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A kind of preparation method of small grain nay type molecular sieve

A small-grain, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problem of poor hydrothermal stability of fine-grained Y-type molecular sieve, uneven distribution of silicon and aluminum, and technical problems. Complicated steps and other problems, to achieve the effect of improving the effective utilization rate, concentrating the distribution range of grains, and uniform distribution of silicon and aluminum

Active Publication Date: 2017-02-15
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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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
[0011] At present, during the preparation process of small-grain NaY molecular sieves in the existing method, silicon and aluminum are easily lost, the utilization rate of silicon is low, and the distribution of silicon and aluminum is not uniform, and agglomeration is easy to occur. Therefore, the existing method is still unable to prepare silicon-aluminum ratio. , and small crystal NaY molecular sieve with good thermal stability and hydrothermal stability

Method used

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  • A kind of preparation method of small grain nay type molecular sieve
  • A kind of preparation method of small grain nay type molecular sieve
  • A kind of preparation method of small grain nay type molecular sieve

Examples

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Embodiment 1

[0034] (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.

[0035] (2) Preparation of amorphous silicon-aluminum precursor

[0036] Prepare solid sodium aluminate to a concentration of 0.3L for 100g A1 2 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 the tank, stir and heat to 70°C, open the valves of the sulfur containers respectively (a), (b) and (c) at the sa...

Embodiment 2

[0042] (1) Preparation of guiding agent: Dissolve 10 g of sodium hydroxide solid in 90 g of water, add 3 g of sodium metaaluminate (Al 2 o 3 Content is 45wt%, Na 2 O content is 41wt%), then add 50g water glass (SiO 2 Content is 28wt%, Na 2 The O content is 8wt%), mixed evenly, and aged at 20° C. for 4 hours to prepare the directing agent.

[0043] (2) Preparation of amorphous silicon-aluminum precursor

[0044] Prepare solid aluminum sulfate to a concentration of 80g A1 in 0.5L 2 o 3 / L aluminum sulfate 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 0.4L concentration is 150g SiO 2 / L sodium silicate working solution (c). Take a 5-liter steel reaction tank, add 0.5 liter of distilled water to the tank, stir and heat to 70°C, open the valves of the containers (a), (b) and (c) at the same time, control (a) and ...

Embodiment 3

[0050] (1) Preparation of the directing agent: The preparation of the directing agent is the same as in Example 1.

[0051] (2) Preparation of amorphous silicon-aluminum precursor

[0052] Prepare solid aluminum chloride to 0.5L concentration to be 100g A1 2 o 3 / L aluminum chloride 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 0.4L concentration of 125g SiO 2 / L sodium silicate working solution (c). Take a 5-liter steel reaction tank, add 0.5 liter of distilled water to the tank, stir and heat to 70°C, open the valves of the containers (a), (b) and (c) at the same time, control (a) and ( c) the flow rate to keep the neutralization reaction time at 40 minutes, and quickly adjust the flow rate of (b) to keep the pH value of the system at 7-8, and control the temperature of the system at about 60°C. After the alu...

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Abstract

The invention discloses a preparation method of a small-grain NaY-type molecular sieve. According to the invention, an amorphous silica-alumina precursor, a directing agent synthesized under a low temperature, part of a silicon source, and the like are mixed under a low temperature, such that silica-alumina gel is prepared; and crystallization is carried out, such that the small-grain NaY-type molecular sieve is obtained. According to the amorphous silica-alumina precursor, a part of a silicon-containing material is added in an aluminum-containing material before and / or during a gelling process; and the rest of the silicon-containing material is added after gelling and before aging, such that silica-alumina forms a stable structure, and can cooperate with subsequent steps. With the method, a phenomenon of silicon agglomeration or loss caused by the addition of a large amount of the silicon source in prior arts is avoided. The addition amount of silicon is reduced; silicon effective utilization rate is improved; the silica-to-alumina ratio is improved; and the obtained small-grain molecular sieve has good stability. The small-grain NaY-type molecular sieve provided by the invention can be used in a hydrocracking reaction, and has good cracking activity and product selectivity.

Description

technical field [0001] The invention relates to a method for preparing a Y-type molecular sieve, in particular to a method for preparing a small-grain NaY-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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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/24
CPCC01B39/24C01P2002/72C01P2004/03C01P2004/62C01P2006/12C01P2006/32
Inventor 孙晓艳樊宏飞王占宇
Owner CHINA PETROLEUM & CHEM CORP
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