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N,N-二甲基羟胺(DMHAN)是一类羟胺二取代衍生物,它能快速将Pu(Ⅳ)还原成不易被TBP萃取的Pu(Ⅲ),有望作为有机无盐还原剂应用于乏燃料后处理流程中,以实现铀钚分离。本工作采用大型合成装置研究建立了DMHAN的放大合成工艺。以工业纯N,N-二甲基环己胺和30%双氧水作为原料,将氧化反应控制为40～60℃,中间氧化产物采用减压热解。合成结果表明,此放大工艺合成周期较短(约1～2d),单批次DMHAN合成能力约为3kg,产率为53.2%,纯度为99%,产品性能可满足工艺要求。
N, N-Dimethylhydroxylamine (DMHAN) is a kind of hydroxylamine disubstituted derivatives, which can rapidly reduce Pu (Ⅳ) to Pu (Ⅲ) which is not easy to be extracted by TBP. It is expected to be used as an organic salt- Fuel reprocessing process to achieve uranium-plutonium separation. This work using large-scale synthesis device to establish a DMHAN amplification synthesis process. The industrial pure N, N-dimethylcyclohexylamine and 30% hydrogen peroxide as the raw material, the oxidation reaction is controlled to 40 ~ 60 ℃, the intermediate oxidation product was decompression pyrolysis. The synthesis results show that the synthesis cycle of this amplification process is short (about 1 ~ 2d), the DMHAN synthesis capacity of single batch is about 3kg, the yield is 53.2% and the purity is 99%. The product performance can meet the process requirements.