The invention discloses a de-ironing method for methyl stannous sulfonate ferric mother liquor. The de-ironing method for methyl stannous sulfonate ferric mother liquor comprises the following steps: (1) heating: taking a methyl stannous sulfonate ferric mother liquor in which Fe<2+> is higher or equal to 135ppm and acidity is 70-85g/l, stirring and heating to 100-125 DEG C to obtain a de-ironing solution; (2) concentrating in vacuum: concentrating the de-ironing solution at a vacuum degree of -0.6MPa to -0.7MPa, replenishing the de-ironing solution when the primary de-ironing solution is concentrated to one thirds of the initial volume and further concentrating, wherein the volume of the replenished de-ironing solution is two fifths to one half that of the primary de-ironing solution, repeating the step for 3-7 times and stopping concentration until the acidity achieves the fact that the concentration of methyl stannous sulfonate is 180-230g/l; and (3) separating solid and liquid: cooling the materials subjected to vacuum concentration to room temperature and separating the solids from the liquid to obtain a de-ironed methyl stannous sulfonate mother liquor. The de-ironing method for methyl stannous sulfonate ferric mother liquor has the advantages of simple process, low cost, no environment pollution, and conforms to the requirements of circular economy and sustainable production and development.