Recycling Zinc and Preparing High-Value-Added Nanozinc Oxide

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Recycling zinc and preparing high-value-added nanozinc oxide from waste zinc-manganese batteries by high temperature evaporation-separation and oxygen control oxidation Lu Zhan, Ouyang Li, Zhengyu Wang, and Bing Xie ACS Sustainable Chem. Eng., Just Accepted Manuscript • DOI: 10.1021/acssuschemeng.8b02430 • Publication Date (Web): 30 Jul 2018 Downloaded from http://pubs.acs.org on July 30, 2018

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ACS Sustainable Chemistry & Engineering

Recycling zinc and preparing high-value-added nano-zinc oxide from waste zinc-manganese batteries by high temperature evaporation-separation and oxygen control oxidation Lu Zhan∗ a,b, Ouyang Li a, Zhengyu Wang a, Bing Xie a,b a Shanghai Key Lab for Urban Ecological Processes and Eco-Restoration, School of Ecological and Environmental Science, East China Normal University, 500 Dongchuan Road, Shanghai 200241, China b Shanghai Institute of Pollution Control and Ecological Security, 1515 North Zhongshan Road, Shanghai 200092, China

ABSTRACT: In this work, zinc was recycled and nano-zinc oxide with high added values was prepared from waste zinc-manganese batteries by high temperature evaporation-separation and oxygen control oxidation. Air was used as both the oxidant and carrier gas. Due to the relatively fast oxidation rate of zinc, this paper attempts to balance the evaporation rate and oxidation rate of zinc by adding foreign materials to contend for the oxygen or covering the zinc with porous materials to isolate the oxygen. The results showed that the oxidation rate was still fast and the effect of contending for the oxygen by adding carbon powder or lead powder was not satisfied. The zinc hull were oxidized fast in the crucible and mixed with other oxides together, while covering the porous material (wire mesh, fiber felt) can accomplish the purpose of oxygen controlling. Zinc can be evaporated and separated from the zinc hull and oxidized during the zinc evaporation process, which is benefit for producing pure nano-zinc oxides. Under the experimental condition of 1123K heating temperature, 3kPa air pressure and blowing air at 723K, using fiber mat to cover zinc hull, the recovery efficiency of zinc is about 98.99% and the uniform morphology of tetrapod-shaped nano-zinc oxide was prepared successfully. This study provides a novel and environmentally-friendly method for the resource utilization of zinc from waste zinc-manganese batteries. KEYWORDS: Waste zinc-manganese batteries; Vacuum; Evaporation-separation; Corresponding

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Oxygen control oxidization; Nano-ZnO particles INTRODUCTION It is estimated that there are more than 60 billion zinc-manganese batteries produced each year in the world.1,2 The production of batteries consumes large amounts of mineral resources every year.3 For China, a country devoid of mineral resource, there were 15 billion zinc-manganese batteries produced in 2002. If the waste of 500,000 t waste batteries in China can be recovered and utilized, it can recover 110,000t of Mn, 7000t of Zn, 14000t of Cu.4 Zinc is one of the main components of zinc-manganese battery. Guo et al. reported that more than 300,000 tons of zinc were used in zinc based batteries manufacturing in 2003 and the number increased to 535,000 tons in 2005 in China.5 Quantities of waste zinc-manganese batteries with highly containing zinc are considerable

secondary resources of zinc. Although the

mercury-free or

mercury-micro of zinc-manganese battery is realized basically , the presence of zinc, manganese and waste alkali still caused pollutions to the environment, especially water and soil, and posed a serious threat to human health. Muyssen’s studies show that high concentrations of zinc may block the body's absorption of calcium, resulting in in the loss of calcium. 6 Scholars in the world have proposed many technical processes of recycling zinc from waste batteries, which can be divided into hydrometallurgy and pyrometallurgy.7 In the case of hydrometallurgy process, different acidic solutions were used to dissolve metals, then the leaching solutions were electrodeposited or precipitated to recover different metals.8-12 However, various chemicals are heavily consumed and it is easy to cause secondary pollution because of the discharged wastewater. Some researchers focused on bio-hydrometallurgy (bioleaching) which requires no industrial acids in leaching process.13 But the bioleaching processes are time consuming. Pyrometallurgy recycling method can be divided into normal pressure metallurgy and vacuum metallurgy according to the different pressure of system. There are many reports on normal pressure metallurgy. 2


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However, this method

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should be equipped with state-of-art tail gas treatment equipment, which is usually expensive. Burcak Ebin et al. have adopted vacuum metallurgy to recycle zinc and manganese from waste batteries, but it was not used for preparing nano-ZnO.15 Recently, researchers are paying more and more attention to vacuum metallurgy recycling because of its environmentally friendly benefits.16-21 Due to the lower boiling points of metals under vacuum, recycling of metals by vacuum metallurgy consumes less energy compared with traditional pyrometallurgy methods.22,23 Zinc oxide is a kind of new wide band gap semiconductor materials with fine performance and high excitation energy. It is widely used in ceramics, piezoelectric sensors and luminescent devices.24 Nano-zinc oxide as a new type of functional materials, shows attractive application prospect in the light absorption, sensitive, catalytic and other features.25 Studying the reclamation of zinc-manganese waste battery by preparing a new type of multifunctional inorganic material (nano-zinc oxide) is not only conducive to reducing environmental pollution and improving the living environment, but also conforms to the idea of sustainable development. In general, high values of the resource index indicate that the waste is important to the economy and has significant potential as are source.26 Herein, we propose a simple but effective procedure to separate zinc and prepare nano-zinc oxide with high added values from waste zinc-manganese batteries by high temperature evaporation-separation and oxygen control oxidation. Air was used as both the oxidant and carrier gas. Different oxygen controlling methods including chemical method and physic method were explored, and the operation parameters influencing the morphology of the final products were studied. It is hoped that this work can provide a theoretical foundation for zinc recycling with high added values from waste zinc-manganese batteries.

MATERIALS AND METHODS Apparatus. In this study, a self-designed vacuum furnace system was used for all experiments, and it was described in details in literature.27 Briefly, the system was 3



consisted of four sections: gas supply, tube furnace, water cooling jacket and vacuum pump team. The tube furnace had three heating zone which could be respectively heated to different temperatures with the maximum temperature of 1273 K. A quartz tube (Φ10×150 cm) was placed in the middle of the furnace which connected with an inlet valve and a water cooling jacket through vacuum flanges. Plug made of Al2O3 was placed at the heating chamber to prevent heat diffusion. With a hole in the middle of the plug, zinc vapor and air could pass through it into the condensation chamber. Methods. The carbon stick, copper cap, zinc hull and MnO2&electrolyte were separated from the collected waste zinc-manganese batteries by hand. The zinc hull as material was loaded with a corundum crucible. Then the crucible was placed in the first heating zone, while the second and third zones were used as the condensation chamber. A silicon steel sheet fixed by wire was positioned in the condensation area to collect the prepared nano-zinc oxides. The recovery efficiency and purity of zinc were studied respectively under different conditions. Recovery efficiencies of the target element were calculated by the following equation: R=

M 0 − M1 × 100% M0

Where M0 and M1 is the content of target element in the input and residual materials respectively. When the system was sealed with vacuum flanges, the vacuum pump team was started. As the Fig.1 shown, it needs about 80 mins to attain to the final temperature (above 1000 K) in this study. During the process of the temperature increasing (a, b in Figure 1), the air used as both the oxidant and carrier gas was pumped into the quartz tube through the inlet valve at different heating time. And this time was named as ventilated time and the corresponding temperature was named ventilated temperature. After that, the first zone was heated continually to a final heating temperature and maintained for a desired residence time (b, c in Figure 1), and then cooled eventually (c, d in Figure 1). The experimental flow chart is shown in Figure 2. 4


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Figure 1. The process of the heating time and temperature

Figure 2. The experimental process (upper) and schematic diagram (lower) Analysis. When the furnace cooled down, the nanoparticles produced in the condensation area are collected first in a dry environment. The weight of the samples in the crucible was measured before and after the experiment. Then the recovery efficiency of zinc under different experimental conditions was calculated. The morphology and element of the as-prepared products saved in the dry environment was observed by Scanning Electron Microscope (SEM, S-4800, HITACHI, Japan). The phase was characterized by X-Ray Diffraction (XRD-6100, SHIMADZU, Japan) for further analysis. 5



RESULTS AND DISCUSSION Preliminary Experiments. In preliminary experiments, we first blew air at 1123K and maintained 1KPa air pressure, at this condition which is concluded by literatures28-31 zinc can evaporate absolutely from the zinc hull completely. But as the results shown in Figure 3(a), a film of ZnO were observed in the condensation zone because the evaporation rate of zinc was too quick and the air did not duly disperse the zinc vapor. So in the second experiment, we blew air at about 673K when heating the zone for about 40 mins (half of the heating time), and then heated up to 1123K to maintained 1KPa air pressure. There was no film of ZnO prepared. Due to the low evaporation rate of zinc and fast oxidation rate, zinc was oxidized quickly inside the crucible mixing with other impurities oxides together as shown in Figure 3(b). In this work, we tried to slow down the oxidation rate of zinc by adopting chemical or physical methods separately, with the aim of slowly oxidizing the zinc and simultaneously dispersing the zinc vapor during the evaporation process. The final purpose is to obtain nano-zinc oxides with a high purity in the condensation chamber. In particular, the chemical methods include adding carbon or lead powder to contend for the oxygen, and the physical methods include wrapping the crucible with barbed wire or fiber felt to isolate the oxygen.

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Figure 3. (a) the film of ZnO; (b) white zinc oxides and other oxides; (c) white zinc oxides and carbon mixtures in the crucible; (d) white zinc oxides and lead oxides after reaction; (e) pollution caused by the evaporation of lead

Oxygen Control by Chemical Method Carbon Powder Additive. Considering that the chemistry of carbon is more active, it can compete with zinc for contending for oxygen. So the carbon powder was used to cover the zinc surface. The experimental condition of blowing air at 673K, maintaining 1kPa air pressure and heating up to 1123K were concluded by preliminary experiments. But after the experiment, there are few nanometer powders in the condensation area. The zinc was directly oxidized in the crucible without evaporation, and an amount of white zinc oxide generated in the crucible was mixed with unreacted carbon powder, as shown in Figure 3(c). So the zinc oxide cannot be recycled directly and the purity was low. It is speculated that the carbon powder is solid with high melting and boiling point, so the gas-solid reaction between carbon and oxygen is slow. The result is that the oxygen concentration is hard to decrease while the oxidation rate of zinc is still very fast. Lead Powder Additive. Because of the slow oxidation rate between carbon and oxygen, a substance with low melting point and high boiling point was considered to cover the zinc hull so that the oxygen can be contended and the oxidation rate can be 7



slowed down. Under the condition of blowing air at 673K, maintaining 1kPa air pressure and heating up to 1123K, the melting point of lead is lower than the boiling point of zinc, and its boiling point is much higher than that of zinc. At the same time, the melting point of lead is lower than that of zinc so it can melt first and reacted with the oxygen in the air. It means that lead may have the effect of contending for the oxygen and could be chose as the additive. However, under the above conditions, zinc was hardly evaporated nor separated from the hull because the zinc vapor was unable to break through the barrier of the lead oxides generated above the zinc hull. And as shown in Figure 3(d), only a few white zinc oxides were prepared on the surface of the crucible, while some blue-yellow oxides were prepared inside the crucible. Additionally, some lead was also evaporated during this process and polluted the condensation area, as shown in Figure 3(e). Although the added lead powder covering zinc has a certain effect on contending for the oxygen, the capture oxygen ability of lead is still weaker than zinc. Zinc was still oxidized in situ place and mixed up with lead oxide. Additionally, the zinc vapor cannot easily pass through the lead oxides generated above the zinc hull, the zinc oxides were still not generated and collected in the condensation area.

Oxygen Control by Physical Method The experiments above show that using the chemical additive like carbon or lead powder is not satisfied to slow down the oxidation rate of zinc. It is suspected that physical barriers may be used to slow down the oxidation rate of zinc by reducing the amount of oxygen contacting with zinc. Barrier of Barbed Wire. Given that the dense barbed wire (Figure 4a) has a certain isolation effect, so using the wire to cover on the surface of the crucible is practicable. Under this assumption, different aperture-size barbed wires (200mesh, 400mesh, 450mesh and 500mesh) were tested and the experimental condition was the same as the above. From the experimental results, with the number of mesh increasing, the barbed wire becomes denser and the phenomenon of in situ oxidation disappeared 8


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eventually. The recovery efficiency of the zinc shell was higher. As shown in Figure 5(left), the recovery efficiency was 75.61%, 81.79%, 85.63% and 87.60%. It can be concluded that 500-mesh barbed wire is denser and plays a role of isolation. After the optimum condition of aperture-size was obtained, three experiments under different pressures of ventilated air were carried out. The aim is to obtain a better condition of pressure which can disperse the zinc vapor uniformly and carry the zinc vapor to the condensation area. As shown in Figure 5(right), with the increase of pressure, the recovery efficiency firstly increased and then decreased, from 82.19% at 1kPa, 90.65% at 3kPa to 87.60% at 10kPa.

Figure 4. (a) barbed wire; (b) zinc oxides at 10kPa; (c) residual impurity at 3kPa

When the pressure is too low, the carrier gas is small and the flow rate is slow. The zinc vapor cannot be carried to the condensation area in time and be oxidized in situ, which decreased the recovery efficiency. When the pressure is too high, the oxygen partial pressure is higher and the oxidation rate is faster. Zinc vapor was also oxidized exactly inside the crucible. Based on this, comparing the condition of 3kPa with 10kPa, the recovery efficiencies of zinc hull were similar. But more zinc oxides were prepared inside the crucible at 10kPa (Figure 4b). The separation effect of zinc oxides was not obvious. However, there was only some residual impurity in the crucible at 3kPa (Figure 4c), so the condition of 3kPa is better.

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Figure 5. The recovery efficiency of zinc under different aperture-size barbed wires (left); the recovery efficiency of zinc under different pressure (right)

Barrier of Fiber Felt. The metal component of the barbed wire is easy to react with zinc. And the barbed wire is not dense enough; zinc vapor can still break through and react with oxygen quickly. The denser and more stable fiber felt (its chemical composition is silicon dioxide) is considered, which is not easy to react with the zinc. Figure 6(a) shows that the fiber felt is dense enough and has a suitable aperture for making zinc vapor escape. Before formal experiments, the blank experiment of fiber felt was done under the same experimental conditions. It drew a conclusion that there was almost no change in appearance and only some tiny holes of the fiber felt which did not affect the purity of nano-zinc oxide.

Figure 6. (a) SEM image of fiber felt; the crucible before (b) and after (c) reaction 10


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Using fiber felt to wrapped the crucible (Figure 6b), under the condition concluded by previous studies of blowing air at 673K, 1123K heating temperature, 3kPa air pressure, zinc hull was reacted completely. There were only Pb, Mn, Fe oxides and other impurities remained inside the crucible after experiment as shown in Figure 6(c). At the same time, there are also many nano-zinc oxides collected in the silicon steel sheet. It indicated that the fiber felt played a better role in balancing the oxidation and evaporation rate of zinc. After determining the effective blocking effect of fiber felt, the experiments of ventilated temperature were carried out to find a better time when the air is blew. If the ventilated temperature is low, zinc would react in situ and the recovery efficiency is low because of the large oxygen concentration. If the ventilated temperature is high, a film of ZnO would be prepared. Based on the analysis of preliminary experiments, three temperatures were chose. As shown in Figure 7, the recovery efficiency was 76.14% at 623K, 76.40% at 673K and 90.94% at 723K. It can be seen that the recovery efficiency of zinc hull has increased rapidly from 673K to 723K. And in the process of experiment, it was observed that the pressure in tube furnace raised obviously (zinc evaporated into vapor) and then declined (zinc vapor was oxidized) at 723K. Blowing air at this time, zinc vapor can escape from the crucible and nano-zinc oxides were collected in the condensation zone. The evaporation rate and oxidation rate of zinc was balanced. So 723K was a better ventilated temperature.

Figure 7. The recovery efficiency of zinc under different ventilated temperature 11



Characteristic of the Products Under the experimental condition of 1123K heating temperature, 3kPa air pressure and blowing air at 723K, using fiber mat to cover zinc hull, there are odorless nano-powders with pure white appearance prepared in condensation area. From the analysis of the powders, it can be elucidated that they were nano-zinc oxides as shown in Figure 8(a). The XRD diffraction peak of the zinc oxide whisker is sharp, it indicates that the product crystallization is complete and purity is high with no other impurities. From Figure 8(b), it can be seen that the nano-zinc oxide was crystallized. The whisker was well developed with few wafers and the crystal structure was perfect with slender needle body. As shown in Figure 9, the prepared whiskers have a tetrapod-shaped spatial structure. The diameter of the pin foot gradually decreases from the nucleus toward the tip. The length of pin foot is 450~550 nm and the average length of pinpoint is about 100 nm. The core diameter is approximately 80 nm. To sum up, the uniform morphology of tetrapod-shaped nano-zinc oxide with radiated growth was prepared successfully at the above conditions.

Figure 8. (a) XRD pattern of nano-zinc oxide; (b) SEM image of nano-zinc oxide

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Figure 9. SEM image of ZnO fiber

ACKNOWLEDGMENTS This work is partly supported by the National Natural Science Foundation of China (21677050), Shanghai Pujiang Program (17PJD013) and State Key Laboratory of Pollution Control and Resource Reuse Foundation (PCRRF16005). The authors are grateful to the reviewers who help us improve the paper by many pertinent comments and suggestions.

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This figure can be designated as Abstract Art of this manuscript (An environmentally-friendly method is proposed to prepare nano-ZnO particles from waste zinc-manganese batteries, which is beneficial for Zn sustainability)

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Recycling Zinc and Preparing High-Value-Added Nanozinc Oxide

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