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dxyan木虫 (正式写手)
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[求助]
MIL-101的合成及纯化
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采用不用HF合成MIL-101(Cr)，参考文献：Chem. Mater. 2012, 24, 166。但是做了很久比表面上不去。2200左右。其中DMF洗部分也洗了3次，每次12小时，70度，但是比表面积也就2400。DMF洗涤后也用甲醇，丙酮各洗过3，4次。但是BET依旧不行，吸附仪活化也达到足够的时间。合成完后釜壁面有灰色的一层，在各种溶剂洗的过程中离心完后离心管底部有层灰色的，但是大部分是绿色。谁能帮忙分析一下会是什么原因。原料或者釜的原因吗？加HF酸的方法也试过了，水洗醇洗后，加入氟化铵，然后再水洗，醇洗。但是比表面都2000以下。氟化铵交换2次，BET才达到2200。求各位帮忙分析一下，谢谢！ Cr(NO3)3·9H2O (1.0 g, 2.5 mmol), terephthalic acid (0.42 g, 2.5 mmol), and deionized water (10 mL) were blended and briefly sonicated resulting in a dark blue-colored suspension. The suspension was placed in a Teflon-lined autoclave bomb and kept in an oven at 218 °C for 18 h. After the bomb cooled down to room temperature, the resultant fine green MIL-101 crystals were separated from water using a centrifuge and washed with water, methanol and acetone. The suspension in acetone was centrifuged and separated, the solids were placed in N, N-dimethylformamide (10 mL) and the suspension was sonicated for 10 min and then kept at 70 °C overnight. The resulting solids were separated by centrifugation, repeatedly washed with methanol and acetone, dried at 75 °C overnight, |
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2楼2024-11-13 21:55:13