The relation between the properties and the activities of phosphoric acid catalyst, and also the method of preparation for highly active catalysts were studied.The activity of the catalyst is affected by the amount of phosphoric acid content and the properties of the surface of carriers, and the amount of phosphoric acid content showing maximum activity varies, depending upon carriers. Catalysts of high activity can be prepared from carriers which have large porous volume, thereby carrying large quantities of phosphoric acid. Such carriers are prepared by treating molded kieselguhr with alkali solution, washing with water, then treating with dilute acid solution.