Unique Halloysite Nanotubes–Polyvinyl Alcohol–Polyvinylpyrrolidone Composite Complemented with Physico–Chemical Characterization

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Abstract
A halloysite nanotubes–polyvinyl alcohol–polyvinylpyrrolidone (HNTs–PVA–PVP) composite has been investigated for a quite long time aiming at improving the physico–chemical characterization of HNTs. In this work, HNTs–PVA–PVP composite were prepared based on a unique procedure characterized by crosslinking two polymers with HNTs. The composite of two polymers were modified by treating HNTs with phosphoric acid (H3PO4) and by using malonic acid (MA) as a crosslinker. The composite was also treated by adding the dispersion agent sodium dodecyl sulfate (SDS). The HNTs–PVA–PVP composite shows better characteristics regarding agglomeration when HNTs is treated in advance by H3PO4. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), brunauer–emmett–teller (BET), size distribution, and atomic force microscopy (AFM) are used to characterize the physio-chemical properties of the composite. FTIR shows additional peaks at 2924.29, 1455.7, and 682.4 cm−1 compared to the neat HNTs due to adding MA. Despite that, the XRD spectra do not show a significant difference, the decrease in peak intensity could be attributed to the addition of semi-crystalline PVA and the amorphous PVP. The images taken by TEM and FESEM show the possible effects of MA on the morphology and internal feature of HNTs–PVA–PVP composite treated by MA by showing the deformation of the matrix. The BET surface area increased to 121.1 m2/g compared to the neat HNTs at 59.1 m2/g. This result, the second highest recorded result, is considered a breakthrough in enhancing the properties of HNTs–PVA–PVP composite, and treatment by MA crosslinking may attribute to the size and the number of the pores. The results from these techniques clearly showed that a significant change has occurred for treated HNTs–PVA–PVP composite where MA was added. The characterization of HNTs–PVA–PVP composite with and without treating HNTs and using crosslinker may lead to a better understanding of this new composites as a precursor to possible applications in the dentistry field.

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