Preparation method of zeolite molecular sieve material having three-dimensional penetrating mesoporous multistage tunnel structure
A zeolite molecular sieve and three-dimensional penetrating technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve problems such as uncontrollable, weak interaction between template and precursor, and difficult separation. Achieve the effect of reducing crystallization temperature and time, easy large-scale promotion and application, and solving environmental pollution problems
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[0026] The preparation method of the present invention comprises the following steps:
[0027] (1) Weigh an appropriate amount of aluminum source and mix it with a certain amount of silicon source evenly, add an appropriate amount of water, and stir in a water bath at 5-50°C (for example, 40°C) for 0.5-2 hours to make a preliminary formation of silicon source and aluminum source. the hydrolysis process;
[0028] (2) Weigh the structure-directing agent, and slowly add it dropwise to the mixed solution obtained in step (1) under stirring in a water bath at 5-50°C (for example, 40°C), so that the silicon source and the aluminum source are further hydrolyzed and polymerized;
[0029] (3) Under the conditions of step (2), continue stirring until the precursor gel of zeolite is formed, and continue static aging at a certain temperature for a certain period of time;
[0030] (4) performing crystallization treatment on the zeolite precursor xerogel obtained in (3) under steam conditi...
Embodiment 1
[0044] a) Preparation of zeolite precursor solution: Mix 0.2042g of aluminum isopropoxide and 10.4165g of ethyl orthosilicate uniformly at room temperature for 2h, then add 18g of deionized water, stir in a water bath at 40°C for 2h, then 4.1g of 25wt % tetrapropylammonium hydroxide aqueous solution was added dropwise to the above solution and continued to stir;
[0045] b) Stir the solution in a) in a water bath at 50°C until it forms a gel state, then transfer the precursor gel to an oven at 5°C for aging for a long enough time and grind it into a powder state;
[0046] c) Divide the powder sample in b) into three parts and place them in 80ml hydrothermal kettles for crystallization treatment. Before crystallization, add 0.7g of deionized water to the bottom of each lining, and put them in an oven at 150°C. Steam assisted crystallization treatment for 10h;
[0047] d) Take out the crystallized sample, dry it in an oven at 100°C for 4h, and finally calcinate it in an air atm...
Embodiment 2
[0052] The difference between this embodiment and the first embodiment is that the crystallization temperature used in the steam-assisted crystallization process is 180° C., and the crystallization time is 4 hours. The rest of the content is the same as that described in Example 1.
[0053] Figure 4 A is the nitrogen adsorption-desorption isotherm and pore size distribution diagram of the hierarchical porous structure zeolite molecular sieve material prepared in Example 2. As can be seen from the figure, the nitrogen adsorption-desorption isotherm is also a typical IV type isotherm and H1 type hysteresis loop, at 0.60 <0.9, there is an obvious breakthrough in adsorption, and the pore size distribution also shows that the material has mesopores of about 10nm to 25nm.
[0054] Figure 5 A is the SEM photo of the hierarchically porous zeolite molecular sieve material prepared in Example 2. The material is also a spherical particle, and an obvious mesoporous channel structure c...
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