Molecular sieve catalyst and preparation method thereof
A catalyst and molecular sieve technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as insufficient deamination, insufficient ion exchange, and limitation of ion exchange types to achieve high activity and high The effect of ethylbenzene selectivity
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[0026] The present invention also provides a preparation method of the above molecular sieve catalyst, which includes the following steps:
[0027] (1) The β molecular sieve containing template agent obtained by conventional synthesis is exchanged with ammonium to make the Na 2 The content of O is less than 0.3 wt%.
[0028] (2) Stir and mix the ammonium type β molecular sieve and the copper-containing compound aqueous solution or gel at room temperature. After drying at room temperature to 120°C, heat to 200-450°C in an air atmosphere and calcinate for 2-8 hours to obtain copper-containing β molecular sieve Or the ammonium type β molecular sieve and the copper-containing compound aqueous solution or gel are stirred and mixed at room temperature, after drying at room temperature to 120 ℃, heated to 200 ~ 450 ℃ in an air atmosphere for 2 ~ 8 hours, the calcined sample is added after cooling The ammonium salt aqueous solution with a concentration of 2 to 5 wt% is stirred to exchange ...
Embodiment 1
[0045] Take Naβ zeolite and add 10% (weight) ammonium nitrate solution, liquid / solid = 4:1, ion exchange for 2 hours under the condition of stirring in a water bath at 90°C, filter and wash, dry at 110°C, repeat exchange to obtain a template containing organic amine NH 4 β molecular sieve, so that the Na 2 The content of O is less than 0.3 wt%.
[0046] Weigh 0.61 g of copper chloride dihydrate, add 500 g of water to form a copper chloride aqueous solution, and add 0.48 g of 25% concentrated ammonia water dropwise to prepare a copper hydroxide gel. Weigh 20g of NH 4 The β molecular sieve was stirred and mixed with it at room temperature, filtered, washed, and the filter cake was dried and placed in a muffle furnace. In an air atmosphere, the temperature was raised from room temperature to 400°C, and the mixture was calcined at 400°C for 4 hours to obtain sample S1.
[0047] Sample S1 was analyzed by X-ray fluorescence method, and the copper content was 2.06% by weight based on CuO....
Embodiment 2
[0050] Weigh 2.43 g of copper chloride dihydrate, add 500 g of water to form a copper chloride aqueous solution, and add 1.94 g of 25% concentrated ammonia water dropwise to prepare a copper hydroxide gel. Add 20g of NH obtained by treatment in Example 1 4 The β molecular sieve was stirred and mixed at room temperature, filtered, washed, and the filter cake was dried and placed in a muffle furnace. In an air atmosphere, the temperature was raised to 350°C, and the mixture was roasted at 350°C for 4 hours to obtain sample S2a.
[0051] The calcined sample S2a was pulverized into powder in quartz milling, 100 mL of ammonium acetate aqueous solution with a mass fraction of 10% was added, and the pH was adjusted to about 7.0 with ammonia water. Stir at room temperature for 120-180 minutes, filter, wash, and dry to obtain the final sample S2.
[0052] Sample S2 was analyzed by X-ray fluorescence method, and the copper content was 1.14wt% calculated as CuO.
[0053] The X-ray photoelectro...
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