CN105331836B - A kind of method of outfield intensifying without ammonia leached ions type Rare Earth Mine - Google Patents

A kind of method of outfield intensifying without ammonia leached ions type Rare Earth Mine Download PDF

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Publication number
CN105331836B
CN105331836B CN201510675018.6A CN201510675018A CN105331836B CN 105331836 B CN105331836 B CN 105331836B CN 201510675018 A CN201510675018 A CN 201510675018A CN 105331836 B CN105331836 B CN 105331836B
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rare earth
ammonia
leaching
earth mine
ion
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CN105331836A (en
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尹少华
谢峰
张利波
彭金辉
李世伟
郭胜惠
周俊文
代林晴
许磊
张利华
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Kunming University of Science and Technology
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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
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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

Abstract

The present invention relates to a kind of method of outfield intensifying without ammonia leached ions type Rare Earth Mine, belong to technical field of wet metallurgy.By ion type rareearth ore according to liquid-solid ratio be 1:1~20:1ml/g adds concentration and leaches agent solution without ammonia salt for 1wt%~10wt%, 10~180min of leaching in the presence of room temperature ultrasonic, leach and obtain leachate through solid-liquor separation after completing, wherein without the mixture that ammonia salt leaching agent is calcium chloride or calcium chloride and any ratio of magnesium sulfate.The present invention reduces the generation of ammonia nitrogen waste water while high rare earth leaching rate is ensured, is a kind of green, economic new technology.

Description

A kind of method of outfield intensifying without ammonia leached ions type Rare Earth Mine
Technical field
The present invention relates to a kind of method of outfield intensifying without ammonia leached ions type Rare Earth Mine, belongs to hydrometallurgical technology neck Domain.
Background technology
Rare earth is universally acknowledged developing high-tech, national defence sophisticated technology, indispensable strategy of rebuilding traditional industry Resource.Ion type rareearth ore have it is light, in, heavy rare earth partition it is complete, rich in close with high-tech, high tip, new material industry In related, heavy rare earth element, utilization ion type rareearth ore occupies great strategic position in China's economic development.
The leaching process of ion type rareearth ore is successively selected using sodium chloride and ammonium sulfate as leaching agent, the leaching of ammonium sulfate Selecting property is substantially better than sodium chloride, is advantageous to the extraction of leaching liquid Rare Earth Ion, is the main leaching agent that current rare earth leaches.But It is that ammonium sulfate leaching agent can bring substantial amounts of ammonia nitrogen waste water, to produce 3000 tons of rare earth per year(REO is counted), caused wastewater treatment capacity About 1,800,000 tons/year, about 6000 tons/year of ammonia nitrogen discharge capacity, and pollution control cost is high;In addition, when ammonium sulfate leaches rare earth, leaching It is big to go out agent consumption, causes the wasting of resources.Therefore, developing green, efficient leaching process reduces ammonia nitrogen waste water pollution, realizes economic ring Sustainable development of the Extraction of rare eart of guarantor to China's rare-earth industry has far-reaching significance.
In recent years, outfield intensifying leaching-out technique(Ultrasonic wave)It has been increasingly being applied to metallurgical industry, such as gold, silver, copper The Strengthen education of ore deposit, the microjet for being produced strong impact and high speed to reaction-ure surface using the cavitation effect of ultrasonic wave are rushed Erosion so that the chemical reaction under ultrasound field is easily carried out, and reaches the process of Strengthen education, has certain development prospect.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of outfield intensifying without ammonia leached ions type The method of Rare Earth Mine.The present invention reduces the generation of ammonia nitrogen waste water while high rare earth leaching rate is ensured, be a kind of green, Economic new technology, the present invention are achieved through the following technical solutions.
A kind of method of outfield intensifying without ammonia leached ions type Rare Earth Mine, it is comprised the following steps that:By ion type rareearth ore It is 1 according to liquid-solid ratio:1~20:1ml/g adds concentration and leaches agent solution without ammonia salt for 1wt%~10wt%, in room temperature ultrasonic In the presence of 10~180min of leaching, leach and through solid-liquor separation obtain leachate after completing, wherein being without ammonia salt leaching agent The mixture of calcium chloride or calcium chloride and any ratio of magnesium sulfate.
The ion type rareearth ore refers to that rare earth adsorbs the south on clay mineral with hydrated ion or hydroxyl hydrated ion Square ion type rareearth ore.
The power of the ultrasonic wave is more than 100W.
The beneficial effects of the invention are as follows:(1)The present invention uses no ammonia leaching agent as raw material, fundamentally solves ammonia nitrogen dirt The technical barrier of dye, meet the industrial policy of national development rare-earth trade.(2)The present invention uses the leaching of intensified by ultrasonic wave rare earth Go out, the technology has the advantages that simple to operate, pollution-free while leaching rate is greatly improved.(3)Pass through the method for the present invention Rare earth leaching rate can reach 99.62%, and rare earth leaching rate 72.55% when ammonium sulfate leaches, and improve 37.31%.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
Method of the outfield intensifying without ammonia leached ions type Rare Earth Mine, it is comprised the following steps that:By 1kg ion type rareearth ores (Ion type rareearth ore refers to that rare earth adsorbs the southern ion type rareearth on clay mineral with hydrated ion or hydroxyl hydrated ion Ore deposit, mass percent component are as shown in table 1)It is 1 according to liquid-solid ratio:It is the molten without ammonia salt leaching agent of 1wt% that 1ml/g, which adds concentration, Liquid, the leaching 10min in the presence of room temperature ultrasonic, leach and obtain leachate through solid-liquor separation after completing, wherein without ammonia Salt leaching agent is calcium chloride, and the power of ultrasonic wave is 1500W.
Table 1
The leachate that the present embodiment is prepared uses EDTA titration measuring rare earth leaching rates, is soaked under the conditions of being somebody's turn to do Extracting rate is 92.34%.
Embodiment 2
Method of the outfield intensifying without ammonia leached ions type Rare Earth Mine, it is comprised the following steps that:By 1kg ion type rareearth ores (Ion type rareearth ore refers to that rare earth adsorbs the southern ion type rareearth on clay mineral with hydrated ion or hydroxyl hydrated ion Ore deposit, mass percent component are as shown in table 2)It is 20 according to liquid-solid ratio:1ml/g addition concentration is 10wt% without ammonia salt leaching agent Solution, the leaching 180min in the presence of room temperature ultrasonic, leach and through solid-liquor separation obtain leachate after completing, wherein without Ammonia salt leaching agent is mass ratio 1:1 calcium chloride and sulfuric acid magnesium compound, the power of ultrasonic wave is 100W.
Table 2
The leachate that the present embodiment is prepared uses EDTA titration measuring rare earth leaching rates, is soaked under the conditions of being somebody's turn to do Extracting rate is 99.62%.
Embodiment 3
Method of the outfield intensifying without ammonia leached ions type Rare Earth Mine, it is comprised the following steps that:By 1kg ion type rareearth ores (Ion type rareearth ore refers to that rare earth adsorbs the southern ion type rareearth on clay mineral with hydrated ion or hydroxyl hydrated ion Ore deposit, mass percent component are as shown in table 3)It is 10 according to liquid-solid ratio:It is the molten without ammonia salt leaching agent of 8wt% that 1ml/g, which adds concentration, Liquid, the leaching 120min in the presence of room temperature ultrasonic, leach and obtain leachate through solid-liquor separation after completing, wherein without ammonia Salt leaching agent is mass ratio 2:1 calcium chloride and sulfuric acid magnesium compound, the power of ultrasonic wave is 1500W.
Table 3
The leachate that the present embodiment is prepared uses EDTA titration measuring rare earth leaching rates, is soaked under the conditions of being somebody's turn to do Extracting rate is 93.68%.
The embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party Formula, in those of ordinary skill in the art's possessed knowledge, it can also make on the premise of present inventive concept is not departed from Go out various change.

Claims (1)

1. method of a kind of outfield intensifying without ammonia leached ions type Rare Earth Mine, it is characterised in that comprise the following steps that:By ionic Rare Earth Mine, ion type rareearth ore refer to that rare earth adsorbs the southern ion on clay mineral with hydrated ion or hydroxyl hydrated ion Type Rare Earth Mine, it is 1 according to liquid-solid ratio:1ml/g adds concentration and leaches agent solution without ammonia salt for 1wt%, in the work of room temperature ultrasonic With lower leaching 10min, leach and obtain leachate through solid-liquor separation after completing, wherein being calcium chloride without ammonia salt leaching agent, surpass The power of sound wave is 1500W.
CN201510675018.6A 2015-10-19 2015-10-19 A kind of method of outfield intensifying without ammonia leached ions type Rare Earth Mine Active CN105331836B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110144456A (en) * 2019-06-20 2019-08-20 许瑞高 The technique that calcium chloride directly leaches ion type rareearth is produced with dissolving with hydrochloric acid calcium salt
CN111926180B (en) * 2020-08-14 2022-02-11 南昌大学 Method for extracting ion adsorption type rare earth
CN112410554A (en) * 2020-11-02 2021-02-26 江西理工大学 Environment-friendly extraction method of ionic rare earth ore calcium salt
CN113553787B (en) * 2021-07-22 2023-04-25 江西理工大学 Numerical simulation method for agitation leaching process of ionic rare earth ore

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CN1920068A (en) * 2006-08-22 2007-02-28 扬州大学 Ultrasound leaching technique of concentrated sulfuric acid roasting rare earth concentrate
CN101476033B (en) * 2008-10-28 2011-04-06 黄日平 Novel method for leaching, impurity removing and precipitating ion type rare earth ore
CN102190325B (en) * 2010-03-17 2014-07-16 有研稀土新材料股份有限公司 Method for recovering rare earth from ionic type rare earth crude ore
CN103266224B (en) * 2013-05-27 2016-06-22 江西理工大学 A kind of ion adsorption type re extracting method

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