引用本文:
马楷, 刘绍英, 姚洁, 王公应. 金属醋酸盐催化合成聚丁二酸乙二醇酯预聚体和碳酸二甲酯[J]. 应用化学,
2010, 27(11): 1276-1281.
doi:
10.3724/SP.J.1095.2010.00076
Citation: MA Kai, LIU Shao-Yinga, YAO Jie, WANG Gong-Ying. Simultaneous Synthesis of Poly(ethylene glycol succinate) Oligomers and Dimethyl Carbonate Using Metal Acetates as Catalysts[J]. Chinese Journal of Applied Chemistry, 2010, 27(11): 1276-1281. doi: 10.3724/SP.J.1095.2010.00076
Citation: MA Kai, LIU Shao-Yinga, YAO Jie, WANG Gong-Ying. Simultaneous Synthesis of Poly(ethylene glycol succinate) Oligomers and Dimethyl Carbonate Using Metal Acetates as Catalysts[J]. Chinese Journal of Applied Chemistry, 2010, 27(11): 1276-1281. doi: 10.3724/SP.J.1095.2010.00076
金属醋酸盐催化合成聚丁二酸乙二醇酯预聚体和碳酸二甲酯
摘要:
研究了醋酸盐催化碳酸乙烯酯(EC)和丁二酸二甲酯(DS)同时合成聚丁二酸乙二醇酯(PES)预聚体和碳酸二甲酯(DMC)的耦合反应新工艺。采用气相色谱-质谱联用定性分析馏分组成;红外光谱、核磁共振表征了预聚物的结构;采用乌式粘度计测试了预聚物的特性粘数;气相色谱定量测定馏分碳酸二甲酯的收率以考察耦合反应的进度。以对该反应催化效果最佳的无水醋酸锂为催化剂考察了物料配比、反应温度、反应时间、催化剂用量对耦合反应的影响,结果表明,最佳的工艺条件为:反应温度195~200℃,n(EC):n(DS)=2:1,n(cat):n(EC+DS)=0.02:1,反应时间为2h,耦合反应所得的DMC收率为48.0%,聚丁二酸乙二醇酯预聚物的特性粘数为0.3787。
English
Simultaneous Synthesis of Poly(ethylene glycol succinate) Oligomers and Dimethyl Carbonate Using Metal Acetates as Catalysts
Abstract:
Simultaneous synthesis of poly(ethylene glycol succinate) oligomers and dimethyl carbonate(DMC) was achieved by coupling reaction of ethylene carbonate(EC) and dimethyl succinate(DS) over various metal acetate catalysts.The effluent of coupling reaction was confirmed by GC-MS qualitative analysis.The structure of poly(ethylene glycol succinate) oligomeric product was characterized and assured by 1H NMR and FTIR spectra,and the intrinsic viscosity of poly(ethylene glycol succinate) oligomers was tested by the Ubbelohde type viscometer.The yield of DMC was gained by gas chromatography quantitative analysis,and the extent of coupling reaction could be calculated by the yield of DMC.Results showed that the lithium acetate has the highest catalytic activity.Using this compound as catalyst,the effects of experimental parameters including the molar ratio of EC to DS,reaction temperature,reaction time and amount of catalyst on the coupling reaction were investigated.The optimized reaction conditions are as follows:reaction temperature is in the range of 195 to 200℃,molar ratio of EC to DS is 2:1,the molar fraction of catalyst is about 2%,reaction time is 2 h.Under these conditions,the yield of DMC was 48.0%;the intrinsic viscosity[η]of poly(ethylene glycol succinate) oligomers was 0.3787 dL/g.
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