Industrial production of N,O-dimethylhydroxylamine hydrochloride, usually first obtain a content of ≤ 95% (GC detection, the impurity is methoxyamine hydrochloride) N, O-dimethylhydroxylamine hydrochloride crude product, this purity of crude product using methanol recrystallization process route to obtain the finished product is still ≤ content of 95% (GC). In the case that the recrystallization Chemicalbook art scheme is not feasible, the conventional purification scheme is to first dissolve the crude product in water, add alkaline substances to neutralize, distill out the aqueous solution of methoxyamine and N, O-dimethylhydroxylamine mixture, and then use the distillation column separation method to intercept the N,O-dimethylhydroxylamine fraction, and then manufacture N,O-dimethylhydroxylamine hydrochloride.