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

A technology of molecular sieve and catalyst, which is applied in the field of caprolactam preparation, can solve the problems such as the spray molding of Silicalite-1 molecular sieve, and achieve the effects of reduced product separation energy consumption, high total selectivity and total yield, and improved technical economy

Active Publication Date: 2022-07-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] So far, there have been no relevant documents or patents on spray molding Silicalite-1 molecular sieves containing extremely small or trace amounts of metal ions.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] 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 395 kg of molecular sieve slurry with a solid content of 26.8% by weight. A small amount of the molecular sieve slurry was dried at 120°C for 20 hours to obtain the original Silicate-1 molecular...

Embodiment 2

[0081] 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, the above mixture was moved 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 436 kg of molecular sieve slurry with a solid content of 24.5% by weight. A small amount of the molecular sieve slurry was dried at 120°C for 20 hours to obtain the original Silicate-1...

Embodiment 3

[0086] 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, the above mixture was moved 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 380 kg of molecular sieve slurry with a solid content of 28.4% by weight. A small amount of the molecular sieve slurry was dried at 120°C for 20 hours to obtain the original Silicate-1 molecular sieve p...

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Abstract

The present disclosure relates to a Silicate-1 microsphere molecular sieve catalyst containing trace metal ions, a preparation method thereof, and a method for preparing caprolactam from cyclohexanone oxime. ~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 20-100 μm, and the wear index K is less than 10; BET specific surface area of ​​400‑500 m 2 / g, the weight ratio of silicon oxide to metal ions is (5000‑200000):1. The catalyst has a low attrition index and can effectively improve the selectivity of caprolactam when used in the gas-phase Beckmann rearrangement reaction of cyclohexanone oxime in a fluidized bed process.

Description

technical field [0001] The present disclosure relates to a Silicate-1 microsphere 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 SiO4 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 t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/035B01J35/08B01J37/00C07D223/10C07D201/04
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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