Highly concentrated suspensions of ultrafine alumina powders are prepared using 2-phosphonobutane-1,2,4-tricarboxylic acid as dispersant. The coagulation of these suspensions is carried out at around 278 K by adding a blend of acetic anhydride plus ethylene glycol. Coagulation takes place through a pH shift because of a time-delayed hydration of the acetic anhydride. The coagulation kinetics are studied by viscosity measurements with respect to the temperature and composition of the coagulant blend. Finally, the method is used to produce complex 3D parts of large dimensions for bio-applications by direct coagulation casting and the fired bodies are characterized.