林产化学与工业2018，Vol.38Issue(2)：133-138,6.DOI:10.3969/j.issn.0253-2417.2018.02.018
异长叶烯酮磺酸的合成及其催化性能
Synthesis and Catalytic Performance of Isolongifolenone Sulfonic Acid
摘要
Abstract
Isolongifolenone sulfonic acid (IFSA) was synthesized by sulfonation of isolongifolenone using concentrated sulfuric acid as the sulfonation reagent and isolongifolenone as the starting material, and the catalysis effect of IFSA was investigated by catalyzing the esterification reaction of dipropylene glycol methyl ether (DPM) and acetic acid (HAc). Effects of the charging sequence,dosage of sulfuric acid, reaction temperature, and the amount of acetic anhydride on the sulfonation reaction were examined,and the suitable sulfonation conditions were determined as follows: the reactants mole ratio of isolongifolenone and H2SO41:1.4; acetic anhydride was used as the solvent, and the mass ratio of isolongifolenone/acetic anhydride was 1:2.0;sulfonation temperature 40℃,reaction time 40 min. The yield of IFSA reached 82.36% in the aforesaid conditions. The catalysis effect of IFSA was compared with other catalysts by catalyzing esterification reaction of dipropylene glycol methyl ether (DPM) and acetic acid(HAc),and test results showed that IFSA was the best than others. Effects of DMP/HOAC molar ratio,dose of IFSA,esterification temperature and time on the esterification reaction were examined, and the suitable esterification conditions were as follows:the molar ratio of DPM and HAc 1:1.5, the mass ratio of isolongifolenone sulfonic acid and DPM 0.045:1, cyclohexane as the water-carrying reagent, esterification temperature 90 ℃, esterification time 6 h. The yield of dipropylene glycol methyl ether acetate (DPMA) reached 96.69% at the aforesaid esterification conditions. In addition, the yield of DPMA was still maintained at more than 90.07 % when IFSA was reused for 3 times. Qualitative analysis, quantitative analysis, and structure characterization of the products were carried out by GC, GC-MS, HPLC, FT-IR, 1H NMR, 13C NMR, X-ray single crystal diffraction methods.关键词
异长叶烯酮/磺化反应/异长叶烯酮磺酸/二丙二醇甲醚乙酸酯Key words
isolongifolenone/sulfonation/isolongifolenone sulfonic acid/dipropylene glycol methyl ether acetate分类
化学化工引用本文复制引用
刘艳方,芮坚,徐徐,谷文,王石发..异长叶烯酮磺酸的合成及其催化性能[J].林产化学与工业,2018,38(2):133-138,6.基金项目
国家重点研发计划项目(2016YFD0600804) （2016YFD0600804）
国家自然科学基金资助项目(31470529) （31470529）
