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Quantification of cellulose nanowhiskers sulfate esterification levels
Jin Gu1, Jeffrey M Catchmark, Edward Q Kaiser
1Intercollege Graduate Degree Program in Plant Biology, The Pennsylvania State University, University Park, PA 16802, USA.
Carbohydrate Polymers
|February 13, 2013
Summary
Sulfation of cellulose nanowhiskers (CNWs) using sulfuric acid introduces surface sulfate groups. Desulfation methods partially remove these groups, indicating significant surface modification of CNWs.
Area of Science:
- Materials Science
- Surface Chemistry
- Nanotechnology
Background:
- Cellulose nanowhiskers (CNWs) are derived from cellulose, a renewable biopolymer.
- Surface functionalization of CNWs is crucial for tailoring their properties.
- Sulfation is a common surface modification technique.
Purpose of the Study:
- To quantify the degree of desulfation of cellulose nanowhiskers (CNWs).
- To investigate the effectiveness of different desulfation methods.
- To understand the extent of sulfate esterification on CNW surfaces.
Main Methods:
- Fourier transform infrared spectroscopy (FTIR)
- X-ray photoelectron spectroscopy (XPS)
- Combustion gas analysis
- N(2) adsorption
- Acid-catalyzed desulfation
- Solvolytic desulfation
Main Results:
- Hydrolysis with H(2)SO(4) introduced sulfate groups onto CNWs, increasing sulfur content.
- Commercial cellulose contained sulfur prior to hydrolysis.
- Neither acid-catalyzed nor solvolytic desulfation completely removed sulfate groups.
- Over one-third of surface hydroxyl groups were estimated to be substituted by sulfate.
Conclusions:
- Sulfuric acid hydrolysis leads to significant surface esterification of CNWs.
- Existing desulfation methods are insufficient for complete removal of sulfate groups.
- Surface modification of CNWs with sulfate groups is substantial and persistent.
