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High-stability modified Y-type molecular sieve for high production of isomerized C4 and preparation method of high-stability modified Y-type molecular sieve

A molecular sieve and modification technology, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, refined hydrocarbon oil, etc., can solve the problems of inability to effectively increase the content of isomeric hydrocarbons in gasoline, poor thermal and hydrothermal stability of Y molecular sieve, and low zeolite crystallization retention etc. to achieve the effects of high stability, high crystallinity and low coke selectivity

Active Publication Date: 2020-01-07
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. In this method, 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. Silica Y-type zeolite is the most conventional method, 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 generation of extra-framework aluminum is beneficial to improving the stability of zeolite and forming new acid centers, too much extra-framework aluminum reduces the selectivity of zeolite. Migrated silicon fills up, often causing lattice defects of zeolite, and the crystallization retention of zeolite is low
However, the Y molecular sieve prepared by this method has poor thermal and hydrothermal stability, and usually can only increase the content of isobutane, but cannot effectively increase the content of isomeric hydrocarbons in gasoline

Method used

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  • High-stability modified Y-type molecular sieve for high production of isomerized C4 and preparation method of high-stability modified Y-type molecular sieve
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  • High-stability modified Y-type molecular sieve for high production of isomerized C4 and preparation method of high-stability modified Y-type molecular sieve

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Embodiment approach

[0032] The preparation method of the modified Y-type molecular sieve provided by the invention, a kind of embodiment comprises the following steps:

[0033] (1) NaY molecular sieve (also known as NaY zeolite) is contacted with a mixed solution of soluble calcium salt and rare earth salt for ion exchange reaction, filtered and washed to obtain calcium and rare earth conventional unit cell size Y type with reduced sodium oxide content Molecular sieve; the ion exchange is usually exchanged for 30 to 120 minutes at a temperature of 15 to 95° C., preferably 65 to 95° C.;

[0034] (2) Calcium-containing and rare earth-containing conventional Y-type molecular sieves with a reduced sodium oxide content are calcined for 4.5-7 hours at a temperature of 350-480° C. in an atmosphere containing 30-90% by volume of water vapor, and dried, Obtaining a Y-type molecular sieve with a reduced unit cell constant whose water content is less than 1% by weight; the unit cell constant of the Y-type m...

Embodiment 1

[0043] Get 2000 grams of NaY molecular sieves (on a dry basis) and add to 20 liters of decationized aqueous solution and stir to make it evenly mixed, and add 345ml of Ca(NO 3 ) 2 solution (concentration of the solution in terms of CaO is 248g / L), then add 300ml of RE (NO 3 ) 3 Solution (rare earth solution concentration is RE 2 o 3 Calculated as 319g / L), stirred, heated up 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, a sodium oxide content of 6.6% by weight, and calcium oxide based on CaO. Content 4.9% by weight, with RE 2 o 3 A Y-type molecular sieve with a total rare earth content of 4.4% by weight is then roasted for 6 hours at a temperature of 390° C. in an atmosphere containing 50 volume percent water vapor and 50 volume percent air to obtain a Y-type molecular sieve with a unit cell constant of 2.455 nm. After that, carry out Drying process, so that its water content is les...

Embodiment 2

[0046] 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 368ml of CaCl 2 solution (concentration of solution in terms of CaO: 248g / L), 400ml of RECl 3 solution (in RE 2 o 3 The calculated solution concentration is: 319g / L), stirred, heated up to 90-95°C, 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 5.2% by weight %, Calcium content in terms of CaO is 8.7% by weight, in terms of RE 2 o 3 A Y-type molecular sieve with a total rare earth content of 5.7% 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 rea...

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Abstract

The invention discloses a high-stability modified Y-type molecular sieve for high production of isomerized C4 and a preparation method of the high-stability modified Y-type molecular sieve. The CaO content of the modified Y-type molecular sieve is 0.3-4 wt%, the RE2O3 content is 2 to 7 wt%; the content of Na2O is 0.1 to 0.5 wt%; the total pore volume is 0.33 mL / g to 0.39 mL / g; the pore volume of the secondary pores of 2-100nm accounts for 10-25% of the total pore volume; the lattice constant is 2.440-2.455 nm, the content of non-framework aluminum accounts for not more than 20% of the total aluminum content, the lattice collapse temperature is not lower than 1050 DEG C, and the ratio of the amount of acid B to the amount of acid L measured by a pyridine adsorption infrared method at 200 DEG C is not lower than 2.30. The preparation method comprises 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, lower coke selectivity, higher gasoline yield and isomeric C4 yield, and higher isomeric hydrocarbon content in gasoline.

Description

technical field [0001] The invention relates to a highly stable modified Y-type molecular sieve capable of producing more isomeric C4 hydrocarbons and a preparation method thereof. Background technique [0002] At present, the industrial production of high-silicon Y-type zeolite mainly adopts the hydrothermal method. In this method, 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. Silica Y-type zeolite is the most conventional method, 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 generation of extra-framework aluminum is beneficial to improving the stability of zeolite and forming new acid centers, too much extra-framework alum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/08C10G11/05C10G25/03
CPCB01J29/088C10G11/05C10G25/03B01J2229/18C10G2300/202C10G2300/305B01J35/633B01J35/651B01J35/647
Inventor 袁帅田辉平周灵萍陈振宇张蔚琳沙昊
Owner CHINA PETROLEUM & CHEM CORP
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