Catalyst and preparation method thereof, and method for preparing laurolactam through gas phase rearrangement reaction

A catalyst and fluoride technology, applied in the preparation of lactam, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as equipment corrosion and environmental pollution

Active Publication Date: 2021-04-09
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The invention relates to a catalyst and a preparation method thereof. The catalyst is used for gas-phase rearrangement of cyclododecanone oxime to synthesize laurolactam, and has the advantages of high reaction conversion rate, high selectivity, high mechanical strength and long service life of the catalyst, and There is no by-product of ammonium sulfate in the reaction, which solves the problems of equipment corrosion and environmental pollution in the traditional liquid phase rearrangement process

Method used

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  • Catalyst and preparation method thereof, and method for preparing laurolactam through gas phase rearrangement reaction
  • Catalyst and preparation method thereof, and method for preparing laurolactam through gas phase rearrangement reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0047] 1) Rare earth-doped fluorine-containing SPEEK / Al 2 o 3 -SiO 2 -ZrO 2 Preparation of composite catalyst

[0048] a) Maintain the system at 0-5°C, dissolve 2g TPAOH in 300g deionized water; at the same time slowly add 0.042g (three) scandium nitrate hexahydrate, 0.008g yttrium trichloride, 10g Al(NO 3 ) 3 9H 2 O, 10gZrOCl 2 ·8H 2 0, 20gTEOS, feeding time 1h; under stirring conditions, slowly add 25% ammonia water dropwise to adjust the solution to pH=10, continue to stir for 2h, stop stirring and age for 1h; vacuum filter, wash with deionized water to neutral properties; the filter cake was dried at 120°C for 28 hours, then roasted at 500°C for 2 hours, ground and sieved to obtain rare earth-doped Al 2 o 3 -SiO 2 -ZrO 2 carrier.

[0049] b) Take 10g of rare earth doped Al 2 o 3 -SiO 2 -ZrO 2 The carrier was added to 30 g of a 1% sodium fluoride aqueous solution, soaked at 50°C for 30 minutes, filtered, washed with deionized water, and dried to obtain a flu...

Embodiment 2

[0066] 1) Rare earth-doped fluorine-containing SPEEK / Al 2 o 3 -SiO 2 -ZrO 2 Preparation of composite catalyst

[0067] a) Maintain the system at 0-5°C, dissolve 3g TPAOH in 300g deionized water; at the same time slowly add 0.09g (three) scandium nitrate hexahydrate, 0.01g yttrium trichloride, 12g Al(NO 3 ) 3 9H 2 O, 10g ZrOCl 2 ·8H 2 0, 25gTEOS, feeding time 1h; under stirring condition, slowly add 25% ammonia solution dropwise to adjust the solution to pH=9, continue to stir for 2h, stop stirring and age for 1h; decompression suction filtration, wash with deionized water to Neutral; the filter cake was dried at 120°C for 24h, then roasted at 550°C for 2h, ground and sieved to obtain rare earth-doped Al 2 o 3 -SiO 2 -ZrO 2 carrier.

[0068] b) Take 10g of rare earth doped Al 2 o 3 -SiO 2 -ZrO 2 The carrier was added to 20 g of a sodium fluoride aqueous solution with a mass fraction of 1%, soaked at 50°C for 30 minutes, filtered, washed with deionized water, and...

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Abstract

The invention discloses a catalyst and a preparation method thereof, and a method for preparing laurolactam through a gas phase rearrangement reaction. The catalyst comprises fluoride modified rare earth doped Al2O3-SiO2-ZrO2 and fluorine-containing sulfonated polyetheretherketone, and the loading capacity of the fluorine-containing sulfonated polyetheretherketone in the catalyst is 20-50wt%, preferably 30-45wt%. When the catalyst is used for catalyzing gas-phase rearrangement of cyclododecanone oxime, the conversion rate of cyclododecanone oxime reaches 99% or above, the selectivity of laurolactam reaches 99.5% or above, the service life of the catalyst reaches 3000h or above, no ammonium sulfate byproduct is produced in the reaction, the mechanical strength of the catalyst is high, and the problems of equipment corrosion and environmental pollution of a traditional liquid-phase rearrangement process are solved.

Description

technical field [0001] The invention belongs to the field of catalysts, and in particular relates to a catalyst for gas-phase rearrangement reaction of cyclododecanone oxime to prepare laurolactam. Background technique [0002] Nylon 12 is a special polyamide material and is one of the most representative nylons with long carbon chains. It has outstanding toughness, low temperature resistance, low water absorption, high chemical stability, wear resistance, and light weight. , it is used in a wide range of fields, the most important applications include automotive fuel pipes, pneumatic hoses, high-pressure pipelines, and land and offshore oil and gas pipelines; in addition, it is used in cable protection, electronic appliances, powder coatings, 3D printing, sports equipment , additive manufacturing and other fields have important applications. [0003] Lauryl lactam is a monomer for the production of nylon 12, which is obtained from cyclododecanone oxime (CDOX) through a Bec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/135B01J35/10C07D225/02C07D201/06
CPCB01J27/135B01J35/1004C07D225/02C07D201/06Y02P20/584
Inventor 边新建李俊平吴训锟陈海波黎源张永振袁帅
Owner WANHUA CHEM GRP CO LTD
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