Catalyst for producing caprolactam as well as preparation method and application thereof

A technology of caprolactam and catalyst, which is applied to the catalyst for producing caprolactam and the field of preparation and application thereof, can solve the problems of low catalyst activity, poor stability, and excessive ammonium sulfate, and achieves improved reaction activity, improved stability, and increased hydrophobicity. Effect

Inactive Publication Date: 2015-01-28
江苏黄马化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of cyclohexanone oxime liquid phase rearrangement by-product ammonium sulfate, gas phase rearrangement solid acid catalyst low activity, low selectivity, poor stability, to provide a new cyclohexanone oxime gas phase Catalyst for rearrangement production of caprolactam and its preparation method and application, the catalyst prepared by the method has the characteristics of high activity, high selectivity and good stability

Method used

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  • Catalyst for producing caprolactam as well as preparation method and application thereof
  • Catalyst for producing caprolactam as well as preparation method and application thereof
  • Catalyst for producing caprolactam as well as preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0038] Take 650 grams of ethyl orthosilicate, hydrolyze it with 530 grams of water and 700 grams of 25% tetrapropylammonium hydroxide aqueous solution for one hour, then heat it up to 70°C and remove the alcohol for 2 hours, then transfer the colloid to the autoclave Raise the temperature to 170°C to crystallize for 60 hours, filter, wash and dry, and calcinate at 550°C for 5 hours to obtain the all-silica ZSM-5 zeolite molecular sieve. The XRD spectrum and the scanning electron microscope SEM image are as follows: figure 1 , 2 , It is proved that it is a typical MFI zeolite molecular sieve with a crystal grain size of about 300nm. 50 grams of 25% tetrapropylammonium hydroxide aqueous solution, 30 grams of diethylamine and 30 grams of dimethyldiethoxysilane are dissolved in 500 grams of water to obtain a mixed aqueous solution. Take the above-synthesized all-silicon ZSM-5 150 grams of zeolite molecular sieve was placed in the mixed aqueous solution, modified at 190°C for 48 hour...

Embodiment 2

[0040] 650 grams of 30% silica sol, add 550 grams of deionized water, 450 grams of 25% tetrapropylammonium hydroxide aqueous solution, 120 grams of 25% ammonia, 200 grams of tetrapropylammonium bromide, stir vigorously 2 After hours, it was transferred to an autoclave and heated to 170°C for crystallization for 72 hours, filtered, washed and dried, and calcined at 550°C for 5 hours to obtain the all-silica ZSM-5 zeolite molecular sieve. The XRD spectrum and the scanning electron microscope SEM image are as follows: image 3 , 4 , It is proved that it is a typical MFI zeolite molecular sieve with a crystal grain size of about 300nm. 50 grams of 25% tetrapropylammonium hydroxide aqueous solution, 30 grams of diethylamine and 30 grams of dimethyldiethoxysilane are dissolved in 500 grams of water to obtain a mixed aqueous solution. Take the above-synthesized all-silicon ZSM-5 150 grams of zeolite molecular sieve was placed in the mixed aqueous solution at 155°C for 72 hours for modi...

Embodiment 3

[0042] Take 650 grams of ethyl orthosilicate, hydrolyze it with 530 grams of water and 700 grams of 25% tetrapropylammonium hydroxide aqueous solution for one hour, then heat it up to 70°C and remove the alcohol for 2 hours, then transfer the colloid to the autoclave The temperature was raised to 170°C for crystallization for 60 hours, filtered, washed and dried, and calcined at 550°C for 5 hours to obtain a full-silica ZSM-5 zeolite molecular sieve. 80 grams of 25% tetrapropylammonium hydroxide aqueous solution, 15 grams of diethylamine and 30 grams of dimethyldiethoxysilane are dissolved in 500 grams of water to obtain a mixed aqueous solution. Take the above-synthesized all-silicon ZSM-5 150 grams of zeolite molecular sieve was placed in the mixed aqueous solution at 170°C for 48 hours for modification treatment, filtered, washed and dried. Mix the modified zeolite molecular sieve with 105 grams of silica gel, add 150 milliliters of 1N nitric acid, knead and extrude into a s...

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Abstract

The invention discloses a catalyst for producing caprolactam as well as a preparation method and application of the catalyst. The catalyst for producing the caprolactam is prepared by the following steps: synthesizing an MFI type zeolite molecular sieve; putting the MFI type zeolite molecular sieve into an nitrogen-containing organic alkali and organic silicon mixed water solution, and then carrying out a reaction at the temperature of 120-190 DEG C for 24-72 hours for modification treatment; mixing the zeolite molecular sieve treated by modification with a bonding agent, feeding a nitric acid solution into the mixture, kneading, molding, drying, and roasting to obtain the molecular sieve-based catalysts. After the zeolite molecular sieve is treated by the nitrogen-containing organic alkali combined with organosilane, the hydroxyl active center on the surface of the zeolite molecular sieve is effectively inhibited, so that the hydrophobicity of the catalyst is improved, and the reaction product caprolactam is rapidly diffused outside from pores of the catalyst; therefore, the side reactions of the caprolactam on the surface of the catalyst can be reduced, and the reaction activity, stability and product selectivity of the catalyst are improved.

Description

Technical field [0001] The present invention relates to a catalyst for the production of caprolactam and a preparation method and application thereof. More specifically, the present invention relates to a catalyst prepared by treating a zeolite molecular sieve with a combination of nitrogen-containing organic base and organic silicon, and using the catalyst to Method of producing caprolactam. Background technique [0002] Caprolactam (CPL) is an important organic chemical intermediate. The Beckmann rearrangement of cyclohexanone oxime (CHO) is one of the key steps in the production process of caprolactam. At present, the Beckmann rearrangement of cyclohexanone oxime mainly adopts the traditional homogeneous catalytic process with concentrated sulfuric acid as the catalyst in industry. The process has mild reaction conditions, ideal conversion rate and selectivity, but a large amount of ammonium sulfate is by-produced, and it is easy to cause equipment corrosion and environmental...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/06B01J29/08B01J29/18B01J29/70C07D223/10C07D201/04
CPCY02P20/52
Inventor 陶德志陶圣明
Owner 江苏黄马化工有限公司
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