邻苯二胺席夫碱铜催化氧化松香

Oxidation of Rosin with o-phenylenediamine Schiff Base-Cu^(2+) Complex as Catalyst

合成了邻苯二胺席夫碱铜配合物,以其为催化剂催化H2O2氧化松香,采用正交实验法对氧化条件进行了优化,并对松香氧化产物的结构进行了表征,实验结果表明,氧化反应的各因素的重要性次序为:反应温度>H2O2用量>催化剂用量>反应时间;在无水乙醇作溶剂,邻苯二胺席夫碱铜催化剂用量为0.2%(m/m),反应温度70℃,反应时间3 h,30%H2O2用量为松香∶H2O2=1∶1(m/V)时,最大的转化率为73.9%;红外光谱、紫外光谱、高效液相色谱和气质联用测试表明,松香经邻苯二胺席夫碱铜配合物催化氧化后,在分子结构中产生苯基、羟基、羰基等官能团,主要生成了脱氢枞酸、7-羟基脱氢枞酸、7β-羟基脱氢枞酸和7-羰基脱氢枞酸等氧化产物。

o-phenylenediamine schiff base-Cu^2＋ complex was prepared from o-phenylenediamine schiff base and cupric acetate, characterized by IR and UV spectra. Orthogonal experiment on oxidation of rosin by H2O2 was explored with the complex as catalyst. The result showed that temperature had the greatest influence on the reaction, followed by H2O2 dosage, catalyst dosage and duration of the reaction. The optimum conditions for oxidation： 0.2% of catalyst dosage, 30% of H2O2 dosage of rosin V ： H2O2 = 1 ： 1 at 70℃ for 3 hours in absolute ethyl alcohol. The conversion rate of oxidation reaction could reach 73.9%. Determination by IR, UV, HPLC and GC-MS indicated that after the reaction, there were phenyl, hydroxyl and carbonyl groups in the oxidized products. And dehydroabietic acid, 7-hydroxyl dehydroabietic acid, 7β-hydroxyl dehydroabietic acid and 7- keto dehydroabietic acid were produced.