Preparation method of beta molecular sieve
A beta molecular sieve and crystal seed technology, applied in the field of catalytic chemistry, can solve the problems of low product yield, high system water content, large amount of template agent, etc., achieve high thermal efficiency, improve yield and crystallinity, and shorten synthesis time. Effect
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[0043] The present invention provides a kind of preparation method of β molecular sieve, and this preparation method comprises:
[0044] (1) Synthesis of initial gel: mix silicon source, aluminum source, template agent, alkaline metal source, water, and β molecular sieve seed crystals, stir evenly, and synthesize initial gel; silicon source is SiO 2 In terms of aluminum source as Al 2 o 3 In terms of templating agent TEA + In terms of alkaline metal sources as Na 2 In terms of O, the molar ratio of raw materials for synthesizing the initial gel is: SiO 2 / Al 2 o 3 =25~150, TEA + / SiO 2 =0.07~0.23, Na 2 O / SiO 2 =0.03~0.12,H 2 O / SiO 2 =3.0~11.5, preferably: SiO 2 / Al 2 o 3 =30~120:1, TEA + / SiO 2 =0.07~0.15:1, Na 2 O / SiO 2 =0.05~0.12:1, H 2 O / SiO 2 =3.0~7.5:1; β molecular sieve seed crystal silicon aluminum ratio SiO 2 / Al 2 o 3 =20~100, the amount added is SiO in the silicon source by mass 2 0.5% to 10% of the mass, mixed evenly to get the initial gel; ...
Embodiment 1
[0064] Add 11.00 g of deionized water and 13.00 g of tetraethylammonium hydroxide solution into a container in a water bath at 70° C., and stir evenly. Add 0.31g sodium hydroxide, add 1.85g sodium metaaluminate, stir to dissolve. Add 15.00g of coarse-porous silica gel and stir evenly. Add 0.30 g of β molecular sieve seed crystals and stir evenly to obtain an initial gel. Microwave heating crystallization reaction was carried out on the initial gel, and the temperature was controlled at 160°C for 15 hours. After the reaction is finished, the product is washed and dried, and characterized by X-ray diffraction. The crystallinity of the product is shown in Table 1. SEM and BET analysis were carried out, and the results are shown in Table 2.
Embodiment 2
[0066] Add 11.00 g of deionized water and 13.00 g of tetraethylammonium hydroxide solution into a container in a water bath at 70° C., and stir evenly. Add 0.31g sodium hydroxide, add 1.85g sodium metaaluminate, stir to dissolve. Add 15.00g of coarse-porous silica gel and stir evenly. Add 0.30 g of β molecular sieve seed crystals and stir evenly to obtain an initial gel. Microwave heating crystallization reaction was carried out on the initial gel, and the temperature was controlled at 120°C for 25h. After the reaction is finished, the product is washed and dried, and characterized by X-ray diffraction. The crystallinity of the product is shown in Table 1.
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