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通过配位聚合合成并表征正己基异氰酸酯与3-(三乙氧基甲硅烷基)丙基异氰酸酯的无规共聚物和嵌段共聚物

Synthesis and Characterization of Statistical and Block Copolymers of n-Hexyl Isocyanate and 3-(Triethoxysilyl) Propyl Isocyanate via Coordination Polymerization.

作者信息

Panteli Maria, Mantzara Dimitra, Katara Aikaterini, Choinopoulos Ioannis, Pitsikalis Marinos

机构信息

Industrial Chemistry Laboratory, Department of Chemistry, National and Kapodistrian University of Athens, Panepistimiopolis Zografou, 15771 Athens, Greece.

出版信息

Polymers (Basel). 2023 Oct 17;15(20):4113. doi: 10.3390/polym15204113.

DOI:10.3390/polym15204113
PMID:37896356
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC10610266/
Abstract

Well-defined statistical copolymers of n-hexyl isocyanate, HIC, and 3-(triethoxysilyl)propyl isocyanate, TESPI, were synthesized via coordination polymerization mechanism, employing a chiral half-titanocene complex as initiator. The monomer reactivity ratios of the statistical copolymers were calculated using linear graphical methods and the computer program COPOINT in the frame of the terminal model. The molecular and structural characteristics of the copolymers were also calculated. The kinetics of the thermal decomposition of the statistical copolymers was studied by Thermogravimetric Analysis, TGA, and Differential Thermogravimetry, DTG, and the activation energy of this process was calculated employing several theoretical models. In addition, block copolymers constituted from PHIC and PTESPI blocks were synthesized by sequential coordination polymerization. All samples were characterized by nuclear magnetic resonance, NMR, spectroscopy and size exclusion chromatography, SEC. The thermal stability of the blocks was also studied by TGA and DTG and compared to the corresponding statistical copolymers.

摘要

通过配位聚合机理，以手性半茂钛配合物为引发剂，合成了结构明确的正己基异氰酸酯（HIC）与3-（三乙氧基甲硅烷基）丙基异氰酸酯（TESPI）的统计共聚物。采用线性图解法和计算机程序COPOINT在末端模型框架内计算统计共聚物的单体竞聚率。还计算了共聚物的分子和结构特征。通过热重分析（TGA）和微商热重分析（DTG）研究了统计共聚物的热分解动力学，并采用几种理论模型计算了该过程的活化能。此外，通过顺序配位聚合合成了由PHIC和PTESPI嵌段组成的嵌段共聚物。所有样品均通过核磁共振（NMR）光谱和尺寸排阻色谱（SEC）进行表征。还通过TGA和DTG研究了嵌段的热稳定性，并与相应的统计共聚物进行了比较。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a948/10610266/f438f581ae07/polymers-15-04113-g016.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a948/10610266/07c429194425/polymers-15-04113-g013.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a948/10610266/91fe9f041608/polymers-15-04113-g015.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a948/10610266/f438f581ae07/polymers-15-04113-g016.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a948/10610266/dd0b76bed0d3/polymers-15-04113-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a948/10610266/d87d49a8867b/polymers-15-04113-g011.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/a948/10610266/f438f581ae07/polymers-15-04113-g016.jpg

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