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Response surface statistical optimisation of zeolite-X/silica by hydrothermal synthesis

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Abstract

A hydrothermal alkaline synthesis of self-supporting zeolites from co-generation boiler sugar cane bagasse ash (SCBA) was measured by X-ray powder diffraction (XRD) scan yields (scan area percentages) method. A factorial design and a response surface statistical method were used to optimise the synthesis method. Temperature, NaOH concentration and aluminium/silica (Al/Si) ratio were determined to be the most influential factors in controlling zeolite-X yields, and these three variables were included in a response surface model (RSM) with a central composite design (CCD). The RSM model indicates that optimal zeolite-X formation conditions are 72.5 °C, 5 M NaOH and an Al/Si ratio of 3:5. The RSM/CCD matrix established an efficient statistical modelling of zeolite synthesis optimisation with the fewest possible number of experiments. Scanning electron microscopy examination shows that SCBA particles (20–100 µm) are covered with zeolite crystallites (0.3–0.8 µm in size) producing a self-supporting structure. XRD analyses show a dominance of zeolite-X (33.6%), with zeolite-A (4.7%), and an average Al/Si ratio of 4:5 that is close to published values. The Brunauer–Emmett–Teller (BET) apparent specific surface area measured 228 m2 g−1 (P/Po = 0.045), and ≈ 90% of the micro-porosity distribution is associated with ≈ 7 Å internal micropore, which is typical of zeolite-X. The self-supporting, composite nature and large effective grain size of the zeolites reported in this work opens a number of uses for the materials produced.

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Acknowledgements

The authors are grateful for the financial support, including a PhD scholarship for P. Doumit, provided by Sugar Research Australia (SRA; formally SRDC, Sugar Research Development Corporation) via the SRDC grant SCU03. Financial support was also provided by Australian Biorefining Pty. Ltd., as an industry partner to the SRDC grant SCU03. Many thanks are also extended to the staff and students at the School of Environment Science and Engineering, Southern Cross University, who assisted in the laboratory work for data collection.

Funding

This study was funded by SRDC Grant Number SCU03.

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Authors and Affiliations

  1. School of Environment Science and Engineering, Southern Cross University, PO Box 157, Lismore, NSW, 2480, Australia

    Philip Doumit, Malcolm W. Clark, Lachlan H. Yee & Andrew Rose

  2. Marine Ecology Research Centre, Southern Cross University, PO Box 157, Lismore, NSW, 2480, Australia

    Malcolm W. Clark & Lachlan H. Yee

  3. Southern Cross GeoScience, Southern Cross University, PO Box 157, Lismore, NSW, 2480, Australia

    Malcolm W. Clark & Andrew Rose

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  1. Philip Doumit
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Correspondence to Philip Doumit.

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Doumit, P., Clark, M.W., Yee, L.H. et al. Response surface statistical optimisation of zeolite-X/silica by hydrothermal synthesis. J Mater Sci 54, 14677–14689 (2019). https://doi.org/10.1007/s10853-019-03913-x

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