Preparation method of defective graphene-anchored double-transition metal single-atom ammonia synthesis catalyst

A transition metal, graphene technology, applied in the electrolysis process, electrolysis components, electrodes and other directions, can solve problems such as the inability to obtain catalytic performance, and achieve the effect of broadening the field of catalyst preparation, improving productivity and Faradaic efficiency, and improving catalyst activity.

Active Publication Date: 2022-05-06
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, single-atom catalysts still cannot achieve better catalytic performance due to their limited metal loading.

Method used

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  • Preparation method of defective graphene-anchored double-transition metal single-atom ammonia synthesis catalyst
  • Preparation method of defective graphene-anchored double-transition metal single-atom ammonia synthesis catalyst
  • Preparation method of defective graphene-anchored double-transition metal single-atom ammonia synthesis catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 1.8 g of polyvinylpyrrolidone, 18 g of styrene, and 0.3 g of azobisisobutyronitrile into a mixture of 80 mL of ethanol and 20 mL of water, stir for 12 h under the condition of nitrogen and deoxygenation, and vacuum-dry the product to obtain polyphenylene SEM pictures of ethylene microspheres and polystyrene microspheres are attached figure 1 ,From figure 1 It can be seen that the microspheres are uniform in size and dispersed evenly;

[0031] Add 1 g of polystyrene microspheres to 10 mmol / L hemin solution and ultrasonically homogenize, stir at room temperature for 12 hours, and centrifuge to wash off excess hemin;

[0032] Stir 1 g of polystyrene microspheres adsorbed with hemin and 5 mg / mL defective graphene oxide aqueous solution for 24 h to form a composite structure with polystyrene microspheres as the core and defective graphene oxide as the shell, and vacuum-dry after centrifugation Defective graphene oxide-coated polystyrene microspheres are obtained, and d...

Embodiment 2

[0035] Add 1.8 g of polyvinylpyrrolidone, 15 g of styrene, and 0.2 g of azobisisobutyronitrile into a mixture of 90 mL of ethanol and 10 mL of water, stir for 12 h under nitrogen and deoxygenation conditions, and vacuum-dry the product after centrifugal washing to obtain poly Styrene microspheres, SEM pictures of polystyrene microspheres are attached Figure 6 ,From Figure 6 It can be seen that the polystyrene microspheres are uniformly dispersed, the surface is smooth and the size is uniform;

[0036] Add 1 g of polystyrene microspheres to 20 mmol / L iron phthalocyanine solution and ultrasonically homogenize, stir at room temperature for 12 h, and centrifuge to wash off excess iron phthalocyanine solution;

[0037] Stir 1 g of polystyrene microspheres adsorbed iron phthalocyanine solution with 10 mg / mL defective graphene oxide aqueous solution for 24 h to form a composite structure with polystyrene microspheres as the core and defective graphene oxide as the shell, which is ob...

Embodiment 3

[0040] The implementation mode is the same as in Example 1, only the first transition metal complex is replaced by tetraammine copper dichloride, and the ammonia synthesis yield can be as high as 18.3 μg·h -1 ·mg -1 cat , the Faraday efficiency is as high as 9.1%.

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Abstract

The invention discloses a preparation method of a double-transition metal single-atom ammonia synthesis catalyst anchored by defective graphene. The preparation method comprises: synthesizing polystyrene microspheres, vacuum drying after centrifugal washing; stirring and adsorbing the polystyrene microspheres and a transition metal salt solution; The polystyrene microspheres adsorbing the transition metal salt are stirred with the defective graphene oxide aqueous solution to form a composite structure in which the polystyrene microspheres are the core and the defective graphene oxide is the shell. After centrifugation, vacuum drying is carried out; the above samples are dispersed in the aqueous solution, Add a small amount of another transition metal salt solution, ultrasonically disperse, freeze-dry and anneal at high temperature to obtain the final product. The present invention utilizes polystyrene microspheres to adsorb the first transition metal salt so that it is distributed in the inner shell of the defective graphene oxide; uses the outer shell of the defective graphene oxide to load the second transition metal salt, and uses high temperature annealing to remove the poly Styrene microspheres form defective graphene hollow inner and outer shell layers to support two double transition metal single-atom structures respectively.

Description

technical field [0001] The invention relates to the field of electrocatalytic synthesis of ammonia at room temperature, in particular to the preparation of core-shell defect graphene hollow microspheres by a template method, and double-transition metal single atoms are loaded on both sides of the defect graphene hollow microspheres, and the obtained catalyst is electrolyzed under alkaline conditions It has high synthetic ammonia yield and faradaic efficiency. Background technique [0002] Due to its large specific surface area, high electrical conductivity, adjustable molecular structure, and acid / alkali resistance, graphene has been used in sensors, batteries, and catalysts in recent years. Graphene can capture a variety of substances through π-π interactions, hydrogen bonds, electrostatic interactions and coordination bonds, including organic pollutants, biopolymers and metal ions. Defective graphene adds more to the advantages of graphene. Multiple binding sites. [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B11/052C25B11/091C25B1/27
CPCC25B1/00
Inventor 陈少娜熊梓林卜梦珂代忠旭
Owner CHINA THREE GORGES UNIV
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