Heavy distillate oil hydrogenation catalyst and its preparation method
A technology for hydrotreating and heavy distillate oil, applied in the petroleum industry, refining hydrocarbon oil, etc., can solve the problem that the advantages of small particle zeolite are difficult to fully exert.
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[0015] In the preparation process of the beta zeolite involved in the catalyst of the present invention, the porous solid silica gel can be coarse, mesoporous, and fine pore silica gel. The aluminum source can be solid sodium aluminate and liquid sodium aluminate. The sodium source can be It is a mixture of sodium aluminate or sodium aluminate and sodium hydroxide. The template tetraethylammonium hydroxide comes from tetraethylammonium chloride or tetraethylammonium bromide. The ammonium salt may be ammonium chloride, ammonium nitrate or ammonium sulfate, or a mixed ammonium salt. The inorganic acid used in the acid treatment is generally hydrochloric acid, nitric acid, or sulfuric acid.
[0016] The process of preparing the catalyst by the impregnation method of the present invention is as follows:
[0017] (1) The catalyst carrier is obtained by molding, drying and calcining the modified β zeolite and inorganic refractory oxides of the present invention.
[0018] (2) Add active ...
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[0029] Example 1
[0030] The modified beta zeolite with multi-stage pore structure according to the present invention is prepared. 78g sodium aluminate (laboratory preparation containing Al 2 O 3 19.9m%, containing Na 2 O 21.44m%), 435g of tetraethylammonium hydroxide aqueous solution (product of industrial production, concentration 1.4N), 288g of coarse-pored silica gel particles (produced by Qingdao Ocean Chemical Plant, containing SiO 2 95%) and 120g of purified water are mixed uniformly, and react at 100°C for 20 hours in a 2 liter stainless steel reactor under the condition of sufficient continuous stirring, and then raise to 150°C for crystallization for 40 hours. After the crystallization is completed, the pressure is relieved, the temperature is lowered, and nitric acid is added. The ammonium solution, based on the ammonium nitrate concentration in the system of 2mol / L, was stirred at 95°C for 1 hour and then filtered, and ammonium salt treatmen...
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[0031] Example 2
[0032] 80g sodium aluminate (laboratory preparation containing Al 2 O 3 18.90m%, containing Na 2 O 24.11m%), 382g tetraethylammonium hydroxide aqueous solution (industrial product, concentration 1.55N), 280g coarse-pored silica gel particles (produced by Qingdao Ocean Chemical Plant containing SiO 2 95.2m%) and 158g of purified water are mixed uniformly. Other conditions were the same as in Example 1, and β zeolite B-2 was obtained. The physical and chemical properties of the β zeolite: SiO 2 / Al 2 O 3 It is 98 (molar ratio), the average particle size is 0.20μm, the pore volume is 0.412ml / g, the pores with a pore diameter of 0.1~1.7nm account for 28.9% of the total pore volume, and the pores with a pore diameter >1.7~6.0nm account for the total pores The pore volume is 12.3%, and the pores with a pore diameter of 10.0-90.0 nm account for 54.4% of the total pore volume.
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