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A kind of highly stable modified Y-type molecular sieve and preparation method thereof

A molecular sieve and modification technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of inability to obtain silicon-aluminum ratio, low lattice collapse temperature, crystallinity retention rate and specific surface area retention Low rate and other issues

Active Publication Date: 2020-10-27
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0002] At present, the industrial production of high-silicon Y-type zeolite mainly adopts the hydrothermal method, and the NaY zeolite is subjected to multiple rare earth ion exchange and high-temperature roasting, and high-silicon Y-type zeolite containing rare earths can be prepared, which is also the preparation of high-silicon Y-type zeolite. The most conventional method for Y-type zeolite, but the disadvantage of preparing rare earth high-silicon Y-type zeolite by hydrothermal method is that the structure of zeolite will be destroyed due to too harsh hydrothermal treatment conditions, and Y-type zeolite with high silicon-aluminum ratio cannot be obtained; Although the production of external aluminum is beneficial to improve the stability of zeolite and form new acid centers, too much aluminum outside the framework reduces the selectivity of zeolite. In addition, many dealuminated holes in zeolite cannot be migrated out of the framework in time. The filling of the silicon often causes the lattice defects of the zeolite, and the crystallization retention of the zeolite is low. The lattice collapse temperature is low, the crystallinity retention rate and specific surface area retention rate are low after hydrothermal aging, and the selectivity is poor
However, pore structure analysis showed that gas-phase ultrastable molecular sieves have no secondary pores

Method used

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  • A kind of highly stable modified Y-type molecular sieve and preparation method thereof
  • A kind of highly stable modified Y-type molecular sieve and preparation method thereof
  • A kind of highly stable modified Y-type molecular sieve and preparation method thereof

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Embodiment approach

[0033] The preparation method of the modified Y-type molecular sieve provided by the invention, a kind of embodiment comprises the following steps:

[0034] (1) carry out ion exchange reaction with NaY molecular sieve (also claiming NaY zeolite) and rare earth solution, filter, wash, obtain the Y-type molecular sieve of the conventional unit cell size containing rare earth that sodium oxide content reduces; Said ion exchange is usually stirred, Exchange at a temperature of 15-95°C, preferably 65-95°C, for 30-120 minutes;

[0035] (2) The Y-type molecular sieve with the rare earth-containing conventional unit cell size whose sodium oxide content is reduced is roasted for 4.5 to 7 hours at a temperature of 350 to 480° C. in an atmosphere containing 30 to 90% by volume of water vapor, and dried to obtain water A Y-type molecular sieve with a reduced unit cell constant content of less than 1% by weight; the unit cell constant of the Y-type molecular sieve with a reduced unit cell ...

Embodiment 1

[0044] Get 2000 grams of NaY molecular sieves (calculated on a dry basis) and add them to 20 liters of decationized aqueous solution and stir to make them evenly mixed. Add 600ml of RE(NO 3 ) 3 Solution (rare earth solution concentration is RE 2 o 3 Calculated as 319g / L), stirred, heated to 90-95°C and kept for 1 hour, then filtered, washed, and the filter cake was dried at 120°C to obtain a unit cell constant of 2.471nm and a sodium oxide content of 7.0% by weight. 2 o 3 A Y-type molecular sieve with a total rare earth content of 8.8% by weight is then calcined for 6 hours at a temperature of 390°C in an atmosphere containing 50% by volume of water vapor and 50% by volume of air to obtain a Y-type molecular sieve with a unit cell constant of 2.455nm. After that, carry out Drying process, so that its water content is less than 1% by weight, and then according to SiCl 4 : Y-type molecular sieve (dry basis) = 0.5: 1 weight ratio, feed SiCl vaporized by heating 4 Gas, at a t...

Embodiment 2

[0047]Get 2000 grams of NaY molecular sieves (on a dry basis) and add them to 25 liters of decationized aqueous solution and stir to make them evenly mixed. Add 800 ml of RECl 3 solution (in RE 2 o 3 The calculated solution concentration is: 319g / L), stirred, heated up to 90-95°C for 1 hour, then filtered, washed, and the filter cake was dried at 120°C to obtain a unit cell constant of 2.471nm and a sodium oxide content of 5.5% by weight , with RE 2 o 3 A Y-type molecular sieve with a total rare earth content of 11.3% by weight is then calcined at a temperature of 450°C and 80% water vapor for 5.5 hours to obtain a Y-type molecular sieve with a unit cell constant of 2.461nm, and then dried to reduce its water content at 1 wt%, then follow SiCl 4 : Y-type zeolite = 0.6:1 weight ratio, feed SiCl vaporized by heating 4 The gas was reacted for 1.5 hours at a temperature of 480° C., and then washed with 20 liters of deionized water, and then filtered to obtain a modified Y-typ...

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Abstract

A highly stable modified Y-type molecular sieve and a preparation method thereof. The RE of the modified Y-type molecular sieve is 2 O 3 Content is 5~12% by weight, Na 2 The O content is 0.1~0.7% by weight, the total pore volume is 0.33~0.39mL / g, the pore volume of the secondary pores of 2~100nm accounts for 10~25% of the total pore volume, and the unit cell constant is 2.440~2.455nm. The skeleton aluminum content accounts for no more than 20% of the total aluminum content, the lattice collapse temperature is no less than 1050°C, and the ratio of B acid content to L acid content measured at 200°C using the pyridine adsorption infrared method is no less than 2.50. The preparation method includes the steps of ion exchange, modification treatment under certain temperature and water vapor conditions, and reaction with silicon tetrachloride. The modified Y-type molecular sieve has higher heavy oil conversion activity and lower coke selectivity, and has higher gasoline yield, liquefied gas yield, light oil yield and total liquid recovery.

Description

technical field [0001] The invention relates to a high-stability modified Y-type molecular sieve and a preparation method thereof, and further relates to a high-stability Y-type molecular sieve for heavy oil catalytic cracking and a preparation method thereof. Background technique [0002] At present, the industrial production of high-silicon Y-type zeolite mainly adopts the hydrothermal method, and the NaY zeolite is subjected to multiple rare earth ion exchange and high-temperature roasting, and high-silicon Y-type zeolite containing rare earths can be prepared, which is also the preparation of high-silicon Y-type zeolite. The most conventional method for Y-type zeolite, but the disadvantage of preparing rare earth high-silicon Y-type zeolite by hydrothermal method is that the structure of zeolite will be destroyed due to too harsh hydrothermal treatment conditions, and Y-type zeolite with high silicon-aluminum ratio cannot be obtained; Although the production of external ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/24B01J29/08B01J35/10
CPCC01B39/24B01J29/084C01P2006/12C01P2006/13C01P2006/14C01P2006/17B01J2229/14B01J2229/16B01J35/647
Inventor 周灵萍张蔚琳许明德田辉平朱玉霞
Owner CHINA PETROLEUM & CHEM CORP
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