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Hierarchical pore ZSM-5 molecular sieve with nanosheet layer structure and synthesis method thereof

A ZSM-5, nanosheet technology, applied in the field of molecular sieve synthesis, can solve the problems of complex preparation process, limited research field development and industrial application value, expensive synthesis raw materials, etc., and achieves simplified steps, high yield and reduced preparation cost. Effect

Inactive Publication Date: 2016-10-12
NINGXIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] It is worth pointing out that the synthetic raw materials required for the synthesis of the above various quaternary ammonium salt surfactants are expensive and the preparation process is complicated, thus limiting the development and industrial application value of this research field

Method used

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  • Hierarchical pore ZSM-5 molecular sieve with nanosheet layer structure and synthesis method thereof
  • Hierarchical pore ZSM-5 molecular sieve with nanosheet layer structure and synthesis method thereof
  • Hierarchical pore ZSM-5 molecular sieve with nanosheet layer structure and synthesis method thereof

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Experimental program
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Effect test

Embodiment 1

[0032] (1) Potassium hydroxide (0.939g) was dissolved in 36.166g deionized water to form solution A, and the weighed aluminum isopropoxide (0.274g) was added to part A solution (40% of the total mass) and stirred 2h to form solution B;

[0033] (2) Slowly add an appropriate amount of ethyl tetrasilicate (5.58g) dropwise into the solution of part A (30% of the total mass) and stir for 2 hours to form solution C;

[0034] (3) Add B to C and stir for 5 hours to form solution D;

[0035] (4) Add hexadecyltrimethylammonium bromide (0.488g) into part A solution (30% of the total mass), after stirring for 1-3h, add into D solution and continue stirring for 1h to form a reaction mixture, Hydrothermal crystallization at 175°C for 15 days;

[0036] (5) After the reaction, the sample was taken out, rinsed with a large amount of water, dried overnight at 120°C, and then baked in a muffle furnace at 550°C for 6 hours. The porous grade ZSM-5 molecular sieve with nanosheet structure can b...

Embodiment 2

[0039] (1) Potassium hydroxide (0.939g) was dissolved in 36.166g deionized water to form solution A, and the weighed pseudo-boehmite (0.247g) was added to part A solution (40% of the total mass) Stir for 4h to form solution B;

[0040] (2) Slowly add an appropriate amount of ethyl tetrasilicate (5.58g) dropwise into the solution of part A (30% of the total mass) and stir for 2 hours to form solution C;

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

[0042] (4) Hexadecyltrimethylammonium bromide (0.488g) was added to part A solution (30% of the total mass), stirred for 2h, then added to D solution and continued to stir for 1h to form a reaction mixture, at 175 Hydrothermal crystallization at ℃ for 15d;

[0043](5) After the reaction, the sample was taken out, rinsed with a large amount of water, dried overnight at 120°C, and then baked in a muffle furnace at 550°C for 6 hours. The porous grade ZSM-5 molecular sieve with nanosheet structure can be obtained....

Embodiment 3

[0045] (1) Dissolve potassium hydroxide (0.939g) in 36.166g deionized water to make solution A, add weighed aluminum powder (0.147g) to part A solution (40% of the total mass) and stir for 2h to form Solution B;

[0046] (2) Slowly add an appropriate amount of tetraethyl orthosilicate (5.58 g) dropwise into the solution of part A (30% of the total mass) and stir for 3 hours to form solution C;

[0047] (3) Add B to C and stir for 5 hours to form solution D;

[0048] (4) Hexadecyltrimethylammonium bromide (0.488g) was added to part A solution (30% of the total mass), stirred for 2h, then added to D solution and continued to stir for 1h to form a reaction mixture, at 175 Hydrothermal crystallization at ℃ for 15d;

[0049] (5) After the reaction, the sample was taken out, rinsed with a large amount of water, dried overnight at 120°C, and then baked in a muffle furnace at 550°C for 6 hours. The porous grade ZSM-5 molecular sieve with nanosheet structure can be obtained.

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Abstract

The invention discloses a hierarchical pore ZSM-5 molecular sieve with a nanosheet layer structure and a synthesis method thereof; the hierarchical pore ZSM-5 molecular sieve with the nanosheet layer structure is formed by cluster stacking of nanosheet layers with the thickness of 30 to 50 nm; an amphiphilic cationic surfactant is used as a structure directing agent, potassium hydroxide or sodium hydroxide is used as an alkali source, a synthesis solution with the molar ratio of (20-100)SiO2:(0.4-3)Al2O3:(10-50)ROH:(1000-3000)H2O:(1-10)SDA is prepared and then is subjected to hydrothermal crystallization according to a conventional method, and the product is washed, dried and roasted to obtain the ZSM-5 molecular sieve. The molecular sieve is the hierarchical pore ZSM-5 molecular sieve having the nanosheet layer structure and formed by self assembly of the amphiphilic cationic surfactant and an inorganic species through interaction, has the characteristics of large specific surface area, short diffusion path and good stability; and the preparation method has the advantages of high degree of crystallinity and simple operation.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, in particular to a nano sheet structure hierarchical porous ZSM-5 molecular sieve and a synthesis method thereof. Background technique [0002] Mobil Corporation of the United States first reported the synthesis of ZSM-5 molecular sieves in 1972, because of its ordered microporous structure, large specific surface area, high thermal and hydrothermal stability, skeleton acid centers, and exchangeable cations. It has become one of the most widely used catalysts in industry due to its excellent performance. However, the pores of most microporous ZSM-5 molecular sieves are smaller than 1nm, which makes the transport of molecules difficult. For reactions involving macromolecules, the catalyst is often easily inactivated due to surface area carbon or coking to block the pores, which limits its application range. Researchers generally believe that there are three main methods for obta...

Claims

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Application Information

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IPC IPC(8): C01B39/38B82Y40/00B01J29/40
CPCB01J29/40C01B39/38C01P2002/72C01P2004/03C01P2004/04C01P2004/20C01P2004/64
Inventor 王政宋智
Owner NINGXIA UNIVERSITY
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