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Microfibrillated cellulose: Energy-efficient preparation techniques and applications in paper
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Fibre Technology.
2015 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This work describes three alternative processes for producing microfibrillated cellulose (MFC; also referred to as cellulose nanofibrils, CNF) in which bleached pulp fibres are first pretreated and then homogenized using a high-pressure homogenizer. In one process, fibre cell wall delamination was facilitated by a combined enzymatic and mechanical pretreatment. In the two other processes, cell wall delamination was facilitated by pretreatments that introduced anionically charged groups into the fibre wall, by means of either a carboxymethylation reaction or irreversibly attaching carboxymethylcellulose (CMC) to the fibres. All three processes are industrially feasible and enable energy-efficient production of MFC. Using these processes, MFC can be produced with an energy consumption of 500–2300 kWh/tonne. These materials have been characterized in various ways and it has been demonstrated that the produced MFCs are approximately 5–30 nm wide and up to several microns long.

The MFCs were also evaluated in a number of applications in paper. The carboxymethylated MFC was used to prepare strong free-standing barrier films and to coat wood-containing papers to improve the surface strength and reduce the linting propensity of the papers. MFC, produced with an enzymatic pretreatment, was also produced at pilot scale and was studied in a pilot-scale paper making trial as a strength agent added at the wet-end for highly filled papers.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2015. , 63 p.
Series
TRITA-CHE-Report, ISSN 1654-1081 ; 2015:5
Keyword [en]
Microfibrillated cellulose, microfibrillar cellulose, nanofibrillated cellulose, nanofibrillar cellulose, cellulose nanofibrils, nanocellulose, MFC, NFC, CNF, production techniques, energy efficient, gel properties, films, enzymes, carboxymethylation, carboxymethyl cellulose, CMC, mechanical properties, oxygen barrier, homogenization, linting, papermaking
National Category
Paper, Pulp and Fiber Technology
Research subject
Fibre and Polymer Science
Identifiers
URN: urn:nbn:se:kth:diva-159222ISBN: 978-91-7595-426-4 (print)OAI: oai:DiVA.org:kth-159222DiVA: diva2:783431
Public defence
2015-02-27, F3, Lindstedtsvägen 26, KTH, Stockholm, 10:00 (English)
Opponent
Supervisors
Note

QC 20150126

Available from: 2015-01-26 Created: 2015-01-26 Last updated: 2015-01-28Bibliographically approved
List of papers
1. Enzymatic hydrolysis combined with mechanical shearing and high-pressure homogenization for nanoscale cellulose fibrils and strong gels
Open this publication in new window or tab >>Enzymatic hydrolysis combined with mechanical shearing and high-pressure homogenization for nanoscale cellulose fibrils and strong gels
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2007 (English)In: Biomacromolecules, ISSN 1525-7797, E-ISSN 1526-4602, Vol. 8, no 6, 1934-1941 p.Article in journal (Refereed) Published
Abstract [en]

Toward exploiting the attractive mechanical properties of cellulose I nanoelements, a novel route is demonstrated, which combines enzymatic hydrolysis and mechanical shearing. Previously, an aggressive acid hydrolysis and sonication of cellulose I containing fibers was shown to lead to a network of weakly hydrogen-bonded rodlike cellulose elements typically with a low aspect ratio. On the other hand, high mechanical shearing resulted in longer and entangled nanoscale cellulose elements leading to stronger networks and gels. Nevertheless, a widespread use of the latter concept has been hindered because of lack of feasible methods of preparation, suggesting a combination of mild hydrolysis and shearing to disintegrate cellulose I containing fibers into high aspect ratio cellulose I nanoscale elements. In this work, mild enzymatic hydrolysis has been introduced and combined with mechanical shearing and a high-pressure homogenization, leading to a controlled fibrillation down to nanoscale and a network of long and highly entangled cellulose I elements. The resulting strong aqueous gels exhibit more than 5 orders of magnitude tunable storage modulus G' upon changing the concentration. Cryotransmission electron microscopy, atomic force microscopy, and cross-polarization/magic-angle spinning (CP/MAS) C-13 NMR suggest that the cellulose I structural elements obtained are dominated by two fractions, one with lateral dimension of 5-6 nm and one with lateral dimensions of about 10-20 nm. The thicker diameter regions may act as the junction zones for the networks. The resulting material will herein be referred to as MFC (microfibrillated cellulose). Dynamical rheology showed that the aqueous suspensions behaved as gels in the whole investigated concentration range 0.125-5.9% w/w, G' ranging from 1.5 Pa to 10(5) Pa. The maximum G' was high, about 2 orders of magnitude larger than typically observed for the corresponding nonentangled low aspect ratio cellulose I gels, and G' scales with concentration with the power of approximately three. The described preparation method of MFC allows control over the final properties that opens novel applications in materials science, for example, as reinforcement in composites and as templates for surface modification.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2007
National Category
Chemical Engineering
Identifiers
urn:nbn:se:kth:diva-37114 (URN)10.1021/bm061215p (DOI)000247107900023 ()17474776 (PubMedID)
Note

QC 20110801

Available from: 2011-08-01 Created: 2011-08-01 Last updated: 2017-12-08Bibliographically approved
2. The build-up of polyelectrolyte multilayers of microfibrillated cellulose and cationic polyelectrolytes
Open this publication in new window or tab >>The build-up of polyelectrolyte multilayers of microfibrillated cellulose and cationic polyelectrolytes
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2008 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 24, no 3, 784-795 p.Article in journal (Refereed) Published
Abstract [en]

A new type of nanocellulosic material has been prepared by high-pressure homogenization of carboxymethylated cellulose fibers followed by ultrasonication and centrifugation. This material had a cylindrical cross-section as shown by transmission electron microscopy with a diameter of 5-15 nm and a length of up to 1 mu m. Calculations, using the Poisson-Boltzmann equation, showed that the surface potential was between 200 and 250 mV, depending on the pH, the salt concentration, and the size of the fibrils. They also showed that the carboxyl groups on the surface of the nanofibrils are not fully dissociated until the pH has reached pH = similar to 10 in deionized water. Calculations of the interaction between the fibrils using the Derjaguin-Landau-Verwey-Overbeek theory and assuming a cylindrical geometry indicated that there is a large electrostatic repulsion between these fibrils, provided the carboxyl groups are dissociated. If the pH is too low and/or the salt concentration is too high, there will be a large attraction between the fibrils, leading to a rapid aggregation of the fibrils. It is also possible to form polyelectrolyte multilayers (PEMs) by combining different types of polyelectrolytes and microfibrillated cellulose (MFC). In this study, silicon oxide surfaces were first treated with cationic polyelectrolytes before the surfaces were exposed to MFC. The build-up of the layers was monitored with ellipsometry, and they show that it is possible to form very well-defined layers by combinations of MFC and different types of polyelectrolytes and different ionic strengths of the solutions during the adsorption of the polyelectrolyte. A polyelectrolyte with a three-dimensional structure leads to the build-up of thick layers of MFC, whereas the use of a highly charged linear polyelectrolyte leads to the formation of thinner layers of MFC. An increase in the salt concentration during the adsorption of the polyelectrolyte results in the formation of thicker layers of MFC, indicating that the structure of the adsorbed polyelectrolyte has a large influence on the formation of the MFC layer. The films of polyelectrolytes and MFC were so smooth and well-defined that they showed clearly different interference colors, depending on the film thickness. A comparison between the thickness of the films, as measured with ellipsometry, and the thickness estimated from their colors showed good agreement, assuming that the films consisted mainly of solid cellulose with a refractive index of 1.53. Carboxymethylated MFC is thus a new type of nanomaterial that can be combined with oppositely charged polyelectrolytes to form well-defined layers that may be used to form, for example, new types of sensor materials.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2008
Keyword
molecular-dynamics simulations, aqueous environment, charged surfaces, ionic-strength, layer, films, adsorption, deposition, poly(ethylenimine), nanoscale
National Category
Paper, Pulp and Fiber Technology
Identifiers
urn:nbn:se:kth:diva-17283 (URN)10.1021/la702481v (DOI)000252777700033 ()2-s2.0-39449090645 (Scopus ID)
Note

QC 20100525

Available from: 2010-08-05 Created: 2010-08-05 Last updated: 2015-01-26Bibliographically approved
3. Highly Transparent Films from Carboxymethylated Microfibrillated Cellulose: The Effect of Multiple Homogenization Steps on Key Properties
Open this publication in new window or tab >>Highly Transparent Films from Carboxymethylated Microfibrillated Cellulose: The Effect of Multiple Homogenization Steps on Key Properties
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2011 (English)In: Journal of Applied Polymer Science, ISSN 0021-8995, E-ISSN 1097-4628, Vol. 119, no 5, 2652-2660 p.Article in journal (Refereed) Published
Abstract [en]

We produced microfibrillated cellulose by passing carboxymethylated sulfite-softwood-dissolving pulp with a relatively low hemicellulose content (4.5%) through a high-shear homogenizer. The resulting gel was subjected to as many as three additional homogenization steps and then used to prepare solvent-cast films. The optical, mechanical, and oxygen-barrier properties of these films were determined. A reduction in the quantity and appearance of large fiber fragments and fiber aggregates in the films as a function of increasing homogenization was illustrated with optical microscopy, atomic force microscopy, and scanning electron microscopy. Film opacity decreased with increasing homogenization, and the use of three additional homogenization steps after initial gel production resulted in highly transparent films. The oxygen permeability of the films was not significantly influenced by the degree of homogenization, whereas the mean tensile strength, modulus of elasticity, and strain at break were increased by two or three extra homogenization steps.

Place, publisher, year, edition, pages
Wiley-Blackwell, 2011
Keyword
barrier, biopolymers, fibers, gas permeation, mechanical properties
National Category
Polymer Chemistry
Identifiers
urn:nbn:se:kth:diva-28589 (URN)10.1002/app.32831 (DOI)000285310400021 ()2-s2.0-78649949931 (Scopus ID)
Note

QC 20110117

Available from: 2011-01-17 Created: 2011-01-17 Last updated: 2017-12-11Bibliographically approved
4. Method for providing a nanocellulose involving modifying cellulose fibers
Open this publication in new window or tab >>Method for providing a nanocellulose involving modifying cellulose fibers
2009 (English)Patent (Other (popular science, discussion, etc.))
Abstract [en]

The present invention provides a method for the manufacturing of nanocellulose. The method includes a first modification of the cellulose material, where the cellulose fibres are treated with an aqueous electrolyte-containing solution of an amphoteric cellulose derivative. The modification is followed by a mechanical treatment. By using this method for manufacturing nanocellulose, clogging of the mechanical apparatus is avoided. Also disclosed is nanocellulose manufactured in accordance with said method and uses of said cellulose.

National Category
Paper, Pulp and Fiber Technology
Identifiers
urn:nbn:se:kth:diva-102939 (URN)
Patent
AU 2009234498B2 (2014-01-09)
Note

RU 2519257 C2 (2014-06-10);  US 8911591 B2 (2014-12-16)

Available from: 2012-09-28 Created: 2012-09-28 Last updated: 2015-01-27Bibliographically approved
5. Nanocelluloses: A New Family of Nature-Based Materials
Open this publication in new window or tab >>Nanocelluloses: A New Family of Nature-Based Materials
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2011 (English)In: Angewandte Chemie International Edition, ISSN 1433-7851, E-ISSN 1521-3773, Vol. 50, no 24, 5438-5466 p.Article, review/survey (Refereed) Published
Abstract [en]

Cellulose fibrils with widths in the nanometer range are nature-based materials with unique and potentially useful features. Most importantly, these novel nanocelluloses open up the strongly expanding fields of sustainable materials and nanocomposites, as well as medical and life-science devices, to the natural polymer cellulose. The nanodimensions of the structural elements result in a high surface area and hence the powerful interaction of these celluloses with surrounding species, such as water, organic and polymeric compounds, nanoparticles, and living cells. This Review assembles the current knowledge on the isolation of microfibrillated cellulose from wood and its application in nanocomposites; the preparation of nanocrystalline cellulose and its use as a reinforcing agent; and the biofabrication of bacterial nanocellulose, as well as its evaluation as a biomaterial for medical implants.

Keyword
cellulose, nanocellulose, nanomaterials, nature-based materials, polymers
National Category
Nano Technology
Identifiers
urn:nbn:se:kth:diva-159215 (URN)10.1002/anie.201001273 (DOI)000291997000004 ()2-s2.0-79958021496 (Scopus ID)
Note

QC 20150126

Available from: 2015-01-26 Created: 2015-01-26 Last updated: 2017-12-05Bibliographically approved
6. Reduction of the linting and dusting propensity of newspaper using starch and microfibrillated cellulose
Open this publication in new window or tab >>Reduction of the linting and dusting propensity of newspaper using starch and microfibrillated cellulose
2010 (English)In: Nordic Pulp & Paper Research Journal, ISSN 0283-2631, E-ISSN 2000-0669, Vol. 25, no 4, 495-504 p.Article in journal (Refereed) Published
Abstract [en]

It is well known that a high linting and dusting tendency of newsprint will almost certainly cause a higher frequency of production stops in offset printing. Such stops are connected with production losses, health hazards and high costs for blanket cleaning. This report deals with the area of surface and internal treatments of thermomechanical pulp (TMP) containing paper grades such as newsprint. The objective of such treatments was to reinforce the surface strength of the paper in order to decrease the linting and dusting of the paper during printing. Surface treatments are usually employed in commercial practice by applying modified starches to the paper surface using film-press technology. Internal treatments of modified starches may also reduce the delamination resistance. In this investigation, laboratory TMP-sheets and commercial newsprint sheets were coated with microfibrillated cellulose (MFC) and anionic starch (A-starch). The surface treatments were also compared with internally treated TMP-sheets using cationic starch. The linting propensity of the sheets was evaluated using the Innventia linting propensity tester (Innventia-LPT). Both MFC and A-starch treatments greatly improved the linting propensity of the coated sheets. It was also found that there is a strong synergistic effect of using a mixture of microfibrillated cellulose and anionic starch. A mixture of these two additives gave a lower linting propensity than if either additive was used alone. When using MFC alone, sheet delamination may occur, due to the strong water retention and hold-out properties of MFC, but if anionic starch was used together with MFC a film anchoring of the coating to the base sheet was achieved, improving the linting propensity without risk for delamination.

Keyword
Anionic starch, Cationic starch, Dry strength, Dusting, Innventia linting propensity tester, Linting, Microfibrillated cellulose, Nanocellulose, Newsprint, Offset printing, Surface sizing, Surface treatment
National Category
Paper, Pulp and Fiber Technology
Identifiers
urn:nbn:se:kth:diva-159216 (URN)10.3183/NPPRJ-2010-25-04-p495-504 (DOI)
Note

QC 20150126

Available from: 2015-01-26 Created: 2015-01-26 Last updated: 2017-12-05Bibliographically approved
7. The use of microfibrillated cellulose in fine paper manufacturing: Results from a pilot scale papermaking trial
Open this publication in new window or tab >>The use of microfibrillated cellulose in fine paper manufacturing: Results from a pilot scale papermaking trial
2014 (English)In: Nordic Pulp & Paper Research Journal, ISSN 0283-2631, E-ISSN 2000-0669, Vol. 29, no 3, 476-483 p.Article in journal (Refereed) Published
Abstract [en]

In this work the strength enhancing capabilities of microfibrillated cellulose (MFC) in highly filled papers was studied. Both the MFC production and the paper making were done in pilot scale under realistic industrial conditions. The results clearly show that MFC (2.5 - 5.0wt-%) could improve the mechanical properties of highly filled papers (20 - 35 wt-% filler contents). All studied dry mechanical properties were improved and the improvements were most pronounced for Z-strength and fracture toughness. By combining the MFC with a C-starch dosage further improvements in mechanical properties could be achieved. The improvements in mechanical properties enabled increased filler content with retained properties. The filler increase could be achieved at the same time as the sheet formation and the dry content after pressing were improved.

Keyword
Mechanical properties, Microfibrillated cellulose, Nanocellulose, Papermaking
National Category
Paper, Pulp and Fiber Technology
Identifiers
urn:nbn:se:kth:diva-159218 (URN)10.3183/NPPRJ-2014-29-03-p476-483 (DOI)2-s2.0-84907664893 (Scopus ID)
Note

QC 20150126

Available from: 2015-01-26 Created: 2015-01-26 Last updated: 2017-12-05Bibliographically approved
8. On the manufacture of carboxymethylated microfibrillated cellulose from different pulp types
Open this publication in new window or tab >>On the manufacture of carboxymethylated microfibrillated cellulose from different pulp types
(English)Manuscript (preprint) (Other academic)
National Category
Paper, Pulp and Fiber Technology
Identifiers
urn:nbn:se:kth:diva-159220 (URN)
Note

QS 2015

Available from: 2015-01-26 Created: 2015-01-26 Last updated: 2015-01-26Bibliographically approved

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