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Method for preparing nitrogen and phosphorus codoped porous graphene material

A porous graphene, co-doping technology, applied in directions such as graphite, can solve the problems of toxic etchants, difficult industrial production, application limitations, etc., and achieve the effects of convenient method, large specific surface area and large pore volume.

Inactive Publication Date: 2014-02-12
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, porous graphene is mainly prepared by inorganic nanoparticles (silicon dioxide, nano-calcium carbonate, etc.), polymer hard spheres (polystyrene (PS) and polymethyl methacrylate (PMMA) spheres) as templates or inorganic salts as templates. etchant to prepare porous graphene, but because the use of inorganic nanoparticles requires a relatively toxic etchant, it is difficult to produce industrially, and the polymer hard spheres used are all in the large pore size range (hundreds of nanometers to micrometers), and its The contribution to the specific surface area is very effective, so the application in capacitors, batteries, gas adsorption, etc. is limited

Method used

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  • Method for preparing nitrogen and phosphorus codoped porous graphene material
  • Method for preparing nitrogen and phosphorus codoped porous graphene material
  • Method for preparing nitrogen and phosphorus codoped porous graphene material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1. The preparation of a kind of nitrogen-phosphorus co-doped porous graphene

[0024] (1) Add 16.8 g of 4-vinylbenzyl chloride, 29.8 g of triphenylphosphine and 100 mL of acetone into a dry flask equipped with a magnetic stirring device, and react in a water bath at 45 °C under a nitrogen atmosphere for 10 hours, then filtered, washed with acetone and dried in a vacuum oven for 12 h;

[0025] (2) Add 4.148 g of PIL monomer obtained in step (1), 6 g of allyl glycidyl ether, and 0.08 g of azobisisobutyronitrile to 260 mL of methanol solution, and react at 70 °C After 6 h, it was added to a large amount of ether solution. The precipitated product was filtered, washed three times with tetrahydrofuran and deionized water, and then dried in vacuum for 12 h;

[0026] (3) Add 32 mg of PPIL and 64 mg of graphene oxide obtained in step (2) into 80 mL of water, disperse evenly by ultrasonication, add 5 mL of ammonia solution, and react at 180 °C for 12 h. After cooli...

Embodiment 2

[0027] Embodiment 2. Preparation of a nitrogen-phosphorus co-doped porous graphene

[0028] (1) Add 33.6 g of 4-vinylbenzyl chloride, 59.6 g of triphenylphosphine and 200 mL of acetone into a dry flask equipped with a magnetic stirring device, and react in a water bath at 45 °C under a nitrogen atmosphere for 10 hours, then filtered, washed with acetone and dried in a vacuum oven for 12 h;

[0029] (2) Add 8.296 g of PIL monomer obtained in step (1), 12 g of allyl glycidyl ether, and 0.16 g of azobisisobutyronitrile to 260 mL of methanol solution, and react at 70 °C After 6 h, it was added to a large amount of ether solution. The precipitated product was filtered, washed three times with tetrahydrofuran and deionized water, and then dried in vacuum for 12 h;

[0030] (3) Add 64 mg of PPIL and 128 mg of graphene oxide obtained in step (2) into 160 mL of water, disperse evenly by ultrasonic, add 10 mL of ammonia solution and react at 180 °C for 12 h. After cooling to room tem...

Embodiment 3

[0031] Embodiment 3. Preparation of a nitrogen-phosphorus co-doped porous graphene

[0032] (1) Add 84 g of 4-vinylbenzyl chloride, 149 g of triphenylphosphine and 500 mL of acetone into a dry flask equipped with a magnetic stirring device, and react in a water bath at 45 °C under a nitrogen atmosphere for 10 hours, then filtered, washed with acetone and dried in a vacuum oven for 12 h;

[0033](2) Add 20.744 g of PIL monomer obtained in step (1), 30 g of allyl glycidyl ether, and 0.4 g of azobisisobutyronitrile to 1300 mL of methanol solution, and react at 70 °C After 6 h, it was added to a large amount of ether solution. The precipitated product was filtered, washed three times with tetrahydrofuran and deionized water, and then dried in vacuum for 12 h;

[0034] (3) Add 512 mg of PPIL and 320 mg of graphene oxide obtained in step (2) into 160 mL of water, disperse evenly by ultrasonic, add 10 mL of ammonia solution, and react at 180 °C for 12 h. After cooling to room temp...

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Abstract

The invention belongs to the field of preparation of nanometer materials, and provides a method for preparing a nitrogen and phosphorus codoped porous graphene material. The nitrogen and phosphorus codoped porous graphene material is prepared by taking phosphorus-containing polyion liquid microgel as a novel soft ball template and phosphorus-doped precursor, and ammonium hydroxide as a nitrogen source and another pore-forming agent. The prepared porous graphene material has a thin pore wall, large specific surface area and pore diameter, uniform and stable properties, and has potential application prospect in fields such as supercapacitors, security check and catalysis. According to the method, the source of raw materials is wide; the method is simple and easy to operate, is beneficial for mass production in large scale, and has good industrial production basis and wide application prospect.

Description

technical field [0001] The invention belongs to the field of nanomaterial preparation. Phosphorus-containing ionic liquid microgel is prepared by one-step dispersion polymerization, and after being uniformly compounded with graphene oxide through supramolecular interaction, an intercrosslinked nitrogen-phosphorus gel is obtained by calcining under an argon atmosphere. Preparation method of co-doped porous graphene material. Background technique [0002] Porous carbon materials refer to carbon materials with different pore structures, which have excellent properties such as large specific surface area and pore volume, controllable pore structure, and adjustable pore size; thus, they are widely used in nanomedicine, catalysis, separation, energy conversion and storage, etc. Applications. Graphene is a recently developed two-dimensional honeycomb lattice material in which carbon atoms in a planar single layer are tightly bound together, and is considered to be the building blo...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/21
Inventor 刘勇武培怡
Owner FUDAN UNIV
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