Abstract: A new route for the preparation of 4-hydroxy-2, 2, 6, 6 - tetramethylpiperidinyl-1-oxy with hydrogen peroxide (30%) in the presence of Mg-Al hydrotalcite was proposed. The structure of the product was verified by elemental analysis, IR, and GC-MS. The effects of reaction time, molar ratio of reactants and catalyst dosage on the yield were investigated. The best reaction conditions were as follows：mole ratio of H2O2 to 4-hydroxy -2,2,6,6- tetramethyl- piperidine 3.0∶1.0, catalyst dosage（based on the amount of 4- hydroxyl -2,2,6,6- tetramethylpiperidine）2.5 %，reaction temperature 70 ºC and reaction time 2.5 h. Under these conditions，a high yield of over 97% was obtained. The catalyst could be reused with high activity. This heterogeneous catalyst had the advantages of high activity，simple workup procedure，non-pollution and reusability，which contributed to the green process greatly.