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Preparation method of small-grain Y-type molecular sieve

A molecular sieve and small-grain technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem of poor hydrothermal stability of small-grain NaY molecular sieves and fine-grain Y-type molecular sieves. Poor performance, complex process steps and other problems, to achieve excellent cracking activity and product properties, maintain good crystallinity, and facilitate the effect of diffusion

Active Publication Date: 2017-01-18
CHINA PETROLEUM & CHEM CORP +1
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AI Technical Summary

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
[0014] At present, due to the poor hydrothermal stability and unstable structure of small-grain NaY molecular sieves, small-grain Y-type molecular sieves with complete structure, high crystallinity and many secondary pores cannot be obtained after subsequent modification.

Method used

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  • Preparation method of small-grain Y-type molecular sieve
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  • Preparation method of small-grain Y-type molecular sieve

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Embodiment 1

[0047] This embodiment is to prepare raw material small grain NaY type molecular sieve

[0048] Preparation of NY-1

[0049] (1) Preparation of directing 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 8wt%), mixed evenly, and aged at 18° C. for 4 hours to prepare the directing agent.

[0050] (2) Preparation of amorphous silicon-aluminum precursor

[0051] 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 wate...

Embodiment 2

[0065] Firstly, ammonium exchange is carried out on the raw material small grain NaY molecular sieve NY-1. Formulated with NH 4 + and H + Concentrations of 1.0mol / L and 0.02mol / L solution (ammonium chloride and hydrochloric acid mixed solution) 10 liters. Weigh 1,000 grams of small-grain NaY molecular sieves, add them to the above mixed solution, stir at 300 rpm, and stir at a constant temperature of 90°C for 1 hour, then filter the molecular sieves, and leave a small sample for analysis of NaY 2 O content; repeat the above operation until Na in the molecular sieve 2 The content of O reached 1.5wt%, and the sample number after drying was NNY-1.

Embodiment 3

[0067] Firstly, ammonium exchange is carried out on the raw material small grain NaY molecular sieve NY-2. Formulated with NH 4 + and H + 10 liters of solutions (mixed solution of ammonium nitrate and nitric acid) with concentrations of 0.8.0mol / L and 0.01mol / L respectively. Weigh 1,000 grams of small-grain NaY molecular sieves, add them to the above mixed solution, stir at 300 rpm, and stir at a constant temperature of 95°C for 1 hour, then filter the molecular sieves, and leave a small sample for analysis of NaY 2 O content; repeat the above operation until Na in the molecular sieve 2 The O content reached 1.5wt%, and the sample number after drying 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 ammonium exchange, primary hydro-thermal treatment, treatment with an alkali-containing solution, secondary 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, retains 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 Y-type molecular sieve, in particular to a preparation method of deeply dealuminated 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, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/24B01J29/08
Inventor 孙晓艳樊宏飞王占宇
Owner CHINA PETROLEUM & CHEM CORP
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