Trimethylsilylcellulose synthesis revisited |
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| Institution: | 1. Center for Rubber Composite Materials and Structures, Harbin Institute of Technology, Weihai, 264209, China;2. Center for Composite Materials, Harbin Institute of Technology, 150001, China;3. Indian Institutes of Technology at Kanpur, 208016, India;1. Laboratory of Polysaccharide Chemistry, Institute of Bioorganic Chemistry, Uzbekistan Academy of Sciences, M. Ulugbek str. 83, 100125 Tashkent, Uzbekistan;2. Centre of Excellence for Polysaccharide Research, Institute of Organic and Macromolecular Chemistry, Friedrich Schiller University of Jena, Humboldtstraße 10, D-07743 Jena, Germany |
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| Abstract: | A simplification of the overall method of producing trimethylsilylcellulose solutions in common organic volatile solvents is reported. Microcrystalline cellulose was derivatized aiming its solubilization in tetrahydrofuran and toluene to obtain ultra-thin films of cellulose by spin-coating. The main simplifications are: 1) elimination of a swelling step before dissolution in the binary solvent N,N-dimethylacetamide/LiCl by using microcrystalline cellulose; 2) derivatization of cellulose –OH groups with –Si(CH3)3 groups was successful with no additional catalyst, like trimethylsilyl chloride, the degree of substitution (DS) being 2.2 ± 0.1. The DS at the extreme surface of the films was computed from the X-ray Photoelectron Spectroscopy data: using solely C 1s fitted component areas and, alternatively, from both C 1s and Si 2p areas. The DS estimated with a technique specific of the surface is close to the bulky one obtained from gravimetric measurements reported in the literature for materials synthesized with catalyst. The topographic uniformity is shown by Atomic Force Microscopy. |
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| Keywords: | Cellulose Silylation Solubilization XPS AFM |
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