Different and alternative methods for the preparation of Ni/pillared clays based on impregnation and encapsulation procedures are reported. Several nickel precursors and metal loadings are considered in order to evaluate their influence on the structural, textural and catalytic properties of the resulting solids. The behaviour of the optimum solids as catalysts has been proved in the selective catalytic reduction of nitrogen oxides with propene, and the relevance of the oxidant nature was checked by changing the composition of the oxidant mixture. Of all the factors studied, the nature of the nickel precursors appears as the most important one, owing to the formation of different active nickel species during the synthesis procedure.