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以马来海松酸和正辛醇为原料,对甲苯磺酸为催化剂,正辛烷为带水剂,合成了环保增塑剂马来海松酸三正辛酯。考察了醇酸摩尔比、催化剂用量、反应时间、带水剂用量和反应温度对酯化反应的影响,经单因素实验得到的最佳工艺条件为:n(马来海松酸)∶n(正辛醇)=1∶4.5,催化剂用量为马来海松酸质量的3.6%,带水剂用量为马来海松酸质量的17.5%,反应温度180～200℃,N2保护下反应8.3 h,产物为浅黄色透明油状液体,产率92.3%,经HPLC测定酯色谱纯度为99.24%,1HNMR及FTIR对产物进行了结构表征,元素分析确定了产物分子式为C48H82O6,GPC测得其重均相对分子质量为755。测定了其酸值、加热减量、开口闪点、体积电阻、黏度、热重曲线等,结果表明,马来海松酸三正辛酯符合增塑剂的性能要求。
Maleated pimaric acid and n-octanol as raw materials, p-toluenesulfonic acid as a catalyst, n-octane as water-bearing agent, the synthesis of an environmentally friendly plastic mariplatic acid tri-n-octyl ester. The effects of molar ratio of alkyd, amount of catalyst, reaction time, the amount of water-carrying agent and reaction temperature on the esterification reaction were investigated. The optimum technological conditions were as follows: n (maleic pimaric acid): n Octanol) = 1: 4.5, the amount of catalyst was 3.6% of the mass of maleopimaric acid, the amount of water-borne agent was 17.5% of the mass of maleopimaric acid, the reaction temperature was 180 ~ 200 ℃, the reaction was carried out under N2 for 8.3 h, The yield was 92.3%. The chromatographic purity was 99.24% by HPLC. The product was characterized by 1HNMR and FTIR. The product was identified as C48H82O6 by elemental analysis. The weight average molecular weight was 755. The acid value, heating loss, opening flash point, volume resistivity, viscosity and thermogravimetric curve were measured. The results showed that the tri-n-octyl maleate could meet the performance requirements of plasticizer.