ABSTRACT This doctoral thesis is involved in the synthesis of microporous materials, which show applications in separation, catalysis, electronic, and biomedicine. Zeolites are cristalline microporous materials forming channels and cavities in their structure. The advantages of zeolites are their thermal and chemical stability, with the possibility to variate the topology and dimensions of their channel system. The principal aim of this work is to create a new methodology for the synthesis of these materials by using high-throughput techniques. The introduction of these techniques is recent in the field of materials, and therefore, their application for developing new materials is in its first age. The use of this methodology for discovering new microporous materials and optimizing known materials is applied. The effect of organic structure directing agents (rigidity and flexibility), the introduction of different elements to Si (Ge or Ti), the presence of trivalent atoms that introduce negative charges in the framework (Al or B), the mineralizing agents (OH- or F- media), and gel concentration is studied. Finally, the use of high-throughput techniques generates a large number of data, being necessary the development of data-mining techniques. In the last section of this phD thesis, new data-mining approach in the material synthesis, as modelling, classification and mapping-exploration of zeolites is shown.