A method for preparing hierarchically porous zeolite in one step without secondary template
A technology of pore zeolite and sub-template, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., to achieve reduced synthesis cost, high acid site accessibility, and high acid site accessibility Effect
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Embodiment 1
[0019] According to SiO 2 :Al 2 o 3 :NaOH:TPA + :H 2 O = 1:0.025:0.153:0.105:22.322 molar ratio, weigh 5.01g tetrapropylammonium bromide, 0.46gγ-Al at room temperature 2 o 3 , Dissolve 1.1g of sodium hydroxide in 51mL of distilled water, stir and clarify, slowly add 21mL of silica sol with a mass fraction of 40% dropwise, mix well, transfer to a stainless steel reaction kettle with a volume of 100mL, and crystallize at 140°C for 5 days , the resulting solid product was washed with distilled water until neutral, filtered, dried, and then calcined in a muffle furnace at 550° C. with air for 5 hours to obtain a hierarchically porous ZSM-5 zeolite.
[0020] figure 1 The SEM images of the obtained ZSM-5 crystals show that the obtained ZSM-5 crystals present a core-shell structure, and the shell layer is formed by the interlaced growth of strip-shaped ZSM-5 zeolites. Pore and macroporous structure; TEM shows that there are obvious mesopore and macroporous structure between...
Embodiment 2
[0022] According to SiO 2 :Al 2 o 3 :NaOH:TPA + :H 2 The mol ratio of O=1.000: 0.033: 0.279: 0.210: 22.322, at room temperature 10.02g tetrapropylammonium bromide, 0.86g pseudo-boehmite (70%Al 2 o 3 , 30%H 2O), 2g of sodium hydroxide were dispersed in 41mL of distilled water, after stirring and clarification, 31mL of silica sol with a mass fraction of 30% was slowly added dropwise. The resulting solid product was washed with distilled water to neutrality, filtered, dried, and then calcined in a muffle furnace at 550° C. for 5 hours with air to obtain a hierarchically porous ZSM-5 zeolite.
[0023] SEM showed that the interior of the spherical ZSM-5 zeolite crystal was formed by the accumulation of nanocrystals, and there were obvious mesopores and macropores; figure 2 The TEM shows that the crystal lattice orientation of the nanocrystals is inconsistent, and obvious mesopore and macropore structure can be observed between the grains; N 2 The adsorption-desorption resu...
Embodiment 3
[0025] According to SiO 2 :Al 2 o 3 :NaOH:TPA + :H 2 O = 1.000: 0.025: 0.204: 0.084: 19.222 molar ratio, 4.65g tetrapropylammonium bromide, 0.81g aluminum hydroxide, 1.7g sodium hydroxide were dissolved in 48mL distilled water at room temperature, stirred and clarified, slowly dripped Add 24mL of silica sol with a mass fraction of 40%, mix well, transfer to a stainless steel reaction kettle with a volume of 100mL, crystallize at 170°C for 2 days, wash the obtained solid product with distilled water until neutral, filter, dry, and then The multi-level porous ZSM-5 zeolite was obtained by calcining in a muffle furnace at 550°C for 5 hours with air flowing through it.
[0026] SEM showed that the spherical ZSM-5 zeolite crystal was formed by the accumulation of nano-grains, and there were obvious mesopores and macropores; TEM showed that there were obvious mesoporous structures between the nano-grains; image 3 N 2 In the adsorption-desorption curve, the as-prepared ZSM-5 z...
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