We herein report for the first time, a new and efficient method using ultrasonic activation for intercalation by ion exchange and microwave heating for formation of zirconium polyoxycationic species in the preparation of ZrO2-pillared clay composite with improved physico-chemical properties and significant reduction in processing time. Acetic anhydride under solventless conditions with microwave irradiation in the presence of ZrO2-pillared clay was used for the mono-acylation of diols and alcohols in very good yield. (C) 2003 Elsevier B.V. All rights reserved.