Integrated Process To Recover NiMH Battery Anode Alloy with

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An Integrated Process to Recover NiMH Battery Anode Alloy with Selective Leaching and Multi-stage Extraction Chuanying Liu, Yuefeng Deng, Ji Chen, Dan Zou, and Wenrou Su Ind. Eng. Chem. Res., Just Accepted Manuscript • DOI: 10.1021/acs.iecr.7b01427 • Publication Date (Web): 14 Jun 2017 Downloaded from http://pubs.acs.org on June 15, 2017

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Industrial & Engineering Chemistry Research

An Integrated Process to Recover NiMH Battery Anode Alloy with Selective Leaching and Multistage Extraction Chuanying Liu,†,‡ Yuefeng Deng,† Ji Chen,*,† Dan Zou,† and Wenrou Su†,‡

† State Key Laboratory of Rare Earth Resource Utilization, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences,Changchun, 130022, P. R. China

‡ University of Chinese Academy of Sciences, Beijing, 100039, P. R. China

KEYWORDS: NiMH Battery, Rare Earth Recovery, Selective Leaching, Multi-stages Extraction

ABSTRACT

Hydrometallurgy is a widely studied recovery process to recover NiMH battery, but the large chemical consumption restricted its application in industry. To achieve a low chemical consumption recovery process of NiMH battery anode alloy, an integrated process with selective leaching and multi-stage extraction was designed. In selective leaching, the leaching procedure was divided into four stages. The acid used could be reacted with the battery anode alloy totally except in the last stage. The metal components of the alloy have different reaction activities with acid, they were leached into liquor by the sequence: La>Pr>Nd>Ce>Al>Mn>Co>Ni. Hence, the selectivity of metals was achieved to make the following extraction much easier. The total chemical consumption was calculated by the ratio of UMAC/UMACmin and S, which in

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this integrated process was 60% less than in traditional recovery process. Through this recovery process, the recovery rate of rare earth elements (REEs) reached 90.5%, and the purity of REO product exceeded 99%. This integrated process was considered as a practical approach to recover the waste alloy.

INTRODUCTION Every year, million tons of electrical and electronic equipment containing critical metals like indium, cobalt, rare earth elements (REEs) has flowed into waste stream without proper management.1,2 With these metals inside, the electronic waste is regarded as a considerable secondary resource for the critical metals. Considering the positive environmental impact and potential economic benefits, the recovery of secondary resources has attracted widespread interest from researchers, industries, and policy makers. The NiMH battery is a noticeable secondary resource with high content of valuable metals (3-4% Co, 36-42% Ni, 8-10% REEs).3 During the past decades , the NiMH battery has a large reserve for the widely application in hybrid car and portable devices, but the total recovery rate of this battery was less than 1% until 2010.3,4 Much research in recent years has focused on applying hydrometallurgy in the NiMH battery recovery process.3,5 In a hydrometallurgy recovery process of NiMH-Battery, the battery is mechanically dismantled firstly to obtain the electrode materials (as shown in Scheme 1). Then the electrode materials were leached by mineral acids. The leachates can be separated by solvent extraction or precipitation to recover REEs, cobalt, nickel as oxide products. Compared with other recovery method like the pyrometallurgy route, the hydrometallurgy route has the following advantages: low energy cost, large flexibility, high selectivity, and high recovery yield of trace elements.1,3,6 Nevertheless, the large chemical consumptions and discharge of wastewater limit the application of this technique in the recovery of secondary resources.


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Scheme 1. The components of NiMH Battery: (a) four parts of NiMH battery; (b) the components of anode. The chemical consumption in hydrometallurgy recovery process is mainly concentrated in leaching and extraction procedure.7,8 It can be evaluated by two indicators, the unit mass acid consumption (UMAC) for leaching procedure and the amount of extracting solvent (S) for extraction procedure.8,9 The minimum amount of UMAC is defined to be the acid consumed by the stoichiometry of leaching equation exactly. The UMACmin in battery leaching can be calculated from eq 1 and eq 2.

UMAC, = ∑ ∙ (1)

UMAC, = 1/[

)/( )∙ ∑( )/( )∙!

∑(

+ 17] (2)

Where, ωi and Mi represent the mass fraction and molar mass of each metal in the electrodes. The ei is the stoichiometry of hydrogen ion reacted with anode or cathode materials according to the reaction equations in Meshram’s work10. The S is a dimensionless quantity which represents the largest amount of the molar flow rate of extractant when the molar flow rate of metal ions in the aqueous phase is 1 mol/min. This value can indicate the chemical consumptions for a given countercurrent extraction separation. The Smin can be calculated by the equation mentioned in the literature11. % =

&∙'(,) *'+,) ,'&,.

(3)

Where fA,a and fB,a represent the aqueous feed flow rates of A and B. The β and fo denotes to the separation factor and exiting flow rates of organic stream. With the normalization of UMAC, the chemical consumption (C) of leaching and extraction procedure was expressed as eq 4. /012

C = /012

∙ 1 + % (4)

34

The UMACmin of several leaching procedures were listed in Table 1. In most cases, the acid consumed in leaching exceeded the UMACmin more than double. This result not only caused the high chemical consumption in leaching procedure, but also influenced the following procedure by increasing the base


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required to neutralize the residue acid.12-14 For this reason, an integrated process with low leaching acid consumption would be a good solution for the battery recovery industry. Table 1. Summary of UMACmin and actual acid consumption in previous research works

UMACmin (mmol/g)

leaching acid

S/L ratio

UMAC (mmol/g)

mixed electrodes15

31.92

2M H2SO4

20

mixed electrodes16

19.11~29.36a

2M H2SO4

mixed electrodes17

19.84~26.78a

mixed electrodes12

Materials

Leaching efficiency (%) REEs

Co

Ni

80

96

100

97

20

80

83.06

92.31

82.59

2M+1M H2SO4

6.67

40

100

100

99

15.62~26.46a

12M HCl

6.67

80

-

-

-

anode powder6

30.82

20% HCl

10

64.66

95.16

-

-

mixed electrodes10

18.58~31.57a

2M H2SO4

10

40

90.2

97.8

91.6

a: These data are in a range because the ratio between anode and cathode material has not been mentioned in this works. To recover the NiMH battery anode alloy with low chemical consumption, an integrated process composed of selective leaching and multi-stage extraction was introduced in this work. The mass integration is a concept widely applied in process optimization.18,19 This concept was introduced to build the interaction between leaching and extraction. Selective leaching refers to the selective removal of one element from an alloy by corrosion processes. In selective leaching, the separation among elements can be achieved while the environmental impacts can be minimized.20-22 The multi-stage extraction is the main technique in REEs separation industry. The 2-ethylhexyl phosphoric acid mono (2-ethylhexyl) ester (P507) was selected as extractant for its high selectivity, high extractability and good physical–chemical phenomena in REEs and Co/Ni separation.23-25 This study applied sulfuric acid to selectively leach the battery anode alloy; then the leachates were separated by P507; at last, the REO product was obtained by precipitation. EXPERIMENTAL SECTION Reagent and Apparatus


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The Ni-MH batteries used in this work were provided by Baotou Research Institute of Rare Earths. The extractant, 2-ethylhexyl phosphoric acid mono (2-ethylhexyl) ester (P507) (>93.0% purity), was supplied by Luoyang Aoda Chemical Co., Ltd. It was diluted with kerosene and was saponified by NaOH before the multistage extraction. Stock solutions of REEs were prepared by dissolving their oxides (>99.9%) into concentrated sulfuric acid. Stock solutions of Co, Ni, Mn, and Al were prepared by dissolving their sulfate (>99.9%). All the other chemicals were of analytical grade. The pH values were measured by a model PHS-3C pH meter. The metal concentrations were determined by inductively coupled plasma optical emission spectrometers (ICPOES, Thermo iCAP 6000). The structure of anode alloy was determined by X-ray diffraction (XRD) analysis on a Bruker AXS D8 Advance Powder X-ray diffractometer (using Cu Kα radiation: λ=1.5418 Å). Pretreatment The NiMH battery was treated by the Mantuano’s method14 to obtain and characterize the anode alloy. Several NiMH batteries were dismantled manually, and the anode alloy was scraped from the supporting metal-mesh. Then all the alloy scraps were washed by deionized water and ethanol, dried in oven for 24h at 60℃, grinded in agate mortar and sieved. With these treatment, the anode alloy powders with particle size фNd>Ce>Al>Mn>Co>Ni,31 which is in consistent with the experiment data in Figures 2a and 3a. The Se values which were calculated by eq 10 and listed in the Supporting Information (SI) Table S2 also indicated that in stage one, the leaching has positive selectivity towards REEs (SeL1,REEs=2.13) and Mn (SeL1,Mn=2.56), almost no selectivity towards Co (SeL1,Co=1), and negative selectivity towards Ni (SeL1,Ni=0.19). As the reaction proceeded, the elements inside the alloy could hardly contact the Ni2+, and the balance was reached at about 60 min. In stage 2, as shown in Figure 3b, the mass fraction of all elements remained constant after five minutes, and the values were similar to the beginning of reaction in stage 1. The main reaction in this stage was between H+ and metals. The displacement between metals was not observed because the Ni reduced and precipitated in the alloy surface in stage 1 prevented other active metals from replacing the Ni2+ in liquor. This can be verified by Table S2. The SeL2 values of all metals except Al were close to 1, indicating that almost no selectivity among these metals. As most of the active metals, REEs and Mn, were dissolved in the first two stages, it can be inferred that the leaching process in stage 3 and 4 were similar to stage 2.


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Figure 3. Effect of reaction time on the elemental composition of leaching: (a) stage 1; (b) stage 2 ([H2SO4]=0.75mol/L, S/L=3:16, T=40℃, particle size: Al>Mn>Co>Ni. Over 95% of La was extracted when pH=2, while the extractions of Co and Ni have not begun until pH=2.5. The slopes of log(D) versus log(H) of each metal are demonstrated in Figure 4b. They are -2.7, -5.6, -2.0,-2.0, -1.8 for La, Al, Mn, Co, Ni. This result indicates that the extractions are cation exchange process during the experiment acidity range.23


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Figure 4. Effect of acid concentration on extraction of single elements ([P507]=1.31mol/L, [La3+]=1.21×102

mol/L, [Co2+]=1.09×10-2mol/L, [Ni2+]=0.98×10-2mol/L. [Mn2+]=1.07×10-2mol/L. [Al3+]=1.03×10-2mol/L, O/A=1:1,

T=25℃, t=30 min). The β values are calculated according to the extraction data by eq 8. The βLa/Al is 170 (pH=1.6); βLa/Mn is 1300 (pH=2); βMn/Co is 22; βCo/Ni is 6.6. These values imply that the REEs can be separated from other metals easily when pH≤2. The β values of Co/Ni and Co/Mn in the simulated bi-mixture are listed in Table 5. The mole ratio of metals in the mixed solution is consistent with that in the leachates. All the β values are in the range 6-9. This result suggests that the Co, Mn, Ni in the practical leachate can be separated by P507. Table 5. The values of βCo/Mn, βCo/Ni in bi-mixturea Co/Mn

Co/Mn

Co/Ni

Co/Ni


14

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pH

3.01

3.2

3.54

3.11

molar ratio

1.88

5.72

2.50

0.20

β

7.82

8.43

8.44

6.12

a: ([P507]=1.31mol/L, 30% saponified, O/A=1:2, T=25℃, t=30 min) Multi-stage extraction When extracting the practical leachates, a four-stage procedure was employed to separate REEs, Co and Ni. The elemental composition of raffinates was shown in Figure 5. Over 96% REEs with most Mn, Al and few Co, Ni were extracted into organic phase. The Co was mostly left in last two stages' raffinates. The mole ratio of Co/ Ni in R3 and R4 reached 2.7 and 0.17, which were suitable for the following separation. Most of the REEs and Mn left in raffinates were in R4. No Al was detected in all the four raffinates. As other metals had been extracted, the mass fractions of Ni in R1 and R2 both exceeded 98, which were suitable for producing high pure NiO.

Figure 5. Elemental composition of raffinate of each extraction stage ([P507]=1.31mol/L, 30% saponified, O/A=4:1, T=25℃, t=30 min). Stripping and precipitation Over 99% of the metal cations in loaded organic phase can be stripped by hydrochloric acid in just one stag. According to Fernandes’s work12, the REEs can be separated from other metal at low pH value by oxalic acid,


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thus no scrubbing was adopted in this process. After stripping, the REO was obtained through precipitation by oxalic acid and calcination. The elemental composition of the REO was exhibited in Table 6. The total recovery rate of REEs in the entire process was 90.5%, and the purity of REO product exceeded 99%. Table 6. Elemental composition of REO product

ω/%

REEs

Co

Mn

Al

Other metals

99.30

0.07

0.02

0.61

90%. The results of Taguchi method indicated, in


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one stage leaching, large amount of acid was necessary to ensure high leaching rate. In selective leaching, the amount of acid was reduced to 1.04 times of the UMACmin, and the total leaching efficiency of REEs, Co and Ni were 99%, 96%, and 93%. The metals were leached through dealloy mechanism by the sequence: REEs>Al>Mn>Co>Ni. Because the metals were pre-separated in selective leaching, the chemical consumed in extraction was also reduced. The total chemical consumption was less than 60% of the traditional recovery process. As the reduction in chemical consumption was achieved by establishing interaction between leaching and extraction procedure through selective leaching, this method could be applied on the recovery of other waste alloys containing different metals with small amount but critical value. Supporting Information L9 (34) Randomized Experimental Plan Table; Results of three-stage selective leaching; Results of five-stage selective leaching; The Se values of the four leaching stages AUTHOR INFORMATION Corresponding Author * Tel.: +86-431-85262646. Fax: +86-431-85262646. E-mail: [email protected]. Notes The authors declare no competing financial interest. ACKNOWLEDGMENTS This work was supported by the National Basic Research Program of China (Grant 2012CBA01202), the Natural Science Foundation of China (Grant 51174184), and the Science and Technology Planning Project of Baotou City (Grant 2012X2006) REFERENCES


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Table of Contents and Abstract Graphics


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Integrated Process To Recover NiMH Battery Anode Alloy with

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