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Synthesis, Characterization And Application Of The Mesoporous Molecular Sieve Contain Phosphorus

Posted on:2013-10-20Degree:MasterType:Thesis
Country:ChinaCandidate:M M LiFull Text:PDF
GTID:2231330374996622Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
Mesoporous molecular sieve aluminum phosphate was synthesized usingcetyltrimethylammonium bromide (CTAB) as a structure-directing agent and aluminumhydroxide, aluminum, isopropoxide phosphoric acid (85%), as aluminum, phosphorus,sources,under the condition of acidity, basicity and the method of oriented agent. Andmodified by LaCl3. The composition, structure and surface physical and chemical propertiesof the samples were characterized by X-ray EDS analysis, inductively coupled plasma massspectrometry (ICP-MS), elemental analyzer, fourier transform infrared spectroscopy (FTIR),N2adsorption-desorption, NH3chemisorption (NH3-TPD), small-angle X-ray diffraction(XRD), scanning electronic microscope (SEM), transmission electron microscopy (TEM),thermogravimetric analysis (TG), pyridine adsorption (FTIR) and so on.Synthesis method of hydrothermal: the typical worm-like layer structure of AlPO4mesoporous molecular sieve was synthesized under the condition of basicity, TPD acid was0.1642mmol/g, surface area was308.5m2/g, pore volume was0.1336mL/g, and pore size4.761nm; The worm-like layer structure of AlPO4mesoporous molecular sieve wassynthesized under the condition of acidic, TPD acid was0.3498mmol/g, surface area was309.4m2/g, pore volume0.2572mL/g, and pore size3.325nm.AlPO4mesoporous molecular sieve was synthesized by the method of oriented agent TPDacid was0.0395mmol/g, surface area was235.3m2/g, pore volume0.4202mL/g, and pore size4.221nm.The La-AlPO4mesoporous molecular sieve was synthesized by the method of orientedagent, the Structure was not changed, TPD acid was0.1184mmol/g, surface area was212.3m2/g, pore volume0.2401mL/g, and pore size4.535nm.The results of ICP and elementalanalysis showed that the yield were15.7%and1.81%of Al and La for La-AlPO4.Alsoshowed that La has been join the AlPO4skeleton structure. Experimental results show that,the BET surface area was lower, but acid amount and acid strength were enhanced of LaAPO4compare to AlPO4.Catalytic character of AlPO4and LaAPO4were evaluated using reaction of synthesis acetylsalicylic acid. The results showed that both of AlPO4and La-APO4molecular sieve had highcatalytic activity in synthesis of acetyl salicylic acid: under alkaline conditions transformation rate of salicylic acid was64%, under acidic conditions transformation rate of salicylic acidwas69%, transformation rate of salicylic acid was53%of AlPO4was synthesized by orientedagent method, transformation rate of salicylic acid was80%of La-APO4.
Keywords/Search Tags:AlPO4, La-AlPO4, Catalysis, Aspinin
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