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Porous polymer monoliths with large surface area and functional groups prepared via copolymerization of protected functional monomers and hypercrosslinking


Maya, F and Svec, F, Porous polymer monoliths with large surface area and functional groups prepared via copolymerization of protected functional monomers and hypercrosslinking, Journal of Chromatography A, 1317 pp. 32-38. ISSN 0021-9673 (2013) [Refereed Article]

Copyright Statement

2013 Elsevier B.V. All rights reserved.

DOI: doi:10.1016/j.chroma.2013.07.073


A new approach to the preparation of porous polymer monoliths possessing both large surface area and functional groups has been developed. The chloromethyl groups of poly(styrene-co-4-acetoxystyrene-co-vinylbenzyl chloride-co-divinylbenzene) monolith enable post-polymerization hypercrosslinking catalyzed by ferric chloride in dichloroethane leading to a multitude of small pores thus enhancing the surface area. The acetoxy functionalities are easily deprotected using hydrazine to produce polar phenolic hydroxyl groups, which would be difficult to obtain by direct copolymerization of hydroxyl-containing monomers. The hypercrosslinking and deprotection reactions as well as their sequence were studied in detail with bulk polymer monoliths containing up to 50% 4-acetoxystyrene and its progress monitored by infrared spectrometry and nitrogen adsorption/desorption measurements. No significant difference was found for both possible successions. All monoliths were also prepared in a capillary column format, then deprotected and hypercrosslinked. Capillary columns were tested for the separation of small molecules using reversed phase and normal phase chromatographic modes. For polymer monoliths containing 50% deprotected 4-acetoxystyrene, column efficiencies of 40,000 plates/m for benzene in reversed phase mode and 31,800 plates/m for nitrobenzene in normal phase mode, were obtained. The percentage of hydroxyl groups in the monoliths enables modulation of polarity of the stationary phase. They also represent functionalities that are potentially suitable for further modifications and formation of new types of stationary phases for liquid chromatography.

Item Details

Item Type:Refereed Article
Keywords:polymers, hypercrosslinking, porous monolith, hypercrosslinked polymer, capillary liquid chromatography, protected monomers, poly(styrene-co-acetoxystyrene-co-divinylbenzene), small molecules
Research Division:Chemical Sciences
Research Group:Analytical chemistry
Research Field:Separation science
Objective Division:Expanding Knowledge
Objective Group:Expanding knowledge
Objective Field:Expanding knowledge in the chemical sciences
UTAS Author:Maya, F (Mr Fernando Maya Alejandro)
ID Code:127856
Year Published:2013
Web of Science® Times Cited:37
Deposited By:Chemistry
Deposited On:2018-08-19
Last Modified:2018-09-07

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