Facile Intercalation of Organic Molecules into Hydrotalcites by Liquid-Assisted Grinding: Yield Optimization by a Chemometric Approach

The liquid-assisted grinding (LAG) method was employed for the preparation of low cost, stable, and efficient functional materials, based on organic molecules intercalated into hydrotalcite (LDH). LAG is here exploited to produce hybrid materials with facile preparation methods, low solvent consumption, short reaction times, and high yields, and to allow an easy scale up of the synthesis to industrial production. Six molecules were tested to assess potentialities and limitations of LAG. The experiments showed a significant sensitivity to the molecular nature of the intercalant, resulting in different final yields and also different physical forms of the products (powdery vs pasty materials). With 2-naphtalenesulfonic acid (2-NSA), where the standard recipe gives a yield of about 50%, experimental procedures were optimized by design of experiment (DoE) and simplex chemometric techniques to find the optimal intercalation conditions, reaching 76% of yield. A chemometric-driven strategy with wide applicability in material chemistry for high throughput screening and preparation of intercalated compounds is thus proposed.