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Preparation and characterization of sizable macroporous epoxy resin-based monolithic supports for flow-through systems
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
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2009 (English)In: Journal of Separation Science, ISSN 1615-9306, E-ISSN 1615-9314, Vol. 32, no 15-16, 2608-2618 p.Article in journal (Refereed) Published
Abstract [en]

This paper presents further results from our efforts to prepare sizable macroporous monolithic materials from epoxy resins and polyamines by emulsion polymerization. For their uses as supports in flow systems, the study aimed at developing materials possessing maximum fluid permeability, high mechanical stability, and a controlled porosity and surface area. Characterization of the materials has been carried out using different techniques, focusing on morphological and mechanical features, and on the surface chemistry. Morphology and porosity were studied with SEM, nitrogen adsorption/desorption, mercury intrusion porosimetry (MIP), and (2)H NMR cryoporosimetry. The chemical composition of the bulk structures and their surfaces was studied by means of bulk elemental analysis and X-ray photoelectron spectroscopy, and potentiometric titration was used to assess the relative amounts of amines and epoxy groups. Essentially, the morphological features were a high fluid permeability, but rather low specific surface area. Convective flow was facilitated by large, interconnected, and evenly spaced macropores which were formed by nonporous skeletons of the connected-rod type. Despite the interfacial nature of the polymerization, the bulk and the surface of the fully cured materials showed similar elemental compositions. All materials were found to have a high surface density of hydroxyl groups, which facilitates functionalization reactions.

Place, publisher, year, edition, pages
Wiley InterScience , 2009. Vol. 32, no 15-16, 2608-2618 p.
Keyword [en]
Characterization, Chromatography, Condensation polymerization, Epoxy-amine, Macroporous, Monolithic sorbents
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:umu:diva-25954DOI: 10.1002/jssc.200900242PubMedID: 19670275OAI: oai:DiVA.org:umu-25954DiVA: diva2:235270
Available from: 2009-09-15 Created: 2009-09-15 Last updated: 2017-12-13Bibliographically approved
In thesis
1. New approaches to preparation of macroporous monoliths for use in liquid chromatography
Open this publication in new window or tab >>New approaches to preparation of macroporous monoliths for use in liquid chromatography
2009 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

High performance liquid chromatography (HPLC) is one of the major techniques in separat-ion sciences. Faster separation and higher efficiency are required to meet ever-growing demands. Despite numerous studies and achievements on improving mass transfer in particulate packings discontinuity seems to be the cornerstone drawback in their development. Macroporous continuous beds or monoliths are therefore a promising alternative to the particle medium. This thesis deals with preparation of new monoliths used as carrier for HPLC. Two different approaches were developed for two polymer systems. One was based on polycondensation of epoxy resins and polyamines which were components of an oil-in-water emulsion. An epoxy resin mixture was dispersed in aqueous polyamine phase with the aid of a surfactant. The other involved a traverse of a ready-made polymer solution around its upper critical solution temperature (UCST). In other words, linear polyamides, non-covalently crosslinked polymers, dissolved in a solvent at temperature higher than their UCST followed by slow cooling to below the critical temperature to precipitate the polymers. Partly re-established hydrogen bonds resulted in the formation of crystallites that interconnected into a network structure. Factors controlling morphology and porosity of final products were investigated. The study also deals with surface modifying for chromatographic applications. Functionalization pathways attempted in the thesis were quaterization of inherent amine of the epoxy-based monoliths and grafting tentacle ion groups via glycidyl methacrylate by atom transfer radical polymerization (ATRP) for ion exchange chromatography (IEC).

Place, publisher, year, edition, pages
Umeå: Umeå University, Department of Chemistry, 2009. 53 p.
Keyword
monolith, polycondensation, dissolution-precipitation, epoxy-amine, poly-amide, nylon, emulsion polymerization, characterization, protein separation, liquid chromatography
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:umu:diva-20890 (URN)978-91-7264-772-5 (ISBN)
Distributor:
Kemiska institutionen, 90187, Umeå
Public defence
2009-04-17, KB3A9, Umeå University, Chemistry, Umeå, 13:00 (English)
Opponent
Supervisors
Available from: 2009-03-30 Created: 2009-03-27 Last updated: 2014-03-10Bibliographically approved

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