液-液相转移反应萃取法合成戊二醛

A Liquid-Liquid Phase Transfer Reactive Extraction Process for Glutaraldehyde Synthesis

提出了液-液相转移反应萃取法制备成二醛（GA）新工艺。此工艺过程是在相转移催化剂（PTC）与杂多酸（HPA）的参与下，用过氧化氢在有机相氧化环戊烯（CPE），生成的GA被萃取至水相。反应混合物经沉降分去合GA的水层后，有机相（主要含溶剂、催化剂、末反应物和中间产物）方便地循环使用。通过对溶剂、PTC、氧化催化剂、助催化剂的考察，建立了适宜的液-液相转移反应萃取体系。适宜的溶剂是1，2-二氯乙烷（DCE）、适宜的HPA是H3PMo10W2O40、适宜的PTC是三辛基丁基溴化铵（TOBAB）。在优化的条件下GA收率超过70％。

A new process-liquid-liquid phase transfer reactive extraction-for glutaraldehydesynthesis was presented. The process is that cyclopentene (CPE) was oxidized, in the presence of phasetransfer catalyst (PTC) and heteropoly acid (HPA), by hydrogen peroxide in organic phase, and theformed glutaraldehyde was then extracted to water phase. The organic phase, containing solvent, PTC,HPA, unconverted CPE and the intermediates, could be recycled conveniently by settling the reactionfixture and partitioning the water layer in which glutaraldehyde mainly contained. An effective liquidliquid phase transfer reactive extraction system was obtained by screening the solvent, phase transfercatalyst, oxidative catalyst, and cocatalyst. The suitable solvent is l,2-dichloroethane (DCE), thesuitable HPA is H3PMo10W2O40 and the suitable PTC is trioctylbutylammonium bromide (TOBAB).Under the optimum conditions the yield of glutaraldehyde with more than 70% was achieved.