In the present study, a sulphated siliceous zirconia catalyst (SSZ-550) has been prepared and characterized by XRD and FTIR analysis to indicate the incorporation of sulphate group over the matrix. X-ray photoelectron spectroscopy also revealed that sulphur group was incorporated over the matrix to impart the Brønsted acidity to the catalyst which is vital for the acetylation activity. To optimize the reaction parameters, viz. reagent molar ratios (3–12; glycerol/acetic acid), catalyst amount (1–5 wt%; catalyst/glycerol), reaction duration (20–50 min) and reaction temperature (30–100 °C) have been varied to obtain the optimum catalyst activity for the maximum glycerol triacetate yield. Finally, under the optimized reaction parameters of 9:1 glycerol/acetic acid molar ratio, 3 wt% catalyst, 80 °C reaction temperature and 40 min of reaction duration, a 93% glycerol triacetate yield was obtained. The catalyst was recovered from the reaction mixture and reused during six consecutive reaction runs while retaining 50% glycerol triacetate selectivity in the last cycle. A plausible mechanism suggests the heterogeneous catalyst-assisted protonation of carbonyl group of acetic acid to initiate the stepwise esterification of the hydroxyl groups of glycerol.

中文翻译：

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硫酸功能化硅质氧化锆作为合成三乙酸甘油酯的有效且可重复使用的催化剂

在本研究中，已制备了硫酸化硅质氧化锆催化剂（SSZ-550），并通过XRD和FTIR分析对其进行了表征，以表明在基体上引入了硫酸根。X射线光电子能谱还表明，在基体上结合了硫基团，以赋予催化剂布朗斯台德酸度，这对于乙酰化活性至关重要。为了优化反应参数，即。试剂摩尔比（3–12；甘油/乙酸），催化剂量（1–5 wt％；催化剂/甘油），反应时间（20–50分钟）和反应温度（30–100°C）已改变为获得最大的甘油三乙酸酯收率的最佳催化剂活性。最后，在9：1的甘油/乙酸摩尔比，3 wt％的催化剂，80°C的反应温度和40分钟的反应持续时间的优化反应参数下，获得93％的甘油三乙酸酯产率。从反应混合物中回收催化剂，并在六个连续的反应过程中重复使用，同时在最后一个循环中保持50％的甘油三乙酸酯选择性。一个合理的机理表明，乙酸羰基的非均相催化剂辅助质子化可引发甘油羟基的逐步酯化。