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Method for preparing hierarchical pore carbonic oxide microsphere material

A technology of multi-level pores and carbon-nitrogen, applied in the manufacture of hybrid/electric double layer capacitors, hybrid capacitor electrodes, etc., can solve the problems of cumbersome steps, unfavorable industrial production, and high production costs of nitrogen-doped porous carbon materials, and achieve excellent structures Stability, excellent electrochemical performance, short reaction time

Inactive Publication Date: 2017-02-22
CHONGQING UNIV OF ARTS & SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0006] Although nitrogen-doped porous carbon materials have broad application prospects in the field of supercapacitors, there are still the following problems in the research on this aspect: (1) The preparation of nitrogen-doped carbon materials usually uses expensive raw material reagents and toxic Nitrogen sources, such as pyrrole, ammonia or hydrogen cyanide, generally have problems such as high production costs, poor safety, and environmental pollution; (2) the steps for preparing nitrogen-doped porous carbon materials are cumbersome and time-consuming It is beneficial to industrial production; (3) At present, most of the research on nitrogen-doped carbon materials focuses on the research on nitrogen-doped activated carbon or nitrogen-doped mesoporous carbon materials, and the research on nitrogen-doped hierarchical porous carbon materials is rare; (4) Although there has been some research on nitrogen-doped carbon materials and hierarchically porous carbon electrode materials, the research on combining nitrogen-doped modification with pore structure optimization to design high-performance supercapacitor electrode materials is rarely reported; (5) Most of the studied nitrogen-doped carbon materials for supercapacitors are in the form of powder or bulk, and there is no relevant literature or patent report on the use of flower-like hierarchical porous carbon spheres as supercapacitor electrode materials; (6) The nitrogen content of nitrogen-doped carbon materials used as supercapacitor electrode materials is usually relatively low. In order to give full play to the advantages of nitrogen doping, the nitrogen content needs to be further increased

Method used

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  • Method for preparing hierarchical pore carbonic oxide microsphere material
  • Method for preparing hierarchical pore carbonic oxide microsphere material
  • Method for preparing hierarchical pore carbonic oxide microsphere material

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 1. To prepare the hierarchically porous carbon-nitrogen microsphere material, follow the steps below:

[0036] (1) Preparation of PAA solution

[0037]Polyamic acid (PAA) is obtained by polycondensation of pyromellitic dianhydride (PMDA) and 4,4'-diaminodiphenyl ether (ODA) in the polar solvent N-methylpyrrolidone (NMP). Firstly, ODA and PMDA were recrystallized with ethanol and acetic anhydride respectively, and sealed for storage; the water in NMP was removed by vacuum distillation, and the redistilled NMP was stored in a desiccator; , ODA and PMDA with a molar ratio of 1:1 were added to the solvent NMP, stirred for 6hr, and polycondensed to prepare a polyamic acid solution with a mass percentage of 5wt%.

[0038] (2) Preparation of Hierarchical Porous Carbon Nitrogen Microspheres

[0039] A, adopt 15ml concentration to be the PAA solution impregnation volume of 5wt% be 15cm 3 The commercial polyurethane (PU) foam was dried under vacuum at 50°C for 20h.

[0040] B...

Embodiment 2

[0049] 1. To prepare the hierarchically porous carbon-nitrogen microsphere material, follow the steps below:

[0050] (1) Preparation of PAA solution

[0051] PAA is obtained by polycondensation of pyromellitic dianhydride (PMDA) and 4,4'-diaminodiphenyl ether (ODA) in the polar solvent N,N-dimethylacetamide (DMAC). Firstly, ODA and PMDA were recrystallized with ethanol and acetic anhydride respectively, and sealed for storage; the water in DMAC was removed by vacuum distillation, and the redistilled DMAC was stored in a desiccator; , ODA and PMDA with a molar ratio of 1:1 were added to the solvent DMAC, stirred for 8 hours, and polycondensed to prepare a PAA solution with a mass percentage of 10 wt%.

[0052] (2) Preparation of Hierarchical Porous Carbon Nitrogen Microspheres

[0053] A, adopt 10ml concentration to be the PAA solution impregnation volume of 10wt% be 12cm 3 The commercial PU foam was dried under vacuum at 70°C for 15h.

[0054] B. Heat the impregnated PU f...

Embodiment 3

[0061] 1. To prepare the hierarchically porous carbon-nitrogen microsphere material, follow the steps below:

[0062] (1) Preparation of PAA solution

[0063] PAA is obtained by polycondensation of pyromellitic dianhydride (PMDA) and 4,4'-diaminodiphenyl ether (ODA) in the polar solvent N,N-dimethylformamide (DMF). First, recrystallize ODA and PMDA with ethanol and acetic anhydride respectively, and seal them for storage; use vacuum distillation to remove the water in DMF, and put the re-distilled DMF in a desiccator; , ODA and PMDA with a molar ratio of 1:1 were added to the solvent DMF, stirred for 10 hr, and polycondensed to prepare a PAA solution with a mass percent content of 15 wt%.

[0064] (2) Preparation of Hierarchical Porous Carbon Nitrogen Microspheres

[0065] A, adopt 5ml concentration to be the PAA solution impregnation volume of 15wt% be 10cm 3 The commercial PU foam was dried under vacuum at 90°C for 6h.

[0066] B. Heat the impregnated PU foam under a nit...

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Abstract

The invention discloses a method for preparing a hierarchical pore carbonic oxide microsphere material. The method comprises the following steps: A, impregnating PU foam with a PAA solution, and drying for 6-20 hours at 50-90 DEG C in vacuum; B, heating the PU foam after impregnating and drying in an inert gas atmosphere, namely heating for 0.5-3 hours at 80-120 DEG C, increasing the temperature to 170-230 DEG C and heating for 0.5-3 hours, and increasing the temperature to 270-330 DEG C and heating for 0.5-3 hours; and C, roasting for 1-6 hours at 500-800 DEG C in the inert gas atmosphere after the heating treatment in the step B is completed, and cooling to room temperature. The method is simple, has low cost and short reaction time, and is suitable for industrial production; and the prepared carbonic oxide microsphere material has an ideal flower-like spherical shape, a micropore-mesopore-macropore hierarchical porous structure, a large specific surface area, high nitrogen content and excellent electrochemical performance, and has huge application prospects in the field of super-capacitors.

Description

technical field [0001] The invention relates to a preparation technology of a novel carbon material, in particular to a preparation method of a multi-level porous carbon-nitrogen microsphere material. Background technique [0002] Supercapacitor is a new type of energy storage device between traditional capacitors and batteries. It has the advantages of high power density, long cycle life, good high and low temperature performance, safety and pollution-free, and has attracted more and more attention. Consumer electronics, mobile communications, information technology, electric vehicles, medical equipment, aerospace, military and many other fields have broad application prospects. Electrode material is a key factor affecting the performance of supercapacitors. Due to the advantages of low price, good electrochemical stability, large specific surface area and pore volume, carbon materials have become the electrode materials of choice for supercapacitors. However, porous carb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01G11/24H01G11/42H01G11/86
CPCY02E60/13H01G11/24H01G11/42H01G11/86
Inventor 刘玉荣张进刘碧桃
Owner CHONGQING UNIV OF ARTS & SCI
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