The polymerization of MMA and EMA by using a catalyst of Fe(acac)3-Al(i-Bu)3-8-hydroxy quinoline was investigated．The structure of the polymers is characterized by using NMR and IR techniques. The polymers obtained have mainly isotactic and syndiotactic structures．Molecular weight and its distribution were studied by GPC. The polymerization can be realized in solvents such as aromatic hydrocarbon and alkane. The yield is higher in alkane then in the others. The suitable Fe／8-hydroxy quinoline molar ratio is unity．The suitable Al／Fe molar ratio is eight. The suitable concentration of catalysts is [Fe] =8.0×10-3～ 1.2×10-2 mol／L．The increasing reaction temperature causes an increase of the polymer yield．The suggested temperature range is 70～90℃. Kinetic studies show that the MMA and EMA polymerization are reactions of first order with respect to the monomer concentration. The apparent activation energies of MMA and EMA polymerization are 36.3 kJ／mol and 46.4 kJ／mol

respectively.