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Revisiting the dissolution of cellulose in H3PO4(aq) through cryo-TEM PTssNMR and DWS

2021-01Journal article Restricted access
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dc.contributor.authorAlves, Luis
dc.contributor.authorMedronho, Bruno
dc.contributor.authorFilipe, Alexandra
dc.contributor.authorRomano, Anabela
dc.contributor.authorRasteiro, Maria G.
dc.contributor.authorLindman, Bjorn
dc.contributor.authorTopgaard, Daniel
dc.contributor.authorDavidovich, Irina
dc.contributor.authorTalmon, Yeshayahu
dc.date.accessioned2021-09-08T10:58:11Z
dc.date.available2021-09-08T10:58:11Z
dc.date.issued2021-01
dc.description.abstractCellulose can be dissolved in concentrated acidic aqueous solvents forming extremely viscous solutions, and, in some cases, liquid crystalline phases. In this work, the concentrated phosphoric acid aqueous solvent is revisited implementing a set of advanced techniques, such as cryo-transmission electronic microscopy (cryo-TEM), polarization transfer solid-state nuclear magnetic resonance (PTssNMR), and diffusing wave spectroscopy (DWS). Cryo-TEM images confirm that this solvent system is capable to efficiently dissolve cellulose. No cellulose particles, fibrils, or aggregates are visible. Conversely, PTssNMR revealed a dominant CP signal at 25 degrees C, characteristic of C-H bond reorientation with correlation time longer than 100 ns and/or order parameter above 0.5, which was ascribed to a transient gel-like network or an anisotropic liquid crystalline phase. Increasing the temperature leads to a gradual transition from CP to INEPT-dominant signal and a loss of birefringence in optical microscopy, suggesting an anisotropic-to-isotropic phase transition. Finally, an excellent agreement between optical microrheology and conventional mechanical rheometry was also obtained.
dc.description.sponsorshipPortuguese Foundation for Science and Technology, FCTPortuguese Foundation for Science and Technology [PTDC/AGR-TEC/4814/2014, PTDC/ASP-SIL/30619/2017, UIDB/05183/2020, IF/01005/2014, CEECIND/01014/2018]; ESMI (European Soft Matter Infrastructure) [E160700746]; FCTPortuguese Foundation for Science and TechnologyEuropean Commission [UIDB00102/2020]; Technion Russell Berrie Nanotechnology Institute (RBNI)
dc.description.sponsorshipE160700746
dc.description.versioninfo:eu-repo/semantics/publishedVersion
dc.identifier.doi10.1016/j.carbpol.2020.117122
dc.identifier.issn0144-8617
dc.identifier.urihttp://hdl.handle.net/10400.1/17054
dc.language.isoeng
dc.peerreviewedyes
dc.publisherElsevier
dc.relationMediterranean Institute for Agriculture, Environment and Development
dc.relationFrom Forest to Textiles: Development of Sustainable Processes for the Production of Ecological Man-made Cellulose Fibres
dc.relationNot Available
dc.relationChemical Process Engineering and Forest Products Research Centre
dc.subjectPhosphoric acid
dc.subjectCellulose dissolution
dc.subjectAnisotropy
dc.subjectLiquid crystalline phase
dc.subjectPTssNMR
dc.subjectDWS
dc.subjectcryo-TEM
dc.subject.otherChemistry; Polymer Science
dc.titleRevisiting the dissolution of cellulose in H3PO4(aq) through cryo-TEM PTssNMR and DWS
dc.typejournal article
dspace.entity.typePublication
oaire.awardTitleMediterranean Institute for Agriculture, Environment and Development
oaire.awardTitleFrom Forest to Textiles: Development of Sustainable Processes for the Production of Ecological Man-made Cellulose Fibres
oaire.awardTitleNot Available
oaire.awardTitleChemical Process Engineering and Forest Products Research Centre
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/3599-PPCDT/PTDC%2FAGR-TEC%2F4814%2F2014/PT
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/9471 - RIDTI/PTDC%2FASP-SIL%2F30619%2F2017/PT
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/6817 - DCRRNI ID/UIDB%2F05183%2F2020/PT
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/Investigador FCT/IF%2F01005%2F2014%2FCP1234%2FCT0004/PT
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/CEEC IND 2018/CEECIND%2F01014%2F2018%2FCP1540%2FCT0002/PT
oaire.awardURIinfo:eu-repo/grantAgreement/FCT/6817 - DCRRNI ID/UIDB%2F00102%2F2020/PT
oaire.citation.startPage117122
oaire.citation.titleCarbohydrate Polymers
oaire.citation.volume252
oaire.fundingStream3599-PPCDT
oaire.fundingStream9471 - RIDTI
oaire.fundingStream6817 - DCRRNI ID
oaire.fundingStreamInvestigador FCT
oaire.fundingStreamCEEC IND 2018
oaire.fundingStream6817 - DCRRNI ID
person.familyNameMedronho
person.familyNameRomano
person.givenNameBruno
person.givenNameAnabela
person.identifier.ciencia-id6918-9AB3-8D22
person.identifier.ciencia-id8A18-7E9A-3B0E
person.identifier.orcid0000-0003-0972-1739
person.identifier.orcid0000-0002-7204-7428
person.identifier.ridP-5927-2014
person.identifier.scopus-author-id9940656700
person.identifier.scopus-author-id56249997600
project.funder.identifierhttp://doi.org/10.13039/501100001871
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project.funder.identifierhttp://doi.org/10.13039/501100001871
project.funder.nameFundação para a Ciência e a Tecnologia
project.funder.nameFundação para a Ciência e a Tecnologia
project.funder.nameFundação para a Ciência e a Tecnologia
project.funder.nameFundação para a Ciência e a Tecnologia
project.funder.nameFundação para a Ciência e a Tecnologia
project.funder.nameFundação para a Ciência e a Tecnologia
rcaap.rightsrestrictedAccess
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