δ-环戊内酯的制备及其光谱分析

Preparation ofδ-Valerolactone and Its Spectral Analysis

采用溶胶-凝胶法制备了CuO/ZnO/Al2O3,以1,5-戊二醇气相催化脱氢制备δ-环戊内酯为探针反应,评价其催化活性。通过XRD分别检测了新鲜的CuO/ZnO/Al2O3和长周期反应后的CuO/ZnO/Al2O3,揭示了CuO/ZnO/Al2O3微观结构和内在规律,发现金属离子之间存在协同效应。催化剂失活后,晶体粒径明显增大,出现了ZnO的特征衍射峰。通过1,5-戊二醇、δ-环戊内酯的FTIR光谱分析,揭示其内部化学键和分子结构,产物δ-环戊内酯的纯度很高。通过对δ-环戊内酯及其聚合物的DSC分析检测,发现δ-环戊内酯的稳定性很差,非常容易发生自聚反应,提高单体的稳定性,值得重点关注。本研究为1,5-戊二醇气相催化脱氢制备δ-环戊内酯的中试和工业放大性研究,提供了基础数据和实验依据。

In the study ,CuO/ZnO/Al2 O3 was prepared by sol‐gel method .Its catalytic activity was evaluated by gas‐phase cata‐lytic dehydrogenation of 1 ,5‐Pentanediol to δ‐valerolactone as a probe reaction .CuO/ZnO/Al2 O3 and long period reactive CuO/ZnO/Al2 O3 were detected by XRD .Micro‐structure and essence disciplinarian of CuO/ZnO/Al2 O3 were disclosed .Metal ions had a cooperative effects during the catalytic dehydrogenation of 1 ,5‐pentanediol to δ‐valerolactone .After CuO/ZnO/Al2 O3 deac‐tivation ,crystal particle size was increased clearly .It were found that characteristic diffraction peaks were caused by the catalyst temperature raising in methanol catalytic synthesis of ZnO .1 ,5‐Pentanediol and δ‐valerolactone were detected by FTIR .Their internal chemical bond and molecular structure were disclosed .The purity of δ‐valerolactone product was very high .δ‐Valerolac‐tone and its polymer were detected by DSC .δ‐Valerolactone possessed with poor stability .Polymerization reaction was easily happened by itself .So it was worth focusing on how to improve the stability of the δ‐valerolactone monomer .This study could provide basic data and experimental basis for gas‐phase catalytic dehydrogenation of 1 ,5‐Pentanediol to δ‐valerolactone in pilot and industrial scale up research .