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Study on the Purification Process of Waste Silicon Powder in the Synthesis Process of Organosilicon Monomer

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Abstract

Due to waste contact and waste slurry generated in the production process of silicone monomer after copper extraction of the residue (WSP), a significant accumulation leads to environmental pollution and waste of resources. Therefore, there is an urgent need to explore a suitable method to recover the silicon resources therein. In this study, the morphology and composition of WSP are systematically investigated, and the optimized method of removing impurities by combining low-temperature oxidative roasting and mixed acid leaching is proposed, by taking advantage of the low-temperature oxidizability of amorphous carbon as well as the corrosive effect of HF on the SiO2 layer. Carbon removal using oxidative roasting of WSP is analyzed, and the effects of different roasting temperatures and times on carbon removal are explored. The effects of HF concentration, acid leaching temperature, and time on the impurity leaching rate are studied. The results show that the removal of impure carbon is as high as 98.46% when roasted at 500 °C for 3 h in the atmosphere. The optimal conditions for mixed-acid leaching are as follows: HF concentration of 4 mol·L−1; leaching temperature of 70 °C; 2 h period. The removal rates of Cl, Ca, and Fe are superior to 99%, and the removal rates of Al and Ti are superior to 94%. This simple method is key for the recovery of silicon resources from WSP.

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References

  1. Komiyama T, Minami Y, Hiyama T (2017) Recent advances in transition-metal-catalyzed synthetic transformations of organosilicon reagents. ACS Catal 7:631–651. https://doi.org/10.1021/acscatal.6b02374

    Article  CAS  Google Scholar 

  2. Eduok U, Faye O, Szpunar J (2017) Recent developments and applications of protective silicone coatings: a review of PDMS functional materials. Prog Org Coat 111:124–163. https://doi.org/10.1016/j.porgcoat.2017.05.012

    Article  CAS  Google Scholar 

  3. Rochow EG (1945) The direct synthesis of organosilicon compounds. J Am Chem Soc 67:963–965. https://doi.org/10.1021/ja01222a026

    Article  CAS  Google Scholar 

  4. Hurd DT, Rochow EG (1945) On the mechanism of the reaction between methyl chloride and silicon-copper. J Am Chem Soc 67:1057–1059. https://doi.org/10.1021/ja01223a007

    Article  CAS  Google Scholar 

  5. Blaser E, Rosier C, Huet M et al (2022) Catalytic cracking of CH3Cl on copper-based phases. Catal Sci Technol 12:2006–2014. https://doi.org/10.1039/d1cy02226a

    Article  CAS  Google Scholar 

  6. Zhang Y, Ji YJ, Li J et al (2017) Hierarchical zinc-copper oxide hollow microspheres as active Rochow reaction catalysts: the formation and effect of charge transferable interfaces. J Catal 348:233–245. https://doi.org/10.1016/j.jcat.2017.02.030

    Article  CAS  Google Scholar 

  7. Zhang Y, Li J, Liu HZ et al (2019) Recent advances in Rochow-Müller process research: driving to molecular catalysis and to a more sustainable silicone industry. ChemCatChem 11:2757–2779. https://doi.org/10.1002/cctc.201900385

    Article  CAS  Google Scholar 

  8. Wessel TJ, Rethwisch DG (1996) Deactivation of CuSi and CuZnSnSi due to coke formation during the direct synthesis of methylchlorosilanes. J Catal 161:861–866. https://doi.org/10.1006/jcat.1996.0248

    Article  CAS  Google Scholar 

  9. Yu J, Zhan HH, Wang YH et al (2013) Graphite microspheres decorated with Si particles derived from waste solid of organosilane industry as high capacity anodes for Li-ion batteries. J Power Sources 228:112–119. https://doi.org/10.1016/j.jpowsour.2012.11.083

    Article  CAS  Google Scholar 

  10. Zhao LP, Li ZY, Xi FS et al (2023) Purification of organosilicon waste silicon powder with hydrometallurgy. Metals 13:950. https://doi.org/10.3390/met13050950

    Article  CAS  Google Scholar 

  11. Wang GJ, Ye ZP, Dong SH et al (2023) Harmless process of organic matter in organosilicon waste residue by fluidization-like DDBD reactor: temperature action and mechanism. Chemosphere 322:138116. https://doi.org/10.1016/j.chemosphere.2023.138116

    Article  CAS  PubMed  Google Scholar 

  12. Liu HZ, Ji YJ, Zhu YX et al (2018) Converting industrial waste contact masses into effective multicomponent copper-based catalysts for the Rochow process. Particuology 37:1–8. https://doi.org/10.1016/j.partic.2017.05.008

    Article  CAS  Google Scholar 

  13. Guo XL, Zhang ZY, Xing PF et al (2023) Kinetic mechanism of copper extraction from methylchlorosilane slurry residue using hydrogen peroxide as oxidant. Chin J Chem Eng 60:228–234. https://doi.org/10.1016/j.cjche.2023.02.007

    Article  Google Scholar 

  14. Li D, Zhu MT, Qiao JX et al (2023) Efficient extraction of copper from organosilicon waste contact and preparation of high purity copper. Trans Nonferrous Met Soc China. https://doi.org/10.11817/j.ysxb.1004.0609.2022-43730

  15. Shi L, Wang WK, Wang AB et al (2014) Facile synthesis of scalable pore-containing silicon/nitrogen-rich carbon composites from waste contact mass of organosilane industry as anode materials for lithium-ion batteries. J Mater Chem A 2:20213–20220. https://doi.org/10.1039/c4ta03561e

    Article  CAS  Google Scholar 

  16. Zhang ZL, Wang Y, Ren WF et al (2014) Scalable synthesis of interconnected porous silicon/carbon composites by the rochow reaction as high-performance anodes of lithium ion batteries. Angew Chem-Int Edit 126:5265–5269. https://doi.org/10.1002/ange.201310412

    Article  Google Scholar 

  17. Feng L, Shen YB, Gao L (2014) Comprehensive utilization of the spent silicon contact mass. New Chem Mater 42:226–228+237

  18. Xi FS, Li SY, Ma WH et al (2021) A review of hydrometallurgy techniques for the removal of impurities from metallurgical-grade silicon. Hydrometallurgy 201:105553. https://doi.org/10.1016/j.hydromet.2021.105553

  19. Holze R (2003) Electrochemistry of silicon and its oxides. J Solid State Electrochem 7:318–319. https://doi.org/10.1007/s10008-003-0371-2

    Article  CAS  Google Scholar 

  20. Yang SC, Wan XH, Wei KX et al (2020) Occurrence state and dissolution mechanism of metallic impurities in diamond wire saw silicon powder. ACS Sustain Chem Eng 8:12577–12587. https://doi.org/10.1021/acssuschemeng.0c03912

    Article  CAS  Google Scholar 

  21. Santos MFM, Fujiwara E, Schenkel EA et al (2015) Processing of quartz lumps rejected by silicon industry to obtain a raw material for silica glass. Int J Miner Process 135:65–70. https://doi.org/10.1016/j.minpro.2015.02.002

    Article  CAS  Google Scholar 

  22. Li XX, Li TH, Gao JX et al (2016) A novel “green” solvent to deeply purify quartz sand with high yields: a case study. J Ind Eng Chem 35:383–387. https://doi.org/10.1016/j.jiec.2016.01.018

    Article  CAS  Google Scholar 

  23. Popescu C-M, Broda M (2021) Interactions between different organosilicons and archaeological waterlogged wood evaluated by infrared spectroscopy. Forests 12:268. https://doi.org/10.3390/f12030268

    Article  Google Scholar 

  24. Yang HL, Liu IT, Liu CE et al (2019) Recycling and reuse of kerf-loss silicon from diamond wire sawing for photovoltaic industry. Waste Manage 84:204–210. https://doi.org/10.1016/j.wasman.2018.11.045

    Article  CAS  Google Scholar 

  25. Zhu YY, Wu JJ, Wei KX et al (2022) Recovery and purification of silicon from diamond wire saw wasted silicon powder by a technique of induction smelting followed by directional solidification. Metall Mater Trans B 53(4):2704–2711. https://doi.org/10.1007/s11663-022-02561-y

    Article  CAS  Google Scholar 

  26. Li L, Ge J, Chen RJ et al (2010) Environmental friendly leaching reagent for cobalt and lithium recovery from spent lithium-ion batteries. Waste Manage 30:2615–2621. https://doi.org/10.1016/j.wasman.2010.08.008

    Article  CAS  Google Scholar 

  27. Xin W, Srinivasakannan C, Xin-hui D et al (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

    Article  CAS  Google Scholar 

  28. Yang SC, Wan XH, Wei KX et al (2020) Dissolution and mineralization behavior of metallic impurity content in diamond wire saw silicon powder during acid leaching. J Clean Prod 248:119256. https://doi.org/10.1016/j.jclepro.2019.119256

    Article  CAS  Google Scholar 

  29. Zhang ZY, Guo XL, Wang YX et al (2023) Leaching kinetic mechanism of iron from the diamond wire saw silicon powder by HCl. Waste Manage 169:82–90. https://doi.org/10.1016/j.wasman.2023.06.028

    Article  CAS  Google Scholar 

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Acknowledgements

The authors wish to acknowledge the financial support on this research from the Talent Training Program of Yunnan of China (202005AC160041 and KKXY202252002), and the major R&D project of Yunnan of China (202202AG050012).

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Authors and Affiliations

  1. Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming, 650093, People’s Republic of China

    Xinyue Cai, Jijun Wu, Kuixian Wei & Wenhui Ma

  2. National Engineering Research Center of Vacuum Metallurgy, Kunming University of Science and Technology, Kunming, 650093, People’s Republic of China

    Xinyue Cai, Jijun Wu, Kuixian Wei & Wenhui Ma

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  1. Xinyue Cai
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  2. Jijun Wu
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Contributions

Xinyue Cai: Investigation, Experiment development, Data Integration, Writing-original draft. Jijun Wu: Conceptualization, Resources, Supervision, Funding acquisition, Project administration. Kuixian Wei: Supervision, Data curation. Wenhui Ma: Resources, Supervision, Provide ideas.

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Correspondence to Jijun Wu or Kuixian Wei.

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Cai, X., Wu, J., Wei, K. et al. Study on the Purification Process of Waste Silicon Powder in the Synthesis Process of Organosilicon Monomer. Silicon 16, 821–829 (2024). https://doi.org/10.1007/s12633-023-02720-z

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  • DOI: https://doi.org/10.1007/s12633-023-02720-z

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