National Institute of Oceanography and Fisheries, NIOF, Kayet Bey, El-Anfoushy, Alexandria, Egypt.
Sci Rep. 2022 Apr 4;12(1):5643. doi: 10.1038/s41598-022-09669-w.
Ferric perchlorate was tested for the first time as a new catalyst to accelerate the esterification of microcrystalline cellulose (MCC) at room temperature in a less amount of acetic anhydride compared to the amount used in the conventional methods. It was possible to manufacture cellulose acetate (CA) with a high yield of up to 94%. The influence of changes in reaction time, catalyst amounts, and acetic anhydride on the characterization of cellulose acetate produced was investigated. The optimum condition for esterification of 2.0 g (12.34 mmol) MCC was found to be: 10 mL (105.98 mmol) ACO, 200 mg (0.564 mmol, anhydrous basis) of Fe(ClO)·xHO and 1 h reaction time at room temperature. The substitution degree of CA was investigated by FTIR and H-NMR spectroscopy. Thermal stability of CA was studied using TGA, DTA and DSC analyses. The degree of polymerization and the polydispersity index (PDI) were obtained using Gel permeation chromatography (GPC). This study verified the direct and efficient synthesis of di- and tri-cellulose acetate in one-pot reaction using Fe(ClO)·xHO as a catalyst without using solvent.
高氯酸铁首次被测试为一种新型催化剂,可在室温下,与传统方法相比,在较少的乙酸酐用量下,加速微晶纤维素(MCC)的酯化反应。有可能以高达 94%的高产率制造纤维素醋酸酯(CA)。研究了反应时间、催化剂用量和乙酸酐变化对所制得的醋酸纤维素的特性的影响。发现 2.0g(12.34mmol)MCC 酯化的最佳条件为:10mL(105.98mmol)ACO、200mg(0.564mmol,无水基础)Fe(ClO)·xHO 和 1h 室温反应时间。通过傅里叶变换红外光谱(FTIR)和氢核磁共振光谱(H-NMR)研究了 CA 的取代度。通过热重分析(TGA)、差示热分析(DTA)和差示扫描量热分析(DSC)研究了 CA 的热稳定性。通过凝胶渗透色谱(GPC)获得了聚合度和多分散指数(PDI)。该研究验证了使用 Fe(ClO)·xHO 作为催化剂,在无溶剂的情况下,一锅法直接、高效地合成二和三醋酸纤维素。