A method for effectively preventing polymerization of acrylic acid during an azeotropic dehydration distillation in an acrylic acid manufacturing process and thus enabling stable operation of the azeotropic dehydration column over an extended period of time. The acrylic acid is separated in an azeotropic dehydration column from an acrylic acid aqueous solution fed therein, and the method includes withdrawing from the bottom of the azeotropie dehydration column a bottom effluent containing 50% or more of glyoxal (including the hydrates thereof) contained in the acrylic acid aqueous solution fed into the azeotropic dehydration column.