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] Said porous solid silica gel in the preparation process of the beta zeolite involved in the catalyst of the present invention can be coarse-pored, medium-pored, fine-pored silica gel, said aluminum source can be solid sodium aluminate and liquid sodium aluminate, and the sodium source can be It is sodium aluminate or a mixture of sodium aluminate and sodium hydroxide. Said templating agent tetraethylammonium hydroxide comes from tetraethylammonium chloride or tetraethylammonium bromide. Ammonium salt can be ammonium chloride, ammonium nitrate or ammonium sulfate, also can be mixed ammonium salt. The inorganic acid used in acid treatment is generally hydrochloric acid, nitric acid or sulfuric acid.
[0016] The process of preparing catalyst by impregnation method of the present invention is as follows:
[0017] (1) Forming, drying and calcining the modified β zeolite and inorganic refractory oxides involved in the present invention to obtain the catalyst carrier.
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Embodiment 1
[0030] The modified beta zeolite with multi-level pore structure described in the invention is prepared. With 78g sodium aluminate (laboratory preparation contains Al 2 o 3 19.9m%, containing Na 2 O 21.44m%), 435g tetraethylammonium hydroxide aqueous solution (the product of industrial production, concentration 1.4N), coarse porous silica gel particle 288g (Qingdao ocean chemical plant production, containing SiO 2 95%) and 120g of purified water are mixed evenly, and reacted in a 2-liter stainless steel reactor at 100°C for 20 hours under sufficient continuous stirring conditions, and then raised to 150°C for crystallization for 40 hours. Ammonium solution, based on the ammonium nitrate concentration in the system being 2 mol / L, was stirred at 95°C for 1 hour and then filtered, and ammonium salt treatment was carried out again according to the above conditions. Then filter, wash with water, dry, remove organic ammonium by three-stage temperature-controlled roasting, dehydr...
Embodiment 2
[0032] With 80g sodium aluminate (laboratory preparation contains Al 2 o 3 18.90m%, containing Na 2 O 24.11m%), 382g tetraethylammonium hydroxide aqueous solution (industrial product, concentration 1.55N), coarse porous silica gel particle 280g (Qingdao Ocean Chemical Factory produces SiO 2 95.2m%) and 158g of purified water are mixed evenly. Other conditions were the same as in Example 1 to obtain zeolite beta B-2. The physical and chemical properties of the beta zeolite are: SiO 2 / Al 2 o 3 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 of >1.7-6.0nm account for the total pores The pores with a diameter of 10.0-90.0nm accounted for 54.4% of the total pore volume.
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