The present work discloses a new methodology for the production of detached nanorods of 2Li(2)O/MgO catalyst particles on the internal surface of alpha-Al2O3 porous supports to be used as efficient catalysts for the oxidative coupling of methane reaction (OCM). The peculiarity of our preparatory recipe is the success in producing "detached" nanosized entities on the support surface. The performance of the new catalyst/support system for the OCM reaction has been evaluated using a special reactor assembly with cross flow of methane and oxygen gas streams. Under the optimum process conditions, the yield of C-2(+) product is 25% at an average reaction temperature of 750 degrees C. Under the optimum conditions, the yield of ethylene reaches 8%. It is shown that the enhanced catalytic properties of the new catalyst/support composite may be attributed to nanoeffects. (C) 2009 American Institute of Chemical Engineers AIChE J, 56: 717-728, 2010