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Microsphere silicate-1 molecular sieve catalyst and its preparation method and method for preparing caprolactam

A molecular sieve and catalyst technology, applied in the field of preparing caprolactam, achieves the effects of high total selectivity and total yield, reduced energy consumption for product separation, high strength and wear resistance

Active Publication Date: 2022-06-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 its preparation method and method for preparing caprolactam
  • Microsphere silicate-1 molecular sieve catalyst and its preparation method and method for preparing caprolactam

Examples

Experimental program
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Effect test

Embodiment 1

[0082] 416kg of ethyl orthosilicate, 360kg of 22.5% by weight of tetrapropylammonium hydroxide (abbreviated as TPAOH), 56.2g of Fe (NO 3 ) 3 ·9H 2 O and 415kg of water were mixed, and stirred at room temperature for 5 hours to form a colloidal mixture with a pH value of 12.8. In the mixture, SiO 2 :TPAOH:H 2 O (molar ratio) = 1:0.2:20, SiO 2 with Fe 3+ The weight ratio of 15347:1, 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 crystallization product is 13.57, then use a 50nm six-tube membrane for membrane filtration and wash with water at 40-60 °C, and the amount of washing water is 6.8m 3 The pH of the post-crystallized product reached 9.1. The slurry obtained after washing was concentrated to obtain 395kg of molecular sieve slurry with a solid content of 26.8% by weight, which was sent to microwave drying and dried at 100-150°C for 1 hour to obtain about 125kg of Silicate-1 molecular sieve r...

Embodiment 2

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

Embodiment 3

[0096] 416kg of tetraethyl orthosilicate, 360kg of 22.5% by weight of tetrapropylammonium hydroxide (abbreviated as TPAOH), 8.4g of ZrOCl 2 ·8H 2 Mix O and 420kg of water, and stir at room temperature for 5 hours to form a colloidal mixture with a pH value of 12.46. In the mixture, SiO 2 :TPAOH:H 2 O (molar ratio) = 1:0.2:20, SiO 2 with Zr 4+ The weight ratio of 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 crystallization product is 13.42, then use a 50nm six-tube membrane for membrane filtration and wash with water at 40-60°C, and the amount of washing water is 6.7m 3 The pH of the post-crystallized product reached 9.1. The slurry obtained after washing was concentrated to obtain 310kg of molecular sieve slurry with a solid content of 28.4% by weight, which was sent to microwave drying and dried at 100-150°C for 1 hour to obtain about 127kg of Silicate-1 molecular sieve raw powder.

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Abstract

The present 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, based on the dry weight of the catalyst, the catalyst comprising 70 ~95% by weight of Silicate-1 molecular sieve containing trace metal ions, and 5-30% by weight of binder; the particle size of the catalyst is 20-300 μm, and the wear index K is less than 8; the BET of the Silicate-1 molecular sieve The specific surface area is 400‑500 meters 2 / g, the weight ratio of silicon oxide to metal ions is (5000‑200000):1. The wear index of the catalyst is low, and the gas-phase Beckmann rearrangement reaction of cyclohexanone oxime in a fluidized bed process can effectively improve the selectivity of caprolactam.

Description

technical field [0001] The present disclosure relates to a microsphere Silicate-1 molecular sieve catalyst containing trace 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 by E.M. Flanigen of UCC Company in 1978, 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 topology. It is the simplest molecular sieve in the ZSM-5 molecular sieve family. Its skeleton only contains silicon atoms and oxygen atoms. The structural unit is SiO 4 tetrahedron. All-silicon-1 molecular sieve has abundant microporous structure and regular and uniform three-dimensional fine pore channels. It has the definite crystal structure of ZSM-5 molecular sieve, high internal specific surface area, good...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/03B01J29/035B01J35/02B01J35/10C07D201/04C07D223/10B01J35/00
CPCY02P20/52
Inventor 程时标谢丽张树忠慕旭宏宗保宁
Owner CHINA PETROLEUM & CHEM CORP