulations) where the equipment is installed, etc. it can.
  • the heating method includes heat transfer heating with a heater, high frequency induction heating, far-infrared heating, microwave heating, etc., and should be appropriately selected according to the heat treatment conditions, the size, shape, mechanism, etc. of the heating furnace. Can do.
  • the furnace body 226 of the heating furnace includes metal materials excellent in oxidation resistance at high temperatures, such as SUS material, inconel material, Fe—Co alloy, Ni-base alloy, alumina, zirconia, silicon nitride, silicon carbide. Ceramic materials typified by quartz and the like are preferable, and can be appropriately selected according to the heat treatment conditions, the size, shape, mechanism, etc. of the heating furnace.
  • the gas generated in the heat treatment process is rendered harmless and discharged out of the system.
  • the abatement apparatus in the gas abatement section include a dry apparatus that uses an abatement cylinder, a combustion apparatus that burns gas, and a wet apparatus that uses treatment chemicals.
  • an optimal apparatus can be appropriately selected according to the amount of gas generated, processing cost, and the installation environment (legal regulations, etc.) of the apparatus.
  • an optimum gas is appropriately supplied according to the atmosphere of the buffer and the heat treatment conditions of the heating furnace.
  • the shutter 222 on the inlet side of the buffer 221 is opened, the shutter 222 on the outlet side is closed, and the sample is conveyed into the buffer 221.
  • the inside of the buffer is evacuated by the evacuation device 223.
  • the same atmospheric gas as that of the heating furnace 224 is supplied from the gas supply unit 210 into the buffer.
  • the buffer is filled with a gas having a predetermined atmosphere and pressure, only the shutter 222 on the outlet side is opened, and the sample is conveyed to the heating furnace 224.
  • the shutter 222 on the exit side is closed. In the following buffers, samples are taken in and out through the same procedure.
  • an inert gas such as argon gas or nitrogen is preferably supplied from the gas supply unit 210 in order to perform chlorination using ammonium chloride, which is the first step of the heat treatment. Further, at this time, it is preferable to use a so-called dry gas having a low water content with a gas dew point temperature of ⁇ 60 ° C. or less. This is because when the water content is low, the desired chloride is easily generated.
  • the gas generated by the heat treatment in the heating furnace 224 is discharged out of the system through the gas abatement part 240.
  • the sample heat-treated in the heating furnace 224 is transported to the heating furnace 227 via the buffer 221 installed between the heating furnace 224 and the heating furnace 227.
  • the heating furnace 227 in order to perform the deammonium treatment, which is the second step of the heat treatment, it is preferable to carry out the treatment in a reduced pressure exhaust atmosphere.
  • An inert gas such as argon gas or nitrogen can be supplied from the supply unit. In this case as well, it is preferable to use a gas having a low dew point as described above.
  • the heat-treated sample is transported to a buffer 221 installed between the heating furnace 227 and the heating furnace 228.
  • ammonium chloride is generated with the dechlorination ammonium treatment.
  • the generated ammonium chloride is recovered by the ammonium chloride recovery unit 230.
  • the ammonium chloride recovery unit maintains the temperature, atmosphere, and pressure at which ammonium chloride generated as a gas in the heating furnace 227 is solidified, and recovers ammonium chloride in a solid powder state.
  • the recovered ammonium chloride is transported to the raw material adjustment step 10 through the ammonium chloride recovery pipe 260 and reused as the raw material.
  • an ammonium chloride measuring unit 250 is provided during this period to determine the amount and purity of the recovered ammonium chloride. It is preferable to measure.
  • the ammonium chloride recovery pipe 260 is connected to the ammonium chloride supply unit 120, but may be connected to a pipe on the way to the mixing and grinding unit 140.
  • fluorescent X-ray analysis energy dispersive X-ray spectroscopy, inductively coupled plasma spectroscopy, atomic absorption spectroscopy, X-ray diffraction, etc. can be used. It is not limited to.
  • the second heat treatment step is performed in the same atmosphere as the first step, it is possible to use the same heating furnace for the first step and the second step. In this case, use the heating furnace 224.
  • the raw material supplied from the raw material adjustment step 10 can be supplied to the heating furnace 227 via a buffer, and the first step and the second step can be performed continuously in the heating furnace 227.
  • the sample processed in the heating furnace 227 is transported to the heating furnace 228 via the buffer 221 installed between the heating furnace 227 and the heating furnace 228.
  • oxygen-containing gas is supplied in order to perform chloride acidification, which is the third step of heat treatment.
  • the ratio of oxygen contained in the gas and the amount of moisture (dew point) contained in the gas can be appropriately selected as appropriate in accordance with the target rare earth component and the amount of heat treatment.
  • the gas generated by the heat treatment in the heating furnace 228 is discharged out of the system through the gas abatement part 240 as described above.
  • Neodymium oxide (Nd 2 O 3 ) and dysprosium oxide (Dy 2 O 3 ) were used as rare earth materials.
  • Ammonium chloride was mixed so that the amount of ammonium chloride was 15 mol with respect to 1 mol of the mixed powder mixed so that Dy / Nd was 1/7 by weight.
  • This mixed powder was supplied to the buffer 1 installed in the front stage of the heating furnace in the first step.
  • the vacuum pump is evacuated to about 20 Pa with a rotary pump, and after the vacuum evacuation-gas introduction operation for introducing argon gas with a dew point of ⁇ 70 ° C. is repeated five times, the mixed powder is supplied from buffer 1 to the heating furnace in the first step. did.
  • the first step heat treatment is performed at 300 ° C. for 5 hours while flowing the argon gas at a flow rate of 500 mL / min using a rotary kiln furnace in which the argon gas atmosphere is made of Inconel. A mixture of chloride and Dy chloride was formed. This mixture was conveyed to the buffer 2 installed between the heating furnace of the first step and the heating furnace of the second step.
  • the same vacuum exhaust-gas introduction operation as described above was performed once. Then, the mixture was supplied to the heating furnace of the second step.
  • the ammonium chloride treatment was performed under the conditions of 400 ° C. and 4 hours while evacuating with a rotary pump using a rotary kiln furnace made of Inconel as the furnace body.
  • the mixture after ammonium dechlorination treatment was conveyed to the buffer 3 installed between the heating furnace in the second step and the heating furnace in the third step.
  • the recovered ammonium chloride was dissolved in water in the ammonium chloride recovery section, supplied to the raw material adjustment step in a solution state, and reused.
  • the same vacuum exhaust-gas introduction operation as described above was performed 5 times using dry air having a dew point of ⁇ 60 ° C. Then, the mixture was supplied to the heating furnace in the third step.
  • the third step was a dry air atmosphere. Using a rotary kiln furnace having a furnace body made of Inconel, heat treatment was performed at 350 ° C. for 5 hours while flowing dry air at a flow rate of 500 mL / min to produce a mixture of Dy acid chloride and Nd chloride. The mixture after the oxidation treatment was recovered and then supplied to the separation step.
  • the separation process was performed using pure water in the separation step. Since Nd chloride is easily dissolved and Dy acid chloride is easily precipitated, the Dy separation rate is 90% and the recovery rate is 90%, and a sufficient separation rate and recovery rate are obtained even in one step.
  • Cerium oxide (Ce 2 O 3 ) and lanthanum oxide (La 2 O 3 ) were used as rare earth materials.
  • Ammonium chloride was mixed so that the amount of ammonium chloride was 12 mol with respect to 1 mol of the mixed powder mixed so that Ce / La was 1/1 by weight ratio.
  • This mixed powder was supplied to the buffer 1 installed in the front stage of the heating furnace in the first step.
  • buffer 1 After evacuating to about 20 Pa with a rotary pump, the evacuation-gas introduction operation of introducing dry nitrogen gas having a dew point of ⁇ 60 ° C. was repeated five times, and then the mixed powder was transferred from buffer 1 to the heating furnace in the first step. Supplied.
  • the first step using a batch furnace using an alumina-based heat insulating material as the furnace body in the nitrogen gas atmosphere, while flowing the nitrogen gas at a flow rate of 1000 mL / min, conditions of 350 ° C. and 3 hours And a mixture of Ce chloride and La chloride was formed. This mixture was conveyed to the buffer 2 installed between the heating furnace of the first step and the heating furnace of the second step.
  • the same vacuum exhaust-gas introduction operation as described above was performed once. Then, the mixture was supplied to the heating furnace of the second step.
  • an ammonium chloride treatment was performed at 450 ° C. for 2 hours using a rotary kiln furnace having an inconel as the furnace body while evacuating with a rotary pump.
  • the mixture after ammonium dechlorination treatment was conveyed to the buffer 3 installed between the heating furnace in the second step and the heating furnace in the third step.
  • the recovered ammonium chloride was recovered in a powder state in the ammonium chloride recovery section, and then supplied to the raw material adjustment step for reuse.
  • the same vacuum exhaust-gas introduction operation as described above was performed 5 times using dry air having a dew point of ⁇ 60 ° C. Thereafter, the sample was supplied to the heating furnace in the third step.
  • the third step was a dry air atmosphere. Using a rotary kiln furnace made of quartz as the furnace body, heat treatment was carried out at 250 ° C. for 5 hours while flowing dry air at a flow rate of 500 mL / min to produce a mixture of Ce acid chloride and La chloride. The mixture after the oxidation treatment was recovered and then supplied to the separation step.
  • Neodymium oxide (Nd 2 O 3 ) and dysprosium oxide (Dy 2 O 3 ) were used as rare earth materials.
  • Ammonium chloride was mixed so that the amount of ammonium chloride was 18 mol with respect to 1 mol of the mixed powder mixed so that Dy / Nd was 1/1 by weight ratio.
  • This mixed powder was supplied to the buffer 2 installed in the front stage of the heating furnace in the second step.
  • buffer 2 After evacuating to about 20 Pa with a rotary pump, the evacuation-gas introduction operation for introducing dry nitrogen gas having a dew point of ⁇ 60 ° C. was repeated five times, and the mixed powder was transferred from buffer 2 to the heating furnace in the second step. Supplied.
  • heat treatment is performed at 300 ° C. for 5 hours while flowing the nitrogen gas at a flow rate of 500 mL / min using a rotary kiln furnace in which the furnace body is made of SUS material.
  • a mixture of Nd chloride and Dy chloride was formed.
  • the dechlorination treatment in the second step was performed at 400 ° C. for 6 hours while flowing the nitrogen gas at a flow rate of 500 mL / min.
  • the mixture after the dechlorination ammonium treatment was transported to the buffer 3 installed between the heating furnace in the second step and the heating furnace in the third step.
  • the recovered ammonium chloride was dissolved in water in the ammonium chloride recovery section, supplied to the raw material adjustment step in a solution state, and reused.
  • the third step was a dry air atmosphere. Using a rotary kiln furnace whose furnace body is made of SUS material, heat treatment was performed at 300 ° C. for 3 hours while flowing dry air at a flow rate of 500 mL / min, and a mixture of Dy acid chloride and Nd chloride was generated. .

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Abstract

La présente invention concerne un appareil destiné à séparer et à récupérer plusieurs types d'éléments de terres rares, l'appareil étant équipé : d'un premier four de réchauffage destiné à chlorer une matière première de terres rares contenant plusieurs types d'éléments de terres rares ; d'un second four de réchauffage destiné à réchauffer la matière première de terres rares chlorée sous atmosphère enrichie en oxygène ; et d'une unité de séparation solide-liquide destinée à mélanger la matière première de terres rares, qui a été réchauffée sous atmosphère enrichie en oxygène, avec un solvant et à séparer les multiples types d'éléments de terres rares les uns des autres par le biais d'une séparation solide-liquide. Le premier four de réchauffage et le second four de réchauffage comprennent des dispositifs d'échange d'atmosphères au niveau des entrées et des sorties de la matière première de terres rares.
PCT/JP2013/071312 2013-08-07 2013-08-07 Appareil de séparation et de récupération de terres rares WO2015019434A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2015530599A JPWO2015019434A1 (ja) 2013-08-07 2013-08-07 希土類分離回収装置
PCT/JP2013/071312 WO2015019434A1 (fr) 2013-08-07 2013-08-07 Appareil de séparation et de récupération de terres rares

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PCT/JP2013/071312 WO2015019434A1 (fr) 2013-08-07 2013-08-07 Appareil de séparation et de récupération de terres rares

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108034964A (zh) * 2017-12-20 2018-05-15 宁波市鄞州智伴信息科技有限公司 一种从稀土矿中分离和提取磷钇稀土的工艺

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
WO2009119720A1 (fr) * 2008-03-26 2009-10-01 財団法人生産技術研究奨励会 Procédé et appareil pour la collecte d'éléments terres rares
WO2012137727A1 (fr) * 2011-04-08 2012-10-11 株式会社日立製作所 Procédé de séparation et de récupération de terres rares

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
WO2009119720A1 (fr) * 2008-03-26 2009-10-01 財団法人生産技術研究奨励会 Procédé et appareil pour la collecte d'éléments terres rares
WO2012137727A1 (fr) * 2011-04-08 2012-10-11 株式会社日立製作所 Procédé de séparation et de récupération de terres rares

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108034964A (zh) * 2017-12-20 2018-05-15 宁波市鄞州智伴信息科技有限公司 一种从稀土矿中分离和提取磷钇稀土的工艺
CN108034964B (zh) * 2017-12-20 2019-09-06 精细化学品集团有限公司 一种从稀土矿中分离和提取磷钇稀土的工艺

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