Abstract
A new purification method for molybdenum disulfide via NaNO3–HCl–HNO3 synergistic leaching at 80 °C was developed. The effects of the concentration of NaNO3, HCl, and HNO3, and liquid–solid ratio and the leaching time on the purification of molybdenum disulfide were investigated by orthogonal array design methodology. The results of Taguchi method utilizing L25 (55) orthogonal array indicated that the NaNO3 concentration had the greatest impact on the purification of molybdenum disulfide. The optimum conditions for the purification of molybdenum disulfide were as follow: concentration of NaNO3 = 2.5%, concentration of HCl = 11%, concentration of HNO3 = 1.0%, liquid–solid ratio = 3, and the leaching time = 10 h. Under optimum conditions, the content of molybdenum increased from 55.1 to 59%, and the contents of iron, copper, lead, and calcium decreased from 0.35 to 0.21%, 0.027 to 0.008%, 0.054 to < 0.005%, and 0.27 to 0.035%, respectively. Based on molecular formula of molybdenum disulfide, the content of molybdenum disulfide increased from 91.93 to 98.44%. XRD and SEM indicated that this method removed only the impurities and did not affect the phase and particle size of molybdenum disulfide. The results show that the new purification method avoids the roasting process and will achieve the “green” production. The new method based on orthogonal array is effective for the purification of molybdenum disulfide via acid leaching.
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References
Aydogan S, Aras A, Canbazoglu M (2005) Dissolution kinetics of sphalerite in acidic ferric chloride leaching. Chem Eng J 114:67–72. https://doi.org/10.1016/j.cej.2005.09.005
Dhanasekaran S, Gnanamoorthy R (2007) Dry sliding friction and wear characteristics of Fe–C–Cu alloy containing molybdenum disulphide. Mater Design 28:1135–1141. https://doi.org/10.1016/j.matdes.2006.01.030
Guo PM, Pang JM, Zhao P (2012) Preparation of ultra pure MoS2 powder. Nonferrous Metals (Extractive Metallurgy) 7:50–52. https://doi.org/10.3969/j.issn.1004-0536.2009.02.015
Huang CM, Wu SF, Sanchez AM, Peters JJP, Beanland R, Ross JS, Rivera P, Yao W, Cobden DH, Xu XD (2014) Lateral heterojunctions within monolayer MoSe2–WSe2 semiconductors. Nat Mater 13:1096–1101. https://doi.org/10.1038/nmat4064
Laursen AB, Kegnaes S, Dahl S, Chorkendorff I (2012) Molybdenum sulfides—efficient and viable materials for electro-and photoelectrocatalytic hydrogen evolution. Energy Environ Sci 5:5577–5591. https://doi.org/10.1039/C2EE02618J
Lee K, Kim HY, Lotya M, Coleman JN, Kim GT, Duesberg GS (2011) Electrical characteristics of molybdenum disulfide flakes produced by liquid exfoliation. Adv Mater 23:4178–4182. https://doi.org/10.1002/adma.201101013
Li DJ, Maiti UN, Lim J, Choi DS, Lee WJ, Oh Y, Lee GY, Kim SO (2014) Molybdenum sulfide/N-doped CNT forest hybrid catalysts for high-performance hydrogen evolution reaction. Nano Lett 14:1228–1233. https://doi.org/10.1021/nl404108a
Mondal S, Paul B, Kumar V, Singh DK, Chakravartty JK (2015) Parametric optimization for leaching of cobalt from Sukinda ore of lateritic origin-A Taguchi approach. Sep Purif Technol 156:827–834. https://doi.org/10.1016/j.seppur.2015.11.007
Praveena M, Jayaram V, Biswas SK (2012) Friction between a steel ball and a steel flat lubricated by MoS2 particles suspended in hexadecane at 150 °C. Ind Eng Chem Res 51:12321–12328. https://doi.org/10.1021/ie3011337
Safarzadeh MS, Moradkhani D, Ilkhchi MO, Golshan NH (2008) Determination of the optimum conditions for the leaching of Cd–Ni residues from electrolytic zinc plant using statistical design of experiments. Sep Purif Technol 58:367–376. https://doi.org/10.1016/j.seppur.2007.05.016
Shanmugam M, Durcan CA, Yu B (2012) Layered semiconductor molybdenum disulfide nanomembrane based Schottky-barrier solar cells. Nanoscale 4:7399–7405. https://doi.org/10.1039/C2NR32394J
Tedstone AA, Lewis DJ, Hao R, Mao SM, Bellon P, Averback RS, Warrens CP, West KR, Howard P, Gaemers S, Dillon SJ, Brien PO (2015) Mechanical properties of molybdenum disulfide and the effect of doping: an in situ TEM study. ACS Appl Mater Interfaces 7:20829–20834. https://doi.org/10.1021/acsami.5b06055
Wang X, Srinivasakannan C, Duan XH, Peng JH, Yang DJ, Ju SH (2013) Leaching kinetics of zinc residues augmented with ultrasound. Sep Purif Technol 115:66–72. https://doi.org/10.1016/j.seppur.2013.04.043
Yang J (2000) Preparation of high purity molybdenum disulfide. Nonferrous Metals 5:19–23. https://doi.org/10.3969/j.issn.1671-9492.2000.05.005
Yang WH, Tang YS (1998) Design optimization of cutting parameters for turning operations based on Taguchi method. J Mater Process Technol 84:122–129. https://doi.org/10.1016/S0924-0136(98)00079-X
Yin A, Wei X, Cao Y, Li H (2016) High-quality molybdenum disulfide nanosheets with 3d structure for electrochemical sensing. Appl Surf Sci 385:63–71. https://doi.org/10.1016/j.apsusc.2016.05.066v
Yu W (2009) Preparation technology and application of molybdenum disulfide. Rare Metals Cem Carbides. 37:55–57. https://doi.org/10.3969/j.issn.1004-0536.2009.02.015
Zong X, Yan HJ, Wu GP, Ma GJ, Wen FY, Wang L, Li C (2008) Enhancement of photocatalytic H2 evolution on CdS by loading MoS2 as cocatalyst under visible light irradiation. J Am Chem Soc 130:7176–7177. https://doi.org/10.1021/ja8007825
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The authors are grateful for the financial support from the National Natural Science Foundation (no. 51664037).
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Guo, D., Fu, L., Wang, S. et al. Application of Taguchi method for optimization of process parameters in preparation of high-purity molybdenum disulfide. Chem. Pap. 72, 2997–3003 (2018). https://doi.org/10.1007/s11696-018-0544-1
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DOI: https://doi.org/10.1007/s11696-018-0544-1