N,N-二苄基羟胺的清洁化合成工艺研究

Study on cleaning synthetic technology of N,N-Dibenzylhydroxylamine

摘要:

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。

Abstract:

The cleaning production technology for N,N-Dibenzyl hydroxylamine(Referred to as DBHA)was studied. Using benzyl chloride and hydroxylamine hydrochloride as raw material，triethylamine as proton acceptor，DBHA was synthesized in organic solvents after the two-phase reaction. The optimal conditions of synthesis were as following：the molar ratio of hydroxylamine hydrochloride and benzyl chloride was 1：2.3，the first-phase reaction was carried at 50 ℃ for 80 min，while the second-phase reaction at 80 ℃ for 220 min. Under the above optimum conditions，the yield of the product was 81.3％ with the melting point of 123.6～125.3 ℃. The structure of product was confirmed by IR、1H RMR、13C NMR、MS. This technology was adopted to resolve the problem of sewage including salt and organic solvents which were generated by traditional technology. Compared with traditional technology，this new one was suitable for industrial production.