合成N,N,N',N'-四(2-甲酯基乙基)乙二胺的绿色工艺研究

为了解决合成聚酰胺-胺时回收液处理复杂、能耗大、并污染环境的问题,以合成N,N,N',N'-四(2-甲酯基乙基)乙二胺(TMCEDA)为研究对象,对不同真空度条件下的回收液进行了定性定量分析,在此基础上,采用分段减压蒸馏分离合成TMCEDA中的过量原料与溶剂,直接循环使用真空度在50 kPa-100 kPa的回收液的新工艺.应用气相色谱分析技术跟踪分析循环使用的回收液的成分,结果表明,经过40次循环使用的回收液,仍未见明显的杂质积累现象.该工艺对回收液的直接使用率高达98.0%,实现了TMCEDA的实验室绿色合成,可为其工业化生产提供参考.图7,表2,参11.

Studies on Green Synthesis Technology of N,N,N',N'-tetra-2-Methoxycarbonylethylethylenediamine

In the synthesis of poly(amidoamine) ,there are some problems with the reclaimed liquid,such as complex disposal,high energy consumption,and environmental pollution. In order to solve those problems,N,N,N', N'-tetra-2-methoxycarbonyl ethylethylenediamine(TMCEDA)is studied. Based on the qualitative and quantitative analysis of recovered liquid at several vacuity,a novel technique is proposed for removing the excesses of methyl acrylate and methanol by stepwise vacuum distillation method in the synthesis of TMCEDA. The components of the recycle recoveries were continuously determined by gas chromatographic analysis,the analytical results show that the recovery of methyl acrylate and methanol under lower vacuum conditions(from 50 to 100 kPa)can be reused directly,and the reclaimed liquid has not appeared the impurity accumulation phenomenon obviously after being reused 40 times,and there are more than 98.0% recovered liquid being reused in our experiment. This process make the laboratory green synthesis of TMCEDA come to reality,and provide significance references for industry production.7fig.,2tabs.,11refs.