SOLVOTHERMAL SYNTHESIS AND CHARACTERIZATION OF TEREPHTHALIC ACID-BASED METAL-ORGANIC FRAMEWORKS AND THEIR CATALYTIC APPLICATION IN BIODIESEL PRODUCTION

C. Odu, C. Obunwo, O. Bull
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Abstract

Metal-Organic Frameworks (MOFs) are a class of porous crystalline materials, consisting of metal ions or nodes linked with organic ligands. The study was aimed at solvothermal synthesis and characterization of terephthalic acid-based Metal-Organic Frameworks and their catalytic application in biodiesel production. Three MOFs of Cu-, Fe-, and Cr-based were solvothermally synthesized, characterized and applied as catalysts in biodiesel production using ethanol and oil extracted from Yellow Oleander seeds. The MOFs were synthesized using terephthalic acid as the linker and copper (II), iron (III) and chromium (III) nitrates as metal ion sources. Each of the synthesized MOFs showed high melting point exceeding 360 oC. Microscopic view and powder X- ray diffraction analysis indicated Cu-MOF to be crystalline with numerous sharp peaks while those for Fe- and Cr-MOFs were amorphous. A comparison of the FT-IR spectra of the ligand and those of the MOFs confirmed the presence of the ligand in the synthesized MOFs. In the absence of a catalyst, the transesterification was not achieved. However, in the presence of the more crystalline Cu-MOF as catalyst resulted to high yield (83.33%) and in a shorter time compared to the less crystalline Fe- (33.33%) and Cr- (25.00%) MOFs. Thus, catalytic ability of the MOFs were in the order: Cu-MOF > Fe-MOF > Cr-MOF. Hence MOFs especially Cu-MOFs can be applied as catalyst in biodiesel production. Further studies and characterization (single X-ray diffraction) should be done for proper elucidation of the crystal structure of the MOFs.  
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对苯二甲酸基金属有机骨架的溶剂热合成与表征及其在生物柴油生产中的催化应用
金属有机骨架(mof)是一类由金属离子或节点与有机配体连接而成的多孔晶体材料。研究了以对苯二甲酸为基础的金属有机骨架的溶剂热合成、表征及其在生物柴油生产中的催化应用。以黄夹竹桃种子为原料,以乙醇和油为原料,溶剂热合成了三种铜基、铁基和铬基mof,并对其进行了表征,并将其作为催化剂应用于生物柴油生产。以对苯二甲酸为连接剂,以铜(II)、铁(III)和硝酸铬(III)为金属离子源,合成了mof。每一种合成的MOFs均具有超过360℃的高熔点。显微观察和粉末X射线衍射分析表明,Cu-MOF呈结晶状,有许多尖峰,而Fe-和cr - mof呈非晶态。将该配体与mof的红外光谱进行比较,证实了该配体存在于合成的mof中。在没有催化剂的情况下,酯交换反应不能进行。然而,与结晶度较低的Fe- mof(33.33%)和Cr- mof(25.00%)相比,结晶度较高的Cu-MOF在较短的时间内获得了较高的收率(83.33%)。因此,mof的催化性能依次为Cu-MOF > Fe-MOF > Cr-MOF。因此,mof特别是cu - mof可以作为催化剂应用于生物柴油的生产。进一步的研究和表征(单x射线衍射)需要正确地阐明mof的晶体结构。
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