研究了乙酰丙酮盐催化碳酸乙烯酯(EC)和丁二酸二甲酯(DS)耦合反应合成聚丁二酸乙二酯(PES)预聚体和碳酸二甲酯(DMC)的新工艺。结果表明,乙酰丙酮氧钛对EC和DS耦合反应的催化效果最好。并以乙酰丙酮氧钛为催化剂考察了反应温度、催化剂用量、物料配比、反应时间对耦合反应的影响,得到最佳的工艺条件:反应温度225℃~235℃,n(EC)=0.23 mol,n(DS)=0.1 mol,n(cat)=3.3mol,反应时间3h。在该工艺条件下,DMC收率51.3%,PES预聚体的特性黏数0.1358。
A technology of simultaneous synthesis of poly(ethylene succinate) oligomers and dimethyl carbonate was obtained by coupling reaction of ethylene carbonate and dimethyl succinate through various metal acetylacetone catalysts.The results show that the titanium(IV) oxide acetylacetonate catalyst exhibits the highest activity in this coupling reaction.Under this catalyst,the effects of material ratio,reaction temperature,reaction time,the amount of titanium(IV) oxide acetylacetonate catalyst on the coupling reaction of ethylene carbonate and dimethyl succinate were investigated.The preferable reaction conditions were as followed: the reaction temperature 225 ℃~235 ℃,the molar of dimethyl succinate 0.1 mol,the molar ethylene carbonate of 0.23 mol,and the titanium(IV) oxide acetylacetonate catalyst 3.3 mmol,reaction time 3h.Under the selected reaction conditions,the yield of dimethyl carbonate is 51.3%,intrinsic viscosity of polyethylene succinate is 0.1358 dL/g.
参考文献
[1] | Maeda Y.;Kawasaki N.;Hayashi K.;Aiba S.;Yamamoto N.;Nakayama A. .RING-OPENING COPOLYMERIZATION OF SUCCINIC ANHYDRIDE WITH ETHYLENE OXIDE INITIATED BY MAGNESIUM DIETHOXIDE[J].Polymer: The International Journal for the Science and Technology of Polymers,1997(18):4719-4725. |
[2] | 刘伟,石峰晖,王进锋,蒋志敏,季君晖.高分子量生物可降解聚丁二酸乙二醇酯的合成与表征[J].高分子材料科学与工程,2009(04):8-11. |
[3] | Tserki, V;Matzinos, P;Pavlidou, E;Panayiotou, C .Biodegradable aliphatic polyesters. Part II. Synthesis and characterization of chain extended poly(butylene succinate-co-butylene adipate)[J].Polymer Degradation and Stability,2006(2):377-384. |
[4] | 魏彤,王谋华,魏伟,孙予罕,钟炳.氧化钙室温催化碳酸丙烯酯和甲醇的酯交换合成碳酸二甲酯[J].催化学报,2003(01):52-56. |
[5] | 王小莺,廖凯荣,全大萍,伍青.乙酰丙酮铁催化丙交酯开环聚合的研究[J].高分子学报,2005(01):113-118. |
[6] | 曹平,杨建,杨先贵,姚洁,王越,王公应.有机钛化合物催化碳酸二甲酯与乙酸苯酯合成碳酸二苯酯[J].催化学报,2009(01):65-68. |
- 下载量()
- 访问量()
- 您的评分:
-
10%
-
20%
-
30%
-
40%
-
50%