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Surface-initiated ring-opening metathesis polymerisation from cellulose fibres
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.ORCID iD: 0000-0002-8348-2273
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.ORCID iD: 0000-0002-8194-0058
2012 (English)In: POLYM CHEM-UK, ISSN 1759-9954, Vol. 3, no 3, 727-733 p.Article in journal (Refereed) Published
Abstract [en]

In this study, cellulose fibres have been grafted utilizing surface-initiated ring-opening metathesis polymerisation (SI-ROMP). Initially, a Grubbs' type catalyst was immobilized onto filter paper whereafter SI-ROMP of norbornene was performed from the surface of the fibres at three different reaction temperatures, room temperature (RT), 0 degrees C and -18 degrees C, and for different reaction times. The evaluation of the grafted cellulose was performed by contact angle measurements, FT-Raman spectroscopy, FE-SEM and TGA. After the grafting, all samples were clearly hydrophobic with weight increases up to over 100%. The FT-Raman spectroscopy analysis showed significant structural changes after polymerization for cellulose substrates polymerized at 0 degrees C and RT, confirming that a polymer was grafted from the surface. FE-SEM images verified that these samples are covered by polynorbornene and that the fibrillar structure of the native cellulose disappeared. For the samples grafted at -18 degrees C, no significant changes were seen with these analysis methods. However, SI-ROMP appears to be a versatile method to modify cellulose fibres.

Place, publisher, year, edition, pages
Royal Society of Chemistry, 2012. Vol. 3, no 3, 727-733 p.
National Category
Polymer Chemistry
URN: urn:nbn:se:kth:diva-90921DOI: 10.1039/c2py00554aISI: 000300049900023ScopusID: 2-s2.0-84857335793OAI: diva2:507539
QC 20120305Available from: 2012-03-05 Created: 2012-03-05 Last updated: 2014-02-03Bibliographically approved
In thesis
1. Surface Modification of Cellulose by Covalent Grafting and Physical Adsorption
Open this publication in new window or tab >>Surface Modification of Cellulose by Covalent Grafting and Physical Adsorption
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The interest in new environmentally friendly cellulose‐based productshas increased tremendously over the last years. At the same time theSwedish forest industry faces new challenges in its strive to increase the utilization of cellulose fibers in high‐value end‐products. The aim of this study was to expand the toolbox for surface modification of cellulose byemploying covalent surface‐initiated (SI) polymerizations or by physicaladsorption of polymers. SI‐ring‐opening polymerization (ROP) of ε‐caprolactone (ε‐CL) was performed from filter paper (FP) and high surface area nanopaper (NP).Larger amounts of polycaprolactone (PCL) were grafted from NP, compared to FP, owing to the higher amount of available initiating hydroxyl groups. Furthermore, the mechanical properties of PCL were improved by the grafting of FP and NP, as compared to pure PCL.It is challenging to characterize a polymer grafted from a surface. Hence, quartz crystal microbalance with dissipation (QCM‐D) was employed to investigate SI‐ROP in real time from a cellulose model surface. Furthermore, it was shown by colloidal probe AFM that increased lengthof grafted PCL, from cellulose microspheres, improved the interfacialadhesion to a pure PCL surface, suggesting that chain entanglements havea significant impact on the interfacial properties. Increased temperatureand time in contact also improved the adhesion.In order to investigate the degree of substitution (DS) and the degree of polymerization (DP), PCL‐grafted hydrolyzed cellulose cotton linters (HCCL) were studied by solid state NMR. It was found that despite a DS of only a few percent, the surface character changed considerably; furthermore, the DS was virtually independent of the DP. To increase theamount of grafted polymer, ring‐opening metathesis polymerization (ROMP) of norbornene was performed from FP. Short polymerizationtimes and low temperatures resulted in highly grafted surfaces. Alternatively, physical adsorption by electrostatic interactions was employed to modify a cellulose model surface in the QCM‐D. Cationic latex nanoparticles of poly(dimetylaminoethyl methacrylate‐co‐methacrylicacid)‐block‐poly(methyl methacrylate) were produced by reversible addition‐fragmentation chain‐transfer (RAFT)‐mediated surfactant‐freeemulsion polymerization by polymerization‐induced self‐assembly (PISA).This strategy does not require any organic solvents and could potentiallybe introduced in industrial processes.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2014. 77 p.
TRITA-CHE-Report, ISSN 1654-1081 ; 2014-2
Surface modification, cellulose, covalent modification, physical adsorption, polymer synthesis
National Category
Polymer Technologies
urn:nbn:se:kth:diva-140859 (URN)978-91-7501-987-1 (ISBN)
Public defence
2014-02-21, Kollegiesalen, Brinellvägen 8, KTH, Stockholm, 10:00 (English)
Knut and Alice Wallenberg Foundation, KFCE 8508Formas

QC 20140203

Available from: 2014-02-03 Created: 2014-02-03 Last updated: 2014-02-03Bibliographically approved

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