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MFI topological structure silicon molecular sieve and its preparation method and application

A technology of silicon molecular sieve and molecular sieve, which is applied in the field of MFI topological structure silicon molecular sieve and its preparation, can solve the problems of high content of amorphous silicon oxide, poor relative crystallinity, large crystal particles, etc., achieve good catalytic performance and improve conversion rate , good catalytic performance

Active Publication Date: 2022-06-07
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The all-silicon molecular sieve synthesized in the prior art has more amorphous silicon oxide content, relatively poor crystallinity and large crystal particles

Method used

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  • MFI topological structure silicon molecular sieve and its preparation method and application
  • MFI topological structure silicon molecular sieve and its preparation method and application
  • MFI topological structure silicon molecular sieve and its preparation method and application

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preparation example Construction

[0037] A second aspect of the present invention provides a method for preparing a silicon molecular sieve with an MFI topology structure, the method comprising:

[0038] (1) mixing silicon source, organic amine, organic template agent, metal source, organic alcohol and water to obtain a colloidal mixture, wherein the molar ratio of the consumption of silicon source, organic amine, organic template agent, organic alcohol and water is 1:(0.05 -0.5): (0.05-0.5): (4-20): (5-100), the mass ratio of silicon source to metal source is (10000-200000): 1, the silicon source is SiO 2 The metal source is calculated as the metal element;

[0039] (2) The colloidal mixture is crystallized in a two-stage temperature-variable alcohol-hydrothermal system, and the conditions for crystallization of the two-stage temperature-variable alcohol-hydrothermal system include: crystallization at 40-70° C. for 0.5-5 days, and then Crystallize at 80-130°C for 0.5-5 days;

[0040] (3) the crystallization...

Embodiment approach

[0053] According to a specific embodiment of the present invention, the first mixing is performed under stirring conditions, and the stirring time is not particularly limited, as long as the ethanol, the organic amine and the organic template are uniformly mixed. Specifically, the method may further include, after adding the metal source and water, stirring, and then adding the ethyl orthosilicate.

specific Embodiment approach

[0054] According to a specific embodiment of the present invention, the method may further include: after adding ethyl orthosilicate, stirring to obtain the colloidal mixture. In the present invention, the stirring conditions are not particularly limited, as long as the colloidal mixture can be obtained. For example, it can be stirred at normal temperature (25°C) for 2-6 hours.

[0055] According to another preferred embodiment of the present invention, the silicon source is methyl orthosilicate, and the organic alcohol is methanol. The inventors of the present invention found in the research process that the combined use of methyl orthosilicate as a silicon source and methanol as an organic alcohol is more conducive to further improving the catalytic performance of the prepared molecular sieve. Preferably, the mixing in step (1) includes: mixing methanol, an organic amine and an organic template agent for a second time, then adding a metal source and water, and then adding m...

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Abstract

The invention relates to the field of silicon molecular sieves, and discloses a silicon molecular sieve with an MFI topological structure and its preparation method and application. The molecular sieve contains silicon elements, oxygen elements and metal elements. Based on the total amount of molecular sieves, the content of metal elements is 5 ‑100μg / g; the BET specific surface area of ​​the molecular sieve is 400‑500m 2 / g, the metal element is selected from at least one of transition metal elements and Group IIIA metal elements. In the preparation method provided by the present invention, alcohol and metal sources are additionally added during the synthesis process, organic amines and organic templates are added at the same time, and a two-stage temperature-variable alcohol-hydrothermal system is used for crystallization, which is very conducive to the entry of trace metal ions into molecular sieves framework, the prepared molecular sieve has good catalytic performance. Applying the molecular sieve provided by the invention as a catalyst in the production of caprolactam can improve the conversion rate of cyclohexanone oxime and the selectivity of caprolactam.

Description

technical field [0001] The invention relates to the field of silicon molecular sieves, in particular to a silicon molecular sieve with an MFI topology structure and a preparation method and application thereof. Background technique [0002] Silicalite-1 molecular sieve, also known as all-silicon, pure silicon molecular sieve, was successfully synthesized for the first time in 1978 by E.M. Flanigen of United Carbide Company, etc. It is one of the members of the "Pentasil" family. All-silicon molecular sieve is an aluminum-free molecular sieve with MFI topology. It is the simplest molecular sieve in the ZSM-5 molecular sieve family. Its skeleton only contains silicon atoms and oxygen atoms, and its basic structural unit is SiO. 4 tetrahedron. The all-silicon molecular sieve with MFI topology has abundant microporous structure and regular and uniform three-dimensional fine pore channels. Capability and other performance. The development and application of all-silicon molecul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/00C07D223/10C07D201/06
CPCC01B37/005C07D223/10C07D201/06Y02P20/52
Inventor 王松林沈飞王韩徐锦龙
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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