METHOD FOR PRODUCING MICROPOROUS THREE-PHASE COMPOSITE Russian patent published in 2023 - IPC C01B39/42 C01B39/04 B01J29/40 

FIELD: zeolites based on composites.

SUBSTANCE: invention relates to the field of obtaining zeolites based on composites, namely, to a method for obtaining a microporous three-phase composite ZSM-5/ZSM-11/ZSM-12, for the first time using a quaternary ammonium salt as a template - monoethanol-N,N,N-trimethylammonium chloride. A method for producing a microporous three-phase composite is proposed, characterized in that: an aqueous solution with pH = 8.5-9.5 is mixed, containing an aluminum compound and a template - monoethanol-N,N,N-trimethylammonium chloride, which is adjusted with dry alkali or an aqueous solution of alkali to pH = 11.5-13.5, and an aqueous solution containing a silicon compound, which is used as a solution of colloidal silicon dioxide or tetraethoxysilane, until a gel-like mass is obtained, while the mixture of solutions is prepared based on the following molar ratios of the components used: template/ SiO₂ = 0.06-0.15, SiO₂/Al₂O₃ = 100-600, H₂O/SiO₂ = 4-16; crystallization of the resulting gel-like mass is carried out for 5-6 days at a temperature of 145-155°C, followed by separation of the crystalline product, washing it with distilled water until the pH of the filtrate reaches 9.0-9.5, drying to constant weight and annealing the resulting powder at 550±10°C for 8-12 hours; an ion exchange reaction of the obtained powder is carried out by treatment with an aqueous solution of ammonium salt, followed by separation of the product, washing it with distilled water until the pH of the filtrate reaches 7.8-8.3, drying to constant weight and calcining at 500±10°C for 4-7 hours.

EFFECT: proposed method makes it possible to obtain a crystalline microporous composite (the degree of crystallinity is more than 90%); the content of sodium oxide or potassium oxide in the finished product is not more than 0.05 wt.%, for not more than 220 hours (this time consists of mixing reagents, formation of the primary gel structure, crystallization, filtration, drying, template removal, ion exchange, filtration, drying and calcination after ion exchange).

10 cl, 1 dwg, 2 tbl, 12 ex