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Synthesis and structural characterization of zirconium complexes supported by tridentate pyrrolide-imino ligands with pendant N-, O- and S-donor groups and their application in ethylene polymerization†
New Journal of Chemistry ( IF 2.7 ) Pub Date : 2017-12-18 00:00:00 , DOI: 10.1039/c7nj04074a
A. C. Pinheiro 1, 2, 3, 4 , S. M. da Silva 1, 2, 3, 4 , T. Roisnel 5, 6, 7, 8, 9 , E. Kirillov 5, 6, 7, 9, 10 , J.-F. Carpentier 5, 6, 7, 9, 10 , Osvaldo L. Casagrande 1, 2, 3, 4
Affiliation  

Zirconium complexes {L}ZrClx(THF)n [L = 2-(C4H3N-2′-CH[double bond, length as m-dash]N)C2H4NHPh, x = 3, n = 1, 2a; L = 2-(C4H3N-2′-CH[double bond, length as m-dash]N)C6H4-2-OPh, x = 3, n = 0, 2b; L = 2-(C4H3N-2′-CH[double bond, length as m-dash]N)C6H4-2-SPh, x = 3, n = 1, 2c; L = 2-(C4H3N-2′-CH[double bond, length as m-dash]N)CH2C6H4-2-OMe, x = 3, n = 0, 2d; L = 2-(C4H3N-2′-CH[double bond, length as m-dash]N)C2H4NPh, x = 2, n = 0, 4a] were prepared and characterized by elemental analysis, NMR spectroscopy, and by X-ray crystallography for 2a and 4a. In the solid state, 2a and 4a are monomeric with the pyrrolide-imino-amine adopting a mer-configuration. Upon activation with methylaluminoxane (MAO), all Zr(IV) precatalysts were active in ethylene polymerization and exhibited high thermal stability operating effectively at 100 °C with activities up to 453 kg(PE) mol[Zr]−1 h−1. The high-density polyethylenes produced are strictly linear with melting temperatures in the range of 134–136 °C, and crystallinities varying from 56% to 70%.

中文翻译:

具有N-O-S-侧链供体基团的三齿吡咯化物-亚氨基配体负载的锆配合物的合成,结构表征及其在乙烯聚合中的应用

锆配合物{L} ZrCl x(THF)n [L = 2-(C 4 H 3 N-2'-CH [双键,长度为m-破折号]N)C 2 H 4 NHPh,x = 3,n = 1,2a ; L = 2-(C 4 H 3 N-2′-CH [双键,长度为m-破折号]N)C 6 H 4 -2-OPh,x= 3,n0,2b;L = 2-(C 4 H 3 N-2′-CH [双键,长度为m-破折号]N)C 6 H 4 -2-SPh,x= 3,n1、2c;L = 2-(C 4H 3 N-2'-CH [双键,长度为m-破折号]N)CH 2 C 6 H 4 -2-OMe,x = 3,n = 0,2d;L = 2-(C 4 H ^ 3 N-2'- CH [双键,长度为m-破折号]N)C号2 ħ 4 NPH,X = 2,Ñ = 0,图4a ]的制备和表征通过元素分析,NMR谱,并通过X射线晶体学对于2a4a。在固态下,图2a图4a是单体与吡咯亚氨基胺采用聚体-配置。在用甲基铝氧烷(MAO)活化后,所有Zr(IV)预催化剂均在乙烯聚合反应中具有活性,并显示出高的热稳定性,可在100°C下有效运行,且活性高达453 kg(PE)mol [Zr] -1 h -1。所生产的高密度聚乙烯在134-136°C的熔融温度范围内具有严格的线性,结晶度从56%到70%不等。
更新日期:2017-12-18
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