Substituted Nickel Phthalocyanines Methods Of Preparation

Author : Yuping Bao
Publisher :
ISBN 13 :
Total Pages : 0 pages
Book Rating : 4.:/5 (136 download)

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Download or read book Synthesis of Substituted Phthalocyanines, Incorporation Into Hierarchically Porous Carbons and Faujasites and Evaluation As Heterogenous Catalysts written by Yuping Bao and published by . This book was released on 2022 with total page 0 pages. Available in PDF, EPUB and Kindle. Book excerpt: Hierarchically porous carbon and faujasite are two supports in which metal phthalocyanines are incorporated for evaluation as heterogeneous catalysts. Water-soluble metal phthalocyanine metal phthalocyanine tetra carboxylate/acid (MPCTC), anionic phthalocyanine, amphiphilic phthalocyanine tetra PEGylated metal phthalocyanine (TPEGMPC), and neutral phthalocyanine were synthesized and incorporated into hierarchically porous carbon (HPC) using a co-gelation method. The metals explored with both phthalocyanines were, M = Ni, Cu, Co, Fe, Ru, and VO. The tetra PEGylated metal phthalocyanines explored had peg molecular weights of 50, 200, 400 and 600. The synthesis of MPCTC used trimellitic acid as starting material in a one pot process. It was found that the anionic form of phthalocyanine is not soluble in the solvent used for HPC formation at low pH but soluble at high pH. The synthesis of TPEGMPC was through a two-step process starting from 4-nitrophthalonitrile in which a metal ion behaves as a template that facilitates the tetramerization/cyclization process. TPEGMPC was found insoluble or only slightly soluble for the lower peg chain lengths but solubility was increased with increasing peg chain length. Formation of the PEG-1000 was not possible as cyclization did not occur with PEG -1000. HPC was prepared by a resorcinol/formaldehyde polymerization process to which the non-ionic surfactant F-127, was added to give mesopore formation. 1,6-diaminohexane (DAH) was added as a structure directing agent to give macropores. After the polymerization is completed in a curing step, the polymer was converted to a hierarchically porous carbon by pyrolysis at 500 ℗ʻC. HPC synthesis was carried out with addition of various MCMPC's and of TPEGMPCs. It was observed that after the curing step, MPCTC had separated from the bulk of the material and been spatially concentrated at the bottom of the sample. Similar phase separation was observed with the shortest peg chain length TPegMPC, while with higher peg chain length uniform color in the material was observed. Physical characterization of the carbon incorporating TPEGMPCs was done by SEM, TEM, XRD, gas absorption, UV-Vis, and FTIR. These carbons were evaluated as catalysts for oxidation of cyclohexene and reduction of p-nitrophenol. For both copper and nickel TPEGMPCs, large metal nanoparticles were observed for the 200 and 600 molecular weight TPEGMPCs. The 400 molecular weight sample showed much smaller nanoparticles, about 1/5th to 1/10 as large. The catalytic activity did not follow this trend, with the activity decreasing as the Peg molecular weight increased. Metal perfluoro phthalocyanines (MPfPC) were synthesized with the M=Fe and VO using tetrafluoro phthalonitrile as starting material. Viable synthesis procedures were developed by modifying an established synthesis route. Both MPfPC and MPCTC were successfully incorporated into a zeolite sodium faujasite by adding the phthalocyanine to the synthesis gel from which the sodium faujasite is grown.