Diaminoglyoxime (DAG) was synthesized by glyoxal and hydroxylamine hydrochloride through one-pot reaction and its structure and purity was characterized and analyzed through various technologies including infrared spectrum, elemental analysis, melting point test, high efficiency liquid chromatography. According to single factor analysis and orthogonal experiment design, the optimal technology condition was obtained while the feed mole ratio of hydroxylamine to glyoxal was 4.8:1 and the reagents was heated to 90℃ with oil bathing under the condition of heating circumfluence for 4.5h at a pH of 8.5. As a result, the production yield reached 73.1%. To avoid the environmental pollution caused by waste liquid, a green treatment technology was designed for the harmlessness of the wastewater from the perspective of environmental protection. At last, a pollution-free circular synthetic technology which reuse the wastewater as ingredient was achieved and the yield was effectively improved.