Method for loading nanometer metal phosphide on porous carbon

Abstract

The invention discloses a method for loading nano metal phosphide on porous carbon, and belongs to the technical field of nano material preparation. Using sugar as a carbon source, phosphate (phosphoric acid) and metal salts can form a uniform mixed system under certain conditions. After dehydration and carbonization, porous carbon is formed in situ, and then the metal is formed into phosphorus under high-temperature reducing gas heat treatment. phosphides to prepare porous carbon-supported transition metal phosphide materials. In the present invention, by changing the synthesis conditions such as raw material ratio, reaction time and heat treatment temperature, the loaded nanometer material with simultaneously controllable load capacity, particle size and composition can be obtained. The whole process has the advantages of simple operation, low cost, abundant and easy-to-obtain raw materials, etc., and has great application prospects in many aspects such as industrial catalysis, electrochemistry, and hydrodesulfurization and denitrification of oil products.

Description

technical field

[0001] The invention provides a method for preparing porous carbon-loaded nano metal phosphides, which belongs to the technical field of nano material preparation. Background technique

[0002] Nanomaterials have unique properties that are obviously different from bulk materials and single molecules, such as surface effects, volume effects, and macroscopic tunnel effects, making them widely used in electronics, optics, chemical engineering, ceramics, biology, and medicine. Application prospect.

[0003] Due to their unique structural properties, such as high specific surface area, uniform distribution of mesopores, better hydrothermal stability, and chemical inertness, porous carbon materials have been widely used in the fields of adsorption and separation, catalysis, and conductive materials. In the field of catalysis, porous carbon has been proved to be an excellent catalyst support. At present, there have been a large number of reports on the preparation...

Examples

Embodiment 1

[0028] Example 1: Porous carbon loaded MoP

[0029] Synthetic raw materials: glucose, ammonium dihydrogen phosphate, ammonium molybdate

[0030] (1) Weigh 1g glucose, 0.01g ammonium dihydrogen phosphate and 0.1g ammonium molybdate (H 24 Mo 7 N 6 o 24 ?4H 2 O) Put it in a 100ml beaker, then grind the medicine in the beaker with a mortar for 10 minutes, and then heat it to form a molten state;

[0031] (2) Put the molten material in (1) in a crucible tank and put it in a tube furnace, and put the sample at 800°C H 2 Calcined under the same conditions for 5 hours, a dark brown bulky solid was obtained, which was determined to be molybdenum carbide (MoP) supported on porous carbon by XRD.

Embodiment 2

[0032] Example 2: Porous carbon loaded nano WP

[0033] Synthetic raw materials: glucose, ammonium dihydrogen phosphate, ammonium tungstate

[0034] (1) Weigh 2g glucose, 0.5g ammonium dihydrogen phosphate, 0.3g ammonium tungstate ((NH 4 )10H 2 (W 2 o 7 ) 6 ) in a 100mL beaker, heated and stirred to form a molten state;

[0035] (2) Afterwards, put the beaker into an oven at 120°C and react for 4 hours to obtain a dark brown puffy solid.

[0036] (3) Grind the product obtained in (2) with a mortar and put it in a crucible. The product obtained from the reaction was heated at 800°C 2 Under the condition of heat treatment for 7 hours, the porous carbon supported WP was obtained.

Embodiment 3

[0037] Example 3: Porous carbon loaded nano-Ni 2 P

[0038] Synthetic raw materials: sucrose, ammonium dihydrogen phosphate, nickel nitrate

[0039] (1) Weigh 3g sucrose, 0.5g ammonium dihydrogen phosphate and 2.5g nickel nitrate (Ni(NO 3 ) 2 ·6H 2O) Put it in a 100mL beaker, then place the beaker in a heatable magnetic stirrer, raise the temperature of the magnetic stirrer to 120°C, and keep stirring for 10min until the drug in the beaker forms a molten state.

[0040] (2) Afterwards, put the molten liquid into an oven at 180°C and react for 48 hours to obtain a dark brown fluffy solid.

[0041] (3) Grind the product obtained in (2) with a mortar and put it in a crucible. The product obtained from the reaction was heated at 700°C in 5% H 2 / Ar heat treatment for 5 hours to obtain porous carbon supported Ni 2 p.

technical field

[0001] The invention provides a method for preparing porous carbon-loaded nano metal phosphides, which belongs to the technical field of nano material preparation. Background technique

[0002] Nanomaterials have unique properties that are obviously different from bulk materials and single molecules, such as surface effects, volume effects, and macroscopic tunnel effects, making them widely used in electronics, optics, chemical engineering, ceramics, biology, and medicine. Application prospect.

[0003] Due to their unique structural properties, such as high specific surface area, uniform distribution of mesopores, better hydrothermal stability, and chemical inertness, porous carbon materials have been widely used in the fields of adsorption and separation, catalysis, and conductive materials. In the field of catalysis, porous carbon has been proved to be an excellent catalyst support. At present, there have been a large number of reports on the preparation...

Examples

Embodiment 1

[0028] Example 1: Porous carbon loaded MoP

[0029] Synthetic raw materials: glucose, ammonium dihydrogen phosphate, ammonium molybdate

[0030] (1) Weigh 1g glucose, 0.01g ammonium dihydrogen phosphate and 0.1g ammonium molybdate (H 24 Mo 7 N 6 o 24 ?4H 2 O) Put it in a 100ml beaker, then grind the medicine in the beaker with a mortar for 10 minutes, and then heat it to form a molten state;

[0031] (2) Put the molten material in (1) in a crucible tank and put it in a tube furnace, and put the sample at 800°C H 2 Calcined under the same conditions for 5 hours, a dark brown bulky solid was obtained, which was determined to be molybdenum carbide (MoP) supported on porous carbon by XRD.

Embodiment 2

[0032] Example 2: Porous carbon loaded nano WP

[0033] Synthetic raw materials: glucose, ammonium dihydrogen phosphate, ammonium tungstate

[0034] (1) Weigh 2g glucose, 0.5g ammonium dihydrogen phosphate, 0.3g ammonium tungstate ((NH 4 )10H 2 (W 2 o 7 ) 6 ) in a 100mL beaker, heated and stirred to form a molten state;

[0035] (2) Afterwards, put the beaker into an oven at 120°C and react for 4 hours to obtain a dark brown puffy solid.

[0036] (3) Grind the product obtained in (2) with a mortar and put it in a crucible. The product obtained from the reaction was heated at 800°C 2 Under the condition of heat treatment for 7 hours, the porous carbon supported WP was obtained.

Embodiment 3

[0037] Example 3: Porous carbon loaded nano-Ni 2 P

[0038] Synthetic raw materials: sucrose, ammonium dihydrogen phosphate, nickel nitrate

[0039] (1) Weigh 3g sucrose, 0.5g ammonium dihydrogen phosphate and 2.5g nickel nitrate (Ni(NO 3 ) 2 ·6H 2O) Put it in a 100mL beaker, then place the beaker in a heatable magnetic stirrer, raise the temperature of the magnetic stirrer to 120°C, and keep stirring for 10min until the drug in the beaker forms a molten state.

[0040] (2) Afterwards, put the molten liquid into an oven at 180°C and react for 48 hours to obtain a dark brown fluffy solid.

[0041] (3) Grind the product obtained in (2) with a mortar and put it in a crucible. The product obtained from the reaction was heated at 700°C in 5% H 2 / Ar heat treatment for 5 hours to obtain porous carbon supported Ni 2 p.

Images