<正>ZSM-5/βco-crystalline zeolites with different content of ZSM-5 have been synthesized by adding different amount of ZSM-5 to the synthetic system of βzeolite with NaAlO2, silica sol as the source of aluminum and silica, respectively, and TEA+ as the template under controlled condition of the synthesis. The ZSM-5/βco-crystalline zeolite was studied by XRD, SEM, BET and NH3-TPD. The reaction activity of toluene alkylation was investigated with a mixture of toluene-methanol as the feedstock in a pulse micro-reactor over the ZSM-5/βco-crystalline zeolite. It is found that ZSM-5/βco-crystalline zeolite has two kinds of zeolite structure including ZSM-5 and βzeolite, not in the form of a physical mixture. The pore structure of ZSM-5/βco-crystalline zeolites is different from that for βzeolite, ZSM-5 and their physical mixture. In addition, the peaks of both high and low temperature desorption of ammonia over the ZSM-5/βco-crystalline zeolite shift 23℃to lower temperatures and the acid amount of its strong acid is 3% more than the physical mixture. So the ZSM-5/βco-crystalline zeolite produces the highest content of xylene, which is 10.4% higher than the physical mixture. And the ZSM-5/βco-crystalline zeolite has better selectivity for toluene alkylation and weaker de-methylation than βzeolite, ZSM-5 and their physical mixture.