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Preparation of Porous Cellulose Beads via Introduction of Diamine Spacers
Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Engineering Sciences, Nanotechnology and Functional Materials.
Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Engineering Sciences, Nanotechnology and Functional Materials.
Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Engineering Sciences, Nanotechnology and Functional Materials.
Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Engineering Sciences, Nanotechnology and Functional Materials.
2016 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 32, no 22, 5600-5607 p.Article in journal (Refereed) Published
Resource type
Text
Abstract [en]

The current work presents a synthesis route based on the reductive amination of 2,3-dialdehyde cellulose beads with diamines to render micrometer-sized beads with increased specific surface area (SSA) and porosity in the mesoporous range. Specifically, the influence of the reductive amination of 2,3-dialdehyde cellulose (DAC) using aliphatic and aromatic tethered mono- and diamines on bead microstructure was investigated. Aliphatic and aromatic tethered monoamines were found to have limited utility for producing porous beads whereas the introduction of diamines provided beads with a porous texture and an SSA increasing from <1 to >30 m(2)/g. Both aliphatic and aromatic diamines were found to be useful in producing porous beads having a pore size distribution range of 10 to 100 nm, as verified by N-2 gas adsorption and mercury intrusion porosimetry analyses. The true density of the functionalized DAC beads decreased to an average of about 1.36 g/cm(3) as compared to 1.48 g/cm(3) for the unfunctionalized, fully oxidized DAC beads. The total porosity of the beads was, according to mercury porosimetry, in the range of 54-64%. Reductive amination with 1,7-diaminoheptane provided beads that were stable under alkaline conditions (I M NaOH). It was concluded that the introduction of tethered diamines into DAC beads is a facile method for producing mesoporous beads.

Place, publisher, year, edition, pages
2016. Vol. 32, no 22, 5600-5607 p.
National Category
Nano Technology Materials Engineering
Identifiers
URN: urn:nbn:se:uu:diva-299045DOI: 10.1021/acs.langmuir.6b01288ISI: 000377631300017PubMedID: 27181427OAI: oai:DiVA.org:uu-299045DiVA: diva2:948803
Funder
Knut and Alice Wallenberg FoundationGöran Gustafsson Foundation for promotion of scientific research at Uppala University and Royal Institute of Technology
Available from: 2016-07-13 Created: 2016-07-13 Last updated: 2017-08-23Bibliographically approved
In thesis
1. Functionalization, Characterization and Applications of Oxidized Nanocellulose Derivatives
Open this publication in new window or tab >>Functionalization, Characterization and Applications of Oxidized Nanocellulose Derivatives
2017 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Cellulose, a sustainable raw material derived from nature, can be used for various applications following its functionalization and oxidation. Nanocellulose, inheriting the properties of cellulose, can offer new properties due to nanoscale effects, in terms of high specific surface area and porosity. The oxidation of cellulose can provide more active sites on the cellulose chains, improving its functionalization and broadening applications. Two kinds of oxidation and their corresponding applications are described in this thesis: periodate oxidation and Oxone® oxidation.

2,3-dialdehyde cellulose (DAC) beads were prepared from Cladophora nanocellulose via periodate oxidation, and were further modified with amines via reductive amination. Several diamines were selected as possible crosslinkers to produce porous DAC beads, which showed higher porosity, stability in alkaline solution and enhanced thermal stability.

After functionalization of DAC beads with L-cysteine (DAC-LC), thiol, amine and carboxyl groups were introduced into the DAC beads, endowing the DAC-LC beads with high adsorption capacity for palladium. The synthesized DAC-LC beads were character­ized with SEM, FTIR, XPS, TGA, BET and XRD and the palladium adsorption process was investigated.

Chitosan was employed as a crosslinker in functionalization of DAC beads (DAC-CS). The conditions for the synthesis of DAC-CS beads were screened and verifying the stability of the beads in alkaline solution. The DAC-CS beads produced were investigated using SEM, FTIR, XPS, TGA and BET, and the adsorption and desorption capacity of Congo red was studied, indicating DAC-CS beads have potential as sorbent.

Oxone oxidation of cellulose is a novel one-pot oxidation method in which mainly the hydroxyl groups on C6 are oxidized to produce carboxylic acid groups on the cellulose chains. To increase the efficiency of Oxone oxidation, several reaction parameters were studied. Cellulose pulp and Cladophora nanocellulose were chosen as prototypes to investigate the effects of oxidation, and the physico­chemical properties of the oxidized products were characterized. Cellulose pulp, pretreated with Oxone oxidation, was disintegrated by homogenization to prepare cellulose nanofibers (CNF). The effect of pre­treat­ment on the preparation of CNF was studied, and the results indicated that Oxone oxidation was efficient in the production of CNF.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2017. 68 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1548
Keyword
Nanocellulose, Periodate oxidation, Oxone oxidation, Adsorption, Palladium, Congo red dye, Cellulose nanofibers
National Category
Nano Technology
Research subject
Engineering Science with specialization in Nanotechnology and Functional Materials
Identifiers
urn:nbn:se:uu:diva-328388 (URN)978-91-513-0048-1 (ISBN)
Public defence
2017-10-13, Polhemsalen, Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, 09:30 (English)
Opponent
Supervisors
Available from: 2017-09-21 Created: 2017-08-23 Last updated: 2017-10-17

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