Síntese de membranas zeolíticas (Mordenita/α-alumina) utilizando os métodos de síntese hidrotérmica, dip-coating e transporte em fase vapor e avaliação na separação emulsão óleo/água.

Abstract

The objective of the present work is to synthesize zeolite membranes (Mordenite/α-alumina) using hydrothermal synthesis, secondary growth: dip-coating and vapor-phase transport, to be evaluated in the oil/water emulsion separation process. The influence of the crystallization time on the synthesis of the mordenite zeolite, the influence of the precursor (aluminum sulphate and gibsite) on the synthesis of the zeolite membrane, influence of the synthesis methods of the zeolite membranes and the water permeation tests and the oil/water emulsion separation process. The synthesis of the mordenite zeolite was performed using the hydrothermal method at 170°C, with crystallization times of 24, 36, 48, 72, 96 and 120 hours, in order to evaluate the crystallinity of the zeolite, and to select the best time for the synthesis of zeolite membranes. The α-alumina ceramic supports were prepared from the decomposition of the aluminum sulfate precursors at 1000°C and gibsite at 1200°C for 2 hours, and conformed, compacted and sintered at 1300°C for 2h, and then submitted to the characterization techniques: (XRD), Nitrogen Physical Adsorption, Scanning Electron Microscopy (SEM), X-ray Fluorescence Spectroscopy (FRX-ED) and Thermogravimetric/Differential Thermal (TG/DTA). The zeolite membranes were synthesized by hydrothermal synthesis, secondary growth: dip-coating and vapor-phase transport at 170°C for 72 hours and characterized by XRD and SEM. Ceramic supports and zeolite membranes were evaluated in water permeation tests and in the oil/water emulsion separation system of a synthetic effluent using a membrane separation process. The tests were carried out under the conditions of initial concentration of the emulsion 100 mg.L-1, temperature of 25°C and pressure of 2,5 bar, allowing to evaluate the permeability and the selectivity from the variation of the permeate concentration in (mg. L-1) and the percentage of oil rejection (% R). From the results obtained for the synthesis of the materials, it is possible to observe the effective formation of zeolite mordenite in pure and crystalline phase. The precursors were satisfactorily decomposed to give the α-alumina phase. The maintenance of the post-production α-alumina phase of the ceramic supports was confirmed after characterization. The MZMOR/α-alumina zeolite membranes presented a homogeneous and uniform distribution of the zeolite crystals corresponding to the mordenite phase, without the presence of impurities, free of defects and without cracks, confirming the formation of the structure of the zeolite membrane by the three methods of synthesis, used in this work. The mordenite zeolite showed excellent adhesion and formation of the zeolitic layer on the ceramic support α-alumina. From the evaluation of the permeability and selectivity in the oil/water emulsion separation tests, it can be concluded that the insertion of the mordenite zeolite to the ceramic supports improved the separation process of the oil/water emulsion. In terms of efficiency in the separation process, the zeolite membrane MZMOR/α-Al2O3(SHGB) was considered to have the best relationship between flow and selectivity, showing the efficacy of zeolite membranes. All zeolite membranes synthesized and evaluated were promising.