The isomerization of limonene over natural the zeolite, clinoptilolite, was studied. The main products of limonene isomerization were terpinolene, α-terpinene, γ-terpinene and p-cymene. These products have numerous applications in the cosmetic, food and pharmaceutical industries. The main parameters affecting limonene isomerization were reaction time, temperature and catalyst content. These parameters varied within the following ranges: reaction time 15–1440 min; temperature 155–175°C; and catalyst content 5–15 wt.%. Terpinolene was obtained after reaction for 60 min at 175°C using 10 wt.% catalyst. p-Cymene was produced using similar conditions as for terpinolene except for a longer reaction time of 1440 min. The use of optimum experimental conditions allowed the greatest amounts of the desired products to be obtained in the shortest time.

In the current study, the isomerization of geraniol over a natural sepiolite as a catalyst was investigated and optimized. Prior to application in the isomerization process, the physical and chemical properties of sepiolite were characterized using a battery of instrumental techniques, including XRD, nitrogen adsorption at 77 K, SEM, EDXRF, UV-Vis and FT-IR. Results indicated that geraniol isomerization is very complicated due to the large number of reactions taking place. The catalytic studies showed that the main reaction products were β-pinene, ocimenes, linalool, nerol, citrals, thunbergol and isocembrol; all chemical products with commercial applications. The quantity of each of these products depended on the temperature, catalyst content and reaction time employed in the isomerization process. During the current study, these parameters were varied in a step-wise approach over the ranges 80-150 °C (temperature), 5-15 wt% catalyst content and reaction time of 15-1440 min. As linalool is one of the most commercially important reaction products, the geraniol isomerization method was studied to identify conditions producing the highest selectivity for this compound. The most beneficial conditions for geraniol conversion and linalool formation were established as a temperature of 120 °C, catalyst content of 10 wt% and a reaction time of 3 h.

This work presents studies on the activity of the Ti-SBA-16 (SBA—Santa Barbara Amorphous) catalyst in the isomerization of limonene and S-carvone. The Ti-SBA-16 catalyst was synthesized by a two-step method: first, the SBA-16 material was produced, and then it was impregnated with the titanium source. The Ti-SBA-16 catalyst was subjected to detailed characterizations by means of instrumental methods: XRD (X-ray Diffraction), UV-Vis (Ultraviolet–Visible) spectroscopy, FTIR (Fourier-Transform Infrared) spectroscopy, SEM (Scanning Electron Microscopy) with EDX (Energy Dispersive X-ray) spectroscopy, and EDXRF (Energy Dispersive X-ray Fluorescence). Both limonene and S-carvone underwent isomerization over the Ti-SBA-16 catalyst. In the isomerization of limonene, the main product was terpinolene, and its highest yield amounted to 39 mol% after 300 min at 170 °C with a catalyst content of 15 wt%. Under these conditions, the conversion of limonene reached 78 mol%. In contrast, the highest yield of carvacrol (65 mol%) was obtained with the catalyst content of 15 wt%, at 200 °C, and with the conversion of S-carvone reaching 79 mol%.

Sepiolite and the sepiolite-based materials were studied in terms of carbon dioxide adsorption. The pore structure and the surface characterization of the obtained materials were specified based on adsorption-desorption isotherms of nitrogen measured at –196oC and carbon dioxide at 0oC. The specific surface area (SSA) was calculated according to the BET equation. The pore volume was estimated using the DFT method. Pristine sepiolite has shown the following value of SSA and CO2 uptake at 0oC – 105 m2/g and 0.27 mmol/g, respectively. The highest value of these parameters was found for material obtained by KOH activation of mixture sepiolite and molasses (MSEP2) – 676 m2/g and 1.49 mmol/g. Sample MSEP2 also indicated the highest value of total pore volume and micropores volume with a diameter up to 0.8 nm.

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