Preparation method for small-grain Y type molecular sieve

A molecular sieve and small-grain technology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of complete structure, poor thermal and hydrothermal stability, high crystallinity, etc., and achieve good Good performance, good stability and high crystallinity

Active Publication Date: 2015-08-12
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0004] The method for preparing fine-grained Y-type molecular sieves proposed in CN1081425A is to precrystallize the NaY synthesis solution at 80°C to 180°C for 1 to 10 hours, then add the directing agent after cooling to room temperature, and then add the directing agent at 80°C to 100°C. Continue to crystallize for 5 to 25 hours, the process steps are more complicated and difficult to control, and the hydrothermal stability of the fine-grained Y-type molecular sieve obtained is poor
CN1382632A discloses a super-stabilizing method of small-grain Y-type zeolite, which is obtained by c

Method used

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  • Preparation method for small-grain Y type molecular sieve

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Embodiment 1

[0045] This embodiment is to prepare raw material small grain NaY molecular sieve

[0046] Preparation of NY-1

[0047] (1) Preparation of guiding agent: Dissolve 8 g of sodium hydroxide solid in 80 g of water, add 2.5 g of sodium metaaluminate (Al 2 o 3 Content is 45wt%, Na 2 O content is 41wt%), then add 40g water glass (SiO 2 Content is 28wt%, Na 2 The O content is 8 wt%), mixed evenly and aged at 18°C ​​for 4 hours to prepare the directing agent.

[0048] (2) Preparation of amorphous silicon-aluminum precursor

[0049] Prepare solid sodium aluminate to a concentration of 0.3L for 100g A12 o 3 / L sodium aluminate working solution (a). Dilute the concentrated ammonia water with an appropriate amount of distilled water to obtain about 10wt% dilute ammonia water (b). SiO 2 28wt% sodium silicate solution, then diluted to 0.5L concentration is 140g SiO 2 / L sodium silicate working solution (c). Take a 5-liter steel reaction tank, add 0.5 liter of distilled water to t...

Embodiment 2

[0063] First, carry out alkali treatment on the raw material small-grain NaY molecular sieve, beat and mix 1000 grams of NY-1 with 5 L of NaOH solution with a concentration of 1 mol / L, and maintain the temperature of 80 ° C for 2 hours, filter and wash to the solution Close to neutrality; contact the filter cake with 10 liters of 0.5 mol / L ammonium nitrate aqueous solution, stir at 300 rpm, stir at 90°C for 1 hour, then filter molecular sieves, and leave a small sample for analysis of Na 2 O content; repeat the above operation until Na in the molecular sieve 2 The O content reached 2.5wt%, and the sample number after drying was NNY-1.

Embodiment 3

[0065] First, carry out alkali treatment on the raw material small-grain NaY molecular sieve, beat and mix 1000 grams of NY-2 with 5 L of KOH solution with a concentration of 0.8 mol / L, and keep stirring at 80°C for 2 hours, filter, and wash with water until the solution Close to neutral; contact the filter cake with 10 liters of 0.5 mol / L ammonium nitrate aqueous solution, stir at 300 rpm, stir at a constant temperature of 95 ° C for 1 hour, then filter molecular sieves, and leave a small sample for analysis of Na 2 O content; repeat the above operation until Na in the molecular sieve 2 The content of O reached 2.5wt%, and the number of the dried sample was NNY-2.

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Abstract

The invention discloses a preparation method for a small-grain Y type molecular sieve. According to the method, a NaY type molecular sieve raw material with a high silica-alumina ratio, a high degree of crystallization and good stability is employed and successively undergoes alkali washing, ammonium exchange, aluminum removal and silicon supplement, hydro-thermal treatment and treatment with a mixed solution of acid and an ammonium salt; and the obtained small-grain Y type molecular sieve has a high SiO2/Al2O3 mol ratio and a high proportion of secondary pores, remains the stability of a Y type molecular sieve and has a high specific surface area and a high degree of crystallization. The small-grain Y type molecular sieve prepared in the invention is applicable as a cracking component for a hydrocracking catalyst used for high and medium oil and enables the hydrocracking catalyst to have good activity, medium oil selectivity and product properties.

Description

technical field [0001] The invention relates to a preparation method of a Y-type molecular sieve, in particular to a preparation method of a small-grain Y-type molecular sieve. Background technique [0002] Y-type molecular sieve is currently the most common cracking active component in the field of heavy oil cracking. The crystal grain is generally about 1000nm. After the reaction, the product is also difficult to diffuse out, so its cracking activity and selectivity of the target product are restricted. Compared with conventional Y-type molecular sieves, small-grain Y-type molecular sieves have a larger outer surface area and more active centers on the outer surface, which is conducive to improving the cracking capacity of macromolecular hydrocarbons, and thus has superior catalytic performance. At the same time, reducing the grain size of the Y-type molecular sieve can also improve the utilization rate of active sites on the inner surface. In general, the diffusion of r...

Claims

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Application Information

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IPC IPC(8): C01B39/24
Inventor 樊宏飞孙晓艳王占宇
Owner CHINA PETROLEUM & CHEM CORP
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