Method for preparing zeolite molecular sieve catalyst through circulating gas phase method
A zeolite molecular sieve and circulating gas technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of difficulty in regulating the relative humidity of water vapor, unfavorable industrialization, silica-alumina dry glue and template agent or water vapor problems such as poor mass transfer effect, to achieve the effect of shortening synthesis time, conducive to industrial production, reducing environmental pollution and production costs
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Embodiment 1
[0050] Fully mix 50 grams of silica gel, 3.7 grams of SB powder and 4.3 grams of sodium hydroxide, and the material ratio (molar ratio) of the reactants is: SiO 2 :Al 2 o 3 :OH - =30:1:3.9, after fully mixing, add 5 grams of nitric acid, 3.3 grams of pore-enlarging agent PEG-20000 and 70 grams of deionized water to the mixture to obtain silica-alumina dry glue, and then extrude the silica-alumina dry glue into strips, Dry at 60°C to obtain cylindrical particles. Take 12 grams of formed cylindrical particles, put them into the partition plate in the autoclave in 3 layers, the height of each layer is about 0.03 meters, there are 40 grams of HMI and 160 grams of deionized water in the liquid storage tank, and the preheating temperature is 80 ℃, the temperature of the high-pressure reactor is 150 ℃, the pressure is 0.36MPa, and the organic template agent steam and water vapor are circulated by a double plunger pump, and the space velocity is 0.5h -1 , in situ crystallization f...
Embodiment 2
[0052] Get 12 grams of formed cylindrical granules in Example 1, put them on the dividing plate in the autoclave in 3 layers, each layer has a height of about 0.03 meters, and the residual liquid in Example 1 is in the liquid storage tank, preheating The temperature is 80°C, the temperature of the autoclave is 150°C, and the pressure is 0.36MPa. The steam of the organic template agent and the water vapor are circulated by a double plunger pump, and the space velocity is 0.5h -1 , in situ crystallization for 6 days. Take it out, wash it, filter it, dry it at 90°C, exchange it with ammonium, and roast it at 540°C for 6 hours to get the product. The obtained zeolite molecular sieve catalyst was determined by XRD to be an MCM-22 zeolite molecular sieve catalyst with a crystallinity of 94.6% (compared with the crystallinity in Example 1).
Embodiment 3
[0054] 50 grams of white carbon black, 18.3 grams of aluminum sulfate, 3.3 grams of sodium hydroxide and 152 grams of mass fraction 35% tetraethylammonium hydroxide are fully mixed, and the material ratio (molar ratio) of the reactant is: SiO 2 :Al 2 o 3 :OH - :TEAOH=30:1:3:13, evaporate water at 60°C to obtain silica-alumina dry glue. Take 12 grams of powdery silica-alumina dry glue, put it into the partition plate in the high-pressure reactor in 3 layers, the height of each layer is about 0.03 meters, there is 120 grams of deionized water in the liquid storage tank, and the preheating temperature is 80 ° C. The temperature of the high-pressure reactor is 140°C, the pressure is 0.26MPa (at this time, the water vapor is in a saturated state), and the double plunger pump is used to circulate the water vapor, and the space velocity is 0.5h -1 , in situ crystallization for 24h. Take it out, wash it, filter it, dry it at 90°C, exchange it with ammonium, and roast it at 540°C f...
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