Pillared layered solids (PLS), a promising materials for a wide spectrum of industrial applications, are seriously hampered by lack of engineering knowledge for producing them in any great quantity. The underlying physico-chemical principles involved with the move from 1-5 g preparations to the kg quantities were examined in order to establish clear procedures for the preparation of pilot-scale amounts of PILCs. As the synthetic aspects were investigated characterization facilities were also developed. Some of these were well established whilst others were new and demonstrated to be of real value in understanding the chemistry taking place during exchange and pillaring of the clays (eg, pillaring with the aid of a vacuum, microwave heating and conductivity measurements). Overall, key steps in the preparation of PILCs were explored and the potential for using PILCs in commercial areas identified.