C22-脂环族三羧酸（酐）的合成工艺改进

Improvement on Synthesis of C22-cycloaliphatic Tricarboxylic Acid （Anhydride）

介绍了一种生物基多官能团有机酸——C22-脂环族三羧酸(酐)的改进合成工艺,并与其相关的文献报道进行了比较。在单质碘的催化作用下,从海蓬籽油制备的共轭亚油酸与顺丁烯二酸酐进行Diels-Alder反应合成了上述产物;通过L9(34)正交试验优化了合成工艺条件;选用正庚烷为溶剂分离产物,并经FT-IR、MS和NMR证实。正交试验得到的优化工艺条件为:顺丁烯二酸酐与共轭亚油酸的物质的量比为1.2、催化剂用量0.2wt%、反应温度60℃、反应时间2.0h,此条件下产率高达96.5%。改进合成工艺具有低温、常压、高效、产物分离相对简单等优点。

The improved synthetic process for the preparation of C22-cycloaliphatic tricarboxylic acid(anhydride),a bio-based multifunctional organic acid,was present and compared with that reported in the other publications.In order to obtain this product,Diels-Alder reaction of conjugated linoleic acid derived from salicornia herbacea seed oil with maleic anhydride,was carried out using iodine as a catalyst.An orthogonal test design L9(34)was applied to determine the optimum condition for the preparation.The n-heptane was chosen as the solvent to separate the product which was confirmed by FT-IR,MS and NMR.The optimum conditions were obtained as follow:mass ratio of substances of maleic anhydride to conjugated linoleic acid of 1.2,dosage of catalyst of 0.2 wt%(in respect to the total mass of the reactants),reaction temperature of 60℃and reaction time of 2.0 h,under which the yield could reach 96.5%.The improved synthetic process showed various advantages such as low-temperature,atmosphericpressure,high-efficiency,and relatively simple product separation.