Separation Science and Technology

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Adsorption of Re(VII) from sulfuric acid solutions

by coated impregnated resins containing TBP

Zhong-chen Ma, Xue-yi Guo, Dong Li & Qing-hua Tian

To cite this article: Zhong-chen Ma, Xue-yi Guo, Dong Li & Qing-hua Tian (2019): Adsorption
of Re(VII) from sulfuric acid solutions by coated impregnated resins containing TBP, Separation
Science and Technology, DOI: 10.1080/01496395.2019.1706577

To link to this article: https://doi.org/10.1080/01496395.2019.1706577

Published online: 23 Dec 2019.

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SEPARATION SCIENCE AND TECHNOLOGY
https://doi.org/10.1080/01496395.2019.1706577

Adsorption of Re(VII) from sulfuric acid solutions by coated impregnated resins

containing TBP
Zhong-chen Maa,b, Xue-yi Guoa,b, Dong Lia,b, and Qing-hua Tiana,b
a
School of Metallurgy and Environment, Central South University, Changsha, P.R. China; bNational & Regional Joint Engineering Research
Center of Nonferrous Metal Resource Recycling, Changsha, P.R. China

ABSTRACT ARTICLE HISTORY

The experiments on the adsorption of Re(VII) onto Tributyl phosphate (TBP) coated solvent- Received 15 August 2019
impregnated LS-300 resins (TBP-CSIRs) were performed systematically. The optimal TBP concen- Accepted 25 November 2019
tration for the impregnation was 70%. The adsorption equilibrium reached in 6 h and the KEYWORDS
saturation adsorption capacity was 24.48 mg/g. The highest separation coefficients of rhenium Re(VII); Coated solvent
over copper, iron, zinc, nickel, and arsenic were 93, 412, 348, 72 and 51, respectively. The impregnated resins; TBP;
adsorption capacity maintained in 93.50% after five times recycles. A 97.57% rhenium was Adsorption
recovered from waste acid with TBP-CSIRs, respectively. This study would contribute to the direct
recovery of rhenium from waste acid.

Introduction low recovery rate, troublesome operation and the loss of

extractant in precipitation-leaching-extraction.[10] To solve
Rhenium has been widely used for the manufacture of
the problems mentioned above, researchers have
high-temperature supper-alloys because of its high
done lots of work. Adsorption, anion exchanger[13],
hardness and high-temperature resistance.[1] In addi-
photoreduction[14], magnetic liquid separation,[15] and
tion, it is an essential element for the synthesis of
electrolytic extraction[16] have been developed for the
catalysis that is used for petroleum reforming.[2] In
recovery of Re(VII) from aqueous solutions. Adsorption,
recent studies, it was also found that ReS2, a two-
which has been used for the adsorption of various metallic
dimensional material, has a significant application
ions, is considered as the most promising method for the
value in the field of optoelectronics.[3–5] Therefore, the
efficient recovery of Re(VII) from aqueous solutions.[17]
demand for rhenium will increase rapidly in the com-
Many adsorbents have been prepared in the latest decade
ing decades.
for the adsorption of Re(VII).[18–20] However, the adsor-
Rhenium mostly exists as a trace element in the copper
bents are needed to be further developed, especially in the
and molybdenum ores.[4] During the copper smelting pro-
respects of selectivity and the resistance to strong acidity.
cess, rhenium enters the smelter off-gas in the form of Re2
Solvent-impregnated resins (SIRs), consisting of inner
O7 and then dissolves in the purification solutions of sulfur
resins and extractant, are considered as a promising adsor-
dioxide.[5,6] The purification solutions, namely waste acid,
bent for the adsorption of metallic ions with the benefits of
mostly consist of various metallic ions with high sulfuric
high selectivity and resistance to strong acidity.[21]
acidity.[7] Solvent extractant, ion exchange, and precipita-
In recent years, SIRs have been used for the adsorp-
tion-leaching-extraction have been applied for the recovery
tion of many metallic ions, such as Fe(Ⅲ)[22], La (Ⅲ),
of Re(VII) from waste acid.[8–10] Solvent extractant has
Ce(Ⅲ)[23], In(Ⅲ)[24], Cr(VI)[25], Pu(Ⅳ)[26] and V
been used for the extraction of Re(VII) with the benefit of
(Ⅳ).[27] Tributyl phosphate (TBP, and its structure is
being highly selective. However, it is usually required that
shown in Fig.1), has a wide range of applications in the
the rhenium should be at a high concentration in aqueous
extraction of metallic ions, such as Re(VII)[11], Hf
solutions.[11] As another main method, ion exchange is
(Ⅳ)[28], U(Ⅳ)[29], Au(Ⅲ)[30] and Li(I)[31], with the ben-
limited by the problem of low selectivity. This will result
efits of low price and excellent separation property. The
in the poison of ion exchange resins and make it difficult for
inertia resin-LS-300, which is made of polystyrene, was
further purification.[12] In addition, there are many pro-
selected as the extractant carrier with the benefits of
blems, such as high reagent consumption, low selectivity,
high specific surface area and low cost, and it has no

CONTACT Dong Li dongli@csu.edu.cn School of Metallurgy and Environment, Central South University, Changsha 410083, P.R. China
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/lsst.
© 2019 Taylor & Francis Group, LLC
2 Z. MA ET AL.
Figure 1. The structure of tributyl phosphate.
adsorption for any ions in the aqueous solutions.
Furthermore, the film coated on the surfaces of SIRs
is necessary to minimize the loss of extractant, which
has been investigated in certain papers.[32,33]
In this study, the coated solvent-impregnated resins
containing TBP (TBP-CSIRs) were prepared for the
selective adsorption of Re(VII) from sulfuric acid solu-
tions. Each batch experiment for the adsorption of
TBP-CSIRs on Re(VII), containing adsorption kinetics
and isotherms, was conducted systematically. The selec-
tive adsorption of Re(VII) onto TBP-CSIRs were also
investigated. The stability between the coated and the
un-coated solvent-impregnated resins was evaluated. In
addition, TBP-CSIRs were used for the selective
adsorption of Re(VII) from waste acid. This study
would contribute to the direct recovery of rhenium
from waste acid generated from the copper smelter.
Experimental
Materials
LS-300 resin (surface area 600–700 m2/g, pore diameter
10 nm and bead size 20–60 mesh) was supplied by
Lanshen, Shanxi (China). Tributyl phosphate (TBP),
Ammonium perrhenate, Na2HAsO4 · 7H2O, CuSO4 ·
5H2O, Fe2(SO4)3·xH2O, ZnSO4 · 7H2O, NiSO4 · 6H2O,
Polyvinyl alcohol (PVA), Boric acid were supplied by
Sigma-Aldrich, sulfuric acid (95%-98%) was supplied
by Sinopharm Chemical Regent Co., Ltd. All reagents
Figure 2. The schematic diagram of adsorption reaction.
were analytical grade. Waste acid was generated from
a copper smelter, Henan province, China.
Preparation of TBP-CSIRs
As the extractant carrier, LS-300 resins were soaked by
ethanol followed by washing with dilute sulfuric acid to
remove the organic and inorganic residues. Then, the
pretreated resins were added into the mixed solutions
of TBP and ethanol (L:S = 20:1). Subsequently, the
mixed solutions were shaken in an oscillator for 24
h at 40°C. The TBP impregnated resins (TBP-SIRs)
were separated and washed with ultrapure water.
Then, dried TBP impregnated resins were added into
the 3 wt% PVA solutions shaking for 18 h at 40°C to
coat the PVA film on the surfaces of TBP-SIRs. Finally,
the saturated boric acid solutions were used to improve
the stability of PVA film by a cross-linked reaction for
8 h at 25°C. The impregnation ratio of TBP was calcu-
lated via Equation (1).
m2  m1
n¼ (1)
m2
where m2 is the mass of TBP-CSIRs (g) and m1 is the
mass of the pretreated LS-300 resins (g).
Experimental procedures
Adsorption experiments were conducted in a conical
flask. In each batch experiment, 100 mg of adsorbent
was added into 250 mL of feed solutions and then kept
the conical flasks shaking in a shaker for a certain time.
Adsorption capacity (Qe, mg/g) and separation coeffi-
cient (β) were calculated via Equations (2) and (3),
respectively. Adsorption reaction was shown in
Fig. 2.[11]
ðC0  Ce ÞV
Qe ¼ (2)
m



C0=Re  Ce=Re =Ce=Re
βRe=X ¼
(3)
C0=X  Ce=X =Ce=X
where initial concentration (C0) and equilibrium con-
centration (Ce) of metallic ion (mg/L); the volume of
feed solutions (V, L); the quality of TBP-CSIRs (m, mg),
X represents the element of Cu, As, Fe, Zn or Ni.
Analysis and characterization
ICP-OES (Spectro Blue Sop, Germany) was used to
measure the concentrations of metallic ion in feed
solutions. SEM (JSM-IT300LA, Japan) was used to
examine the morphology of samples and the element
distributed in the pores of resins.
Results and discussion
SEM and EDS analysis
To confirm the existence of the PVA film on the surfaces of
TBP-CSIRs, the samples were evaporated for 2 h at 120°C
and then they were sliced. The SEM images of TBP-CSIRs
were shown in Fig. 3. It is found that the gelatinous mem-
brane is on the surfaces of TBP-CSIRs (Fig. 3 a, b). The
smooth surface is observed in the coating region while the
rough surface is observed on the damage region.
Furthermore, the thickness of the film is about 5 μm
(Fig. 3 c, d), which is similar to the reports in other
studies.[32,33] The element mapping of Re (Fig. 4b) indicated
Figure 3. The SEM images of TBP-CSIRs.
SEPARATION SCIENCE AND TECHNOLOGY 3
that Re(VII) distributes evenly on the cross section of
Re(VII)-TBP-CSIRs, suggesting that TBP is impregnated
in the entire pores of resins.
Effect of extractant concentration on adsorption
To evaluate the optimal TBP concentration for the
preparation of TBP-CSIRs, the effect of TBP concentra-
tion on the adsorption of Re(VII) was investigated
(Fig. 5). With the increasing concentration of TBP
from 40% to 70%, the adsorption capacity of TBP-
CSIRs on Re(VII) increases from 6.75 to 12.07 mg/g
due to the increasing availability of TBP. However, the
adsorption capacity decreases to 10.68 mg/g when the
TBP concentration is up to 80%. It is the fact that the
excess TBP forms multilayers.[29] Therefore, 70% of
TBP concentration should be selected for the prepara-
tion of TBP-CSIRs.
Adsorption kinetics
In order to investigate the adsorption behaviors during
the adsorption process, the adsorption kinetics were
studied. The adsorption kinetic data were fitted by the
pseudo-first-order model Equation (4) and the pseudo-
second-order Equation (5) model, respectively.[34]


Qt ¼ Qm 1  ek1 t (4)
4 Z. MA ET AL.

Figure 4. The SEM image (a) and element mapping of Re (b) for TBP-CSIRs loaded Re(VII).

model (/min), K2 is the adsorption constant of pseudo-

Figure 5. Effect of TBP concentration on extraction, C0=
100 mg/L, C(H2SO4) = 0.5 mol/L, t = 12 h, T = 25 °C, 250 rpm.
Q2m k2 t
Qt ¼
1 þ Qm k2 t
where Qt is the adsorption capacity of t min (mg/g), K1
is the adsorption constant of the pseudo-first-order
first-order mg/g·min−1/2), and t is the adsorption
time (min).
As shown in Fig. 6, it is found that the adsorption
rate is rapid during the first 2 h, and the adsorption
capacity is up to 46.02, 9.47 and 11.91 mg/g with the
initial concentration of Re(VII) of 25, 50 and 75 mg/L,
respectively. Following the adsorption capacity
increases with 0.97, 2.00 and 1.73 mg/g during the
following 4 h, respectively. Finally, the adsorption capa-
cities increase slightly when the contacting time exceeds
6 h, where the maximum adsorption capacity is 7.01,
11.86 and 14.44 mg/g, respectively. All parameters cal-
culated by the equation of kinetic models are summar-
ized in Table 1. The highest correlation coefficient (R2
= 0.995, 0.990 and 0.992) and the distribution of experi-
mental data on the fitting curve suggest that the
(5) pseudo-second-order model fitted better than the
pseudo-first-order model. In addition, the saturation
adsorption capacities calculated from the equation of
the pseudo-second-order model are much close to the

Figure 6. Adsorption kinetics data and fitted models of Re (VII) onto TBP-CSIRs: Pseudo-first-order, pseudo-second-order, C(H2SO4) =
0.5 mol/L, T= 25 °C, 250 rpm.
 SEPARATION SCIENCE AND TECHNOLOGY 5

Table 1. Kinetic parameters of different models for the sorption temperatures.[34,35] The adsorption equilibrium experi-
of Re(VII) onto TBP-CSIRs at different initial concentrations. ments were conducted at 288, 298 and 308 K, respec-
C0 (mg/L) tively. Experimental results concerning the effect of
Kinetic Model 25 50 75 temperature on the adsorption of Re(VII) at different
Pseudo-first-order
k1 (1/min) 1.196 1.244 1.807
concentrations could be observed from Fig. 7. It was
Qe, 1 (mg/g) 6.92 11.38 13.61 observed that the adsorption ratio increased with the
R2 0.989 0.947 0.946
Pseudo-second-order increase of temperature, while the adsorption capacity
k2 (mg/g·min1/2) 0.238 0.157 0.188 decreased, indicating that the adsorption of Re(VII) is
Qe, 2 (mg/g) 7.52 12.32 14.60
R2 0.995 0.990 0.992 an exothermic process. The Langmuir model fits well
with a higher correlation coefficient at various initial
concentrations under various temperatures (Table 2).
The saturation adsorption capacities calculated by the
experimental equilibrium adsorption capacities. equation of the Langmuir model are 24.48, 17.35 and
Therefore, the adsorption of TBP-CSIRs on Re(VII) is 12.49 mg/g, respectively, which are close to the experi-
a chemisorbed process, and the time of adsorption mental adsorption capacities. Therefore, the adsorption
equilibrium is about 6 h with the initial concentration of TBP-CSIRs on Re(VII) is in the form of a monolayer
of from 25 to 75 mg/L.[34] molecule with the saturation adsorption capacity of
24.48 mg/g. Different from the previous studies[18–20],
Adsorption isotherms this study was carried out at the high sulfuric acidity
(initial pH value was zero), the comparation of the
The relationship between the adsorption capacity and adsorption capacity of Re(VII) onto TBP-CSIRs with
the equalized concentration was explored. Adsorption those adsorbents previously reported is not considered.
isotherm models, namely Langmuir Equation (6) and
Freundlich Equation (8), were used to describe the
adsorption behaviors of Re(VII) onto TBP-CSIRs.[34] Selectivity adsorption of TBP-CSIRs on Re(VII)
Q m KL C e To investigate the selective adsorption of Re(VII) onto
Qe ¼ (6)
1 þ KL C e TBP-CSIRs from mixed solutions, the adsorption tests
were carried out with different concentrations of sulfu-
Qe ¼ KF Ce1=n (7)
ric acid solutions. The impurity elements contained As,
where Qe (mg/g) is the equilibrium adsorption capacity, Cu, Fe, Zn and Ni. It is found that the adsorption
Ce (mg/L) is the equilibrium concentration of Re(VII), capacity of Re(VII) onto TBP-CSIRs from the single
Qm (mg/g) is the theoretical maximum adsorption Re(VII)-containing system increases from 11.90 to
capacity and KL (L/g) is the Langmuir adsorption con- 18.17 mg/g with the increasing sulfuric acidity
stant. KF and n are adsorption equilibrium constant (Fig. 8). It is the fact that the H+ concentration
and concentration index, respectively. increases with the increase in sulfuric acidity, which
It is well known that the equilibrium constant and will produce more hydrogen bonds.[36] In addition,
adsorption capacity will change under different the adsorption capacities barely decrease from 11.60

Figure 7. Adsorption isotherm data and fitted models of Re (VII) onto TBP-CSIRs, Langmuir (a), Freundlich (b), C(H2SO4) = 0.5 mol/L,
t = 12 h, 250 rpm.
6 Z. MA ET AL.

Table 2. Isotherms parameters of different models for adsorp- Re(VII) loaded on TBP-CSIRs and TBP-SIRs could be
tion of Re(VII) onto TBP-CSIRs at different temperatures. stripped by ammonia solution (5 mol/L, L:S = 20:1),
T (K) and the desorption ratio could be both up to 95.00%. In
Isotherm Model 288 298 308 addition, the continuously recycle tests suggest that
Langmuir
Qm (mg/g) 24.48 17.35 12.49 TBP-CSIRs have an excellent stability for reuse (Fig.
KL (L/mg) 0.024 0.022 0.020 9). After being five times recycles, the adsorption capa-
R2 0.996 0.985 0.989
Freundlich city of Re(VII) onto TBP-CSIRs decreases from 16.71 to
KF (L/mg) 3.717 2.540 1.660 15.62 mg/g, while the adsorption capacity of Re(VII)
n (mg/g) 3.132 3.101 2.975
R2 0.917 0.894 0.917 onto TBP-CSIRs decreases significantly from 13.80 to
6.91 mg/g. It is suggested that the TBP-CSIRs is of
excellent stability for reuse.
to 17.15 mg/g in the multiple system while the max-
imum adsorption capacities for impurity ions are lower
Adsorption of Re(VII) from waste acid
than 0.5 mg/g. The highest separation coefficients of
The recovery of Re(VII) from waste acid was carried
rhenium over copper, iron, zinc, nickel, and arsenic are
out and the results are reported in Table 4. It is found
93, 412, 348, 72 and 51, respectively (Table 3). It is the
that TBP-CSIRs show the highest selectivity adsorption
fact that As(V) could mostly form HAsO3 at the high
for Re(VII) in the multiple system with the adsorption
sulfuric acidity.[37] The results suggest that TBP-CSIRs
have an excellently selective adsorption for Re(VII)
from mixed solutions. Table 3. Separation coefficient of Re(VII) onto TBP-CSIRs versus
contaminant ions at various acidities.
Sulfuric acid concentration (mol/L)
0.5 1.0 2.0 3.0 4.0
Regeneration and recovery studies
βRe/Cu 93 39 37 42 41
Regeneration cycles βRe/Fe 412 37 50 49 48
βRe/Zn 348 37 57 54 52
Desorption performance is an important performance βRe/Ni 56 49 72 67 49
βRe/As 51 28 41 41 33
of the adsorbent. It had been investigated that the

Figure 8. Adsorption behavior of TBP-CSIRs for various metal ions as a function of sulfuric acid concentration, C0 = 50 mg/L, t = 12 h,
T = 25°C, 250 rpm.
 SEPARATION SCIENCE AND TECHNOLOGY 7

93.50% after being five times recycles. Rhenium was

recovered at the ratio of 97.57% from waste acid by
TBP-CSIRs.

Funding
This work was supported by the National Natural Science
Foundation of China [51604303];Hunan Natural Science
Fund for Distinguished Young Scholar [2019JJ20031];
Fundamental Research Funds for the Central Universities of
Central South University [2019zzts243];

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