The Synthesis Of 1,4-Butanediolbis (Anhydrotrimellitate) And It's Application To Study Epoxy Resin

Trimellitic anhydride is an important high temperature epoxy curing agent, it cures resins in a short time and the epoxy resin systems have good physical properties: excellent heat resistance, Mechanical properties, electrical properties, and chemical resistance and so on. But the development is limited by it's "high-melting point", which makes the need of harsh conditions and complex operations when using TMA. For a long time, it's always the research hotspot that obtaining a new anhydride derivative with lower melting point and higher activity in a lower or room temperature by using physical or chemical means. In this paper, a new derivatives of TMA with low melting point was obtained by the selective esterification, which reacted with the carboxyl group, as well as retaining the anhydride groups who plays a role of curing. As a result, the current difficulties mentioned above were overcome and the application of TMA was extended and promoted. The specific work as follows:In the first stage, by using TMA and thionyl chloride as raw materials and pyridine as a catalyst, an acylation reaction was occurred under certain conditions. The optimum process conditions were determined as: reaction temperature of 70?, reaction time of 7h,the quantity of thionyl anhydride of 5 times more than the mass of TMA, and the products' yield is 96.5%. In addition, the expected products was proved as trimellitic anhydride chloride(TMAC) by FT-IR and1 HNMR.In the second stage, by using TMAC and 1,4-butylene glycol as raw materials and pyridine as a catalyst, an esterification reaction was occurred under certain conditions. The optimum process conditions were determined as: reaction temperature of 85?, reaction time of 2h, the ratio of row materials of 1:0.5:1.05. Then, the products' yield is 86.36% and the melting point of the products is measured as 69.8~70.1?. In addition, the expected products was proved as 1,4-Butylene glycol bis(anhydrotrimellitate)(TMB) by1 HNMR.On the basis of the synthetic work before, a conclusion was got that there was little difference in the heat resistance, tensile and bending strength between the two epoxy resinsystems of TMA and TMB. The temperature of TMB/resin system when the weight lost50% was measured higher than the TMA/resin system. In addition, the tensile strength,bending strength and impact strength of the TMB/epoxy resin system were 37.7MPa,128.8MPa and 2.12kJ/m2 respectively. Relatively, there was little difference between the two systems, while the impact strength of TMB system was improved.