摘要
以马来海松酸和月桂醇为原料,对甲苯磺酸为催化剂,正辛烷为带水剂,合成了增塑剂马来海松酸三月桂酯。考察了各因素对酯化反应的影响,经正交试验得到的最佳工艺条件为:n(马来海松酸)∶n(月桂醇)1∶5,催化剂用量为马来海松酸质量的3.6%,反应温度200～210℃,带水剂正辛烷15 mL,N2保护下反应8 h,产物为浅黄透明油状液体。通过HPLC测定酯色谱纯度为99.14%,采用1H NMR、13C NMR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C60H106O6。测得其酸值0.98 mg/g、加热减量≤0.08%、体积电阻率2.6×1011Ω.m、开口闪点269℃、凝固点-55℃、密度0.980 g/cm3、折光率1.484 6、含水量0.08%、黏度0.200 Pa.s、测定了其热重-差热曲线,结果表明,马来海松酸三月桂酯色泽浅,体积电阻率大,闪点高,黏度低,加热后酸值、色泽与加热前变化较小,耐挥发性好,符合增塑剂的要求,且一些指标比同类型产品性能好。
The plasticizer tri-lauryl maleopimarate was synthesized from maleopimaric acid（MPA） and lauryl alcohol using p-toluenesulfonic acid as catalyst and n-octane as water entrainer.The optimal synthesis conditions were as follows： n（MPA） ∶n（lauryl alcohol）1 ∶5,catalyst dosage（3.6 % of mass MPA）,the water entrainer n-octane 15 mL,reaction time 8 h,reaction temperature 200-210 ℃ under nitrogen atmosphere.The contents of tri-lauryl maleopimarate reached 99.14 % by HPLC.The structure of tri-lauryl maleopimarate was characterized by FT-IR,1H NMR and 13C NMR respectively.The molecular formula of tri-lauryl maleopimarate determined by elementary analysis was C60H106O6.The properties of the product were as follows： acid value 0.98 mg/g,heat weight loss 0.08 %,volume electric resistivity 2.6×1011Ω·m,open-cup flashing point 269 ℃,freezing point-55 ℃,density 0.980 g/cm3,index of refraction 1.484 6,moisture content ≤0.08 %,viscosity 0.200 Pa·s,respectively.TG-DSC curve of product was also measured.The results confirmed that it could satisfy the requirements of plasticizer.
出处
《林产化学与工业》
EI
CAS
CSCD
北大核心
2011年第4期46-52,共7页
Chemistry and Industry of Forest Products
基金
广西科学研究与技术开发资金资助项目(桂科攻0895003-9)
关键词
马来海松酸
马来海松酸三月桂酯
增塑剂
月桂醇
合成
maleopimaric acid
tri-lauryl maleopimarate
plasticizer
lauryl alcohol
synthesis
