Small-angle neutron scattering from cellulose solutions in phosphoric acid at different water content

Cellulose from biomass is an abundant and renewable alternative source for chemicals and fuels, yet its utilization by chemical or biological process requires pre-treatment in order to release the macromolecules from their tightly packed crystal structure. Phosphoric acid (PA) has been known for man...

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Main Authors: Gilad Alfassi, Aurel Radulescu, Sapir Lifshiz-Simon, Sapir Rappoport, Yachin Cohen
Format: Article
Language:English
Published: Elsevier 2024-03-01
Series:Giant
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S2666542524000110
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author Gilad Alfassi
Aurel Radulescu
Sapir Lifshiz-Simon
Sapir Rappoport
Yachin Cohen
author_facet Gilad Alfassi
Aurel Radulescu
Sapir Lifshiz-Simon
Sapir Rappoport
Yachin Cohen
author_sort Gilad Alfassi
collection DOAJ
description Cellulose from biomass is an abundant and renewable alternative source for chemicals and fuels, yet its utilization by chemical or biological process requires pre-treatment in order to release the macromolecules from their tightly packed crystal structure. Phosphoric acid (PA) has been known for many years to be an efficient solvent for crystalline cellulose. It is also established that a certain quantity of water content in PA is required for efficient pretreatment. This study uses small-angle neutron scattering (SANS) measurements to evaluate cellulose dissolution in deuterated phosphoric acid (dPA), at different wt% dPA between 78 and 97 % (different D2O content). The SANS method is useful for this purpose due to the availability of deuterated dPA, its contrast in scattering length density towards cellulose, and its low incoherent scattering cross-section. The results indicate that most of the cellulose in 2 wt% solution is dissolved in PA as individual chains, at acid content of 81–94 wt% PA. Structural differences of the dissolved cellulose in PA of the various water compositions in this range are insignificant. At 78 % dPA the cellulose crystal still seem to be disrupted, yet the structure can be modeled as mass-surface fractals of small fibrils with irregular surface, possibly due to dissolved chain segments, which are aggregated as mass fractals of rods. At 97 % dPA evidence for a small content of undissolved fibrils is noted.
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spelling doaj.art-c7273b593df0478baf27a3fd3b30436e2024-03-23T06:26:13ZengElsevierGiant2666-54252024-03-0117100246Small-angle neutron scattering from cellulose solutions in phosphoric acid at different water contentGilad Alfassi0Aurel Radulescu1Sapir Lifshiz-Simon2Sapir Rappoport3Yachin Cohen4Department of Biotechnology Engineering, Braude College of Engineering, Karmiel 2161002, IsraelForschungszentrum Jülich GmbH, Jülich Centre for Neutron Science (JCNS-4) at Heinz Maier-Leibnitz Zentrum (MLZ), Garching D-85747, GermanyDepartment of Chemical Engineering, Technion - Israel Institute of Technology, Haifa 3200003, IsraelDepartment of Chemical Engineering, Technion - Israel Institute of Technology, Haifa 3200003, IsraelDepartment of Chemical Engineering, Technion - Israel Institute of Technology, Haifa 3200003, Israel; Corresponding author.Cellulose from biomass is an abundant and renewable alternative source for chemicals and fuels, yet its utilization by chemical or biological process requires pre-treatment in order to release the macromolecules from their tightly packed crystal structure. Phosphoric acid (PA) has been known for many years to be an efficient solvent for crystalline cellulose. It is also established that a certain quantity of water content in PA is required for efficient pretreatment. This study uses small-angle neutron scattering (SANS) measurements to evaluate cellulose dissolution in deuterated phosphoric acid (dPA), at different wt% dPA between 78 and 97 % (different D2O content). The SANS method is useful for this purpose due to the availability of deuterated dPA, its contrast in scattering length density towards cellulose, and its low incoherent scattering cross-section. The results indicate that most of the cellulose in 2 wt% solution is dissolved in PA as individual chains, at acid content of 81–94 wt% PA. Structural differences of the dissolved cellulose in PA of the various water compositions in this range are insignificant. At 78 % dPA the cellulose crystal still seem to be disrupted, yet the structure can be modeled as mass-surface fractals of small fibrils with irregular surface, possibly due to dissolved chain segments, which are aggregated as mass fractals of rods. At 97 % dPA evidence for a small content of undissolved fibrils is noted.http://www.sciencedirect.com/science/article/pii/S2666542524000110Cellulose dissolutionPhosphoric acidWater contentNeutron scattering
spellingShingle Gilad Alfassi
Aurel Radulescu
Sapir Lifshiz-Simon
Sapir Rappoport
Yachin Cohen
Small-angle neutron scattering from cellulose solutions in phosphoric acid at different water content
Giant
Cellulose dissolution
Phosphoric acid
Water content
Neutron scattering
title Small-angle neutron scattering from cellulose solutions in phosphoric acid at different water content
title_full Small-angle neutron scattering from cellulose solutions in phosphoric acid at different water content
title_fullStr Small-angle neutron scattering from cellulose solutions in phosphoric acid at different water content
title_full_unstemmed Small-angle neutron scattering from cellulose solutions in phosphoric acid at different water content
title_short Small-angle neutron scattering from cellulose solutions in phosphoric acid at different water content
title_sort small angle neutron scattering from cellulose solutions in phosphoric acid at different water content
topic Cellulose dissolution
Phosphoric acid
Water content
Neutron scattering
url http://www.sciencedirect.com/science/article/pii/S2666542524000110
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AT sapirlifshizsimon smallangleneutronscatteringfromcellulosesolutionsinphosphoricacidatdifferentwatercontent
AT sapirrappoport smallangleneutronscatteringfromcellulosesolutionsinphosphoricacidatdifferentwatercontent
AT yachincohen smallangleneutronscatteringfromcellulosesolutionsinphosphoricacidatdifferentwatercontent