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Preparation method of defective graphene anchored double transition metal monatomic synthesis ammonia catalyst

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

Active Publication Date: 2021-08-10
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 monatomic synthesis ammonia catalyst
  • Preparation method of defective graphene anchored double transition metal monatomic synthesis ammonia catalyst
  • Preparation method of defective graphene anchored double transition metal monatomic synthesis ammonia 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 the condition of purging nitrogen and removing oxygen, 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 sh...

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 defective graphene anchored double transition metal monatomic synthesis ammonia catalyst, and the preparation method comprises the following steps: synthesizing polystyrene microspheres, centrifugally washing, and drying in vacuum; stirring and adsorbing the polystyrene microspheres and a transition metal salt solution; stirring the polystyrene microspheres adsorbing the transition metal salt with a defective graphene oxide aqueous solution to form a composite structure taking the polystyrene microspheres as a core and the defective graphene oxide as a shell, performing centrifuging, and performing drying in vacuum; dispersing the sample in an aqueous solution, adding a small amount of another transition metal salt solution, carrying out ultrasonic dispersion, performing freeze-drying, and carrying out high-temperature annealing to obtain a final product. According to the invention, polystyrene microspheres are utilized to adsorb a first transition metal salt, so the first transition metal salt is distributed in an inner shell layer of defective graphene oxide; a second transition metal salt is loaded by utilizing a defective graphene oxide shell layer, and the polystyrene microspheres are removed by utilizing high-temperature annealing to form a structure that the defective graphene hollow inner shell layer and the defective graphene hollow shell layer are respectively loaded with two double-transition metal monatomic structures.

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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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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