含4,4'-二苯乙烯二羧酸之鉻金屬有機骨架的優化合成與氣體吸附性質研究

Synthesis optimization and gas adsorption of chromium metal-organic frameworks based on 4,4'-stilbene carboxylic acid

黃芷娟(Zhi-Juan Huang)

指導教授 ： 林嘉和

中原大學/理學院/化學研究所/碩士(2014年)

https://doi.org/10.6840/cycu201400591

摘要

在本論文中，利用等結構的概念(Isoreticular chemistry)52延展有機配位基(ligand)長度來合成金屬有機骨架(Metal-Organic Framewoks, MOFs)化合物，所採用的配位基為4,4'-二苯乙烯二羧酸(4,4'- stilbenedicarboxylic acid, H2SDC)。優化合成上利用氟化銨(NH4F)，氟化鉀(KF)作為合成時不同含氟添加劑的來源以合成出MOFs孔洞材料，分別為：

[Cr3F/OH(H2O)2O(SDC)3]……..(1)
[Cr(OH)(SDC)]…………...........(2)

在結構鑑定上，以粉末X-光繞射儀(PXRD)來鑑定產物是否被成功的合成出；利用掃描式電子顯微鏡(SEM) 觀察晶體形貌來佐證PXRD的結果，並測量熱重分析(TGA)測定樣品熱重損失及用氣體吸脫附儀分析氣體孔洞特性，驗證合成上是否優化。優化合成上顯示氟化銨或氟化鉀的添加量在 約0.06~0.10 毫莫耳左右可使MOFs孔洞材(1)有最佳的表面積。另外，氟化銨比氟化鉀的添加展現較高的孔洞性。

關鍵字

金屬有機骨架，4‚4'-二苯乙烯二羧酸

並列摘要

In this thesis, the concept of isoreticular chemistry was used by extended the length of organic ligands in the synthesis of Metal-Organic frameworks (MOFs). The ligand used in this study is 4,4'-stilbene dicarboxylic acid (H2SDC).The optimization synthesis was achieved by using ammonium fluoride (NH4F), potassium fluoride (KF) as additives. The study MOFs were listed as:

[Cr3F/OH(H2O)2O(SDC)3]……..(1)
[Cr(OH)(SDC)]…………...........(2)

On the structural identification, powder X-ray diffraction can identify the product phases; scanning electron microscopy (SEM) displays the crystal morphology and size; thermogravimetric analysis (TGA) measures sample weight loss under heating; gas adsorption displays the porous behaviors. All measurements confirmed the optimization synthesis in both MOFs. The final results display optimized addition of ammonium fluoride and potassium fluoride is about 0.06~0.10 mmole and result in higher specific surface area of MOF (1). In addition, the higher porosity can be observed in the addition of ammonium fluoride when compare to potassium fluoride.

並列關鍵字

4‚4'- stilbenedicarboxylic acid ； Metal-Organic Framewoks

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