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Monolithic space-filling porous materials from engineering plastics by thermally induced phase separation
Umeå University, Faculty of Science and Technology, Department of Chemistry. (Research Group for Reactive Polymers in Analytical Chemistry (RPAC))
Umeå University, Faculty of Science and Technology, Department of Chemistry. (Research Group for Reactive Polymers in Analytical Chemistry (RPAC))
2014 (English)In: ACS Applied Materials and Interfaces, ISSN 1944-8244, E-ISSN 1944-8252, Vol. 6, no 18, 15653-15666 p.Article in journal (Refereed) Published
Abstract [en]

Six different uncompounded engineering and commodity polymers were evaluated for their ability to produce space-filling monolithic entities by thermally induced phase separation (TIPS) from 22 different solvents. Attempts were first made to dissolve the polymers at elevated temperatures, selected below the boiling point of each solvent. Then the solutions of polymers that were homogeneous dissolved underwent a controlled temperature decrease to induce a phase separation as the upper critical solution temperature was passed. Twelve of the solvents gave monolithic entities by this procedure, materials that were characterized with regard to their specific surface area and pore size distribution. These measured parameters were then correlated with their macroporous morphology, assessed by scanning electron microscopy. Monolithic materials with widely different mesoporous properties were obtained with specific surface areas ranging from 169 m(2)/g to structures with essentially nonporous skeletons and distinct mesopore size distribution modes from 6 to 15 nm. The materials furthermore had a wide variation in their macroporous morphologies-among the same polymer processed in different solvents and between different polymers dissolved in the same solvent. TIPS processing therefore appears to be a viable route to prepare space-filling meso- and macroporous support materials for a wide variety of purposes in separation science and heterogeneous chemistry.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2014. Vol. 6, no 18, 15653-15666 p.
Keyword [en]
monolithic supports, polymeric scaffolds, heterogeneous chemistry, separation science, thermally induced phase separation
National Category
Chemical Sciences Nano Technology
Research subject
Analytical Chemistry
URN: urn:nbn:se:umu:diva-89306DOI: 10.1021/am502977zISI: 000342328300006OAI: diva2:719773
Swedish Research Council, 2012-4000

Included in thesis in manuscript form.

Available from: 2014-05-27 Created: 2014-05-27 Last updated: 2014-10-31Bibliographically approved
In thesis
1. Porous Polymeric Monoliths by Less Common Pathways: Preparation and Characterization
Open this publication in new window or tab >>Porous Polymeric Monoliths by Less Common Pathways: Preparation and Characterization
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis focuses on my endeavors to prepare new porous polymeric monoliths that are viable to use as supports in flow-through processes. Polymer monoliths of various porous properties and different chemical properties have been prepared utilizing the thermally induced phase separation (TIPS) phenomenon and step-growth polymerization reactions. The aim has been to find appropriate synthesis routes to produce separation supports with fully controlled chemical, physical and surface properties. This thesis includes preparation of porous monolithic materials from several non-cross-linked commodity polymers and engineering plastics by dissolution/precipitation process (i.e. TIPS). Elevated temperatures, above the upper critical solution temperature (UCST), were used to dissolve the polymers in appropriate solvents that only dissolve the polymers above this critical temperature. After dissolution, the homogeneous and clear polymer-solvent solution is thermally quenched by cooling. A porous material, of three dimensional structure, is then obtained as the temperature crosses the UCST. More than 20 organic solvents were tested to find the most compatible one that can dissolve the polymer above the UCST and precipitate it back when the temperature is lowered. The effect of using a mixture of two solvents or additives (co-porogenic polymer or surfactant) in the polymer dissolution/precipitation process have been studied more in depth for poly(vinylidine difluoride) (PVDF) polymers of two different molecular weight grades. Monolithic materials showing different pore characteristics could be obtained by varying the composition of the PVDF-solvent mixture during the dissolute­ion/precipitation process. Step-growth polymerization (often called polycondensat­ion reaction) combined with sol-gel process with the aid of porogenic polymer and block copolymer surfactant have also been used as a new route of synthesis for production of porous melamine-formaldehyde (MF) monoliths. In general, the meso- and macro-porous support materials, for which the synthesis/preparation is discussed in this thesis, are useful to a wide variety of applications in separation science and heterogeneous reactions (catalysis).

Place, publisher, year, edition, pages
Umeå: Umeå university, 2014. 63 p.
Monolith, commodity polymer, thermally induced phase separation, dissolution-precipitation, polymer solvents, porogenic polymer, step-growth polymerization, separation science, melamine-formaldehyde
National Category
Analytical Chemistry Polymer Chemistry Materials Chemistry
urn:nbn:se:umu:diva-89322 (URN)978-91-7601-088-4 (ISBN)
Public defence
2014-06-13, KB3B1, KBC-huset, Umeå universitet, Umeå, 13:00 (English)
Available from: 2014-05-28 Created: 2014-05-27 Last updated: 2014-05-28Bibliographically approved

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