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Synthesis method of integral hierarchical-pore ZSM-5 molecular sieve

A synthesis method, ZSM-5 technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of reduced content of active components of catalysts, blockage of molecular sieve channels, complex operating procedures, etc., to achieve short Diffusion path, reduction of preparation cost, effect of large specific surface area

Inactive Publication Date: 2017-05-31
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] However, the synthesized nanosheet structure hierarchical porous ZSM-5 molecular sieve reported in the literature is a micron-sized powder, and it is necessary to add a binder or a surfactant to shape it or improve its strength.
The use of additives will block the pores of the molecular sieve, resulting in a reduction in the content of the active components of the catalyst, thereby reducing its catalytic performance
Although some researchers have also prepared monolithic catalysts, multi-step treatment or addition of special supports is required in the synthesis process, and there are still difficulties to be overcome such as complicated operating procedures and high synthesis costs.

Method used

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  • Synthesis method of integral hierarchical-pore ZSM-5 molecular sieve
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  • Synthesis method of integral hierarchical-pore ZSM-5 molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0036]A kind of synthetic method of monolithic hierarchical porous ZSM-5 molecular sieve, comprises the following steps:

[0037] (1) Add sodium metaaluminate, sodium hydroxide, tetrapropylammonium bromide (TPABr) and deionized water into the beaker and stir evenly, then gradually add sodium silicate into the beaker, stir vigorously to form a uniform gel, pour Put it into a polytetrafluoroethylene-lined stainless steel reactor for crystallization at 160°C for 3 days, and the molar composition of the product obtained (the aluminum source is represented by Al 2 o 3 In terms of sodium hydroxide as Na 2 Calculated as O, silicon source as SiO 2 Count) is n (Na 2 O) :n(SiO 2 ): n(TPABr):n(Al 2 o 3 ):n(H 2 O) = 10.5: 20: 20: 1: 5000;

[0038] (2) The product obtained in step (1) was repeatedly washed with deionized water until the pH value was close to neutral, and dried at 100°C to obtain a ZSM-5 molecular sieve;

[0039] (3) The ZSM-5 molecular sieve was calcined at 550° C...

Embodiment 2

[0041] A kind of synthetic method of monolithic hierarchical porous ZSM-5 molecular sieve, comprises the following steps:

[0042] (1) Add sodium metaaluminate, sodium hydroxide, tetrapropylammonium bromide (TPABr) and deionized water into the beaker and stir evenly, then gradually add tetraethyl orthosilicate into the beaker, stir vigorously to form a uniform gel , poured into a polytetrafluoroethylene-lined stainless steel reactor for crystallization at 150°C for 7 days, the molar composition of the product obtained (the aluminum source is represented by Al 2 o 3 In terms of sodium hydroxide as Na 2 Calculated as O, silicon source as SiO 2 Count) is n (Na 2 O):n(SiO 2 ): n(TPABr) :n(Al 2 o 3 ):n(H 2 O) = 10: 50: 20: 1: 1000;

[0043] (2) The product obtained in step (1) was repeatedly washed with deionized water until the pH value was close to neutral, and dried at 100°C to obtain a ZSM-5 molecular sieve;

[0044] (3) The ZSM-5 molecular sieve was calcined at 500° C...

Embodiment 3

[0046] A kind of synthetic method of monolithic hierarchical porous ZSM-5 molecular sieve, comprises the following steps:

[0047] (1) Add aluminum sulfate, sodium hydroxide, tetrapropylammonium hydroxide (TPAOH) and deionized water into a beaker and stir evenly, then gradually add silica sol into the beaker, stir vigorously to form a uniform gel, pour poly Crystallization at 150-180°C for 2-7 days in a stainless steel reactor lined with vinyl fluoride, the molar composition of the obtained product (the aluminum source is Al 2 o 3 In terms of sodium hydroxide as Na 2 Calculated as O, silicon source as SiO 2 Count) is n (Na 2 O) :n(SiO 2 ) :n(TPAOH) :n(Al 2 o 3 ):n(H 2 O) = 15: 100: 10: 1: 1500;

[0048] (2) The product obtained in step (1) was repeatedly washed with deionized water until the pH value was close to neutral, and dried at 100°C to obtain a ZSM-5 molecular sieve;

[0049] (3) The ZSM-5 molecular sieve was calcined at 650° C. for 4 hours in an oxygen atmosp...

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Abstract

The invention provides a synthesis method of an integral hierarchical-pore ZSM-5 molecular sieve. The synthesis method comprises the following steps that 1, an aluminum source, sodium hydroxide, an organic template agent and deionized water are added to a beaker (1) to be mixed evenly, then a silicon source is gradually added to the beaker, intense stirring is performed to form homogeneous gel, and the homogeneous gel is poured into a stainless steel reaction kettle with a polytetrafluoroethylene liner and is crystallized at the temperature of 100-220 DEG C for 1-7 days; 2, the product obtained in the step 1 is repeatedly washed with the deionized water till a pH value is approximately neutral, and drying is performed at the temperature of 90-110 DEG C to obtain a ZSM-5 molecular sieve; 3, the ZSM-5 molecular sieve is roasted, and the organic template agent is removed to obtain the integral hierarchical-pore ZSM-5 molecular sieve. The steps of an existing integral hierarchical-pore catalyst preparation technology are simplified, expensive auxiliary materials such as structure guiding agents and special integral carriers are not needed, and the preparation cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve preparation, and in particular relates to a method for synthesizing an integral multi-level porous ZSM-5 molecular sieve. Background technique [0002] U.S. Mobil Corporation reported the synthesis of ZSM-5 molecular sieve for the first time in 1972 (USP3702886), because of its ordered microporous structure, larger specific surface area, higher thermal and hydrothermal stability, skeleton acid center, It has become one of the most widely used catalysts in industry due to its excellent properties such as exchanged cations. However, the smaller micropore channels of the microporous ZSM-5 molecular sieve prevent larger molecules from entering the zeolite channels for adsorption and catalytic reactions, and limit the diffusion of macromolecules. In order to overcome the limitation of a single channel, researchers have considered solutions that combine the characteristics of channels at all le...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40B01J29/40
CPCC01B39/40B01J29/40C01P2002/72C01P2004/03C01P2006/12C01P2006/17
Inventor 郭泉辉袁世阳汤雁婷李娟马新起张锡兰李东风
Owner HENAN UNIVERSITY
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