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Microsphere Silicate-1 molecular sieve catalyst and preparation method thereof, and caprolactam preparation method

A technology of molecular sieve and catalyst, applied in the field of preparing caprolactam

Active Publication Date: 2019-05-07
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 documents or patents on the Silicalite-1 molecular sieve containing trace metal ions being rotated (rotated) into microspheres and then applied to the gas phase Beckmann rearrangement reaction of cyclohexanone oxime

Method used

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  • Microsphere Silicate-1 molecular sieve catalyst and preparation method thereof, and caprolactam preparation method
  • Microsphere Silicate-1 molecular sieve catalyst and preparation method thereof, and caprolactam preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] With 416kg orthosilicate ethyl ester, 360kg 22.5% by weight tetrapropyl ammonium hydroxide (abbreviated as TPAOH), 56.2gFe(NO 3 ) 3 9H 2 O and 415kg water were mixed, stirred at room temperature for 5 hours to form a colloidal mixture with a pH value of 12.8, and SiO in the mixture 2 :TPAOH:H 2 O (molar ratio) = 1:0.2:20, SiO 2 with Fe 3+ The weight ratio is 15347:1, move the above mixture into 2m 3 In a stainless steel reaction kettle, crystallize at 100°C for 3 days, the pH of the crystallized product is 13.57, and then use a 50nm six-tube membrane for membrane filtration and wash with water at 40-60°C. The amount of washing water is 6.8m 3 The pH of the post-crystallization product reached 9.1. Concentrate the slurry obtained after washing to obtain 395kg of molecular sieve slurry with a solid content of 26.8% by weight, send it to microwave drying, and dry it at 100-150°C for 1 hour to obtain about 125kg of Silicate-1 molecular sieve powder.

[0083] The abov...

Embodiment 2

[0090] With 416kg tetraethyl orthosilicate, 360kg 22.5% by weight of tetrapropylammonium hydroxide (abbreviated as TPAOH), 0.236kgAl (NO 3 ) 3 9H 2 O and 410kg of water were mixed, and stirred for 5 hours at room temperature to form a colloidal mixture with a pH value of 12.35, and SiO in the mixture 2 :TPAOH:H 2 O (molar ratio) = 1:0.2:20, SiO 2 with Al 3+ The weight ratio is 7067:1, move the above mixture into 2m 3 In a stainless steel reaction kettle, crystallize at 100°C for 3 days, the pH of the crystallized product is 13.71, then use a 50nm six-tube membrane for membrane filtration and wash with water at 40-60°C, the amount of washing water is 6.6m 3 The pH of the post-crystallization product reached 9.0. Concentrate the slurry obtained after washing to obtain 310kg of molecular sieve slurry with a solid content of 34.5% by weight, send it to microwave drying, and dry it at 100-150°C for 1 hour to obtain about 125kg of Silicate-1 molecular sieve powder.

[0091] T...

Embodiment 3

[0096] With 416kg tetraethyl orthosilicate, 360kg 22.5% by weight of tetrapropylammonium hydroxide (abbreviated as TPAOH), 8.4gZrOCl 2 ·8H 2 O and 420kg of water were mixed and stirred for 5 hours at room temperature to form a colloidal mixture with a pH value of 12.46, and SiO in the mixture 2 :TPAOH:H 2 O (molar ratio) = 1:0.2:20, SiO 2 with Zr 4+ The weight ratio is 50596:1, move the above mixture into 2m 3 In a stainless steel reaction kettle, crystallize at 100°C for 3 days, the pH value of the crystallized product is 13.42, then use a 50nm six-tube membrane for membrane filtration and wash with water at 40-60°C, the amount of washing water is 6.7m 3 The pH of the post-crystallization product reached 9.1. Concentrate the slurry obtained after washing to obtain 310kg of molecular sieve slurry with a solid content of 28.4% by weight, send it to microwave drying, and dry it at 100-150°C for 1 hour to obtain about 127kg of Silicate-1 molecular sieve powder.

[0097] The...

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Abstract

The present invention relates to a microsphere Silicate-1 molecular sieve catalyst containing a trace amount of metal ions, and a preparation method thereof, and a method for preparing caprolactam from cyclohexanone oxime. According to the present invention, based on the weight of the dry base of the catalyst, the catalyst comprises 70-95 wt% of a Silicate-1 molecular sieve catalyst containing a trace amount of metal ions, and 5-30 wt% of a binder; the catalyst has a particle size of 20-300 [mu]m and a wear index K of less than 8; the Silicate-1 molecular sieve has a BET specific surface areaof 400-500 m<2> / g and a weight ratio of silicon oxide to metal ions of (5000-200000):1; and the catalyst has the low wear index, can be used for the vapor phase Beckmann rearrangement reaction of cyclohexanone oxime in a fluidized bed process, and can effectively increase the selectivity of caprolactam.

Description

technical field [0001] The disclosure relates to a microsphere Silicate-1 molecular sieve catalyst containing a trace amount of metal ions, a preparation method thereof and a method for preparing caprolactam from cyclohexanone oxime. Background technique [0002] Silicalite-1 molecular sieve (referred to as all-silicon-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. All-silicon-1 molecular sieve 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. The structural unit is SiO 4 tetrahedron. All-silicon-1 molecular sieve has a 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 thermal stability, adsorption and desorpti...

Claims

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Application Information

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IPC IPC(8): B01J29/03B01J29/035B01J35/02B01J35/10C07D201/04C07D223/10
CPCY02P20/52
Inventor 程时标谢丽张树忠慕旭宏宗保宁
Owner CHINA PETROLEUM & CHEM CORP
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