摘要
建立了2,5-二甲基呋喃(DMF)的气相色谱(GC)定量分析方法,跟踪测定DMF在低温下的氧化过程及动力学,用碘量法测定了DMF过氧化物的生成,并测定了DMF的氧化产物。结果表明,DMF与氧气在低温下的氧化呈现表观一级反应,温度为323.15,333.15,343.15,353.15,363.15 K时的反应速率常数分别为:0.004 6,0.006 4,0.008 9,0.011 8,0.015 0 h^(-1),反应表观活化能为29.08 k J/mol。在363.15 K反应10 h,主要氧化产物为5-甲基-2-呋喃甲醇(7.3%),反-3-己烯-2,5-二酮(70.8%),5-甲基-2-呋喃甲醛(13.4%),其他(8.5%)。
Gas chromatography( GC) with area-external standard method was applied to quantitative analysis of DMF and to monitor oxidation process of DMF at low temperatures; peroxide of DMF was detected by iodimetry and oxidation products of DMF was presented after analyzed by GC-MS,IR and1 H NMR.The results showed that: the early oxidation reaction of DMF with oxygen was apparent first-order reaction; at 323. 5,333. 15,343. 15,353. 15 and 363. 15 K,the reaction rate constant respectively was0. 004 6,0. 006 4,0. 008 9,0. 011 8,0. 015 0 h^(-1); the apparent activation energy is 29. 08 k J/mol; after10 h reaction at 363. 15 K,the main oxidation product was 5-methyl-2-furylmethanol( 7. 3%),trans-3-hexene-2,5-dione( 70. 8%),5-furaldehyde( 13. 4%) and other( 8. 5%).
出处
《应用化工》
CAS
CSCD
北大核心
2016年第5期829-832,共4页
Applied Chemical Industry
基金
国家自然科学基金(11462001)