AbstractAqueous slurry free radical terpolymerization of acrylonitrile (AN) with vinyl acetate (VAc) and a constant amount of 2-acrylamido-2-methylpropane sulfunic acid (AMPS) using K2S2O8/NaHSO3 redox initiator was carried out in a 15-l continuous stirred tank reactor at constant temperature (60°C) and atmospheric pressure. A three-level response surface method based on central composite design was applied to investigate the effect of VAc concentration (wt%) in monomer mixture, bisulfite- to-persulfate ratio in redox initiator system $\left( {\frac{{{\text{[HSO}}_3^ - ]}}{{[{{\text{S}}_2}{\text{O}}_8^{ - 2}]}}} \right)$ and bisulfite-to-monomer mixture ratio $\left( {\frac{{[{\text{HSO}}_3^ - ]}}{{{\text{AN}} + {\text{VAc}}}}} \right)$ on the monomer conversion percentage to polymer, intrinsic viscosity [(η)] and sulfur end groups (SEG) index of the prepared polymers. Experimental results showed that the optimum conditions for synthesis of AN-VAc-AMPS system can be addressed as VAc=9 wt%, $\left( {\frac{{[{\text{HSO}}_3^ - ]}}{{[{{\text{S}}_2}{\text{O}}_8^{ - 2}]}}} \right) = 9.6$ and $\left( {\frac{{[{\text{HSO}}_3^ - ]}}{{{\text{AN}} + {\text{VAc}}}}} \right) = 0.027.$ Monomer conversion percentage to polymer, intrinsic viscosity and SEG index under optimum conditions were 75%, 1.38 dl/g and 190, respectively. The synthesized polymer under these optimum conditions can satisfy the requirements for acrylic fiber production in which its characterization was confirmed with Fourier transform infrared spectroscopy, nuclear magnetic resonance, elemental analysis, X-ray diffraction, differential scanning calorimetry and scanning electron microscope.