Mesoporous self-bonded transition metal-containing AIPO-5 spheres were prepared by a multi-step procedure using macroporous cation exchange resin beads as a template. Aluminum was firstly introduced into the resin by ion exchange using an aluminum chlorohydrate solution. After separation and drying, tf Al-resin composite was mixed with phosphoric acid, tetraethylammonium hydroxide distilled water and hydrothermally treated to yield AIPO-5-resiii composite. Thereafter, vanadium or chromium were ion exchanged into the AIPO-5-resiii composites utilizing the residual ion exchange capacity of the resistor. Finally, the resin was combusted leaving behind Me-AlPO-5 (where Me is V or Cr) spheres similar in shaping and size to the original resin beads. The appearance of the spheres and the nature of the metal species were dependent on the metal loading. The metal introduction affected mainly the mesopore structure of the Mesophare AlPO-5 spheres.