Phenylphosphonates of zinc (Zn-PPh), calcium (Ca-PPh) and magnesium (Mg-PPh) were synthesized by the hydrothermal method. Samples showed characteristic X-ray diffraction (XRD) patterns of layered compounds with basal spacing in the range of 14-15 Å. According to Fourier transform infrared spectroscopy (FTIR), all compositions showed the presence of characteristic bands attributed to phenyl aromatic rings, phosphonate and lattice metal-oxygen (M-O) vibrations. Different concentrations of phenylphosphonate particles were applied to stabilize water-in-oil Pickering emulsions using vaseline oil in different w/o fractions. The three particle types showed greater affinity for the oil phase (wettability) and the ability to stabilize the emulsions via the Pickering effect. Ca-PPh particles contained a greater emulsified fraction after 20 days of evaluation. This result can be attributed to the particle morphology observed by scanning electron microscopy (SEM). The fibrous morphology of Ca-PPh particles is believed to increase the steric hindrance effect at the surface around the droplets, while the Zn-PPh and Mg-PPh layered particles tended to form clusters.

Layered double hydroxides (LDH) with the composition Zn2Cr, intercalated with acetate and chloride ions were synthesized by co-precipitation with increasing pH and characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and inductively coupled plasma-optical emission spectrometry (ICP-OES). The samples synthesized at optimized pH showed XRD patterns with basal diffraction peaks typical of layered structures, with basal distances of 7.88 and 12.69 Å for intercalated chloride (Zn2Cr/Cl) and acetate (Zn2Cr/Ac), respectively. After optimization experiments, exchange reactions were performed with different anions, using an excess of five times the anions to be intercalated. Zn2Cr/Cl was exchanged with CH3COO-, F-, Br-, I-, SO42- and NO3-, and Zn2Cr/Ac was exchanged with F-, Cl-, Br-, I-, SO42- and NO3-. Not all reactions were effective, indicating that among the evaluated anions, CH3COO- was preferred for exchange, mainly attributed to the pre-expansion with bigger anions, facilitating the exchange with smaller anions.

RESUMO No presente trabalho, utilizou-se a caulinita como material base para a obtenção de materiais nanocompósitos. A caulinita foi utilizada na forma in natura, tratada termicamente à 700 ºC e quimicamente com ácidos fosfórico e sulfúrico na concentração de 6 mol L-1. O objetivo dos tratamentos foi modificar e preparar a estrutura da caulinita para ser usada como um suporte para o TiO2. Por meio do método dos precursores poliméricos foi sintetizado o TiO2 e nanocompósitos à base de caulinita e TiO2. Os nanomateriais foram caracterizados por Difratometria de Raios X (DRX), UV-Vis, para determinar o Bandgap, Espectroscopia na Região do Infravermelho com Transformada de Fourier (FTIR), Microscopia Eletrônica de Varredura (MEV) e Espectroscopia de Energia Dispersiva (EDS). Por meio dos espectros de FTIR foi possível verificar as bandas características da caulinita in natura e o aparecimento de vibrações características da metacaulinita. A análise de DRX revelou que foi possível promover o aumento da cristalinidade das amostras de caulinita após tratamento com o citrato de titânio, isto pode ser decorrente da adesão do óxido de titânio na superfície da caulinita. Pela análise de EDS foi possível determinar a porcentagem de Ti (m/m) nas amostras sintetizadas, sendo que seu valor ficou entre 2,03 e 4,16 %. As análises por ICP-OES indicam que as amostras apresentam de 2,65 a 4,07% de Ti e os dados do Bandgap variam de 1,69 a 3,44 eV para as amostras com e sem Ti em sua composição.

ABSTRACT The present work used kaolinite as base material to obtain nanocomposite materials. Kaolinite was used in its natural form, heat treated at 700 ºC and chemically using 6 mol L-1 phosphoric and sulfuric acids. The objective of the acid treatments was to modify and prepare the kaolinite structure to be used as a support for TiO2. Using the polymeric precursor method, TiO2 and nanocomposites based on kaolinite and TiO2 were synthesized. Nanocomposites were characterized by X-ray Diffraction (XRD), UV-Vis, to determine Band Gap, Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and Dispersive Energy Spectroscopy (EDS). Through the FTIR spectra it was possible to verify the characteristic bands of in natura kaolinite, and the appearance of characteristic vibrations of metakaolin. XRD analysis revealed that it was possible to promote increased crystallinity of kaolinite samples after treatment with titanium citrate, this may be due to the adhesion of oxide on the kaolinite surface. By EDS analysis it was possible to determine the percentage of Ti (m/m) in the synthesized samples, and its value was between 2.03 and 4.16%. ICP-OES analyzes indicate that samples have 2.65 to 4.07% Ti and Bandgap data range from 1.69 to 3.44 eV for samples with and without Ti in their composition.