A phase transfer technique was employed to prepare nanosize Cu-ZnO/Al2O3 catalyst particles. Due to adsorption of metal surfactants, sol particles are transferred from the aqueous phase to the organic phase. Consequently, the agglomeration of particles can be reduced. Cu-ZnO/Al2O3 catalyst of about 5-mm particle size was prepared by this technique. It was found that organic solvents with aliphatic chains were more effective than aromatic solvents. A solvent-to-salt ratio of about 2200 mi solvent per mole of salt appeared to be ideal. The preparation procedure comprises preparation of aqueous sol and metal surfactant solution in organic solvent, mixing, stirring, and so on. The mol fraction of metal surfactant versus total metal was approximately 0.3. The concentration of salt and precipitant was 0.2-0.4 mol/L.