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Hierarchical pore FAU structure molecular sieve and preparation method thereof

A molecular sieve, multi-stage pore technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, other chemical processes, etc., can solve the problem of large damage to the original FAU micropore structure of molecular sieves, narrow silicon-aluminum ratio range, and mesopore pore size. Problems such as poor distribution, to achieve the effect of high microporous crystal shape retention, uniform distribution and good acidity

Active Publication Date: 2020-03-31
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The post-treatment methods for molecular sieves with FAU structure reported have the following disadvantages: the distribution of mesopore size is not good; Need to add organic template agent

Method used

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  • Hierarchical pore FAU structure molecular sieve and preparation method thereof
  • Hierarchical pore FAU structure molecular sieve and preparation method thereof
  • Hierarchical pore FAU structure molecular sieve and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0099] Take 50g of molecular sieve with FAU structure (Si / Al=5.2), press the molecular sieve powder into pieces and put it into a quartz tube, then pass water through the molecular sieve at 550°C to carry out steam treatment for 2.0h; Add 10 g of molecular sieves to 200 ml of 0.50 mol / L NaOH solution, stir magnetically at 80 °C for 1.0 h, then filter and wash until neutral, dry in an oven at 120 °C for 12 h, then place in a muffle furnace Calcined at 600°C for 3.0h. The obtained molecular sieve was designated as sample A. The yield of sample A after treatment was 60.1%, and its silicon-aluminum ratio was 4.4. Add sample A to 1.0 mol / L ammonium nitrate solution with a solid-to-liquid ratio of 1:30, and magnetically stir at 85°C for 2h, then filter and wash, dry in an oven at 120°C for 12h, and then dry in a horse Calcined at 500°C for 3.5h in a Furnace to obtain hydrogen molecular sieve HA.

Embodiment 2

[0105] Take 50g of molecular sieve with FAU structure (Si / Al=5.2), press the molecular sieve powder into tablets, break into pieces and put them into a quartz tube, then pass water through the molecular sieve at 400°C for the first steam treatment for 2.0h, And the obtained molecular sieve was subjected to water vapor treatment for the second time at 600° C. for 4.0 h; 10 g of the obtained molecular sieve was added to 400 ml of 0.50 mol / L NaOH solution, and magnetically stirred at 90° C. for 1.5 h, Then it was filtered and washed until neutral, dried in an oven at 120°C for 12h, and then calcined in a muffle furnace at 600°C for 3.0h. The obtained molecular sieve was designated as sample B. The yield of sample B after treatment was 62.3%, and its silicon-aluminum ratio was 4.6. Add sample B to 1.0 mol / L ammonium nitrate solution with a solid-to-liquid ratio of 1:30, and magnetically stir at 85 °C for 2 h, then filter and wash, dry in an oven at 120 °C for 12 h, and Calcined ...

Embodiment 3

[0107] Take 50g of molecular sieve with FAU structure (Si / Al=2.4), press the molecular sieve powder into pieces and put it into a quartz tube, then pass water through the molecular sieve at 600°C to carry out steam treatment for 6.0h; Add 10 g of molecular sieves to 200 ml of 0.40 mol / L NaOH solution, stir magnetically at 80 ° C for 0.5 h, then filter and wash until neutral, dry in an oven at 120 ° C for 12 h, and then place in a muffle furnace Calcined at 400°C for 5.0h. The obtained molecular sieve is designated as sample C. The yield of sample C after treatment was 65.5%, and its silicon-aluminum ratio was 2.2. Sample C was added to 1.0 mol / L ammonium nitrate solution with a solid-to-liquid ratio of 1:30 and magnetically stirred at 85 °C for 2 h, then filtered and washed, dried in an oven at 120 °C for 12 h, and then placed in a horse Calcined at 500°C for 3.5h in a Furnace to obtain hydrogen molecular sieve HC.

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Abstract

The invention discloses a hierarchical pore FAU structure molecular sieve and a preparation method thereof, and a modified hierarchical pore FAU structure molecular sieve, and belongs to the field ofmolecular sieve modification, adsorption material preparation and catalyst preparation. The hierarchical pore FAU structure molecular sieve has a microporous channel system with an FAU topological structure and a mesoporous system with a pore size range of 2-10 nm. The preparation method comprises the following steps: carrying out water vapor treatment and alkali treatment on an FAU structure molecular sieve precursor, and roasting the treated product. According to the invention, the hierarchical pore FAU structure molecular sieve is high in crystal form retention degree, wide in silicon-aluminum ratio application range, uniform in micropore and mesopore distribution and good in acidity, and can be converted into a hydrogen type or other ionic hierarchical pore FAU structure molecular sieves through ion exchange; and the preparation method can reduce the cost, is wide in the silicon-aluminum ratio application range of the precursor molecular sieve, and can generate expected mesopores in the case of the keeping of original micropores, so that the controllable pore channel adjustment of the FAU structure molecular sieve is realized.

Description

technical field [0001] The application relates to a molecular sieve with a hierarchical porous FAU structure, a preparation method thereof, and a modified molecular sieve with a FAU hierarchical porous structure, belonging to the fields of molecular sieve modification, adsorption material preparation and catalyst preparation. Background technique [0002] Molecular sieves have been widely used as main catalytic materials, adsorption separation materials and ion exchange materials in petroleum refining, Petrochemical, environmental protection, fine chemical and other fields. Among them, the Y-type molecular sieve with FAU topology has a unique three-dimensional pore structure and is an important catalytic material, which is widely used in catalytic cracking, hydrocracking and other oil refining and petrochemical fields. However, due to the small pore size of FAU molecular sieves, it is not conducive to the diffusion of macromolecules inside the channels, resulting in low cha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B82Y30/00B82Y40/00B01J20/18B01J20/30
CPCB01J20/186B82Y30/00B82Y40/00C01B39/026C01P2002/72C01P2004/03C01P2004/04C01P2006/12C01P2006/14C01P2006/17B01J20/18B01J20/30C01B39/02C01B39/20C01B39/22C01B39/24
Inventor 黄声骏张大治
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI