Catalyst containing MFI topological structure silicon molecular sieve, preparation method and application thereof, and gas phase Beckmann rearrangement reaction method

A silicon molecular sieve and catalyst technology, applied in the field of catalyst preparation, can solve the problems of cyclohexanone oxime conversion rate, low caprolactam selectivity, low catalyst strength, low wear index and the like

Pending Publication Date: 2020-10-20
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to provide a catalyst containing silicon molecular sieve with MFI topological structure and its preparation method, application and A method for gas-phase Beckmann rearrangement reaction of cyclohexanone oxime, the catalyst has the characteristics of lower wear index, higher conversion rate of cyclohexanone oxime and higher caprolactam selectivity

Method used

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  • Catalyst containing MFI topological structure silicon molecular sieve, preparation method and application thereof, and gas phase Beckmann rearrangement reaction method
  • Catalyst containing MFI topological structure silicon molecular sieve, preparation method and application thereof, and gas phase Beckmann rearrangement reaction method
  • Catalyst containing MFI topological structure silicon molecular sieve, preparation method and application thereof, and gas phase Beckmann rearrangement reaction method

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specific Embodiment approach

[0040] According to the present invention, the molecular sieve also contains silicon element and oxygen element, and the present invention has a wide selection range for the content of silicon element and oxygen element in the molecular sieve. In a specific implementation mode, based on the total amount of molecular sieve, In the molecular sieve, the sum of the silicon element content, the oxygen element content and the metal element content is 100%.

[0041] In the present invention, metal elements whose ions have Lewis acid properties can be used in the present invention. Preferably, the metal elements are selected from at least one of transition metal elements, group IIA and group IVA elements.

[0042] According to the present invention, preferably, the transition metal element is at least one selected from Group IB, Group IIB, Group IVB, Group VB, Group VIB, Group VIIB and Group VIII.

Embodiment approach

[0043] According to a preferred embodiment of the present invention, the metal element is selected from Al, Ga, Ge, Ce, Ag, Co, Ni, Cu, Zn, Mn, Pd, Pt, Cr, Fe, Au, Ru, Rh, Pt , Rh, Ti, Zr, V, Mo and W elements at least one.

[0044] Still further preferably, the metal element has an ion valence state of +3 valence and / or an ion valence state of +4 valence. The inventors of the present invention found in the course of research that the use of metal elements with +3 valence and / or +4 valence is more conducive to metal elements entering the molecular sieve framework, and more conducive to charge balance.

[0045] According to the present invention, the metal element is further preferably at least one of Fe, Al, Ga, Cr, Ti, Zr and Ce elements. In this preferred embodiment, it is more beneficial to improve the performance of the catalyst, thereby improving the conversion rate of cyclohexanone oxime and the selectivity of caprolactam.

[0046] According to a preferred embodiment o...

Embodiment 1

[0128] Prepare catalyst according to the method provided by the invention, concrete steps are as follows:

[0129] (1) 482kg content is that the ethanol of 95% by weight and the tetrapropyl ammonium hydroxide aqueous solution that 302kg content is 22.5% by weight are added respectively to 2M 3 In the stainless steel reaction kettle, stir, then add 347kg orthosilicate ethyl ester, continue to stir, then add 332kg water and 38.6 grams of Fe(NO 3 ) 3 9H 2 O, continue stirring for 4 hours at room temperature to obtain a colloidal mixture; wherein, SiO 2 The molar ratio of ethyl orthosilicate: ethanol: tetrapropylammonium hydroxide: water is 1:10:0.2:20; 2 The weight ratio of tetraethyl orthosilicate in terms of metal elements to the metal source in terms of metal elements is 18666:1;

[0130] (2) The above-mentioned colloidal mixture is subjected to ethanol-hydrothermal system crystallization, and the conditions of the crystallization include: first crystallize at 70°C for 1 d...

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Abstract

The invention relates to the field of preparation of catalysts, and discloses a catalyst containing an MFI topological structure silicon molecular sieve, and a preparation method and application of the catalyst. The catalyst includes the molecular sieve and a binder; based on the dry basis weight of the catalyst, the content of the molecular sieve in the catalyst is 50-95 wt%, and the content of the binder is 5-50 wt% based on the dry basis weight; the molecular sieve contains metal elements, and ions of the metal elements have Lewis acid characteristics; and based on the total amount of the molecular sieve, the content of the metal elements in the molecular sieve is 5-100 [mu]g / g. The catalyst has the characteristics of low wear index, high cyclohexanone-oxime conversion rate and high caprolactam selectivity.

Description

technical field [0001] The invention relates to the field of preparation of catalysts, in particular to a catalyst containing silicon molecular sieve with MFI topological structure, its preparation method and application, and a method for gas-phase Beckmann rearrangement reaction of cyclohexanone oxime. Background technique [0002] Silicon molecular sieve is an aluminum-free molecular sieve with MFI topological structure. Silicon molecular sieve can be used as a material for membrane separation and as a catalyst for the gas-phase Beckmann rearrangement reaction of cyclohexanone oxime to produce caprolactam. However, the silicon molecular sieve synthesized in the prior art has a large content of amorphous silicon oxide, relatively poor crystallinity and large crystal particles. [0003] US4061724A discloses a silicon molecular sieve. Its preparation raw materials do not contain aluminum source, only silicon source, alkali source, template agent and water, which is different ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/035B01J35/02C01B39/48C07D201/04C07D223/10
CPCB01J29/0356B01J35/023B01J35/026B01J2229/183C01B39/48C01P2002/60C01P2002/72C01P2004/03C01P2004/04C07D201/04C07D223/10
Inventor 程时标何怡璇蒋肇斌胡志敏
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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