The synthesis of dimethylacetal using acetaldehyde and methanol as raw material in the presence of Smopex 101 fibres as catalyst and adsorbent in batch reactor and in a fixed bed adsorptive reactor, respectively, was Studied. In the batch reactor the determination of thermodynamic and reaction kinetics data for acetalization reaction was presented. A kinetic model based on a pseudo-honnogeneous rate expression using activities was proposed to describe the experimental kinetic results. The dynamic binary adsorption experiments were carried out in the absence of reaction at 293.15 K in a laboratory scale column. The experimental results of the adsorption of binary non-reactive mixtures are reported and used to obtain multi-component adsorption equilibrium isotherms of Langmuir type. The mathematical model was proposed to describe the adsorptive reactor dynamic behaviour. The experimental results obtained for the reaction and regeneration experiments were compared with the model proposed. Model equations were solved by orthogonal collocation on finite elements (OCFE) implemented by the PDECOL package, using the measured model parameters and was validated for both reaction and regeneration steps. (c) 2006 Elsevier Ltd. All rights reserved.