Poly(trimethylene terephthalate) (PTT) is an excellent fiber materials. Although it was synthesized as early as 1940s, obtaining high-molecular weight PTT suitable for spinning is not easy due to no evident breakthrough in the catalysts for PTT synthesis. Patents and literatures disclosed a lot of the catalysts of preparing PTT, but which are more or less disadvantageous. Based on acid catalytic mechanism of PTT preparation, a series of solid acid as x% MoO 3 /(50% Al 2 O 3 À 50% TiO 2 ) (briefly written as xM/(A À T), x ¼ 0, 10, 15, 20 by weight) were prepared by sol-gel coprecipitation and wetting impregnation methods, and first used for PTT synthesis in this work. When 50% Al 2 O 3 À 50% TiO 2 (briefly written as A À T) was supported by MoO 3 using wetting impregnation technique of (NH 4 ) 6 Mo 7 O 24 .4H 2 O aqueous solution, a lot of Brunsted acid and Lewis acid sites were formed on xM/(A À T) catalyst surfaces, which was confirmed by the characteristics of their NH 3 -TPD (temperature programmed desorption). All the prepared catalysts were highly active ones toward synthesis of PTT. PTT with high-intrinsic viscosity (IV) was obtained in the presence of trace amount of the catalysts. IV ranging of the PTT synthesized from 0.66 to 0.95 dL g À1 corresponds to weight average molecular weight ðM w Þ from 49,197 to 73,004.