Abstract: Copolymers of trioxane with cyclic acetals may be prepared by copolymerization of the monomers in solid phase. For this purpose the monomers are first mixed homogeneously in a liquid phase with a catalyst, the mixture is then solidified by cooling and finally polymerized by heating, while maintaining it in a solid phase. The liquid phase mixture is cooled to solidify it immediately after mixing and prior to development of turbidity in the liquid mixture. Cooling can be effected, for example, on a chilled rotating roll. The moulding composition, obtained after having worked up the copolymer as usual, is a suitable material for the preparation of molded semi-finished products and finished articles.