纳迪克酸酐聚酯PVC增塑剂的制备及其性能研究

Preparation and Characterization of Polyester Plasticizer for PVC Derived from NA

以纳迪克酸酐(NA)、甲基丙二醇(MPO)为原料、2-乙基己醇为封端剂、环己烷为带水剂、钛酸四正丁酯为催化剂的条件下,经过缩聚、减压蒸馏制备增塑剂聚纳迪克酸甲基丙二醇酯(P-MPO-NA)。通过对醇酸物质的量比、反应时间、封端剂及催化剂用量的考察,得到反应的最佳工艺条件为:纳迪克酸酐、甲基丙二醇、2-乙基己醇物质的量比为1.0 1∶.20 0∶.60,催化剂质量分数为0.15%,反应时间7 h,酯化率达到99.60%。通过红外光谱分析(FT-IR)、热重分析(TG)等对P-MPO-NA的结构和热稳定性进行了表征。将其与邻苯二甲酸二(2-乙基己基)酯(DOP)、邻苯二甲酸二丁酯(DBP)、柠檬酸三丁酯(TBC)分别加入到聚氯乙烯(PVC)树脂中,进行耐抽出、耐迁移、拉伸强度、断裂伸长率和热稳定性能对比研究。结果表明:该聚酯增塑剂较DOP、DBP、TBC有更好的耐迁移、耐抽出性,并且韧性好,同时提高了PVC的热稳定性。

Poly（2-methyl-1,3-propanediol nadic anhydride）（P-MPO-NA）was synthesized through a polycondensation reaction and reduced pressure distillation with tetra-n-butyl titanate as the catalyst,cyclohexane as dehydrating agent,2-ethyl-hexanol as capping agent,nadic anhydride（NA）and 2-methyl-1,3-propanediol（MPO）as raw material.The influences of reaction conditions,such as stuff ratio,amount of used capping agent and catalyst dosage,reaction time were investigated.The results showed that the optimal reaction conditions were as follows：the molar ratio of NA,MPO and 2-ethyl-hexanol was 1.0∶1.20∶0.60,catalyst（0.15% of total mass）,reaction time 7 h.Esterification yield was 99.60%.FT-IR and TG were used to characterize the structure and thermal stability of P-MPO-NA.P-MPO-NA,DOP,DBP and TBC were respectively added to PVC with the equal quality.Mechanical properties of the plasticized PVC films,as well as tests of migration,tests of exudation,tests of tensile strength and tests of elongation at break were performed in order to evaluate the efficiency of plasticization.The tests indicated that the plasticized sample with P-MPO-NA presented a higher extraction and migration resistance into six solvents and active carbon respectively.The thermal stability of PVC was improved also.