CAJ | 학술논문

在微通道反应器中，由 H2O2、乙酸酐反应连续合成过氧乙酸氧化剂，再与环己酮经 Baeyer-Villiger 氧化连续合成ε-己内酯。先后考察了过氧乙酸氧化剂合成中乙酸酐与H2O2摩尔比、反应温度、停留时间等因素的影响，环己酮氧化反应中原料摩尔配比、反应温度、停留时间等因素对ε-己内酯合成的影响，优化了工艺条件。结果表明，当n(乙酸酐)∶n(H2O2)=1.2∶1、反应温度为70℃、停留时间为115s时，H2O2转化率达88.9%，过氧乙酸收率达86.7%；当n(过氧乙酸)∶n(环己酮)=1.1∶1、反应温度为90℃、停留时间为90s时，环己酮转化率达96.2%，ε-己内酯的收率达80.9%。与传统间歇釜式反应工艺相比，微通道反应工艺提高了ε-己内酯的收率和选择性，缩短了反应时间，减少了原料消耗，实现了连续化操作，提高了生产安全性。
재미통도반응기중，유 H2O2、을산항반응련속합성과양을산양화제，재여배기동경 Baeyer-Villiger 양화련속합성ε-기내지。선후고찰료과양을산양화제합성중을산항여H2O2마이비、반응온도、정류시간등인소적영향，배기동양화반응중원료마이배비、반응온도、정류시간등인소대ε-기내지합성적영향，우화료공예조건。결과표명，당n(을산항)∶n(H2O2)=1.2∶1、반응온도위70℃、정류시간위115s시，H2O2전화솔체88.9%，과양을산수솔체86.7%；당n(과양을산)∶n(배기동)=1.1∶1、반응온도위90℃、정류시간위90s시，배기동전화솔체96.2%，ε-기내지적수솔체80.9%。여전통간헐부식반응공예상비，미통도반응공예제고료ε-기내지적수솔화선택성，축단료반응시간，감소료원료소모，실현료련속화조작，제고료생산안전성。
Peracetic acid was prepared as an oxidant from acetic anhydride and H2O2 firstly,and thenε-caprolactone was synthesized by Baeyer-Villiger oxidization of cyclohexanone in a continuous flow micro-channel reactor. The effects of reactants molar ratio,reaction temperature and residence time on reactant conversion and product yield were investigated for both preparation of peracetic acid and synthesis ofε-caprolactone,and the process conditions were optimized. Under conditions of n(acetic anhydride) ∶n(H2O2)=1.2∶1,reaction temperature at 70℃,residence time of 115s,conversion of H2O2 reached 88.9% and yield of peracetic acid reached 86.7%. Under conditions of n(peracetic acid) ∶n(cyclohexanone)=1.1∶1,reaction temperature at 90℃,residence time of 90s,conversion of cyclohexanone reached 96.2% and yield of ε-caprolactone reached 80.9%. Comparing with the traditional batch reaction process,the selectivities and yields of target products in this continuous micro-channel reaction process were increased with shortened reaction time and lessened raw material consumption,and process continuity ensured higher operation safety.