Cold NaOH/urea aqueous dissolved cellulose for benzylation: Synthesis and characterization |
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Authors: | Ming-Fei Li Shao-Ni Sun Feng Xu Run-Cang Sun |
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Institution: | aInstitute of Biomass Chemistry and Technology, Beijing Forestry University, 100083 Beijing, China;bState Key Laboratory of Pulp and Paper Engineering, South China University of Technology, 510640 Guangzhou, China |
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Abstract: | Cold NaOH/urea aqueous dissolved cellulose was studied for the synthesis of benzyl cellulose by etherification with benzyl chloride. By varying the molar ratios of benzyl chloride to OH groups in cellulose (1.5–4.0) and reaction temperatures (65–70 °C), benzyl cellulose with a degree of substitutions (DS) in the range of 0.29–0.54 was successfully prepared under such mild conditions. The incorporation of benzyl groups into cellulose was evidenced by multiple spectroscopies, including FT IR, 1H NMR, 13C NMR, CP/MAS 13C NMR and XRD. In addition, the thermal stability and surface morphology of the benzyl cellulose was also investigated with regard to the degree of substitution. The results indicated that the benzyl cellulose product with a low DS (0.51) in the present study reached the same solubility in many organic solvents as compared to those prepared in heterogeneous media. After benzylation, the sample decomposed at a lower temperature with a wider temperature range, which indicated that the thermal stability of benzyl cellulose was lower than that of the native cellulose. In addition, benzylation resulted in a pronounced reduction in crystallinity as well as a fundamental alteration of morphology of the native cellulose. |
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Keywords: | Benzyl cellulose Etherification NaOH/urea aqueous solution NMR spectroscopy Thermal stability |
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