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

A molecular sieve and catalyst technology, applied in the field of preparing caprolactam, can solve the problems of high gas-solid separation requirements, difficult pumping, low thermal efficiency of spray forming, etc.

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

[0014] The thermal efficiency of spray molding is low. For viscous paste materials, pumping is difficult, and it needs to be diluted before spray molding. At the same time, the requirements for gas-solid separation are high, and the equipment is huge.

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0092] (1) Tetrapropyl ammonium hydroxide (abbreviated as TPAOH) of 41.6g tetraethyl orthosilicate, 36g 22.5% by weight (abbreviated as TPAOH), 23g ethanol (abbreviated as EtOH), 0.0056gFe(NO 3 ) 3 9H 2 O and 41.5g of water were mixed, and 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 :EtOH:TPAOH:H 2 O (molar ratio) = 1:6.5:0.2:20, SiO 2 with Fe 3+ The weight ratio was 15347:1. The above mixture was transferred into a 300ml stainless steel reactor and crystallized at 100°C for 3 days to obtain 140g of molecular sieve slurry with a solid content of 8.5% by weight and a pH of 13.60. Take a small amount of the molecular sieve slurry and dry it at 120°C for 20 hours to obtain Silicate-1 molecular sieve raw powder containing trace metal ions. The measured iron ion content is 64ppm, and the BET specific surface area is 446m 2 / g, the outer specific surface is 61 meters 2 / g, the particle size is 0.1-0.2μm....

Embodiment 2

[0098] (1) Tetrapropyl ammonium hydroxide (abbreviated as TPAOH) of 41.6g tetraethyl orthosilicate, 36g 22.5% by weight (abbreviated as TPAOH), 23g ethanol (abbreviated as EtOH), 0.0236gAl (NO 3 ) 3 9H 2 O and 41g of water were mixed and stirred at room temperature for 5 hours to form a colloidal mixture with a pH value of 12.4, and SiO in the mixture 2 :EtOH:TPAOH:H 2 O (molar ratio) = 1:6.5:0.2:20, SiO 2 with Al 3+ The weight ratio was 7067:1. The above mixture was transferred into a 300ml stainless steel reactor and crystallized at 100°C for 3 days to obtain 140g of molecular sieve slurry with a solid content of 8.57% by weight and a pH of 13.76. Take a small amount of the molecular sieve slurry and dry it at 120°C for 20 hours to obtain Silicate-1 molecular sieve raw powder containing trace metal ions. The measured aluminum ion content is 140ppm, and the BET specific surface area is 433m 2 / g, the outer specific surface is 51 meters 2 / g, the particle size is 0.1-0.2...

Embodiment 3

[0104] (1) 41.6g tetrapropyl ammonium hydroxide (abbreviated as TPAOH), 0.0008g ZrOCl 2 ·8H 2 O and 42g of water were mixed and stirred at room temperature for 5 hours 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 was 50596:1. The above mixture was transferred into a 300ml stainless steel reactor, and crystallized at 100°C for 3 days to obtain 140g of molecular sieve slurry with a solid content of 8.57% by weight and a pH value of 13.42. Take a small amount of the molecular sieve slurry and send it to dry at 120°C for 20 hours to obtain Silicate-1 molecular sieve raw powder containing trace metal ions. The measured zirconium ion content is 20ppm, and the BET specific surface area is 428 meters 2 / g, the outer specific surface is 48 meters 2 / g, the particle size is 0.1-0.25μm.

[0105] (2) Mix and stir 13.1g tetraethyl orthosilicate and 22g deionized water, adjust th...

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Abstract

The present invention relates to a Silicate-1 microsphere 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 40-150 [mu]m and a wear index K of less than 5; 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 Silicate-1 microsphere 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 SiO4 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 desorption...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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