The characteristics and structure of alternating copolymerization of maleic anhydride with epichlorohydrin by Fe- Al- α,α - dipyridyl were presented and discussed.The copolymerwas characterized and discussed.The copolymer was characterized by IR and1H- NMR.The copolymer is a product of high alternation.Meleic anhydride is48.6% in the copolymer.The coploymerization can be realized in the solvents such as aromatic hydrocarbon and alkane.The yield is higherin aromatic hydrocarbon than the others.The suitable Al/Fe molar ratio is2~ 6.The suitable Fe/α,α - dipyridyl molar ratio is1.