Method for preparing porous carbon spheres doped with nitrogen and phosphorus and application

Abstract

The invention belongs to the technical fields of inorganic material chemistry and new energy, and discloses a method for preparing porous carbon spheres doped with nitrogen and phosphorus and an application. Water serves as a solvent, polyphosphazenes microspheres and activating agents are mixed in a mass ratio of (0.2-2):1, concentration of the polyphosphazenes microspheres is maintained at a level of 10-30wt%, stirring is performed completely, the mixture of the polyphosphazenes microspheres and the activating agents is obtained through centrifugal separation, the mixture of the polyphosphazenes microspheres and the activating agents is subjected to carbonization, and finally the porous carbon spheres doped with the nitrogen and the phosphorus are obtained. The activating agents are potassium hydroxide, sodium hydroxide, calcium chloride or zinc chloride. The polyphosphazenes microspheres serve as a carbon precursor in the method, are synthesized directly under the room temperature condition, and has a simple art process and high productivity. Simultaneously, the activating agents are used for processing polyphosphazenes so as to improve specific surface areas and pore structures of the porous carbon spheres greatly and be beneficial to improve hydrogen storage capacity.

Description

technical field

[0001] The invention belongs to the technical field of inorganic material chemistry and new energy, and specifically relates to a preparation method and application of nitrogen and phosphorus doped porous carbon spheres. Background technique

[0002] Hydrogen is a renewable and clean energy source with a wide range of sources, and it is also an important industrial raw material. It has become the most ideal fuel for fuel cells and hydrogen internal combustion engines. Due to the low density of hydrogen gas, it is easy to explode, so the key technology of hydrogen energy utilization lies in the storage of hydrogen gas.

[0003] Research and development of hydrogen storage materials with excellent performance is the key to solving the problem of hydrogen energy storage. In recent years, porous carbon materials have become one of the important research objects of hydrogen storage materials due to their advantages such as low density, high specific surface area,...

Examples

Embodiment 1

[0032] (1) In a 150 mL dry flask, add 100 mL of acetonitrile, weigh 0.001 mol of hexachlorocyclotriphosphazene and 0.003 mol of 4,4′-dihydroxydiphenyl sulfone, mix them evenly and add 0.01 mol of three Ethylamine, seal the flask immediately, and react in an ultrasonic cleaner (100W, 40kHz) water bath for 2h at 40°C. Centrifuge after the reaction, and wash the centrifuged product with ethanol and deionized water for 3 to 4 times, and finally dry the product at 80° C. for 24 hours to obtain polyphosphazene microspheres.

[0033] (2) Weigh 0.6g of polyphosphazene microspheres and 0.6g of potassium hydroxide, disperse them in 4 mL of deionized water, stir for 2 hours to fully immerse the activator potassium hydroxide into the polyphosphazene microspheres, and then dissolve the above mixed solution Centrifuge and dry at 80°C for 24 hours to obtain a polyphosphazene microsphere / potassium hydroxide mixture.

[0034](3) Put the obtained polyphosphazene microspheres / potassium hydroxid...

Embodiment 2

[0053] (1) In a 150 mL dry flask, add 50 mL of acetone, weigh 0.001 mol of hexachlorocyclotriphosphazene and 0.0028 mol of 4,4′-diaminodiphenyl sulfone, mix them well and add 0.006 mol of three Ethylamine, seal the flask immediately, and react in an ultrasonic cleaner (100W, 40kHz) water bath for 10h at 20°C. Centrifuge after the reaction, and wash the centrifuged product with ethanol and deionized water for 3 to 4 times, and finally dry the product at 50° C. for 20 hours to obtain polyphosphazene microspheres.

[0054] (2) Weigh 0.6g of polyphosphazene microspheres and 0.3g of sodium hydroxide, disperse them in 2 mL of deionized water, stir for 2 hours to fully immerse the activator sodium hydroxide into the polyphosphazene microspheres, and then dissolve the above mixed solution Centrifuge and dry at 50°C for 20 hours to obtain a polyphosphazene microsphere / sodium hydroxide mixture.

[0055] (3) Put the obtained polyphosphazene microspheres / sodium hydroxide mixture in a por...

Embodiment 3

[0058] (1) In a 150 mL dry flask, add 500 mL of ethanol, weigh 0.001 mol of hexachlorocyclotriphosphazene and 0.0032 mol of hydroquinone, mix well, add 0.012 mol of triethylamine to it, and immediately seal the flask , react in an ultrasonic cleaner (100W, 40kHz) water bath for 1h at 80°C. Centrifuge after the reaction, and wash the centrifuged product with ethanol and deionized water for 3 to 4 times, and finally dry the product at 70° C. for 12 hours to obtain polyphosphazene microspheres.

[0059] (2) Weigh 0.6g of polyphosphazene microspheres and 3g of calcium chloride, disperse them in 6 mL of deionized water, stir for 2 hours to fully immerse the activator calcium chloride into the polyphosphazene microspheres, and then centrifuge the above mixed solution And dry at 70° C. for 12 hours to obtain a polyphosphazene microsphere / calcium chloride mixture.

[0060] (3) Put the obtained polyphosphazene microspheres / calcium chloride mixture in a porcelain boat and send it to th...

technical field

[0001] The invention belongs to the technical field of inorganic material chemistry and new energy, and specifically relates to a preparation method and application of nitrogen and phosphorus doped porous carbon spheres. Background technique

[0002] Hydrogen is a renewable and clean energy source with a wide range of sources, and it is also an important industrial raw material. It has become the most ideal fuel for fuel cells and hydrogen internal combustion engines. Due to the low density of hydrogen gas, it is easy to explode, so the key technology of hydrogen energy utilization lies in the storage of hydrogen gas.

[0003] Research and development of hydrogen storage materials with excellent performance is the key to solving the problem of hydrogen energy storage. In recent years, porous carbon materials have become one of the important research objects of hydrogen storage materials due to their advantages such as low density, high specific surface area,...

Examples

Embodiment 1

[0032] (1) In a 150 mL dry flask, add 100 mL of acetonitrile, weigh 0.001 mol of hexachlorocyclotriphosphazene and 0.003 mol of 4,4′-dihydroxydiphenyl sulfone, mix them evenly and add 0.01 mol of three Ethylamine, seal the flask immediately, and react in an ultrasonic cleaner (100W, 40kHz) water bath for 2h at 40°C. Centrifuge after the reaction, and wash the centrifuged product with ethanol and deionized water for 3 to 4 times, and finally dry the product at 80° C. for 24 hours to obtain polyphosphazene microspheres.

[0033] (2) Weigh 0.6g of polyphosphazene microspheres and 0.6g of potassium hydroxide, disperse them in 4 mL of deionized water, stir for 2 hours to fully immerse the activator potassium hydroxide into the polyphosphazene microspheres, and then dissolve the above mixed solution Centrifuge and dry at 80°C for 24 hours to obtain a polyphosphazene microsphere / potassium hydroxide mixture.

[0034](3) Put the obtained polyphosphazene microspheres / potassium hydroxid...

Embodiment 2

[0053] (1) In a 150 mL dry flask, add 50 mL of acetone, weigh 0.001 mol of hexachlorocyclotriphosphazene and 0.0028 mol of 4,4′-diaminodiphenyl sulfone, mix them well and add 0.006 mol of three Ethylamine, seal the flask immediately, and react in an ultrasonic cleaner (100W, 40kHz) water bath for 10h at 20°C. Centrifuge after the reaction, and wash the centrifuged product with ethanol and deionized water for 3 to 4 times, and finally dry the product at 50° C. for 20 hours to obtain polyphosphazene microspheres.

[0054] (2) Weigh 0.6g of polyphosphazene microspheres and 0.3g of sodium hydroxide, disperse them in 2 mL of deionized water, stir for 2 hours to fully immerse the activator sodium hydroxide into the polyphosphazene microspheres, and then dissolve the above mixed solution Centrifuge and dry at 50°C for 20 hours to obtain a polyphosphazene microsphere / sodium hydroxide mixture.

[0055] (3) Put the obtained polyphosphazene microspheres / sodium hydroxide mixture in a por...

Embodiment 3

[0058] (1) In a 150 mL dry flask, add 500 mL of ethanol, weigh 0.001 mol of hexachlorocyclotriphosphazene and 0.0032 mol of hydroquinone, mix well, add 0.012 mol of triethylamine to it, and immediately seal the flask , react in an ultrasonic cleaner (100W, 40kHz) water bath for 1h at 80°C. Centrifuge after the reaction, and wash the centrifuged product with ethanol and deionized water for 3 to 4 times, and finally dry the product at 70° C. for 12 hours to obtain polyphosphazene microspheres.

[0059] (2) Weigh 0.6g of polyphosphazene microspheres and 3g of calcium chloride, disperse them in 6 mL of deionized water, stir for 2 hours to fully immerse the activator calcium chloride into the polyphosphazene microspheres, and then centrifuge the above mixed solution And dry at 70° C. for 12 hours to obtain a polyphosphazene microsphere / calcium chloride mixture.

[0060] (3) Put the obtained polyphosphazene microspheres / calcium chloride mixture in a porcelain boat and send it to th...

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