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Nickel-based metal organic framework derived nitrogen-phosphorus-oxygen co-doped nickel/carbon composite material as well as preparation method and application thereof

An organic framework, composite material technology, applied in nanotechnology for materials and surface science, hybrid/electric double layer capacitor manufacturing, hybrid capacitor electrodes, etc., can solve difficult in-situ co-doping, cumbersome preparation process, material Large loss and other problems, to achieve the effect of improving capacitor performance, increasing reaction area, and small size

Active Publication Date: 2021-06-01
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used doping elements are nitrogen, phosphorus, and oxygen. Most materials are introduced into polymers and biomass materials through additional steps during the preparation process for ex-situ doping. However, it is difficult to achieve in-situ co-doping of multi-heteroatom co-doped materials. Doping requires gradual doping of different heteroatoms, the preparation process is cumbersome, and the material loss is large

Method used

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  • Nickel-based metal organic framework derived nitrogen-phosphorus-oxygen co-doped nickel/carbon composite material as well as preparation method and application thereof
  • Nickel-based metal organic framework derived nitrogen-phosphorus-oxygen co-doped nickel/carbon composite material as well as preparation method and application thereof
  • Nickel-based metal organic framework derived nitrogen-phosphorus-oxygen co-doped nickel/carbon composite material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Dissolve 5g of hexachlorocyclotriphosphazene and 14.34g of ethyl p-hydroxybenzoate in 150ml of tetrahydrofuran, reflux at 70°C for 24 hours under anhydrous and oxygen-free conditions, and obtain the ligand precursor after rotary evaporation and drying;

[0042] 2. Add 2.8g of the ligand precursor to 100ml of potassium hydroxide solution and tetrahydrofuran mixed solution, stir and reflux at 90°C for 2 hours, and remove the tetrahydrofuran by rotary evaporation to obtain solution A;

[0043] 3. Add solution A dropwise to 1.5mol / L sulfuric acid solution to obtain a white precipitate, which is filtered and then vacuum-dried at 60°C for 12 hours to obtain the ligand;

[0044]4. Add 100mg of nickel acetate and 130mg of ligand to 15ml of dimethyl sulfoxide solution and stir at room temperature for 5min to obtain mixed solution B;

[0045] 5. Wash the mixed solution B with dimethyl sulfoxide and tetrahydrofuran solution, centrifuge twice, and vacuum-dry at room temperature ...

Embodiment 2

[0048] 1. Dissolve 5g of hexachlorocyclotriphosphazene and 14.34g of ethyl p-hydroxybenzoate in 150ml of tetrahydrofuran, reflux at 70°C overnight under anhydrous and oxygen-free conditions, and obtain the ligand precursor after rotary evaporation and drying;

[0049] 2. Add 2.8g of the ligand precursor to 100ml of sodium hydroxide solution and tetrahydrofuran mixed solution, stir and reflux at 70°C for 2 hours, and remove the tetrahydrofuran by rotary evaporation to obtain solution A;

[0050] 3. Add solution A dropwise to 1mol / L hydrochloric acid solution to obtain a white precipitate, filter it and dry it in vacuum at 60°C for 12 hours to obtain the ligand;

[0051] 4. Add 100mg of nickel acetate and 130mg of ligand into 14ml of N,N-dimethylformamide solution and stir at room temperature for 5min to obtain mixed solution B;

[0052] 5. Wash the mixed solution B with N, N-dimethylformamide and tetrahydrofuran solutions, centrifuge twice, and dry it in vacuum at room temperat...

Embodiment 3

[0055] 1. Dissolve 5g of hexachlorocyclotriphosphazene and 14.34g of ethyl p-hydroxybenzoate in 173ml of tetrahydrofuran, reflux at 80°C overnight under anhydrous and oxygen-free conditions, and obtain the ligand precursor after rotary evaporation and drying;

[0056] 2. Add 2.8g of ligand precursor to 105ml of sodium hydroxide solution and tetrahydrofuran mixed solution, stir and reflux at 70°C for 2 hours, and remove tetrahydrofuran by rotary evaporation to obtain solution A;

[0057] 3. Add solution A dropwise to 1mol / L hydrochloric acid solution to obtain a white precipitate, filter it and dry it in vacuum at 60°C for 12 hours to obtain the ligand;

[0058] 4. Add 100mg of nickel acetate and 130mg of ligand to 14ml of dimethyl sulfoxide solution and stir at room temperature for 5min to obtain mixed solution B;

[0059] 5. Wash the mixed solution B with dimethyl sulfoxide and tetrahydrofuran solution, centrifuge twice, and vacuum-dry at room temperature for 6 hours. Under t...

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Abstract

The invention belongs to the field of supercapacitor materials, and discloses a nickel-based metal organic framework derived nitrogen-phosphorus-oxygen co-doped nickel / carbon composite material as well as a preparation method and application thereof. The preparation method of the composite material comprises the following steps: dissolving phosphonitrilic chloride trimer and ethyl p-hydroxybenzoate in tetrahydrofuran, performing refluxing at 70-90 DEG C under anhydrous and anaerobic conditions, and carrying out rotary evaporation and performing drying to obtain a ligand precursor; adding the ligand precursor into a mixed solution of an alkaline solution and tetrahydrofuran, performing refluxing at 70-90 DEG C, and carrying out rotary evaporation to remove tetrahydrofuran to obtain a solution A; dropwise adding the solution A into dilute acid to obtain a precipitate, and performing drying to obtain a ligand; adding nickel acetate and the ligand into an organic solvent, and performing stirring at room temperature to obtain a solution B; and performing centrifuging, washing, drying in vacuum, and performing calcining at the temperature of 450-750 DEG C in a protective atmosphere. The composite material has a nano-particle structure and a large specific surface area, solves problems of poor conductivity, poor cycle performance and the like of a nickel-containing electrode, and is simple in method and mild in condition.

Description

technical field [0001] The invention belongs to the technical field of supercapacitor materials, and more specifically relates to a nickel-based metal-organic framework-derived nitrogen-phosphorus-oxygen co-doped nickel / carbon composite material and its preparation method and application. Background technique [0002] Supercapacitor is a new type of energy storage device, which has the characteristics of high power density, short charging time, long service life, good temperature characteristics, energy saving and environmental protection, so it has a wide range of uses. The excellent electrochemical properties of transition metal oxides make them ideal candidates for high-performance pseudocapacitive electrode materials. Among them, the excellent electrochemical stability and high theoretical specific capacitance of nickel oxide-based materials, coupled with their advantages of low toxicity, low cost and abundant resources, are regarded as very promising electrode materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/24H01G11/26H01G11/34H01G11/30H01G11/86B82Y30/00B82Y40/00
CPCH01G11/24H01G11/26H01G11/34H01G11/30H01G11/86B82Y30/00B82Y40/00Y02E60/13
Inventor 孙志鹏余锦超史晓艳
Owner GUANGDONG UNIV OF TECH
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