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Preparation of Organo-Montmorillonites and the Relationship Between Microstructure and Swellability
- Wei Hua Yu, Ting Ting Zhu, Dong Shen Tong, Min Wang, Qi Qi Wu, Chun Hui Zhou
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- Journal:
- Clays and Clay Minerals / Volume 65 / Issue 6 / December 2017
- Published online by Cambridge University Press:
- 01 January 2024, pp. 417-430
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Hydrophobicity, swellability, and dispersion are important properties for organo-montmorillonites (OMnt) and have yet to be fully characterized for all OMnt configurations. The purpose of the present work was to examine the preparation of OMnt from the reaction of Ca2+-montmorillonite (Ca2+-Mnt) with a high concentration of surfactant and to reveal the relevant properties of hydrophobicity and dispersion of the resultant OMnt. A series of OMnt samples were prepared using a small amount of water and cetyltrimethylammonium bromide (CTAB) with a concentration more than the CTAB critical micelle concentration (CMC). The relationship between OMnt microstructure and the hydrophobicity and swellability properties was investigated in detail. The resulting OMnt samples were characterized using powder X-ray diffraction patterns (XRD), Fourier-transform infrared (FTIR) spectroscopy, thermogravimetric and differential thermogravimetry (TG-DTG), water contact angle tests, swelling indices, and transmission electron microscopy (TEM). The addition of CTAB and water in the OMnt preparation affected the OMnt microstructure and properties. An increase in CTAB concentration led to a more ordered arrangement of cetyltrimethylammonium (CTA+) cations in the interlayer space of the OMnt and a large amount of CTA+ cations on the outer surfaces of the OMnt. The swelling indices and the water contact angles of OMnt samples depended on the distribution of the CTAB surfactant on OMnt and the orientation of the surfactant hydrophilic groups on the inner and on the outer surfaces of OMnt. A maximum swelling index of 39 mL/g in xylene was achieved with an average water contact angle of 62.0° ± 2.0° when the amount of CTAB added was 2 times the cation exchange capacity (CEC) of Mnt and the lowest water to dry Mnt mass ratio was 3 during the preparation of OMnt samples. The platelets of OMnt aggregated together in xylene by electrostatic attraction and by hydrophobic interactions.
Optimized purification procedure for Iranian calcium bentonite for producing montmorillonite nanosheets
- Fatemeh Ahmadi, Hajar Ghanbari, Faraz Shabani Moghaddam, Rahim Naghizadeh
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- Journal:
- Clay Minerals / Volume 57 / Issue 2 / June 2022
- Published online by Cambridge University Press:
- 27 October 2022, pp. 120-130
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In polymer composites, montmorillonite nanosheets are crucial as fire retardants, reinforcers, anti-corrosives, detoxifying agents and ultraviolet-protection agents. However, the quality of montmorillonite nanosheets can be improved by optimizing the raw bentonite purification process in which undesirable phases are removed. Optimization of Iranian calcium bentonite purification for nanomontmorillonite synthesis considering various parameters based on various physical approaches to dispersion and ultrasonication was investigated; the calcium bentonite purification was performed using sodium hexametaphosphate followed by either sedimentation or centrifugation, and the nanomontmorillonite synthesis was performed using ultrasonic treatment. The effects of suspension concentration, milling type, pH and centrifugation duration and speed on the separation of various impure phases were evaluated qualitatively and optimized. The raw and purified bentonite and the synthesized nanomontmorillonite were characterized using X-ray powder diffraction, X-ray fluorescence spectroscopy, Fourier-transform infrared spectroscopy and scanning electron microscopy. The cation-exchange capacity was also measured in the raw and purified samples. Optimal experimental conditions in the dispersed samples were achieved at a 2.5 wt.% concentration of bentonite suspension and planetary milling at pH 7. While the ultrasonic treatment was more effective than the dispersion approach for cristobalite elimination, a smaller lateral size of the montmorillonite sheets, optimized at 0.5 wt.% concentration of the suspension, was achieved. The increased cation-exchange capacity after the purification improved the exfoliation and delamination of montmorillonite nanosheets in the presence of cetyltrimethylammonium bromide as the surfactant. The interplanar spacing of (001) planes of 15 Å in raw bentonite shifted to 21 Å and 19 Å in purified and non-purified samples, respectively, after synthesis.