Mesoporous aluminosilicates with cubic and hexagonal structure have been synthesized by structure units of β zeolite in a two step crystallization process and characterized by XRD, IR, N 2 physical adsorption and desorption, 27 Al MAS NMR and NH 3 TPD techniques. The results show that MB48(25) and MB41(25) were similar to MCM 48 and MCM 41 on the long range structure respectively and MB48 with a cubic structure can be synthesized under the condition of a lower n (CTMAB)/ n (SiO 2) ratio. HMB48(25) and HMB41(25) exhibit a stronger acidic strength than conventional HMCM 41. The catalytic activity of HMB48(25) was the highest for cumene cracking and alkylation of 2,4 tert butylphenol with tert butylalcohol.