Three-step high temperature programmed hydrothermal preparation of ZSM-5 was investigated by using different crystallization times and temperatures. The synthesized nanostructured catalysts were analyzed by XRD, FESEM, EDX, BET-BJH, FTIR, TPD-NH3 and TGA techniques. According to the obtained characterization results, synthesis of ZSM-5(250-30,300-15,350-5) by short time temperature programmed showed a significant effect on the crystallinity, phase purity, morphology, textural properties and acidity of the nanostructured catalyst. Furthermore, this sample had small crystals with higher intercrystalline porosity and also proper distribution of acid sites. The synthesized catalysts were applied in the methanol to propylene (MTP) process under the operating conditions of T=460??C and GHSV=10,500 cm3/gcat??h in a fixed-bed reactor. The ZSM-5(250-30,300-15,350-5) catalyst exhibited high selectivity toward propylene (73%) with slow deactivation rate. Also, the possible reaction pathway for pure MFI preparation via three-step short-time temperature-programmed was presented.