A kind of preparation method of hierarchical porous zsm-5 nano-aggregate
A technology of ZSM-5 and agglomerates, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of increased energy consumption, large zeolite size, and poor uniformity. Achieve the effects of reducing production energy consumption, reducing the generation of miscellaneous crystals, and accelerating the growth rate
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Embodiment 1
[0030] (1) Preparation of MFI nanostructure microcrystalline liquid
[0031] Mole ratio TPAOH:TEOS:H 2 O: EtOH=7.5:28:360:1000, 24.7mlTPAOH, 4mlH 2 O, 23.6ml EtOH and 25.8ml TEOS were mixed uniformly at room temperature; then loaded into a polytetrafluoroethylene-lined kettle, statically crystallized in an oven at 80°C for 3 days, cooled to room temperature, and MFI microcrystalline liquid with a size of no more than 80nm was obtained.
[0032] (2) Preparation of hierarchically porous ZSM-5 aggregates in a template-free system
[0033] According to the molar ratio of alkali source, silicon source, aluminum source, potassium dihydrogen phosphate and water 9.5:100:2.86:10.8:2126, 0.43g sodium metaaluminate, 0.47g sodium hydroxide, 1.34g potassium dihydrogen phosphate, Added into 24.3ml of deionized water, mechanically stirred at room temperature for 30min to a clear state; then added 15.4ml of silica sol, stirred at room temperature for 30min, added 0.5wt% microcrystalline liq...
Embodiment 2
[0035] (1) The preparation method of the MFI nanostructure microcrystalline liquid is the same as that in Example 1.
[0036](2) According to the molar ratio of alkali source, silicon source, aluminum source, potassium dihydrogen phosphate and water 9.5:100:2.86:21.6:2126, 0.43g sodium metaaluminate, 0.47g sodium hydroxide, 2.68g diphosphate Potassium hydrogen was added to 24.3ml of deionized water, stirred mechanically at room temperature for 30min to a clear state; then added 15.4ml of silica sol, stirred at room temperature for 30min, then added 0.5% wt of the seed liquid synthesized in step (1), and aged for 1h to Gel state; put into polytetrafluoroethylene-lined kettle; static crystallization at 60°C for 4 hours, then static crystallization at 170°C for 8 hours; cool to room temperature, centrifuge, wash until neutral; then dry in an oven at 100°C After 6h, hierarchical porous ZSM-5 nanoaggregates were obtained. The yield of the synthesized sample is 94.4%; the aggregate...
Embodiment 3
[0038] (1) Preparation of MFI nanostructure microcrystalline liquid
[0039] Mole ratio TPAOH:TEOS:H 2 O: EtOH=7.5:28:360:1000, 24.7mlTPAOH, 4mlH 2 O, 23.6ml of EtOH and 25.8ml of TEOS were mixed uniformly at room temperature; then loaded into a polytetrafluoroethylene-lined kettle, statically crystallized in an oven at 60°C for 5 days, cooled to room temperature, and MFI microcrystalline liquid with a size of no more than 80nm was obtained.
[0040] (2) According to the molar ratio of alkali source, silicon source, aluminum source, potassium dihydrogen phosphate and water 12:100:2.5:32.4:1063, 0.38g sodium metaaluminate, 0.59g sodium hydroxide, 4.02g diphosphate Potassium hydrogen was added to 12.1ml of deionized water, stirred mechanically at room temperature for 30min to a clear state; then added 15.4ml of silica sol, stirred at room temperature for 30min, then added 0.5wt% of the seed liquid synthesized in step (1), and aged for 1h to Gel state; put into a polytetrafluor...
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