Separation and Purification Technology ( IF 8.1 ) Pub Date : 2023-05-06 , DOI: 10.1016/j.seppur.2023.124022 Zixin Qi , Zhaofeng Zhang , Tianyu Ren , Nan Jiang , Mengfan Wang , Shengping You , Wei Qi , Rongxin Su
Because of the high complexity of the product and the similar physicochemical properties between G and S counterparts, the separation of aromatic monomers is one of the greatest challenges in the lignin chemical valorization, which limits its further utilization and conversion. In this study, the preparation method of the dihydroconiferyl alcohol & dihydrosinapyl alcohol-enriched oil and high purity dihydrosinapyl alcohol from reductive catalytic fractionation products catalyzed by Pd/C was first reported. Moreover, a purification process with alkali extraction - organic solvent extraction - dichloromethane reverse extraction - crystallization in the KOH ethanol solution as the main unit operation was designed. As a result, a monomer-enriched oil in which dihydroconiferyl alcohol (G-3OH) and dihydrosinapyl alcohol (S-3OH) could totally account for more than 83% was obtained, and S-3OH with a purity of 90.2% was separated by crystallization. In addition, this purification process was scaled up to 10 times. The monomer-enriched oil with a G-3OH and S-3OH content of 87.2% was obtained. The recoveries of G-3OH and S-3OH were 81.0% and 91.5%, respectively. The purity of S-3OH was 89.4%, and the recovery was 51.6%. The integrated process realizes the effective separation of the reductive depolymerization products of lignin, which can provide technical support for its industrial production.
中文翻译:
多级萃取结晶分离木质素还原解聚产物中的二氢芥子醇
由于产品的高度复杂性以及G和S对应物之间相似的物理化学性质,芳香单体的分离是木质素化学增值中最大的挑战之一,这限制了其进一步利用和转化。本研究首次报道了Pd/C催化还原催化分馏产物制备富二氢松柏醇&二氢芥子醇油和高纯度二氢芥子醇的方法。并设计了以碱萃取-有机溶剂萃取-二氯甲烷反萃取-KOH乙醇溶液结晶为主要单元操作的纯化工艺。因此,得到二氢松柏醇(G-3OH)和二氢芥子醇(S-3OH)合计占83%以上的富单体油,结晶分离出纯度为90.2%的S-3OH。此外,该纯化过程放大了 10 倍。获得G-3OH和S-3OH含量为87.2%的富含单体的油。G-3OH和S-3OH的回收率分别为81.0%和91.5%。S-3OH的纯度为89.4%,回收率为51.6%。该一体化工艺实现了木质素还原解聚产物的有效分离,为其工业化生产提供技术支持。获得G-3OH和S-3OH含量为87.2%的富含单体的油。G-3OH和S-3OH的回收率分别为81.0%和91.5%。S-3OH的纯度为89.4%,回收率为51.6%。该一体化工艺实现了木质素还原解聚产物的有效分离,为其工业化生产提供技术支持。获得G-3OH和S-3OH含量为87.2%的富含单体的油。G-3OH和S-3OH的回收率分别为81.0%和91.5%。S-3OH的纯度为89.4%,回收率为51.6%。该一体化工艺实现了木质素还原解聚产物的有效分离,为其工业化生产提供技术支持。