{"title":"Cellulose phosphorylation for cellulose nanofibrils production: impact of curing on the color change and chemical surface characterization","authors":"Arnaud Benard, Julien Bras, Cécile Sillard, Denis Curtil, Gaël Depres, Naceur Belgacem","doi":"10.1007/s10570-025-06415-z","DOIUrl":null,"url":null,"abstract":"<div><p>Cellulose phosphorylation as a pretreatment for CNF production is a robust process allowing to modify the surface charge of the fiber. However, cellulose phosphorylation is associated with a yellowing of the substrate and variations in the grafting of phosphate groups leading to crosslinking during intense curing. In this study, a design of experiment was conducted on a process of paper impregnation to limit the color change and maximize the degree of grafting of cellulose. The impregnation of the substrate was found to occur very rapidly, namely at 10s maximum. Whereas the color change was found to be dependent only on the curing parameters (time and temperature). The charge content model was reduced to 2 variables, i.e., the curing parameters, since the impregnation time was previously established to be very short and complete. Consequently, both models were combined allowing to determine optimal curing parameters: a temperature of 150°C for 20 min., yielding a minimum color change (6.0) and maximum charge content (1.0 mmol/g). Moreover, cellulose phosphorylation was characterized in bulk and surface by XPS and NMR, respectively. It did not reveal crystallinity changes in the pretreated cellulose. <sup>31</sup>P NMR allowed the estimation of the amount of crosslinking within cellulose matrix.</p><h3>Graphical abstract</h3>\n<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":511,"journal":{"name":"Cellulose","volume":"32 4","pages":"2599 - 2615"},"PeriodicalIF":4.9000,"publicationDate":"2025-02-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Cellulose","FirstCategoryId":"88","ListUrlMain":"https://link.springer.com/article/10.1007/s10570-025-06415-z","RegionNum":2,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"MATERIALS SCIENCE, PAPER & WOOD","Score":null,"Total":0}
引用次数: 0
Abstract
Cellulose phosphorylation as a pretreatment for CNF production is a robust process allowing to modify the surface charge of the fiber. However, cellulose phosphorylation is associated with a yellowing of the substrate and variations in the grafting of phosphate groups leading to crosslinking during intense curing. In this study, a design of experiment was conducted on a process of paper impregnation to limit the color change and maximize the degree of grafting of cellulose. The impregnation of the substrate was found to occur very rapidly, namely at 10s maximum. Whereas the color change was found to be dependent only on the curing parameters (time and temperature). The charge content model was reduced to 2 variables, i.e., the curing parameters, since the impregnation time was previously established to be very short and complete. Consequently, both models were combined allowing to determine optimal curing parameters: a temperature of 150°C for 20 min., yielding a minimum color change (6.0) and maximum charge content (1.0 mmol/g). Moreover, cellulose phosphorylation was characterized in bulk and surface by XPS and NMR, respectively. It did not reveal crystallinity changes in the pretreated cellulose. 31P NMR allowed the estimation of the amount of crosslinking within cellulose matrix.
期刊介绍：
Cellulose is an international journal devoted to the dissemination of research and scientific and technological progress in the field of cellulose and related naturally occurring polymers. The journal is concerned with the pure and applied science of cellulose and related materials, and also with the development of relevant new technologies. This includes the chemistry, biochemistry, physics and materials science of cellulose and its sources, including wood and other biomass resources, and their derivatives. Coverage extends to the conversion of these polymers and resources into manufactured goods, such as pulp, paper, textiles, and manufactured as well natural fibers, and to the chemistry of materials used in their processing. Cellulose publishes review articles, research papers, and technical notes.
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