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Integrating Ring-Size Adjustable Cycloalkyl and Benzhydryl Groups as the Steric Protection in Bis(arylimino)trihydroquinoline-Cobalt Catalysts for Ethylene Polymerization
European Journal of Inorganic Chemistry ( IF 2.2 ) Pub Date : 2021-09-07 , DOI: 10.1002/ejic.202100573 Randi Zhang 1 , Irina V. Oleynik 2 , Jianqing Li 3 , Gregory A. Solan 4 , Yanping Ma 1 , Liqun Jin 3 , Ivan I. Oleynik 2 , Xinquan Hu 3 , Wen-Hua Sun 5
European Journal of Inorganic Chemistry ( IF 2.2 ) Pub Date : 2021-09-07 , DOI: 10.1002/ejic.202100573 Randi Zhang 1 , Irina V. Oleynik 2 , Jianqing Li 3 , Gregory A. Solan 4 , Yanping Ma 1 , Liqun Jin 3 , Ivan I. Oleynik 2 , Xinquan Hu 3 , Wen-Hua Sun 5
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Combined condensation and complexation of 2-acetyl-5,6,7-trihydroquinolin-8-one, cobalt(II) chloride and the corresponding aniline has been employed as an effective one-pot route to the 2-(1-(arylimino)ethyl)-8-arylimino-5,6,7-trihydroquinoline-cobalt(II) chlorides (aryl=2-Me-4-(CHPh2)-6-(C5H9)C6H2 Co1, 2-Me-4-(C5H9)-6-(CHPh2)C6H2 Co2, 2-(C5H9)-4-Me-6-(CHPh2)C6H2 Co3, 2-(C5H9)-4,6-(CHPh2)2C6H2 Co4, 2-(C6H11)-4,6-(CHPh2)2C6H2 Co5, 2-(C8H15)-4,6-(CHPh2)2C6H2 Co6, 2-F-4,6-(CHPh2)2C6H2 Co7, 2-Cl-4,6-(CHPh2)2C6H2 Co8, 2-Me-4,6-(CHPh2)2C6H2 Co9). All complexes have been well characterized including by single crystal X-ray diffraction for Co3. On activation with either MAO or MMAO, Co1 was the most active for ethylene polymerization with the MAO-activated precatalyst reaching a peak level at 60 °C (up to 13.66×106 g (PE) mol−1(Co) h−1). By varying the electronic and steric properties of the ortho- and/or the para-substituents of the N-aryl groups, excellent control over molecular weight could be achieved with values falling in the range 0.97–101.63 kg mol−1 obtainable. Notably, with a benzhydryl group positioned on the ortho-position of the N-aryl group, a significant enhancement of the molecular weight was observed, while the least bulky ortho-cyclopentyl substituent led to increased catalytic activity. As a final point, distinctive microstructural characteristics of the polyethylenes were observed with Co1/MAO producing near quantitative levels of vinyl end groups.
中文翻译：
在乙烯聚合的双（芳基亚氨基）三氢喹啉-钴催化剂中整合环大小可调的环烷基和二苯甲基作为空间保护
2-乙酰基-5,6,7-三氢喹啉-8-酮、氯化钴 (II) 和相应苯胺的联合缩合和络合已被用作生成 2-(1-(芳基亚氨基)乙基)-8-芳基亚氨基-5,6,7-三氢喹啉-钴(II)氯化物(芳基=2-Me-4-(CHPh 2 )-6-(C 5 H 9 )C 6 H 2 Co1 , 2- Me-4-(C 5 H 9 )-6-(CHPh 2 )C 6 H 2 Co2 , 2-(C 5 H 9 )-4-Me-6-(CHPh 2 )C 6 H 2 Co3 , 2- (C 5 H 9)-4,6-(CHPh 2 ) 2 C 6 H 2 Co4 , 2-(C 6 H 11 )-4,6-(CHPh 2 ) 2 C 6 H 2 Co5 , 2-(C 8 H 15 )- 4,6-(CHPh 2 ) 2 C 6 H 2 Co6 , 2-F-4,6-(CHPh 2 ) 2 C 6 H 2 Co7 , 2-Cl-4,6-(CHPh 2 ) 2 C 6 H 2 Co8 , 2-Me-4,6-(CHPh2 ) 2 C 6 H 2 Co9 )。所有配合物都已被很好地表征，包括Co3 的单晶 X 射线衍射。在用 MAO 或 MMAO 活化时，Co1对乙烯聚合最活跃，MAO 活化的预催化剂在 60 °C 达到峰值水平（高达 13.66×10 6 g (PE) mol -1 (Co) h -1）。通过改变N-芳基的邻位和/或对位取代基的电子和空间性质，可以实现对分子量的出色控制，数值范围为 0.97–101.63 kg mol-1可获得。值得注意的是，当二苯甲基位于N-芳基的邻位时，观察到分子量显着增加，而体积最小的邻环戊基取代基导致催化活性增加。最后一点，观察到聚乙烯具有独特的微观结构特征，Co1 /MAO 产生接近定量水平的乙烯基端基。
更新日期：2021-10-08
中文翻译：
在乙烯聚合的双（芳基亚氨基）三氢喹啉-钴催化剂中整合环大小可调的环烷基和二苯甲基作为空间保护
2-乙酰基-5,6,7-三氢喹啉-8-酮、氯化钴 (II) 和相应苯胺的联合缩合和络合已被用作生成 2-(1-(芳基亚氨基)乙基)-8-芳基亚氨基-5,6,7-三氢喹啉-钴(II)氯化物(芳基=2-Me-4-(CHPh 2 )-6-(C 5 H 9 )C 6 H 2 Co1 , 2- Me-4-(C 5 H 9 )-6-(CHPh 2 )C 6 H 2 Co2 , 2-(C 5 H 9 )-4-Me-6-(CHPh 2 )C 6 H 2 Co3 , 2- (C 5 H 9)-4,6-(CHPh 2 ) 2 C 6 H 2 Co4 , 2-(C 6 H 11 )-4,6-(CHPh 2 ) 2 C 6 H 2 Co5 , 2-(C 8 H 15 )- 4,6-(CHPh 2 ) 2 C 6 H 2 Co6 , 2-F-4,6-(CHPh 2 ) 2 C 6 H 2 Co7 , 2-Cl-4,6-(CHPh 2 ) 2 C 6 H 2 Co8 , 2-Me-4,6-(CHPh2 ) 2 C 6 H 2 Co9 )。所有配合物都已被很好地表征，包括Co3 的单晶 X 射线衍射。在用 MAO 或 MMAO 活化时，Co1对乙烯聚合最活跃，MAO 活化的预催化剂在 60 °C 达到峰值水平（高达 13.66×10 6 g (PE) mol -1 (Co) h -1）。通过改变N-芳基的邻位和/或对位取代基的电子和空间性质，可以实现对分子量的出色控制，数值范围为 0.97–101.63 kg mol-1可获得。值得注意的是，当二苯甲基位于N-芳基的邻位时，观察到分子量显着增加，而体积最小的邻环戊基取代基导致催化活性增加。最后一点，观察到聚乙烯具有独特的微观结构特征，Co1 /MAO 产生接近定量水平的乙烯基端基。
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