离子液体复配溶剂体系改进壬二酸的合成工艺

化工进展

离子液体复配溶剂体系改进壬二酸的合成工艺

阿依夏木古丽·努尔艾买提，吾满江·艾力

中科院新疆理化技术研究所

出版日期:2007-07-25 发布日期:2007-07-25

Improved synthesis process for azelaic acid with ionic liquid as a basic reaction system

Xinjiang Technical Institute of Physics and Chemistry，Chinese Academy of Sciences

Online:2007-07-25 Published:2007-07-25

摘要/Abstract

摘要： 以油酸为原料，50%的H₂O₂为氧化剂，在离子液体作为主要溶剂的条件下，采用钨酸为催化剂所得中间产物用自制的过氧乙酸继续氧化裂解合成了高纯度壬二酸。其中分别对异丙醇、离子液体（BMIMPF6和BMIMBF4）单独作溶剂以及二者复配作溶剂的各种情况作了详细比较。最终经过收率、熔点、FT-IR及HPGC等手段将对上述各产物品质进行了表征与分析，从而得出了合成壬二酸的最佳条件为n(C₁₈H₃₄O₂)∶n(H₂O₂)∶n(H₂WO₄)= 1.0∶3.0∶0.04，V(BMIMPF₆) ∶V(isopropanol)=1∶0.7，所得中间产物中加入300 mL含量为25%的过乙酸在90℃氧化裂解3 h。最终壬二酸收率可达46%，纯度高于95%。

Abstract: The synthesis of high purity azelaic acid through oxidation of oleic acid with 50% hydrogen peroxide was studied by using tungstic acid as a catalyst and ionic liquid as a basic reaction system .Then the epoxide of oleic acid was further oxidized and fragmented by peracetic acid to make azelaic acid. Various solvent conditions were discussed and compared. The optimum technological conditions were determined as follows： The mixture of oleic acid was oxidized by hydrogen peroxide by stirring at 60 ℃ for 1 h with the molar ratio of n(C18H34O2)∶n(H2O2)∶n(H2WO4)= 1.0∶3.0∶0.04，and the mixed solvent of BMIMPF6 and isopropanol was the best reaction system with the blending ratio of 1∶0.7. The semi-finished product was further oxidized by 25% peracetic acid at 90℃for 3 hours . Finally，the compound was confirmed by reaction yield，melting point，IR and GC-MS analysis after purification and the yield of azelaic acid was up to 46% with the purity about 95%.

阿依夏木古丽·努尔艾买提，吾满江·艾力. 离子液体复配溶剂体系改进壬二酸的合成工艺 [J]. 化工进展.