光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
Spectroscopy and Spectral Analysis
2015年
10期
2810-2813
,共4页
冯世宏%贾太轩%张震斌%高杰%蔺岩%刘自力
馮世宏%賈太軒%張震斌%高傑%藺巖%劉自力
풍세굉%가태헌%장진빈%고걸%린암%류자력
CuO/ZnO/Al2 O3%1 ,5-戊二醇%δ-环戊内酯%催化脱氢
CuO/ZnO/Al2 O3%1 ,5-戊二醇%δ-環戊內酯%催化脫氫
CuO/ZnO/Al2 O3%1 ,5-무이순%δ-배무내지%최화탈경
CuO/ZnO/Al2 O3%1,5-pentanediol%δ-valerolactone%Catalytic dehydrogenation
采用溶胶‐凝胶法制备了CuO/ZnO/Al2 O3,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/Al2 O3和长周期反应后的CuO/ZnO/Al2 O3,揭示了CuO/ZnO/Al2 O3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。
採用溶膠‐凝膠法製備瞭CuO/ZnO/Al2 O3,以1,5‐戊二醇氣相催化脫氫製備δ‐環戊內酯為探針反應,評價其催化活性。通過XRD分彆檢測瞭新鮮的CuO/ZnO/Al2 O3和長週期反應後的CuO/ZnO/Al2 O3,揭示瞭CuO/ZnO/Al2 O3微觀結構和內在規律,髮現金屬離子之間存在協同效應。催化劑失活後,晶體粒徑明顯增大,齣現瞭ZnO 的特徵衍射峰。通過1,5‐戊二醇、δ‐環戊內酯的FTIR光譜分析,揭示其內部化學鍵和分子結構,產物δ‐環戊內酯的純度很高。通過對δ‐環戊內酯及其聚閤物的DSC分析檢測,髮現δ‐環戊內酯的穩定性很差,非常容易髮生自聚反應,提高單體的穩定性,值得重點關註。本研究為1,5‐戊二醇氣相催化脫氫製備δ‐環戊內酯的中試和工業放大性研究,提供瞭基礎數據和實驗依據。
채용용효‐응효법제비료CuO/ZnO/Al2 O3,이1,5‐무이순기상최화탈경제비δ‐배무내지위탐침반응,평개기최화활성。통과XRD분별검측료신선적CuO/ZnO/Al2 O3화장주기반응후적CuO/ZnO/Al2 O3,게시료CuO/ZnO/Al2 O3미관결구화내재규률,발현금속리자지간존재협동효응。최화제실활후,정체립경명현증대,출현료ZnO 적특정연사봉。통과1,5‐무이순、δ‐배무내지적FTIR광보분석,게시기내부화학건화분자결구,산물δ‐배무내지적순도흔고。통과대δ‐배무내지급기취합물적DSC분석검측,발현δ‐배무내지적은정성흔차,비상용역발생자취반응,제고단체적은정성,치득중점관주。본연구위1,5‐무이순기상최화탈경제비δ‐배무내지적중시화공업방대성연구,제공료기출수거화실험의거。
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 .