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Recycling metals from wastes: a novel application of mechanochemistry Quanyin Tan, and Jinhui Li Environ. Sci. Technol., Just Accepted Manuscript • DOI: 10.1021/es506016w • Publication Date (Web): 17 Apr 2015 Downloaded from http://pubs.acs.org on May 3, 2015
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Recycling metals from wastes: a novel application of mechanochemistry
1
2 3
Quanyin Tan a, Jinhui Li a, *
4
a
5
Environment, Tsinghua University, Beijing, 100084, China
6
Address:
7
Quanyin Tan: Room 813, Sino-Italian Environmental and Energy-efficient Building,
8
School of Environment, Tsinghua University, Haidian District, Beijing 100084, China
9
(
[email protected])
State Key Joint Laboratory of Environment Simulation and Pollution Control, School of
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Jinhui Li: Room 805, Sino-Italian Environmental and Energy-efficient Building, School
11
of Environment, Tsinghua University, Haidian District, Beijing 100084, China
12
(
[email protected])
13 14
*Corresponding
author:
[email protected] (Tel:
+86-10-6279
15
+86-10-6277 2048, Address: Room 805, Sino-Italian Environmental and Energy-efficient
16
Building, School of Environment, Tsinghua University, Haidian District, Beijing 100084,
17
China)
18 19
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Fax:
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Recycling metals from wastes: a novel application of mechanochemistry
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Abstract
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Recycling metals from wastes is essential to a resource-efficient economy, and increasing
23
attention from researchers has been devoted to this process in recent years, with emphasis on
24
mechanochemistry technology. The mechanochemical method can make technically feasible the
25
recycling of metals from some specific wastes, such as cathode ray tube (CRT) funnel glass and
26
tungsten carbide waste, while significantly improving recycling efficiency. Particle size
27
reduction, specific surface area increase, crystalline structure decomposition and bond breakage
28
have been identified as the main processes occurring during the mechanochemical operations in
29
the studies. The activation energy required decreases and reaction activity increases, after these
30
changes with activation progress. This study presents an overall review of the applications of
31
mechanochemistry to metal recycling from wastes. The reaction mechanisms, equipment used,
32
method procedures, and optimized operating parameters of each case, as well as methods
33
enhancing the activation process are discussed in detail. The issues to be addressed and
34
perspectives on the future development of mechanochemistry applied for metal recycling are also
35
presented.
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Key Words
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Mechanochemistry, metal, recycling, activation, wastes
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1 Introduction
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Mechanochemistry is a branch of chemistry, which the widely accepted definition of it is
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proposed by Heinicke in 1984 1, 2. It focuses on the chemical and physicochemical changes during
44
aggregation, induced by the effects of mechanical energy. The processes providing the mechanical
45
energy for mechanochemistry include milling, grinding, scratching, polishing, shearing, and rapid
46
friction
47
connected to new developments in milling technology and equipment. Typically, the equipment
48
used for mechanical activation includes the retschmill, tumbling mill, stirring ball mill, vibration
49
mill, pin mill, rolling mill, and planetary ball mill.
3, 4
. Equipment plays the key role in mechanochemistry, whose progress is closely
50
Recent innovative procedures in mechanochemistry are more environmentally friendly, and
51
include many advantages when compared with traditional technological procedures. For example,
52
the number of technological stages in the milling process has been decreased by excluding
53
operations involving the use of solvents and gases 5, simplifying the process and making it
54
possible to obtain metastable products that are difficult or even impossible to obtain with
55
conventional methods 6.
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Mechanochemistry has been well established in chemistry and material science 7. Various
57
processes take place during the mechanochemical procedure, such as the comminution of particles
58
to small size, the generation of new surfaces, point defects and dislocations in crystalline structure,
59
and polymorphic transformations8-10. Some chemical reactions, including decomposition,
60
oxidation-reduction, ionic exchange, and complex and adduct formation, will occur as well
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Two similar terms—mechanical activation (MA) and mechanochemical activation (MCA)—are
62
frequently used in mechanochemistry depending on the effect caused during the activation
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.
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operation. MA involves an increase in the reactivity of target substances 7, while MCA refers to
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the accumulation of defects (amorphization process), the formation of polymorphs and the
65
occurrence of chemical reactions 13. Mechanochemistry has been applied in a wide range of fields,
66
such as chemical engineering, materials engineering, mineral processing, the coal industry, the
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building industry, pharmacy, agriculture, and extractive metallurgy 14. The field of waste treatment
68
has also benefited from mechanochemistry, for instance, removing organic pollutants from the soil,
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waste rubber recycling and fly ash modification 15, 16.
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Metal recycling is an essential component of the goal of closed-loop material systems and
71
sustainability17. Although the recycling rate for the "base metals" (iron, aluminum, zinc, copper
72
etc.) is above 50%; it is less than 1% for the “rare” metals used for precise technological purposes
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in small quantities, such as indium, lithium, and rare earth elements
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more difficult to separate out. In recent decades, intensive efforts and research have been devoted
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to recycling metals from wastes, such as spent lithium-ion batteries (LIBs)
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tube (CRT) glass 21, waste fluorescent lamps (FLs) 22, catalysts 23, and magnets 24.
18, 19
. These metals are also
20
, scrap cathode ray
Hydrometallurgy is one of the commonly used approaches for metal recycling25,
77
26
, and
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mechanochemistry has demonstrated the ability to significantly modify and enhance that process
79
27
80
hardly be leached out from wastes. It also can improve the leaching efficiency and enhance the
81
yield of the original process. It changes the technical route that the wastes have been treated
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through the introduction of new reactions to obtain a better recycling performance for metals. For
83
instance, lead in waste CRT glass could hardly be leached out (90% Pb: 99%, Zr & Ti: >90%, La: about 60%
2.8%
planetary
41
86%
CRT funnel glass
RE Es
1 M H2SO4, room temperature, 1h 1 M H2SO4, room temperature, 1h 1 M H2SO4, room temperature, 1h 1 M H2SO4, room temperature, 1h --
1.2%
planetary stirring
Sourc e
90-95% 10-15% 80% 97-98% (indium pellet)
CRT funnel glass planetary
Leaching condition c
94
21,
29,
46, 47
28
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WM, water, L/S: 10, 2h WM, 10% HCl, L/S: 10, 2h
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51% 44%
10% HCl, L/S: 10 -48%
planetary
phosphors
planetary
DM, 2h WM, water, L/S: 10, 2h WM, 7% H2SO4, L/S: 5, 2h DM, 2h
waste phosphors planetary
DM, 3 times (in mass) of NaOH, 5h
7% H2SO4, L/S: 5 7% H2SO4, L/S: 5 7% H2SO4, L/S: 5
62% 70% 59% Y: about 100%; Eu, La, Ce and Tb: > 80% Y: about 100%, Eu: > 90% Ce, La and Tb: >95%
1 M HCl, L/S: 50, ambient temperature, 1h 3 M H2SO4, L/S: 20, 50 ℃, 4h 3 M H2SO4, L/S: 20, 50 ℃, 4h
Co: 35%, Li: 70% Co: >90%, Li: about 100%
1 M HCl, L/S: 100, ambient temperature, 2h
76
Co: 0, Li: about 60% Co: >90%, Li: about 100%
water, L/S: 250, ambient temperature, 1h
77, 78
64
71
electrode scrap from LIS battery
planetary
LiCo2 powder
planetary
W
WC tool waste
planetary
DM DM, 2 times (in mass) of KMnO4, 15 min
W: 25% W: 100%
1 M NaOH, L/S: 20, ambient temperature, 1h
81, 82
Cu
waste PCBs
planetary
DM, 0.5 times (in mass) of S powder, 20 min
88.0%
3 M H2SO4, 30 wt% H2O2, L/L/S: 15:15:1, ambient temperature, 1h
91
Au
gold-containing waste
Co & Li
577 578
DM, 0.5 times (in mass) of quartz powder, 4h DM, 30h DM, equal-molar ratio of PVC, 30h
78% stirring
WM, water, L/S: 4, 1h WM, acid thiourea solution, L/S: 4, 1h
98% 99%
a
acid thiourea solution (as mentioned above), L/S: 40; 2h (unactivated), 1.5h (activated in water), 1h (activated in thiourea)
DM – dry milling, WM – wet milling; the time refers to time for milling; b the values in “italics” are the yields of original (unactivated) samples; c “--” means no leaching operation was needed; L/S refers to the liquid-to-solid ratio in mL/g; the time refers to the leaching time.
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The structural decomposition resulting from the milling process makes it easier for the leachant
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to attack the metals, as in the decomposition of CRT funnel glass, ceramic, and ITO containing
582
cullet. The yield of Pb from CRT funnel glass increased from a negligible 1.2-2.8% to a more than
583
92%, Ti and Zr yields from ceramic increased from 50-60% to more than 90%.
584
Meanwhile, the external energy added by the activation can also lead to bond breakage and
585
even chemical reaction, which could significantly improve the dissolution and/or leaching
586
properties and raise the leaching efficiency of the target metal. For instance, it was confirmed that
587
the Pb-O bond in CRT glass could be broken during activation, and the LiCoO2 in batteries and
588
the WC in tungsten carbide waste could be transformed to easily leachable LiCl, CoCl2 and
589
K2WO4. The reduction in particle size and the increase in specific surface area could also enhance
590
the leaching of metals with the progress of activation. These physical and chemical changes after
591
activation indicate a decrease in activation energy and an increase in reaction activity, making the
592
extraction more likely to occur, in less time.
593
The milling operations can also be enhanced with the addition of hard particles as grinding aids, 41
or quartz
76
594
such as Al2O3
. Some solid reactions could be introduced to assist the recycling
595
process through dry milling operations with reagents, such as the reduction of indium by Li3N 43,
596
oxidation of tungsten by KMnO4
597
target metals can also be partially or totally extracted from waste simultaneously with a wet
598
milling process, which is designed to carry out the activation and leaching in one step, and can
599
achieve the advantages of saving time and simplifying the procedure.
81, 82
, and transformation of copper by sulfur
89
. What is more,
600
Obvious improvements of recycling metals in wastes by mechanochemical methods have been
601
validated via practices from the perspective of recycling efficiency. Herein, a brief energy balance
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and economic assessment is conducted to have an insight to the application of mechanochemistry
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to metal recycling from waste from other perspectives, taking the study by Ou and Li91 as a
604
specific case. The detailed methodology and data used are presented in the Supporting Information.
605
According the energy balance, no more than 44.2% of the electricity consumed during the milling
606
process can be effectively used for introducing the reaction, most of the external energy is
607
transformed into heat, mechanical energy of equipment etc. A revenue of approximately 43.44
608
CNY (49.27 CNY after further optimization) can be obtained from the copper sulfate recovered
609
(for recycling 1 kg enriched samples). This value can cover the cost (39.67 CNY) of this approach
610
when the cost of the capital equipment, transporting, or labor etc., is not counted. At the same time,
611
the cost also can be reduced through improvements on the energy efficiency and materials
612
consumption when the scale is expanded.
613
There are still some theoretical issues waiting for further investigation before its industrial
614
application. The efficiency of mechanical and mechanochemical activation obtained in studies
615
may need further improvement. It is time- and energy-consuming to determine experimentally the
616
optimum conditions for mechanochemical processes in practical application, using pilot projects
617
and then implementing them on a wide scale in industrial plants.
618
The planetary ball mill is the most often used apparatus in the studies. It can generate a
619
relatively higher energy density, producing high mechanical and mechanochemical activation in a
620
relatively short milling time 101. The pot mill and stirring mill apparatus are the other two types of
621
mills used in the studies. However, proper milling apparatus that can generate sufficient rotational
622
speed, impact energy essentially, for industrial applications should be developed, considering the
623
control of other process parameters, such as temperature and atmosphere.
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Application of mechanochemical methods to recycling metals from various wastes is still
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conducted at the lab scale. More attention needs to be devoted to addressing the difficulty of
626
scalability of the mechanochemical operation, as well as predicting the relevant energy
627
consumption and outcomes. After that, mechanochemistry technology can be expected to
628
significantly contribute and broaden its application to the recycling of metals from wastes, and
629
benefits the environment and society.
630
Acknowledgments
631
This study is financially supported by the National Nature Science Foundation of China
632
(21177069) and is also supported by the National Key Technologies R&D Program (NO.
633
2014BAC03B04). We would also like to thank Dr. Xianlai Zeng and Dr. Qingbin Song for their
634
valuable advices. The authors are also very grateful to Brenda Lopez for reviewing the grammar
635
of the manuscript.
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