This work presents the development of a novel process for the production of diethylacetal from the reaction between ethanol and acetaldehyde catalyzed by the acid resin Amberlyst (R) 15 using simulated moving-bed reactor (SMBR) technology. The methodology used combines modeling/simulation with laboratory- and pilot-scale experiments. The kinetic law of the reaction was measured from experiments in a batch catalytic reactor. The adsorption parameters were obtained from experiments performed in a fixed-bed adsorption column. Laboratory experiments in fixed-bed adsorptive reactors were performed and used to validate model and simulation tools. The SMBR technology was applied for diethylacetal production and separation with 87% purity and the acetaldehyde conversion was about 98%. The influence of feed composition, switching time, and mass-transfer resistance on the SMBR performance was analyzed by simulation. The reaction/separation region was determined using separation zone methodology. Simulated results show that high acetal purities can be achieved for 100% acetaldehyde conversion. (c) 2005 American Institute of Chemical Engineers.