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研究了羟胺类抗氧剂N,N-二苄基羟胺(DBHA)的清洁化生产工艺方法。以氯化苄、盐酸羟胺为原料,三乙胺为缚酸剂,在有机溶剂中经两步反应合成DBHA。考察了合成DBHA适宜的工艺条件,n(盐酸羟胺)∶n(氯化苄)=1∶2.3,一阶反应温度50℃,反应时间80 min;二阶反应温度80℃,反应时间220 min的条件下,DBHA的收率达81.3%,熔点123.6～125.3℃。经IR、1HRMR、13CNMR、MS分析,确定产品与化合物N,N-二苄基羟胺结构相符。合成工艺解决了传统生产工艺中所产生的高盐、有机废水的处理问题,便于工业化生产。
The clean production process of hydroxylamine antioxidant N, N-dibenzylhydroxylamine (DBHA) was studied. Using benzyl chloride, hydroxylamine hydrochloride as raw materials and triethylamine as acid-binding agent, DBHA was synthesized by two-step reaction in organic solvent. The optimum technological conditions for the synthesis of DBHA were investigated. N (hydroxylamine hydrochloride): n (benzyl chloride) = 1: 2.3, the first reaction temperature was 50 ℃, the reaction time was 80 min; the second reaction temperature was 80 ℃ and the reaction time was 220 min Under the conditions, DBHA yield 81.3%, melting point 123.6 ~ 125.3 ℃. The product was identified as N, N-dibenzylhydroxylamine by IR, 1H NMR, 13CNMR, MS analysis. Synthetic process to solve the traditional production process generated by salt, organic wastewater treatment problems, to facilitate industrial production.