丙烯酸松香加成物与GMA酯化物的合成与表征  

Synthesis and Characterization of Ester of Acrylic Rosin Adduct and GMA

作　　者：许建本 余彩莉[1] 边峰[1] 张发爱[2] XU Jianben YU Caili BIAN Feng ZHANG Faai(Coltege of Chemistry and Biology Engineering,Guilin University of Technology, Guilin 541004, China College of Material Science and Engineering,Guilin University of Technology, Guilin 541004, China)

机构地区：[1]桂林理工大学化学与生物工程学院,广西桂林541004 [2]桂林理工大学材料科学与工程学院,广西桂林541004

出　　处：《生物质化学工程》2017年第4期47-52,共6页Biomass Chemical Engineering

基　　金：国家自然科学基金资助项目(31160148);广西自然科学基金重点项目资助(2012GXNSFDA053006)

摘　　要：以丙烯酸松香加成物(RA)和甲基丙烯酸缩水甘油酯(GMA)为单体,三乙胺为催化剂,对苯二酚为阻聚剂,在有机溶剂甲苯中合成了RA与GMA酯化物(RAG),采用单因素和正交试验对酯化反应进行优化。通过傅里叶变换红外光谱(FT-IR)、凝胶渗透色谱(GPC)、黏度计、核磁共振氢谱(~1H NMR)和热重(TG)对酯化物进行了分析与表征。结果表明,RA与GMA酯化物较优合成条件为n_(GMA)∶n_(RA)=2∶1,三乙胺用量为RA质量的0.5%,120℃下反应4 h,该条件下合成的酯化物为深黄棕色澄清液体,酯化率为99.5%,数均相对分子质量为547,重均相对分子质量为848,25℃下测得其质量分数51%甲苯溶液的黏度为10 mPa·s。FT-IR和~1H NMR分析表明成功合成了RA与GMA酯化物。TG分析表明酯化物热稳定性高于丙烯酸松香加成物。The ester（ RAG） was synthesized with acrylic rosin adduct（ RA） and glycidyl methacrylate（ GMA） as monomers,triethylamine as catalyst,hydroquinone as inhibitor in toluene solution. The esterification reaction conditions were optimized by single factor experiment and orthogonal experiments. The RAG was analyzed and characterized by Fourier transform infrared spectroscopy（ FT-IR）,gel permeation chromatography（ GPC）,viscometer,nuclear magnetic resonance（~1H NMR）,and thermal gravimetric（ TG） analysis. The results showed that the optimum conditions were the molar ratio of GMA and RA at 2 ∶ 1,the dosage of triethylamine 0. 5 %（ based on RA weight）,120 ℃ and 4 h. Under these conditions,the ester was deep yellowish brown clear liquid,the esterification rate was 99. 5 %,the number average relative molecular weight was 547,the weight average relative molecular weight was 848,and the viscosity of the ester in toluene was 10 mPa·s at 25 ℃ with the mass fraction of 51 %.The FT-IR and ~1 H NMR showed that RAG was successfully prepared. The TG showed that the thermal stability of the ester was higher than that of the acrylic rosin adduct.

关 键 词：丙烯酸松香加成物 甲基丙烯酸缩水甘油酯 溶剂法 酯化物 

分 类 号：TQ351.471[化学工程]