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Elastomeric polyethylenes accessible via ethylene homo-polymerization using an unsymmetrical α-diimino-nickel catalyst
Polymer Chemistry ( IF 4.1 ) Pub Date : 2017-04-05 00:00:00 , DOI: 10.1039/c7py00434f Xinxin Wang 1, 2, 3, 4, 5 , Linlin Fan 1, 2, 3, 4, 5 , Yanping Ma 4, 5, 6, 7, 8 , Cun-Yue Guo 1, 2, 3, 4 , Gregory A. Solan 4, 5, 6, 7, 8 , Yang Sun 4, 5, 6, 7, 8 , Wen-Hua Sun 4, 5, 6, 7, 8
Polymer Chemistry ( IF 4.1 ) Pub Date : 2017-04-05 00:00:00 , DOI: 10.1039/c7py00434f Xinxin Wang 1, 2, 3, 4, 5 , Linlin Fan 1, 2, 3, 4, 5 , Yanping Ma 4, 5, 6, 7, 8 , Cun-Yue Guo 1, 2, 3, 4 , Gregory A. Solan 4, 5, 6, 7, 8 , Yang Sun 4, 5, 6, 7, 8 , Wen-Hua Sun 4, 5, 6, 7, 8
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Five types of unsymmetrical bis(arylimino)acenaphthenes, 1-[2,4,6-(CHPh2)3C6H2N]-2-(ArN)C2C10H6 (Ar = 2,6-Me2Ph L1, 2,6-Et2Ph L2, 2,6-i-Pr2Ph L3, 2,4,6-Me3Ph L4 and 2,6-Et2-4-MePh L5), each containing a single N-2,4,6-tribenzhydrylphenyl group, have been prepared and fully characterized. The interaction of L1–L5 with (DME)NiBr2 (DME = 1,2-dimethoxyethane) afforded the corresponding 1
:1 nickel(II) bromide chelates, LNiBr2 (Ni1–Ni5), in good yield. Distorted tetrahedral geometries are a feature of the X-ray structures of Ni1 and Ni3; broad paramagnetically shifted peaks are seen in the 1H NMR spectra for all the nickel complexes in solution. Upon activation with relatively low amounts of Et2AlCl or Me2AlCl (200–700 equivalents), Ni1–Ni5 exhibited exceptionally high activities for ethylene polymerization (up to 1.07 × 107 g of PE (mol of Ni)−1 h−1), displayed good thermal stability [2.97 × 106 g of PE (mol of Ni)−1 h−1 even at 90 °C] and produced hyperbranched polyethylenes. Dynamic mechanical analysis and stress–strain testing reveal that the polymeric materials possess good elastomeric recovery and high elongation at break, indicating a promising alternative material to thermoplastic elastomers (TPEs).
中文翻译：
通过使用不对称α-二亚氨基镍催化剂的乙烯均聚可得到的弹性聚乙烯
五种不对称的双（芳基）对ena啶，1- [2,4,6-（CHPh 2）3 C 6 H 2 N] -2-（ArN）C 2 C 10 H 6（Ar = 2,6-Me 2博士L1，2,6-的Et 2博士L2，2,6--I-PR 2博士L3，2,4,6--ME 3博士L4和2,6-的Et 2 -4-麦菲L5），每片含已经制备并完全表征了单个N -2,4,6-三苯甲酰基苯基。L1-L5与（DME）NiBr 2的相互作用（DME = 1,2-二甲氧基乙烷）以高收率得到相应的1：1溴化镍（II）螯合物L NiBr 2（Ni1-Ni5）。扭曲的四面体几何形状是Ni1和Ni3的X射线结构的特征。在溶液的所有镍配合物的1 H NMR光谱中均可见到宽的顺磁位移峰。当用相对少量的Et 2 AlCl或Me 2 AlCl（200-700当量）活化时，Ni1-Ni5表现出极高的乙烯聚合活性（高达1.07×10 7 g PE（Ni摩尔）-1 ħ -1），显示良好的热稳定性[2.97×10 6克PE中的镍的（摩尔） -1 ħ -1即使在90℃]和产生的超支化的聚乙烯。动态力学分析和应力应变测试表明，聚合物材料具有良好的弹性回复率和高断裂伸长率，表明它是热塑性弹性体（TPE）的有前途的替代材料。
更新日期：2017-05-04
:1 nickel(II) bromide chelates, LNiBr2 (Ni1–Ni5), in good yield. Distorted tetrahedral geometries are a feature of the X-ray structures of Ni1 and Ni3; broad paramagnetically shifted peaks are seen in the 1H NMR spectra for all the nickel complexes in solution. Upon activation with relatively low amounts of Et2AlCl or Me2AlCl (200–700 equivalents), Ni1–Ni5 exhibited exceptionally high activities for ethylene polymerization (up to 1.07 × 107 g of PE (mol of Ni)−1 h−1), displayed good thermal stability [2.97 × 106 g of PE (mol of Ni)−1 h−1 even at 90 °C] and produced hyperbranched polyethylenes. Dynamic mechanical analysis and stress–strain testing reveal that the polymeric materials possess good elastomeric recovery and high elongation at break, indicating a promising alternative material to thermoplastic elastomers (TPEs).
中文翻译：
通过使用不对称α-二亚氨基镍催化剂的乙烯均聚可得到的弹性聚乙烯
五种不对称的双（芳基）对ena啶，1- [2,4,6-（CHPh 2）3 C 6 H 2 N] -2-（ArN）C 2 C 10 H 6（Ar = 2,6-Me 2博士L1，2,6-的Et 2博士L2，2,6--I-PR 2博士L3，2,4,6--ME 3博士L4和2,6-的Et 2 -4-麦菲L5），每片含已经制备并完全表征了单个N -2,4,6-三苯甲酰基苯基。L1-L5与（DME）NiBr 2的相互作用（DME = 1,2-二甲氧基乙烷）以高收率得到相应的1
：1溴化镍（II）螯合物L NiBr 2（Ni1-Ni5）。扭曲的四面体几何形状是Ni1和Ni3的X射线结构的特征。在溶液的所有镍配合物的1 H NMR光谱中均可见到宽的顺磁位移峰。当用相对少量的Et 2 AlCl或Me 2 AlCl（200-700当量）活化时，Ni1-Ni5表现出极高的乙烯聚合活性（高达1.07×10 7 g PE（Ni摩尔）-1 ħ -1），显示良好的热稳定性[2.97×10 6克PE中的镍的（摩尔） -1 ħ -1即使在90℃]和产生的超支化的聚乙烯。动态力学分析和应力应变测试表明，聚合物材料具有良好的弹性回复率和高断裂伸长率，表明它是热塑性弹性体（TPE）的有前途的替代材料。
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