The synthesis of Zr-SBA-15 materials from zirconocene dichloride as metal precursor has been investigated. These materials can be prepared with a high loading of zirconium while preserving good mesoscopic ordering. Zr-SBA-15 materials display acid properties which have revealed to confer high catalytic activity in the transesterification of crude palm oil with methanol for biodiesel synthesis, achieving yields to FAME over 70% in a batch reactor under the following reaction conditions: 200 degrees C, 3 h, methanol to oil molar ratio 30:1 and using 10 wt.% catalyst loading referred to oil. Furthermore, Zr-SBA-15 materials display excellent stability in palm oil transesterification, being fully regenerated by calcination at 550 degrees C after at least eight consecutive reaction runs. The incorporation of titanium, molybdenum and tungsten as doping metals produces slightly promotion of the acidity of Zr-SBA-15 materials, though this is not translated into higher catalytic activity. (C) 2010 Elsevier B.V. All rights reserved.