A kind of synthetic method of large particle size beta molecular sieve
A synthesis method and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve problems such as restricting the industrial production and large-scale application of Beta molecular sieves, increasing the burden of industrial production on the economy and the environment, and difficulties in the solid-liquid separation of molecular sieve slurries. Excellent hydrothermal stability, improved gel reaction rate, and improved industrial production efficiency
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Embodiment 1
[0040] A kind of synthetic method of large particle diameter Beta molecular sieve, comprises the following steps:
[0041] (1) Gel preparation: Add 1767.6 g of 25wt% tetraethylammonium hydroxide (template agent R) aqueous solution and 600g of 40wt% sodium hydroxide aqueous solution into the container, and stir in a water bath at 30°C for 20 minutes. Add 2571.4g alkaline silica sol (35wt% SiO 2 content), stirred for 40 min. Then add 399.4g of aluminum sulfate octadecahydrate and 2042.8g of water to prepare a mixed solution, keep stirring at 25°C for 4 hours to obtain a gel;
[0042] (2) Crystallization: heat the gel up to 165°C at a heating rate of 25°C / h and keep it warm for 84 hours. Stir at a constant speed of 100r / min while heating up. After the crystallization is completed, suction filter and wash with deionized water. Washing to pH = 7.0, drying at 70°C;
[0043] (3) Ammonium exchange and activation: The dried sample was roasted at 10 °C / min at 550 °C for 6 h; after co...
Embodiment 2
[0046] A kind of synthetic method of large particle diameter Beta molecular sieve, comprises the following steps:
[0047] (1) Gel preparation: Add 3314.3g of 20wt% tetraethylammonium hydroxide (template agent R) aqueous solution and 400g of 30wt% sodium hydroxide aqueous solution into the container, and stir in a water bath at 30°C for 15 minutes. Add 3000g of alkaline silica sol (30wt% SiO2 content), and stir for 35 min. Then add 599.8g aluminum sulfate octadecahydrate and 1428.6g water to prepare the original solution, keep stirring at 30°C for 3 h. Add 1.35g of dimethyl carbonate (accelerator), continue to stir for 1 hour, and use a ball mill to grind for 10 minutes to obtain a gel;
[0048] (2) Pre-crystallization: transfer the gel to a hydrothermal reaction kettle, evacuate with a circulating water vacuum pump until the pressure in the kettle is -0.092 MPa, stir the gel at a stirring speed of 100 r / min for 24 hours, and Under high pressure conditions, the temperature w...
Embodiment 3
[0053] A kind of synthetic method of large particle diameter Beta molecular sieve, comprises the following steps:
[0054] (1) Gel preparation: Add 450.2g of 35wt% tetraethylammonium bromide (template agent R) aqueous solution and 800g of 45wt% sodium hydroxide aqueous solution into the container, and stir in a water bath at 15°C for 30min. Add 2250g alkaline silica sol (40wt% SiO 2 content), stirred for 60 min. Then add the original solution prepared by 80g aluminum chloride and 1967.2g water, keep stirring at 15°C for 6 h. Add 88.5g of diethyl carbonate (accelerator), continue stirring for 2 hours, and grind for 30 minutes with a ball mill to obtain a gel;
[0055] (2) Pre-crystallization: transfer the gel to a hydrothermal reaction kettle, evacuate with a circulating water vacuum pump until the pressure inside the kettle is -0.090MPa, stir the gel at a stirring speed of 300 r / min for 6 hours, and then Raise the temperature to 90°C at a heating rate of 10°C / h, and keep it...
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