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A method for synthesizing zsm-5 in situ with kaolin microspheres

A ZSM-5, kaolin microsphere technology, applied in chemical instruments and methods, crystalline aluminosilicate zeolite, physical/chemical process catalysts, etc., can solve problems such as complex processes

Active Publication Date: 2022-03-01
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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  • A method for synthesizing zsm-5 in situ with kaolin microspheres
  • A method for synthesizing zsm-5 in situ with kaolin microspheres
  • A method for synthesizing zsm-5 in situ with kaolin microspheres

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Experimental program
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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 from kaolin microspheres, specifically by adjusting the in-situ crystallization process, that is, first mixing the calcined soil balls with the sodium hydroxide solution used for crystallization, and then directly After adding seed crystals, adding a silicon source and adjusting the alkalinity, the in-situ crystallization method of ZSM‑5 with high crystallinity, large pore volume and large specific surface area can be directly obtained. This method avoids the conventional addition of special Functional component, method to improve pore structure and increase ZSM‑5 content. Moreover, this method reduces the production cost of the in-situ crystallization product, specifically showing that the amount of external silicon source can be greatly reduced, and the synthesized ZSM-5 exists in the in-situ form rather than attached crystal growth, and gathers on the surface of the microsphere.

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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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40
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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