己二酸二酰肼合成工艺研究

Synthesis of Adipic Acid Dihydrazide by Two Steps

对两步法合成己二酸二酰肼(ADH)的工艺条件进行了研究。首先采用己二酸和甲醇酯化反应合成了己二酸二甲酯,然后将己二酸二甲酯与水合肼酰肼化,得到了高纯度己二酸二酰肼,并确定了适宜的工艺条件:对于酯化反应,催化剂为KHSO4,用量为己二酸质量数的5.5%,n(醇)/n(酸)为4.0,反应时间1.0 h,在该条件下,产品己二酸二甲酯质量分数高达99.8%,收率为77%;对于酰肼化反应,n(肼)/n(酯)、n(醇)/n(酯)比均为4.0,反应时间为1.5 h,此条件下,ADH收率达99%,质量分数高达99.5%。

The synthesis of adipic acid dihydrazide by two steps was investigated in this paper. Adipic acid was first esterified with methanol under the catalysis of KHSOa to give dimethyl adipate, which was further reacted with hydrazine hydrate to produce adipic acid dihydrazide （ADH） with a high purity. The optimal conditions for the esterification reaction were determined as catalyst amount was 5.5% of the weight amount of adipic Under these conditions, For nol acid the hydrazide reactio acid, molar ratio of methanol to adipic acid was 4.0, the purity of dimethyl adipate was as high as 99.8% n, the optimal conditions were ： molar ratio of both hyd to dimethyl adipate was 4.0, reaction time was 1.5 h. Under these condi dihydrazide reached 99% and the purity was 99.5%. reaction and the razine hy tions, th time was 1.0 h. yield was 77%. drate and metha- e yield of adipic