The invention belongs to the technical field of treatment of chemical industrial waste residues and relates to a dimethyl sulfate residue treatment method. The treatment method includes: subjecting dimethyl sulfate residues to hydrolysis, etherification and esterification reactions to obtain crude products of dimethyl sulfate; subjecting the crude products of dimethyl sulfate to reduced pressure distillation to separate dimethyl sulfate out and obtain black brown sulfuric acid mother liquor; performing vacuum distillation on the sulfuric acid mother liquor to increase concentration, and mixing with an oxidizing agent to react under the action of a catalyst to obtain light yellow transparent liquid; decolorizing the light yellow transparent liquid by an ion exchange resin system to obtain colorless transparent sulfuric acid. The dimethyl sulfate residue treatment method solves the problem of insufficiency in treatment of the dimethyl sulfate residues and has advantages of low equipment investment, mild process conditions, freeness of environment pollution, safety and environment friendliness.