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Hierarchical pore ZSM-5 molecular sieve and synthetic method thereof

A technology of ZSM-5 and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., which can solve the problems of blocking molecular sieve channels, high synthesis cost, and reduced content of catalyst active components, etc. problem, to achieve high yield, reduce production cost, and high crystallinity

Inactive Publication Date: 2013-09-11
NINGXIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the synthetic 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 to make it shape 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 prepared monolithic catalysts, multi-step treatment or addition of special carriers is required in the synthesis process, complicated operating procedures, high synthesis costs, etc. are still difficulties that require customer service.

Method used

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  • Hierarchical pore ZSM-5 molecular sieve and synthetic method thereof
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  • Hierarchical pore ZSM-5 molecular sieve and synthetic method thereof

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Embodiment 1

[0039] (1) Using ethyl orthosilicate, tetrapropylammonium hydroxide (20%), and deionized water as starting materials, the molar ratio of preparation is 9TPAOH: 25SiO 2 : 480H 2O: 100EtOH synthesis solution, hydrothermally crystallized at 80°C for 6 hours, took out the crystallized product after cooling, and used it as a seed crystal gel for later use;

[0040] (2) Dissolve potassium hydroxide in deionized H 2 Prepare solution A in O, add weighed tetrapropylammonium hydroxide and aluminum isopropoxide into 30% solution A and stir for 2 hours to form solution B, add weighed ethyl orthosilicate slowly Rapidly stir in 30% solution A for 2 hours to form solution C;

[0041] (3) Add B to C and stir rapidly for 5 hours to form solution D;

[0042] (4) Add 0.483g cetyltrimethylammonium bromide (CTA) into 40% solution A, heat at 50°C for 1 hour, then add it into solution D and continue stirring for 1 hour to form a reaction mixture;

[0043] (5) The prepared seed crystal gel was ad...

Embodiment 2

[0046] In step (2) of the present embodiment, potassium hydroxide is dissolved in deionized H 2 Prepare solution A in O, add weighed tetrapropylammonium bromide and aluminum isopropoxide into 20% A solution and stir for 2 hours to form solution B, slowly add weighed tetrapropylammonium bromide 20% solution A was rapidly stirred for 2 hours to form solution C, and other steps were the same as in Example 1.

Embodiment 3

[0048] In step (2) of the present embodiment, potassium hydroxide is dissolved in deionized H 2 Solution A was formulated in O, and the weighed benzyltriethylammonium bromide and aluminum isopropoxide were added to 25% A solution and stirred for 2 hours to form solution B, and the weighed ethyl orthosilicate Slowly add 25% solution A and stir rapidly for 2 hours to form solution C. Other steps are the same as in Example 1.

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Abstract

The invention discloses a hierarchical pore ZSM-5 molecular sieve and a synthetic method thereof. The hierarchical pore ZSM-5 molecular sieve is formed by the accumulation of crystalline grains with order nano-layered structures and is integrally structured. The synthetic method comprises the following steps of: with quaternary ammonium salt as a structure-directing agent (SDA), tetraethoxysilane (TEOS) as a silicon source, aluminium isopropoxide (AIP) as an aluminum source, and potassium hydroxide (KOH) as an alkali source, adding a cationic surface active agent (CSF) to prepare a synthetic liquid with the molar ratio of (20-100) SiO2: (1-3) Al2O3: (10-30) SDA: (10-50) KOH: (1,000-3,000) H2O: (1-10) CSF; adding 10 to 20% of Silicalite-1 molecular sieve seed crystal gel; performing hydrothermal crystallization according to the conventional method; processing a product by washing, drying and roasting to obtain the ZSM-5 molecular sieve. The molecular sieve is an agglomeration which is formed by the self-assembly under mutual effect of CSF, seed crystal gel and an inorganic species and is of a lamella and hierarchical zeolite structure; the molecular sieve is relatively high in specific surface area, relatively short in a diffusion path and relatively high in stability. The preparation method also has the advantages of high degree of crystallinity, high yield and simple operation steps, and is easy to separate.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, in particular to a multi-level porous ZSM-5 molecular sieve with a monolithic nanosheet structure and a synthesis method thereof. 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
Inventor 王政邵秀丽安梅岳祥龙雷芳鱼婷姚军康年佩
Owner NINGXIA UNIVERSITY
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