Chemical Engineering Journal 326 (2017) 540–550

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Chemical Engineering Journal

journal homepage: www.elsevier.com/locate/cej

Supergravity separation for recovering metals from waste printed circuit

boards
Long Meng, Zhe Wang, Yiwei Zhong, Lei Guo, Jintao Gao, Kuiyuan Chen, Huijing Cheng, Zhancheng Guo ⇑
State Key Laboratory of Advanced Metallurgy, University of Science and Technology Beijing, 30 Xueyuan Road, Beijing 100083, People’s Republic of China

h i g h l i g h t s g r a p h i c a l a b s t r a c t

E-waste contains complex Based on the different melting points of metals or alloys, three alloys (Pb-Sn, Sn-Cu and Cu-Zn) were
combinations of alloys, metals, and selectively and gradually recovered from granulated computer printed circuit boards (CPCBs) by super-
toxic substances. gravity separation.

Cost-effective and environmental
recovery are difficult via traditional
methods.

Supergravity separation provides
highly efficient recovery of metals
from PCBs.

Higher gravity coefficient improved
recovery rates.

The process achieves closed-loop,
clean recycling of e-waste with high
efficiency.

a r t i c l e i n f o a b s t r a c t

Article history: The recovery of metals from electronic waste has become increasingly important due to environmental
Received 20 February 2017 concerns and potential risks to the supply of strategic raw materials. Electronic waste, especially waste
Received in revised form 18 April 2017 printed circuit boards from a variety of sources, is of inherently high complexity in composition, phase,
Accepted 30 April 2017
and physiochemical properties. Waste PCBs contain valuable metals and multiple toxic substances, moti-
Available online 3 May 2017
vating a search for processes or technologies to allow their cost-effective and environmental recycling. A
novel process was developed, using supergravity separation to recover valuable metals (Pb, Sn, Zn, and
Keywords:
Cu) from granulated computer printed circuit boards. A three-step separation process was adopted to
Printed circuit boards
Supergravity separation
selectively recover metals or alloys and to concentrate precious metals. Total recovery values for Pb,
Recover Sn, Zn, and Cu were 96.37%, 92.32%, 93.71%, and 97.90%, respectively. The mass fraction of (Pb + Sn) in
Concentrate Pb-Sn alloy, (Sn + Cu) in Sn-Cu alloy, and (Cu + Zn) in Cu-Zn alloy reached 94.84%, 85.18%, and 84.73%,
Metals respectively, during the individual separation steps. Compared with the contents of Au (44 ppm), Ag
(124 ppm), and Pd (6.5 ppm) in the computer printed circuit boards, the contents of Au, Ag, and Pd in
the residues after three-step separation were concentrated to 150 ppm, 550 ppm, and 12 ppm, respec-
tively. By a combination of appropriate hydrometallurgical process and supergravity separation of metals
or alloys, this process can achieve closed-loop, clean recycling of electronic waste with significant
efficiency.
Ó 2017 Published by Elsevier B.V.

1. Introduction

Due to technological advances and obsolescence of electrical

⇑ Corresponding author. and electronic equipment (EEE), the production of electronic waste
E-mail address: zcguo@ustb.edu.cn (Z. Guo).

http://dx.doi.org/10.1016/j.cej.2017.04.143
1385-8947/Ó 2017 Published by Elsevier B.V.
 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550 541

(e-waste) is increasing [1]. In 2016, global production of e-waste 2. Experimental

was about 45 million tons, with annual growth of 2 million tons
per year. As an important part of EEE, waste printed circuit boards 2.1. Materials
(WPCBs) accounted for about 3% of total e-wastes generated. PCBs
contain many valuable metals such as Cu, Pb, Sn, Cd, Au, and Ag. Waste CPCBs were purchased from an enterprise in Hunan Pro-
However, the toxic substances (i.e., brominated flame retardants vince, China, and crushed and milled into powder samples of par-
(BFR), polyvinyl chloride plastic (PVC), and heavy metals) in WPCBs ticle size approximately 1.0 mm (Fig. 2).
can pose serious environmental threats if not properly treated [2].
Therefore, recycling of WPCBs is an important subject not only for 2.2. Equipment and methods
the recovery of valuable materials, but also for protection of the
environment. The CPCBs were placed into a furnace that put into a centrifugal
To date, many technologies have been developed to recover apparatus. The supergravity field was generated by a centrifugal
valuable metals, including hydrometallurgy [3–5], bioleaching apparatus from the vertical angle with the heating furnace and
[6–8], pyrometallurgy [9–11], and physical methods [12–14]. the counterweight fixed symmetrically onto the horizontal rotor
These methods can successfully recover and recycle different met-
als, but have some notable shortcomings in some cases. The
hydrometallurgical recycling of various metals in WPCBs is a very
long and complicated process, leading to higher costs; further-
more, large amounts of waste acid liquid and sludge are produced,
which require careful treatment [15]. Bioleaching processes are
hindered by the difficulty of selecting suitable bacteria, and by
the long period. Traditional pyrometallurgical procedures are
highly dependent on investment, and generate atmospheric pollu-
tion due to evolution of toxic dioxins, furan gases, and carcinogenic
compounds [16]. Physical methods have some disadvantages but
were the earliest and most widely used approach for separating
and recovering metals from WPCBs. Compared with other meth-
ods, physical recovery offers advantages such as high efficiency,
low cost and pollution, simple principles, and ease of upscaling
production. However, due to the complex compositions of raw
materials, traditional physical methods can not completely sepa-
rate the constituent metals. Supergravity, as a physical method of
strengthening mass transfer, can effectively separate components
from complex materials. Supergravity is the force of matter greater
than that under normal gravity acceleration (9.80 m/s2). In the
supergravity field, molecular diffusion and mass transfer process
are faster and liquid phase can flow in and out of porous media
Fig. 1. Flow chart of the separation and concentration of metals from CPCB
or channels and contact with other phases at hundreds of times particles.
than in normal gravity field. Great shearing force by supergravity
tears liquid into micron to nanometer liquid membranes, filaments
and droplets, then forms huge and new phase interface, making the
micro mixing and mass transfer process greatly improved. The
technology has been successfully applied to the enrichment of
valuable elements from different slags [17–19], the fabrication of
functionally graded materials [20–22], and removal of impurities
from alloys or metals [23–25].
The use of supergravity offers a highly attractive and promising
technology with many advantages such as improved environmen-
tal performance, high efficiency, low investment cost, and wide
range of practical applications. The difference in melting point
between the solid-particle and liquid melt results in the gradual
distribution and separation of particles along the centrifugal direc-
tion in a supergravity field [26,27]. The supergravity field is pro-
vided by a centrifugal force produced by a centrifugal apparatus.
The differing melting points of metals and alloys within waste
computer PCBs (CPCBs) enable their selective separation by super-
gravity. In this study, supergravity technology was used for separa-
tion and recovery of Sn, Pb, Zn, and Cu from CPCBs at different
temperatures. A flow chart of the various steps for separating met-
als from granulated CPCBs is given in Fig. 1. The main objective of
the present study was to recover valuable or strategic metals from
complex waste electrical and electronic equipment by integrating
fundamental physical principles with the aim of minimized
environmental effects, lower energy consumption, and improved
recovery efficiency. Fig. 2. CPCBs used in the experiments.
542 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550

Fig. 3. Schematic diagram of centrifugal separation apparatus.

Fig. 4. SEM mappings of CPCB particles.

 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550 543

2.3. Experimental procedures

As shown in Fig. 3, a 36 g sample of CPCB particles was placed

into a set of graphite crucibles of inner diameter 19 mm. The bot-
tom of the upper graphite crucible included small holes (1 mm),
through which materials passed in the liquid phases. Graphite felt
(thickness 3 mm) was laid at the bottom of the upper crucible to
retain small solid particles. Similarly, graphite felt (thickness
5 mm) was laid on the CPCB particles to avoid oxidization during
the separation process. When the graphite crucible was heated to
the preset temperature, the centrifugal device was rotated at a
specified angular velocity. After a specific time, the device was shut
off, and the lower graphite crucible was removed and rapidly
quenched in water. The separation residues (1#CPCB residues) in
the upper graphite crucible were then re-heated, separated, and
quenched in water again. Finally, the separation resides (2#CPCB
residues) were again heated, separated and quenched in water.

Fig. 5. XRD pattern of CPCB particles.

(Fig. 3). The temperature was controlled by a programmed con-

troller with an R type thermocouple with an error of ±3 °C. Based
on the different melting points of metals, Pb, Sn, Cu, and Zn were
separated and recovered from CPCBs in a supergravity field. The
gravitational field was determined by the gravity coefficient.
The gravity coefficient (G) was calculated as the ratio of super
gravitational acceleration to normal gravitational acceleration via
Eq. (1) [28].
rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
 ffi
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi 2
N 2 p2 R
g 2 þ ðx2 RÞ
2 g2 þ 900
G¼ ¼ : ð1Þ
g g
where x is the angular velocity (rad/s); N is the rotating speed of
the centrifugal (rev/min); R is the distance from the centrifugal axis
to the center of sample (m), in the experiment, R = 0.25 m; and g is
Fig. 7. TG and DTA curves of CPCBs.
normal gravitational acceleration.

Fig. 6. Mineral liberation mapping of CPCB particles (a: SEM of CPCBs; b: MLA of CPCBs.)

Table 1
The chemical composition of the CPCBs.

Element Cu Sn Zn Fe Pb Al Mn Ni Ag Au Pd
Content/wt% 52.36 10.31 11.48 3.38 5.01 1.01 0.13 0.15 1.24  102 4.4  103 6.5  104
544 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550

2.4. Characterization the X-ray diffraction pattern of CPCB particles. The main peaks
were Cu, Zn, and Cu-Zn alloy, and other peaks were primary metals
The CPCB particles were characterized by scanning electron such as Pb and Sn. Al was mainly present in the form of Al2O3. The
microscope and energy disperse spectrum (SEM/EDS, MLA 250, results were consistent with those of SEM mappings.
FEI Quanta, USA), X-ray diffraction (XRD, Smartlab, Rigaku Corpo- The metals contained in electronic waste are mainly in the form
ration, Japan), mineral liberation analysis (MLA, MLA 250, FEI of the elemental metal and various alloys. Mineral liberation anal-
Quanta, USA), and inductively coupled plasma-optical emission ysis of the CPCB particles is shown in Fig. 6. The results reflect the
spectroscopy (ICP-OES, Optima 7000DV, Perkin Elmer, USA). distribution of various phases in raw materials. As shown, Cu, Sn,
The products collected in the lower graphite crucible in this CuZn, CuZnPb, SnPb, Al, and precious metal phases were identified
process were sectioned longitudinally along the center axis. One as the different major mineral phases. Cu and its alloys are mainly
part was characterized by XRD and SEM/EDS. In order to achieve derived from wires and fillers. Sn, Pb, and their alloys mostly derive
the chemical composition of different alloys obtained by super-
gravity separation, the other part of alloys were dissolved by acid
leaching and analyzed by ICP-OES.
The recovery value (Ri) of Pb, Sn, Zn and Cu was calculated by
Eq. (2).
mi
Ri ¼  100% ð2Þ
mC  xi
where mi is the mass of Pb, Sn, Zn or Cu that is separated from
CPCBs (g); mC is the mass of CPCBs; xi is the mass fraction of Pb,
Sn, Zn or Cu in the CPCBs.

3. Results and discussion

3.1. Characterization of CPCB particles

The CPCB particles were characterized by scanning electron

microscope and energy disperse spectrum, and the results are
shown in Fig. 4. From the surface distribution diagram, it can be
seen that Cu, Zn, Pb, Sn were the main elements contained in the
CPCB granules. Cu, Zn, Pb, and Sn were exited in their elemental
states and in the form of Cu-Zn and Pb-Sn alloys. Fig. 5 shows Fig. 9. XRD pattern of the first separation product.

Fig. 8. Vertical profiles of samples obtained by supergravity separation compared with parallel sample (a: G = 1, T = 400 °C, t = 10 min; b: G = 600, T = 400 °C, t = 10 min).
 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550
from solders. Precious metals are frequently used as contact mate-
rials, for electroplating, and/or as connectors. Specifically, Ag is
used in contacts, switches, and solders; Au as a bonding wire, con-
tacts, and in integrated circuits; Pd in multilayer capacitors and
connectors; and Pt in computer hard disks, for proton exchange
membrane fuel cells, and in thermocouples [29]. Additionally, a
proportion of Al was in the form of Al2O3. The phase compositions
of CPCB particles were mainly metals or alloys with a small propor-
tion of metal oxides. The chemical compositions of the major met-
als were analyzed by inductively coupled plasma-optical emission
spectroscopy; combined with the analysis in Fig. 6, the correspond-
ing results are shown in Table 1.
3.2. Thermal gravimetric and differential thermal analysis of CPCB
particles
Thermal gravimetric (TG) and differential thermal analysis
(DTA) were used to determine the appropriate temperature ranges
for selective separation of metals or alloys from the CPCB particles.
It was implemented at a flow rate of 100 mL/min in nitrogen atmo-
sphere with a heating rate of 10 °C/min from 25 °C to 1200 °C. As
shown in Fig. 7, the thermal behavior of the CPCBs revealed two
weight-loss steps with a total weight loss of 16.95%. The first
weight loss (approximately 0.77%) was attributed to the elimina-
tion of adsorbed water. The second weight loss occurred at temper-
ature >830 °C, and was attributed to the pyrolysis of organic
materials and the volatilization of Zn (above 907 °C).
The DTA data show an endothermic peak at 183 °C, indicating
the initial melting temperature of Pb-Sn alloy. This result was con-
Fig. 10. Micrographs and energy spectrums of Pb-Sn alloy obtained by supergravity separation at G = 600, T = 400 °C, t = 10 min (a: SEM of Pb-Sn alloy; b, c, and d: EDS of
point 1, 2, and 3 in the SEM, respectively).
545
sistent with the Pb-Sn binary alloy phase diagram [30]. Combined
with binary alloy phase diagrams for Sn-Cu and Zn-Cu [31–33], the
endothermic peaks at 774 °C, 903 °C, and 995 °C were attributed to
Sn-Cu solid solution (I), Sn-Cu solid solution (II), and Cu-Zn solid
solution, respectively.
From Fig. 6, it can be seen that the CPCBs included Pb-Sn, Cu-Zn
phases; in addition, Sn and Cu easily formed Sn-Cu alloy at high
temperature during the separation process. Based on the different
melting points of the alloys of Pb-Sn, Sn-Cu, and Cu-Zn, in order to
separate them gradually, the separation temperature was higher
than the melting point. However, the traditional physical separa-
tion method was not effective. Supergravity, as a way of strength-
ening mass transfer, can separate different metals or alloys
gradually at different temperatures. In the supergravity field, mol-
ten metal and alloys were quickly separated from solid particles by
solid–liquid separation. In this study, the CPCB particles were
heated incrementally to more than the melting point of Cu, and
metals or alloys were selectively separated at different tempera-
ture stages. Therefore, Pb-Sn alloy was recovered at temperatures
<400 °C, then Sn-Cu alloy was recycled at temperatures of 400–
900 °C, and finally, Cu-Zn alloy was separated above 900 °C.
3.3. Separation of Pb and Sn
Pb and Sn, which have low melting points, are the main compo-
nents of solder and the essential elements in the CPCBs. Pb and Sn
were the first phases to be separated from CPCBs. During the sep-
aration process, the effects of gravity coefficient (G), temperature
(T), and separation time (t) were investigated. Fig. 8 shows the ver-
546 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550
tical profiles of samples obtained by supergravity separation and
normal gravity separation. Supergravity separation was conducted
under conditions of G = 600, T = 400 °C, t = 10 min (Fig. 8a), while
the normal gravity separation process used G = 1, T = 400 °C,
t = 10 min (Fig. 8b). Obviously, Compared with normal gravity sep-
aration, supergravity separation can separate the sample quickly.
In the first separation process, the recovery values of Pb and Sn
were 38.07% and 32.36%, respectively.
The XRD pattern of the first separation product (see Fig. 9)
shows that the diffraction peaks were mostly Pb and Sn. In order
to further study the microstructure of Pb-Sn alloy, the sample
was characterized by SEM and EDS (Fig. 10). Pb and Sn were uni-
formly distributed and no macrosegregation was observed in the
sample in Fig. 10(a). From Fig. 10(b–d), the gray (point 1), gray-
white (point 2) and black (point 3) parts in Fig. 10(a) were Sn,
Pb, and Al2O3, respectively. Al2O3 was the principal impurity in
the Pb-Sn alloy. In this separation process, the (Pb + Sn)% and mass
ratio (Pb/Sn) of Pb-Sn alloy were 94.84% and 0.55, respectively.
This Pb-Sn alloy can yield raw materials for the preparation of sol-
ders and ornaments.
3.4. Separation of Sn and Cu
After the first supergravity separation process, the 1#CPCB resi-
dues were heated and separated. In the first separation process, the
main reason for the low recovery value of Sn was the formation of
Fig. 11. Vertical profile of product by supergravity separation.
solid solution of Sn and Cu. Therefore, the second separation pro-
cess continued the separation and recovery of Sn and Cu. The sec-
ond supergravity separation process was conducted at G = 800,
T = 800 °C, t = 5 min. The vertical profile and XRD pattern of the
resulting products are shown in Figs. 11 and 12. The results sug-
gested that the diffraction peaks were Sn-Cu, Cu-Zn, and Pb.
According to the phase diagram of binary Cu-Sn alloy, it is easy
to form intermetallic compounds between 600 and 800 °C [31].
Because of the good wetting ability between solder and Cu, solder
spread on the Cu particles. Sn of liquid solder diffused into Cu par-
ticles. Cu-Sn intermetallics were formed on the surface of copper
particles. In the second separation process, the recovery values of
Sn and Cu were 30.01% and 19.42%, respectively.
Fig. 13 shows the SEM mappings of Sn-Cu alloy obtained by
supergravity separation. The results indicated that Sn and Cu were
uniformly distributed, and no macrosegregation was observed in
the sample. The deep-gray (point 1) and gray (point 2) parts were
Sn-Cu alloy with differing Cu contents (as shown in Table 2), and
the black (point 3) and white (point 4) parts were SiO2 and Pb,
respectively. In the Sn-Cu alloy, the mass fractions of Sn and Cu
were 17.96% and 67.22%, respectively, and those of Pb and Zn were
6.38% and 5.94%, respectively. This Sn-Cu alloy can be used in the
manufacture of bearings, worm gears, gears, etc.
3.5. Separation of Cu and Zn
Cu and Zn elements are abundant in CPCB particles and have
high economic rate. The Zn content of the CPCB particles was more
than that of zinc ones. Based on the previous two separation pro-
cesses, the 2#CPCB residues were heated and the Cu-Zn alloy
was separated and recovered at 900–1200 °C. Figs. 14 and 15 show
the vertical profiles and XRD patterns of the products obtained by
supergravity separation at G = 1000, T = 1200 °C, t = 5 min. The
results show that the supergravity method successfully separated
and recovered most of the Cu content of the CPCB residues. The
XRD results show diffraction peaks for Cu-Zn, Cu-Sn, Fe-Zn, and
Pb. According to the phase diagram of binary Cu-Zn alloy, the
Cu-Zn solid solution is easy to form when the temperature exceeds
1000 °C.
Gravity coefficient played an important role in the separation
process. A series of separation experiments was carried out by
varying the gravity coefficient from 100 to 1000. Fig. 16 shows
the effect of gravity coefficient on the recovery of Cu and Zn in
the third separation experiments (temperature 1200 °C, holding
Fig. 12. XRD pattern of the second separation product.
 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550 547

time 30 min, centrifugal time 5 min). With increase in gravity coef- To further study the microstructure of Cu-Zn alloy, the sample
ficient from 100 to 1000, Cu recovery increased from 47.75% to was characterized by SEM and EDS (Fig. 17). Cu and Zn were uni-
78.48% and Zn recovery increased from 48.73% to 76.48%. formly distributed, and no macrosegregation was observed. It is

Fig. 13. SEM mappings of Sn-Cu alloy by supergravity separation at G = 800, T = 800 °C, t = 5 min (a: SEM of Sn-Cu alloy; b, c, d, and e: distribution of Cu, Sn, Pb, and Zn in the
SEM of Sn-Cu alloy, respectively).
548 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550
Table 2
Elemental compositions (wt%) at the points marked in Fig. 13.
Point No. Cu Sn Pb Si
1 91.06 8.94
2 79.05 20.95
3 20.37 54.75
4 100
Fig. 14. Vertical profile of product obtained by supergravity separation at G = 1000,
T = 1200 °C, t = 5 min.
observed that the gray (point 1), white (point 2), and black (point
3) parts were Cu-Zn, Sn-Cu, and Fe, respectively. The elemental
compositions at the points are shown in Table 3. In this separation
process, the mass fractions of Cu and Zn in the Cu-Zn alloy were
74.29% and 10.44%, while those of Pb, Sn, and Fe were 2.77%,
5.30%, and 3.52%, respectively. This Cu-Zn alloy can be used in
the manufacture of sheet, strip, and casting parts. After three step
separation processes, the total recovery values of Pb, Sn, Zn, and Cu
were 96.37%, 92.32%, 93.71%, and 97.90%, respectively.
3.6. Concentration of precious metals
After the third separation process, most metals were separated
and recovered, leaving behind precious metals (e.g., Au, Ag, and Pd)
and those with high melting points (e.g., Fe, Ni, and Mn) in the final
(3#CPCB) residues. These residues have high economic value.
Table 4 shows the chemical composition of precious metals
extracted from the 3#CPCB residues at G = 1000, T = 1200 °C,
t = 5 min. Compared with Table 1, Au, Ag, and Pd in the 3#CPCB
O
24.88
Fig. 15. XRD pattern of the third separation product.
Fig. 16. Effect of gravity coefficient on rates of Cu and Zn recovery.
residues were concentrated to 150 ppm, 550 ppm, and 12 ppm,
respectively. These concentrated precious metals will be fed into
available precious metals treatment processes for recovery [34].
3.7. Development of a clean separation process for waste PCBs
recovery
On the basis of the above results, a process to separate and
recover Pb, Sn, Zn, Cu, and to concentrate precious metals was pro-
posed. A flow chart of the separation and concentration of metals
from CPCB particles is given in Fig. 1. Under certain conditions,
based on the differing melting points of metals, three separation
processes were conducted with CPCB particles and alloys of Pb-
Sn, Sn-Cu, and Cu-Zn were obtained in the different stages. The
final separation residues were concentrated precious metals.
Throughout the separation process, the waste gases produced by
burning organic matter were collected and treated by a tail gas col-
lecting and processing device. By a combination of appropriate
hydrometallurgical process and supergravity separation of metals
or alloys, this process can achieve closed-loop recycling of elec-
tronic waste with significant efficiency. The method can improve
the grade of metals, and greatly improve the technical, economic
 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550 549

Fig. 17. SEM mappings of Cu-Zn alloy obtained by supergravity separation at G = 1000, T = 1200 °C, t = 5 min (a: SEM of Cu-Zn alloy; b, c, d, e and f: distribution of Cu, Sn, Pb,
Zn and Fe in the SEM of Cu-Zn alloy, respectively).

and environmental benefits of subsequent purification treatment. ciency, short flow, clean, and environmentally friendly. The super-
The method can realize the gradual recovery of Pb, Sn, Cu, Zn gravity separation process is believed to contribute significantly to
and the concentration of precious metals. The process is high effi- the physical processing of complex electronic waste.
550 L. Meng et al. / Chemical Engineering Journal 326 (2017) 540–550

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