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ZSM-5 hybrid nanosheet molecular sieve with medium silica-alumina ratio and preparation method thereof

A technology of ZSM-5 and nanosheets, applied in molecular sieve catalysts, nanotechnology, nanotechnology, etc., can solve problems such as limiting applications and hindering the growth of nanosheets

Pending Publication Date: 2022-02-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the presence of aluminum hinders the growth of nanosheets
At present, the dual-template method can only synthesize ZSM-5 hybrid nanosheet molecular sieves with a silicon-aluminum ratio higher than 300, which greatly limits its application in acid-catalyzed reactions.

Method used

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  • ZSM-5 hybrid nanosheet molecular sieve with medium silica-alumina ratio and preparation method thereof
  • ZSM-5 hybrid nanosheet molecular sieve with medium silica-alumina ratio and preparation method thereof
  • ZSM-5 hybrid nanosheet molecular sieve with medium silica-alumina ratio and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 4

[0038] The SEM picture of embodiment 4 is as Figure 4 shown. From Figure 4 It can be seen from the figure that the epitaxial growth of hybrid molecular sieve nanosheets still maintains the morphology, but there are some catalysts with only internal block structures, and no particles covering the outer nanosheets. Compared with Example 1, the adjustment of water volume will To affect the morphology of hybrid molecular sieves, only by reasonably adjusting the amount of water and the ratio of silicon to aluminum to form a balance can ensure that the long carbon chain quaternary ammonium salt template exists in the amphiphilic equilibrium solution, that is, the formed mixed gel will not appear after standing for half an hour Only by delamination phenomenon can a complete hybrid molecular sieve be synthesized.

[0039] [Examples 6-8] Weighed 5.105g of tetrapropylammonium hydroxide, 5.832g of tetraethyl orthosilicate, and 0.078g of aluminum sulfate octadecahydrate to prepare a m...

Embodiment 6

[0041] The SEM picture of embodiment 6 is as Figure 5 As shown, the morphology of the hybrid molecular sieve does not have much influence. Compared with Example 1, it can be seen that the aging temperature and time in the synthesis have little effect on the morphology of the hybrid nanosheet molecular sieve.

[0042] [Examples 9-11] Weighed 5.105g of tetrapropylammonium hydroxide, 5.832g of tetraethyl orthosilicate, and 0.078g of aluminum sulfate octadecahydrate to prepare a mixed solution, and stirred the mixed solution at 60°C for 3h to obtain Aging gel. Then 0.610g long carbon chain surfactant C 22 h 45 -N + Br - (CH 3 ) 2 -C 6 h 12 -N + Br - (CH 3 ) 2 -C 6 h 13 Prepare a mixed solution with 9.6g of water, add it to the aging gel, stir the mixed solution at 60°C for 2h, transfer it to a crystallization kettle, and carry out hydrothermal crystallization at 130°C with a stirring speed of 30rmp for 5d. The sample was washed with deionized water until neutral, d...

Embodiment 9

[0044] The SEM picture of embodiment 9 is as Figure 6 As shown, compared with Example 1, the crystallization time has no obvious effect on the morphology of the hybrid molecular sieve, and the hybrid nanosheet molecular sieve can be synthesized under the crystallization conditions of the present invention.

[0045] [Examples 12-15] Weighed 4.534g of tetrapropylammonium hydroxide, 5.832g of tetraethyl orthosilicate, and 0.078g of aluminum sulfate octadecahydrate to prepare a mixed solution, and stirred the mixed solution at 60°C for 3h Get aging gel. Then 0.610g long carbon chain quaternary ammonium salt surfactant C 22 h 45 -N + Br - (CH 3 ) 2 -C 6 h 12 -N + Br - (CH 3 ) 2 -C 6 h 13 Prepare a mixed solution with 9.6g of water, add it to the aging gel, stir the mixed solution at 60°C for 2h, transfer it to a crystallization kettle, and carry out hydrothermal crystallization at 150°C with a stirring speed of 30rmp for 5d. The sample was washed with deionized wate...

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Abstract

The invention discloses a ZSM-5 hybrid nanosheet molecular sieve with a medium silica-alumina ratio and a preparation method thereof, and belongs to the technical field of catalysts. The hybrid molecular sieve is composed of an internal microporous substrate and a nanosheet layer epitaxially growing outside the microporous substrate, the silica-alumina ratio range of the hybrid molecular sieve is adjustable in a range of 100-300, and the preparation method specifically comprises the following steps: 1) dissolving a micromolecule template agent, a silicon source and an aluminum source in water, and uniformly stirring to form gel; 2) aging under a stirring condition; (3) continuously adding a long-carbon-chain amphiphilic surfactant solution and uniformly stirring; 4) aging under the stirring condition; and 5) crystallizing to obtain the hybrid ZSM-5 molecular sieve. The preparation method solves the problem that the morphology of the molecular sieve is limited by the silica-alumina ratio of the nanosheet-block hybrid molecular sieve synthesized at the present stage, and breaks through the limitation that the growth of the outer nanosheet cannot be maintained if the silica-alumina ratio is reduced, and the prepared hybrid molecular sieve has great application prospects in the catalytic fields of preparation of low-carbon olefins and the like.

Description

technical field [0001] The invention belongs to the field of catalysts, and particularly relates to a ZSM-5 hybrid nanosheet molecular sieve with a medium silicon-aluminum ratio and a preparation method thereof. The molecular sieve can be used as a catalyst for the preparation of low-carbon olefins, and has good low-carbon olefin selectivity and resistance Carbon deposition performance. Background technique [0002] Hierarchical molecular sieves combine the acid catalytic performance of microporous molecular sieves with the diffusion and mass transfer characteristics of mesopores or macropores. The introduction of mesopores improves the coking resistance of traditional microporous catalysts, making them widely used in the chemical industry prospect. The key to synthesizing hierarchically porous molecular sieves with good catalytic performance lies in the balance between acid catalytic function and mesopore size. [0003] At present, the methods for synthesizing hierarchica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40B01J29/40B01J37/10C07C4/06C07C11/04C07C11/06B82Y30/00B82Y40/00
CPCC01B39/40B82Y30/00B82Y40/00B01J29/40B01J37/10C07C4/06C01P2004/64C01P2004/20C01P2004/30C01P2004/50C01P2004/03C01P2004/04C01P2002/72C01P2006/12C01P2006/14B01J35/40C07C11/04C07C11/06Y02P20/52
Inventor 程党国郝靓陈丰秋詹晓力
Owner ZHEJIANG UNIV
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