CN103484668A - Weathering crust illuviation-type rare-earth ore leaching agent and method for extracting rare earths by using same - Google Patents

Weathering crust illuviation-type rare-earth ore leaching agent and method for extracting rare earths by using same Download PDF

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Publication number
CN103484668A
CN103484668A CN201310481335.5A CN201310481335A CN103484668A CN 103484668 A CN103484668 A CN 103484668A CN 201310481335 A CN201310481335 A CN 201310481335A CN 103484668 A CN103484668 A CN 103484668A
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rare
earth
citrate
ore
leaching
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池汝安
李琼
徐志高
张臻悦
何正艳
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Wuhan Institute of Technology
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Wuhan Institute of Technology
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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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Abstract

The invention provides a weathering crust illuviation-type rare-earth ore leaching agent and a method for extracting rare earths by using the same, particularly a leaching agent solution for weathering crust illuviation-type rare-earth ores. The active component is citrate, wherein the citrate is any one of ammonium citrate, sodium citrate, potassium citrate and magnesium citrate, or mixture of sodium citrate, potassium citrate and magnesium citrate. The method for extracting rare earths from weathering crust illuviation-type rare-earth ores comprises the following steps: leaching by using the citrate as the active component of the leaching agent to obtain a rare-earth leaching mother solution, removing impurities, and adding a precipitant to obtain a rare-earth enriched substance. In the weathering crust illuviation-type rare-earth extraction process, cation exchange interaction and anion (citrate ion) complex action exist, and the two actions can cooperate to enhance the rare-earth recovery rate and lower the concentration and consumption of the leaching agent.

Description

A kind of weathered superficial leaching rare-earth ore soaks the method for ore deposit agent and Extraction of rare earth thereof
Technical field
The invention belongs to the hydrometallurgy field, be specifically related to a kind of method that weathered superficial leaching rare-earth ore soaks ore deposit agent and Extraction of rare earth thereof.
Background technology
Weathered superficial leaching rare-earth ore is a kind of special rare earth mineral, and middle heavy rare earths partition is high, is the strategic mineral of national development.The weathered superficial leaching rare-earth ore rare earth elements mainly is adsorbed on clay mineral with the form of hydration or hydroxyl hydrated ion, and the rare earth grade is low, is only 0.05～0.3%.Ore grain size is superfine, the rare earth more than 50% be stored in productive rate be 24～32%-the 0.78mm grade in, it is corresponding rare earth ore concentrate that conventional physical concentration can't make rare-earth enrichment, so can only adopt chemical leaching technology.
When weathered superficial leaching rare-earth ore is used the drip washing of salt electrolyte solution, rare earth ion will exchanged get off, and is similar to ion exchange process.No matter be highly basic, strong acid, salt of weak acid, strong acid weak base salt, high price salt or low price salt or organic acid, and can form the alkali of title complex with rare earth, when strength of solution is suitable, all can effectively leach the Ion Phase rare earth in weathered superficial leaching rare-earth ore.
In order to improve leaching efficiency, reduce resource consumption, reduce environmental pollution, realize the efficient utilization of weathered superficial leaching rare-earth resource, people start with from every side its leaching technology are improved, and wherein, the selection of soaking the ore deposit agent directly has influence on the height of leaching yield, produces required cost, therefore very important, be the problem of the current primary study of a lot of scientists.The ore deposit agent of soaking of generally using at present is generally 1～4% ammonium sulfate, has higher rare earth yield, but in south, produces lessly, and ore dressing of rare earth is very large to its demand, therefore usually cause that supply falls short of demand.Therefore, find a kind of alternative ammonium sulfate to soak the ore deposit agent very necessary.
Summary of the invention
The object of the invention is to provide a kind of new weathered superficial leaching rare-earth ore to soak the ore deposit agent, this Novel immersion ore deposit agent is in the process of leaching rare earth, not only exist cationic exchange interaction also to exist the cooperation of negatively charged ion to help the effect of soaking, soak the ore deposit agent with the ammonium sulfate generally used at present and compare, there are the characteristics of lower leaching concentration and less consumption.
For achieving the above object, adopt technical scheme as follows:
A kind of for weathered superficial leaching rare-earth ore soak the ore deposit agent solution, its activeconstituents is Citrate trianion.
Press such scheme, described Citrate trianion be ammonium citrate, Trisodium Citrate, Tripotassium Citrate and magnesium citrate any one or mix arbitrarily.
Press such scheme, described Citrate trianion active component content is 0.5-2.0wt%.
Press such scheme, the described ore deposit agent solution pH value of soaking is between 3.0-8.0.
A kind of from weathered superficial leaching rare-earth ore the method for Extraction of rare earth, comprise and use Citrate trianion to obtain rare earth leaching mother liquor as soaking ore deposit agent activeconstituents, removal of impurities, add precipitation agent to obtain rareearth enriching material.
Press such scheme, described Citrate trianion be ammonium citrate, Trisodium Citrate, Tripotassium Citrate and magnesium citrate any one or mix arbitrarily.
Press such scheme, described Citrate trianion active component content is 0.5-2wt%.
Press such scheme, also comprise and regulate the pH value to 3.0-8.0 to soaking the ore deposit agent solution.
Press such scheme, adopt hydrochloric acid while regulating the pH value.
Press such scheme, described precipitation agent is oxalic acid or bicarbonate of ammonia.
Weathered superficial leaching rare-earth ore leaching essence is an ion exchange reaction, the clay Rare Earth Ion with soak cationic exchange process in the agent of ore deposit.The chemical equation of ammonium sulfate when soaking the ore deposit agent is as follows:
[Al 4(Si 4O 10)(OH) 8] m·nRE 3+ (s)+3nNH 4 + (aq)=[Al 4(Si 4O 10)(OH) 8] m·3nNH 4 + (s)+nRE (aq)
Thereby the exchange cation-adsorption occurs to mineral surface in the rare earth ion of leaching exchange cation and mineral surface, and rare earth ion enters in solution.Soak the ore deposit agent while being Citrate trianion when used, following chemical reaction occur:
[Al 4(Si 4O 10)(OH) 8] m·nRE 3+ (s)+nC 6H 5O 7 3-+3nM (aq)=[Al 4(Si 4O 10)(OH) 8] m·3nM (s)+nC 6H 5O 7REM=NH 4 +,Na +,K +,Mg 2+/2
From above reaction, in soaking the ore deposit process, the positively charged ion of citric acid has played the ion exchange with rare earth ion, and negatively charged ion (citrate ion) participates in the mating reaction of rare earth ion, having promoted to soak the ore deposit reaction carries out to the right, promote the leaching of rare earth, thereby improved rare earth yield.
Beneficial effect of the present invention is:
1) the present invention use in Citrate trianion a kind of or wherein several mixture as soaking the ore deposit agent, soaking the ore deposit agent with other of current use compares, in the process that weathered superficial leaching rare-earth extracts, except there being cationic exchange interaction also to have the mating reaction of negatively charged ion (citrate ion), two kinds of collaborative rare earth yields that can improve of effect reduce working concentration and the consumption that soaks the ore deposit agent.
2) Citrate trianion used, containing containing the ammonium root on a small quantity or not, can reduce ammonia nitrogen waste water and pollute, and can eliminate ammonia nitrogen waste water if use without ammonium salt and pollute.
Embodiment
Below in conjunction with example, the invention will be further described, but do not limit the present invention.
The mensuration of Ion Phase rare earth total content: the weathered superficial leaching rare-earth ore 250.0g that takes oven dry, the ammoniumsulphate soln that is 2% by mass percent is for soaking the ore deposit agent, weathered superficial leaching rare-earth ore is carried out to post to be soaked, until almost do not have rare earth to leach, merge and collect leaching liquid, the total Ion Phase content of rare earth of EDTA volumetric determination is the REO1.139mmol/250g rare-earth mineral.
Embodiment 1
Take the weathered superficial leaching rare-earth ore 250.0g of oven dry, the ammonium citrate ((NH that the preparation mass percent is 0.5% 4) 3c 6h 5o 7) solution is for soaking the ore deposit agent, ratio in solid-to-liquid ratio (solid masses with soak ore deposit agent volume ratio) 1:2, regulate flow rate control at 0.4mL/min, weathered superficial leaching rare-earth ore is carried out to post to be soaked, obtaining rare earth leaching mother liquor employing EDTA volumetric determination content of rare earth is the REO1.119mmol/250g rare-earth mineral, with the oxalate precipitation method enrichment, filter calcination under 900 ℃ of conditions after washing after removal of impurities.
Measure by analysis, rare earth yield be 94.3%(calcination thing directly weigh be recycled rate with total Ion Phase content of rare earth contrast), purity is that 92.6%(adopts GB/T14635-2008).
Embodiment 2
Take the weathered superficial leaching rare-earth ore 250.0g of oven dry, the magnesium citrate (Mg that the preparation mass percent is 1.5% 2(C 6h 5o 7) 3) solution is for soaking the ore deposit agent, add salt acid for adjusting pH to 5.0, ratio in solid-to-liquid ratio 1:2, regulate flow rate control at 0.4mL/min, weathered superficial leaching rare-earth ore is carried out to post to be soaked, obtaining rare earth leaching mother liquor, to adopt EDTA volumetric determination content of rare earth be the REO0.0962mmol/250g rare-earth mineral, after removal of impurities with the oxalate precipitation method enrichment, calcination under 900 ℃ of conditions after filtration washing.
Measure by analysis, rare earth yield is 92.3%, and purity is 92.3%.
Embodiment 3
Take the weathered superficial leaching rare-earth ore 250.0g of oven dry, the Trisodium Citrate (Na that the preparation mass percent is 1.0% 3c 6h 5o 72H 2o) solution is for soaking the ore deposit agent, ratio in solid-to-liquid ratio 1:2, regulate flow rate control at 0.4mL/min, weathered superficial leaching rare-earth ore is carried out to post to be soaked, obtaining rare earth leaching mother liquor employing EDTA volumetric determination content of rare earth is the REO1.108mmol/250g rare-earth mineral, after removal of impurities with the ammonium bicarbonate precipitation method enrichment, calcination under 900 ℃ of conditions after filtration washing.
Measure by analysis, rare earth yield is 93.4%, and purity is 92.1%.
Embodiment 4
Take the weathered superficial leaching rare-earth ore 250.0g of oven dry, the Tripotassium Citrate (K that the preparation mass percent is 1.0% 3c 6h 5o 7h 2o) solution is for soaking the ore deposit agent, ratio in solid-to-liquid ratio 1:2, regulate flow rate control at 0.4mL/min, weathered superficial leaching rare-earth ore is carried out to post to be soaked, obtaining rare earth leaching mother liquor employing EDTA volumetric determination content of rare earth is the REO1.110mmol/250g rare-earth mineral, after removal of impurities with the ammonium bicarbonate precipitation method enrichment, calcination under 900 ℃ of conditions after filtration washing.
Measure by analysis, rare earth yield is 93.6%, and purity is 92.7%.
Embodiment 5
Take the weathered superficial leaching rare-earth ore 250.0g of oven dry, the following Citrate trianion that mixes of preparation soaks ore deposit agent (mass percent): 0.5% Trisodium Citrate, 0.5% Tripotassium Citrate, 0.5% magnesium citrate, all the other are water, adding the salt acid for adjusting pH is 7.3, ratio in solid-to-liquid ratio 1:2, regulate flow rate control at 0.4mL/min, weathered superficial leaching rare-earth ore is carried out to post to be soaked, obtaining rare earth leaching mother liquor employing EDTA volumetric determination content of rare earth is the REO1.111mmol/250g rare-earth mineral, after removal of impurities with the oxalate precipitation method enrichment, calcination under 900 ℃ of conditions after filtration washing.
Measure by analysis, rare earth yield is 94.2%, and purity is 92.2%.
Embodiment 6
Take the weathered superficial leaching rare-earth ore 250.0g of oven dry, in the ratio of solid-to-liquid ratio 1:2, use respectively 1% ammonium sulfate and 1.28% ammonium citrate ((NH 4) 3c 6h 5o 7) solution is for soaking the ore deposit agent, consistent (the 0.151mol/L NH of ammonium ion content in two kinds of ammonium salts that this time use 4 +), weathered superficial leaching rare-earth ore is carried out to post and soaks, obtain rare earth leaching mother liquor and adopt EDTA volumetric determination content of rare earth, after removal of impurities with the oxalate precipitation method enrichment, calcination under 900 ℃ of conditions after filtration washing.
Measure by analysis, ammonium sulfate leach liquor Rare-Earth Content is the REO0.9646mmol/250g rare-earth mineral, and rare earth yield is 81.3%, and purity is 92.3%; And ammonium citrate leach liquor Rare-Earth Content is the REO1.127mmol/250g rare-earth mineral, rare earth yield is 95.0%, and purity is 92.2%.
Embodiment 7
Take the weathered superficial leaching rare-earth ore 250.0g of oven dry, use respectively 2% Trisodium Citrate (Na in the ratio of solid-to-liquid ratio 1:2 3c 6h 5o 72H 2o) and 1.192% sodium chloride solution for soaking the ore deposit agent, the consistent (0.204mol/LNa of sodium ions content in two kinds of ammonium salts that this time use +), weathered superficial leaching rare-earth ore is carried out to post and soaks, obtain rare earth leaching mother liquor and adopt EDTA volumetric determination content of rare earth, after removal of impurities with the oxalate precipitation method enrichment, calcination under 900 ℃ of conditions after filtration washing.
Measure by analysis, Leaching of sodium chloride liquid Rare-Earth Content is the 0.3319mmol/250g rare-earth mineral, and rare earth yield is 28.1%, and purity is 92.6%; And ammonium citrate leach liquor Rare-Earth Content is the 1.126mmol/250g rare-earth mineral, rare earth yield is 94.9%, and purity is 92.3%.
Embodiment 8
Take the weathered superficial leaching rare-earth ore 250.0g of oven dry, in the ratio of solid-to-liquid ratio 1:2, use respectively 1.5% sal epsom and 1.88% magnesium citrate solution (Mg 2(C 6h 5o 7) 3) for soaking the ore deposit agent, two kinds that this time use are soaked consistent (the 0.125mol/L Mg of magnesium ion content in the agent of ore deposit 2+), weathered superficial leaching rare-earth ore is carried out to post and soaks, obtain rare earth leaching mother liquor and adopt EDTA volumetric determination content of rare earth, after removal of impurities with the oxalate precipitation method enrichment, calcination under 900 ℃ of conditions after filtration washing.
Measure by analysis, sal epsom leach liquor Rare-Earth Content is that 0.7393mmol/250g rare-earth mineral rare earth yield is 62.3%, and purity is 92.0%; And ammonium citrate leach liquor Rare-Earth Content is 1.112mmol/250g rare-earth mineral rare earth yield, be 93.7%, purity is 92.1%.
The result of example 6,7,8 can find out, when soaking ore deposit agent cation concn one regularly, the rare earth leaching yield that Citrate trianion soaks the ore deposit agent is higher, because citrate has promoted to soak with the mating reaction of rare earth ion the carrying out that react in ore deposit, has improved rare earth yield.

Claims (10)

  1. One kind for weathered superficial leaching rare-earth ore soak the ore deposit agent solution, it is characterized in that activeconstituents is Citrate trianion.
  2. As claimed in claim 1 for weathered superficial leaching rare-earth ore soak the ore deposit agent solution, it is characterized in that described Citrate trianion be ammonium citrate, Trisodium Citrate, Tripotassium Citrate and magnesium citrate any one or mix arbitrarily.
  3. As claimed in claim 1 for weathered superficial leaching rare-earth ore soak the ore deposit agent solution, it is characterized in that described Citrate trianion active component content is 0.5-2.0wt%.
  4. As claimed in claim 1 for weathered superficial leaching rare-earth ore soak the ore deposit agent solution, it is characterized in that the described ore deposit agent solution pH value of soaking between 3.0-8.0.
  5. 5. the method for an Extraction of rare earth from weathered superficial leaching rare-earth ore, comprise and use Citrate trianion to obtain rare earth leaching mother liquor as soaking ore deposit agent activeconstituents, and removal of impurities, add precipitation agent to obtain rareearth enriching material.
  6. 6. the method for Extraction of rare earth from weathered superficial leaching rare-earth ore as claimed in claim 5, it is characterized in that described Citrate trianion be ammonium citrate, Trisodium Citrate, Tripotassium Citrate and magnesium citrate any one or mix arbitrarily.
  7. 7. the method for Extraction of rare earth from weathered superficial leaching rare-earth ore as claimed in claim 5, is characterized in that described Citrate trianion active component content is 0.5-2wt%.
  8. 8. the method for Extraction of rare earth from weathered superficial leaching rare-earth ore as claimed in claim 5, characterized by further comprising and regulate the pH value to 3.0-8.0 to soaking the ore deposit agent solution.
  9. 9. the method for Extraction of rare earth from weathered superficial leaching rare-earth ore as claimed in claim 5, adopt hydrochloric acid while it is characterized in that regulating the pH value.
  10. 10. the method for Extraction of rare earth from weathered superficial leaching rare-earth ore as claimed in claim 5, is characterized in that described precipitation agent is oxalic acid or bicarbonate of ammonia.
CN201310481335.5A 2013-10-15 2013-10-15 Weathering crust illuviation-type rare-earth ore leaching agent and method for extracting rare earths by using same Pending CN103484668A (en)

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CN103924105A (en) * 2014-03-17 2014-07-16 赵书生 Novel method for leaching rare earth
CN104459083A (en) * 2014-11-28 2015-03-25 武汉工程大学 Mineral prospecting method for middle and heavy rare earth enrichment area of weathered crust elution-deposited rare earth ore
CN104498738A (en) * 2014-11-28 2015-04-08 武汉工程大学 Method for leaching rare earth from weathering crust leaching type rare-earth ore heap
CN104611547A (en) * 2015-03-09 2015-05-13 龙南县锦易矿业有限公司 Ore leaching process for south rare earth ore
CN105331835A (en) * 2015-10-11 2016-02-17 江西理工大学 Auxiliary leaching agent applied to ion-absorbed rare earth ore leaching process and ore leaching method of auxiliary leaching agent
CN105695741A (en) * 2016-02-29 2016-06-22 中铝广西有色崇左稀土开发有限公司 Ionic type rare earth mother solution treatment process
CN108998663A (en) * 2018-09-30 2018-12-14 许瑞高 It is a kind of to leach ion adsorption type re technique with aluminum aluminum sulfate work leaching mine agent
CN113025817A (en) * 2021-03-09 2021-06-25 中南大学 Method for extracting weathering crust elution-deposited rare earth ore
CN113046554A (en) * 2021-03-09 2021-06-29 中南大学 Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism
CN113151697A (en) * 2021-03-09 2021-07-23 中南大学 Method for leaching weathering crust leaching type rare earth ore
CN115181866A (en) * 2022-07-25 2022-10-14 中南大学 Combined leaching agent and application thereof in anode leaching

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103924105A (en) * 2014-03-17 2014-07-16 赵书生 Novel method for leaching rare earth
CN104459083A (en) * 2014-11-28 2015-03-25 武汉工程大学 Mineral prospecting method for middle and heavy rare earth enrichment area of weathered crust elution-deposited rare earth ore
CN104498738A (en) * 2014-11-28 2015-04-08 武汉工程大学 Method for leaching rare earth from weathering crust leaching type rare-earth ore heap
CN104459083B (en) * 2014-11-28 2016-04-13 武汉工程大学 The methods of prospecting for ore deposits of heavy rare earth enrichment region in a kind of weathered superficial leaching rare-earth ore
CN104611547A (en) * 2015-03-09 2015-05-13 龙南县锦易矿业有限公司 Ore leaching process for south rare earth ore
CN105331835B (en) * 2015-10-11 2017-07-28 江西理工大学 A kind of leaching agent and its leaching ore deposit method that ore deposit process is soaked applied to ion type rareearth ore
CN105331835A (en) * 2015-10-11 2016-02-17 江西理工大学 Auxiliary leaching agent applied to ion-absorbed rare earth ore leaching process and ore leaching method of auxiliary leaching agent
CN105695741A (en) * 2016-02-29 2016-06-22 中铝广西有色崇左稀土开发有限公司 Ionic type rare earth mother solution treatment process
CN108998663A (en) * 2018-09-30 2018-12-14 许瑞高 It is a kind of to leach ion adsorption type re technique with aluminum aluminum sulfate work leaching mine agent
CN113025817A (en) * 2021-03-09 2021-06-25 中南大学 Method for extracting weathering crust elution-deposited rare earth ore
CN113046554A (en) * 2021-03-09 2021-06-29 中南大学 Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism
CN113151697A (en) * 2021-03-09 2021-07-23 中南大学 Method for leaching weathering crust leaching type rare earth ore
CN113025817B (en) * 2021-03-09 2021-12-31 中南大学 Method for extracting weathering crust elution-deposited rare earth ore
CN113046554B (en) * 2021-03-09 2022-03-11 中南大学 Method for leaching weathering crust elution-deposited rare earth ore by using metabolite of microorganism
CN115181866A (en) * 2022-07-25 2022-10-14 中南大学 Combined leaching agent and application thereof in anode leaching

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Application publication date: 20140101