The invention discloses a preparation method for preparing
methoxyamine hydrochloride by using 2, 3-butanedione, which comprises the following steps: S1, adding 2, 3-butanedione and
hydroxylamine hydrochloride into water, and carrying out oximation reaction under the action of alkali to prepare 2, 3-butanedioxime; s2, 2, 3-
dimethylglyoxime and
dimethyl sulfate are subjected to a
methylation reaction, 2, 3-bis (methoxyimino)
butane is prepared, and in the reaction process, alkali liquor is adopted to control the pH of a
reaction system to be 7-9; s3, the 2, 3-bis (methoxyimino)
butane is subjected to an acidolysis reaction, and
methoxyamine hydrochloride is prepared. According to the method, 2, 3-butanedione and
hydroxylamine hydrochloride are taken as raw materials, so that the conversion rate of
methylation reaction is increased, the generation of polymethylation impurities (O, N-dimethyl
hydroxylamine hydrochloride) is reduced, the yield is relatively high, meanwhile, the reaction condition is mild, the operation is simple, synthesis is easy, the byproduct 2, 3-butanedione can be recycled, the material
utilization rate is high, and the method is suitable for industrial production. And the cost and the
energy consumption can be reduced.