环保增塑剂马来海松酸三辛酯的合成及表征
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广西科学研究与技术开发资金资助项目(桂科攻0895003-9)


Synthesis and Structural Characterization of the Environmentally-friendly Plasticizer Tri-n-octyl Maleopimarate
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    摘要:

    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,产物为浅黄透明油状液体,产率92.3%,HPLC测定酯含量为99.24%,1HNMR及FT-IR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测得重均分子质量为755。测定了其酸值、加热减量、开口闪点、体积电阻、粘度、热重曲线等性质,结果表明马来海松酸三正辛酯符合增塑剂的性能要求

    Abstract:

    Abstract:The environmentally-friendly plasticizer tri-n-octyl maleopimarate(n-TOMP) was synthesized by the reaction of Maleopimaric acid (MPA) with n-octanol using p-toluenesulfonic acid(PTSA) as catalyst and n-octane as water entrainer. The optimal reaction conditions were as follows: n(MPA):n(n-octyl) = 1:4.5, PTSA (3.6% of mass of MPA),water entrainer(17.5% of mass of MPA), reaction time 8.3 h and the reaction temperature(180-200℃) under nitrogen. The yield is 92.3% and the content of tri-n-octyl maleopimarate ranged up to 99.24% by HPLC. The structure of tri-n-octyl maleopimarate was confirmed by FT-IR and 1HNMR.The acid value,heat weight loss,open-cup flashing point,volume electric resistivity,viscosity and TG-DSC curve of product were measured. In conclusion, tri-n-octyl maleopimarate can satisfy the requirements of plasticizer.

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王春平,李浩,李鹏飞,雷福厚.环保增塑剂马来海松酸三辛酯的合成及表征[J].精细化工,2011,28(4):

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  • 收稿日期:2010-10-20
  • 最后修改日期:2011-01-28
  • 录用日期:2011-02-16
  • 在线发布日期: 2011-04-12
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