Understanding heat driven gelation of anionic cellulose nanofibrils: Combining Saturation Transfer Difference (STD) NMR, Small Angle X-ray Scattering (SAXS) and rheology

Vincenzo Calabrese, Juan C. Muñoz-García, Julien Schmitt, Marcelo A. Da Silva, Janet L. Scott, Jesús Angulo, Yaroslav Z. Khimyak, Karen J. Edler

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Abstract

A novel mechanism of heat-triggered gelation for oxidised cellulose nanofibrils (OCNF) is reported. We demonstrate that a synergistic approach combining rheology, small-angle X-ray scattering (SAXS) and saturation transfer difference NMR (STD NMR) experiments enables a detailed characterisation of gelation at different length scales. OCNF dispersions experience an increase in solid-like behaviour upon heating as evidenced by rheological studies, associated with enhanced interfibrillar interactions measured using SAXS. Interactions result in an increased fibrillar overlap and increased population of confined water molecules monitored by STD NMR. In comparison, cationic cellulose nanofibrils (produced by reaction of cellulose with trimethylglycidylammonium chloride) were found to be heat-unresponsive.
Original languageEnglish
Pages (from-to)205-213
Number of pages9
JournalJournal of Colloid and Interface Science
Volume535
Early online date25 Sep 2018
DOIs
Publication statusPublished - 1 Feb 2019

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oxidized cellulose
Gelation
X ray scattering
Rheology
Cellulose
Nuclear magnetic resonance
Dispersions
Chlorides
Heating
Molecules
Water
Experiments
Hot Temperature

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title = "Understanding heat driven gelation of anionic cellulose nanofibrils: Combining Saturation Transfer Difference (STD) NMR, Small Angle X-ray Scattering (SAXS) and rheology",
abstract = "A novel mechanism of heat-triggered gelation for oxidised cellulose nanofibrils (OCNF) is reported. We demonstrate that a synergistic approach combining rheology, small-angle X-ray scattering (SAXS) and saturation transfer difference NMR (STD NMR) experiments enables a detailed characterisation of gelation at different length scales. OCNF dispersions experience an increase in solid-like behaviour upon heating as evidenced by rheological studies, associated with enhanced interfibrillar interactions measured using SAXS. Interactions result in an increased fibrillar overlap and increased population of confined water molecules monitored by STD NMR. In comparison, cationic cellulose nanofibrils (produced by reaction of cellulose with trimethylglycidylammonium chloride) were found to be heat-unresponsive.",
author = "Vincenzo Calabrese and Mu{\~n}oz-Garc{\'i}a, {Juan C.} and Julien Schmitt and {Da Silva}, {Marcelo A.} and Scott, {Janet L.} and Jes{\'u}s Angulo and Khimyak, {Yaroslav Z.} and Edler, {Karen J.}",
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TY - JOUR

T1 - Understanding heat driven gelation of anionic cellulose nanofibrils: Combining Saturation Transfer Difference (STD) NMR, Small Angle X-ray Scattering (SAXS) and rheology

AU - Calabrese, Vincenzo

AU - Muñoz-García, Juan C.

AU - Schmitt, Julien

AU - Da Silva, Marcelo A.

AU - Scott, Janet L.

AU - Angulo, Jesús

AU - Khimyak, Yaroslav Z.

AU - Edler, Karen J.

PY - 2019/2/1

Y1 - 2019/2/1

N2 - A novel mechanism of heat-triggered gelation for oxidised cellulose nanofibrils (OCNF) is reported. We demonstrate that a synergistic approach combining rheology, small-angle X-ray scattering (SAXS) and saturation transfer difference NMR (STD NMR) experiments enables a detailed characterisation of gelation at different length scales. OCNF dispersions experience an increase in solid-like behaviour upon heating as evidenced by rheological studies, associated with enhanced interfibrillar interactions measured using SAXS. Interactions result in an increased fibrillar overlap and increased population of confined water molecules monitored by STD NMR. In comparison, cationic cellulose nanofibrils (produced by reaction of cellulose with trimethylglycidylammonium chloride) were found to be heat-unresponsive.

AB - A novel mechanism of heat-triggered gelation for oxidised cellulose nanofibrils (OCNF) is reported. We demonstrate that a synergistic approach combining rheology, small-angle X-ray scattering (SAXS) and saturation transfer difference NMR (STD NMR) experiments enables a detailed characterisation of gelation at different length scales. OCNF dispersions experience an increase in solid-like behaviour upon heating as evidenced by rheological studies, associated with enhanced interfibrillar interactions measured using SAXS. Interactions result in an increased fibrillar overlap and increased population of confined water molecules monitored by STD NMR. In comparison, cationic cellulose nanofibrils (produced by reaction of cellulose with trimethylglycidylammonium chloride) were found to be heat-unresponsive.

U2 - 10.1016/j.jcis.2018.09.085

DO - 10.1016/j.jcis.2018.09.085

M3 - Article

VL - 535

SP - 205

EP - 213

JO - Journal of Colloid and Interface Science

JF - Journal of Colloid and Interface Science

SN - 0021-9797

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