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Water redispersible cellulose nanofibrils adsorbed with carboxymethyl cellulose
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Biocomposites.ORCID iD: 0000-0002-4100-6076
KTH, School of Biotechnology (BIO), Glycoscience. KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center.ORCID iD: 0000-0001-9832-027X
2014 (English)In: Cellulose (London), ISSN 0969-0239, E-ISSN 1572-882X, Vol. 21, no 6, 4349-4358 p.Article in journal (Refereed) Published
Abstract [en]

Cellulose nanofibrils (CNFs) are difficult to redisperse in water after they have been completely dried due to the irreversible agglomeration of cellulose during drying. Here, we have developed a simple process to prepare water-redispersible dried CNFs by the adsorption of small amounts of carboxymethyl cellulose (CMC) and oven drying. The adsorption of CMC onto CNFs in water suspensions at 22 and 121 °C was studied, and the adsorbed amount of CMC was measured via conductimetric titration. The water-redispersibility of dried CNFs adsorbed with different amounts of CMC was characterized by sedimentation test. Above a critical threshold of CMC adsorption, i.e. 2.3 wt%, the oven dried CNF–CMC sample was fully redispersible in water. The morphology, rheological, and mechanical properties of water-redispersed CNF–CMC samples were investigated by field emission scanning electron microscopy, viscosity measurement, and tensile test, respectively. The water-redispersed CNFs preserved the original properties of never dried CNFs. This new method will facilitate the production, transportation and storage, and large-scale industrial applications of CNFs.

Place, publisher, year, edition, pages
2014. Vol. 21, no 6, 4349-4358 p.
Keyword [en]
Cellulose nanofibrils, Carboxymethyl cellulose, Adsorption, Redispersion
National Category
Organic Chemistry Polymer Chemistry
URN: urn:nbn:se:kth:diva-155178DOI: 10.1007/s10570-014-0452-7ISI: 000344802700041ScopusID: 2-s2.0-84911998076OAI: diva2:760033
Formas, 2009-1687

QC 20141103

Available from: 2014-11-03 Created: 2014-11-03 Last updated: 2015-01-12Bibliographically approved
In thesis
1. Tailoring Cellulose Nanofibrils for Advanced Materials
Open this publication in new window or tab >>Tailoring Cellulose Nanofibrils for Advanced Materials
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Cellulose nanofibrils (CNFs) are nanoscale fibers of high aspect ratio that can be isolated from a wide variety of cellulosic sources, including wood and bacterial cellulose. With high strength despite of their low density, CNFs are a promising renewable building block for the preparation of nanostructured materials and composites. To fabricate CNF-based materials with improved inherent rheological and mechanical properties and additional new functionalities, it is essential to tailor the surface properties of individual CNFs. The surface structures control the interactions between CNFs and ultimately dictate the structure and macroscale properties of the bulk material. In this thesis we have demonstrated different approaches, ranging from non-covalent adsorption and covalent chemical modification to modification of cellulose biosynthesis, to tailor the structure and surface functionalities of CNFs for the fabrication of advanced materials. These materials possess enhanced properties such as water-redispersibility, water absorbency, dye adsorption capacity, antibacterial activity, and mechanical properties.

In Paper I, CNFs were modified via the irreversible adsorption of carboxymethyl cellulose (CMC). The adsorption of small amounts of CMC onto the surface of CNFs prevented agglomeration and co-crystallization of the nanofibrils upon drying, and allowed the recovery of rheological and mechanical properties after redispersion of dried CNF samples.

In Paper II, CNFs bearing permanent cationic charges were prepared through quaternization of wood pulp fibers followed by mechanical disintegration. The activation of the hydroxyl groups on pulp fibers by alkaline treatment was optimized prior to quaternization. This optimization resulted in individual CNFs with uniform width and tunable cationic charge densities. These cationic CNFs demonstrated ultrahigh water absorbency and high adsorption capacity for anionic dyes.

In Paper III, via a similar approach as in Paper II, CNFs bearing polyethylene glycol (PEG) were prepared by covalently grafting PEG to carboxylated pulp fibers prior to mechanical disintegration. CNFs with a high surface chain density of PEG and a uniform width were oriented to produce macroscopic ribbons simply by mechanical stretching of the CNF hydrogel network before drying. The uniform grafted thin monolayer of PEG on the surface of individual CNFs prevented the agglomeration of CNFs and facilitated their alignment upon mechanical stretching, thus resulted in ribbons with ultrahigh tensile strength and modulus. These optically transparent ribbons also demonstrated interesting biaxial light scattering behavior.

In Paper IV, bacterial cellulose (BC) was modified by the addition of chitin nanocrystals (ChNCs) into the growing culture medium of the bacteria Acetobacter aceti which secretes cellulose in the form of entangled nanofibers. This led to the in situ incorporation of ChNCs into the BC nanofibers network and resulted in BC/ChNC nanocomposites exhibiting bactericidal activity. Further, blending of BC nanofibers with ChNCs produced nanocomposite films with relatively lower tensile strength and modulus compared to the in situ cultivated ones. The bactericidal activity increased significantly with increasing amount of ChNCs for nanocomposites prepared by direct mixing of BC nanofibers and ChNCs.

In Paper V, CNFs were isolated from suspension-cultured wild-type (WT) and cellulose-binding module (CBM) transformed tobacco BY-2 (Nicotiana tabacum L. cv bright yellow) cells. Results from strong sulfuric acid hydrolysis indicated that CNFs from transgenic cells overexpressing CBM consisted of longer cellulose nanocrystals compared to CNFs from WT cells. Nanopapers prepared from CNFs of transgenic cells demonstrated significantly enhanced toughness compared to CNFs of WT cells.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2014. 82 p.
TRITA-CHE-Report, ISSN 1654-1081 ; 2014:52
cellulose nanofibrils, bacterial cellulose, surface modification, carboxymethyl cellulose, polyethylene glycol, chitin nanocrystals, bactericidal activity, nanofibrils orientation, water redispersability, mechanical properties, dye removal
National Category
Polymer Technologies
Research subject
Fibre and Polymer Science
urn:nbn:se:kth:diva-155056 (URN)978-91-7595-329-8 (ISBN)
Public defence
2014-11-21, sla F3, Lindstedtsvägen 26, KTH, Stockholm, 13:30 (English)

QC 20141103

Available from: 2014-11-03 Created: 2014-10-29 Last updated: 2014-11-14Bibliographically approved

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