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Mesoporous-microporous composite Y molecular sieve with through hole structure and preparation method thereof

A molecular sieve and through-hole technology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of the proportion of mesopores to be further improved, the introduction of sieve heteroatoms is low, and the improvement can be achieved. and utilization rate, high introduction amount, and the effect of reducing diffusion resistance

Active Publication Date: 2021-04-20
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the heteroatom molecular sieve prepared by the direct hydrothermal synthesis method currently has a low amount of heteroatom introduction, and the proportion of mesopores formed after removing heteroatoms needs to be further improved.

Method used

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  • Mesoporous-microporous composite Y molecular sieve with through hole structure and preparation method thereof
  • Mesoporous-microporous composite Y molecular sieve with through hole structure and preparation method thereof
  • Mesoporous-microporous composite Y molecular sieve with through hole structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1) In the first step, place the boron-containing Beta molecular sieve (i.e. B-Beta molecular sieve) in a muffle furnace at 550° C. for 6 h to remove the template agent, and weigh 5 g of the boron-containing Beta molecular sieve (B-Beta molecular sieve) to remove the template agent. 2 o 3 Content 2wt%, SiO 2 content 93.6wt%) was dissolved in 50ml of concentrated NaOH (3mol / L) solution, heated to boiling, stirred for 30min until the molecular sieves were completely dissolved and set aside.

[0037] 2) In the second step, 1.79g of sodium metaaluminate (Al 2 o 3 The content is 41wt%, Na 2 O content is 28.7%) is dissolved in 25.19g deionized water, adds 6.13g sodium hydroxide (purity 96%) under mechanical stirring, continues stirring, makes it dissolve completely, obtains high alkalinity sodium metaaluminate solution. In a stirring state, the above-mentioned high alkalinity sodium metaaluminate solution was added to 24.7g water glass (SiO 2 The content is 26.2wt%, Na 2...

Embodiment 2

[0041] 1) In the first step, the boron-containing Beta molecular sieve is placed in a muffle furnace at 580° C. for 5 h to remove the template agent, and 5 g of the boron-containing Beta molecular sieve (B 2 o 3 content of 2.3wt%, SiO2 content of 96.0wt%) was dissolved in 50ml of concentrated NaOH (3mol / L) solution, heated to boiling, stirred for 30min until the molecular sieves were completely dissolved and set aside.

[0042] 2) In the second step, 1.79g of sodium metaaluminate (Al 2 o 3 The content is 41wt%, Na 2 O content is 28.7%) is dissolved in 25.19g deionized water, adds 6.13g sodium hydroxide (purity 96%) under mechanical stirring, continues stirring, makes it dissolve completely, obtains high alkalinity sodium metaaluminate solution. In a stirring state, the above-mentioned high alkalinity sodium metaaluminate solution was added to 24.7g water glass (SiO 2 The content is 26.2wt%, Na 2 O content is 8.3%), after mixing evenly, continue to stir for 2 hours, and th...

Embodiment 3

[0046] 1) In the first step, the boron-containing Beta molecular sieve is placed in a muffle furnace at 600° C. for 4 h to remove the template agent, and 5 g of the boron-containing Beta molecular sieve (B 2 o 3 Content 2.5wt%, SiO 2 content 96.7wt%) was dissolved in 50ml of concentrated NaOH (3mol / L) solution, heated to boiling, stirred for 30min until the molecular sieves were completely dissolved and set aside.

[0047] 2) In the second step, 1.79g of sodium metaaluminate (Al 2 o 3 The content is 41wt%, Na 2 O content is 28.7%) is dissolved in 25.19g deionized water, adds 6.13g sodium hydroxide (purity 96%) under mechanical stirring, continues stirring, makes it dissolve completely, obtains high alkalinity sodium metaaluminate solution. In a stirring state, the above-mentioned high alkalinity sodium metaaluminate solution was added to 24.7g water glass (SiO 2 The content is 26.2wt%, Na 2 O content is 8.3%), after mixing evenly, continue to stir for 2 hours, and then s...

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Abstract

The preparation method comprises the following steps: pretreating a B-Beta molecular sieve with a high boron content to prepare a boron-containing precursor, adding a silicon source, an aluminum source, an alkali source, a crystallization guiding agent and water into the boron-containing precursor, enabling the gel ratio to be (0.5-20)Na2O:1Al2O3:(3-40)SiO2:(0.005-2.0)B2O3:(80-800)H2O, stirring for 0.5-4 hours at the temperature of 5-70 DEG C, heating the gel to 80-120 DEG C, crystallizing for 12-100 hours to obtain a heteroatom B-Y molecular sieve with higher boron content, and carrying out ammonium exchange and hydrothermal hyperstabilization treatment on the synthesized heteroatom B-Y molecular sieve twice to obtain the mesoporous-microporous composite Y molecular sieve with a through hole structure. The mesoporous-microporous composite Y molecular sieve prepared by adopting the method provided by the invention has rich mesoporous structures, good connectivity between pore channels, low diffusion resistance in the pore channels of the molecular sieve, and high accessibility and utilization rate of active centers.

Description

technical field [0001] The invention belongs to the field of molecular sieve materials and preparation thereof, and in particular relates to a mesoporous composite Y molecular sieve with a through-pore structure and a preparation method thereof. Background technique [0002] Y molecular sieves are widely used in the fields of adsorption, separation and catalysis because of their excellent pore structure and suitable surface acidity. With the increasingly heavy feed oil, improving the accessibility of the active center of refining catalysts and improving their catalytic conversion ability to macromolecules has become the focus of petrochemical catalyst development. Due to the mesoporous or macroporous structure of mesoporous molecular sieves, it is beneficial to the mass transfer of macromolecular substances, which can improve the accessibility of catalytic active centers and the utilization rate of heavy oil. At the same time, the rich and unobstructed pore structure reduce...

Claims

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Application Information

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IPC IPC(8): C01B39/24
Inventor 洪美花臧甲忠刘冠锋宫毓鹏彭晓伟洪鲁伟季超宋万仓石芳
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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