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Preparation method of hierarchical pore FAU type zeolite molecular sieve with house-of-cards-like structure

A zeolite molecular sieve and multi-stage pore technology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of unavoidable organic compounds, unfavorable industrial production, and reduce synthesis costs, etc., to achieve large-scale Large-scale commercial production, reduced manufacturing process costs, and good thermal stability

Active Publication Date: 2017-12-26
SHENZHEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method avoids the use of expensive long-chain organic amine templates and reduces the synthesis cost, but the use of organic compounds is still unavoidable.
Recently, A.Inayat et al. used zinc nitrate or lithium carbonate as inorganic salt additives to modify the morphology of X-type molecular sieves and prepared sheet-like X-type molecular sieves. However, a large amount of inorganic salts such as lithium salts and zinc salts were used. The cost is not low, which is not conducive to industrial production

Method used

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  • Preparation method of hierarchical pore FAU type zeolite molecular sieve with house-of-cards-like structure
  • Preparation method of hierarchical pore FAU type zeolite molecular sieve with house-of-cards-like structure
  • Preparation method of hierarchical pore FAU type zeolite molecular sieve with house-of-cards-like structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Add 0.5g of sodium hydroxide and 1.2g of sodium aluminate into 6.7g of deionized water, and stir until a clear solution;

[0025] (2) to the clear solution of step (1), slowly add 3.88g water glass (wherein the content of active ingredient is SiO 2 27.13 wt%, Na 2 (8.74wt%), stir evenly, ultrasonic, obtain uniform dilute colloid;

[0026] (3) Put the dilute colloid obtained in step (2) into a hydrothermal reaction kettle, and crystallize at a constant temperature of 75°C for 48h, wherein the molar ratio of the reaction mixture is Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=1.43:1.0:2.4:70.2;

[0027] (4) After the crystallization is completed, the solid product is filtered and washed, dried in a blast oven at 70°C for 24 hours, and then calcined at a constant temperature of 450°C in air for 5 hours (the heating rate is 1°C min -1 ), to obtain a "plug-in" structure hierarchical porous FAU type zeolite molecular sieve.

[0028] The characterization and analysis of the "pl...

Embodiment 2

[0034] (1) Add 0.5g of sodium hydroxide and 1.2g of sodium aluminate into 6.7g of deionized water, and stir until a clear solution;

[0035] (2) to the clear solution of step (1), slowly add 3.88g water glass (wherein the content of active ingredient is SiO 2 27.13 wt%, Na 2 (8.74wt%), stir evenly, ultrasonic, obtain uniform dilute colloid;

[0036] (3) Put the dilute colloid obtained in step (2) into a hydrothermal reaction kettle, crystallize at a constant temperature of 60°C for 72h, wherein the molar ratio of the reaction mixture is Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=1.43:1.0:2.4:70.2;

[0037] (4) After the crystallization is completed, the solid product is suction filtered, washed, dried in a blast oven at 70°C under normal pressure for 24 hours, and then calcined at a constant temperature of 500°C in air for 4 hours (the heating rate is 1°C min -1 ), obtain " plug-in card " type multi-stage hole FAU type molecular sieve 2.2g, productive rate is 18% (product accounts...

Embodiment 3

[0040] (1) Add 0.5g sodium hydroxide and 1.2g sodium aluminate to 4.7g deionized water, and stir until a clear solution;

[0041] (2) to the clear solution of step (1), slowly add 3.88g water glass (wherein the content of active ingredient is SiO 2 27.13 wt%, Na 2 (8.74wt%), stir evenly, ultrasonic, obtain uniform dilute colloid;

[0042] (3) Put the dilute colloid obtained in step (2) into a hydrothermal reaction kettle, and crystallize at a constant temperature of 75°C for 48h, wherein the molar ratio of the reaction mixture is Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=1.43:1.0:2.4:54.8;

[0043] (4) After the crystallization is completed, the solid product is suction filtered, washed, dried in a blast oven at 70°C under normal pressure for 24 hours, and then calcined at a constant temperature of 450°C in air for 4 hours (the heating rate is 1°C min -1 ) to obtain 2.1 g of "plug-in card" type multi-stage porous FAU molecular sieves, with a productive rate of 20.4% (the mass rat...

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Abstract

The invention discloses a preparation method of a hierarchical pore FAU type zeolite molecular sieve with a house-of-cards-like structure, and belongs to the technical field of inorganic chemistry. The preparation method comprises the following steps: at first, dissolving an inorganic alkali source and an aluminum source into deionized water, slowly adding a silicon source, fully and evenly stirring to obtain uniform sol, and then subjecting the sol to a hydrothermal crystallization treatment to obtain the hierarchical pore FAU type zeolite molecular sieve with a plug-in card structure. The hierarchical pore FAU type zeolite molecular sieve is synthesized in the absence of inorganic / organic templates and an inorganic salt additive, the synthesis cost is greatly reduced, and the preparation method is simple and environmentally friendly. The FAU type zeolite molecular sieve has prominent structural characteristics of micropore, mesopore, and macropore, has the advantages of large external surface, strong acidity, and good stability, and has a wide application prospect in fields such as detergent aid, hard water softening, catalyst, adsorbent, catalyst carrier, and the like.

Description

technical field [0001] The invention belongs to the technical field of synthesis of inorganic porous materials, and in particular relates to a low-cost, green and rapid preparation method of a multi-level porous FAU type zeolite molecular sieve with a "plug-in" structure. Background technique [0002] Faujasite type (FAU) molecular sieves have a three-dimensional twelve-membered ring channel structure, the pore diameter is about 0.74 nm, and the skeleton silicon-alumina ratio is relatively low, including X-type molecular sieves and Y-type molecular sieves. Among them, SiO 2 / Al 2 o 3 The ratio less than 3 is X-type molecular sieve, SiO 2 / Al 2 o 3 The ratio between 3 and 6 is Y-type molecular sieve. The low-silicon X-type molecular sieve knot has good ion exchange and adsorption capacity, and is an important industrial detergent additive and hard water softener. The high-silica Y-type molecular sieve is the most widely used fluidized catalytic cracking (fluidized catal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/22C01B39/24
CPCC01B39/22C01B39/24C01P2002/72C01P2002/80C01P2004/03C01P2004/34C01P2004/61C01P2004/62C01P2006/12C01P2006/17
Inventor 邹继兆刘丽佳王洪宾黄麟曾燮榕黎晓华姚跃超余良
Owner SHENZHEN UNIV
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