Effect of pretreatment temperature on the surface modification of diatomite with trimethylchlorosilane

Diatomite samples from Costa Rica were purified using acidic treatments with hydrochloric acid, thermally treated (400–1000 °C) and then silylated with trimethylchlorosilane in toluene under inert atmosphere. The purification process allows to decrease the concentration of metals presented in the crude diatomite, as is confirmed by X-ray Fluorescence (XRF) Analysis. The silylated materials were analyzed by using Hyperpolarized ¹²⁹Xe Nuclear Magnetic Resonance Spectroscopy (HP ¹²⁹Xe NMR), Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA), rehydration tests, and contact angle measurements. XRD measurements indicate that diatomite is mainly amorphous, but presents several crystalline phases (kaolinite, cristobalite, and quartz). Pretreatments at high temperatures cause changes in those crystalline phases, resulting in more amorphous materials. However, there is no difference in the overall structure of purified and thermally treated diatomite samples with respect to the silylation products. In addition, SEM measurements show no effect over the pore structure of the materials. On the other hand, TGA measurements and rehydration tests show lower losses of water for silylated materials prepared using higher pretreatment temperatures. Moreover, HP ¹²⁹Xe NMR, FTIR, and contact angle measurements evidence a modification due to covalent attachment of Si(CH₃)₃-groups to the surface, which increases for higher pretreatment temperatures. The results provide valuable information about external factors that influence the surface modification of diatomite. This can be useful to control modifications that can be achieved in a similar way.