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Method for preparing mesopore-containing high-crystallinity Y-type molecular sieve

A high crystallinity, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, fajhedral crystalline aluminosilicate zeolite, etc., can solve the problems such as limited improvement of acidity and hydrothermal stability, failure to meet the requirements of FCC use, etc. To achieve the effect of obvious mesoporous characteristics, simple preparation method and less dosage

Active Publication Date: 2020-05-01
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0003] Disclosed in CN1349929A ​​is a molecular sieve with medium pore and high crystallinity, which is characterized in that the primary and secondary structural units of Y-type zeolite are introduced in the molecular sieve pore wall, so that it has the basic structure of traditional Y-type molecular sieve, but its acidity and water The improvement of thermal stability is still very limited and cannot meet the requirements of FCC

Method used

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  • Method for preparing mesopore-containing high-crystallinity Y-type molecular sieve
  • Method for preparing mesopore-containing high-crystallinity Y-type molecular sieve
  • Method for preparing mesopore-containing high-crystallinity Y-type molecular sieve

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preparation example Construction

[0018] A method for preparing Y-type molecular sieves containing medium pores and high crystallinity, characterized in that the preparation method comprises:

[0019] (1) Preparation of crystallization directing agent: according to Al 2 o 3 :(1~35)SiO2 2 :(10~35)Na 2 O:(180~400)H 2 The molar ratio of O is to mix the silicon source, the aluminum source and water, and then carry out static aging at 0-80°C for 0.5-60h to obtain the crystallization directing agent;

[0020] (2) The cationic starch template modified by 2,3-epoxypropyltrimethylammonium chloride with a degree of substitution of 0.01% to 10% and the alkali source and water according to the conditions of the cationic starch template, alkali source and water The mass ratio is (0.1~5):(0.1~3):(1~100) mixed, and then hydrolyzed at 30~150°C to obtain the hydrolyzate;

[0021] (3) According to Al 2 o 3 :(1~20)SiO2 2 :(1~10)Na 2 O:(120~300)H 2 The molar ratio of O is to mix the silicon source, aluminum source and w...

Embodiment 1

[0039] According to Al 2 o 3 :15SiO2 2 :16.5Na 2 O:320H 2 O molar ratio, 30ml of water glass (modulus 3.3) was added to 20.8ml of sodium metaaluminate solution, stirred to dissolve, and then aged at 45°C for 5h to obtain a crystallization director.

[0040] Take 2g of YZA-2 cationic starch (degree of substitution: 0.5%) in 60g of water, add 1g of NaOH, stir evenly, heat up to 60°C, stir at constant temperature for 1h for hydrolysis treatment.

[0041] Then add the above 18g of directing agent to 65ml of water glass (modulus 3.3), stir for 0.5h, then add the aqueous solution of YZA-2 cationic starch (substitution degree 0.5%) after the above hydrolysis treatment, stir for 1h, then add 40ml of aluminum sulfate and 18ml of sodium metaaluminate, continue to stir for 1 hour after adding, and finally put the mixture into a stainless steel crystallization kettle, seal it and carry out dynamic crystallization in a rotary oven at 95°C for 28 hours, filter, wash, and filter the cake...

Embodiment 2

[0064] According to Al 2 o 3 :15SiO2 2 :16.5Na 2 O:320H 2 O molar ratio, 30ml of water glass (modulus 3.3) was added to 20.8ml of sodium metaaluminate solution, stirred to dissolve, and then aged at 30°C for 20 hours to obtain a crystallization directing agent.

[0065] Take 1g of YZA-1 cationic starch (substitution degree 1%) and put it in 60g of water, then add 0.5g of NaOH, stir evenly, heat up to 40°C, stir at constant temperature for 1h for hydrolysis treatment.

[0066] Then add the above 12g of directing agent to 50ml of water glass (modulus 3.3), stir for 0.5h, then add the aqueous solution of YZA-1 cationic starch (substitution degree 1%) after the above hydrolysis treatment, stir for 1h, then add 30ml of aluminum sulfate and 10ml of sodium metaaluminate, and continue to stir for 1 hour after the addition, and finally put the mixture into a stainless steel crystallization kettle, seal it and perform dynamic crystallization in a rotary oven at 90°C for 30 hours, fi...

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Abstract

The invention relates to a method for preparing a mesopore-containing high-crystallinity Y-type molecular sieve. The method is characterized by comprising the following steps: mixing a cationic starchtemplate agent modified by 2,3-epoxypropyl trimethyl ammonium chloride with a substitution degree of 0.01-10%, an alkali source and water, carrying out hydrolysis to obtain a hydrolysate; adding reactive silica-alumina gel into the hydrolysate to obtain an initial mixture, fully and uniformly mixing the initial mixture to obtain a gel mixture, and carrying out dynamic crystallization in a closedcrystallization kettle. The preparation method provided by the invention breaks through the technical barrier that the high-crystallinity NaY molecular sieve cannot be synthesized by conventional dynamic crystallization.

Description

technical field [0001] The invention relates to a method for preparing a Y-type molecular sieve with medium pores and high crystallinity. Background technique [0002] Y-type molecular sieves for conventional industrial applications mainly include HY with a relatively high silicon-aluminum ratio, dealuminated ultra-stabilized USY, and REY or REUSY for rare earth exchange for catalytic cracking reactions. Fluid catalytic cracking (FCC) is an important process in the secondary processing of crude oil. With the heavy and poor quality of crude oil, the excellent properties of Y-type molecular sieves with mesopores and high crystallinity gradually emerged. The Y-type molecular sieve with mesopores and high crystallinity has a micropore and mesopore dual-pore model pore distribution structure, combining mesoporous materials (excellent diffusion performance) and microporous zeolite molecular sieves (strong acidity, high stability, etc.) It is considered to be a new type of cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/24
CPCC01B39/24C01P2002/72C01P2006/12C01P2006/14
Inventor 王成强郑金玉罗一斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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