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2554
2554

NEODYMIUM SEPARATION FROM MIXED RARE EARTH USING

PRECIPITATION METHOD COMBINED WITH EXTRACTION VIA HOLLOW FIBER
SUPPORTED LIQUID MEMBRANE
By
Rakthai Chusee
A Thesis Submitted in Partial Fulfillment of the Requirements for the Degree

MASTER OF ENGINEERING
Department of Chemical Engineering
Graduate School
SILPAKORN UNIVERSITY
2011
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52404215 :
: /////
:
. : ..
. 150 .

93.2 92.5
70.0
- 1 5
Cyanex 272
0.1 0.5

0.1 1.5

100
-
3 87.9
0.3 92.1
0.3
86.2 80.1

........................................
2554
........................................
52404215 : MAJOR : (CHEMICAL ENGINEERING)

KEY WORD : EXTRACTION/NEODYMIUM/PRASEODYMIUM/MIXED RARE EARTH/
PRECIPITION METHOD/LIQUID MEMBRANE/HOLLOW FIBER
RAKTHAI CHUSEE : NEODYMIUM SEPARATION FROM MIXED RARE EARTH
USING PRECIPITION METHOD COMBINED WITH EXTRACTION VIA HOLLOW FIBER
SUPPORTED LIQUID MEMBRANE. THESIS ADVISOR :
ASST.PROF.WEERAWAT
PATTHAVEEKOVGKA, D.Eng., 150 pp.
This research study, neodymium separation from mixed rare earth using precipitation
method combined with extraction via hollow fiber supported liquid membrane. Feed solution
is prepared from precipitation mixed rare earth with ammonium hydroxide at (pH 4.6 and 7.8),
respective. The results showed that the unwanted elements could be reduced and there was
the pure cerium up to 93.2 percent and pure lanthanum up to 92.5, respective. The solution,
Neodymium in has a amount of 70.0 percent, was used as a solvent in the extraction by
hollow fiber supported liquid membrane. By studying, the influence of pH in the range of 1 to
5.The liquid membrane was fabricated from a solution of Cyanex 272 dissolved in kerosene
solvent before embedded in the microstructure of porous hollow fibers. The concentrations
used were in the range of 0.1 to 0.5 moles per liter. In the experiment, Nitric acid solution,
used as reagent strip, Influence of concentration in the range of 1 to 5. Then, the feed
solution to flow inside the hollow fiber and stripping solution to flow outside, both do the
same flow through the flow rate of 100 ml per minute.
The results showed that the pH of the feed solution for extraction is equal to 3 percent
of the maximum was 87.9. The influence of the concentration of the extract was concentrated
to 0.3 moles per liter, can be extracted from the equivalent figure is 92.1 percent. And the
concentration of the strip. The concentration of 0.3 mole per liter to strip most of 86.2 percent
and 80.1 percent purity.
Department of Chemical Engineering

Student's signature ........................................
Thesis Advisor's signature ........................................
Graduate School, Silpakorn University

Academic Year 2011

. .
. . .
.

ICP

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1
1
12
20
20
20
21
22
22
23
23
24
25
28
29
35
37
38
41
41
46

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pH ...........................................
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4 ...................................................................
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pH ...........................................
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5 ......................................................................................................
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46
49
50
54
55
56
58
59
59
64
64
67
72
76
78
79
82
84
89
90
92
115
139
142
150
1-1
2-1
2-2
3-1
3-2
3-3
-1
-2
-1
-2
-3
-4
-5
-1
-2
-3
..............................................................................
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......................................
................................................................................
...................................................
..........................................................
(Tube Side) ................................................
(Shell Side) ........................................

Mixed rare earth ....................
.........................................................................
pH
...................................................................................
pH
...................................................................................
......

.....................................................
-
.................................

.................................
10
24
34
44
53
58
90
90
93
94
103
106
114
116
118
121

-4
-5
-6
-7
-8
-9
-10
-11
-12

.................................
-
....................

...................................................

...................................................
-
.................................

...................................................

...................................................
-
....................
....................
124
127
128
129
130
131
132
133
134

-13
-14
-15
-16
....................
-
....

....................
....................
135
136
137
138
1-1
1-2
1-3
1-4
1-5
1-6
2-1
2-2
2-3
2-4
2-5
2-6
2-7
3-1
3-2
3-3
3-4
3-5
3-6
3-7
3-8
3-9
mischmetal........................................................................ 3
.. 2553-2573................................................................ 4
.................................................................. 5
(Catalytic converter) ................................................ 6

...................... 8
......................................................... 9
........ 28
........................... 30
PTFE ........................... 35
............................................................. 36
........................................ 37
.............................................. 39
...................................................................... 40
............................................................. 42
............................................................................. 43
Inductively Coupled Plasma
Optical Emission Spectroscopy (ICP-OES) ............................................. 45
.............................................................. 47
................................................................... 48
............................................................. 50
Hollow fiber liquid membrane.................................................................. 51
....................................... 51
................................................................................. 52

4-1
4-2
4-3
4-4
4-5
4-6
4-7
4-8
4-9
4-10
4-11
4-12
-1
............................................................. 59
Mixed rare earth
............................................................................... 61
Mixed rare earth
................................................................................. 63
Mixed rare earth
.............................................................................. 65
................................................................. 65
Mixed rare earth ................................................ 68
......................................................... 69
..................................... 70
............................... 71
-
.......................................... 76
Cyanex 272
.......................................... 78
.......................................... 79
............................................................ 91
1.1

[1] Gilmer "

" (.) 2555
2554

mischmetal
(Ce) ( 30-50 )
(mischmetal
: (Ce) 45-50 (La) 22-25 (Nd) 18 (Pr) 5 Sm 1 ) mischmetal
[1]
1-1 mischmetal
mischmetal 3 Zr 1
450-600
mischmetal
mischmetal Fe ( Fe
30 ) (pyrophoric)
mischmetal
cross-section
,
( Y) hydrogen-moderator carrier

4
Y
Cr 5 U 95 1000
( 149Sm cross-section )
( Tm) (
Eu)
1-2 .. 25532573 [27]

CeO2 CeO2 40
Nd2O2 Pr2O3 La2O3
(optical glass) CeO2

CeO2 Nd2O3 Fe2+ Pr2O3
3 ZrO2 CeO2
(nitrides)
(carbides)
(oxides) (sulfides) (borides)

()
1-3
(hydrogenation-
dehydrogenation)

(petroleum cracking) (heterogeneous
catalysts) ( )
(defect
structure)

1-4 (Catalytic
converter) [6]
(garnets) 3La2O35Fe2O3 ( Ln =
)
(ferrimagentic
substance) (eddy current)

Ln = Y
( yig) (selenides)
(titanates) (stannates)
(tellurides)
(low temperature coefficient of capacitance)

(ceramic capacitors)
NdFeB Nd 31-34 Fe 3
B 1.3 900-1,000

NdFeB 5-10 [4]
Coercivity 750-2000 kA/m (energy Product)
200-400 kJ/cu.m (curie Temperature)
310-400
1-5 [5]

(concentrates) 200
0.01 ( ) 10
10
3 95 3
(bastnaestie) (monazite) (xenotime)
1-6 [3]

[2]

"" "rare earth elements" "rare earths"

"lanthanide series" lanthanides lanthanons
lanthanoids
15 57-71
(La) (Ce) (Pr) (Nd) (Pm) (Sm)
(Eu) (Gd) (Tb) (Dy) (Ho) (Er)
(Tm) (Yb) (Lu) "group III
A" Group 2 (Sc) (Y)
21 39

(ion-exchange separation)
10
(nuclear fission) .. 1947
J.A.Marinsky, L.E.Glendenin C.D.Coryell 15
2
57-63 ( 90 )
64-71 (
21 39 ) 1-1
1-1
()
()
La Ce Pr Nd Pm Sm Eu
( Th )
Y Tb Dy Ho Gd Er Tm Yb Lu
( Sc )
(electron configuration)
5d1 6s2 (
4d1 5s2)

(paramagnetic substance)
4f 7
7

f
11
(light filter)

(didymium glass)

(monazite ore break-down process)
Mixed rare earth

15
(fractionation)

(fractional crystallization)

( Sedimentation )

(flocculant)

Flocculation
12
(Ion Exchange)

(Extraction)

2
2

70 (La) (Ce)
(Pr) (Nd)

1.2
Nwe Nwe Soe (2008) [7] Monazite
13.44%

96
H. Singh (2006) [8]
(Yttrium) carboxylic acids
cekanoic, neo-heptanoic, naphthenic Versatic 10 acids
(Kex) separation factors () monomeric
neutral complex ([M(HA2)3]) La<Ce<Pr<Nd<Sm<Gd<Dy<Ho
13
neo-heptanoic Versatic 10 acids
(heavy rare earths) cekanoic naphthenic
(lighter rare earths) logKex
La Ce cekanoic acid- naphthenic acid> neo-heptanoic acid> Versatic 10 acid
Pr, Nd, Sm, Gd, Dy Ho cekanoic acidd naphthenic acid> neoheptanoic acid
H. Singh (2006) [9] 1.5 M
(equilibration time), oxalic acid, ,
D2EHPA+ 0.2 M TBP uranium ammonium carbonate

organic phase phase
oxalic acid first order kinetic activation energy 77

kJ/mole 4 1.5 M D2EHPA+0.2 M TBP+14.8 g/L U3O8 +1.12
g/L Fe (III)+b1.0 g/L phase (A/O) 3 55 C
uranium < 0.2% ammonium carbonate 12%
yielded 99% uranium
Naglaa E. El-Hefny (2007) [10]

Nd(III) CYANEX 921 kerosene thiocyanate
sulphuric Lewis cell
Lewis cell
thiocyanate/kerosene
interfacial properties CYANEX 921 first order
CYANEX 921
Sulphuric acid
neodymium CYANEX 921 kerosene

W. Patthaveekongka [11]

14
Thioridazine.HCl
Shell
100 ml/min
30 Thioridazine 0.0005 M
0.05 M - 2
29.10% 0.3 M

> >
>

3

65%
Muhammad Idiris Saleh [12]

La nitrate-acetato Cyanex 272 toluene
single drop (kF) 10-7 m/s
- Ea, 'Sr, 'Hr 'G300r 71 kJ/mol, -155J/molK, 69
kJ/mol 115 kJ/mol
FLa = 10-7[La3+][H2A2](0)[H+]-1(i) kmol/m2s
[La(HA2)]2+ La3+ HA-2
La
SN2
Muhammad Idiris Saleh [13] La
nitrate-acetato Cyanex 272 toluene TOPO
, La3+, H+, NO-3 Ac- Cyanex
272 TOPO
La3+ 7.34 mM La3+ 9.79 mM
La3+ pH log
[La(Ac)2A3HA]
15
[La(Ac)A2B] TOPO pH 1
TOPO TOPO
acetate
TOPO TOPO acetate
TOPO [La(Ac)2A3HA] [La(Ac)A2B]
TOPO ' H
60 kJ/mol Kex 0.21 TOPO
3
lanthanum
Cyanex 272 15.97 g La(III)/100 g Cyanex 272 phosphorus

J.Kraikaew [14] isomolar tributylphosphate (TBP)
di-(2-ethylhexyl) (D2EHPA) 35 1
TBP 50 (Kd)
Synergistic coefficients [S = (Kd,a)TBP, D2EHPA / {(Kd,a)TBP+(Kd,a)D2EHPA}] Ce
(S> 1) 1.0 TBP D2EHPA
La (S <1) 1.5
TBP D2EHPA Y
Nwe Nwe Soe (2008) [15] monazite

27.35
monazite Myitsone Area monazite 3
monazite
oxalic cerium oxalate
Masakuni Ozawa [16] thermal rare earth
(RE = La, Ce, Pr) hydroxides oxides hexamethylene-
16
tetramine thermal gravimetry
infrared spectrometry X-ray diffraction
La(OH)3 CeO2 Pr(OH)3 Ce cubic fluorite cerium dioxide
lanthanum trihydroxide oxides
340 500 C
La(OH)3 LaOOH+H2O
2LaOOHLa O +H O
2 3
('H) 390 kJ/mol Pr(OH)3 carbonate

carbonate HMT La Pr
CO2
Mari E. de Vasconcellos [17] rare earths
ammonium carbonate ammonium carbonate ammonium
hydroxide carbonate rare earths ammonium carbonate
ammonium carbonate ammonium hydroxide
hydrogen peroxide rare earth carbonates
rare earth peroxicarbonates rare earths
carbonateperoxide
aging
rare earths Sm, Gd, Dy, Y, Yb Tm ammonium
carbonate Ho, Eu Tb ammonium carbonate La, Ce,
Pr Nd ammonium carbonate Ce, Pr, Nd, Sm, Eu Dy
ammonium carbonate ammonium hydroxide La
Tb peroxicarbonates La, Ce, Pr,
17
Nd, Sm, Eu, Gd, Dy Ho quantitatively precipitated Er
peroxicarbonate quantitative aging 24 Y

J.E. Dutrizac [18] rare earths sodium, potassium

lead jarosites sulphate chloride
end-member rare earth analogues sodium jarosite potassium jarosite
< 0.3 wt.% rare earths e jarosite structure

earths
sodium jarosite potassium jarosite rare

rare earths sodium jarosite potassium jarosite
pH ferric ion yields
structural rare earths jarosite Sodium jarosite
potassium jarosite predominantly chloride rare earth
jarosites sulphate Lead jarosite
rare earth < 0.2 wt.% rare earths SEM rare earths
morphology sodium, potassium lead jarosites trivalent rare
earth (RE) trivalent iron jarosite structure
co-ordination hydrolyzability trivalent
rare earth ions ferric ion
Qiong Jia [28]
sec-nonylphenoxy acetic acid (CA100) bis(2,4,4-trimethylpentyl) dithiophosphinic acid (Cyanex301) bis(2,4,4-trimethylpentyl) monothiophosphinic acid (Cyanex302)
n-heptane lanthanum (III) CA100
Cyanex301 slop analysis
lanthanum (III) log -1.41
H, G S
18
CA100 Cyanex301 Cyanex302

Elias Bou-Maroun [29] Ln(III)
(Ln: La, Eu, Lu) NaNO3 0.1 bis(4-acyl-5-hydroxy
pyrazoles)
1,12-bis(1-phenyl-3-methyl-5-hydroxy-4-pyrazolyl)-dodecane-1,12-
dione (HL-10-LH) 1,6-bis(1-phenyl- 3-methyl-5-hydroxy-4-pyrazolyl)-hexane-1,6-dione

(HL-4-LH) chloroform
HL-10-LH
lanthanides biscoordinated
tetracoordinated lanthanum europium biscoordinated lutetium
Lu(L-10-LH)3 europium HL-4-LH Eu(L4-L)(L-4-LH) corresponding extraction HL-10-LH
polynuclear high extraction yields HL-10-LH
Ln (La < Eu < Lu) HL-10-LH
HPMBP (1-phenyl-3-methyl-4-benzoyl-5-hydroxy-pyrazole)
HL-10-LH
selectivity HL-10-LH
V.V. Belova [30] rare earthmetals (REM)
chloride nitrate binary trioctylmethylammonium
dialkylphosphinic, dialkylmonothiophosphinic, dialkyldithiopho-sphinic acids
toluene aqueous organic phases Isotherms
rare earth trioctylmethyl ammonium bis(2,4,4-trimethylpentyl)
phosphinate binary organic
aqueous (NaCl, NaNO3) Cex:CLn(org)
REM chlorides 3 REM nitrates 1 organic
19
binary
lanthanum chloride
lanthanum nitrate : dialkylphosphinate> dialkylmonothiophosphinate

>>dialkyldithiophosphinate quaternary ammonium(QAB)
chlorides nitrates lanthanides

binary
chloride nitrate
Dongbei Wu [31] Pr (III) Nd
, -, ,
(III) 8- hydroxyquinoline chloride-acetate
acetate , chloride,
8-hydroxyquinoline (HQ) 2-ethylhexyl phosphoric acid mono-2ethyl hexyl ester (P507)
Pr(III), Nd (III) La (III) 8-hydroquiloline HQ
P507 Pr (III), Nd (III) La (III)
HQ P507 Pr(III), Nd (III) La (III)
20
1.3
1.
70
2.
1.4
70
1.
2.
1.5
1.
2.
(Chemical Treatment Process)

-

(Distribution ratio)

21
22
(Chemical Precipitation) [32]

()

[16]
1. (Hydroxide Precipitation)

pH

(OH-)

Ln3+
AOH
(2.1)
23
2. (Sulfite Precipitation)
Na2S NaHS

pH

Ln
(2.2)
3+
3. (Carbonate Precipitation)
Na2CO3

pH

Ln3+
(2.3)
24
4. (Sodium Borohydride Precipitation)

pH

(2.4)

(2.5)
Ln
3+
2-1 [32]
1.
1.
pH
2.
3.
1.
2. Chelating agent
3.
1. Cd Pb
pH
2.
1.
2.
Chelating agent
1. H2S
2.
3.
1.
2.
1. pH 8-11
25

2.1

1.
2.
4.
3. pH

( )
Ln3+
Ln3+

(Chemical Extraction and Leaching)
26

2

7
Di(2-ethylhexyl) phosphate (D2EHP), TBP, bis(2,4,4-trimethylpentyl)phosphinic acid
(Cyanex 272), trioctylphosphine oxide (Cyanex 923), LIX 860-I, LIX 84-I Aliquat336
TBP
TBP

2.6 2.7 [21, 24]

(2.6)

(2.7)
D2EHP, Cyanex 272 Cyanex 923

COOH, =P(O)OH, -SO3H

[12-14,19,23-24]

(2.8)
27

pH

LIX 860-I LIX 84-I (Chelation)
(complex
(Donor groups)
molecules)
(Bidentate complexes) [33-34]

(2.9)
2.9
Aliquat336

(Quaternary ammonium halides) (Ammonium salt) (Primary, RNH2) (Secondary, R2NH) (Tertiary,
R3N) (Quaternary ammonium salts, R4N+)
(Anionic species)
[22,23]

(2.10)
28

(2.11)
R3NHA

[LnY]-n 2.10
2

1. (Solvent Extraction) [25]

2
2-1
2-1 [25]
29
2-1
(Feed solution)
(Solute) ( )
(Solvent)

(Extract)
(Stripping solution)

(feed to strip ratio)
(distribution ratio)
2. (Liquid Membrane)

30

2-2 [26]
2-2
3

1 2

5
1. Mn+

31
( 1) (Concentration Gradient)
1
2. 1
(MRn)
(nH+)
1 2.12

(2.12)
aq (Aqueous Phase) org

(Organic Phase)
2.13

(2.13)
2.14

RH
k
k2ex
(2.14)
32
3. (MR)
1
(Concentration Gradient) 2
4.
2
2 2.15

(2.15)
2.16

(2.16)

2.17

(2.17)
k
1ex
k2ex
5. 2
2
(Concentration Gradient)

2

33

2 1
5 -
(pH Gradient) (Concentration
Gradient)
3
Liquid Membrane (SLM))

(Supported
(Emulsion Liquid Membrane (ELM) Liquid Surfactant Membrane)
(Electrostatic Pseudo Liquid Membrane (ESPLIM)) 2-2

(Supported Liquid Membrane
(SLM))
2-6

34
2-2 [25]
1.
2.
3.
1.
2.
3.
4.
1.
1.
2.
3.
4.
1.
2.
3.
4.
2.
3.
1.
2.
3.
4.
5.
Immobilized
Liquid Membrane

2 (Hydrophilic
35
microporous)
(Hydrophobic Microporous)
(Flat Sheet) (Spiral-Wound
Module) (Hollow Fiber)

2.1 (Flat Sheet)
(Porosity)
(PP), (PF),
(PTFE)
2-3 PTFE [6]

2-3

(Electro Affinity),
(Capillary Force) (Hydrophilic or Hydrophobic Microporous)
36

2-4
[25]
2-4

3 ,

37

2.2 (Spiral-Wound Module)
2-5
[25]
(a) 1. , 2.
, 3. , 4. , 5.
, 6. , 7. , 8.

38
(b)
Fi , Si , Mi
, Fo , So
Mo
2-5

2.3 (Hollow Fiber)
(Tubular Tube)
39

2-6 [25]
2-6

(Prefiltration)
40
[25]
2-7
2-7

,

(Rare Earth)
7
Di(2-ethylhexyl) phosphate (D2EHP), TBP, bis(2,4,4-trimethylpentyl)phosphinic acid
(Cyanex 272), trioctylphosphine oxide (Cyanex 923), LIX 860-I, LIX 84-I Aliquat336
1 4
41
42
1.

1:1 ( :) 50 50

1 : 20 (:) 3-1
(a)
(c)
(b)
(d)
3-1 (a) Mixed rare earth (b)

(c) (d)
43
2.
Di(2-ethylhexyl) phosphate (D2EHP), TBP, bis(2,4,4-trimethyl
pentyl)phosphinic acid (Cyanex 272), trioctylphosphine oxide (Cyanex 923), LIX 860-I, LIX 84-I
Aliquat336 3-1
0.03 M
3.
(solvent extraction)

1/1 20
20 30

3-2
(a)
(b)
3-2 (a) (b)
44
3-1
Tri-n-butyl phosphate
TBP
Di(2-ethylhexyl) phosphate
D2EHPA
Bis(2,4,4-trimethylpentyl)phosphinic acid
Cyanex 272
Trioctylphosphine oxide
Cyanex 923
2-hydroxy-5-nonylactophenome oxime
LIX 84
5-dodecylsalicylaldoxime
LIX860
N-Methyl-N,N-dioctyloctan-1-aminium chloride
Aliquat 336
45
4. Inductively Coupled Plasma - Optical
Emission Spectroscopy (ICP-OES)
ICP-AES ICP
(multi-element) 10,000

ppb refractory element
3-3
3-3 Inductively Coupled Plasma - Optical Emission Spectroscopy (ICP-OES)
46
4.1
ICP-OES
1 5
4.2
(% Extraction)

(3.1)
Cf,in =
Cf,out =

(RE(OH)3 (s)) pH

2
1.
3

47
1.1

100
24
50
150 3-4
(a)
(b)
3-4 (a)
(b)
1.2
65 pH
0.3
3-5
48
(a)
( b)
(c)
3-5 (a) pH (b)

(c)
1.3
(% Purity)

(3.2)

Ci = i
Cfeed,i = i
Ctotal =
(3.3)
49
2.
3

2.1
65 %
1 : 1 ( : ) 50 50
(:)
1 : 20
2.2
25 % pH

3-6
(a)
(b)
(b)
3-6 (a) pH (b)

(c)
50
2.3
(% Purity)
1.3
3 pH

Liqui-Cel Liquid/Liquid Extraction System
Cat. #5PCM-106 Hoechst Celanese Corporation
3-7
51
3-7 Hollow fiber liquid membrane
3-8 (One through operation)
52
1.
6.
2.
7.
3.
8.
4.
9.
5.
3-9
Celgard X-30 240 Microporous Polypropylene Hollow
Fiber 3-2
53
3-2
(Polypropylene)
240 (m)
300 (m)
0.05 (m)
30%
4.2 Kg/cm (60 psi)
1.4 m2 (15.2 ft2)
29.3 cm2/cm3 (74.4 m2/m3)
1 C 60 C
(DXL)
2.5 8 (inch)
4
Hollow fiber liquid membrane
(One through operation) 100 ml/min
3-9 2

54

Cyanex 272

1. pH
1.1
1 3
2.3 5
pH 1, 3 5
1.2
Cyanex 272
1 0.1
1.3
0.5
5
1.4

100
3-9
5, 10, 15, 20, 25, 30, 35 40
ICP-OES
55
1.5 Inductively Coupled Plasma - Optical
(% Extraction) (% Stripping )

(3.5)

(3.4)
Cf,in =
Cf,out =
CS,out =
2.
2.1
2.3 5
pH 3.1
2.2

1 0.1, 0.3 0.5
56
2.3
0.5
5
2.4

100
5, 10, 15, 20,25, 30, 35 40
3-9
ICP-OES

3.4 3.5
3.
3.1
2.3 5
pH 3.1
3.2
Cyanex 272
1 3.2
57
3.3
0.5, 1.0
1.5 5
3.4

100
3-9
5, 10, 15, 20,25,30, 35 40
ICP-OES

3.4 3.5
58
3.2
3-3
TBP
D2EHPA
Cyanex 272
Cyanex 923
LIX 84-I
LIX 860-I
Aliquat336
Inductively Coupled Plasma - Optical

pH meter

250, 500, 1000 mL
4

Mixed rare earth
3
,
Mixed Rare Earth

ICP
4-1 (
: -1)
4-1 Mixed rare earth
59
60
4 Ce, La, Nd Pr 4

20,104 mg/l Ce 8,999 mg/l
44.8 La 4,323 mg/l 21.5
Nd 3,799 mg/l 18.9 Pr
1,405 mg/l 7.0
Ce
10,583 mg/l 47.6 La
22,602 mg/l
4,534 mg/l 19.2 Nd 3,816 mg/l

16.9 Pr 1,689 mg/l 7.6
(solvent extraction)
Mixed rare Earth
O/A 1/1 Di(2-ethylhexyl) phosphate

(D2EHP), TBP, bis(2,4,4-trimethylpentyl)phosphinic acid (Cyanex 272), Trioctyl-phosphine
oxide (Cyanex 923), LIX 860-I, LIX 84-I Aliquat336
0.03 M
ICP
Mixed rare Earth

Ce, La, Nd Pr 4 4-2 4-3 (
: -2)
61
Mixed rare earth
100
TBP
D2EHPA
75
LIX84
50
LIX860
25
0
La
Pr
Nd
Cy 272
Cy 923
Ce
Aliq 336
(a)
Mixed rare earth

5,000
TBP
mg/l
4,000
D2EHPA
3,000
LIX84
2,000
LIX860
1,000
Cyanex 272
Cyanex 923
La
Pr
Nd
Ce
Aliq 336
(b)
4-2 Mixed rare earth (a)
(b) mg/l
62
4-2 Di(2-ethylhexyl)
phosphate (D2EHPA), TBP, bis(2,4,4-trimethylpentyl)phosphinic acid (Cyanex 272), Trioctylphosphine oxide (Cyanex 923), LIX 860-I, LIX 84-I Aliquat336 Mixed
rare earth
Ce Aliquat336
La Cyanex 272 Nd Cyanex
272 Pr Cyanex 272
Mixed rare earth
100
TBP
75
D2EHPA
LIX 84
50
LIX 860
25
Cy 272
Cy 923
La
Pr
Nd
(a)
Ce
Aliq336
63
Mixed rare earth

6,000
TBP
5,000
D2EHPA
mg/l
4,000
LIX 84
3,000
2,000
LIX 860
1,000
Cyanex 272
La
Pr
Nd
Cyanex 923
Ce
Aliq336
(b)
(a) (b) mg/l
4-3 Di(2-ethylhexyl)
phosphate (D2EHPA), TBP, bis(2,4,4-trimethylpentyl)phosphinic acid (Cyanex 272), Trioctylphosphine oxide (Cyanex 923), LIX 860-I, LIX 84-I Aliquat336 Mixed
rare earth
Ce LIX 84
La LIX 84 Nd LIX 84
Pr LIX 84
64

Mixed Rare Earth

2.1
(RE(OH)3 (s)) Mixed Rare Earth 65 %

4.1
3
4.1 4

4.2
pH 2

pH
4-4 (
: -3)
65
Mixed Rare Earth

50,000
40,000
30,000
mg/l
La
Pr
20,000
Nd
10,000
0
2.0
2.5
3.0
3.5
4.0
Ce
4.5
5.0
6.0
(a)
Mixed Rare Earth
100
75
La
50
Pr
Nd
Ce
25
2.0
2.5
3.0
3.5
4.0
4.5
5.0
6.0
(b)
mg/l (b)
66
4-3
pH
La pH 5 50 Nd
pH 2.78 32.5 Pr pH
1.91 6.5
pH 4-3
La, Pr, Nd, Ce pH Ce
70
pH 6.3 3.00 Ce
(bond dissociation energy)
0.120
0.100
mol
0.080
0.060
0.040
RE
0.020
RE
0.000
0.0 2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5
ml
4-5
4-5
4.1 4.2
67
2.2

pH

4-6 (
: -4)
60,000
Rare Earth
Mixed
mg/l
50,000
40,000
La
30,000
Pr
Nd
20,000
Ce
10,000
0
5.8
6.0
6.2
6.4
6.6
6.8
(a)
7.0
7.2
7.4
7.6
7.8
68
Mixed Rare Earth
100
75
La
50
Pr
Nd
25
5.8
6.0
6.2
6.4
6.6
6.8
7.0
7.2
Ce
7.4
7.6
7.8
(b)
(b)
pH
pH
4-6
La pH 7 7.82
94.6 pH 7.8
Mixed Rare Earth
Ce La Nd
4-7
69
Mixed Rare Earth
HNO3 Digestion
Ce Pr cake
La Nd solution
of La
Precipitation
La solution
Nd cake
HNO3 Digestion
Extraction
4-7
Mixed Rare Earth
4-7
pH 4.6 2 Ce
cake La Nd 4-7
70
Mixed rare earth

250,000
mg/l
200,000
150,000
100,000
50,000
0
Feed
Ce cake
La, Nd
Ce
La
Nd
Pr
195,100
45,112
27,340
10,865
195,100
2,716
2,188
8,112
42,396
25,152
2,753
4-8 Mixed Rare Earth

4-8
pH 4.6 Mixed rare earth 2
Ce cake La Nd solution Ce cake
93.2
3.9 La Nd solution
55.6 33.0
La
Na Mixed Rare Earth pH 7.8
4-8
71
Mixed rare earth

35,000
30,000
mg/l
25,000
20,000
15,000
10,000
5,000
0
La
Nd cake
La
Nd
Pr
30,592
1,385
1,104
6,535
18,216
1,287
4-9 Mixed Rare Earth

4-9
pH 7.8 La Nd solution Mixed rare earth
2 La solution Nd cake La solution
92.5 Nd cake
70.0
90

72

- Cyanex 272

(coupled transport) (counter transport) (permeant) (Nd3+) (H+)

(4.3)
(
1 2-3)
(concentration gradient)
1 1
2
(NdR3) (H+)
73

(4.4)
(4.5)

2
2 2
2

1 2
- (pH Gradient)
(concentration Gradient)

(non-equilibrium)

Cyanex 272

74
Cyanex
272 4.3
4.6

(4.6)
4.6
ratio)
(distribution
(FluxExtract : Jf)
4.7

(4.7)
4.7

Cyanex 272 Cyanex

272 4.6

(4.8)
75

(4.9)
4.9)
(continuous process)
4.8

(4.10)
4.10

( )

4.10 Cyanex 272

100
Cyanex 272
2 Mixed rare earth
76
1. pH
-
-
4-10 (
: -6 , : -1 )
100
75
50
25
0
pH 1
pH 3
pH 5
4-10 -
4-10
-
- 3.0

4.3

77

(4.11)
4.12

(4.12)
4.12 4-10 -
4.12

[H+]F,aq

([Nd3+]F,aq)
([H+]F,aq)
4.12

(4.13)

(Kex,f)
- (pH 3)

-

78
2.
Cyanex 272

4-11 (
: -7 , :
-2)
100
75
50
25
0
0.1 M
0.3 M
0.5 M
4-11 Cyanex 272
4-11
Cyanex 272
Cyanex 272
Cyanex 272 0.3
Cyanex 272 [(HR)2]org
4.11 4.12
79
Cyanex 272

3.
: -8 , : -3 )
4-12 (
100
75
50
% Extrac
% Stip
25
0
0.5 M
1.0 M
1.5 M
4-12
80
4-12

4.3
4.14

4.15

(4.14)
(4.15)
4.15 4-12
[H+]S,aq 4.15

([Nd3+]S,aq)
([H+]S,aq)

4.16

(4.15)

( )
81

(continuous process)

( 4.3 )
1.

8 Di(2-ethylhexyl) phosphate (D2EHP), TBP, bis(2,4,4-trimethylpentyl)phosphinic acid (Cyanex 272), trioctylphosphine oxide (Cyanex 923), LIX 860-I, LIX 84-I
Aliquat336
2.
pH
pH 6.3 3.00
pH
pH
pH 7.8
3.
4-9
pH 4.6
93.2 pH 7.8
92.5
70.0
82
83
4.

Cyanex 272
100
pH
pH
pH 3 pH 3
pH
pH
Cyanex 272
0.3

0.5 1.0

0.1
84
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ammonium carbonate plus ammonium hydroxide: Precipitation of their peroxicarbonates,
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[18]
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[19]
Basudev Swain and Emmanuel O. Out, 2011. Competitive extraction of lanthanides by

solvent extraction using Cyanex 272: Analysis, classiflcation and mechanism. Separation
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[20]
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for the separation of rare earth ionsby combination of conversion of
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ZHU Liyang , DUAN Wuhua , XU Jingming and ZHU Yongjun, 2009. Kinetics of
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[22]
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.
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Minerals Engineering, Vol. 10, No. 12, 1421-1427
89
90
-1
(Tube Side)
()
(ml)
(ml/min)
1
2
3
1
50
119.8 120.5 119.9 120.07
24.99
2
100 119.2 120.8 118.9 119.63
50.15
3
100
60.3 58.2 59.1 59.20
101.35
4
100
38.9 39.5 39.9 39.43
152.16
5
100
32.2 28.9 29.9 30.33
197.80
6
100
25.3 23.9 25.2 24.80
241.94
-2
(Shell Side)
()
(ml)
(ml/min)
1
2
3
1
50
121.8 119.5 120.9 120.73
24.85
2
100 120.5 119.8 120.7 120.33
49.86
3
100
61.2 60.5 60.1 60.60
99.01
4
100
40.1 39.8 40.9 40.27
149.01
5
100
31.9 29.6 30.9 30.80
194.81
6
100
25.9 24.1 25.5 25.17
238.41
91
300
ml/l
250
200
150
Tube
100
Shell
50
0
-1
92
93
-1 Mixed rare earth
(ppm)
(La)
4,323
21.5
4,534
19.2
(Pr)
1,405
7.0
1,689
7.6
(Nd)
3,799
18.9
3,816
16.9
(Sm)
601
3.0
752
3.3
(Gd)
338
1.7
437
1.9
(Y)
490
2.4
631
2.8
(Ce)
8,999
44.8
10,583
47.6
0.0
0.0
(Dy)
136
0.7
157
0.7
(Yb)
0.0
0.0
(Th)
0.0
0.0
(U)
0.0
0.0
(Eu)
(ppm)
94
-2
Mixed rare earth
1. TBP
2. D2EHPA
TBP
Cin
Cout
(ppm)
(ppm)
La
4,323 2,382
Pr
1,405
Nd
3,799 2,090
794
D2EHPA
%
%
Extracti
(ppm)
Pure
on
1,942
44.9 21.7
Extraction
Cin
Cout
(ppm)
(ppm)
La
4,323 2,812
%
%
Extracti
(ppm)
Pure
on
1,511
35.0 17.5
Extraction
611
43.5
6.8
Pr
1,405
855
550
39.1
6.4
1,709
45.0
19.1
Nd
3,799 2,061
1,738
45.8
20.2
269
44.8
3.0
Sm
601
158
443
73.6
5.1
Sm
601
332
Gd
338
185
153
45.2
1.7
Gd
338
11
327
96.9
3.8
490
267
223
45.5
2.5
490
489
99.8
5.7
8,999 5,053
3,946
43.9
44.2
Ce
8,999 5,547
3,452
38.4
40.0
Ce
Eu
93.8
0.1
Eu
82.8
0.1
Dy
136
70
66
48.6
0.7
Dy
136
36
100
73.5
1.2
Yb
98.9
0.1
Yb
99.1
0.1
Th
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
95
3. LIX 84-I
4. LIX 860-I
LIX 84-I
Cin
Cout
(ppm)
(ppm)
LIX 860-I
%
%
Extracti
(ppm)
Pure
on
1,340
31.0 22.7
Extraction
La
4,323 2,984
Pr
1,405 1,027
378
26.9
Nd
3,799 2,598
1,201
Cout
(ppm)
(ppm)
%
%
Extracti
(ppm)
Pure
on
1,603
37.1 22.3
Extraction
La
4,323 2,720
6.4
Pr
1,405
930
475
33.8
6.6
31.6
20.4
Nd
3,799 2,371
1,428
37.6
19.9
164
27.3
2.8
Sm
601
393
208
34.6
2.9
92
27.3
1.6
Gd
338
220
118
34.8
1.6
490
320
171
34.8
2.4
8,999 5,870
3,129
34.8
43.5
Sm
601
437
Gd
338
246
490
358
132
26.9
2.2
8,999 6,466
2,533
28.1
43.0
Ce
Ce
Cin
Eu
90.4
0.1
Eu
86.6
0.1
Dy
136
95
40
29.7
0.7
Dy
136
85
51
37.5
0.7
Yb
87.1
0.1
Yb
83.9
0.1
Th
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
96
6. Cyanex 923
5. Cyanex 272
Cyanex 272
Cin
Cout
(ppm)
(ppm)
Cyanex 923
%
%
Extracti
(ppm)
Pure
on
1,987
46.0 21.7
Extraction
La
4,323 2,337
Pr
1,405
780
625
44.5
Nd
3,799 2,037
1,762
Cout
(ppm)
(ppm)
%
%
Extracti
(ppm)
Pure
on
749
17.3 13.4
Extraction
La
4,323 3,575
6.8
Pr
1,405 1,018
387
27.6
7.0
46.4
19.3
Nd
3,799 2,231
1,568
41.3
28.2
278
46.2
3.0
Sm
601
311
290
48.3
5.2
157
46.5
1.7
Gd
338
200
138
40.7
2.5
490
385
105
21.4
1.9
8,999 6,737
2,262
25.1
40.6
Sm
601
323
Gd
338
181
490
240
250
51.0
2.7
8,999 4,996
4,003
44.5
43.8
Ce
Ce
Cin
Eu
93.4
0.1
Eu
91.8
0.1
Dy
136
66
70
51.6
0.8
Dy
136
80
56
41.0
1.0
Yb
74.3
0.0
Yb
95.1
0.1
Th
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
97
7. Aliquat336
Aliquat336
Cin
Cout
(ppm)
(ppm)
%
%
Extracti
(ppm)
Pure
on
999
23.1 14.3
Extraction
La
4,323 3,324
Pr
1,405 1,215
190
13.5
2.7
Nd
3,799 2,819
980
25.8
14.0
200
33.3
2.9
90
26.6
1.3
Sm
601
401
Gd
338
248
490
390
100
20.4
1.4
8,999 4,634
4,365
48.5
62.4
Ce
Eu
53.6
0.1
Dy
136
66
70
51.5
1.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
98
Mixed rare earth
1. TBP
2. D2EHPA
TBP
Cin
Cout
(ppm)
(ppm)
La
4,534 2,638
Pr
1,689 1,014
Nd
3,816 2,322
D2EHPA
%
%
Extracti
(ppm)
Pure
on
1,896
41.8 20.7
Extraction
Cin
Cout
(ppm)
(ppm)
%
%
Extracti
(ppm)
Pure
on
97
2.1 3.4
Extraction
La
4,534 4,438
7.4
Pr
1,689 1,566
123
7.3
4.3
39.2 16.3
Nd
3,816 3,349
467
12.2
16.3
314
41.8
3.4
Sm
752
366
386
51.3
13.4
675
40.0
1,494
Sm
752
437
Gd
437
248
189
43.3
2.1
Gd
437
35
401
91.9
14.0
631
357
274
43.5
3.0
631
631
100.0
22.0
10,583 6,368
4,216
39.8 46.1
Ce
10,583 9,981
603
5.7
21.0
Ce
Eu
100.0
0.0
Eu
100.0
0.2
Dy
157
78
79
50.5
0.9
Dy
157
157
100.0
5.5
Yb
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
99
4. LIX 860-I
3. LIX 84-I
LIX 84-I
Cin
Cout
(ppm)
(ppm)
LIX 860-I
%
%
Extracti
(ppm)
Pure
on
1,749
38.6 16.8
Extraction
La
4,534 2,943
Pr
1,689 1,131
790
46.8
Nd
3,816 2,583
1,703
Cout
(ppm)
(ppm)
%
%
Extracti
(ppm)
Pure
on
1,591
35.1 21.0
Extraction
La
4,534 2,943
7.6
Pr
1,689 1,131
558
33.1
7.4
44.6
16.4
Nd
3,816 2,583
1,233
32.3
16.2
752
489
262
34.9
3.5
Gd
437
278
158
36.2
2.1
3.0
631
402
229
36.3
3.0
48.2
49.0
Ce
10,583 7,096
3,487
33.0
45.9
Sm
752
489
391
52.0
3.8
Sm
Gd
437
278
241
55.2
2.3
631
402
315
49.9
10,583 7,096
5,101
Ce
Cin
Eu
86.5
0.0
Eu
100.0
0.1
Dy
157
91
107
68.0
1.0
Dy
157
91
66
42.2
0.9
Yb
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
100
6. Cyanex 923
5. Cyanex 272
Cyanex 272
Cin
Cout
(ppm)
(ppm)
Cyanex 923
%
%
Extracti
(ppm)
Pure
on
1,568
34.6 20.4
Extraction
La
4,534 2,967
Pr
1,689 1,133
556
32.9
Nd
3,816 2,430
1,386
Cout
(ppm)
(ppm)
%
%
Extracti
(ppm)
Pure
on
1,543
34.0 20.9
Extraction
La
4,534 2,992
7.2
Pr
1,689 1,146
544
32.2
7.4
36.3
18.0
Nd
3,816 2,609
1,207
31.6
16.3
752
496
255
34.0
3.5
Gd
437
282
154
35.3
2.1
3.1
631
408
223
35.3
3.0
32.7
44.9
Ce
10,583 7,185
3,398
32.1
46.0
Sm
752
490
262
34.8
3.4
Sm
Gd
437
279
158
36.1
2.0
631
391
240
38.0
10,583 7,127
3,456
Ce
Cin
Eu
100.0
0.1
Eu
100.0
0.1
Dy
157
89
68
43.1
0.9
Dy
157
92
65
41.3
0.9
Yb
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
101
7. Aliquat336
Aliquat336
Cin
Cout
(ppm)
(ppm)
%
%
Extracti
(ppm)
Pure
on
999
22.0 14.3
Extraction
La
4,534 3,535
Pr
1,689 1,499
190
11.2
2.7
Nd
3,816 2,836
980
25.7
14.0
Sm
752
552
200
26.6
2.9
Gd
437
347
90
20.6
1.3
631
531
100
15.9
1.4
10,583 6,218
4,365
41.2
62.4
Ce
Eu
96.6
0.1
Dy
157
87
70
44.7
1.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
103
-3 pH
1.
pH
2.0
2.5
3.0
3.5
4.0
4.5
5.0
La
43,530
43,093
41,534
36,315
26,588
10,005
2,089
144
Pr
6,801
6,548
1,053
176
15
Nd
34,024
33,228
31,806
26,246
16,740
5,261
793
112
Sm
6,284
6,050
5,762
4,652
2,834
893
104
20
Gd
3,864
3,718
3,589
3,036
1,992
713
94
4,840
4,646
4,514
4,052
3,018
1,388
309
Ce
292
Eu
119
113
103
84
64
42
Dy
1,424
1,332
1,251
1,031
660
219
13
Yb
Th
174
181
192
214
236
261
282
330
3,226
3,260
3,230
2,715
1,759
744
344
317
3,326
6,266
5,217
6.0
104
pH
2.0
2.5
3.0
3.5
4.0
4.5
5.0
6.0
La
41.6
42.2
42.3
43.5
46.5
48.6
49.7
15.4
Pr
6.5
6.4
6.4
6.2
5.8
5.1
4.2
1.6
Nd
32.5
32.5
32.4
31.4
29.3
25.6
18.9
11.9
Sm
6.0
4.3
2.5
2.1
Gd
3.7
5.0
5.9
5.6
5.9
3.6
3.7
3.6
3.5
3.5
2.2
0.0
4.6
4.5
4.6
4.8
5.3
6.7
7.4
0.0
Ce
0.3
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Eu
0.1
0.1
0.1
0.1
0.1
0.2
0.0
0.0
Dy
1.4
1.3
1.3
1.2
1.2
1.1
0.3
0.0
Yb
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Th
0.2
0.2
0.2
0.3
0.4
1.3
6.7
35.2
3.1
3.2
3.3
3.2
3.1
3.6
8.2
33.8
105
2.
pH 1.9
ppm
La
7,050
5.4
Pr
10,970
8.5
Gd
889
0.7
1,680
1.3
Ce
100,400
77.5
Eu
0.0
Dy
598
0.5
Yb
0.0
Th
96
0.1
0.0
6,121
4.7
Sm
1,806
1.4
Nd
106
-4 pH
1.
pH
5.8
La
Pr
5.9
6.0
6.1
6.2
6.3
6.4
6.5
6.6
6.7
6.8
24,500 24,660 21,740 23,620 21,640 23,770 21,220 21,720 20,650 15,850 14,700
8,546
8,631
7,597
8,230
7,572
8,194
7,327
7,340
6,751
4,971
4,401
Nd 19,380 19,590 17,180 18,560 17,110 18,390 16,360 16,140 14,630 10,020 8,484
Sm
3,749
3,769
3,318
3,551
3,247
3,439
3,014
2,851
2,417
1,397
1,012
Gd
2,099
2,101
1,845
1,983
1,803
1,902
1,666
1,550
1,267
648
412
3,155
3,164
2,774
2,996
2,728
2,910
2,559
2,416
1,992
1,047
665
Ce
54,230 54,580 48,060 52,070 48,000 51,950 46,670 46,870 43,040 32,360 28,850
Eu
Dy
769
767
657
710
631
650
544
457
309
77
Yb
Th
107
pH
6.9
La
7.0
10,680 12,530
7.1
7.2
7.3
7.4
7.5
7.6
7.7
7.8
9,468
8,360
8,167
6,889
5,298
4,956
4,488
3,905
1,324
961
860
440
244
151
79
60
Pr
3,195
3,391
Nd
6,199
5,832
1,382
873
1,040
309
232
114
104
128
Sm
767
507
80
53
145
33
38
20
22
26
Gd
310
135
24
460
205
20,730 22,580
9,351
6,820
5,859
3,106
1,508
807
191
11
Ce
Eu
Dy
Yb
Th
108
pH
5.8
5.9
6.0
6.1
6.2
6.3
6.4
6.5
6.6
6.7
6.8
La
21.0
21.0
21.1
21.1
21.1
21.4
21.4
21.9
22.7
23.9
25.1
Pr
7.3
7.4
7.4
7.4
7.4
7.4
7.4
7.4
7.4
7.5
7.5
Nd
16.6
16.7
16.7
16.6
16.7
16.5
16.5
16.2
16.1
15.1
14.5
Sm
3.2
3.2
2.9
2.7
2.1
1.7
Gd
1.8
1.8
2.7
Ce
3.0
3.2
3.2
3.1
3.2
1.8
1.8
1.8
1.7
1.7
1.6
1.4
1.0
0.7
2.7
2.7
2.7
2.7
2.6
2.6
2.4
2.2
1.6
1.1
46.6
46.5
46.6
46.6
46.7
46.7
47.0
47.2
47.3
48.8
49.3
Eu
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Dy
0.7
0.7
0.6
0.6
0.6
0.6
0.5
0.5
0.3
0.1
0.0
Yb
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
109
pH
6.9
7.0
7.1
7.2
7.3
7.4
7.5
7.6
7.7
7.8
La
25.2
27.7
43.8
49.0
50.7
63.9
72.4
81.9
91.9
94.6
Pr
7.5
7.5
6.1
5.6
5.3
4.1
3.3
2.5
1.6
1.5
Nd
14.6
12.9
6.4
5.1
6.5
2.9
3.2
1.9
2.1
3.1
Sm
1.8
1.1
0.3
0.4
0.6
Gd
0.7
0.3
0.0
0.0
0.2
0.0
0.0
0.0
0.0
0.0
1.1
0.5
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Ce
49.0
50.0
43.3
40.0
36.4
28.8
20.6
13.3
3.9
0.3
Eu
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Dy
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Yb
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.5
0.4
0.3
0.9
0.3
110
2.
pH
5.8
5.9
6.0
La
185
208
Pr
102
114
Nd
319
361
Sm
103
116
Gd
57
6.1
216
6.2
222
6.3
236
6.4
259
6.5
276
6.6
6.7
6.8
345
395
576
649
117
120
128
144
154
192
223
336
399
375
390
419
479
519
652
763
1,130
1,347
119
123
132
154
167
213
250
364
425
63
63
63
66
77
84
111
133
205
241
60
62
62
62
62
71
74
107
137
237
289
Ce
557
604
604
604
628
689
722
918
1,065
1,686
2,019
Eu
Dy
32
33
33
33
33
37
38
52
61
89
97
Yb
Th
111
pH
6.9
7.0
7.1
7.2
7.3
7.4
7.5
7.6
7.7
7.8
La
705
879
1,434
1,517
1,718
1,800
1,944
2,015
2,088
2,109
Pr
432
549
932
971
1,052
1,077
1,111
1,122
1,130
1,132
Nd
1,452
1,801
2,702
2,766
2,869
2,899
2,928
2,938
2,945
2,952
Sm
448
517
607
612
617
619
621
622
623
624
Gd
253
289
323
323
323
323
323
323
323
323
304
360
419
419
419
419
419
419
419
419
Ce
2,188
2,846
5,163
5,401
5,953
6,116
6,358
6,424
6,470
6,470
Eu
Dy
97
100
101
101
101
101
101
101
101
101
Yb
Th
112
pH
5.8
5.9
6.0
6.1
6.2
6.3
6.4
6.5
6.6
6.7
6.8
La
13.1
13.3
13.6
13.7
13.9
13.6
13.6
13.3
13.0
12.5
11.9
Pr
7.2
7.3
7.4
7.4
7.5
7.5
7.6
7.4
7.4
7.3
7.3
Nd
22.5
23.2
23.6
24.1
24.6
25.1
25.5
25.2
25.2
24.4
24.6
Sm
7.3
7.4
8.2
8.3
7.9
7.8
Gd
4.0
4.0
4.2
Ce
8.2
7.6
7.7
8.0
7.5
3.9
3.9
3.9
4.1
4.1
4.3
4.4
4.4
4.4
4.0
3.9
3.8
3.6
3.7
3.7
4.1
4.5
5.1
5.3
39.3
38.7
38.0
37.4
36.9
36.1
35.5
35.4
35.2
36.5
36.9
Eu
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Dy
2.3
2.1
2.0
2.0
1.9
1.9
1.9
2.0
2.0
1.9
1.8
Yb
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
113
pH
6.9
7.0
7.1
7.2
7.3
7.4
7.5
7.6
7.7
7.8
La
12.0
12.3
12.5
13.2
13.5
14.1
14.4
14.8
14.9
12.0
Pr
7.5
8.0
8.0
8.1
8.1
8.0
8.0
8.0
8.0
7.5
Nd
24.5
23.1
22.8
22.0
21.7
21.2
21.0
20.9
20.9
24.5
Sm
7.0
5.2
4.4
4.4
7.0
Gd
3.9
2.8
2.7
2.5
2.4
2.3
2.3
2.3
2.3
3.9
4.9
3.6
3.5
3.2
3.1
3.0
3.0
3.0
3.0
4.9
Ce
38.8
44.2
44.6
45.6
45.8
46.1
46.0
45.9
45.8
38.8
Eu
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Dy
1.4
0.9
0.8
0.8
0.8
0.7
0.7
0.7
0.7
1.4
Yb
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
4.5
5.1
4.7
4.6
4.5
114
-5
pH 4.6
pH 7.6
ppm
ppm
La
42,396
55.6
Pr
2,753
3.6
Nd
25,152
33.0
2,188
1.0
Ce
0.0
195,100
93.2
2,716
%
1.3
ppm
ppm
30,592
92.5
6,535
25.1
3.3
1,287
4.9
1,385
4.2
18,216
69.9
0.0
0.0
1,104
8,112
3.9
116
- 1
(
)
Time Feed in Feedout Stripin Stripout
% Extraction %Stripping
(min) (ppm) (ppm) (ppm) (ppm)
5
6,834 2,037
0
923
70.19
19.25
10
6,834
2,037
1,204
70.20
25.10
15
6,834
2,006
1,432
70.65
29.65
20
6,834
2,036
1,663
70.21
34.65
25
6,834
2,028
2,023
70.32
42.10
30
6,834
2,036
2,313
70.21
48.20
35
6,834
2,033
2,405
70.25
50.10
40
6,834
2,036
2,457
70.21
51.20
45
6,834
2,034
2,453
70.23
51.10
50
6,834
2,035
2,473
70.22
51.54
55
6,834
2,034
2,480
70.24
51.67
60
6,834
2,033
2,490
70.25
51.86
: [HNO3]S= 0.005 M, VF=VS= 10 L, [Cyanex 272]=0.1 M, QF=QS= 100 ml/min
116
Time
(min)
FluxE
FluxS
DE
DS
6,853
515
2.35
0.24
10
6,853
672
2.35
0.34
15
6,897
799
2.41
0.42
6,854
928
2.36
25 6,866 1,129 2.37

20
0.53
0.73
30
6,854
1,291
2.36
0.93
35
6,859
1,342
2.36
1.00
40
6,854
1,371
2.36
1.05
45
6,857
1,369
2.36
1.05
50
6,856
1,380
2.36
1.06
55
6,857
1,384
2.36
1.07
60
6,859
1,390
2.36
1.08
117
-2 -

( )
pH Feed 1
Feed in Feedout Stripin Stripout
(ppm) (ppm) (ppm) (ppm)
La
Pr
Nd
939
299
317
217
0
396
6,834 1,353
0 3,338
1,007
68.2
49.5
78.5
50.1
80.2
60.9
Sm
900
433
230
51.9
49.3
Gd
499
191
157
61.7
50.9
200
80
85
60.0
70.7
Ce
0.0
0.0
Eu
0.0
0.0
Dy
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
118
pH Feed 3

% Extraction
%Stripping
La
939
268
342
71.5
50.9
Pr
1,007
186
410
81.5
49.9
Nd
6,834
827
4,157
87.9
69.2
Sm
900
52.7
55.1
61.2
51.1
Gd
0
261
499 194
0
156
426
200
200
0.0
0.0
Ce
0.0
0.0
Eu
0.0
0.0
Dy
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
119
pH Feed 5

% Extraction
%Stripping
La
939
270
333
71.2
49.8
Pr
1,007
247
457
75.5
60.1
Nd
6,834
1,893
3,251
72.3
65.8
Sm
900
52.8
52.8
59.3
50.9
Gd
0
251
499 203
0
151
425
200
200
0.0
0.0
Ce
0.0
0.0
Eu
0.0
0.0
Dy
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
120
-3
(
)
[Cyanex 272] = 0.1 M
La
Pr
Nd
939
268
342
186
0
410
6,834
827
0 4,157
1,007
71.5
50.9
81.5
49.9
87.9
69.2
Sm
900
426
261
52.7
55.1
Gd
499
194
156
61.2
51.1
200
200
0.0
0.0
Ce
0.0
0.0
Eu
0.0
0.0
Dy
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
: Feed pH = 3, [HNO3]S= 1.0. M, VF=VS= 5 L, QF=QS= 100 ml/min
121
[Cyanex 272] = 0.3 M
% Extraction
%Stripping
La
939
260
428
72.3
63.1
Pr
1,007
163
550
83.8
65.2
Nd
6,834
540
4,752
92.1
75.5
Sm
900
60.1
45.2
65.5
43.3
Gd
0
244
499 172
0
142
359
200
200
0.0
0.0
Ce
0.0
0.0
Eu
0.0
0.0
Dy
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
: Feed pH = 3, [HNO3]S= 1.0 M, VF=VS= 5 L, QF=QS= 100 ml/min
122
[Cyanex 272] = 0.5 M
% Extraction
%Stripping
La
939
259
415
72.4
61.1
Pr
1,007
160
463
84.1
54.6
Nd
6,834
513
4,444
92.5
70.3
Sm
900
61.1
50.1
66.4
49.6
Gd
0
275
499 168
0
164
350
200
200
0.0
0.0
Ce
0.0
0.0
Eu
0.0
0.0
Dy
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
123
-4
(
)
[HNO3]= 0.5 M
La
Pr
Nd
939
260
428
163
0
550
6,834
540
0 4,752
1,007
72.3
63.1
83.8
65.2
92.1
75.5
Sm
900
359
244
60.1
45.2
Gd
499
172
142
65.5
43.3
200
200
0.0
0.0
Ce
0.0
0.0
Eu
0.0
0.0
Dy
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
: Feed pH = 3, [Cyanex 272]=0.01 M, VF=VS= 5 L, QF=QS= 100 ml/min
124
[HNO3]= 1.0 M

% Extraction
%Stripping
La
939
270
436
71.2
65.2
Pr
1,007
190
546
81.1
66.8
Nd
6,834
95.2
86.2
Sm
900
62.3
46.3
Gd
499
0 5,608
339
0
260
328
175
144
64.9
44.4
200
200
0.0
0.0
Ce
0.0
0.0
Eu
0.0
0.0
Dy
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
125
[HNO3] = 1.5 M

% Extraction
%Stripping
La
939
259
445
72.4
65.5
Pr
1,007
160
567
84.1
66.9
Nd
6,834
92.5
85.9
Sm
900
61.1
46.8
Gd
499
0 5,430
350
0
257
513
168
148
66.4
44.6
200
200
0.0
0.0
Ce
0.0
0.0
Eu
0.0
0.0
Dy
0.0
0.0
Yb
0.0
0.0
Th
0.0
0.0
0.0
0.0
126
-5 -

( )
pH 1.0
pH 3.0
pH 5.0
La
914
959
956
Pr
1,129
1,173
1,086
667
677
679
Gd
440
436
423
171
Ce
Eu
Dy
Yb
Th
7,059
7,830
8,581
Sm
Nd
127
-6
(
)
0.1 M
0.3 M
0.5 M
La
959
970
971
Pr
1,173
1,206
1,210
677
773
786
436
467
473
Ce
Eu
Dy
Yb
Th
9,030
8,581
8,991
Sm
Nd
Gd
128
-7
(
)
0.5 M
1.0 M
1.5 M
La
970
956
971
Pr
1,206
1,167
1,210
773
801
786
467
463
473
Ce
Eu
Dy
Yb
Th
9,030
8,991
9,294
Sm
Nd
Gd
129
-8 -

( )
pH 1.0
pH 3.0
pH 5.0
La
177
191
186
Pr
221
229
255
128
146
140
Gd
88
87
84
47
Ce
Eu
Dy
Yb
Th
1,814
1,863
2,320
Sm
Nd
130
-9
(
)
0.1 M
0.3 M
0.5 M
La
191
239
232
Pr
229
307
258
146
136
153
Gd
87
79
92
Ce
Eu
Dy
Yb
Th
2,480
2,320
2,652
Sm
Nd
131
-10
(
)
0.5 M
1.0 M
1.5 M
La
239
243
248
Pr
307
305
316
136
145
143
Gd
79
80
83
Ce
Eu
Dy
Yb
Th
3,030
2,652
3,129
Sm
Nd
132
-11
-
( )
pH 1.0
pH 3.0
pH 5.0
La
2.1
2.5
2.5
Pr
3.6
4.4
4.1
7.3
Sm
1.1
1.1
3.1
Gd
1.6
1.6
1.5
1.5
0.0
0.0
Ce
0.0
0.0
0.0
Eu
0.0
0.0
0.0
Dy
0.0
0.0
0.0
Yb
0.0
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
Nd
2.6
1.1
133
-12

( )
0.1 M
0.3 M
0.5 M
La
2.5
2.6
2.6
Pr
4.4
5.2
5.3
7.3
11.7
Sm
Nd
12.3
1.1
1.5
1.6
Gd
1.6
1.9
2.0
0.0
0.0
0.0
Ce
0.0
0.0
0.0
Eu
0.0
0.0
0.0
Dy
0.0
0.0
0.0
Yb
0.0
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
134
-13

( )
0.5 M
1.0 M
1.5 M
La
2.6
2.5
2.6
Pr
5.2
4.3
5.3
11.7
19.8
Sm
1.5
1.7
Nd
12.3
1.6
Gd
1.9
1.9
2.0
0.0
0.0
0.0
Ce
0.0
0.0
0.0
Eu
0.0
0.0
0.0
Dy
0.0
0.0
0.0
Yb
0.0
0.0
0.0
Th
0.0
0.0
0.0
0.0
0.0
0.0
135
-14
-
( )
pH 1.0
pH 3.0
pH 5.0
La
0.98
1.04
0.99
Pr
1.01
1.00
1.56
2.25
Sm
0.97
1.23
1.51
Gd
1.04
1.05
1.04
2.43
0.00
0.00
Ce
0.00
0.00
0.00
Eu
0.00
0.00
0.00
Dy
0.00
0.00
0.00
Yb
0.00
0.00
0.00
Th
0.00
0.00
0.00
0.00
0.00
0.00
Nd
1.92
1.12
136
-15

( )
0.1 M
0.3 M
0.5 M
La
1.04
1.71
1.57
Pr
1.00
1.87
2.25
3.08
Sm
1.21
Nd
2.37
1.23
0.82
1.00
Gd
1.05
0.77
0.98
0.00
0.00
0.00
Ce
0.00
0.00
0.00
Eu
0.00
0.00
0.00
Dy
0.00
0.00
0.00
Yb
0.00
0.00
0.00
Th
0.00
0.00
0.00
0.00
0.00
0.00
137
-16

( )
0.5 M
1.0 M
1.5 M
La
1.71
1.87
1.89
Pr
1.87
2.01
3.08
6.24
Sm
2.03
Nd
6.09
0.82
0.86
0.88
Gd
0.77
0.80
0.81
0.00
0.00
0.00
Ce
0.00
0.00
0.00
Eu
0.00
0.00
0.00
Dy
0.00
0.00
0.00
Yb
0.00
0.00
0.00
Th
0.00
0.00
0.00
0.00
0.00
0.00
140
-1 (% Extract)
% (% Extract) =
-2 (% Recovery)
% (% Recovery) =

-3 (FluxExtract)
(FluxExtract) =
-4 (FluxRecovery)
(FluxRecovery) =
141
-5 (Distribution ratio of extraction)

-6 (Distribution ratio of recovery)

141
143
-1 (% Extract)
: -3 ( Cyanex 272 0.1 M)
- Cyanex 272
6,834 ppm
1,353 ppm
(mg/l)
0.1 M
(mg/l)
(% Extract)
( -3)
144
-2
: -3 ( Cyanex 272 0.1 M)
- Cyanex 272
= 0.1
= 6,834 ppm (mg/l)
= 1,353 ppm (mg/l)
- =
ppm (mg/l)
- = 3,338 ppm (mg/l)
= 6,834*5 = 34,170
= 1,353*5 = 6,765 mg
= 0*5
=0
= 3,338*5
= 16,690 mg
mg
( -3)
mg
145
-3 (FluxExtract)
: -3 ( Cyanex 272 0.1 M)
- Cyanex 272
0.1
34,170 mg
6,765 mg
100 ml/min
Resident Time =
Volume of Tube / Mass Flow Rate
= (250
ml)/ (100
ml/min)
= 2.5 min
3-2 : = 1.4 m2
(FluxExtract)
= 7,830 mg/m2min
146
-4 (FluxRecovery)
: -3 ( Cyanex 272 0.1 M)
- Cyanex 272
0.1
0 mg
16,690 mg
100
ml/min
Volume
of
Tube
/ Mass Flow Rate
= (640 mg) / (100 mg/min)
Resident Time =
=
6.4 min
3-2 : = 1.4 m2
(FluxRecovery) =
=
1,862.72 mg/m2 min
147
-5
: -3 ( Cyanex 272 0.1 M)
-
34,170 mg
6,765 mg
16,690 mg
mg
(Accumulate : mg)
=
[Nd+Nd
Nd3+ Accumulate
3+
Feed
3+
Stri[ inlet
] -[ Nd3+Feed+Nd3+Stri[]out
[34,179+0]-[6,765+16,690]
10,724 mg
148
-6 (Distribution ratio of
extraction)
: -3 ( Cyanex 272 0.1 M)
-
34,170 mg
6,765 mg
16,690 mg
=
=
mg
4.05
149
-6 (Distribution ratio of
recovery)
: -3 ( Cyanex 272 0.1 M)
-
34,170 mg
6,765 mg
16,690 mg
mg
=
=
1.56
150

3 ...
1-2 3
4-6
1-6
2551

2552

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2554

NEODYMIUM SEPARATION FROM MIXED RARE EARTH USING

A Thesis Submitted in Partial Fulfillment of the Requirements for the Degree

52404215 : MAJOR : (CHEMICAL ENGINEERING)

Department of Chemical Engineering

Graduate School, Silpakorn University

(Tube Side) ................................................

(Shell Side) ........................................

(Catalytic converter) ................................................ 6

[1] Gilmer "

1-2 .. 25532573 [27]

(oxides) (sulfides) (borides)

substance) (eddy current)

(low temperature coefficient of capacitance)

"" "rare earth elements" "rare earths"

Mixed rare earth

(equilibration time), oxalic acid, ,

D2EHPA+ 0.2 M TBP uranium ammonium carbonate

oxalic acid first order kinetic activation energy 77

neodymium CYANEX 921 kerosene

Muhammad Idiris Saleh [12]

Cyanex 272 15.97 g La(III)/100 g Cyanex 272 phosphorus

Nwe Nwe Soe (2008) [15] monazite

('H) 390 kJ/mol Pr(OH)3 carbonate

J.E. Dutrizac [18] rare earths sodium, potassium

< 0.3 wt.% rare earths e jarosite structure

sodium jarosite potassium jarosite rare

dione (HL-10-LH) 1,6-bis(1-phenyl- 3-methyl-5-hydroxy-4-pyrazolyl)-hexane-1,6-dione

lanthanum nitrate : dialkylphosphinate> dialkylmonothiophosphinate

(Chemical Treatment Process)

(Chemical Extraction and Leaching)

D2EHP, Cyanex 272 Cyanex 923

(Bidentate complexes) [33-34]

aq (Aqueous Phase) org

Liquid Membrane (SLM))

(Emulsion Liquid Membrane (ELM) Liquid Surfactant Membrane)

(Electrostatic Pseudo Liquid Membrane (ESPLIM)) 2-2

(Flat Sheet) (Spiral-Wound

Module) (Hollow Fiber)

2-3 PTFE [6]

(Capillary Force) (Hydrophilic or Hydrophobic Microporous)

2.3 (Hollow Fiber)

3-1 (a) Mixed rare earth (b)

3-2 (a) (b)

3-3 Inductively Coupled Plasma - Optical Emission Spectroscopy (ICP-OES)

3-5 (a) pH (b)

3-6 (a) pH (b)

3-7 Hollow fiber liquid membrane

3-8 (One through operation)

4.2 Kg/cm (60 psi)

1.4 m2 (15.2 ft2)

29.3 cm2/cm3 (74.4 m2/m3)

5, 10, 15, 20,25, 30, 35 40

2.5 Inductively Coupled Plasma - Optical

5, 10, 15, 20,25,30, 35 40

3.5 Inductively Coupled Plasma - Optical

Inductively Coupled Plasma - Optical

Mixed Rare Earth

4-1 Mixed rare earth

4,534 mg/l 19.2 Nd 3,816 mg/l

O/A 1/1 Di(2-ethylhexyl) phosphate

Mixed rare earth

Mixed rare earth