Abstract: A method for preparation of solid particulate polyacetal carboxylate. The method comprises agglomerating a solution comprising less than about 1% by weight methanol and between about 30% by weight and about 60% by weight polyacetal carboxylate onto a substrate to produce a free-flowing particulate solid. The solid comprises between about 30% by weight and about 55% by weight polyacetal carboxylate. The polyacetal carboxylate corresponds to the formula: ##STR1## where n is at least about 4 and represents the average chain length of the polyacetal carboxylate in the mixture, R.sub.1 and R.sub.2 are independently selected chemically stable groups that stabilize the polymer against rapid depolymerization in alkaline solution, and M is selected from the group consisting of alkali metals, ammonium, alkyl groups of 1 to about 4 carbon atoms, tetraalkyl ammonium groups, and alkanolamine groups having from 1 to about 4 carbon atoms in the alkyl chain.