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maple_5211

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[求助] 请教一下钼钒杂多酸的重结晶具体方法已有1人参与

之前做了几中钼钒磷杂多酸，做了ICP，感觉钼、钒、磷的比例不是很对，我觉得可能是重结晶的不好，杂质太多，求大家指教下重结晶的具体方案，感觉杂多酸在水中溶解度太大了，热过滤的话是不是损失的太多啊？还有如果有高人有更好的制备纯净的H4PMo11VO4•xH2O、H5PMo10V2O40•xH2O 、H6PMo9V3O40•xH2O 也请帮忙说下，十分感谢啊！

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1楼 2013-11-12 17:07:06

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yingkai

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6楼: Originally posted by smq712 at 2013-11-22 22:17:08
没反应的原料一般都会有的，沉淀一般都是以粉末形式存在的，对不对？也有用浓硫酸重结晶的，然后放在冰箱里结晶。...

您好，请我用这种方式做的H4PMo11VO40，如何重结晶呢？谢谢您！ The molybdovanadophosphoric heteropolyacid H4PMo11VO40 was prepared according to the procedure reported in the literature31 as follows: 15.8 g of MoO3 and 0.91 g of V2O5 were added into 250 mL of deionized water and the suspension was then heated up to 100 ℃ under stirring. Afterward, 1.15 g of H3PO4 (85 wt.% aqueous solution) was added into the above−prepared suspension. After the suspension became clear and transparent（透明的）, it was cooled to room temperature. Finally, the water in the solution was evaporated in a rotary evaporator（旋转蒸发仪） at 50 °C and an orange solid was collected, into which a suitable amount of deionized water was added for the puriﬁcation of H4PMo11VO40 powder by recrystallization