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Preparation, Characterization and Catalytic Application of Organic-inorganic Hybrid Mesoporous Silicas Incorporating Functionalized Ionic Liquid Moieties

Author: ZhaoHaiHong
Tutor: YinDongHong
School: Hunan Normal University
Course: Organic Chemistry
Keywords: Functionalized ionic liquids Organic - inorganic hybrid mesoporous materials Fu - g alkylation G Brain Man Gail reaction Benzyl alcohol oxidation
CLC: O643.36
Type: PhD thesis
Year: 2010
Downloads: 610
Quote: 1
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Abstract


Functionalized ionic liquids for its excellent thermal stability, good solubility and anion and cation structures can be designed as a solvent and catalyst in the fine chemical and catalytic reaction shows an attractive prospect. For homogeneous catalysis in ionic liquid amount is large and the catalyst easily separated shortcomings, this paper mesoporous silicon-based materials with adjustable nanopores and high specific surface area, etc., the new functional ionic liquid structure is introduced mesoporous silicon-based materials pore or skeleton construct a special structure and function of the catalytic active center functionalized to prepare a series of novel ionic liquids hybrid mesoporous silicon-based material. Functionalized ionic liquids such hybrid mesoporous silicon material retains the homogeneous ionic liquids advantages of high catalytic activity, but also has a heterogeneous catalyst to facilitate separation and reusable features. After grafting using the acid chloride of iron through the imidazolium ionic liquid grafted onto MCM-41 mesoporous materials pore surface Lewis acid ionic liquids were prepared hybrid mesoporous silicon-based materials. Using XRD, N2 adsorption - desorption, FT-IR and TG-DTG were characterized by means of its structure was confirmed. The results show that, Lewis acidic ionic liquids have been successfully grafted on the pore surface material, and did not affect the carrier channel characteristics. In the Friedel-Crafts (Fu - g) alkylation reaction, the iron chloride supported acid ionic liquids exhibit relatively homogeneous acid chloride ionic liquid iron higher catalytic efficiency of iron chloride acid catalyst is only the amount of ionic liquids 1/50, and can be easily separated and reused 10 times more efficient. Moreover, the channels of MCM-41 with a direct load of FeCl3 catalyst, better reuse. Designed and synthesized bridge type structure containing ionic liquid silicone precursor it with TEOS (TEOS) of hydrolysis - condensation prepared skeleton structure containing ionic liquids embedded hybrid bridge bonds SBA-15 mesoporous materials, indium chloride anion exchange, prepared acid chloride ionic liquid indium structural units Mesoporous silicon-based materials. Using XRD, TEM, FT-IR, NMR, N2 adsorption - desorption characterization methods and their structures were confirmed. In the Friedel-Crafts alkylation reaction, the resulting catalyst exhibits excellent catalytic activity and can be easily separated and reused six times more efficient. Directly supported on pure silica mesoporous material within the pores InCl3 catalyst, this type of immobilized acid chloride ionic liquid indium in the process of re-use showed higher selectivity and a lower degree of wastage In. Furthermore, the catalyst is not sensitive to water, without strict control of the reaction carried out under anhydrous conditions, a strong industrial application value. Designed and synthesized with amine functionalized organosiloxane alkaline ionic liquid precursor by the sol - gel method or post-grafting method, preparation of three alkaline ionic liquids Hybrid Mesoporous silicon-based materials. With water as a medium in the Knoevenagel (g brain text Gale) reaction, the three materials showed a homogeneous ionic liquid catalyst than the corresponding higher catalytic activity. Which, after grafting material prepared by catalytic performance is better, especially after the grafting method using SBA-15 mesoporous material as a carrier catalyst prepared with high efficiency and effective repetition catalytic characteristics. In addition, amine functionalized mesoporous silicon hybrid materials, the basic ionic liquid Mesoporous silicon material with higher repetition performance. The ionic liquid grafted onto silicon SBA-15 type mesoporous materials pore surface, with hexamethyl disilazane residual silanols gas mask, and then with phosphotungstic acid anion exchange, phosphotungstic acid was prepared by ionic liquids Miscellaneous oriented silicon SBA-15 mesoporous materials. Imidazolium cation of the ionic liquid metal centers and weakly-coordinating ionic liquid polar intermediates are conducive to stable catalytic reaction, improves the catalytic activity and stability. In water as solvent, hydrogen peroxide (30%) as oxidant benzyl alcohol oxidation reaction, the catalyst showed over SBA-15 directly supported phosphotungstic acid catalysts better catalytic performance. Under optimum conditions, the conversion of benzyl alcohol and benzaldehyde selectivity of 97% and 96%. Since silanols are masked, phosphotungstic acid anion exchange mode only with ionic liquids unit and, accordingly, the catalyst showed better reusability in repeated use seven times, the catalytic activity was not significantly decreased.

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CLC: > Mathematical sciences and chemical > Chemistry > Physical Chemistry ( theoretical chemistry ),chemical physics > Chemical kinetics,catalysis > Catalytic > Catalyst
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