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[求助]
MOF177的合成 已有1人参与
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跪求一份mof177的合成方法 @jackdeng @lich666 发自小木虫Android客户端 |
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【答案】应助回帖
| The synthesis of hexagonal geometry based MOF-177 (Fig. 1) involves the mixing of bromothymol blue (BTB) (0.07 gm) and salt Zinc Nitrate Hexahydrate (Zn-(NO3)2·6H2O) (0.32 gm) was dissolved in a mixture of organic solvents N,N-diethylformamide (DEF) (20 mL). The mixture was subjected to degassing three times using freeze-pump-thaw method and then stored in a reaction vial (20 mL) with filled and closed tightly. The reaction vial was placed in an oven for 7 days to maintain temperature at 67 °C. after 7 days, clear and transparent MOF-177 and can be seen at the bottom of the reaction vial. The reaction vial is than removed from the oven, decanted and washed with organic solvent N,N-diethylformamide (DEF) to remove the unreacted salt zinc nitrate hexahydrate (Zn-(NO3)2·6H2O). after this step, the reaction vial was filled with chloroform, closed tightly and put in an oven at 70 °C for another three days, and it was replenished with fresh chloroform every day. Because the MOF-177 crystals are vulnerable to moisture and air [22], they were stored and transported in a Schlenk flask under vacuum or in a vial filled with chloroform. |
3楼2024-11-19 08:59:32
rlafite
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【答案】应助回帖
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MOF-177的合成通常包括以下步骤： 材料准备 金属盐：常用的是锌盐（如醋酸锌或硝酸锌）。 有机配体：常用的是三苯基甲烷三羧酸（H3BTC）。 溶剂：常用的是二甲基甲酰胺（DMF）或其他适合的极性溶剂，如甲醇或乙醇。 合成步骤 溶液制备：将一定量的锌盐溶解在溶剂中，形成均匀的锌溶液。 将有机配体H3BTC溶解在另一份溶剂中，充分混合。 混合与加热：将金属盐溶液和有机配体溶液混合在一起，搅拌均匀。 将混合溶液转移到密封的反应容器（如高压反应釜或Teflon衬里的不锈钢反应釜）中。 在120°C左右的温度下加热12-24小时，进行溶剂热反应。 冷却与过滤：反应完成后，将反应釜冷却至室温。 过滤反应产物，收集固体。 清洗与干燥：用适量的新鲜溶剂（如DMF或甲醇）洗涤固体以去除未反应的残留物。 在适当的温度下（如60-100°C）干燥产物以得到MOF-177。 注意事项 溶剂纯度和反应温度对产物的晶体结构和孔隙特性有显著影响。 使用手套和通风良好的实验室环境，确保安全操作。 |
2楼2024-11-03 01:06:29
【答案】应助回帖
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MOF-177: Zn4O(C27H15O6)2. Benzene-1,3,5-tris(4-benzoic acid) (2.0 g, 4.6 *10-3 mol) and Zn(NO3)2·4H2O (7.2 g, 2.8*10-2 mol) were dissolved in 200ml of diethylformamide in a 500-ml jar.The jar was capped tightly and placed in a 100°C oven for 24 h. The mother liquor was decanted, and the colorless crystalline prod uct was washed with dimethylformamide and immersed in HPLC-grade (pentene-stabilized) chloroform, which was de canted and replaced with fresh chloroform three times over 4 days. Solvent was decanted from the product, which was placed in a Schlenk flask. The opening of the flask was cracked slightly to vacuum (just enough to see a pressure change on the Schlenk line) and left for 12 h. It was then opened slightly more and left for 12 h. It was then opened fully to vacuum and left for 24 h at room temperature. The sample was backfilled and stored under nitrogen. The BET surface area of the sample was measured to be 3,875 m2/g. |
4楼2024-11-19 09:07:03
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5楼2024-12-04 15:20:08
