This paper reports on the preparation of simple and cost-effective nanocomposite that involved intercalation of sandwich-type polyoxometalate (STPOM) anion [(OCe)3(PW9O34)2]12− into Mg/Al layered double hydroxides (donated as Mg3Al–Ce3W18) using an ion-exchange method. The catalytic performance of nanocomposite catalyst was examined in green synthesis of aryl sulfonyl benzene diols via oxidative coupling between 1,2-benzenediols and sodium benzenesulfinates under mild green condition (; in water at room temperature) with good yields (63–75%). Besides, the nanocomposite catalyst exhibited excellent reusability up to five subsequent runs. SEM, EDX and BET were employed to characterize the as-fabricated nanocomposite.
