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Preparation method of trace rear earth ion-containing spherical MFI topological structured all-silicon molecular sieve catalyst and preparation method of caprolactam

A technology of all-silicon molecular sieve and rare earth ions, which is applied in the preparation of caprolactam and the preparation of spherical MFI topological structure all-silicon molecular sieve catalyst, achieving the effect of obvious cost advantage and low cost

Active Publication Date: 2019-06-04
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there have been no related literatures or patents on the rolling molding of all-silicon molecular sieves with MFI topological structure containing extremely small amounts of rare earth ions and then applied to the gas-phase Beckmann rearrangement reaction of cyclohexanone oxime.

Method used

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  • Preparation method of trace rear earth ion-containing spherical MFI topological structured all-silicon molecular sieve catalyst and preparation method of caprolactam
  • Preparation method of trace rear earth ion-containing spherical MFI topological structured all-silicon molecular sieve catalyst and preparation method of caprolactam

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preparation example Construction

[0062] A method for preparing a spherical MFI topological structure all-silicon molecular sieve catalyst containing a trace amount of rare earth ions, comprising the following steps:

[0063] a. Mix silicon source, rare earth ion source, organic template and water to obtain a colloidal mixture; wherein, SiO in the colloidal mixture 2 The molar ratio of organic template agent and water is 1:(0.05-0.50):(5-100); in terms of silicon dioxide, the mass ratio of silicon source to rare earth ions is (10000-200000):1.

[0064] b. The colloidal mixture is subjected to two-stage variable temperature hydrothermal crystallization to obtain a crystallized product.

[0065] c. Washing and separating the crystallized product to obtain an all-silicon molecular sieve with an MFI topological structure containing a trace amount of rare earth ions.

[0066] d. The MFI topological structure all-silicon molecular sieve is subjected to roll forming treatment, roasting treatment and post-treatment w...

Embodiment 1

[0098] This example is used to illustrate the preparation method of the spherical MFI topological structure all-silicon molecular sieve catalyst containing a very small amount of rare earth ions provided by the present invention.

[0099] With 208kg tetraethyl orthosilicate, 180kg22.5% by weight of tetrapropylammonium hydroxide, 7.3 grams of Ce (NO 3 ) 4 ·7H 2 O and 220kg of water are mixed, stirred at room temperature for 4 hours to form a colloidal mixture, and the molar ratio of the mixture is SiO 2 :TPAOH:H 2 O=1:0.2:20, SiO 2 with Ce 3+ The mass ratio of 30300:1, the above mixture was transferred to 1M 3 In a stainless steel reaction kettle, first hydrothermally crystallize at 60°C for 1 day, then hydrothermally crystallize at 120°C for 2 days, wash, filter, and dry at 120°C for 24 hours to obtain the all-silicon molecular sieve required for rolling molding in this example. Grind it into the required mesh size for roll forming on the pulverizer.

[0100] The all-si...

Embodiment 2

[0106] This example is used to illustrate the preparation method of the spherical all-silicon molecular sieve catalyst containing a very small amount of rare earth ions provided by the present invention.

[0107] With 208kg orthosilicate ethyl ester, the tetrapropyl ammonium hydroxide of 180kg22.5% by weight, 14 grams of Ce(NO 3 ) 3 ·6H 2 O and 220kg of water are mixed, stirred at room temperature for 3 hours to form a colloidal mixture, and the molar ratio of the mixture is SiO 2 :TPAOH:H 2 O=1:0.2:20, SiO 2 with Ce 3+ The mass ratio of 13500:1, the above mixture was transferred to 1M 3 In a stainless steel reaction kettle, first hydrothermally crystallize at 50°C for 1 day, then hydrothermally crystallize at 100°C for 2 days, wash, filter, and dry at 120°C for 24 hours to obtain the all-silicon molecular sieve required for rolling molding in this example. Grind it into the required mesh size for roll forming on the pulverizer.

[0108] The all-silicon molecular sieve ...

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Abstract

The invention relates to the field of all-silicon molecular sieves and discloses a preparation method of a trace rear earth ion-containing spherical MFI topological structured all-silicon molecular sieve catalyst and a preparation method of caprolactam. The preparation method of the spherical MFI topological structured all-silicon molecular sieve catalyst comprises the following steps: a, mixing asilicon source, a rare earth ion source, an organic template and water to obtain a colloid admixture; b, carrying out two-stage variable-temperature hydrothermal crystallization on the colloid admixture to obtain a crystallization product; c, washing the crystallization product and carrying out separation treatment to obtain rare earth ion-containing all-silicon molecular sieve; and d, moulding the rare earth ion-containing all-silicon molecular sieve, roasting and postprocessing with a nitrogen compound-containing alkaline buffer solution, washing, separating, and drying to obtain the spherical all-silicon molecular sieve catalyst containing trace rear earth ions. By the method, performance of the all-silicon molecular sieve catalyst can be changed effectively. By applying the catalyst to production of caprolactam, a good effect can be achieved.

Description

technical field [0001] The invention relates to the field of all-silicon molecular sieves, in particular to a preparation method of a spherical MFI topological structure all-silicon molecular sieve catalyst containing trace rare earth ions and a preparation method of caprolactam. Background technique [0002] The all-silicon molecular sieve with MFI topology was successfully synthesized for the first time in 1978 by E.M.Flanigen of UCC, etc., and belongs to the last member of the "Pentasil" family. All-silicon molecular sieve is an aluminum-free molecular sieve. 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. All-silicon molecular sieve has rich microporous structure and regular and uniform three-dimensional fine channels, and has a definite crystal structure of ZSM-5 molecular sieve, high internal specific surface area, good ther...

Claims

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Application Information

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IPC IPC(8): B01J29/035C07D201/04C07D223/10
CPCY02P20/52
Inventor 王松林沈飞王韩
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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