Raquel Trujillano

The mechanosynthesis by dry-milling and characterization of layered double hydroxides (LDH) containing Zn²⁺ in the layer and Cl⁻ as interlayer anion has been investigated. The solids were synthesized by mechanosynthesis, by means of a dry-milling method using a planetary mill. This kind of synthesis is totally ecological as the stoichiometric amounts of reactants have been used to obtain the original solids, so, there was no need for washing or calcination thus avoiding water or atmospheric contamination. To compare results and prove that Cl⁻ is the interlayer anion, a carbonate-LDH has been synthesized by the coprecipitation method. Original solids were calcined at 450 °C to obtain the oxides. Samples were fully characterized and used as catalysts in the paracetamol photodegradation to test the usefulness of these ecologically obtained solids as decontaminants. An assortment of techniques, such as XRD, FT-IR, TG-DTA, and N₂ adsorption–desorption isotherms, has been utilized to prove the goodness of the dry-mill method applied. The X-ray diffraction data and the FT-IR and thermal results confirmed that the samples synthesized were hydrotalcites with the Cl⁻ as the interlayer anion. The paracetamol photodegradation tests indicated that the dry milling procedure enhances the reaction.

Aluminum is the most used non–ferrous metal. It can be recycled saving several natural resources, but generates large amounts of residues with a complex composition—still containing a valuable amount of aluminum, although also including contaminant compounds. The laboratory-scale valorization of an industrial aluminum residue is here used as a powerful didactic resource in Inorganic and Analytical Chemistry and related fields such as Chemistry, Chemical Engineering, Environmental Engineering, Materials Engineering, and related university degrees, since concepts like acid-base properties (particularly amphoterism), redox reactions, speciation diagrams, or solubility–precipitation concepts are applied. The students are encouraged to look for information on the topic, to teamwork, and to elaborate a well-written laboratory report. At the same time, this laboratory work introduces them to advanced laboratory techniques and to incorporate concepts of Circular Economy and various Sustainable Development Goals, educating the students with respect to the environment. Although focused on University studies, this manuscript also contains excellent ideas for secondary teachers to motivate STEM vocations, particularly for Chemistry and Chemical and Environmental Engineering, and is also ideal for being included in the preparation of future Secondary School teachers.

Professor Vicente Rives developed a very long and fruitful career as a teacher of Inorganic Chemistry and Materials Chemistry and has been a dedicated researcher in these and related fields

Layered double hydroxides with the hydrotalcite-like structure, containing Mg²⁺, Al³⁺, and Fe³⁺ (with different Al/Fe ratios) in the layers, have been synthesized and fully characterized, as have the mixed oxides formed upon their calcination at 500 °C. Both series of solids (original and calcined ones) have been tested for methylene blue adsorption. In the case of the Fe-containing sample, oxidation of methylene blue takes place simultaneously with adsorption. For the calcined samples, their reconstruction to the hydrotalcite-like structure plays an important role in their adsorption ability.

Aluminum from saline slags generated during the recycling of this metal, extracted under reflux conditions with aqueous NaOH, was used in the synthesis of hydrocalumite-type solids with the formula Ca₂Al_1–mFe_m(OH)₆Cl·2H₂O. The characterization of the obtained solids was carried out by powder X-ray diffraction, infrared spectroscopy, thermal analysis, element chemical analysis, N₂ adsorption-desorption at −196 °C and electron microscopy. The results showed the formation of Layered Double Hydroxide-type compounds whose characteristics varied as the amount of incorporated Fe³⁺ increased. These solids were calcined at 400 °C and evaluated for the catalytic photodegradation of ibuprofen, showing promising results in the elimination of this drug by advanced oxidation processes. The CaAl photocatalyst (without Fe) showed the best performance under UV light for the photodegradation of ibuprofen.

Hydrotalcite is the name of a mineral discovered in Sweden in 1842 whose formula is Mg₆Al₂(OH)₁₆CO₃·4H₂O and presents a layered crystal structure that consists of positively charged hydroxide layers neutralized by interlayer anions as carbonate, also containing water molecules. The ease of their synthesis and the possibility of incorporating other layer cations and interlayer anions have made this type of layered double hydroxides (LDH) a group of very interesting materials for industry. In addition to LDH and due to the name of the most representative mineral, this group of compounds is commonly called hydrotalcite-like materials, or simply hydrotalcites. Another way of referring to them is as anionic clays because of their layered structure but, unlike classical clays, their layers are positive and their interlayers are anionic. The main fields of application of these solids comprise catalysis, catalyst support, anion scavengers, polymer stabilizers, drug carriers, or adsorbents. This paper briefly summarizes some of the work carried out by Professor Rives over more than thirty years, focused, among other topics, on the study of the synthesis, characterization, and applications of hydrotalcites. This research has led him to train many researchers, to collaborate with research groups around the world and to publish reference papers and books in this field. This contribution, written to be included in the Special Issue “A Themed Issue in Honor of Prof. Dr. Vicente Rives”, edited on the occasion of his retirement, only shows a small part of his scientific research and intends to value and recognize his cleverness and his enormous scientific and human quality.

Two titania photocatalysts have been prepared using the sol–gel method using TiCl₄ as a precursor, and two different alcohols, namely, ethanol or propanol (Et or Pr). The main aim of this work was to study the effect of the nature of the alcohol on the chemical, structural and photocatalytic properties for paracetamol photodegradation of the final solids. The TiCl₄/alcohol molar ratio to obtain the corresponding alkoxides (TiEt and TiPr) was 1/10. These alkoxides were calcined at 400 °C to prepare the oxide catalysts (named as TiEt400 and TiPr400). Powder X-ray diffraction (PXRD) of the original samples showed the presence of anatase diffraction peaks in sample TiPr, while TiEt is a completely amorphous material. Contrary to commercial TiO₂-P25, the PXRD diagrams of the calcined samples showed anatase as the exclusive crystalline phase in both solids. The specific surface area (S_BET) of sample TiPr400 was larger than that of sample TiEt400, and both larger than that of TiO₂-P25. The three solids have been tested in the photodegradation of paracetamol in aqueous solution. It has been established that the alcohol used influences the properties and catalytic activity of the final oxides. The synthesized solids exhibit a higher activity than commercial TiO₂-P25, because of their structural characteristics and larger S_BET.

Nylon/saponite nanocomposites were synthesized and characterized. The nanocomposites were prepared by means of a fast, efficient, low cost, and environmentally friendly method. All of the tested preparations resulted in the pre-designed nanocomposites. To this end, delaminated saponites were directly synthesized to be used as a filler in a polymer matrix formed by nylon-6 by the in situ intercalation polymerisation of an ε-caprolactam monomer without the use of surfactants or other organic reagents to organophilise the clay, thus avoiding the drawbacks of contamination. The efficiency of the preparation method increased, and significant savings were achieved in terms of both energy reaction time, savings of 60% and 70%, respectively, by using microwave radiation as an energy source during the synthesis of the nanocomposites. In addition, given that the method that was followed avoids the use of contaminating organophilic agents, it is important to highlight the savings in reagents and the fact that there was zero environmental contamination.