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

A technology of molecular sieve and catalyst, applied in the preparation of Silicate-1 molecular sieve catalyst and the field of catalyst and preparation of caprolactam

Active Publication Date: 2020-10-27
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 small amounts of precious 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 of silicate-1 molecular sieve catalyst, catalyst and method for preparing caprolactam
  • Preparation method of silicate-1 molecular sieve catalyst, catalyst and method for preparing caprolactam
  • Preparation method of silicate-1 molecular sieve catalyst, catalyst and method for preparing caprolactam

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preparation example Construction

[0049] The first aspect of the present invention: provide a kind of preparation method of the Silicate-1 molecular sieve catalyst containing noble metal ion, this method comprises: a, silicon source, noble metal source, organic templating agent and water are mixed, obtain colloidal mixture, wherein, in mole Ratio, SiO in the colloidal mixture 2 : noble metal ion: organic template agent: H 2 O=1: (2.6×10 -8 -1×10 -6 ): (0.05-0.50): (5-100), preferably, SiO 2 : noble metal ion: organic template agent: H 2 O=1: (1×10 -7 -1×10 -6 ): (0.15-0.25): (10-50); b, hydrothermal crystallization of the colloidal mixture obtained in step a, to obtain a crystallized product; c, the crystallized product obtained in step b Washing and separation treatment are carried out to obtain the Silicate-1 molecular sieve containing noble metal ions; d, after the Silicate-1 molecular sieve containing noble metal ions obtained in step c is subjected to molding treatment, roasting treatment and an alk...

Embodiment 1

[0075] This example is used to illustrate the preparation method of the Silicate-1 molecular sieve catalyst containing noble metal ions provided by the present invention.

[0076] With 208 grams of ethyl orthosilicate, 180 grams of 22.5% by weight tetrapropylammonium hydroxide (abbreviated as TPAOH), 0.0032 grams of H 2 PtCl 6 ·6H 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 : Pt 4+ :TPAOH:H 2 O=1: (6×10 -6 ): 0.2:20, the above mixture was moved into a 1000 ml stainless steel reaction kettle 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 to obtain this Silicate-1 molecular sieve prepared in the examples.

[0077] The platinum content of the Silicate-1 molecular sieve sample prepared in this embodiment is 19.5ppm, and the BET specific surface area is 442 meters 2 / g, the outer s...

Embodiment 2

[0083] This example is used to illustrate the preparation method of the Silicate-1 molecular sieve catalyst containing noble metal ions provided by the present invention.

[0084] With 208 grams of ethyl orthosilicate, 180 grams of 22.5% by weight of tetrapropylammonium hydroxide (abbreviated as TPAOH), 0.0060 grams of Pd (NO 3 ) 2 2H 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 :Pd:TPAOH:H 2 O=1: (2.3×10 -5 ): 0.2:20, the above mixture was moved into a 1000 ml stainless steel reaction kettle 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 to obtain this Silicate-1 molecular sieve prepared in the examples.

[0085] The palladium content of the Silicate-1 molecular sieve sample prepared in this embodiment is 40.5ppm, and the BET specific surface area is 461 meters 2 / g, the outer ...

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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 following steps: a, mixing a silicon source, a noble metal source, an organic template agent and water to obtain a colloid mixture; b, conducting hydrothermal crystallization on the colloid mixture obtained in the step a to obtain a crystallization product; c, washing and separating the crystallization product obtained in the step b to obtain a silicate-1 molecular sieve containing a noble metal ion; and d, conducting molding treatment on the silicate-1 molecular sieve containing the noble metal ion obtained in the step c, conducting calcination treatment, conducting post-treatment by using a nitrogen-containing compound alkaline buffer solution, and then successively conducting washing, separation and drying to obtain the silicate-1 molecular sieve catalyst containing the noble metal ion. According to the invention, the performance of the silicate-1 molecular sieve catalyst is effectively changed by adopting the method, and when the catalyst is used in the production of caprolactam, unexpected effects 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] Caprolactam is the main raw material for the production of three series of products: nylon, industrial cord and nylon engineering plastics. Its demand has been relatively high, and it is generally prepared through the Beckmann rearrangement reaction of cyclohexanone oxime. At present, the liquid phase rearrangement process using concentrated sulfuric acid or oleum as a catalyst is usually used in industry. The caprolactam produced by this process accounts for about 90% of the world's total production of caprolactam, but this process needs to consume a large amount of sulfuric acid and ammonia water. Generally, 1.3-1.8 tons of ammonium sulfate will be produced as a by-product for every ton of caprolactam produced....

Claims

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Application Information

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IPC IPC(8): B01J29/035C07D223/10C07D201/04
CPCB01J29/0354B01J2229/18C07D201/04C07D223/10Y02P20/52
Inventor 丁璟程时标张树忠谢丽
Owner CHINA PETROLEUM & CHEM CORP
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