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Method of preparing macroporous/mesoporous zeolite molecular sieve through seed crystal induction

A technology of mesoporous zeolite and molecular sieve, applied in the field of zeolite molecular sieve and its preparation, can solve problems such as large diffusion resistance, and achieve the effects of simple method, simple process and wide adaptability

Inactive Publication Date: 2018-01-30
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the problem of large diffusion resistance in the pores of existing microporous zeolite molecular sieves, and provide a method for preparing large / mesoporous zeolite molecular sieves induced by crystal seeds, which can adjust the silicon-aluminum ratio in a wide range, It can adapt to the preparation of various molecular sieves, and the obtained products have a large number of mesopores and macropores, high purity, high crystallinity, and controllable meso / macropore structure, which can be used as high-performance catalysts and adsorbents

Method used

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  • Method of preparing macroporous/mesoporous zeolite molecular sieve through seed crystal induction
  • Method of preparing macroporous/mesoporous zeolite molecular sieve through seed crystal induction
  • Method of preparing macroporous/mesoporous zeolite molecular sieve through seed crystal induction

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Experimental program
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Effect test

Embodiment 1

[0069] Add 51.6 g of 25% tetrapropylammonium hydroxide solution and ethyl orthosilicate into a round-bottomed flask containing deionized water and stir for 2 h, so that the molar ratio of the mixed solution is SiO 2 :TPAOH:H 2 O: EtOH=92:25:900:368 (EtOH comes from the hydrolysis reaction of tetraethyl orthosilicate and water), and then the mixture was heated to 100°C for 48 h to obtain ZSM-5 molecular sieve seeds . Then the above-mentioned ZSM-5 molecular sieve seed crystals (calculated based on silica) were mixed with NaOH, 29g 40wt% silica sol (based on SiO 2 to calculate), NaAlO 2 Mix and stir with deionized water at a molar ratio of 2.5:3.5:60:4:2500 for 1 hour, so that all raw materials are mixed uniformly, then add it to a sealed high-pressure hydrothermal crystallization kettle, and crystallize at 180°C for 48 h . After the hydrothermal kettle was cooled to normal temperature, the product was taken out and filtered, washed repeatedly, dried at 110°C for 12 hours, a...

Embodiment 2

[0072] Add 32.3 g of tetrapropylammonium hydroxide solution and ethyl orthosilicate with a mass fraction of 40% into a round-bottomed flask containing deionized water and stir for 2 h, so that the molar ratio of the mixed solution is SiO 2 :TPAOH:H 2 O: EtOH=92:50:900:368 (EtOH comes from the hydrolysis reaction of tetraethyl orthosilicate and water), and then the mixture was heated to 100°C for 48 h to obtain ZSM-5 molecular sieve seeds . Then the above-mentioned ZSM-5 molecular sieve seed crystals (calculated based on silica) were mixed with NaOH, 29g 40wt% silica sol (based on SiO 2 to calculate), NaAlO 2 Mix and stir with deionized water at a molar ratio of 0.5:3.5:60:4:2500 for 1 hour, so that all raw materials are mixed uniformly, and then add it into a sealed high-pressure hydrothermal crystallization kettle, and crystallize at 180 °C for 48 h . After the hydrothermal kettle was cooled to normal temperature, the product was taken out and filtered, washed repeatedly,...

Embodiment 3

[0075] Add 51.6 g of 25% tetrapropylammonium hydroxide solution and ethyl orthosilicate into a round-bottomed flask containing deionized water and stir for 2 h, so that the molar ratio of the mixed solution is SiO 2 :TPAOH:H 2 O: EtOH=92:50:900:368 (EtOH comes from the hydrolysis reaction of tetraethyl orthosilicate and water), and then the mixture was heated to 120°C for 24 h to obtain ZSM-5 molecular sieve seeds . Then the above-mentioned ZSM-5 molecular sieve seed crystals (calculated based on silica) were mixed with NaOH, 29g 40wt% silica sol (based on SiO 2 to calculate), NaAlO 2 Mix and stir with deionized water at a molar ratio of 2.5:5.5:60:2:2500 for 1 hour, so that all raw materials are mixed uniformly, then add it into a sealed high-pressure hydrothermal crystallization kettle, and crystallize at 180 °C for 48 h . After the hydrothermal kettle was cooled to normal temperature, the product was taken out and filtered, washed repeatedly, dried at 110°C for 12 hours...

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Abstract

The invention discloses a method of preparing macroporous / mesoporous zeolite molecular sieve through seed crystal induction. The method includes: using an organic template plate to prepare zeolite molecular sieve seed crystal; adding a small amount of the seed crystal into synthesis liquid of a zeolite molecular sieve, and performing simple high-temperature hydrothermal crystallization to obtain the mesoporous / macroporous zeolite molecular sieve uniform in size. The macroporous / mesoporous zeolite molecular sieve prepared by the method is formed by self-assembling zeolite molecular sieve nanorods or nanoparticles of 5-500nm, and rich mesoporous / macroporous pores exist among the zeolite molecular sieve nanorods or nanoparticles. The method is simple, safe and suitable for ZSM-5, ZSM-11, beta-type or TS-1 molecular sieves. The method is simple and safe, and the macroporous / mesoporous zeolite molecular sieve is high in purity and crystallinity, controllable in mesoporous / macroporous structure and suitable for serving as a membrane separation material or a catalyst for catalytic reaction.

Description

technical field [0001] The invention relates to the field of zeolite molecular sieves and preparation thereof, in particular to a method for preparing large / mesoporous zeolite molecular sieves induced by crystal seeds. Background technique [0002] Molecular sieve is a kind of crystalline aluminosilicate, which has a pore structure that runs through the crystal, and the pore size is at the molecular scale. Molecular sieves have the advantages of high specific surface area, high thermal and hydrothermal stability, easily adjustable acidity and regular skeleton structure, so they are widely used in many fields such as heterogeneous catalysis, ion exchange, adsorption and separation (Corma A. , Chem. Rev. , 1997, 97, 2373-2420, Cundy CS, Cox PA, Chem. Rev. , 2003, 103, 663-701). There are many types of molecular sieves, and different types of molecular sieves have different skeletons and pore structures. According to the pore size of porous materials, the International Unio...

Claims

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Application Information

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IPC IPC(8): C01B39/40B01J20/18B01J20/30B01J29/04B01J29/40B01J29/70B01J29/89
Inventor 沈葵曹永海李映伟李致贤
Owner SOUTH CHINA UNIV OF TECH
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