Ordered mesoporous zirconium sulfate-aluminum composite oxide solid acid material and its preparation and application
A composite technology of solid acid and aluminum, which can be used in biofuels, fatty acid esterification, chemical instruments and methods, etc., and can solve problems such as small pore size, inactivation, and limitation
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Embodiment 1
[0050] Under vigorous stirring at 30°C, mix 0.25g deionized water, 0.32g citric acid, 3.5g EO 106 PO 70 EO 106 , 1.65g of aluminum isopropoxide and 1.44g of zirconium oxychloride were successively added to 25mL of absolute ethanol, stirred for 5h to make it completely dissolved, and a clear solution was obtained.
[0051] The resulting clear solution was poured into a sealed autoclave and heated to 80°C for solvothermal pretreatment for 12h.
[0052] The solution obtained by solvothermal pretreatment was placed in an open state, firstly subjected to volatilization treatment at 60 °C for 12 h, and then heated to 120 °C for thermal polymerization treatment for 24 h.
[0053] The obtained solid was heated to 550 °C for 5 h at a heating rate of 2 °C / min in an air atmosphere, and the organic template in the mesoporous channels was removed to prepare an ordered mesoporous zirconium-aluminum composite oxide.
[0054] According to the solid / liquid volume ratio of 1:10, the obtained...
Embodiment 2
[0070] Under vigorous stirring at 35°C, mix 0.35g deionized water, 1.6g concentrated hydrochloric acid (36.5wt.%), 0.50g glacial acetic acid, 3.0g EO 30 PO 70 EO 30 , 1.325g aluminum tert-butoxide and 3.49g zirconium isopropoxide were successively added to 35mL absolute ethanol, stirred for 2h to make it completely dissolved, and a clear solution was obtained.
[0071] The resulting clear solution was poured into a sealed autoclave and heated to 100°C for solvothermal pretreatment for 6h.
[0072] The solution obtained by solvothermal pretreatment was placed in an open state, firstly subjected to volatilization treatment at 70 °C for 12 h, and then heated to 100 °C for thermal polymerization treatment for 24 h.
[0073] The obtained solid was heated to 550 °C for 5 h at a heating rate of 2 °C / min in an air atmosphere, and the organic template in the mesoporous channels was removed to prepare an ordered mesoporous zirconium-aluminum composite oxide.
[0074] According to the s...
Embodiment 3
[0081] Under vigorous stirring at 30°C, 0.53g deionized water, 1.0g concentrated nitric acid (65wt.%), 0.60g tartaric acid, 3.5g EO 34 BO 11 EO 34 , 1.97g of aluminum isobutoxide and 3.43g of zirconium nitrate were successively added to 50mL of absolute ethanol, stirred for 2h to completely dissolve, and a clear solution was obtained.
[0082] The resulting clear solution was poured into a sealed autoclave and heated to 80°C for solvothermal pretreatment for 8h.
[0083] The solution obtained by solvothermal pretreatment was placed in an open state, and the solvent was volatilized at 80°C for 12 hours, and then heated to 100°C for thermal polymerization for 24 hours.
[0084] The obtained solid was heated to 550 °C for 5 h at a heating rate of 2 °C / min in an air atmosphere, and the organic template in the mesoporous channels was removed to prepare an ordered mesoporous zirconium-aluminum composite oxide.
[0085] According to the solid / liquid volume ratio of 1:20, the obtai...
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