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Method for in-situ synthesis of ZSM-5 through kaolin microspheres

A technology of ZSM-5 and kaolin microspheres, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve problems such as complex process

Active Publication Date: 2019-12-03
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires high-temperature treatment at two different temperatures, and the process is more complicated.

Method used

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  • Method for in-situ synthesis of ZSM-5 through kaolin microspheres
  • Method for in-situ synthesis of ZSM-5 through kaolin microspheres
  • Method for in-situ synthesis of ZSM-5 through kaolin microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 10 kg of kaolin (dry basis) and water were prepared into a slurry with a solid content of 35%, and 155 g of sodium hydroxide was added as a dispersant for spray molding. The obtained spray soil balls were roasted at 900°C for 4h. Stir 204g of roasted soil balls with 78mL of 10% sodium hydroxide solution, and heat up to 75°C for 240min, then add 4.5g of HZSM-5 seed crystals, 484g of water glass and 600g of water, continue stirring for 0.5h, and finally Add 226g of H 2 SO 4 The solution (18wt%) was heated up to 120°C for static crystallization for 6 hours, then heated up to 184°C for static crystallization for 8h, filtered, washed and dried. Figure 1A and Figure 1B It is the SEM image of this embodiment.

Embodiment 2

[0044] 10 kg of kaolin and water were prepared into a slurry with a solid content of 28%, and 500 g of aluminum sol was added as a dispersant for spray molding. The obtained spray soil balls were roasted at 980°C for 2h. 178.5 g of roasted soil balls and 300 ml of 14% sodium hydroxide solution were stirred, and the temperature was raised to 85° C. for 100 min, then 12 g of HZSM-5 seed crystals, 124 g of white carbon black and 850 g of water were added, and the stirring was continued for 0.5 h. Raise the temperature to 107°C for dynamic crystallization for 5.5 hours, then raise the temperature to 180°C for static crystallization for 12 hours, filter, wash and dry. Figure 2A and Figure 2B It is the SEM image of this embodiment.

Embodiment 3

[0046] 10 kg of kaolin and water were prepared into a slurry with a solid content of 39%, and 200 g of sodium hydroxide sol was added as a dispersant for spray molding. Roast the obtained spray soil ball at 950°C for 5.5h, stir 255g of the roasted soil ball with 85mL of 17% sodium hydroxide solution, and raise the temperature to 60°C and stir for 280min, then add 2.5g NaZSM-5 seed crystal , 165g water glass and 13g white carbon black, 1567g water, finally add 87g of H 2 SO 4 The solution (8wt%) was heated up to 138°C, stirred intermittently for 5 hours, then heated up to 162°C for static crystallization for 19 hours, filtered, washed and dried.

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Abstract

The invention provides a method for in-situ synthesis of ZSM-5 through kaolin microspheres. The method specifically comprises the steps that by regulating an in-situ crystallization process, calcinated soil spheres and a sodium hydroxide solution for crystallization are mixed firstly, then seed crystals are directly added, a silicon source is added, the alkalinity is regulated, and then the in-situ crystallized ZSM-5 with the high crystallinity, large pore volume and large specific area is directly obtained. According to the method, a method that components with special functions are added into the kaolin microspheres conventionally to improve the hole structure and increase the content of the ZSM-5 is avoided; and through the method, the production cost of an in-situ crystallization product is lowered, specifically, the quantity of the added silicon source can be decreased greatly, and more of the synthesized ZSM-5 exists in an in-situ form instead of being gathered on the surfaces ofthe microspheres by outgrowth.

Description

technical field [0001] The invention relates to a synthesis method of in-situ crystallization of ZSM-5 through kaolin microspheres, in particular to a low-cost in-situ crystallization ZSM-5 molecular sieve material with relatively high crystallinity, pore volume and large specific surface area resolve resolution. Background technique [0002] In recent years, with the consensus of refining companies on using catalytic cracking units to increase propylene production to improve economic benefits, increasing the content of ZSM-5 zeolite in the catalyst has become a key issue in increasing the cracking capacity of the catalyst, and introducing ZSM-5 to the carrier through in-situ crystallization 5 zeolite has outstanding advantages in improving catalyst anti-wear performance, heavy oil conversion ability and activity stability. [0003] CN101332995A, CN1872415A have developed an in-situ crystallization method for high-content ZSM-5 zeolite, including modified roasting of kaolin...

Claims

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Application Information

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IPC IPC(8): C01B39/38
CPCC01B39/38C01P2004/03C01P2006/12C01P2006/14
Inventor 王宝杰赵红娟胡清勋熊晓云王久江孙雪芹田爱珍杨周侠张莉滕秋霞赵晓争
Owner PETROCHINA CO LTD
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