γ-十一内酯的反应精馏工艺开发与优化

Design and optimization of reactive distillation process for production of undecan-4-olide

针对γ-十一内酯传统工艺存在的产品收率低、操作复杂等缺点,提出采用反应精馏工艺强化生产过程。首先验证Aspen Plus应用于γ-十一内酯反应精馏工艺模拟的可行性,建立反应精馏稳态模型;其次考察理论板数、回流比(RR)、塔顶采出与进料量摩尔比(D∶F)等7个因素对γ-十一内酯收率的影响;最后对影响显著的5个因素综合考察其交互作用,建立数学模型,并通过实验验证模型的可靠性。结果表明所建立的数学模型可在一定范围内描述γ-十一内酯收率与操作参数的关系,并求得RR为6.5、反应段持液量V为59.6 mL、D∶F为0.6、进料流量F为0.108 mol/h、进料组分摩尔比n(C8)∶n(C3)为15时,γ-十一内酯收率最高,为63.01%,相比传统工艺提高30%以上,实现了生产连续化。

A reactive distillation process was proposed for synthesizing Undecan-4-olide to improve the low production yield and the complex operations of the conventional process.The feasibility of using Aspen Plus for the process simulation was verified and a steady-state model was established.Then the effects to the yield of undecan-4-olide were investigated through 7 different factors including the number of stages in rectifying and stripping section respectively,the reflux ratio,the mole ratio of distillation to feed flow,etc.Furthermore,based on a comprehensive investigation of the interactions of5factors which had significant influences on the yield of undecan-4-olide,a mathematical model was built and its feasibility was evaluated by lab-scale experiments.The results show that,in certain ranges,the model can successfully represent the relationship between the yield and 5 factors and the maximum of the yield is 63.01% when the reflux ratio is6.5,the liquid holdup is 59.6mL,the mole ratio of distillation to feed flow is 0.6,the feed flow rate is0.11mol/h and the mole ratio of n-octanol to acrylic-acid is15.Comparing to the conventional process,the production yield increased over30%and the continuous process was achieved.