Double-level hole distribution ZSM-35 molecular sieve, preparation method thereof and application of molecular sieve
A ZSM-35, dual-stage pore technology, applied in the direction of iron-conglomerate crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of high cost and complicated process, and achieve high repeatability and synthetic method Simple, Controllable Effects
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[0039] The preparation method of the two-stage pore distribution ZSM-35 molecular sieve involved in the second aspect of the present invention comprises:
[0040] In step A, the colloidal mixture solution obtained by mixing the silicon source, the aluminum source, the alkali source, the template agent and water uniformly in the reactor is crystallized to obtain the ZSM-35 molecular sieve crystallization mother liquor; at the same time, a template agent containing mixed composition;
[0041] Step B, after the crystallization is completed, cool down from the crystallization temperature to the pressure relief temperature, open the vent port of the reaction kettle for pressure relief, and obtain the ZSM-35 molecular sieve crystallization mother liquor after the pressure relief; at the same time, the template agent in the gas phase and water vapor for liquefaction and recovery;
[0042] Step C: filter, wash, and dry the ZSM-35 molecular sieve crystallization mother liquor after de...
Embodiment 1
[0071] Example 1: Preparation of ZSM-35 molecular sieve with cyclohexylamine as template
[0072] (1) First, 50 grams of aluminum sulfate (analytical pure, content greater than 99.5%) was added to 785.7 ml of deionized water under stirring at room temperature, and stirred for 40 minutes. After the aluminum sulfate is completely dissolved, slowly add 720 grams of silica sol (SiO 2 content is 25% silica sol), stirred for 1 hour, then slowly added 72 grams of sodium hydroxide, stirred for 1 hour, added 148 g of cyclohexylamine as a templating agent and stirred evenly to obtain a colloidal mixture solution. The colloidal mixture solution has the following molar composition: OH - :Al 2 o 3 :SiO2 2 :R:H 2 O=0.6:0.025:1:0.5:25. Transfer the colloidal mixture solution into an autoclave and crystallize at 200°C under autogenous pressure for 15 hours. After the crystallization is complete, the ZSM-35 molecular sieve crystallization mother liquor is obtained. At the same time, a mi...
Embodiment 2
[0079] Present embodiment step (1) and (3) are identical with embodiment 1, difference is step (2):
[0080]Lower the temperature through the cooling coil, drop the temperature from 200°C (crystallization temperature) to 170°C (pressure relief temperature) by 30°C, perform pressure relief operation until the pressure (gauge pressure) in the kettle is zero, and obtain ZSM-35 molecular sieve crystals after pressure relief The initial pressure of depressurization is 0.8Mpa, the cooling rate is controlled at 0.7°C / min, and the depressurization time is controlled for 5h; the gas phase part in the reaction system is a mixture of cyclohexylamine and water vapor, and the heat is recovered through the heat exchanger Finally, it is introduced into the condenser through the pipeline to condense, and is directly recovered to the liquid storage tank.
[0081] The obtained ZSM-35 molecular sieve powder is subjected to X-ray powder diffraction phase analysis (XRD), and the results (not shown...
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