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Nano MFI-type molecular sieve with hierarchical pore structure and preparation method and application thereof

A technology of nano-molecular sieve and molecular sieve, which is applied in the direction of molecular sieve catalysts, nanotechnology, chemical instruments and methods, etc. It can solve the problems of complex preparation of nano-MFI zeolite, low yield of nano-molecular sieve, and restrictions on wide-scale application, and achieve high propylene yield. The effect of catalyst stability, easy separation, and high hydrothermal stability

Active Publication Date: 2013-12-18
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, compared with the synthesis of conventional micron-sized MFI molecular sieves, the preparation of nano-MFI zeolites is a very complicated process
Usually, the synthesized nanocrystals are suspended in the mother liquor, and these nano-zeolites must be separated by high-speed centrifugation, which is very difficult for large-scale industrial preparation, and the nano-molecular sieves obtained by high-speed centrifugation low rate
In particular, nanomolecular sieve crystals have high activity and poor hydrothermal stability due to their large outer surface.
The above two points restrict its wide-scale application

Method used

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  • Nano MFI-type molecular sieve with hierarchical pore structure and preparation method and application thereof
  • Nano MFI-type molecular sieve with hierarchical pore structure and preparation method and application thereof
  • Nano MFI-type molecular sieve with hierarchical pore structure and preparation method and application thereof

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Embodiment 1

[0034] In this embodiment, the preparation method of high hydrothermal stability, easy separation, nano ZSM-5 type zeolite molecular sieve:

[0035] First, prepare a mother liquor containing nano-sized ZSM-5 molecular sieve: mix ethyl orthosilicate, tetrapropylammonium hydroxide, sodium metaaluminate, and deionized water in a molar ratio of 1:0.32:0.02:29, After complete hydrolysis of ethyl acetate, the above solution was placed in a reaction kettle for hydrothermal synthesis, and hydrothermal synthesis was performed at 130° C. for 6 hours to obtain a mother liquid of nano ZSM-5 molecular sieve. Add polybenzamide to the above-mentioned molecular sieve mother liquor (the amount of polybenzamide added is 5% of the mass of the molecular sieve mother liquor), stir at 12,000 rpm for 2 hours, then add to the reaction kettle, and conduct hydrothermal synthesis at 160°C for 6 hours, Made nano ZSM-5 molecular sieve compound. The obtained molecular sieve composite was filtered through ...

Embodiment 2

[0042] In this embodiment, the preparation method of high hydrothermal stability, easy separation, nano ZSM-5 type zeolite molecular sieve:

[0043] First, prepare a mother liquor containing nano-ZSM-5 molecular sieve: mix ethyl orthosilicate, tetrapropylammonium hydroxide, sodium metaaluminate, and deionized water in a molar ratio of 1:0.32:0.02:29, and wait for orthosilicate After complete hydrolysis of the ethyl ester, the above solution was placed in a reaction kettle for hydrothermal synthesis, and the hydrothermal synthesis was performed at 130° C. for 6 hours to obtain the nano ZSM-5 molecular sieve mother liquid. Add polydiallyldimethylammonium chloride (the amount of polydiallyldimethylammonium chloride is 7.5% of the mass of the molecular sieve mother liquor) to the above molecular sieve mother liquor, and stir at a high speed of 12000 rpm for 2 hours Afterwards, it was added to a reaction kettle, and was hydrothermally synthesized at 130° C. for 12 hours to make a n...

Embodiment 3

[0046] In this embodiment, the preparation method of high hydrothermal stability, easy separation, nano ZSM-5 type zeolite molecular sieve:

[0047] First, prepare a mother liquor containing nano-ZSM-5 molecular sieve: mix ethyl orthosilicate, tetrapropylammonium hydroxide, sodium metaaluminate, and deionized water in a molar ratio of 1:0.32:0.02:29, and wait for orthosilicate After complete hydrolysis of ethyl ester, the above molecular sieve mother liquor was placed in a reaction kettle for hydrothermal synthesis, and hydrothermal synthesis was carried out at 130° C. for 6 hours to obtain nano ZSM-5 molecular sieve mother liquor. Add cetyltrimethylammonium bromide to the above solution (the amount of cetyltrimethylammonium bromide is 3% of the mass of the molecular sieve mother liquor), stir at a high speed at 12000 rpm for 2 hours, then add Reactor, at 120°C, hydrothermally synthesized for 24 hours to make nano ZSM-5 molecular sieve composite. The obtained molecular sieve ...

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Abstract

The invention belongs to the technical field of a catalyst and an application thereof, and particularly relates to a nano MFI-type molecular sieve which is easy to separate and has high hydrothermal stability and a hierarchical pore channel structure, and a preparation method and application thereof. The method comprises the following steps: (1) selecting a prepared nano MFI-type molecular sieve suspension as a mother liquid; (2) adding a cationic flocculant into the mother liquid to assemble the nano molecular sieve; (3) putting the assembled nano molecular sieve into a reaction kettle for hydrothermal synthesis to obtain a nano molecular sieve compound with a block size of 100 nanometers to 100 microns. The nano molecular sieve compound is subjected to conventional filtering, washing, drying and roasting to obtain the nano MFI-type molecular sieve with a hierarchical pore channel structure. The nano MFI-type molecular sieve prepared by the method can be separated through a filtering operation and has the advantages of open intercrystalline pore channel structure, large pore volume, high crystallization rate and high hydrothermal stability; in a methanol-to-propylene reaction, the nano MFI-type molecular sieve shows higher propylene yield and stability than the nano MFI-type molecular sieve prepared by a conventional method.

Description

technical field [0001] The invention belongs to the technical field of catalysts and their applications, and in particular relates to a nano MFI zeolite molecular sieve with easy separation, high hydrothermal stability and multi-level pore structure, a preparation method thereof and its application in methanol to propylene. Background technique [0002] MFI type zeolite molecular sieve is a kind of high silicon microporous zeolite developed by Mobil in the 1970s. It has regular pores, adjustable acidity and good shape selectivity. It is widely used as a solid acid catalyst in the field of petrochemical industry. [0003] At present, most of the MFI molecular sieve catalysts used in industry are large-grained MFI molecular sieves with a size of several microns. Due to the narrow and long channels of MFI molecular sieves and the large grain size, the diffusion resistance of macromolecules in the crystal is relatively high, and carbon deposits are easily generated, resulting in...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J29/89B01J29/03B82Y40/00C07C11/06C07C1/20
CPCY02P20/52
Inventor 张劲松矫义来杨振明
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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