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Preparation method for Silicate-1 molecular sieve catalyst, catalyst and method for preparing caprolactam

A molecular sieve and catalyst technology, which is used in the preparation of Silicate-1 molecular sieve catalyst and the field of catalyst and caprolactam preparation, to achieve the effects of improving conversion rate, fine particle size and good crushing strength

Active Publication Date: 2017-11-10
CHINA PETROLEUM & CHEM CORP +1
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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 extruding ZSM-5 molecular sieves containing extremely small or trace amounts of metal ions for extrusion molding, tablet molding, and rotational molding, and then applying them to the gas phase Beckmann rearrangement reaction of cyclohexanone oxime.

Method used

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  • Preparation method for Silicate-1 molecular sieve catalyst, catalyst and method for preparing caprolactam
  • Preparation method for Silicate-1 molecular sieve catalyst, catalyst and method for preparing caprolactam
  • Preparation method for Silicate-1 molecular sieve catalyst, catalyst and method for preparing caprolactam

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preparation example Construction

[0053] The first aspect of the present invention: provide a kind of preparation method of the Silicate-1 molecular sieve catalyst containing trace metal ion, this method comprises: a, silicon source, metal ion source, organic templating agent and water are mixed, obtain colloidal mixture, wherein, In molar ratio, SiO in the colloidal mixture 2 : organic templating agent: H 2 O=1: (0.05-0.50): (5-100), preferably SiO 2 : organic templating agent: H 2 O=1: (0.15-0.25): (10-50); the mass ratio of silicon oxide to metal ions is (5000-200000): 1, preferably, the mass ratio of silicon oxide to metal ions is (10000-100000) : 1; b, carrying out hydrothermal crystallization of the colloidal mixture obtained in step a, to obtain a crystallized product; c, washing and separating the crystallized product obtained in step b, to obtain a product containing trace metal ions Silicate-1 molecular sieve; d, the Silicate-1 molecular sieve containing trace metal ions obtained in step c is subj...

Embodiment 1

[0080] This example is used to illustrate the preparation method of the Silicate-1 molecular sieve catalyst containing trace metal ions provided by the present invention.

[0081] With 208 grams of ethyl orthosilicate, 180 grams of 22.5% by weight of tetrapropylammonium hydroxide (abbreviated as TPAOH), 0.0281 grams of Fe (NO 3 ) 3 9H 2 O and 220 grams of water were mixed and stirred at room temperature for 3 hours to form a colloidal mixture with a molar ratio of SiO 2 :TPAOH:H 2 O=1:0.2:20, SiO 2 with Fe 3+ The mass ratio of the above mixture is 15347:1, and the above mixture is moved into a 1000 ml stainless steel reactor lined with polytetrafluoroethylene, crystallized at 100°C for 3 days, washed, filtered, dried at 120°C for 24 hours, and roasted at 550°C for 6 hours. The Silicate-1 molecular sieve prepared in this example was obtained.

[0082] The iron ion content of the Silicate-1 molecular sieve product prepared by this embodiment is 64ppm, and the BET specific ...

Embodiment 2

[0088] This example is used to illustrate the preparation method of the Silicate-1 molecular sieve catalyst containing trace metal ions provided by the present invention.

[0089] With 208 grams of ethyl orthosilicate, 180 grams of 22.5% by weight of tetrapropylammonium hydroxide (abbreviated as TPAOH), 0.118 grams of Al (NO 3 ) 3 9H 2 O and 220 grams of water were mixed and stirred at room temperature for 5 hours to form a colloidal mixture with a molar ratio of SiO 2 :TPAOH:H 2 O=1:0.2:20, SiO 2 with Al 3+ The mass ratio of the above mixture is 7067:1. The above mixture is transferred into a 1000 ml stainless steel reactor lined with polytetrafluoroethylene, crystallized at 100°C for 3 days, washed, filtered, dried at 120°C for 24 hours, and roasted at 550°C for 6 hours. The Silicate-1 molecular sieve prepared in this example was obtained.

[0090] The aluminum ion content of the Silicate-1 molecular sieve product prepared in this embodiment is 140ppm, and the BET spec...

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Abstract

The invention discloses a preparation method for a Silicate-1 molecular sieve catalyst, the Silicate-1 molecular sieve catalyst prepared by the method and a method for preparing caprolactam from cyclohexanone oxime. The preparation method for the Silicate-1 molecular sieve catalyst comprises the steps: a. mixing a silicon source, a metal ion source, an organic template agent and water, so as to obtain a colloidal mixture; b. subjecting the colloidal mixture obtained in the step a to hydrothermal crystallization, so as to obtain a crystallized product; c. subjecting the crystallized product obtained in the step b to washing and separating treatment, so as to obtain metal ion containing Silicate-1 molecular sieves; and d. subjecting the metal ion containing Silicate-1 molecular sieves obtained in the step c to forming treatment, roasting treatment and aftertreatment by an alkaline buffer solution of a nitrogen containing compound, and carrying out washing, separating and drying, thereby obtaining the Silicate-1 molecular sieve catalyst containing trace metal ions. By adopting the method, the performance of the Silicate-1 molecular sieve catalyst can be effectively changed; and by applying the catalyst to the production of the caprolactam, an unexpected result can be achieved.

Description

technical field [0001] The invention relates to a preparation method of a Silicate-1 molecular sieve catalyst, a Silicate-1 molecular sieve catalyst prepared by the method and a method for preparing caprolactam from cyclohexanone oxime. Background technique [0002] Silicalite-1 molecular sieve 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. Silicalite-1 is an aluminum-free all-silicon-1 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. The basic structural unit For SiO4 tetrahedron. Silicalite-1 has a rich microporous structure and regular and uniform three-dimensional fine channels. It has a definite crystal structure of ZSM-5 molecular sieve, high internal specific surface area, good thermal stability, adsorption and desorption capabilities...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/035C07D223/10C07D201/04
CPCB01J29/035B01J29/0356B01J29/0358B01J2229/18C07D201/04C07D223/10Y02P20/52
Inventor 程时标张树忠谢丽慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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