Metal or metal oxide loaded mesoporous carbon material and preparation method thereof

Abstract

The invention provides a metal or metal oxide loaded nano ordered mesoporous carbon material. The nano ordered mesoporous carbon material has the spherical appearance with the diameter of 100-300nm, the specific surface area is 500-600m<2> / g, and the pore diameter is 15-20nm. The invention also provides the preparation method of the material. A soft template method is used, firstly, a carbon precursor with a surface active agent is synthesized, then, by virtue of hydrothermal reaction and roasting, the surface active agent of the carbon precursor is removed, and the metal or metal oxide loaded spherical nano ordered mesoporous material is obtained. The method can realize loading of various different metal components, can be used for effectively regulating the material performance, and is expected to expand the use of the nano ordered mesoporous carbon material. The nano ordered mesoporous carbon material synthesized by the invention is consistent in shape and controllable in size, the metal nano constituents are distributed uniformly, operations are simple in preparation process, and the requirement on equipment is low, so that the nano ordered mesoporous carbon material has industrial practicability.

Description

technical field

[0001] The invention belongs to the field of main group metal oxides, and in particular relates to a preparation method of nano mesoporous materials loaded with metals or metal oxides. Background technique

[0002] According to the definition of the International Union of Pure and Applied Chemistry, ordered mesoporous materials refer to a class of materials with a pore size between 2 and 50 nm, uniform pore size, and regular arrangement. In 1992, Kersge et al. first reported a new type of mesoporous silica material MCM-41 with aluminosilicate as the main component in nature. It has the characteristics of high specific surface area, high thermal stability and hydrothermal stability. It has broad application prospects in petroleum refining, molecular catalysis, separation and adsorption, drug purification, biomedicine and nano-optoelectronic devices. Wang Enjun studied the synthesis of silicon-based mesoporous materials with silicon-based molecular sieves as ...

Examples

Embodiment 1

[0038] Example 1: Preparation of ordered mesoporous carbon materials loaded with Au nanoparticles

[0039] Mix 1.6g of phenol, 5.6mL of formaldehyde, 40mL of NaOH solution with a concentration of 0.1mol / L, 2.56g of F127, and 130mL of water, heat and stir in a water bath at 62°C for 20h to prepare a precursor solution. Get this solution 12mL, 0.6mL concentration be that the chloroauric acid solution of 10g / L, 38mL water are placed in the autoclave of 100mL volume, and this autoclave is airtight, is warming up to 130 ℃ and keeps 24h. After cooling to room temperature, it was ultrasonically cleaned three times with water and ethanol, each time for 15 minutes, and dried at 60°C for 3 hours. After drying, at N 2 The ordered mesoporous carbon materials loaded with Au nanoparticles were obtained by calcination at 700°C for 3 h under atmosphere.

[0040] After structural characterization, the obtained ordered mesoporous carbon material loaded with Au nanoparticles was measured by ni...

Embodiment 2

[0043] Example 2 Preparation of Ag nanoparticles-loaded ordered mesoporous carbon material

[0044] Mix 1.0 g of phenol, 3.5 mL of formaldehyde, 40 mL of NaOH solution with a concentration of 0.1 mol / L, 1.6 g of F127, and 130 mL of water, and heat and stir at 63°C for 18 hours to prepare a precursor solution. Take this solution 12mL, 2mL concentration is the silver nitrate solution of 1.6g / L and 36mL water and place in the autoclave of 100mL volume, this autoclave is airtight, is heated up to 130 ℃ and keeps 20h. After cooling to room temperature, it was washed with ethanol ultrasonically for 3 times, then with water for 2 times, and dried at 50°C for 5 hours. After drying, at N 2 The ordered mesoporous carbon materials loaded with Ag nanoparticles were obtained by calcination at 700°C for 3 h under atmosphere.

[0045]After structural characterization, the ordered mesoporous carbon material loaded with Ag nanoparticles was measured by nitrogen adsorption-desorption experime...

Embodiment 3

[0048] Example 3, preparation of ordered mesoporous carbon material loaded with Pt nanoparticles

[0049] Mix 1.2 g of phenol, 4.2 mL of formaldehyde, 40 mL of NaOH solution with a concentration of 0.1 mol / L, 1.92 g of F127, and 130 mL of water, heat and stir in a water bath at 61 °C for 24 h to prepare a precursor solution. Take 12mL of the precursor solution, 0.6mL of chloroplatinic acid solution with a concentration of 10g / L and 38mL of water in a 100mL autoclave. The autoclave is sealed and heated to 130°C for 24h. After cooling to room temperature, ultrasonically wash with ethanol and water three times each, and dry at 40°C for 6h. After drying, at N 2 The ordered mesoporous carbon materials loaded with Pt nanoparticles were obtained by calcination at 700°C for 3 h under atmosphere.

[0050] After structural characterization, the ordered mesoporous carbon material loaded with Pt nanoparticles was measured by nitrogen adsorption-desorption experiments with a pore diamete...

technical field

[0001] The invention belongs to the field of main group metal oxides, and in particular relates to a preparation method of nano mesoporous materials loaded with metals or metal oxides. Background technique

[0002] According to the definition of the International Union of Pure and Applied Chemistry, ordered mesoporous materials refer to a class of materials with a pore size between 2 and 50 nm, uniform pore size, and regular arrangement. In 1992, Kersge et al. first reported a new type of mesoporous silica material MCM-41 with aluminosilicate as the main component in nature. It has the characteristics of high specific surface area, high thermal stability and hydrothermal stability. It has broad application prospects in petroleum refining, molecular catalysis, separation and adsorption, drug purification, biomedicine and nano-optoelectronic devices. Wang Enjun studied the synthesis of silicon-based mesoporous materials with silicon-based molecular sieves as ...

Examples

Embodiment 1

[0038] Example 1: Preparation of ordered mesoporous carbon materials loaded with Au nanoparticles

[0039] Mix 1.6g of phenol, 5.6mL of formaldehyde, 40mL of NaOH solution with a concentration of 0.1mol / L, 2.56g of F127, and 130mL of water, heat and stir in a water bath at 62°C for 20h to prepare a precursor solution. Get this solution 12mL, 0.6mL concentration be that the chloroauric acid solution of 10g / L, 38mL water are placed in the autoclave of 100mL volume, and this autoclave is airtight, is warming up to 130 ℃ and keeps 24h. After cooling to room temperature, it was ultrasonically cleaned three times with water and ethanol, each time for 15 minutes, and dried at 60°C for 3 hours. After drying, at N 2 The ordered mesoporous carbon materials loaded with Au nanoparticles were obtained by calcination at 700°C for 3 h under atmosphere.

[0040] After structural characterization, the obtained ordered mesoporous carbon material loaded with Au nanoparticles was measured by ni...

Embodiment 2

[0043] Example 2 Preparation of Ag nanoparticles-loaded ordered mesoporous carbon material

[0044] Mix 1.0 g of phenol, 3.5 mL of formaldehyde, 40 mL of NaOH solution with a concentration of 0.1 mol / L, 1.6 g of F127, and 130 mL of water, and heat and stir at 63°C for 18 hours to prepare a precursor solution. Take this solution 12mL, 2mL concentration is the silver nitrate solution of 1.6g / L and 36mL water and place in the autoclave of 100mL volume, this autoclave is airtight, is heated up to 130 ℃ and keeps 20h. After cooling to room temperature, it was washed with ethanol ultrasonically for 3 times, then with water for 2 times, and dried at 50°C for 5 hours. After drying, at N 2 The ordered mesoporous carbon materials loaded with Ag nanoparticles were obtained by calcination at 700°C for 3 h under atmosphere.

[0045]After structural characterization, the ordered mesoporous carbon material loaded with Ag nanoparticles was measured by nitrogen adsorption-desorption experime...

Embodiment 3

[0048] Example 3, preparation of ordered mesoporous carbon material loaded with Pt nanoparticles

[0049] Mix 1.2 g of phenol, 4.2 mL of formaldehyde, 40 mL of NaOH solution with a concentration of 0.1 mol / L, 1.92 g of F127, and 130 mL of water, heat and stir in a water bath at 61 °C for 24 h to prepare a precursor solution. Take 12mL of the precursor solution, 0.6mL of chloroplatinic acid solution with a concentration of 10g / L and 38mL of water in a 100mL autoclave. The autoclave is sealed and heated to 130°C for 24h. After cooling to room temperature, ultrasonically wash with ethanol and water three times each, and dry at 40°C for 6h. After drying, at N 2 The ordered mesoporous carbon materials loaded with Pt nanoparticles were obtained by calcination at 700°C for 3 h under atmosphere.

[0050] After structural characterization, the ordered mesoporous carbon material loaded with Pt nanoparticles was measured by nitrogen adsorption-desorption experiments with a pore diamete...

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