The present invention relates to a process for the preparation of a molecular sieve adsorbent for the adsorptive dehydration of alcohols. The invention relates to the preparation and use of surface modified zeolites in the dehydration of alcohols. More specifically, the invention relates to the preparation and use of a molecular sieve adsorbent, which selectively removes water from water - ethanol azeotrope obtained from distillation of the crude synthetic or fermentation feedstock. Microporous solid powder of Zeolite A with a chemical composition [Na12 (AlO2) 12. (SiO2) 12wH2O] was used as the starting material. This zeolite was activated at 400°C to remove the water adsorbed and mixed thoroughly with a solution having known amount of alkoxide in dry solvent, the sample was dried by evaporating solvent under reduced pressure and the alkoxide species deposited on the solids surface was converted into silica by calcinations of the zeolite to obtain molecular sieve adsorbent.
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