High-stability modified Y-type molecular sieve and preparation method thereof

A molecular sieve and modification technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of low retention rate of crystallinity and specific surface area, poor thermal and hydrothermal stability, and retention of zeolite crystals. low coke selectivity, high thermal and hydrothermal stability, and high stability

Active Publication Date: 2018-08-28
CHINA PETROLEUM & CHEM CORP +1
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AI Technical Summary

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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  • High-stability 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

The invention relates to a high-stability modified Y-type molecular sieve and a preparation method thereof, wherein the modified Y-type molecular sieve contains 5-12 wt% of RE2O3 and 0.1-0.7 wt% of Na2O, and has the total pore volume of 0.33-0.39 mL / g, the pore volume of the secondary pores with the pore size of 2-100 nm accounts for 10-25% of the total pore volume, the unit cell constant is 2.440-2.455 nm, the non-framework aluminum content is not more than 20% of the total aluminum content, the lattice collapse temperature is not below 1050 DEG C, and the pyridine adsorption infrared methoddetermination results show that a ratio of the amount of B acid to the amount of L acid is not less than 2.50. The preparation method comprises: ion exchange, modification treatment at a certain temperature under water vapor conditions, and reaction with silicon tetrachloride. According to the present invention, the modified Y-type molecular sieve has advantages of high heavy oil conversion activity, low coke selectivity, high diesel yield, high liquefied gas yield, high light-oil yield and high 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 Applications(China)
IPC IPC(8): C01B39/24B01J29/08B01J35/10
CPCB01J29/084B01J35/1061B01J2229/14B01J2229/16C01B39/24C01P2006/12C01P2006/13C01P2006/14C01P2006/17
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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