Monatomic site iron catalyst with adjustable coordination environment as well as preparation method and application of monatomic site iron catalyst

An iron catalyst and environment technology, which is applied in the preparation of single-atom catalyst materials and its application fields, can solve the problem of single-atom active coordination environment and electronic structure regulation method, low load of active species at single-atom site, and unfavorable industrial application, etc. problem, to achieve the effect of easy scale-up experiment, low cost and simple synthesis method

Active Publication Date: 2022-03-18
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In summary, the iron single-atom catalysts synthesized above generally have low loading of active species at single-atom sites, single-atom active coordination environment and electronic structure regulation methods are single, and the synthesis process is complicated.
Moreover, in terms of catalytic applications, the reaction temperature is high and the time is long, and some even require hydrogenation under high temperature and high pressure conditions, so it is not conducive to industrial applications

Method used

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  • Monatomic site iron catalyst with adjustable coordination environment as well as preparation method and application of monatomic site iron catalyst
  • Monatomic site iron catalyst with adjustable coordination environment as well as preparation method and application of monatomic site iron catalyst
  • Monatomic site iron catalyst with adjustable coordination environment as well as preparation method and application of monatomic site iron catalyst

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Embodiment 1

[0041] A method for preparing a single-atom site iron catalyst with an adjustable coordination environment, comprising the following steps:

[0042] A. Dissolve 8mmol ferrocene formaldehyde in 25mL 1,4-dioxane, stir and mix to form a uniform solution, then transfer it to an ice-water bath, add 1.4mL concentrated sulfuric acid (98wt%) to obtain acidification 25 mL of 1,4-dioxane containing 0.56 mL of pyrrole was then added dropwise to the acidified ferrocene formaldehyde solution, and the stirring was continued in an ice-water bath for 24 hours;

[0043] B. After step A is completed, heat it under reflux at 60°C for 6 hours. After the reaction is completed, precipitate and cool, then deprotonate with 5mL ammonia water, filter, wash and dry after 4 hours to obtain the precursor;

[0044] C. Grind 1g of the precursor prepared in step B with 1g of melamine for 2 hours, put it in a tube furnace under a nitrogen atmosphere, and pyrolyze it at 500°C for 3 hours. The product is named:...

Embodiment 2

[0052] A method for preparing a single-atom site iron catalyst with an adjustable coordination environment, comprising the following steps:

[0053] A. Dissolve 8mmol ferrocene formaldehyde in 25mL 1,4-dioxane, stir and mix to form a uniform solution, then transfer it to an ice-water bath, add 1.4mL concentrated sulfuric acid (98wt%) to obtain acidification 25 mL of 1,4-dioxane containing 0.56 mL of pyrrole was then added dropwise to the acidified ferrocene formaldehyde solution, and the stirring was continued in an ice-water bath for 24 hours;

[0054] B. After step A is completed, heat it under reflux at 60°C for 6 hours. After the reaction is completed, precipitate and cool, then deprotonate with 5mL ammonia water, filter, wash and dry after 4 hours to obtain the precursor;

[0055] C. Grind 1g of the precursor prepared in step B with 1g of melamine for 2 hours, put it in a tube furnace under a nitrogen atmosphere, and pyrolyze it at 600°C for 3 hours. The product is named:...

Embodiment 3

[0064] A method for preparing a single-atom site iron catalyst with an adjustable coordination environment, comprising the following steps:

[0065] A. Dissolve 8mmol ferrocene formaldehyde in 25mL 1,4-dioxane, stir and mix to form a uniform solution, then transfer it to an ice-water bath, add 1.4mL concentrated sulfuric acid (98wt%) to obtain acidification 25 mL of 1,4-dioxane containing 0.56 mL of pyrrole was then added dropwise to the acidified ferrocene formaldehyde solution, and the stirring was continued in an ice-water bath for 24 hours;

[0066] B. After step A is completed, heat it under reflux at 60°C for 6 hours. After the reaction is completed, precipitate and cool, then deprotonate with 5mL ammonia water, filter, wash and dry after 4 hours to obtain the precursor;

[0067] C. Grind 1g of the precursor prepared in step B with 1g of melamine for 2 hours, put it in a tube furnace under a nitrogen atmosphere, and pyrolyze it at 700°C for 3 hours. The product is named:...

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Abstract

The invention provides a monatomic site iron catalyst with an adjustable coordination environment and a preparation method and application thereof, the preparation method comprises the following steps: under an ice-water bath condition, adding concentrated sulfuric acid into a ferrocene formaldehyde solution, mixing a pyrrole solution drop by drop, and continuously stirring for reaction in the ice-water bath; carrying out reflux heating reaction to obtain a precursor, grinding the precursor and a nitrogen-containing compound, and carrying out pyrolysis in an inert atmosphere to obtain iron-nitrogen-sulfur co-doped carbon; and treating with a hydrochloric acid solution, washing and drying to obtain the coordination environment adjustable monatomic site iron catalyst. Compared with the prior art, the method for preparing the monatomic site iron has the advantages that the coordination environment and the carrier electronic structure can be controlled and adjusted, the loading capacity of the monatomic site iron is high, the synthesis method is simple, an amplification experiment is easy, and industrial production can be realized; the catalyst can be used for a benzene oxidation reaction, a styrene epoxidation reaction and a nitro-compound hydrogenation reaction, and has the advantages of high catalytic efficiency, good circulation effect, low cost and the like.

Description

technical field [0001] The invention relates to the field of preparation and application of single-atom catalyst materials, in particular to a single-atom site iron catalyst with adjustable coordination environment, its preparation method and application. Background technique [0002] Single-atom site catalysts, as a class of functional materials with low cost, high activity and 100% atom utilization, are widely used in energy storage (fuel cells, lithium-ion batteries, zinc-air batteries, etc.), gas-solid phase catalysis, electrolysis of water, It has shown positive application value in many fields such as biomedicine, environmental governance, and electrocatalytic organic synthesis. Therefore, chemists and materials scientists have developed numerous synthetic strategies for the effective regulation of high-efficiency iron-based single-atom sites and their coordination environments and electronic structures. [0003] First, active progress has been made in the synthesis a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J27/24C07C37/60C07C209/36C07C39/04C07C211/46C07D301/04C07D301/06C07D303/04
CPCB01J27/24B01J31/1805C07C37/60C07D301/04C07D303/04C07D301/06C07C209/325B01J2231/72B01J2231/70B01J2231/641C07C39/04C07C211/46Y02P20/52
Inventor 叶明富詹林潇吴孔林石罗祥方兆斌尚恒帅王震东魏先文
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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