MFI topological structure silicon molecular sieve as well as preparation method and application thereof

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 , Improve the effect of economy

Active Publication Date: 2021-01-19
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

Method used

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  • MFI topological structure silicon molecular sieve as well as preparation method and application thereof
  • MFI topological structure silicon molecular sieve as well as preparation method and application thereof
  • MFI topological structure silicon molecular sieve as well as preparation method and application thereof

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Example Embodiment

[0037]The 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) Mix the silicon source, organic amine, organic template, metal source, organic alcohol and water to obtain a colloidal mixture, wherein the molar ratio of silicon source, organic amine, organic template, organic alcohol and water is 1:(0.05 -0.5): (0.05-0.5): (4-20): (5-100), the amount-mass ratio of silicon source to metal source is (10000-200000):1, silicon source is SiO2Calculated, the metal source is calculated as the metal element;

[0039](2) The colloidal mixture is subjected to two-stage temperature-changing alcohol-hydrothermal system crystallization, and the conditions for the two-stage temperature-changing alcohol-hydrothermal system crystallization include: crystallization at 40-70°C for 0.5-5 days, then Crystallize at 80-130℃ for 0.5-5 days;

[0040](3) filtering, drying and roasting the crystallization moth...

Example Embodiment

[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, organic amine and organic template are mixed uniformly. Specifically, the method may further include, after adding the metal source and water, stirring, and then adding the ethyl orthosilicate.

Example Embodiment

[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, there is no particular limitation on the stirring conditions, as long as the colloidal mixture can be obtained. For example, it can be stirred at room 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 inventor of the present invention discovered during the research 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: performing a second mixing of methanol, organic amine and organic template, then adding the metal source and water, and then adding methyl ortho...

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Abstract

The invention relates to the field of silicon molecular sieves, and discloses an MFI topological structure silicon molecular sieve as well as a preparation method and application thereof. The molecular sieve contains a silicon element, an oxygen element and a metal element, and based on the total amount of the molecular sieve, the content of the metal element is 5-100 [mu]g/g; the BET specific surface area of the molecular sieve is 400-500 m<2>/g, and the metal element is selected from at least one of transition metal elements and IIIA group metal elements. According to the preparation methodprovided by the invention, alcohol and a metal source are additionally added in the synthesis process, organic amine and an organic template agent are added at the same time, and a two-stage variable-temperature alcohol-hydrothermal system is adopted for crystallization, so that a trace amount of metal ions can enter a molecular sieve skeleton favorably, and the prepared molecular sieve is good incatalytic performance. When the molecular sieve provided by the invention is applied to caprolactam production as a catalyst, the conversion rate of cyclohexanone-oxime and the selectivity of caprolactam can be improved.

Description

technical field [0001] The invention relates to the field of silicon molecular sieves, in particular to silicon molecular sieves with an MFI topological structure and a preparation method and application thereof. Background technique [0002] Silicalite-1 molecular sieve, also known as all-silicon and pure silicon molecular sieve, was successfully synthesized for the first time in 1978 by E.M.Flanigen of Union Carbide Corporation of the United States, and belongs to one of the members of the "Pentasil" family. All-silicon molecular sieve is an aluminum-free molecular sieve with MFI topological structure. It is the simplest molecular sieve in the ZSM-5 structural molecular sieve family. Its skeleton only contains silicon atoms and oxygen atoms, and the basic structural unit is SiO 4 tetrahedron. The all-silicon molecular sieve with MFI topological structure has rich microporous structure and regular and uniform three-dimensional fine pores, has a definite crystal structure o...

Claims

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Application Information

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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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