A kind of catalyst and preparation method thereof, and a kind of method for preparing laurolactam by 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: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of catalyst and preparation method thereof, and a kind of method for preparing laurolactam by gas phase rearrangement reaction
  • A kind of catalyst and preparation method thereof, and a kind of method for preparing laurolactam by gas phase rearrangement reaction

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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 catalysts

[0048] a) Maintain the system at 0-5°C, dissolve 2g TPAOH in 300g deionized water; at the same time, slowly add 0.042g (tri)scandium nitrate hexahydrate, 0.008g yttrium trichloride, 10g Al(NO) to the deionized aqueous solution of the template agent 3 ) 3 ·9H 2 O, 10g ZrOCl 2 ·8H 2 O, 20g TEOS, feeding time 1h; under stirring condition, slowly add 25% ammonia water dropwise to adjust pH=10, continue stirring for 2h, stop stirring and ageing for 1h; filter under reduced pressure, wash with deionized water to medium The filter cake was dried at 120°C for 28h, then calcined at 500°C for 2h, ground and sieved to obtain rare earth-doped Al 2 O 3 -SiO 2 -ZrO 2 vector.

[0049] b) Take 10 g of rare earth doped Al 2 O 3 -SiO 2 -ZrO 2 The carrier was added to 30 g of a sodium fluoride aqueous solution with a mass fraction of 1%, soaked at 50 °C for 30 min, fil...

Embodiment 2

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

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

[0068] b) Take 10 g 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 min, ...

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Abstract

The invention discloses a catalyst and a preparation method thereof, as well as a method for preparing laurolactam by gas-phase rearrangement reaction. The catalyst comprises fluoride modified rare earth doped Al 2 O 3 ‑SiO 2 ‑ZrO 2 and fluorine-containing sulfonated polyether ether ketone, wherein the loading amount of fluorine-containing sulfonated polyether ether ketone in the catalyst is 20-50wt%, preferably 30-45wt%. Using the catalyst to catalyze the gas-phase rearrangement of cyclododecanone oxime, the conversion rate of cyclododecanone oxime can reach more than 99%, the selectivity of laurolactam can reach more than 99.5%, the life of the catalyst can reach more than 3000h, and the reaction has no by-product of ammonium sulfate. , The catalyst has high mechanical strength and solves the equipment corrosion and environmental pollution problems of the traditional liquid phase rearrangement process.

Description

technical field [0001] The invention belongs to the field of catalysts, in particular to a catalyst for preparing laurolactam by gas-phase rearrangement reaction of cyclododecanone oxime. 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, light weight and other performance advantages , its use in a wide range of fields, the most important applications include automotive fuel pipes, pneumatic hoses, high-pressure pipelines, and land and marine oil and gas pipelines, etc.; , additive manufacturing and other fields have important applications. [0003] Laurolactam is a monomer for the production of nylon 12, which is obtained from cyclododecanone oxime (CDOX) via Beckmann rearrangement. [0004] [0005] There are two main processes for preparing laurolactam from c...

Claims

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Application Information

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Patent Type & Authority Patents(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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