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Preparation of binderless MFI/FAU composite zeolite molecular sieve

A composite molecular sieve and zeolite molecular sieve technology is applied in the field of preparation of a binder-free MFI/FAU composite zeolite molecular sieve, which can solve the problems of decreasing adsorption capacity, reducing the content of effective components, single zeolite molecular sieve with single pore size, etc.

Active Publication Date: 2011-08-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that a single zeolite molecular sieve has a single pore size, and there is a diffusion limit for some molecules, which is limited in the application of adsorption and catalysis, and the inert binder added in the molding process of the zeolite molecular sieve in the past will reduce the effective composition. The content of the component will cause the decrease of the adsorption capacity and the reduction of the effective surface area. A new method for preparing the binder-free MFI / FAU composite zeolite molecular sieve is provided.

Method used

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  • Preparation of binderless MFI/FAU composite zeolite molecular sieve
  • Preparation of binderless MFI/FAU composite zeolite molecular sieve
  • Preparation of binderless MFI/FAU composite zeolite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～2

[0015] Use tetrapropylammonium hydroxide (TPAOH) solution, tetraethylorthosilicate (TEOS) and water according to (TPA) 2 O: 5.5TEOS: 90H 2 The molar ratio of O was mixed and stirred evenly, aged and refluxed at 80° C. for three days to obtain the MFI seed crystal directing agent.

[0016] Weigh 30 grams of white carbon black and 70 grams of ultra-stable Y zeolite (USY, SiO 2 / Al 2 o 3 Molar ratio is 12), add the MFI seed crystal directing agent of 20 grams, add the silica sol (SiO 2 The mass percentage is 40%) for kneading and forming.

[0017] 16 grams of triethylamine, 9 grams of ethylenediamine and 5 grams of distilled water were added to the reaction kettle in advance, and 60 grams of the cylindrical product prepared above was placed in the reaction kettle and sealed above the porous stainless steel mesh, and then the gas-solid phase was carried out at 160 ° C. 3 days, 5 days of treatment. After the product was taken out, it was washed with distilled water, dried in ...

Embodiment 3

[0020] Weigh 80 grams of white carbon black and 20 grams of ultra-stable Y zeolite (USY, SiO 2 / Al 2 o 3 Molar ratio is 12), add the ZSM-5 seed crystal directing agent of 20 grams prepared in embodiment 1, add the silica sol (SiO 2 The mass percentage is 40%) for kneading and forming.

[0021] 24 grams of ethylenediamine and 5 grams of distilled water were pre-added into the reaction kettle, and 60 grams of the above-prepared cylindrical product was placed in the reaction kettle above the porous stainless steel mesh and sealed, and gas-solid phase treatment was carried out at 180 ° C for 5 days. After the product was taken out, it was washed with distilled water, dried in the air and then calcined at 550°C in an air atmosphere.

[0022] The XRD pattern of the product treated for 5 days shows that the diffraction peak of Y zeolite molecular sieve is very small, and its main diffraction peak is much smaller than that of MFI zeolite molecular sieve, indicating that the product...

Embodiment 4～6

[0024] Take by weighing 120 grams of white carbon black and 120 grams of NaY zeolite (SiO 2 / Al 2 o 3 Molar ratio is 4.5) mixes the MFI seed directing agent prepared in the embodiment 1 of 40 grams, adds the Al containing 54.4 grams 2 (SO 4 ) 3 18H 2 The aqueous solution of O adjusts the silicon-aluminum ratio of the mixture, and then adds 190 grams of silica sol (SiO 2 The mass percentage is 40%) for kneading and forming.

[0025]A mixture of 24 grams of ethylamine and 3 grams of distilled water was added to the reaction kettle in advance, and 20 grams of the above-prepared cylindrical products were placed in the reaction kettle above the porous stainless steel mesh and sealed, and then gas-solid phase treatment was carried out at 150°C respectively 3, 5 ,7 days. After the product was taken out, it was washed with distilled water, dried in the air and then calcined at 550°C in an air atmosphere.

[0026] The XRD patterns of the products of the three examples all conta...

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Abstract

The invention relates to a method for preparing a no-binding agent MFI / FAU compound zeolite molecular sieve, which mainly aims at overcoming the defects of difficult recovery, easy deactivation and easy aggregation existing in the practical application of the zeolite molecular sieve powder. During the forming process of the conventional zeolite molecular sieve, the binding agent needs to be added, which causes the negative effects of small effective surface area and limited diffusion, etc. and the problem that the single zeolite molecular sieve, in catalysis and adsorption fields, limits the diffusion and the adsorption of the compounds, the sizes of which exceed the sieve pore diameter range. In the invention, silicon-aluminum materials are mixed with the FAU compound zeolite molecular sieve first, and the silicon-aluminum materials which sieved out by the FAU compound zeolite molecular sieve are selectively converted to the MFI zeolite molecular sieve which forms the no-binding agent MFI / FAU compound zeolite molecular sieve. The technical proposal of the invention better resolves the technical problems, and can be applied to the industrial production of the MFI / FAU compound zeolite molecular sieve.

Description

technical field [0001] The invention relates to a method for preparing a binder-free MFI / FAU composite zeolite molecular sieve, in particular to a method for mixing silicon-aluminum raw materials with FAU zeolite molecular sieves for kneading and molding, and then converting the silicon-aluminum raw materials by gas-solid phase treatment to form a A binder-free MFI / FAU composite zeolite molecular sieve method. Background technique [0002] Zeolite molecular sieves have uniform and ordered micropores, large specific surface area, and high hydrothermal stability, and are widely used in the field of catalysis. Due to the small particle size, zeolite powder is not very convenient in practical application, and has weaknesses such as difficult recovery, easy deactivation and aggregation, so it needs to be shaped in advance. Binders are generally required during the molding process, resulting in a reduction in the effective surface area and introducing diffusion limitations. Bind...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/00
Inventor 王德举刘仲能李学礼汪哲明
Owner CHINA PETROLEUM & CHEM CORP