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Recovery of Rare Earth Elements from an Apatite Concentrate
KTH, Skolan för kemi, bioteknologi och hälsa (CBH), Kemiteknik, Teknisk strömningslära.
2018 (engelsk)Doktoravhandling, med artikler (Annet vitenskapelig)
Abstract [en]

Rare earth elements (REE) are a group of 17 elements including lanthanides, yttrium and scandium; which are found in a variety of classes of minerals worldwide. The criticality of the application, lack of high grade and economically feasible REE resources and a monopolistic supply situation has raised significant attention in recovery of these metals from low grade ores and waste materials. In this thesis, the recovery of REE from an apatite concentrate, containing 0.5 mass% of REE, within the nitrophosphate route of fertilizer production has been investigated. Most of the REE (≥ 95%) content can be recovered into a phosphate precipitate with almost 30 mass% REE. Different processes have been developed to convert the REE phosphate precipitate into a more soluble form to obtain a solution suitable for further REE purification and individual separation. It has been shown that after reprecipitation of the REE phosphate concentrate as REE sodium double sulphate and then transformation into a REE hydroxide concentrate, a solution containing 45g/L REE free of Ca, Fe and P can be obtained. The results suggest that the apatite waste after processing of iron ore have the potential to be a very important source for REE in Europe and that the economy is strongly supported by the simultaneous extraction of phosphorous.

The potential of using hollow fiber supported liquid membrane (HFSLM) extraction in individual and group separation of REE has been investigated. A hollow fiber supported liquid membrane plant in pilot scale has been operated according to the three main configurations: standard hollow fiber supported liquid membrane technology (HFSLM); hollow fiber renewal liquid membrane technology (HFRSLM) and emulsion pertraction technology (EPT). The standard HFSLM operation is more selective than HFRSLM and EPT, while higher metal transport rate is observed in EPT followed by HFRSLM and HFSLM. The HFRLM configuration helps to maintain the performance of the liquid membrane.

sted, utgiver, år, opplag, sider
Stockholm, Sweden: KTH Royal Institute of Technology, 2018. , s. 86
Serie
TRITA-CBH-FOU ; 2018:49
Emneord [en]
Rare earth elements, precipitation, nitrophosphate process, hollow fiber supported liquid membrane extraction
HSV kategori
Forskningsprogram
Kemiteknik
Identifikatorer
URN: urn:nbn:se:kth:diva-239058ISBN: 978-91-7873-034-6 (tryckt)OAI: oai:DiVA.org:kth-239058DiVA, id: diva2:1263554
Disputas
2018-12-07, Kollegiesalen, Brinellvägen 8, KTH huset, Stockholm, 14:00 (engelsk)
Opponent
Veileder
Forskningsfinansiär
Swedish Foundation for Strategic Research , IRT 11-0026
Merknad

QC 20181116

Tilgjengelig fra: 2018-11-16 Laget: 2018-11-15 Sist oppdatert: 2018-11-16bibliografisk kontrollert
Delarbeid
1. Recovery of rare earth elements from nitrophosphoric acid solutions
Åpne denne publikasjonen i ny fane eller vindu >>Recovery of rare earth elements from nitrophosphoric acid solutions
2017 (engelsk)Inngår i: Hydrometallurgy, ISSN 0304-386X, E-ISSN 1879-1158, Vol. 169, s. 253-262Artikkel i tidsskrift (Fagfellevurdert) Published
Abstract [en]

In the present study, the recovery of rare earth elements (REEs) from an apatite concentrate in the nitrophosphate process of fertilizer production has been studied. The apatite concentrate has been recovered from iron ore tailings in Sweden by flotation. In the first step, the apatite is digested in concentrated nitric acid, after which Ca(NO3)2.4H2O is separated by cooling crystallization. The solution is then neutralized using ammonia whereby the REEs precipitate mainly as phosphates (REEPO4.nH2O) and together with calcium as REEn Cam (PO4)(3n + 2m) / 3. In this work, the degree of rare earth coprecipitation during seeded cooling crystallization of Ca(NO3)2.4H2O has been studied. The solubility of calcium nitrate tetrahydrate (Ca(NO3)2.4H2O) in acidic nitrophosphoric acid solutions in the temperature range of − 2 °C to 20 °C has been determined. For the neutralization step, it is shown that the calcium concentration and the final pH play an important role in determining the concentration of REEs in the precipitate. It is found that reaching maximum recovery of REE with minimum simultaneous precipitation of calcium requires careful control of the final pH to about 1.8. It is further observed that the precipitation yield of REEs and iron is favored by a longer residence time and higher temperature. Finally, the effect of seeding with synthesized REE phosphate crystals as well as a mixture of REE and Ca phosphates on the precipitation rate and the composition of the precipitate was studied.

sted, utgiver, år, opplag, sider
Elsevier, 2017
Emneord
Cooling crystallization, Nitrophosphate process, REE, Seeded precipitation, Selective precipitation, Apatite, Calcium, Cooling, Flotation, Iron ores, Metal recovery, Ore tailings, Ore treatment, Phosphate minerals, Phosphates, Rare earth elements, Rare earths, Recovery, Calcium nitrate tetra-hydrate, Concentrated nitric acid, Nitrophosphate, Rare earth elements (REEs), Simultaneous precipitation, Precipitation (chemical)
HSV kategori
Identifikatorer
urn:nbn:se:kth:diva-207347 (URN)10.1016/j.hydromet.2017.01.008 (DOI)000401878200031 ()2-s2.0-85011958720 (Scopus ID)
Forskningsfinansiär
Swedish Foundation for Strategic Research , IRT 11-0026
Merknad

QC 20170522

Tilgjengelig fra: 2017-05-22 Laget: 2017-05-22 Sist oppdatert: 2018-11-15bibliografisk kontrollert
2. Upgrading of a rare earth phosphate concentrate within the nitrophosphate process
Åpne denne publikasjonen i ny fane eller vindu >>Upgrading of a rare earth phosphate concentrate within the nitrophosphate process
2018 (engelsk)Inngår i: Journal of Cleaner Production, ISSN 0959-6526, E-ISSN 1879-1786, Vol. 198, s. 551-563Artikkel i tidsskrift (Fagfellevurdert) Published
Abstract [en]

In the nitrophosphate process of fertilizer production, rare earth elements (REE) can be recovered as a REE phosphate concentrate. In this process, after digestion of apatite in concentrated nitric acid, Ca(NO3)2.4H2O is first separated by cooling crystallization and then the REE are precipitated in phosphate form by a partial neutralization step using ammonia. The obtained REE phosphate concentrate is contaminated by mainly calcium and iron, and the main solid phases are CaHPO4.2H2O, FePO4.2H2O and REEPO4.nH2O.

In this study, a process to obtain a concentrate more enriched with REE with low concentration of calcium and iron and free of phosphorous is developed. In the developed process, enrichment and dephosphorization of the rare earth phosphate concentrate has been achieved by selective dissolution and re-precipitation of the REE as a sodium REE double sulfate salt. It is shown that by selective dissolution of the REE concentrate in nitric acid at a pH of 2.4, most of the calcium and phosphorus are dissolved, and a solid phase more enriched in REE is obtained. Thereafter, the REE phosphate concentrate is first dissolved in a mixture of sulfuric-phosphoric acid and then the REE are reprecipitated as NaREE(SO4)2.H2O by addition of a sodium salt. More than 95% of the Ca, Fe and P are removed and a REE concentrate containing almost 30 mass% total REE is obtained.

sted, utgiver, år, opplag, sider
Elsevier, 2018
Emneord
Nitrophosphate process, REE; precipitation, selective dissolution, sodium REE double sulfate
HSV kategori
Forskningsprogram
Kemiteknik
Identifikatorer
urn:nbn:se:kth:diva-231880 (URN)10.1016/j.jclepro.2018.06.242 (DOI)2-s2.0-85053137761 (Scopus ID)
Forskningsfinansiär
Swedish Foundation for Strategic Research , IRT 11-0026
Merknad

QC 20180820

Tilgjengelig fra: 2018-07-03 Laget: 2018-07-03 Sist oppdatert: 2018-11-15bibliografisk kontrollert
3. Processing of a rare earth phosphate concentrate obtained inthe nitrophosphate process of fertilizer production
Åpne denne publikasjonen i ny fane eller vindu >>Processing of a rare earth phosphate concentrate obtained inthe nitrophosphate process of fertilizer production
(engelsk)Manuskript (preprint) (Annet vitenskapelig)
HSV kategori
Identifikatorer
urn:nbn:se:kth:diva-239069 (URN)
Merknad

QC 20181114

Tilgjengelig fra: 2018-11-16 Laget: 2018-11-16 Sist oppdatert: 2018-11-16bibliografisk kontrollert
4. Separation of rare earth elements using hollow fiber supported liquid membrane extraction in pilot scale
Åpne denne publikasjonen i ny fane eller vindu >>Separation of rare earth elements using hollow fiber supported liquid membrane extraction in pilot scale
(engelsk)Manuskript (preprint) (Annet vitenskapelig)
HSV kategori
Identifikatorer
urn:nbn:se:kth:diva-239070 (URN)
Merknad

QC 20181118

Tilgjengelig fra: 2018-11-16 Laget: 2018-11-16 Sist oppdatert: 2018-11-16bibliografisk kontrollert

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