Some observations on the synthesis of fully-dispersible nanocrystalline zeolite ZSM-5.

Abstract

A facile method for the rapid synthesis of fully-dispersible ZSM-5 (Si/Al = 100) of about 30 nm size in high yield (about 91%) is described. The method comprises three steps, viz., concentration of an initial clear solution, low-temperature (80 degrees C) ageing of concentrated sol, and high-temperature (175 degrees C) hydrothermal treatment or microwave heating (175 degrees C) of aged concentrated sol. A simple vacuum-concentration method was used for the extraction of pure NPs of ZSM-5 in solution. XRD, FT-IR, TGA and ASAP characterizations showed that the NPs were partially crystalline. The concentration step accelerated the aggregation of primary units, which helps in the production of a large number of nucleation centers protected by TPA+ ions against aggregation. During low-temperature ageing, the number of critical sized nuclei increases, growing into zeolite. The high-temperature heating results in the complete growth of unreacted silica, giving high yields. A key factor for generating small non-aggregated zeolite crystals is the amount of water in the synthesis sol. The three-step method presented here produces a target material of small and uniform sized, non-aggregated ZSM-5 of about 30 nm in a short reaction time. The results are significant, as the synthesis method adopted here produces much uniform, non-aggregated nanocrystalline ZSM-5 in a shorter time with high yield.