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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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Environmental Science & Technology

Recycling metals from wastes: a novel application of mechanochemistry

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2 3

Quanyin Tan a, Jinhui Li a, *

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a

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Environment, Tsinghua University, Beijing, 100084, China

6

Address:

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Quanyin Tan: Room 813, Sino-Italian Environmental and Energy-efficient Building,

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School of Environment, Tsinghua University, Haidian District, Beijing 100084, China

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([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

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of Environment, Tsinghua University, Haidian District, Beijing 100084, China

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([email protected])

13 14

*Corresponding

author:

[email protected]

(Tel:

+86-10-6279

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+86-10-6277 2048, Address: Room 805, Sino-Italian Environmental and Energy-efficient

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Building, School of Environment, Tsinghua University, Haidian District, Beijing 100084,

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China)

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1 ACS Paragon Plus Environment

4143,

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

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attention from researchers has been devoted to this process in recent years, with emphasis on

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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

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tungsten carbide waste, while significantly improving recycling efficiency. Particle size

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reduction, specific surface area increase, crystalline structure decomposition and bond breakage

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have been identified as the main processes occurring during the mechanochemical operations in

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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

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mechanochemistry to metal recycling from wastes. The reaction mechanisms, equipment used,

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method procedures, and optimized operating parameters of each case, as well as methods

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enhancing the activation process are discussed in detail. The issues to be addressed and

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perspectives on the future development of mechanochemistry applied for metal recycling are also

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presented.


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36 37 38

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

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aggregation, induced by the effects of mechanical energy. The processes providing the mechanical

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energy for mechanochemistry include milling, grinding, scratching, polishing, shearing, and rapid

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friction

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connected to new developments in milling technology and equipment. Typically, the equipment

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used for mechanical activation includes the retschmill, tumbling mill, stirring ball mill, vibration

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mill, pin mill, rolling mill, and planetary ball mill.

3, 4

. Equipment plays the key role in mechanochemistry, whose progress is closely

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Recent innovative procedures in mechanochemistry are more environmentally friendly, and

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include many advantages when compared with traditional technological procedures. For example,

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the number of technological stages in the milling process has been decreased by excluding

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operations involving the use of solvents and gases 5, simplifying the process and making it

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possible to obtain metastable products that are difficult or even impossible to obtain with

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conventional methods 6.

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Mechanochemistry has been well established in chemistry and material science 7. Various

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processes take place during the mechanochemical procedure, such as the comminution of particles

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to small size, the generation of new surfaces, point defects and dislocations in crystalline structure,

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and polymorphic transformations8-10. Some chemical reactions, including decomposition,

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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

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frequently used in mechanochemistry depending on the effect caused during the activation


11, 12

.

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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

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occurrence of chemical reactions 13. Mechanochemistry has been applied in a wide range of fields,

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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

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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

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sustainability17. Although the recycling rate for the "base metals" (iron, aluminum, zinc, copper

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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

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hardly be leached out from wastes. It also can improve the leaching efficiency and enhance the

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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

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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

95


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

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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

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cullet. The yield of Pb from CRT funnel glass increased from a negligible 1.2-2.8% to a more than

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92%, Ti and Zr yields from ceramic increased from 50-60% to more than 90%.

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Meanwhile, the external energy added by the activation can also lead to bond breakage and

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even chemical reaction, which could significantly improve the dissolution and/or leaching

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properties and raise the leaching efficiency of the target metal. For instance, it was confirmed that

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the Pb-O bond in CRT glass could be broken during activation, and the LiCoO2 in batteries and

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the WC in tungsten carbide waste could be transformed to easily leachable LiCl, CoCl2 and

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K2WO4. The reduction in particle size and the increase in specific surface area could also enhance

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the leaching of metals with the progress of activation. These physical and chemical changes after

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activation indicate a decrease in activation energy and an increase in reaction activity, making the

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extraction more likely to occur, in less time.

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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,

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oxidation of tungsten by KMnO4

597

target metals can also be partially or totally extracted from waste simultaneously with a wet

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milling process, which is designed to carry out the activation and leaching in one step, and can

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achieve the advantages of saving time and simplifying the procedure.

81, 82

, and transformation of copper by sulfur

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. What is more,

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Obvious improvements of recycling metals in wastes by mechanochemical methods have been

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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

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specific case. The detailed methodology and data used are presented in the Supporting Information.

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According the energy balance, no more than 44.2% of the electricity consumed during the milling

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process can be effectively used for introducing the reaction, most of the external energy is

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transformed into heat, mechanical energy of equipment etc. A revenue of approximately 43.44

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CNY (49.27 CNY after further optimization) can be obtained from the copper sulfate recovered

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(for recycling 1 kg enriched samples). This value can cover the cost (39.67 CNY) of this approach

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when the cost of the capital equipment, transporting, or labor etc., is not counted. At the same time,

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the cost also can be reduced through improvements on the energy efficiency and materials

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consumption when the scale is expanded.

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There are still some theoretical issues waiting for further investigation before its industrial

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application. The efficiency of mechanical and mechanochemical activation obtained in studies

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may need further improvement. It is time- and energy-consuming to determine experimentally the

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optimum conditions for mechanochemical processes in practical application, using pilot projects

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and then implementing them on a wide scale in industrial plants.

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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

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relatively short milling time 101. The pot mill and stirring mill apparatus are the other two types of

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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

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scalability of the mechanochemical operation, as well as predicting the relevant energy

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consumption and outcomes. After that, mechanochemistry technology can be expected to

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significantly contribute and broaden its application to the recycling of metals from wastes, and

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benefits the environment and society.

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Acknowledgments

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This study is financially supported by the National Nature Science Foundation of China

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(21177069) and is also supported by the National Key Technologies R&D Program (NO.

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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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869


Page 46 of 51

Page 47 of 51

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