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Anion supported TiO2-ZrO2 nanomaterial synthesized by reverse microemulsion technique as an efficient catalyst for solvent free nitration of halobenzene

机译:阴离子支持通过反向微乳液技术合成的TiO2-ZrO2纳米材料作为溶剂自由硝化卤苯的有效催化剂

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摘要

Mixed oxide like TiO2-ZrO2 in nanoscale were synthesized using reverse microemulsion process and characterized by XRD,TEM,FT-IR and surface area measurement.Anion supported mixed oxide systems were evaluated for the solvent free nitration of halobenzene even at low temperature(30 °C)reaction.Nitration yield increases with the increase in reaction temperature up to 70 °C.Mostly 500 °C calcined sample was found to be most active catalyst for nitration reaction and further increase in the calcination temperature decreases the yield.Both the in situ and ex situ sulphated samples show higher yield and para selectivity even at low temperature reaction.Higher para selectivity is explained with a proposed mechanism involving Lewis acid site.It is also marked that the para selectivity decreases with the change in halo group from chloro to iodo keeping the total yield nearly same.The decrease in para selectivity can be explained on the basis of -I effect(Cl > Br > I)of the halo group which effects the nearest ortho position and hence the higher ortho product.
机译:使用反向微乳液法合成纳米级中的TiO 2-ZrO 2如XRD,TEM,FT-IR和表面积测量。评价溶剂的溶剂氧化氢苯并均匀卤苯的混合氧化物体系,即使在低温下(30° c)反应。反应温度的增加,硝化产率随高达70℃的增加而增加。最多500℃煅烧样品是硝化反应的最活性催化剂,煅烧温度的进一步增加降低了产量。原位降低了产量和Ex原位硫酸化样品表明,即使在低温反应下,也显示出更高的产量和对照选择性。用涉及路易斯酸遗址的提出机制来解释高度的对照选择性。还标志着对来自氯对碘的卤素组的变化降低了Para选择性降低保持总收益率几乎相同。可以根据-I效果(Cl> Br> i)的卤素组的-I效应(Cl> Br> I)来解释Para选择性的降低TS最接近的邻接位置,因此较高的Ortho产品。

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