CN109280781A - A kind of method of decomposition and inversion Rare Earth Mine - Google Patents

A kind of method of decomposition and inversion Rare Earth Mine Download PDF

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Publication number
CN109280781A
CN109280781A CN201811242452.5A CN201811242452A CN109280781A CN 109280781 A CN109280781 A CN 109280781A CN 201811242452 A CN201811242452 A CN 201811242452A CN 109280781 A CN109280781 A CN 109280781A
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China
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rare earth
mine
carbon
fluorine
mischmetal
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CN201811242452.5A
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Chinese (zh)
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李洪明
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Priority to CN201811242452.5A priority Critical patent/CN109280781A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00Obtaining rare earth metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/04Making ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C35/00Master alloys for iron or steel
    • C22C35/005Master alloys for iron or steel based on iron, e.g. ferro-alloys

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a kind of methods that Rare Earth Mine is decomposed in conversion, i.e. after the mixing of ferro element, carbon, mischmetal mine or fluorine carbon cerium mischmetal mine, in the high temperature furnace that can be melted in the molten state, carry out fluorine removal, except phosphorus reaction obtains rare earth oxide, then dissolving with hydrochloric acid is added to obtain re chloride rare earth oxide, rare earth yield is up to 97%.

Description

A kind of method of decomposition and inversion Rare Earth Mine
Technical field
The present invention relates to rare earth metallurgy technical fields, in particular to a kind of to utilize ferro element and/or carbon in molten The method that mischmetal mine is decomposed in conversion under state.
Background technique
Rare Earth Mine is rare earth resources important in the world, wherein again including fluorine carbon cerium mischmetal mine, mischmetal mine, mine master Originate from inner mongolia Baotou and U.S. awns court of a feudal ruler Paasche.China Baotou mischmetal mine is that the first in the world is dilute greatly Tu Kuang.Industrial decomposition mischmetal mine has concentrated sulfuric acid high-temperature roasting method and caustic soda decomposition method at present.Concentrated sulfuric acid pyrolytic Method can generate strong corrosive gaseous hydrogen fluoride.Caustic soda decomposition method can generate a large amount of fluoride waste, and its yield only has 90%.
Summary of the invention
In view of above-mentioned shortcoming, the purpose of the present invention is to provide a kind of simple process, do not generate strong caustic gas and Fluoride waste, yield are higher, and can recycle phosphorus, fluorine, the method that Rare Earth Mine is decomposed in environment amenable conversion.
In order to achieve the above object, the invention adopts the following technical scheme: ferro element, carbon, mischmetal mine Or after the mixing of fluorine carbon cerium mischmetal mine, in the high temperature furnace that can be melted in the molten state, fluorine removal is carried out, except phosphorus reaction obtains To rare earth oxide, then dissolving with hydrochloric acid is added to obtain re chloride rare earth oxide, rare earth yield is up to 97%.
Specifically: a method of Rare Earth Mine is decomposed in conversion, comprising the following steps:
(1) fluorine carbon cerium mischmetal mine converts decomposition method: after fluorine carbon cerium mischmetal mine is mixed with carbon in the molten state, carrying out Fluorine removal reacts to obtain rare earth oxide, then adds dissolving with hydrochloric acid to obtain re chloride rare earth oxide.
(2) mischmetal mine converts decomposition method: in molten condition after mischmetal mine is mixed with carbon, ferro element Under, it carries out fluorine removal, obtain rare earth oxide except phosphorus reaction, then add dissolving with hydrochloric acid to obtain rare earth chloride rare earth oxide molten Liquid.
Further, in the step (1) fluorine carbon cerium mischmetal mine and carbon mass ratio are as follows: 1000:(30-100).
Further, in the step (2) mischmetal mine and ferro element, carbon mass ratio are as follows: 1000:(100- 300): (30-80).
Further, the carbon is selected from one of coke, petroleum coke, charcoal or a variety of.
Further, the ferro element be selected from fe, steel, iron oxide, iron sulfide it is one or more.
Further, the mischmetal mine is the composite ore of fluorine carbon cerium mischmetal mine and solitary stone ore.
Carbon is added in the present invention and reacts generation carbon tetrafluoride with the fluorine in Rare Earth Mine, ferro element is added and phosphorus reaction is raw At ferrophosphorus, present invention process does not generate hydrogen fluoride gas, does not generate without washing therefore fluoride waste, and rare earth yield is up to 97%, phosphorus Iron can be used for producing steel alloy, and carbon tetrafluoride gas can be used for electronics industry through collecting compression.
Specific embodiment
Embodiment 1
Mischmetal mine that 1 ton is come from packet header content 50% and 0.1 ton of petroleum coke are mixed and be fitted into electric arc furnaces, is then added 0.1 ton of iron filings, be powered melting, comes out of the stove after melting down.Gained Rare Earth Mine conversion ratio 98%, obtains re chloride through dissolving with hydrochloric acid.
Embodiment 2
The Sichuan fluorine carbon cerium mischmetal mine and 8kg coke powder of 100kg content 70% are mixed, are fitted into graphite crucible intermediate frequency furnace by several times Frit reaction is carried out, remaining be packed into two times is melted again after loading 54kg is to be melted for the first time, is come out of the stove after melting down, gained Rare earth conversion ratio 97.6% obtains re chloride through dissolving with hydrochloric acid.
The above is only highly preferred embodiment of the present invention, is not intended to limit the present invention in any form, and is appointed What those skilled in the art, without departing from the scope of the technical proposal of the invention, using in the method for the disclosure above Appearance makes many possible changes and modifications to technical solution of the present invention, is all within the protection scope of the claims.

Claims (6)

1. a kind of method that Rare Earth Mine is decomposed in conversion, which is characterized in that method includes the following steps:
(1) it after mixing fluorine carbon cerium mischmetal mine with carbon in the molten state, carries out fluorine removal to react to obtain rare earth oxide, so Dissolving with hydrochloric acid is added to obtain re chloride rare earth oxide afterwards;
Or
(2) after mischmetal mine being mixed with carbon, ferro element in the molten state, carry out fluorine removal, except phosphorus reaction obtain it is dilute Native oxide, then adds dissolving with hydrochloric acid to obtain re chloride rare earth oxide.
2. the method according to claim 1, wherein fluorine carbon cerium mischmetal mine and carbon in the step (1) Mass ratio are as follows: 1000:(30-100).
3. the method according to claim 1, wherein mischmetal mine and ferro element, carbon member in the step (2) The mass ratio of element are as follows: 1000:(100-300): (30-80).
4. method according to claim 1 to 3, which is characterized in that the carbon be selected from coke, petroleum coke, One of charcoal is a variety of.
5. method according to claim 1 to 3, which is characterized in that the ferro element be selected from fe, steel, Iron oxide, iron sulfide it is one or more.
6. method according to claim 1 or 3, which is characterized in that the mischmetal mine is for fluorine carbon cerium mischmetal mine and solely Occupy the composite ore of stone ore.
CN201811242452.5A 2018-10-24 2018-10-24 A kind of method of decomposition and inversion Rare Earth Mine Pending CN109280781A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811242452.5A CN109280781A (en) 2018-10-24 2018-10-24 A kind of method of decomposition and inversion Rare Earth Mine

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811242452.5A CN109280781A (en) 2018-10-24 2018-10-24 A kind of method of decomposition and inversion Rare Earth Mine

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Publication Number Publication Date
CN109280781A true CN109280781A (en) 2019-01-29

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109837385A (en) * 2019-04-15 2019-06-04 李洪明 A kind of method that Rare Earth Mine is decomposed in heating melting conversion
CN110684896A (en) * 2018-10-19 2020-01-14 华卫国 High-temperature smelting method for decomposing bastnaesite
WO2021097693A1 (en) * 2019-11-20 2021-05-27 包头稀土研究院 Smelting method for bastnaesite and use of carbon powder
CN114480888A (en) * 2022-01-28 2022-05-13 包头稀土研究院 Method for improving rare earth recovery rate of bastnaesite
CN115305366A (en) * 2022-08-18 2022-11-08 李洪明 Production method of rare earth silicate ore
CN115637339A (en) * 2022-08-25 2023-01-24 华卫国 Production process for extracting phosphorus product and rare earth product from monazite rare earth ore

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CN1373232A (en) * 2001-12-06 2002-10-09 东北大学 Carburizing chlorination process for extracting and separating cerium and non-Ce rare earth from rare-earth ore
CN101967555A (en) * 2010-10-25 2011-02-09 东北大学 Method for dipping and decomposing bastnaesite after activation
CN102399975A (en) * 2010-09-10 2012-04-04 周毅 Clean separation method for bastnaesite (bastnasite)
CN102399983A (en) * 2010-09-10 2012-04-04 周毅 Bastnaesite (bastnasite) separation method
CN103184332A (en) * 2013-03-29 2013-07-03 四川省彭山宇力化工有限公司 Method for roasting, converting and resolving fluorocarbon cerium rare earth mine by adding covering agent to calcium compound
CN105755279A (en) * 2016-05-19 2016-07-13 东北大学 Method for microwave heating, chlorinating and decomposing Baotou mixed rare earth concentrate
CN106048265A (en) * 2016-08-17 2016-10-26 成都理工大学 Extraction method of rare-earth elements from bastnaesite

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CN1373232A (en) * 2001-12-06 2002-10-09 东北大学 Carburizing chlorination process for extracting and separating cerium and non-Ce rare earth from rare-earth ore
CN102399975A (en) * 2010-09-10 2012-04-04 周毅 Clean separation method for bastnaesite (bastnasite)
CN102399983A (en) * 2010-09-10 2012-04-04 周毅 Bastnaesite (bastnasite) separation method
CN101967555A (en) * 2010-10-25 2011-02-09 东北大学 Method for dipping and decomposing bastnaesite after activation
CN103184332A (en) * 2013-03-29 2013-07-03 四川省彭山宇力化工有限公司 Method for roasting, converting and resolving fluorocarbon cerium rare earth mine by adding covering agent to calcium compound
CN105755279A (en) * 2016-05-19 2016-07-13 东北大学 Method for microwave heating, chlorinating and decomposing Baotou mixed rare earth concentrate
CN106048265A (en) * 2016-08-17 2016-10-26 成都理工大学 Extraction method of rare-earth elements from bastnaesite

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110684896A (en) * 2018-10-19 2020-01-14 华卫国 High-temperature smelting method for decomposing bastnaesite
CN109837385A (en) * 2019-04-15 2019-06-04 李洪明 A kind of method that Rare Earth Mine is decomposed in heating melting conversion
WO2021097693A1 (en) * 2019-11-20 2021-05-27 包头稀土研究院 Smelting method for bastnaesite and use of carbon powder
JP2023503871A (en) * 2019-11-20 2023-02-01 包頭稀土研究院 Method for smelting bastnaesite ore and use of carbon powder
JP7296526B2 (en) 2019-11-20 2023-06-22 包頭稀土研究院 Method for smelting bastnaesite ore and use of carbon powder
CN114480888A (en) * 2022-01-28 2022-05-13 包头稀土研究院 Method for improving rare earth recovery rate of bastnaesite
CN115305366A (en) * 2022-08-18 2022-11-08 李洪明 Production method of rare earth silicate ore
CN115305366B (en) * 2022-08-18 2024-06-11 李洪明 Production method of rare earth silicate ore
CN115637339A (en) * 2022-08-25 2023-01-24 华卫国 Production process for extracting phosphorus product and rare earth product from monazite rare earth ore
CN115637339B (en) * 2022-08-25 2023-12-01 华卫国 Production process for extracting phosphorus product and rare earth product from monazite rare earth ore

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Application publication date: 20190129