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maple_5211

木虫 (小有名气)

[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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yingkai

金虫 (正式写手)

引用回帖:
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
10楼2018-10-01 11:55:48
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smq712

银虫 (初入文坛)

【答案】应助回帖

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jiangyun2: 金币+1, 应助指数+1, 谢谢回帖交流,欢迎常来~~ 2013-11-19 09:01:17
maple_5211(jiangyun2代发): 金币+10 2013-11-29 09:14:38
我也重结晶过  5%硫酸,真空干燥箱  没了
2楼2013-11-18 23:01:40
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maple_5211

木虫 (小有名气)

引用回帖:
2楼: Originally posted by smq712 at 2013-11-18 23:01:40
我也重结晶过  5%硫酸,真空干燥箱  没了

就加5%的硫酸,然后热过滤,在干燥就OK了?
3楼2013-11-19 08:57:42
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smq712

银虫 (初入文坛)

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3楼: Originally posted by maple_5211 at 2013-11-19 08:57:42
就加5%的硫酸,然后热过滤,在干燥就OK了?...

热过滤得加过氧化氢  要不该绿了

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4楼2013-11-20 21:03:56
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