摘要
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 of 5 factors 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 is 6.5,the liquid holdup is 59.6 mL,the mole ratio of distillation to feed flow is 0.6,the feed flow rate is 0.11 mol/h and the mole ratio of n-octanol to acrylic-acid is15.Comparing to the conventional process,the production yield increased over 30% and the continuous process was achieved.
引文
[1]田红玉,魏毅,丁瑞,等.γ-内酯类化合物的合成[J].精细化工,2007,24(8):797-799.
[2]刘伟.γ-十一内酯合成工艺改进[J].精细石油化工,1998,1:22-24.
[3]冯佳佳.γ-十一内酯的合成与提纯研究[D].天津;天津大学,2007.
[4]许保云,江孝平,艾波,等.带有侧线出料的真空间歇精馏法提纯桃醛的研究[J].香料香精化妆品,2016,4(2):1-5.
[5]刘朝明.1800吨/年桃醛生产工艺中分离工段的改进与优化设计[D].安徽:合肥工业大学,2014.
[6]MALONE M F,HUSS R S,DOHERTY M F.Green chemical engineering aspects of reactive distillation[J].Environ Sci Technol,2003,37(23):5325-5330.
[7]SUNDMACHER K,KIENLE A.Reactive Distillation:Status and Future Directions[M].Germany:Wiley-VCHVerlag Gmb H&Co.KGa A,2002.
[8]储伟伟,马宏燎,柏子龙.环戊基甲醚反应精馏模拟与优化[J].现代化工,2017,37(2):173-178.
[9]梁志广,蔡旺锋,张旭斌,等.碳酸甲乙酯反应精馏工艺的设计与优化[J].现代化工,2016,36(12):146-149.
[10]BAO Jie,GAO Buliang,WU Xiaoqun,et al.Simulation of industrial catalytic-distillation process for production of methyl tert-butyl ether by developing user's model on Aspen Plus platform[J].Chemical Engineering Journal,2002,90(3):253-260.
[11]LIN Yuder,CHEN Junhong,CHEN Jiankai,et al.Process alternative for methyl acetate conversion using reactive distillation:Transesterification versus hydrolysis[J].Chemical Engineering Science,2008,63(6):1668-1672.
[12]LUYBEN W L,PSZALGOWSIK K M,SCHAEFER MR,et al.Design and control of conventional and reactive distillation processes for the production of butyl acetate[J].Ind Eng Chem Res,2004,43(25):8014-8020.
[13]LUYBEN W L.Distillation design and control using Aspen simulation[M].America:John Wiley&Sons,Inc,2013.
[14]王传昌,许保云,艾波,等.间歇精馏过程的多目标综合优化研究[J].现代化工,2017,37(5):193-196.