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《工程塑料应用》 2020年第05期
DOI:10.3969/j.issn.1001-3539.2020.05.002
N-酰化咪唑啉-2-亚胺镍催化剂制备环烯烃共聚物
李彦青12,肖茹1,蔡正国1
1.东华大学材料科学与工程学院,纤维材料改性国家重点实验室,上海 201620; 2.广西科技大学生物与化学工程学院,广西柳州 545006 
Synthesis of Cyclic Olefin Copolymers Using Nickel Complexes with N-Acylated Imidazolin-2-imine Ligands
Li Yanqing12, Xiao Ru1, Cai Zhengguo1
1. State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620, China; 2. College of Biological and Chemical Engineering, Guangxi University of Science and Technology, Liuzhou 545006, China 
摘要:在助催化剂二氯乙基铝(EtAlCl2)活化作用下,以N-酰化咪唑啉-2-亚胺镍配合物有效催化了降冰片烯/1-己烯共聚,制备出含1-己烯柔性支链的聚(降冰片烯/1-己烯)环烯烃共聚物,研究了助催化剂用量、反应温度及1-己烯反应单体用量对催化剂催化活性及所得聚合物结构和性质的影响。结果表明,N-酰化咪唑啉-2-亚胺镍配合物不仅可高活性催化降冰片烯/1-己烯共聚[催化活性最高达3.88×105 g/(mol·h)],且即使在120℃下仍可有效催化合成出高1-己烯含量的环烯烃共聚物,热稳定性良好;同时,随着EtAlCl2用量和1-己烯反应单体用量增加,聚合物中1-己烯单体插入率逐渐增大,最高可达7.11% (物质的量分数),但配合物催化活性、聚合物数均分子量及玻璃化转变温度呈下降趋势;另外,升高聚合温度有助于提高催化活性及1-己烯单体插入率,但易导致聚合物分子量减小。由此可见,在该催化体系下通过调整EtAlCl2用量,反应温度及1-己烯反应单体用量,即可实现对环烯烃共聚物的结构性能进行有效调控。 
Abstract:The prepared nickel complexes with N-acylated imidazolin-2-imine ligands were used for copolymerizing norbornene with 1-hexene with high catalytic activity to produce cyclic olefin copolymers (COCs) bearing flexible branched chain of 1-hexene in the presence of EtAlCl2, and the effects of EtAlCl2 dosage, polymerization temperature and 1-hexene amount on the catalytic activities of the catalyst system and the structure and performances of the polymer were investigated. The results indicate that the nickel complexes exhibited high catalytic activities [3.88×105 g/(mol·h)] for copolymerization of norbornene and 1-hexene. In particular, the active species is thermally stable and shows high polymerization activities even at 120℃ for preparing COCs with high 1-hexene incorporation rate. Moreover, the copolymerization activity, polymer molecular weight (Mn) and glass transition temperature decrease with the raising of EtAlCl2 dosage and 1-hexene amount, on the contrary, 1-hexene incorporation rate increases up to 7.11 mol%. Furthermore, raising polymerization temperature is favorable to copolymerization activity and 1-hexene incorporation rate in the copolymerization but goes against Mn. So structure and properties of COCs can be controlled in a wide range by the variation of Al/Ni molar ratio, polymerization temperature and 1-hexene amount. 
关键词:镍配合物;降冰片烯;1-己烯;环烯烃共聚物;高活性;热稳定性 
Keywords:nickel complex; norbornene; 1-hexene; cyclic olefin copolymers; high activity; thermal stability 
基金:国家自然科学基金项目(21774018) 
本文引用格式:
李彦青,肖茹,蔡正国. N--酰化咪唑啉-2-亚胺镍催化剂制备环烯烃共聚物[J].工程塑料应用,2020,48(5):6-10.
Li Yanqing,Xiao Ru,Cai Zhengguo. Synthesis of cyclic olefin copolymers using nickel complexes with N--acylated imidazolin-2-imine ligands[J]. Engineering Plastics Application,2020,48(5):6-10. 

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