全氟磺酸树脂催化松香树脂酸的异构化反应.PDF

2011, 26(5):161～ 165 Journal of Northwest Forestry University 黄道战, 吴志, 王雪莲 (1. , 530006;2., 530006) 　:研究在95%乙醇中废弃的全氟磺酸树脂膜(简称PFS )催化松香树脂酸异构化反应, 直 接结晶分 枞酸的可行性。结果表明,在常压加热反应条件下, PFS 能够较好地催化松香树脂 酸的异构化反应;催化剂用量和反应温度对树脂酸异构化反应速度和异构反应平衡溶液中枞酸相 对含量有较大的影响;在松香质量为20 g, 溶剂体积为20 mL,PFS 用量为松香质量的20%,反应 溶液沸腾温度条件下反应5 h, 树脂酸异构反应达到平衡,枞酸相对含量高达78%;过滤分 回收 催化剂后,将异构松香溶液直接冷却结晶, 析出枞酸粗产品, 再在 95%乙醇中重结晶提纯3 次, 得 到纯度为95%、产率为35%的枞酸。 :全氟磺酸树脂;松香树脂酸;催化异构;枞酸;直接结晶分 :S789.2　　　:A 　　　:1001-7461(2011)05-0161-05 Isomerization of osin Acids Catalyzed by Perfluorosulfonic Acid esin HUANG Dao-zhan, WU Zhi, WANG Xue-l ian (1.Colleg eof Chemistry and Ecological Eng ineering, Guangxi University f or Nationalities,N anning, Guang xi 530006, China; 2.K ey Laboratory of Develop ment App lication of Forest Chem icals of Guangxi, N anning, Guangxi 530006, China) Abstract:Isomerization reaction of rosin acids catalyzed by rejected perfluorosulfonic acid resin (PFS )in 95 %alcohol for direct separation of abietic acid by crystallization was studied.The results showed that i- somerization of rosin acids catalyzed by PFS could be easily carried out under conventional heating condi- tion.The isomerization reaction rate of rosin acids and equilibrium content of abietic acid were greatly im- proved by the amount of PFS and reaction temperature.The isomerization equilibrium of rosin acids was reached, and abietic acid content was up to 78%under the optimum condition, i.e., rosin 20 g, 95%al- cohol 30 mL, the mass percentage of PFS (based on rosin mss)20%, 5 h of maintaining the boiling state of the mixtures for reaction.After the catalyst was simply separated from the isomerized rosin acids solu- tion by filtration, a crude product was collected by direct cool crystallization and gave abietic acid by three times of re-crystallization in 95%alcohol.The p