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专业: 理论和计算化学

[求助] 介孔磷酸锆的问题已有2人参与

按照文献的方法制备介孔磷酸锆催化剂，但是烧完以后拿出来的粉末是黑色的，正常情况是应该是白色的，文献方法如下：

In a typical synthesis of mesoporous zirconium oxophosphate, 30 mL absolute ethanol was acidified with 3.30 g (35 wt %) hydrochloric acid. Then 2.0 g triblock copolymer pluronic F127 was added to this acidic ethanol medium and allowed to stir until dissolution. Then 3.84 g (0.01 M) zirconium-
(IV) butoxide (taken in 5 mL ethanol) was added slowly under vigorous stirring and allowed to stir for 30 min. During stirring precipitation should be avoided. Then, to this clear solution 1.16 g of (0.01 M) orthophosphoric acid (88 wt %, taken in 5 mL ethanol) was slowly dropwise added under vigorous stirring at ambient temperature. Then the reaction mixture was covered and allowed to stir overnight at room temperature. The mixture
was placed inside the oven at 343 K to undergo the EISA process. Finally, the obtained solid sample was calcined through slow increase of the temperature to 773 K (1 K min1 ramping rate) followed by heating at 773 K for 5 h in the presence of air to obtain template-free mesoporous zirconium oxophosphate.
(ACS Catal. 2011, 1, 493–501)

文献中用3.3g的盐酸酸化30mL的无水乙醇，然后加入2.0g的F127搅拌至溶解，继而加入3.84g正丁醇锆（5mL乙醇溶液）搅拌30min防止沉淀生成，最后加入1.16g磷酸乙醇溶液。过夜搅拌后，在70℃进行EISA过程（Evaporation induced self-assembly process），最终500℃煅烧得到介孔磷酸锆催化剂。

我在EISA过程是将磷酸锆放在蒸发皿中用带孔铝箔纸盖住放在70℃的烘箱中进行的，制备过程中所有物质的用量为文献中的10倍，煅烧后的粉末为黑色，请教一下做过磷酸锆的虫友是什么原因？

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