钛酸四丁酯无溶剂催化合成偏苯三酸酐异十三醇酯

Solvent-free synthesis of benzene-1,2,4-tricarboxylic acid tris-(11-methyl-dodecyl) ester with tetrabuty titanate as catalyst

以钛酸四丁酯为催化剂,在无溶剂条件下催化合成了偏苯三酸酐异十三醇酯,并对影响产率的诸因素进行了考察。其最佳反应条件为n(偏苯三酸酐)∶n(异构十三醇)=1∶4、w(钛酸四丁酯)=0.2%、反应时间3.0 h、反应温度200℃,并且最佳反应条件下酯化反应产率可高达99.58%,测得最佳反应条件下产品酸值小于0.2 mg KOH/g,皂化值为(487±3)mg KOH/g,且测得酯化反应为不可逆一级反应,酯化反应速度常数k 200=3.236 h-1。

Benzene-1,2,4-tricarboxylic acid tris-(11-methyl-dodecyl)ester(BTE)has been solvent-free synthesized using tetrabuty titanate as catalyst.The related factors affecting the yields were investigated.The results showed that the optimum reaction conditions were as follows:trimellitic anhydride/isomeric tridecanol molar ratio 1∶4,the amount of tetra butyl titanate 0.2%of the reactants,reaction time 3.0 h,reaction temperature 200℃.Under the above optimum conditions,the yield reached 99.58%.And the product properties were as follows:acid value<0.2 mg KOH/g;saponification value(487±3)mg KOH/g.It is detected that the esterification of this reaction is a first order irreversible reaction and the rate constant at 200℃is 3.236 h-1.