鋁金屬有機骨架之合成與孔洞性質探討

Synthesis and Porosity of Aluminum-based Metal-Organic Frameworks

陳玟靜(Wun-Jing, Chen)

指導教授 ： 林嘉和

中原大學/理學院/化學研究所/碩士(2017年)

https://doi.org/10.6840/cycu201700240

摘要

在本研究論文中，藉由「不同加熱方式」及「改變金屬試劑濃度」合成孔洞性鋁金屬有機骨架化合物(Al-MOFs)，Al-MOFs經由最佳活化方法後得到高氮氣吸脫附曲線與BET比表面積。
以溶劑熱法(Solvothermal)及一般加熱法(Heating)將金屬試劑三氯化鋁(AlCl3)與配位基(E)-4-(2-carboxyvinyl)benzoic acid (H2CVB)、4,4'-((1E,1'E)-hydrazine-1,2-iylidenebis(methanylylidene))dibenzoic acid (H2DMDA)進行反應合成Al-MOFs。進一步利用一般加熱法，在固定配位基濃度及溶劑體積的條件下，調控金屬試劑的莫爾數濃度，合成不同M/L比例之Al-MOFs。
Al-MOFs產物經過最佳的活化條件之後，以粉末X-ray繞射儀(PXRD)來鑑定化合物結構，場發射式掃描電子顯微鏡(FE-SEM)觀察表面外觀，孔隙及表面積分析儀測定化合物之孔洞特性與各種比例的氮氣等溫吸附，以及固態核磁共振光譜儀(27Al-NMR)分析鋁金屬的配位模式。實驗結果，AlCVB系統中M/L = 1.30之化合物1c具有最高BET比表面積2939.7 m2/g，孔徑分布10.9、15.6 Å；AlDMDA系統中M/L = 2.00之化合物2e具有最高BET比表面積3561.4 m2/g，孔徑分布32.0 Å。

關鍵字

鋁金屬有機骨架化合物

並列摘要

In this study, two new aluminium metal-organic frameworks (Al-MOFs) have been synthesized via solvothermal methods and heating methods by using aluminium chloride (AlCl3) as matel reagents, with (E)–4-(2–carboxyvinyl)benzoic acid (H2CVB) and 4,4'-((1E,1'E)-hydrazine-1,2-iylidenebis(methanylylidene))dibenzoic acid (H2DMDA) as linkers. Further, we have synthesized Al-MOFs by using various metal/ligand (M/L) ratio with fixed ligand quantity in order to study the influence of M/L ratio on the properties of the resulted Al-MOFs.
The structure of the synthesized Al-MOFs has been studied by using the powder X-ray diffraction (PXRD) data. The field emission scanning electron microscopy (FE-SEM) has been used to analyze and compare the shape and particle size of the Al-MOFs synthesized under various conditions. The surface area and porosity of the synthesized Al-MOFs were characterized by using N2 gas sorption measurements at 77 K. Moreover, the solid state 27Al nuclear magnetic resonance spectral (27Al-NMR) analysis has been used to evaluate the effect of synthetic condition on the coordination environment of Al in the synthesized Al-MOFs.
In the AlCVB system, M/L = 1.30 of compund 1c has the highest BET surface area is 2939.7 m2/g, and pore size distribution is 10.9、15.6 Å; in the AlDMDA system, M/L = 2.00 of compund 2e has the highest BET surface area is 3561.4 m2/g, and pore size distribution is 32.0 Å.

並列關鍵字

Al-MOFs

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