A kind of preparation method of hβ/mcm-22 compound structure molecular sieve and the method for preparing tert-butylphenol
A technology of MCM-22 and composite structure, which is applied in the preparation of organic compounds, molecular sieve catalysts, catalyst activation/preparation, etc., can solve the problems of large size of composite molecular sieves, discounting of catalytic effects and shape-selective effects, and influence on synergistic catalytic effects, etc. Achieve the effect of improving raw material utilization efficiency, enhancing synergistic catalytic effect, and good selectivity
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Embodiment 1
[0031] 20g of Hβ molecular sieves were added to 200ml of polydiallyldimethylammonium chloride solution with mass fractions of 0.01wt%, 0.11wt% and 1wt%, respectively, at 80 °C, treated in a water bath for 1 h, and then ultrasonicated. , 100ml of 1wt% ammonium nitrate was subjected to ammonium exchange, filtration, and drying at 80°C for 8h to obtain three pretreated Hβ molecular sieves. Under the condition of constant stirring, 54g of water and 0.72g of sodium hydroxide were added to the beaker and stirred for 30mins, and then 0.337g was added. 18.3g of silica sol was added and stirred for 2h. Finally, 3.5g of HMI was added and stirred for 3h, and then the gel was transferred to the reaction kettle and obtained by crystallization at a low temperature of 130°C for 6 hours. Then, 2g of pretreated three kinds of Hβ molecular sieves were added to 20ml of MCM-22 low-temperature synthesis mother liquor respectively, transferred to a static reactor and crystallized at 170°C for 24h. A...
Embodiment 2
[0034] 20g Hβ molecular sieve was added to 200ml of 1% polydiallyldimethylammonium chloride solution, cetyltrimethylammonium bromide solution and ammonia water respectively, and treated in a water bath at 80°C. 1h, then ammonium exchange, filtration, and drying at 80°C for 8h were carried out by ultrasound, 100ml of 1% ammonium nitrate to obtain three pretreated Hβ molecular sieves, and then 2 g of the pretreated three kinds of Hβ molecular sieves were added to 20ml of MCM-22 low-temperature synthesis mother liquor ( The preparations were the same as those in Example 1) except that it was crystallized at 80° C. for 10 hours. It was transferred to a static reactor and crystallized at 170° C. for 24 hours. After the crystallization was completed, it was rapidly cooled to room temperature. The samples were filtered, washed, dried at 80°C for 6h, and calcined at 550°C for 6h to obtain Hβ / MCM-22 composite molecular sieves A4, A5, and A6.
[0035] To evaluate the above catalyst, in ...
Embodiment 3
[0037] 20g Hβ molecular sieves were added to 200ml 1% polydiallyl dimethyl ammonium chloride solution, treated in a water bath for 1h at 80°C, and then ammonium exchanged by ultrasonic and 100ml 1% ammonium nitrate. , filtered, and dried at 80°C for 8h to obtain pretreated Hβ molecular sieve, and then pretreated 2g Hβ molecular sieve was added to 20ml of MCM-22 low-temperature synthesis mother liquor (except for crystallization at 150°C for 4h, the rest of the preparations were the same as in Example 1). It was crystallized at 170°C for 24 hours in a static reaction kettle. After the crystallization was completed, it was rapidly cooled to room temperature. The sample was filtered, washed, dried at 80°C for 6h, and calcined at 550°C for 6h to obtain Hβ / MCM-22 composite molecular sieve A7.
[0038] To evaluate the above catalyst, in a 1L reactor, add 240g, 300g of phenol and 10g of the Hβ / MCM-22 composite molecular sieve prepared in the first step, stir, and add 178g of isobutyl...
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