微波辐射下润滑油类双季戊四醇六酯的合成  

Synthesis of lubricating oil dipentaerythritol hexa-esters under microwave radiation

作　　者：张凤秀[1] 张光先[2] 魏世强[3] 

机构地区：[1]西南大学化学化工学院 [2]西南大学物理科学与技术学院 [3]西南大学资源环境学院,重庆400716

出　　处：《化学研究与应用》2006年第11期1360-1364,共5页Chemical Research and Application

基　　金：重点市科学基金攻关项目(6683)资助

摘　　要：Polyol esters of lubricating oil were synthesized by dipentaerythritol（di-PE）with n-Valeric acid,n-Hexanoic acid,n-Heptanoic acid and n-Caprylic acid（C5 to C8 carboxylic acids）under microwave radiation.The best synthetical conditions of di-PE with C5 to C8 carboxylic acids were investigated under microwave radiation.The best molar ratio of C5 to C8 carboxylic acids vs di-PE was 8∶1.The best microwave power was between 300W and 320W.The best composite catalyst was selected,and the ratio of composite catalyst（vitriol oil vs P-Toluene Sulphonic acid）was from 1∶2.5 to 1∶3.0.The esterifiable temperatures of dipentaerythritol hexa-valerianate,dipentaerythritol hexa-caproate,dipentaerythritol hexa-heptylate,dipentaerythritol hexa-caprylate were respectively 114℃～116℃、126℃～128℃、134℃～136℃、140℃～142℃.The yields were at least 93% within 9～10min.The viscosity coefficients were determined by Ubbelohde viscosimeter at 31℃±0.05℃ and were respectively 66.4mm2/s,70.8mm2/s,75.3mm2/s,78.1mm2/s.With the increase of carbon atom number of carboxylic acids,the esterifiable temperatures and viscosities of 3a-3d gradually went up.The structures of 3a-3d were identified by 1H NMR,13C NMR and IR spectra.The refractive indexs of 3a-3d were determined with ZWA-J refractometer.This method is fast,efficient and high-yielding,and may provide a new researchful orientation for traditional technology improvement of esters lubricating oil.Polyol esters of lubricating oil were synthesized by dipentaerythritol （di - PE） with n - Valeric acid, n - Hexanoic acid, n - Heptanoic acid and n - Caprylic acid （C5 to C8 carboxylic acids） under microwave radiation. The best synthetical conditions of di - PE with C5 to C8 carboxylic acids were investigated under microwave radiation. The best molar ratio of C5 to C8 carboxylic acids vs di - PE was 8.1. The best microwave power was between 300W and 320W. The best composite catalyst was selected, and the ratio of composite catalyst （vitriol oil vs P - Toluene Sulphonic acid） was from 1：2.5 to 1：3.0. The esterifiable temperatures of dipentaerythritol hexa - valerianate, dipentaerythritol hexa - caproate, dipentaerythritol hexa - heptylate, dipentaerythritol hexa - caprylate were respectively 114℃～116℃、126℃～128℃、134℃～136℃、140℃～142℃. The yields were at least 93% within 9～10min. The viscosity coefficients were determined by Ubbelohde viscosimeter at 31℃±0.05℃ and were respectively 66.4mm^2/s, 70.8mm^2/s, 75.3mm^2/s, 78.1 mm^2/s. With the increase of carbon atom number of carboxylic acids, the esterifiable temperatures and viscosities of 3a - 3d gradually went up. The structures of 3a - 3d were identified by ^1H NMR, ^13C NMR and IR spectra. The refractive indexs of 3a - 3d were determined with ZWA - J refracto, neter. This method is fast, efficient and high - yielding, and may provide a new researchful orientation for traditional technology improvement of esters lubricating oil.

关 键 词：微波辐射 合成 双季戊四醇 一元羧酸 酯类润滑油 

分 类 号：O623.652[理学—有机化学]