Determination of the effective degree of cross-linking of porous cellulose membranes cross-linked with bifunctional epoxides. (1st January 2021)

• Record Type: Journal Article
• Authors: Ruhr, Dominik; John, Michael; Reiche, Annette
• Is Part Of: Carbohydrate polymers. Volume 251(2021)
• Publication Date: 2021-01-01
• Subjects: AGU anhydroglucose unit -- BDDE 1, 4-butanediol diglycidyl ether -- BDPE 1, 4-butanediol di-(propan-2, 3-diolyl) ether -- CA cellulose acetate -- CrD degree of cross-linking -- CrR effective cross-linker ratio -- DOSY Diffusion Ordered Spectroscopy -- HSQC Heteronuclear Single Quantum Correlation -- HYD Hydrosart® (cross-linked, regenerated cellulose) -- RC regenerated cellulose; Cellulose -- Epoxides -- Cross-linking density -- NMR spectroscopy; Polysaccharides -- Periodicals; Polysaccharides -- Periodicals; Polysaccharides -- Périodiques; Electronic journals; 547.78
• DOI: 10.1016/j.carbpol.2020.117043
• Languages: English
• ISSNs: 0144-8617

Abstract

Highlights: Cellulose membranes were cross-linked with 1, 4-butanediol diglycidyl ether. 1 H NMR method for determination of network parameters was developed. 1 H NMR method for network characterization was compared to gravimetric analysis. Cross-linking density was analyzed by thermogravimetric analysis. Effective cross-linker ratio around 50 %, independent of cross-linking parameters. Abstract: The cross-linking efficiency of a continuous process for the production of porous cellulose membranes cross-linked with 1, 4-butanediol diglycidyl ether (BDDE) under variation of four different process parameters (concentration of cross-linker, catalyst concentration, reaction temperature and reaction time) was studied. The analysis of the resulting network properties is based on gravimetric and titrimetric methods complemented by one-dimensional 1 H NMR analysis after degradation of the cross-linked cellulose membranes in aqueous zinc chloride solution. NMR results indicate that around 50 % of BDDE molecules are effectively cross-linking, the number being almost independent of the cross-linking conditions. Furthermore, thermogravimetric analysis of the cross-linked membranes showed a direct correlation between the degree of cross-linking and the decomposition temperature of the cellulose membranes.