Hydrometallurgy 180 (2018) 132–138

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Hydrometallurgy
journal homepage: www.elsevier.com/locate/hydromet

Recovery of rare earths from nitric acid leach solutions of phosphate ores T
using solvent extraction with a new amide extractant (TODGA)
⁎ ⁎
Dongdong Xu, Zeb Shah, Yu Cui , Limin Jin, Xiujing Peng, Hao Zhang, Guoxin Sun
Institute for Smart Materials & Engineering, School of Chemistry and Chemical Engineering, University of Jinan, No. 336, West of Nan Xinzhuang, Jinan, 250022,
Shangdong, PR China.

A R T I C LE I N FO A B S T R A C T

Keywords: The rare earths in phosphate ores are not effectively utilized and they cannot be directly extracted from leach
TODGA liquor with the traditional extractants, such as organic phosphoric acid. This paper presents a new solvent
Rare earths extraction method for rare earths from nitric acid leaching of phosphate rock using N,N,N′,N′-tetraoctyl diglycol
Phosphate ores amide (TODGA) without interfering with the normal route for fertilizer production. When the concentration of
Solvent extraction
extractant increased to 0.1 mol/L, the extraction rate of lanthanum, cerium, praseodymium, and neodymium
have been found to be 98.1%, 99.1%, 98.8% and 98.6%, respectively. The recovery rate reached to 99.9% when
a three-stage countercurrent extraction was carried out on the simulated leach solution. There was almost no
extraction of other impurity ions and the rare earths could be separated with TODGA from Ca2+, PO43−, Fe3+,
and Mg2+. The presence of phosphoric acid in solution enhanced the extraction of rare earth ions. The stripping
of the loaded rare earth in the organic phase was readily carried out with water under room temperature with
high efficiency. The mixed rare earth oxides (REO) with an assay of > 95% could be recovered as a final product.

1. Introduction
The rare earth elements (REEs) are the fifteen lanthanides in the
periodic table along with scandium and yttrium. They have become a
significant topic of interest in the metals industry due to a global supply
shortage and increasing demand (Humphries, 2010; Jordens et al.,
2013). This situation has motivated many companies to develop pro-
cessing techniques for extracting REEs from rare earths- bearing de-
posits. Phosphate ores are considered as a potential source of rare
earths (Li et al., 2006), in which REEs are substituted in the phosphate
ore lattice for calcium ions or are present as mineral inclusions in the
ore. Phosphate ores usually contains an average of 0.1–0.8% of rare
earth oxides. Therefore, processing of phosphate ores for REEs while
producing phosphate fertilizers and phosphoric acid (Mao et al., 2017)
has recently become a special target (Al-Thyabat and Zhang, 2015; Kim
et al., 2014; Moldoveanu and Papangelakis, 2013; Panda et al., 2014).
Nitric, sulfuric, and hydrochloric acids have been used as leaching
agents for the extraction of REEs from phosphate ores (Antar and Jemal,
2008; Bandara and Senanayake, 2015; Borai et al., 2016; Brahim et al.,
2008; Jorjani et al., 2011; Wang et al., 2010; Zafar et al., 2006).
Compared with sulfuric acid, the rate of REE recovery is much higher
using nitric acid as a leaching agent (Binnemans A et al., 2013;
Fernandes et al., 2013; Rollat, 2016).
Many research efforts have been dedicated to developing more ef-
ficient methods of recovering REEs (Alemrajabi et al., 2017; Aly and
Mohammed, 1999; Banda et al., 2012; Beltrami, 2014; Hirai and
Komasawa, 1991). Solvent extraction has proved to be an efficient
technique for the recovery and enrichment of metal ions. The main
advantages of this technique are the continuous operation, low cost,
effective separation and easy automatic control (Maes et al., 2017; Su
et al., 2016).
A number of extractants have been used for the recovery and se-
paration of REEs from leach liquors. Several neutral extractants have
shown good extraction properties of rare earths. Tributyl phosphate
(TBP) was used to extract rare earths from an aqueous solution pro-
duced by nitric acid leaching of phosphate ore concentrate, and about
95%, 90%, 87% and 80% of neodymium, cerium, lanthanum, and yt-
trium, respectively, could be extracted in optimum conditions (Jorjani
and Shahbazi, 2016). Furthermore, the extraction efficiency of REEs
from nitrate solution by TBP decreases with increasing hydrogen ion
concentration in the aqueous medium (Ferdowsi and Yoozbashizadeh,
2017). A new technique with CH3P(O)(OC8H17)2 (P350) was proposed
to recover rare earths from nitric acid leaching of phosphate ore
without interfering with the normal route for fertilizer production and
there was a better extraction efficiency at 0.4 mol/L HNO3 (Li et al.,
2006). These extractants can extract REEs only at lower acidity in a

⁎
Corresponding authors.
E-mail addresses: chm_cuiy@ujn.edu.cn (Y. Cui), chm_sungx@ujn.edu.cn (G. Sun).

https://doi.org/10.1016/j.hydromet.2018.07.005
Received 9 April 2018; Received in revised form 15 June 2018; Accepted 12 July 2018
0304-386X/ © 2018 Published by Elsevier B.V.
D. Xu et al.
narrow range and they cannot be used to directly extract REEs from
leach liquors.
Certain organic acid extractants have also shown good extraction
properties of rare earths. The recovery of Dy with 97% purity and Tb
with 83% purity from rare earth chloride solution of monazite mineral
using PC 88A has been reported (Mishra et al., 2000). Guo used P204
and P507 to remove rare earth elements, which showed better results at
acidity of 0.30 mol/L with 95% of REEs extraction efficiency (Guo
et al., 2014). Kumar found that the extraction of metals using Tulsion
CH-96 decreases exponentially with the increase in acidity for a given
amount of resin used (Kumar et al., 2010). TOPS 99, an equivalent to
di-(2-ethylhexyl) phosphoric acid has also been employed for the sol-
vent extraction and separation of REEs from phosphoric acid solutions
with 80% extraction efficiency (Radhika et al., 2011). Conventional
acid extractant could not be used over a wide range of acidities, and the
acidity of the leachate needs to be adjusted with NH3 or NaOH before
extraction. Hence, this process increases cost and produces large
amount of waste water. Our previous work has shown that TODGA have
excellent extraction performance towards REEs under a wide acidity
range. The extraction of rare earth metals with TODGA have been
studied recently (Gergoric et al., 2017; Murakami et al., 2016). How-
ever, no one has yet explored the use of TODGA to separate and recover
rare earths from phosphate rock leachate.
We have extended our work to the extraction of REEs from the
phosphate ore leaching liquor with TODGA as the extractant. The new
process is proposed to recover rare earths from phosphate ore without
interfering with the production of phosphoric acid, because almost no
phosphoric acid is extracted. TODGA has been synthesized and applied
in REEs separation in our laboratory owing to the high extractability,
good stability and interfacial property of the TODGA-REE complex.
TODGA has shown lower water-solubility compared to other ex-
tractants (Sasaki et al., 2007; Shimojo et al., 2008; Wang et al., 2017).
Another advantage of TODGA is the rapid extraction of rare earth ions
from nitrate media at high acidity. This eliminates the need for alkali
solutions to adjust the acidity and thus greatly reduces aqueous waste.
The results showed that rare earths could be rapidly separated with
TODGA from nitric acid leaching liquor of phosphate ore. In this work,
the deionized water was selected to strip REE3+ from the loaded or-
ganic phase with a high efficiency. The REEs is precipitated from the
strip solution as rare earth oxalates, then upon calcinations the oxalates
were transformed into rare earth oxides (Li et al., 2006; Maes et al.,
2017). A good separation of the phosphorus in the phosphate form and
the REEs can broaden the nitric acid phosphate fertilizer product chain.
2. Experimental
2.1. Materials and reagents
The extractant TODGA with high purity (> 96%) was prepared in
our lab according to the established procedure (Sun et al., 2010). The
water used in all experiments was deionized water. All other chemicals
were analytical-reagent grade and used directly without further pur-
ification.
Different REE oxides with purities > 99.5% were dissolved in dilute
nitric acid and mixed to prepare the simulated REEs feed solution. Prior
to the extraction experiments, the hydrogen ion concentration of the
liquor was adjusted using analytical grade nitric acid and phosphoric
acid. According to the composition of phosphate rock acid leach solu-
tion (Li et al., 2006), the simulated acid leach solution was prepared
containing Ca (12,800 mg/L), Fe (1325 mg/L), Mg (325 mg/L), P
(5150 mg/L), S (1128 mg/L), and REEs (72.4 mg/L).
2.2. Separation process
The organic phase composed of TODGA and 1-octane, and aqueous
phases were mixed in oscillating tubes and shaken for 30 min. The
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Hydrometallurgy 180 (2018) 132–138
mixtures were then transferred to a centrifuge for two-phase separation,
then the aqueous phase was used for the analysis. The effects of rare
earth ion concentration, pH of the aqueous phase, contact time, tem-
perature, and concentration of extractant in the organic phase were
investigated. All the elements in the aqueous phase, were analyzed by
inductively-coupled plasma atomic emission spectrometry (ICP–AES)
and UV/Vis spectrophotometry.
The back extraction of the rare earth metal ions was carried out with
deionized water.
The stripping solution was subjected to precipitation of rare earths
with H2C2O4 solution, the precipitates were filtered, dried and ignited
at 700–800 °C to obtain the rare earth oxides (Zafar et al., 2006).
The concentration of rare earth metal ions in the organic phase after
the extraction experiments was calculated using a mass balance equa-
tion. The distribution ratio (D) and extraction rate (E%) were calculated
from the equation given below:
C0 − Ci
D=
Ci (1)
C0 − Ci
E% =
C0 (2)
where C0 is the concentration before solvent extraction and Ci is the
concentration of the aqueous phase after solvent extraction equili-
brium.
3. Results and discussion
3.1. Extraction of rare earth elements with TODGA
3.1.1. Effect of acid concentration on extraction of REEs with TODGA
The effects of acidity of HNO3 (in the range of 1.0 to 5.0 mol/L),
H3PO4, and mixed HNO3-H3PO4 on the extraction ability of TODGA
from a mixture of REEs (10−3 mol/L of each metal) was first evaluated.
Experiments were performed with extractant concentration of
0.02 mol/L, a contact time of 30 min, a phase ratio of 1:1, phosphoric
acid concentration of 1.0 mol/L, and a temperature of 25 °C.
The experimental results obtained were used to compare the acidity
effects of the pure nitric acid system, pure phosphoric acid system, and
mixed nitric acid/phosphoric acid extraction system. TODGA showed
almost no extraction of rare earth elements in the presence of pure
phosphoric acid. The extraction efficiency in the mixed acid system was
better than that of the pure nitric acid system (Fig. 1). Due to the basic
nature of the C=O group, TODGA extracted the lipophilic nitric acid
into the organic phase while the phosphoric acid was not extracted.
These data suggested that phosphoric acid enhanced the extraction of
TODGA in the presence of nitric acid.
(a) lanthanum (b) cerium (c) praseodymium (d) neodymium.
When keeping the concentration of H3PO4 at 1.0 mol/L, the ex-
traction performance with increasing concentration of HNO3 is shown
in Fig. 2. The distribution ratio increased with the increasing of the
nitric acid concentration within the range of acidity for all the REEs
studied. This may be due to the common-ion effect of nitrate anion with
the increase of HNO3 concentration. The extraction performance of
TODGA on extraction of REEs was in the order: Nd3 + > Pr3 + > Ce3
+
> La3 +. The extraction and distribution ratio increased gradually
with the increase of the atomic number of lanthanides. Similar results
were reported by Mowafy, et al. for the extraction of lanthanides
(Mowafy and Mohamed, 2014; Mowafy and Mohamed, 2017).
3.1.2. Effect of contact time
Fast extraction kinetics is beneficial for industrial process. To study
the effect of extraction time, the extraction of REEs was performed by
shaking the two phases for different duration ranging from 5 to 60 min.
The other parameters are: TODGA: 0.02 mol/L, HNO3: 3.0 mol/L,
H3PO4: 1.0 mol/L and phase ratio of 1:1 at a temperature of 25 °C. Fig. 3
D. Xu et al.
Fig. 1. The extraction effect of rare earth elements in different system.
Fig. 2. Effect of the concentration of nitric acid on the extraction of rare earth
ions.
shows that the extraction almost reaching equilibrium within five
minutes. The extraction of REEs from mixed acid solutions with TODGA
is fast for practical applications.
TODGA concentration: 0.02 mol/L, temperature: 25 °C, phase ratio:
1:1.
3.1.3. Effect of temperature
The effect of temperatures was studied on the TODGA extraction
efficiency at 15, 25, 35, 45, and 55 °C while keeping all other
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Hydrometallurgy 180 (2018) 132–138
Fig. 3. Extraction effect of REEs as a function of contacting time.
experimental conditions constant. TODGA concentration of 0.02 mol/L,
HNO3 concentration of 3.0 mol/L, H3PO4 concentration of 1.0 mol/L,
phase ratio of 1:1 and contact time of 30 min were used in these ex-
periments. It can be seen from Fig. 4 that the extraction distribution
ratios of La, Ce, Pr and Nd all decreased as the temperature increased,
indicating that the reaction is exothermic and the low temperature is
favorable for the extraction. Thus, 25 °C was selected as the optimal
temperature.
TODGA 0.02 mol/L, phase ratio 1:1, and contact time 30 min.
In order to understand the extraction mechanism, it is helpful to
D. Xu et al. Hydrometallurgy 180 (2018) 132–138

Fig. 4. Effect of temperature on extraction of REEs by TODGA.

obtain the thermodynamic parameters of the extraction because en-

tropy and enthalpy changes could significantly affect the extent of the
metal ion extraction equilibrium. The values of enthalpy change
(ΔrHmθ), entropy change (ΔrSmθ), and Gibbs free energy (ΔrGmθ), were
calculated according to the thermodynamic formula:

⎡ ∂ log K ex ⎤ −∆r Hθm

⎢ ⎥ =
⎢ ∂
⎣ ()
1
T
⎥
⎦P
2.303R
(3)

and

log D = log K ex + nlog[TODGA (O) ] − log YRE (4)

By keeping [TODGA] and YRE constant, the following equation was

derived:

⎡ ∂ log K ex ⎤ ⎡ ∂ log D ⎤
⎢ ⎥ =⎢ ⎥ +0
⎢ ∂
⎣ ()
1
T
⎥
⎦P ⎣ ()
⎢ ∂ 1 ⎥
T ⎦P (5) Fig. 5. A) Effect of phase ratio on extraction of REEs by TODGA. TODGA:
0.02 mol/L, contact time: 30 min, and temperature: 25 °C. B) Extraction rates of
From (3) and (5), Eq. (6) was arrived to obtain the enthalpy change: REEs with 0.04 mol/L and 0.10 mol/L TODGA, phase ratio 1:1, temperature:
25 °C.
⎡ ∂ log D ⎤ −∆r Hθm
⎢ ⎥ = 3.1.4. Effect of phase ratio
⎢ ∂
⎣ ()1
T
⎥
⎦P
2.303R
(6) The volume ratio of the two phases plays an important role in the
extraction process. The ratio of organic to aqueous phase (Vo/Va) was
The gibbs free energy change and entropy change were calculated changed from 1:2 to 2:1, TODGA concentration of 0.02 mol/L. It can be
by the following equations: seen from Fig. 5A that the extraction of REEs increased gradually as the
phase ratio increased. Lanthanum extraction is the weakest of the light
∆r Gθm = −RTlnKθ = ∆r Hθm − T∆r Sθm (7)
rare earths studied. The extraction efficiency of La is lower at low or-
The thermodynamic function values of extracting La, Ce, Pr, Nd ganic phase ratio, and increased dramatically with the organic to
were calculated with Eqs. (6) and (7) and the results are given in aqueous phase up to 1:1, after that point the increase slowed. There-
Table 1. The enthalpy change of several ions is negative, indicating that fore, the phase ratio of 1:1 is suitable for the extraction efficiency of
this type of extraction reaction is exothermic. The variations in the La3+, Ce3+, Pr3+, and Nd3+. The extraction of 0.04 mol/L and
changes of the thermodynamic properties of the extraction process may 0.10 mol/L TODGA with the phase ratio of 1:1 is shown in Fig. 5B,
be due to the differences in the radii of the different ions and the co- which shows that all four rare earth ions have high extraction rates.
ordination of TODGA with the metal ions.
3.1.5. Effect of TODGA concentration
Table 1 The rare earths were extracted by varying the concentration of
TODGA extraction of lanthanide thermodynamic function values. TODGA from 0.02 to 0.1 mol/L dissolved in 1-octane. The extraction
RE3+ ΔrHmθ(kJ·mol−1) ΔrGmθ(kJ·mol−1) ΔrSmθ (J·mol−1﹒K−1) experiments were conducted using 5 mL of the pregnant liquor and
5 mL of the organic phase at a temperature of 25 °C, a contact time of
La3+ −49.97 −22.30 −92.80 30 min, and concentrations of phosphoric acid and nitric acid in the
Ce3 + −54.19 −23.40 −96.60
aqueous solution were 1.0 and 3.0 mol/L, respectively. Fig. 6 shows the
Pr3+ −67.21 −24.78 −140.1
Nd3 + −68.16 −25.50 −143.2 effect of TODGA concentration on the extraction of REEs. When the
TODGA concentration increased from 0.01 to 0.20 mol/L, the amount

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D. Xu et al. Hydrometallurgy 180 (2018) 132–138

Fig. 6. Extraction behavior of REEs as a function of TODGA concentration. Fig. 8. The IR spectra of TODGA and coordination compounds with rare earths.

Fig. 9. Extraction of REE species on TODGA.

Fig. 7. Effect of rare earth ion concentration.

Table 2
Stripping rate of rare earth with pure water.
RE3+ Stripping rate (%)

3+
La 85.6
Ce3 +
90.1
Pr3+ 95.6
Nd3 +
99.9

Table 3
Extraction results of the simulated acid leach solution.
Elements Concentration (g/L) Concentration (g/L) Extraction (%)
(before extraction) (after extraction)

Ca 12.8 12.3 3.58

Fe 1.33 1.30 1.51
Mg 0.33 0.32 0.22
Fig. 10. Three-dimensional structure model.
P 5.15 5.15 0
S 1.13 1.13 0
REEs 0.07 3.90 94.6 3.1.6. Effect of rare earth ion concentration
In this experiment, the effect of the cerium concentration on ex-
traction efficiency of TODGA with the increase in HNO3 concentration
of rare earth extraction increased significantly. At concentration of
was studied. The Ce3+ concentration in the solution was varied from
0.04 mol/L, the extraction efficiency for all ions investigated is over
0.001 mol/L to 0.010 mol/L, and the nitric acid concentration in the
95%, thus it was selected as the suitable concentration for further ex-
feed solution varied from 1 mol/L to 5 mol/L, phosphoric acid 1 mol/L.
periments.
As shown in Fig. 7, the Ce extraction increased with rising concentra-
Contact time 30 min, temperature 25 °C, phase ratio 1:1.
tions of nitric acid and decreased slightly with the increase of Ce3+ ion

136
D. Xu et al.
Fig. 11. The suggested flow chart for recovery of rare earths from phosphate rock with TODGA.
concentration up to 0.01 mol/L in the feed solution. This data con-
firmed that TODGA had high extractability for rare earths from HNO3/
H3PO4 mixed solution.
3.2. Stripping experiment
Usually, the rare earth ions were stripped by mixing the solutions
with aqueous mineral acids (typically, hydrochloric acid or nitric acid),
which lead to the production of additional wastewater. In this research,
deionized water was first tested to strip REE3+ from a loaded organic
phase. The extraction experiments were conducted using 5 mL deio-
nized water and 5 mL of the loaded organic phase at 25 °C, and a
contact time of 20 min. The result is summarized in the Table 2. All the
tested lanthanides, La, Ce, Pr and Nd, had high stripping rates with
deionized water. The stripping rate of Nd was nearly 100%. Therefore,
water was chosen as a good stripping agent in this work. Stripping with
water does not introduce other inorganic salts and acids, which makes
it an ideal choice for the environmental considerations.
3.3. Detection of the extraction of phosphorus and other metal ions
The organic phase, after extraction, was stripped with water and the
phosphorus molybdenum blue method was used to detect if phosphorus
was present. The test was done by taking 2–3 mL of the stripped aqu-
eous liquid in a small beaker, adding 3–5 drops of 6 mol/L nitric acid,
after shaking 1 mL of ammonium molybdate was added. A clear col-
orless solution indicated that there was no phosphoric acid in the or-
ganic phase. These results indicated that the TODGA extraction can
achieve complete separation between the rare earth elements and
phosphoric acid.
The extraction of the coexisting ions, such as Ca2+, PO43−, Fe3+,
and Mg2+, was tested with the simulated phosphate ore acid leach
solution. The concentration of the above ions was analyzed by ICP. As
shown in Table 3, there is < 4% extraction of impurity ions while REEs
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Hydrometallurgy 180 (2018) 132–138
are near 95% extracted. These data show that the rare earths could be
separated effectively from the other substances in the leachate using
TODGA.
3.4. Precipitation and recovery of rare earths
To obtain the oxides of the lanthanides, 5% H2C2O4 solution was
added into the stripping solution which resulted in the oxalate pre-
cipitation of REEs. The REES oxalates were then ignited at 700–800 °C
in an air atmosphere to convert to oxides. The purity of the rare earth
oxides (REO) was > 95% with the recovery rate > 94%.
3.5. Extraction mechanism
3.5.1. IR spectra of ligand and the complexes
According to the IR spectra of the ligand and the complexes (Fig. 8),
the wave number of the stretching frequency of C]O band was shifted
to lower values, from1653 to 1610 cm−1. On the other hand, the ether
stretching vibration, at around 1080 cm−1 did not show any shift. The
results suggested that the carbonyl group of TODGA is more strongly
coordinated with REE than the oxygen atom of the ether group. The
broad band near 1650–1610 cm−1 may be the superposition of the
coordination C]O peak and the free extractant C]O peak, which was
dominated by the coordination peak.
3.5.2. Structural model
A structural model was proposed for the TODGA-rare earth metal
complex as shown below. In this proposed mechanism, each TODGA
ligand with its O]CeCeOeCeC]O backbone acts as tridentate O
donor, where the two carbonyl O atoms and the one ether O atom bind
to the REE metal ion. The central metal ion forms a 9-coordinat
structure. The result is the formation of six 5-membered chelate rings
that improved the stability to the molecular architecture. Strong elec-
trostatic force in the low-dielectric constant organic solvent requires the
D. Xu et al.
presence of anions in the outer-coordination sphere, which are often the
more lipophilic nitrates that is coextracted with the lanthanide ion. It
has been reported that REE in a 3:1 complex of TODGA is nine-co-
ordinated (Antonio et al., 2015; Reilly et al., 2012). Figs. 9 and 10 show
the suggested structure.
3.6. The suggested flow chart for recovery of rare earth elements from
phosphate rock
Based on the studies above, Fig. 11 shows the suggested flow chart
for recovery of rare earth elements from phosphate rock using the
solvent extraction with TODGA. The rare earth elements-bearing
phosphate rock was added into a stirring tank together with nitric acid
for reaction, and the solid-liquid separation was performed to obtain
the leachate containing the rare earth elements. The rare earth elements
were extracted and separated by the extraction experiment, and then
stripped. The rare earth and the fertilizer were recovered. Mixed rare
earth oxides (REO) of which purity was > 95% could be obtained
without interfering with the normal route for fertilizer production. The
good separation of phosphorus and rare earth in the phosphate ore
could broaden the nitrate phosphate fertilizer product chain.
4. Conclusions
In this work, we investigated a novel method to separate rare earths
from phosphorus ore nitric acid leach liquid with a recently developed
extractant TODGA. The influences of phase ratio, acidity, extractant
concentration and contact time on extraction efficiency were in-
vestigated. TODGA showed high extractability for rare earths from si-
mulated leach solutions. The extraction efficiency increased with the
concentration of HNO3 and the presence of phosphoric acid enhanced
the extraction of rare earths. About 94.2%, 98.6%, 98.6%, and 98.4% of
La, Ce, Pr, and Nd, were extracted under the conditions, TODGA:
0.04 mol/L, phosphoric acid: 1 mol/L, nitric acid: 3 mol/L, phase ratio:
1:1 and at 25 °C. When the concentration of extractant increased up to
0.1 mol/L, the extraction rate of all elements was > 98%. Ca2+, PO43−,
Fe3+, and Mg2+ are rarely extracted, which showed very good se-
lectivity from the other substances in the solution.
The distribution ratios of rare earths from nitric acid or mixed acid
system of nitric acid and phosphoric acid increase with increasing
atomic number, so heavy rare earth can also use this extractant to ex-
tract and separate from phosphoric ore leaching solution.
The deionized water was selected to strip RE3+ from loading or-
ganic phase and high efficiency was obtained with a phase ratio (Vo/Va)
of 1:1 and a contact time of 10 min. Precipitation with 5% oxalic acid
and calcination at 750 °C could produce the REOs with > 95% purity.
Acknowledgements
This study was supported by Natural Science Foundation of
Shandong Province of China (ZR201702160381).
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