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Activated Mg-A1 layered double hydroxide (Mg-A1 LDH) with high crystallinity, prepared by urea decomposition, had higher catalytic activity in the alcoholysis of propylene oxide with methanol than the less crystalline material from Mg-A1 LDH synthesized by titration coprecipitation.The Mg-Al LDHs were characterized using XRD, IR, TG-DTA, AFM and SEM.