The development of desulfurization technology involving the onsite direct generation of hydrogen peroxide (H(2)O(2)) from H(2) + O(2), followed by H(2)O(2) oxidation to organic oxides without conventional refining is regarded as one promising approach for reducing capital and operating costs. The objective of our research is to provide bi-functional catalytic materials based on a combined process for the oxidative desulfurization (ODS) using H(2)O(2) in situ generated. We have prepared a series of new bi-functional titanosilicate (NTS, titanium silicalite combined with noble-metal loading), which have been synthesized by combining noble-metal sources with modified titanium silicalite under basic conditions. Here, the synthesis and characterization of NTS samples. and their ODS properties are presented The samples were characterized by various analytical techniques, and their direct ODS performances were investigated. The results indicate that NTS shows well ordered MFI topology and with hollow structure; NTS combined with noble-metal shows potential for application in direct ODS with H(2) + O(2) in one-step process (C) 2009 Elsevier B V. All rights reserved.