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小木蟲論壇-學術(shù)科研互動平臺 » 材料區(qū) » 晶體 » 粉末晶體 » MOF177的合成
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風中搖曳的旭新蟲 (小有名氣)
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[求助]
MOF177的合成 已有1人參與
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跪求一份mof177的合成方法 @jackdeng @lich666 發(fā)自小木蟲Android客戶端 |
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【答案】應助回帖
| 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樓2024-11-19 08:59:32
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【答案】應助回帖
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MOF-177的合成通常包括以下步驟： 材料準備 金屬鹽：常用的是鋅鹽（如醋酸鋅或硝酸鋅）。 有機配體：常用的是三苯基甲烷三羧酸（H3BTC）。 溶劑：常用的是二甲基甲酰胺（DMF）或其他適合的極性溶劑，如甲醇或乙醇。 合成步驟 溶液制備：將一定量的鋅鹽溶解在溶劑中，形成均勻的鋅溶液。 將有機配體H3BTC溶解在另一份溶劑中，充分混合。 混合與加熱：將金屬鹽溶液和有機配體溶液混合在一起，攪拌均勻。 將混合溶液轉(zhuǎn)移到密封的反應容器（如高壓反應釜或Teflon襯里的不銹鋼反應釜）中。 在120°C左右的溫度下加熱12-24小時，進行溶劑熱反應。 冷卻與過濾：反應完成后，將反應釜冷卻至室溫。 過濾反應產(chǎn)物，收集固體。 清洗與干燥：用適量的新鮮溶劑（如DMF或甲醇）洗滌固體以去除未反應的殘留物。 在適當?shù)臏囟认拢ㄈ?0-100°C）干燥產(chǎn)物以得到MOF-177。 注意事項 溶劑純度和反應溫度對產(chǎn)物的晶體結(jié)構(gòu)和孔隙特性有顯著影響。 使用手套和通風良好的實驗室環(huán)境，確保安全操作。 |
2樓2024-11-03 01:06:29
【答案】應助回帖
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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樓2024-11-19 09:07:03
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5樓2024-12-04 15:20:08
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