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Acetylation of glycerol using MgO–CaO catalysts with different CaO loadings
Reaction Kinetics, Mechanisms and Catalysis ( IF 1.7 ) Pub Date : 2020-04-13 , DOI: 10.1007/s11144-020-01774-z
Ma. Elena Manríquez-Ramírez , Ignacio Elizalde , Román Ramírez-López , Martín Trejo-Valdez , Miriam Estrada-Flores

The synthesis of three catalytic samples of MgO–CaO containing 20, 30, 50 wt% of CaO was carried out by a co-precipitation method. Also pure MgO and CaO were prepared. Infrared spectroscopy, Raman, X-ray photoelectron, X-ray diffraction, atomic force microscopy and Temperature-Programmed Desorption of CO2 characterized powder samples. Those analyses permitted to differentiate phases in mixed oxides in catalysts and to identify phases that gave a basic character to solid samples. The powders were used to catalyze the acetylation of glycerol to produce mono, di and triacetin at 70 °C during 280 min. The reaction products were followed by IR, and gas chromatograph analysis. The highest glycerol conversion (89%) was attained by using 50MgO–50CaO catalytic sample, while pure MgO exhibited the poorest conversion (of c.a. 64%). Regarding selectivity toward triacetin, the catalyst containing 50 wt% CaO was the best, reaching a value of ~ 92%, while yielding the lowest diacetin and monoacetin (0.5 and 5%, respectively). Despite the catalyst types, triacetin selectivity profiles showed increased as reaction time did, whereas diacetin underwent a continuous decrease and monoacetin remained almost constant with the reaction time. The study results demonstrated that MgO–CaO mixed oxides provided a synergetic effect in glycerol acetylation in terms of both conversion and selectivity to valuable products.



中文翻译:

使用不同CaO含量的MgO–CaO催化剂对甘油进行乙酰化

通过共沉淀法合成了含有20、30、50 wt%的CaO的MgO-CaO的三个催化样品。还制备了纯MgO和CaO。红外光谱,拉曼光谱,X射线光电子,X射线衍射,原子力显微镜和程序升温脱附的CO 2表征粉末样品。这些分析可以区分催化剂中混合氧化物的相,并鉴定出赋予固体样品基本特征的相。该粉末用于催化甘油的乙酰化反应,在280分钟内于70°C产生甘油单,双和三醋精。反应产物之后进行IR和气相色谱分析。使用50MgO–50CaO催化样品可获得最高的甘油转化率(89%),而纯MgO表现出最差的转化率(约64%)。关于对三醋精的选择性,含50wt%CaO的催化剂是最好的,达到〜92%的值,而产生最低的双醋精和单醋精(分别为0.5和5%)。尽管催化剂类型不同,三醋精的选择性随反应时间的增加而增加,而双醋精持续下降,而单醋精几乎保持恒定不变。研究结果表明,MgO-CaO混合氧化物在甘油乙酰化方面对转化和对有价值产品的选择性均具有协同作用。

更新日期:2020-04-22
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