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Preparation method of house-of-cards-like hierarchical porous ZSM-5 molecular sieve

A ZSM-5, multi-level pore technology, applied in the field of preparation of inorganic porous materials, can solve the problems of unfavorable large-scale commercial production, complex and cumbersome process, high preparation cost, etc., and achieve rich channels, wide application prospects, and large external area Effect

Active Publication Date: 2015-01-07
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The preparation method of the above-mentioned multi-stage molecular sieve usually has problems such as high preparation cost, complex and cumbersome process, and serious environmental pollution, which is not conducive to large-scale commercial production.

Method used

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  • Preparation method of house-of-cards-like hierarchical porous ZSM-5 molecular sieve
  • Preparation method of house-of-cards-like hierarchical porous ZSM-5 molecular sieve
  • Preparation method of house-of-cards-like hierarchical porous ZSM-5 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Add 0.42g of aluminum sulfate octadecahydrate and 0.4g of sodium hydroxide to 9g of deionized water, stir until the solution becomes clear, then add 4g of deionized water and stir evenly;

[0032] (2) Add 2 g of N-methyl-2-pyrrolidone to the clear solution of step (1), and stir evenly;

[0033] (3) Slowly add 1.5g of white carbon black to the clarified solution of step (2), stir evenly, make dilute colloid;

[0034] (4) Evaporate the dilute colloid obtained in step (3) at 60°C for 4 hours with slight heating and stirring (the total mass is reduced by about 4g) to obtain a uniform wet gel;

[0035] (5) Put the wet gel obtained in step (4) into a hydrothermal reaction kettle, and crystallize at 140°C for 72 hours. After the crystallization is completed, the solid product is suction-filtered and washed, dried in an oven at 70°C under normal pressure for 24 hours, and then Calcined at 550°C in air for 5h (heating rate is 1°Cmin -1) to obtain 1.14g of "plug-in" type mu...

Embodiment 2

[0041] (1) Add 0.37g of aluminum sulfate octadecahydrate and 0.4g of sodium hydroxide into 10g of deionized water, stir until a clear solution is obtained, then add 6g of deionized water and stir evenly;

[0042] (2) Add 1 g of N-methyl-2-pyrrolidone to the clear solution of step (1), and stir evenly;

[0043] (3) Slowly add 1.5g of white carbon black to the clarified solution of step (2), stir evenly, make dilute colloid;

[0044] (4) Evaporate the dilute colloid obtained in step (3) with slight heating at 60°C for 6 hours (the total mass is reduced by about 6g) to obtain a uniform wet gel;

[0045] (5) Put the wet gel obtained in step (4) into a hydrothermal reaction kettle, and crystallize at 140°C for 72 hours. After the crystallization is completed, the solid product is suction-filtered and washed, dried in an oven at 70°C under normal pressure for 24 hours, and then Calcined at 500°C in air for 4h (heating rate is 1°Cmin -1 ) to obtain 1.10 g of "plug-in card" type mul...

Embodiment 3

[0047] (1) Add 0.42g of aluminum sulfate octadecahydrate and 0.4g of sodium hydroxide into 5.6g of deionized water, stir until the solution becomes clear, then add 4g of deionized water and stir evenly;

[0048] (2) Add 2 g of N-methyl-2-pyrrolidone to the clear solution of step (1), and stir evenly;

[0049] (3) Slowly add 5.4 g of silica sol (SiO 2 The mass percentage is 25~30%), stir evenly, make dilute colloid;

[0050] (4) Evaporate the dilute colloid obtained in step (3) with slight heating at 70°C for 2 hours (the total mass is reduced by about 4g) to obtain a uniform wet gel;

[0051] (5) Put the wet gel obtained in step (4) into a hydrothermal reaction kettle, and crystallize at 140°C for 60h. After the crystallization, the solid product is suction filtered and washed, dried in an oven at 70°C under normal pressure for 24h, and then Calcined at 550°C in air for 6h (heating rate is 1°Cmin -1 ), to obtain 1.21g of "plug-in card" type multi-stage porous ZSM-5 molecula...

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Abstract

The invention belongs to the technical field of synthesis of inorganic porous materials and particularly relates to a preparation method of a house-of-cards-like hierarchical porous ZSM-5 molecular sieve which is low in cost, environment-friendly and fast. The preparation method comprises the following steps: adding an inorganic alkali source and an aluminum source into deionized water, and adding a proper amount of N-methyl-2-pyrrolidone (NMP); then, slowly adding a silicon source; fully and uniformly stirring; and synthesizing a house-of-cards-like hierarchical porous HCL-ZSM-5 molecular sieve by a one-step hydrothermal method. The molecular sieve has remarkable hierarchical porous structural characteristics, is large in external surface area, strong in acidity and good in stability, and has wide application prospects in the fields of catalysis, adsorption, separation and the like. In an alkaline ZSM-5 synthetic system without an organic template, by using non-toxic and cheap NMP as a structural guiding agent which is used for replacing an expensive macromolecular organic template, the method is an economic, efficient and environment-friendly synthetic method which is expected to be applied to large-scale commercial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic porous materials, and in particular relates to a low-cost, green and rapid preparation method of a "card-inserting" type multi-stage pore ZSM-5 molecular sieve. Background technique [0002] In 1972, Mobil Corporation of the United States (USP3702886) reported for the first time a high-silicon molecular sieve with a three-dimensional straight pore structure——ZSM-5 zeolite molecular sieve. The unique and uniform pore structure endows it with good shape-selective catalytic effect and is widely used in petroleum Catalytic fields such as processing, coal chemical industry and fine chemical industry. [0003] However, the long and narrow micropores of ZSM-5 are not conducive to the rapid transport of macromolecules during the catalytic process, which often leads to many problems such as channel blockage, low catalytic efficiency, and catalyst deactivation. For this reason, people try ...

Claims

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Application Information

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IPC IPC(8): C01B39/40B82Y40/00B82Y30/00
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/64C01P2006/17
Inventor 张宗弢王润伟刘丽佳王洪宾
Owner JILIN UNIV
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