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Nano-sized mesoporous phosphated tin oxide as an efficient solid acid catalyst

机译：纳米级介孔磷酸盐氧化锡作为一种有效的固体酸催化剂

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Herein, we prepared a mesoporous tin oxide catalyst (mSnO _(2) ) activated with phosphate species by the adsorption of phosphate ions from a phosphoric acid solution onto tin oxyhydroxide (Sn(OH) _(4) ) surface. The phosphate content ranged from 3 to 45 wt%. The nonaqueous titration of n -butylamine in acetonitrile was used to determine the total surface acidity level. FTIR of chemically adsorbed pyridine was used to differentiate between the Lewis and Br?nsted acid sites. Thermal and X-ray diffraction analysis indicated that the addition of phosphate groups stabilized the mesostructure of mSnO _(2) and enabled it to keep its crystalline size at the nanoscale. FTIR analysis indicated the polymerization of the HPO _(4) ~(2?) groups into P _(2) O _(7) ~(4?) , which in turn reacts with SnO _(2) to form a SnP _(2) O _(7) layer, which stabilizes the mesoporous structure of SnO _(2) . The acidity measurements showed that the phosphate species are distributed homogeneously over the mSnO _(2) surface until surface saturation coverage at 25 wt% PO _(4) ~(3?) , at which point the acid strength and surface acidity level are maximized. The catalytic activity was tested for the synthesis of hydroquinone diacetate, where it was found that the % yield of hydroquinone diacetate compound increased gradually with the increase in PO _(4) ~(3?) loading on mSnO _(2) until it reached a maximum value of 93.2% for the 25% PO _(4) ~(3?) /mSnO _(2) catalyst with 100% selectivity and excellent reusability for three consecutive runs with no loss in activity.
机译：在这里，我们制备了一种中孔氧化锡催化剂（mSnO _（2）），该吸附剂通过将磷酸离子从磷酸溶液吸附到羟基氧化锡（Sn（OH）_（4））表面上而被磷酸盐激活。磷酸盐含量为3至45重量％。用非水滴定乙腈中的正丁胺来测定总表面酸度。化学吸附吡啶的FTIR用于区分路易斯酸和布朗斯台德酸位点。热和X射线衍射分析表明，磷酸基团的添加稳定了mSnO_（2）的介观结构，使其能够将其晶体尺寸保持在纳米级。 FTIR分析表明，HPO_（4）〜（2？）基团聚合成P _（2）O _（7）〜（4？），后者又与SnO _（2）反应形成SnP _ （2）O _（7）层，可稳定SnO _（2）的介孔结构。酸度测量表明，磷酸盐种类均匀地分布在mSnO _（2）表面上，直到表面饱和度达到25 wt％PO _（4）〜（3？）为止，此时酸强度和表面酸度水平达到最大。 。测试了对苯二酚对苯二酸酯的催化活性，发现对苯二酚对苯二酸酯化合物的％收率随mSnO _（2）上PO _（4）〜（3？）负载的增加而逐渐增加，直至达到25％PO _（4）〜（3？）/ mSnO _（2）催化剂的最大值为93.2％，具有100％的选择性，并且连续三个连续运行具有出色的可重复使用性，而不会损失活性。

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