Ultrasonics Sonochemistry 102 (2024) 106735

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Ultrasonics Sonochemistry
journal homepage: www.elsevier.com/locate/ultson

A clean and efficient route for extraction of vanadium from vanadium slag
by electro-oxidation combined with ultrasound cavitation
Bao Liu, Luyang Duan , Shuang Cai , Qianqian Ren *, Junguo Li *, Yajun Wang , Yanan Zeng

A R T I C L E I N F O A B S T R A C T

Keywords: Extracting vanadium (V) from vanadium slag (VS) by the traditional roasting-leaching process has disadvantages
Vanadium slag of high energy consumption and high poisonous gases emission. In this work, a green and efficient route was
Electro-oxidation developed to extract V from VS without roasting by electro-oxidation combined with ultrasound cavitation
Ultrasound cavitation
(EOUC) intensification in sulfuric acid solution. The leaching parameters (e.g., leaching temperature, sulfuric
Vanadium leaching
Mineralogy
acid concentration, anodic current density, ultrasound power, liquid to solid ratio, leaching time and particle
size) were optimized. The leaching mechanism was explored by comparing the leaching behavior and miner­
alogical evolution of the direct sulfuric acidic leaching (DSL), electro-oxidation-assisted sulfuric acidic leaching
(EOSL), ultrasound cavitation-assisted sulfuric acidic leaching (UCSL) and EOUC methods. The results show that
introducing electric field strengthens the ultrasound cavitation effect on slag particles in sulfuric acid solution.
Under the optimum parameter of EOUC method, the leaching rate of V from VS is as high as 94.64 %. Using
EOUC method can open the silicate-wrapped structure of the spinel, increase pore volume of VS from 0.00127
cm3 g− 1 to 0.01124 cm3 g− 1, decrease slag particle size from 26.8 μm to 16.4 μm and improve specific surface
area from 0.508 m2 g− 1 to 10.855 m2 g− 1, which significantly accelerate V leaching process. The exposed spinel
was oxidized by both electrochemical route and chemical route, forming a mixture of V3+ ion and VO2+ ion after
leaching.

1. Introduction consumption of raw materials and energy. In addition, the roasting

Vanadium (V) is an important rare metal which is widely applied in
chemical production, non-ferrous alloy preparation, steel-making and
batteries [1–3]. The global consumption of V has continuously improved
from 72 kilotons in 2011 to 102 kilotons in 2021 [4]. With the increasing
demand in high strength steel and vanadium-based energy materials, the
consumption of V would grow up to exceeded 130 kilotons by the end of
2024 [5].
Vanadium slag (VS), generated by oxidizing the molten iron con­
taining V in a ladle furnace, accounting for about 70 % of V output. V
mainly exists in insoluble spinel as V(III) in VS [6]. Several methods
have been developed to extract V from VS including sodium salt
roasting-water/acidic leaching [7,8], calcification/lime roasting-acidic
leaching [9–11], non-salt roasting-acidic leaching [12], manganese
roasting-acidic leaching [13], etc. By roasting at high temperature in air
atmosphere, the V(III) in spinel can be fully oxidized, converting stable
spinel into the leachable forms such as NaVO3, Na4V2O7, CaV2O6, etc.
which are easily dissolved in water/acidic/alkaline solution [5]. How­
ever, the roasting-leaching technology has the disadvantages of high
process also produces poisonous gases of SO2, Cl2, HCl, posing threaten
to the environment [14]. Finding a green and efficient route for
extracting V from VS is of a great importance.
The out-field intensification technology of electro-oxidation has been
employed to handle zinc sulfide minerals, vanadium slag, copper sulfide,
pyrite, etc. [14–16]. As reported, applying electro-oxidation intensifi­
cation for directly extracting V from VS has the advantages of flexible,
low energy consumption and no poisonous gas emission, which is an
excellent alternative of the roasting-leaching technology. The electro-
oxidation process can break down the stable spinel and oxidize V(III)
to high valance state, making it easily dissolved into solution during the
leaching process [17]. However, the electro-oxidation method with V
leaching rate about 70 % in sulfuric acid solution is much lower than the
typical roasting-leaching process (87.9–95.0 %) [17–19]. The silicate-
wrapped structure of the spinel in VS inhibits the contact of the spinel
with the surface of the anode, thereby limiting the oxidation of V(III)
and resulting in low V leaching rate [17,20,21].
Ultrasound treatment of a solution would generate cavitation bub­
bles. The collapse of the cavitation bubbles produces high temperature

* Corresponding authors.
E-mail addresses: renqianqian1@126.com (Q. Ren), lijg99@163.com (J. Li).

https://doi.org/10.1016/j.ultsonch.2023.106735
Received 24 October 2023; Received in revised form 7 December 2023; Accepted 15 December 2023
Available online 16 December 2023
1350-4177/© 2023 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).
B. Liu et al. Ultrasonics Sonochemistry 102 (2024) 106735

Fig. 1. Particle size (PS) distribution and BET analysis of the raw VS, (a) particle size distribution, (b) BET analysis.

and high pressure which has mechanical effects of reducing diffusion

Table 1
resistance, accelerating dissolution, and destroying the surface of a
Chemical composition of the raw VS (wt.%).
reactant [2,22]. Ultrasound has draw increasingly attention in nano­
catalysts synthesis[23–26], wastewater treatment[27,28], valuable Element Content Element Content Element Content

metals extraction from minerals [29–32], etc.. Liu et al. [31] reported Fe 29.744 ± Si 6.546 ± P 0.079 ±
that the ultrasound cavitation decreases the particle size of minerals, 2.485 0.478 0.039
Ti 6.687 ± Ca 1.345 S 0.085 ±
exposes the encapsulated copper, increases solid–liquid contact. The ±
1.719 0.162 0.017
copper leaching rate of copper-cadmium slag is as high as 98.46 % at a V 6.667 ± Mg 1.473 ± Cl 0.101 ±
sonication time of 60 min with 800 W of ultrasound power. Said et al. 0.104 0.154 0.126
[33] indicated that the ultrasound cavitation can effectively break the Cr 3.450 ± Al 2.032 ± K 0.115 ±
silicate-wrapped structure of the calcium-bearing phase, renewing the 0.119 0.044 0.025
Mn 4.664 ± Na 0.381 O 36.602 ±
surface of the mineral particles. Using 80 W ultrasound waves, 96 % of
±
0.109 0.082 0.433
calcium is recovered from the steel slag with particle sizes of 50–74 μm
compared to 65 % by mechanical agitation. According to the results of
Wen et al. [34], the ultrasound cavitation can break and disperse the undersized sample (<74 μm) was used for analyzing and leaching ex­
solid minerals of the calcification-roasted chromium-vanadium slag in periments. The Mastersizer 3000 laser particle size analyzer (Malvern,
sulfuric acid solution. The optimal vanadium leaching rate of 96.67 % is UK) and the ASAP 2460 (Mcmurretik Instrument, USA) surface area
achieved at a sonication time of 60 min which is higher than the va­ analyzer were applied to determine the particle size (PS) and the specific
nadium leaching rate of 90.89 % obtained without ultrasound. Rahimi surface area of the sieved VS. Fig. 1 shows the PS distribution and
et al. [35] also indicated that the ultrasound cavitation increases va­ Brunauere-Emmette-Teller (BET) analysis of the raw VS. As exhibited,
nadium leaching rate of fuel–oil fly ash. Using 159 W of ultrasound the D50 value of the raw VS was 26.8 μm. The D10 and D90 values were
power for 2 h under the optimal conditions, the vanadium recovery is 4.1 μm and 69.9 μm, respectively. The obtained VS showed non-porous
88.7 %. It can be seen that the application of ultrasound for V recovery structure with the specific surface area of 0.508 m2 g− 1 and pore volume
from VS in an electric field may break the silicate-wrapped structure of of 0.00127 cm3 g− 1. The chemical composition of the VS was deter­
the spinel, resulting in the improvement of the anode-spinel contact mined using X-ray fluorescence (XRF, PANalytical Axios, PANalytical,
surface area. However, few researches have been carried out on V Netherlands) and listed in Table 1. This slag is rich in Fe, Ti, Si, V, Cr, Mn
leaching from VS under electro-oxidation combined with ultrasound and O. There are also some other minor elements of Ca, Mg, Al, Na, P, S,
intensification. Cl and K in the VS. The weight content of V in the VS was 6.667 wt%.
This work aims at directly extracting V from VS without roasting in Sulfuric acid with analytical grade was applied as the leaching agent.
sulfuric acid solution by electro-oxidation combined with ultrasound The sulfuric acid solutions were prepared using distilled water.
cavitation (EOUC) intensification. The effect of experiment parameters
(e.g., leaching temperature, sulfuric acid concentration, current density,
ultrasonic power, liquid–solid ratio (L/S) leaching time and particle 2.2. Leaching procedure
size) on V leaching efficiency were investigated. The evolution of the
mineralogical composition and morphology before and after leaching The leaching experiments were conducted using a 150 mL glass
was explored. The leaching mechanism of V from VS under EOUC reactor which was placed in the thermostatic magnetic stirrer. The glass
intensification was studied. reactor was equipped with two graphite electrodes with the dimension
of 2.5 cm × 2.5 cm as the anode and the cathode, respectively. The
2. Materials and methods electrode spacing was set as 2 cm. The IT6300 (ITECH, China) direct
current-power with maximum current of 3 A and maximum voltage of
2.1. Materials 30 V was used as the power source. The ultrasonic device (BHYTS-900 N,
Baihang Ultrasonic Technology Co., Ltd, China) with ultrasound work­
Vanadium slag (VS) was sampled from Chengde iron & steel Group, ing frequency of 24 kHz and maximum ultrasound power of 1000 W was
Hebei Province, China. The collected VS was crushed by an ore crusher, applied in this work. The ultrasonic probe with a diameter of 6 mm was
sieved with a 200 mesh (74 μm) sieve and dried at 105 ◦ C for 6 h. The placed in the middle of the anode and the cathode, which was in direct
contact with the leaching agent. The schematic diagram and real picture

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B. Liu et al. Ultrasonics Sonochemistry 102 (2024) 106735

Fig. 2. Schematic diagram (a) and real picture (b) of the experimental apparatus.

of the experimental apparatus are shown in Fig. 2.

10 g VS with PS < 74 μm was placed into the reactor filled with a
certain sulfuric acid concentration (cs = 50, 100, 150, 200, 250 g/L)
under the L/S of 2, 5, 10, 15 and 20. The solution was stirred by a
mechanical agitator at a stirring speed of 600 rpm. The leaching tem­
perature (T) was controlled at 40, 50, 60, 70, 80 and 90 ◦ C by water
bath. The anodic current density (ACD) used in different experiments
was 50, 75, 100, 125, 150 mA cm− 2. The ultrasound power (UP)
investigated in this work was 200, 300, 400, 500, 600, 700, 800 W. The
parameter of leaching time (t) was explored at 30, 60, 120, 180, 240 and
300 min. To investigate the effect of PS on V leaching rate, the VS was
sieved into five PSs of < 58 μm, 58–74 μm, 74–100 μm, 100–150 μm,
and > 150 μm using standard sieves. Each leaching experiment was
conducted three times for reliability and repeatability. After leaching,
the solid–liquid was separated using a 0.45 μm membrane filter. The
leaching rate of V from VS was calculated using the following equation
[14]:
cv × VL
Leaching rate (%) = (1)
ms × WV

Where, cV represents the mean V concentration of the obtained leachate, Fig. 3. XRD patterns of the raw VS.
in g/L, VL represents the leachate volume, in L, ms represents the VS
weight used for leaching experiment, in g, WV represents the mean V massspectrometry (ICP-MS, Agilent ICPMS7800, Agilent, USA) analysis.
weight content of the raw VS, in wt.%. The leachate pH and Eh were determined by pH and Eh meters. The Eh-
To compare the V leaching rate of the electro-oxidation combined pH diagram of V-H2O system at 25 ◦ C was obtained using HSC software
with ultrasound cavitation (EOUC) method and further investigate the based on the basic thermodynamic data. The ultraviolet visible (UV–vis)
leaching mechanism, the direct sulfuric acidic leaching (DSL) experi­ absorption spectra of the obtained leachates were determined using the
ment, electro-oxidation-assisted sulfuric acidic leaching (EOSL) experi­ UV-3600 double-beam spectrometer (Shimadzu, Japan).
ment, and ultrasound cavitation-assisted sulfuric acidic leaching (UCSL)
experiment were performed, respectively. In these three experiments, 3. Results and discussion
the VS, leaching agent, experimental apparatus, measurements were the
same as the EOUC method. The leaching parameter used for these three 3.1. Minerals and morphology of the raw vanadium slag
experiments was the optimum parameter without ultrasound power or
current density of the EOUC method. Fig. 3 presents the XRD patterns of the raw VS. The minerals of the
raw VS were spinel ((Mn, Fe)(V, Cr)2O4), fayalite ((Mn, Fe)2SiO4) and
augite (Ca(Mg, Fe, Al)(Si, Al)2O4). As shown in Fig. 4(a)-(f), (k) and
2.3. Characterization
Table 2, the dark region of the FESEM image mainly consisted of Fe, Mn,
V, Cr, Ti and O. This indicates that V accompanied with Fe, Mn, Cr, Ti, O
X-ray diffraction (XRD, Brucker D8 Advance, Brucker, Germany)
was present in the spinel. A part of the spinel was wrapped by a light
analysis were performed to determine the minerals of the raw VS and the
layers. Fig. 4(b), (c), (g)-(k) and Table 2 depict that the elemental
leaching residues. The morphology and element distribution of the raw
compositions of the light layer were Fe, Mn, Ca, Si, Mg, Al and O, sug­
VS and the leaching residues were detected by a field emission-scanning
gesting that the spinel-wrapped layer consisted of fayalite and augite.
electron microscopy coupled to an energy dispersive spectrometer
The weight contents of Fe and Mn were much higher than Ca, Mg and Al.
(FESEM-EDS, SU8020, Hitachi, Japan). Using the Mastersizer 3000 laser
This indicates that the spinel-wrapped layer mainly composed of
particle size analyzer, the PS of the leaching residues was detected. The
fayalite.
pore volume and specific surface area of the leaching residues were
measured using the ASAP 2460 surface area analyzer. V concentration of
the sampled leachate was determined using inductively coupled plasma

3
B. Liu et al.
Table 2
Elemental composition of the detected micro areas (wt.%).
Micro area Fe Mn V Cr
1 26.90 4.49 15.12 6.59
2 15.04 5.27 0.41 0.16
Fig. 4. Elemental mapping of the raw VS by FESEM-EDS analysis, (a) FESEM image, (b) Fe, (c) Mn, (d) V, (e) Cr, (f) Ti, (g) Ca, (h) Si, (i) Mg, (j) Al, (k) O.
3.2. Effect of leaching parameters on vanadium leaching rate
To optimize the leaching parameters, the influence of T, cs, ACD, UP,
L/S, t and PS on V leaching rate was explored. The evolution of V
leaching rate as a function of the leaching parameters was exhibited in
Fig. 5.
3.2.1. Effect of leaching temperature (T)
The influence of leaching temperature on V leaching rate was
investigated under the experimental conditions of cs = 200 g/L, ACD =
75 mA cm− 2, UP = 300 W, L/S = 10, t = 60 min, PS < 74 μm, T =
40–90 ◦ C. Fig. 5(a) shows that V leaching rate enhanced from 11.85 % to
66.00 % with the increase in leaching temperature from 40 ◦ C to 90 ◦ C.
This may be attributed to that the enhancement of leaching temperature
accelerated diffusion and mass transfer, ensuring the full contact among
the spinel, sulfuric acid solution and anode surface [36]. Although a
high temperature had a high V leaching rate, the further increasing
leaching temperature would enhance energy consumption and result in
water evaporation. Therefore, 90 ◦ C was regarded as the optimum
leaching temperature.
3.2.2. Effect of sulfuric acid concentration (cs)
The influence of cs on V leaching rate was explored at T = 90 ◦ C,
ACD = 75 mA cm− 2, UP = 300 W, L/S = 10, t = 60 min, PS < 74 μm, cs
= 50–250 g/L. Fig. 5(b) depicts that the rise of cs from 50 g/L to 200 g/L
improved V leaching rate from 8.99 % to 66.00 %. This attributes to that
increasing cs enhanced H+ ions amount per unit volume of the solution.
With the same L/S condition, more H+ ions would adsorb on the surface
of the solid particles and react with the minerals [37], which improved V
leaching rate. Meanwhile, enhancing cs also improved the concentration
difference between the mineral particles and the leaching agent,
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Ultrasonics Sonochemistry 102 (2024) 106735
Ti Ca Si Mg Al O
8.93 0.07 0.25 1.02 1.98 34.65
1.57 2.81 20.92 1.63 3.11 49.07
accelerating the internal and external diffusion of reactants [38]. A
decrease trend in V leaching rate was detected when the cs was higher
than 200 g/L. This may be attributed to that the amount of dissolved
oxygen was low in the solution with high cs caused by the salting-out
effect [39], decreasing the oxidation capacity of the leaching system.
Therefore, the cs = 200 g/L was selected as the optimum concentration.
3.2.3. Effect of anodic current density (ACD)
The effect of ACD on V leaching rate was explored under the
experimental conditions of T = 90 ◦ C, UP = 300 W, L/S = 10, t = 60 min,
cs = 200 g/L, PS < 74 μm, ACD = 75–150 mA cm− 2. As shown in Fig. 5
(c), with the increase of ACD from 50 mA cm− 2 to 75 mA cm− 2, the sharp
increase in V leaching rate from 46.70 % to 66.00 % was observed. In an
electrochemical field, the oxidation of spinel can be divided into the
electrochemical oxidation process occurred at the surface of the anode
and the chemical oxidation process related to the reaction between the
spinel and reactive oxygen species (e.g., O2, OH⋅, O–2, O2–
2 , etc.) produced
via oxygen evolution reaction at anode [40]. We noted that the amount
of the micro-sized oxygen bubbles formed on the surface of the anode
increased by enhancing the ACD during the electrolysis process. A
higher ACD was more favorable for the electrochemical oxidation as
well as the production of the reactive oxygen species, resulting in the
increase of V leaching rate. In addition, a higher ACD facilitated the
diffusion of V ions to escape from the spinel to the leachate, which also
contributed to the improvement of V leaching rate [5]. When the ACD
was higher than 75 mA cm− 2, the V leaching rate exhibited a slight
upward trend. Therefore, the ACD of 75 mA cm− 2 was regarded as the
optimum parameter.
3.2.4. Effect of ultrasound power (UP)
The influence of UP ranging from 200 W to 800 W on V leaching rate
B. Liu et al.
Fig. 5. Effect of leaching parameters on V leaching rate of VS, (a) leaching temperature, (b) sulfuric acid concentration, (c) anodic current density, (d) ultrasound
power, (e) L/S, (f) leaching time, (g) particle size.
was investigated under the experimental conditions of T = 90 ◦ C, ACD =
75 mA cm− 2, L/S = 10, t = 60 min, cs = 200 g/L, PS < 74 μm. As
demonstrated in Fig. 5(d), the V leaching rate improved from 53.95 % to
75.51 % with increasing UP from 200 W to 700 W. When the UP value
exceeded 700 W, the improvement of V leaching rate was indistinctive.
Ultrasound wave treatment of a solution created cavitation, mechanical
and chemical effects [31]. The collapse of the cavitation bubbles
generated microjets in the solution. A powerful enough microjet would
damage the solid minerals surface by impacting, which was conductive
to forming pores and cracks on the surface of the minerals and opening
the silicate-wrapped structure of the spinel [41]. A higher UP means it
produced a microjet with stronger stripping ability [42] that increased
the solid-anode-liquid contact surface and accelerated the dissolution of
the spinel, resulting in a higher V leaching rate. In addition, increasing
UP also improved the mass transfer process [43] which is helpful to the
enhancement of V leaching rate. When the UP reached a certain level the
cavitation tended to become saturated. The further increase of UP would
generated a large number of worthless cavitation bubbles [31,42].
Therefore, the UP value of 700 W was selected as the optimum
parameter.
3.2.5. Effect of liquid to solid ratio (L/S)
The effect of L/S on the V leaching rate was explored under the
experimental conditions of T = 90 ◦ C, UP = 700 W, t = 60 min, cs = 200
g/L, ACD = 75 mA cm− 2, PS < 74 μm, L/S = 2, 5, 10, 15 and 20. Fig. 5(e)
shows that L/S significantly impacted on the V leaching rate. With
increasing L/S from 2 to 20, the V leaching rate enhanced from 7.31 % to
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Ultrasonics Sonochemistry 102 (2024) 106735
90.22 %. This attributes to that the low L/S represents insufficient
amounts of sulfuric acid to reacted with the minerals of VS, resulting in
low V leaching rate. In addition, increasing L/S also improved fluidity of
the solution [41,44], promoting the contact among the anode surface,
leaching agent and minerals, which enhanced the V leaching rate. At the
same time, the increase of L/S enhanced cavitation intensity [31], which
was conductive to the damage of the minerals surface and the dissolu­
tion of the spinel. Although L/S = 20 had the maximum V leaching rate,
the high L/S would generate a large amount of wastewater. Therefore,
L/S = 15 was selected as the optimum parameter.
3.2.6. Effect of leaching time (t)
To select the suitable leaching time, the effect of leaching time on V
leaching rate was explored at T = 90 ◦ C, UP = 700 W, cs = 200 g/L, ACD
= 75 mA cm− 2, L/S = 15, PS < 74 μm, t = 30–300 min. As presented in
Fig. 5(f), the V leaching rate sharply improved from 60.47 % to 94.64 %
with increasing leaching time from 30 min to 120 min. Increasing time
could enhance the damage degree of the silicate-wrapped structure of
the spinel, exposing more spinel to contacted with the anode surface and
the leaching agent, which led to the sharp enhancement of V leaching
rate. The further prolonging the leaching time had little effect on V
leaching rate. This may be attributed to that the residual V in VS was
low. To saving energy, the t = 120 min was selected as the optimum
parameter.
3.2.7. Effect of particle size (PS)
The influence of PS on V leaching rate was investigated under the
B. Liu et al. Ultrasonics Sonochemistry 102 (2024) 106735

Fig. 6. Comparison of V leaching rate of VS using different leaching methods (a), and XRD patterns of the leaching residues (b).

Fig. 7. FESEM-EDS analysis of the leaching residues, (a) DSL residue, (b) EOSL residue, (c) UCSL residue, (d) EOUC residue.

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B. Liu et al.
Fig. 8. Particle size (PS) distribution of the leaching residues, (a) DSL residue, (b) EOSL residue, (c) UCSL residue, (d) EOUC residue.
experimental conditions of T = 90 ◦ C, UP = 700 W, t = 120 min, cs =
200 g/L, ACD = 75 mA cm− 2, L/S = 15, PS of < 58 μm, 58–74 μm,
74–100 μm, 100–150 μm, and > 150 μm. Fig. 5(g) shows that the V
leaching rates were 95.78 % and 92.89 % for the smaller particles of
<58 μm and 58–74 μm, respectively, which were much higher than the
larger particles. The reduction in slag PS improved V leaching rate. This
may be attributed to that the decrease in slag PS enhanced the reactive
surface area of minerals to react with the leaching agent and contact
with the anode surface, accelerating the dissolution of spinel. A slight
improvement in V leaching rate was obtained when the PS was smaller
than 74 μm, indicating that slag PS < 74 μm is appropriate for V
recovery.
According to the leaching experiments above, the optimized condi­
tions of the EOUC method were T = 90 ◦ C, UP = 700 W, cs = 200 g/L,
ACD = 75 mA cm− 2, L/S = 15, t = 120 min, PS < 74 μm.
3.3. Characterization of the leaching residues
In the EOUC leaching system, the main factors impacted on the
minerals and morphology of the VS were sulfuric acid, electro-oxidation
and ultrasound cavitation. Therefore, the DSL, EOSL and UCSL experi­
ments were performed under the optimum parameter of the EOUC
method to explore the leaching mechanism. Fig. 6(a) shows the V
leaching rates using different leaching methods. Under the optimum
parameter, the V leaching rates of DSL, EOSL, UCSL and EOUC were
53.99 %, 74.98 %, 63.56 % and 94.64 %, respectively. Both the electro-
oxidation intensification and the ultrasound cavitation intensification
could improve V leaching rate of VS in sulfuric acid solution. The V
leaching rate of EOSL method was 11.42 % higher than that of the UCSL
method. This may be attributed to that although the ultrasound
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Ultrasonics Sonochemistry 102 (2024) 106735
cavitation could expose more spinel to react with the sulfuric acid, the
insoluble property of the spinel led to the less improvement of V
leaching rate compared with the EOSL method. According to the results
of Deng et al. [21], the V(III) in VS can be oxidized to VO2+ ion through
electrochemical oxidation at an anodic potential of 1.23 V vs. SCE. Wang
et al. [40] also indicates that the vanadium spinel is less thermody­
namically stable than the chromium spinel, which can be directly elec­
trochemically oxidized at anode surface. Therefore, in the EOSL system,
the suspended spinel particles were directly oxidized when they collided
with the surface of the anode, promoting the release of V. After the
EOUC treatment, the V leaching rate was 19.66 %, 31.08 %, and 40.65 %
higher than the EOSL, UCSL, DSL, respectively. This can be attributed to
that the ultrasound cavitation occurred more easily and violently after
introducing electric field in sulfuric acid solution [45].
The mineralogical composition of the leaching residues were detec­
ted and present in Fig. 6(b). The mineralogical composition of the
leaching residues was more complex than the raw VS. The reactions
among the sulfuric acid, slag minerals and anode surface generated some
new minerals such as iron oxide, titanomagnetite and tridymite. The
original minerals of spinel, fayalite and augite could still be detected in
the leaching residues. Due to the dissolution of Al, the original augite
(Ca(Mg, Fe, Al)(Si, Al)2O4) was transformed to a new augite of Ca(Mg,
Fe)Si2O6. The intensity of the diffraction peaks relative to the spinel
followed the order of DSL > UCSL > EOSL > EOUC. This indicates that
both the electro-oxidation intensification and the ultrasound cavitation
intensification could promote spinel dissolution in sulfuric acid solution,
releasing more V. The promotion effect of the EOSL method was stronger
than that of the UCSL. The dissolution of the spinel in the EOUC system
was more thorough and more complete compared with that in the DSL,
UCSL, and EOSL system. As a result, the V leaching rate of VS using
B. Liu et al.
Fig. 9. BET analysis of the leaching residues, (a) DSL residue, (b) EOSL residue, (c) UCSL residue, (d) EOUC residue.
EOUC method was the highest. The mineralogical composition change
was consistent with the evolution trend of V leaching rate.
Fig. 7 shows the morphology of the leaching residues using different
leaching methods. As shown in Fig. 7(a), under the DSL process, a
certain amount of the spinel could be dissolved in sulfuric acid solution,
forming a circle of crack among the spinel and the silicates. The silicate-
wrapped layer of the spinel was not broken during the DSL process.
Compared with the DSL process, the electro-oxidation intensification
promoted the dissolution of the spinel, making the crack became larger
(Fig. 7(b)). However, the electro-oxidation also could not effectively
break the silicate-wrapped layer of the spinel in sulfuric acid solution.
The spinel was still wrapped by the silicates, which prevent the contact
among the liquid, solid and anode surface. The morphology of the
leaching residues after UCSL and EOCU processes was significant dif­
ference compared with the DSL residue and the EOSL residue (Fig. 7(c)
and (d)). A rougher surface of the spinel was formed and a greater
amount of the spinel was exposed after the UCSL and EOCU treatment.
This confirmed the fact that the generated microjets by cavitation
bubbles collapse could damage the surface of the spinel and the silicates,
forming pores on the surface of the minerals and opening the silicate-
wrapped structure of the spinel. It facilitated diffusion, interfacial
chemical and electrochemical reaction [31,46], resulting in higher V
leaching rate.
To further investigate the leaching mechanism, the PS distribution
and BET analysis of the leaching residues were performed. Fig. 8 shows
that all the D50 values of the leaching residues were smaller than the raw
VS due to the dissolution and fragmentation of the slag particles [47,48].
The D50 value of the leaching residues followed the order of DSL > EOSL
8
Ultrasonics Sonochemistry 102 (2024) 106735
> UCSL > EOUC. This also indicates that the electro-oxidation intensi­
fication could promote the dissolution of the minerals in sulfuric acid
solution, making the bulk of the EOSL residue particles was smaller than
that of the DSL residue. The ultrasound cavitation brought about the
fragmentation of the mineral particles which decreased the PS of the VS.
Comparing with Fig. 8(b) and (c), it suggests that the effect of the ul­
trasound cavitation intensification on the reduction in PS of VS was
stronger than the electro-oxidation intensification. It is noteworthy that
the PS of the EOUC residue was smaller than the UCSL residue. This
indicates that the electric field strengthened the fragmentation effect of
the ultrasound cavitation on VS particles and promoted V leaching
process.
The specific surface areas of the leaching residues were much larger
than the raw VS (Fig. 9). The improved specific surface area is relative to
the reduced slag PS and the formation of pores and cracks on the surface
of the slag minerals. It can be seen that the values of the specific surface
area and the pore volume of the UCSL residue and the EOUC residue
were higher than the DSL residue and the EOSL residue. This attributes
that the application of ultrasound damaged the VS particles, forming a
greater amount of pores on the surface of the minerals compared with
the DSL and EOSL process. Compared with the UCSL method, the spe­
cific surface area and the pore volume of the EOUC residue were higher.
This indicates that the impact area and strength of the microjet to the VS
particles were enhanced by electric field in sulfuric acid solution.
B. Liu et al. Ultrasonics Sonochemistry 102 (2024) 106735

Fig. 10. Comparison of pH, Eh and vanadium valence state of leachate using different leaching method, (a) pH, (b) Eh, (c) Eh-pH diagram of the V-H2O system, (d)
UV–vis spectra of the leachate.

3.4. Characterization of the leachate

Table 3
The main elemental compositions of the EOUC leachate.
3.4.1. Vanadium valence state in leachate
The leachate pH and Eh measurements, HSC thermodynamic simu­ Elements Fe Cr Ti Mn V
lation and UV–vis spectra analysis were conducted to investigate the Leaching rate 86.14 ± 74.86 ± 82.58 ± 84.57 ± 94.64 ±
effect of sulfuric acid, electro-oxidation and ultrasound cavitation on (%) 3.17 2.03 1.92 2.41 3.50
vanadium valence state of leachate. The pH values of the leachates ob­
tained using DSL, EOSL, UCSL, EOUC were similar (Fig. 10(a)). After
they collided with the surface of the anode as describing by equation (3).
leaching, the leachate pH of this four leaching methods ranged from
1.68 to 1.75. The Eh values were all greater than 0 mV (Fig. 10(b)), MeO⋅V2O3 + 4H+ → Me2+ + 2VO2+ + 2H2O + 2e- (3)
indicating that the obtained leachates showed oxidizing characteristic. It
is noteworthy that the Eh values of the EOSL and EOUC leachates were Besides equation (2), the chemical route also consisted of the
higher than the DSL and UCSL leachates, presenting stronger oxidability. oxidation reactions between the spinel and the generated reactive oxy­
This may be attributed to that the leached metallic ions with low valence gen species in the EOSL and EOUC system.
state were oxidized to high valence state when they contacted with the Fig. 10(d) shows that the characteristic absorption peaks observed at
anode surface. In addition, the reactive oxygen species produced via 600 nm and 768 nm are related to V3+ and VO2+, respectively [9,49].
oxygen evolution reaction at anode could also oxidize the leached This indicates that the obtained leachates were mixtures of V3+ ion and
metallic ions. The direct oxidation of the leached metallic ions at the VO2+ ion. The absorbance value ratios of V3+ ion to VO2+ ion of the
anode surface and the indirect oxidation of the leached metallic ions by EOUC and EOSL leachates were higher than the UCSL and DSL leachates.
producing the reactive oxygen species through anode reaction resulted This indicates that the electro-oxidation intensification promoted the
in the improvement of the Eh value. oxidation of V3+ ion to VO2+ ion which improved V leaching rate of VS.
Fig. 10(c) shows the Eh-pH diagram of the V-H2O system. The va­
nadium ion of all the obtained leachates existed as VO2+ under the 3.4.2. Elemental composition of the EOUC leachate
measured pH and Eh values. This may be attributed to that the Fe3+/ The leaching solution obtained by EOUC method was measured and
Fe2+ has a high electrode potential. The leached V3+ ion could be the main elemental compositions were listed in Table 3. As observed, the
chemically oxidized to VO2+ ion by Fe3+ ion as describing by equation main elemental compositions of the EOUC leachate were Fe, Cr, Ti, Mn,
(2) [9]. V. The leaching rates of Fe, Cr, Ti, Mn, V reached up to 86.14 %, 74.86
%, 82.58 %, 84.57 %, and 94.64 %, respectively. As mentioned above,
Fe3+ + V3+ + O2– → Fe2+ + VO2+ (2) the spinel composed of Fe, Cr, Ti, Mn, V and O. The high leaching rate of
these five elements indicates that a large amount of spinel was dissolved
In the EOSL and EOUC system, the oxidation of V was more complex
through EOUC method.
than the DSL and UCSL system. It included both electrochemical route
and chemical route. In the electrochemical route, the suspended spinel
(MeO⋅V2O3) could be directly oxidized to V(IV)-bearing phases when

9
B. Liu et al.
Fig. 11. Schematic diagram of the leaching mechanism of EOUC method.
3.5. Leaching mechanism
By comparing the leaching residues and leaching behavior of DSL,
EOSL, UCSL and EOUC methods, the leaching mechanism of EOUC
method was investigated. Fig. 11 exhibits the schematic diagram of
EOUC leaching mechanism. The ultrasound treatment of the sulfuric
acid solution generated a large number of cavitation bubbles. The
collapse of the cavitation bubbles leads to the production of the
microjets with high pressure to fragment the slag particles by impacting.
This process opened the silicate-wrapped structure of the spinel, formed
cracks and pores on the surface of the spinel, decreased slag PS and
improved specific surface area. The physical effect of ultrasound on the
slag particles accelerated the leaching process and improved V leaching
rate of VS. In the EOUC system, the oxidation of spinel consisted of
electrochemical route and chemical route. For the electrochemical
route, the V(III) in the exposed spinel was directly oxidized to VO2+
when they collided with the surface of the anode. For the chemical
route, the oxygen evolution reaction occurred on the surface of the
anode produced a certain amount of reactive oxygen species. The
generated reactive oxygen species could react with the exposed spinel,
oxidizing V(III) to VO2+. The electro-oxidation intensification oxidized
the insoluble spinel to the soluble V(IV)-bearing phases, resulting in the
increase of V leaching rate. In addition, introducing electric field could
also strengthened the ultrasound cavitation effect on slag particles in
sulfuric acid solution which also improved V leaching rate.
4. Conclusion
A green and efficient route for extracting V from VS via electro-
oxidation combined with ultrasound cavitation in sulfuric acid solu­
tion was systematically investigated. The optimum parameters of the
EOUC method for V leaching from VS are T = 90 ◦ C, UP = 700 W, cs =
200 g/L, ACD = 75 mA cm− 2, L/S = 15, t = 120 min, PS < 74 μm. Under
this leaching condition, the V leaching rate is 94.64 %. The V leaching
rate of EOUC method is 40.65 %, 19.66 % and 31.08 % higher than the
DSL, EOSL and UCSL methods, respectively. The ultrasound treatment of
VS in sulfuric acid solution can open the silicate-wrapped structure of
the spinel, form cracks and pores on the surface of the spinel, decrease
slag PS and improve specific surface area, which accelerates V leaching
process. In the EOUC system, the exposed spinel can be oxidized both by
electrochemical oxidation on the anode surface and by chemical
oxidation of reactive oxygen species, transforming insoluble spinel to
soluble V(IV)-bearing phases. The obtained VS leachate of EOUC
method is a mixture of V3+ ion and VO2+ ion. Introducing electric field
can strengthen the ultrasound cavitation effect on the slag particles in
10
Ultrasonics Sonochemistry 102 (2024) 106735
sulfuric acid solution which improved V leaching rate. By using the
EOUC method, V can be directly recover from VS without roasting,
meanwhile, no poisonous gases are produced, which is a clean method
for V extraction from VS.
CRediT authorship contribution statement
Bao Liu: . Luyang Duan: Investigation. Shuang Cai: Investigation,
Methodology. Qianqian Ren: Investigation, Methodology, Funding
acquisition, Resources. Junguo Li: Writing – review & editing,
Conceptualization, Supervision, Project administration, Funding acqui­
sition. Yajun Wang: Investigation, Methodology. Yanan Zeng: Inves­
tigation, Methodology.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
This work was financially supported by Hebei Natural Science
Foundation (No. E2021209043, No. E2022209093, No. E2020209043),
Central Guidance Local Science and Technology Development Fund
Project of Hebei Province (236Z1102G), Science and Technology Project
of Hebei Education Department (No. BJ2020022), Tangshan Municipal
Project of Science and Technology (No. 19150201E, No. 22130228H),
Key Program of North China University of Science and Technology (No.
ZD-ST-202312-23), Graduate Student Innovation Foundation of Hebei
Province (No. 2023S09).
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