以甘氨酸乙酯盐酸盐和亚硝酸钠为原料，研究了在微通道反应器中重氮乙酸乙酯的连续流合成工艺。考察了亚硝酸钠用量、反应温度、酸用量、停留时间等工艺条件对反应结果的影响。由于该反应为强放热反应，且产物在高温下稳定性差，因此，若采用传统釜式间歇操作容易造成局部过热，存在较大的安全隐患和产物分解的缺陷；普通的管道反应器又难以克服非均相的传质障碍导致收率偏低。微通道反应器在保持良好的传热效率同时，能打破相界面障碍，保证反应液充分混合，非常适合该工艺的开发。利用微通道反应器的上述优点，进行工艺条件的筛选，提高了反应效率并得到较高的收率。

A continuous flow synthetic process for ethyl diazoacetate is studied in a microchannel reactor by using glycine ethyl ester hydrochloride and sodium nitrite as raw materials.The effects of the dosage of sodium nitrite,reaction temperature,acid dosage and residence time on the reaction yield are investigated.Since this reaction is highly exothermic and the product is unstable under higher temperature,traditional kettle batch operation is very easy to cause locally overheated,leaving major hidden danger and leading to product decomposition.Ordinary pipeline reactors are hard to overcome mass transfer obstacle due to heterogeneity,resulting in lower yield.Microchannel reactors maintain good heat transfer efficiency while fully break through the phase interface obstacle to ensure the sufficient mixing of heterogeneous reaction liquids.So microchannel reactors are very suitable for the development of this synthetic process.By means of the advantages of the microchannel reactor,novel process for ethyl diazoacetate is developed and the process conditions are optimized in order to improve the reaction efficiency and yields.

岳家委(1995-),男,硕士生