A zirconium-containing beta zeolite and its preparation method
A beta zeolite and zeolite technology are applied in the field of modified beta zeolite and its preparation, which can solve the problem of low cracking activity and achieve the effects of high pore volume, high specific surface area, and improved hydrocarbon cracking capacity
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Embodiment 1
[0025] Take 200g sodium type β zeolite (produced by Sinopec Catalyst Qilu Branch, SiO 2 / Al 2 o 3 =25 (molar ratio), dry basis accounted for 75% by weight), mixed with 3000g deionized water and 45g ammonium chloride for beating, stirred at 80°C for 2 hours, then filtered, and repeated the above process 3 times to make the Na in the zeolite 2 The O content is less than 0.2% by weight, roasted at 600°C and 100% steam for 2 hours to obtain ammonium-exchanged zeolite beta, denoted as A-1;
[0026] 52.3g zirconium nitrate Zr (NO 3 ) 4 ·5H 2 O was dissolved in 150g ethanol (analytically pure) to obtain an impregnation solution, and then the above impregnation solution was mixed with ammonium-exchanged β zeolite A-1 evenly, left to stand for 24 hours, dried at 100°C for 24 hours, and then dried in a nitrogen atmosphere at 500°C Lower roasting for 4 hours, denoted as AC-1;
[0027] Add the above roasted β zeolite AC-1 into 2000g of inorganic acid aqueous solution (dilute hydroch...
Embodiment 2
[0030] Take 200g of sodium-type β zeolite (same as above), mix it with 2000g of deionized water and 45g of ammonium chloride, stir at 80°C for 1 hour, then filter, repeat the above process 3 times, and roast at 650°C and 100% steam for 2 Hours, the β zeolite A-2 after ammonium exchange was obtained; Na in zeolite A-2 2 The O content is less than 0.2% by weight, and the water content is 1% by weight;
[0031] Dissolve 18.9g of zirconium isopropoxide in 450g of ethanol, then mix the resulting solution with ammonium-exchanged zeolite A-2 evenly, stir for 24 hours, dry at 100°C for 24 hours, and bake at 550°C in a nitrogen atmosphere for 3 Hour, obtain the beta zeolite AC-2 after roasting;
[0032] Add the above-mentioned roasted β zeolite AC-2 into 1500 g of oxalic acid aqueous solution with an acid concentration of 2.0 mol / L, continue to stir at 90° C. for 1 hour, then filter and wash with deionized water (the amount of washing water is the dry weight of molecular sieve 15 tim...
Embodiment 3
[0035] Take 200g of sodium-type β zeolite (same as above), mix it with 2000g of deionized water and 60g of ammonium chloride for slurry, stir at 90°C for 3 hours, then filter, repeat the above process twice, and Na on the zeolite 2 O content is less than 0.2% by weight, roasted at 500°C for 5 hours to obtain ammonium-exchanged β zeolite A-3;
[0036] 10.5g zirconium nitrate Zr(NO 3 ) 4 ·5H 2 O was dissolved in 200g of ethanol, and then the above solution was mixed evenly with the ammonium-exchanged β zeolite, and dried after standing for 12 hours; the dried zeolite was composed of 25.6g of tetrabutyl titanate and 200g of ethanol Mix the impregnating solution, let it stand for 12 hours, then dry it at 100°C for 24 hours, and roast it under nitrogen atmosphere at 600°C for 2 hours to obtain the roasted zeolite beta, which is denoted as AC-3;
[0037] Add the roasted beta zeolite AC-3 to 1000 g of hydrochloric acid aqueous solution with an acid concentration of 0.5 mol / L, stir...
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