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Preparation method of nitrogen-doped ordered mesoporous carbon supported transition metal nanoparticle catalyst

A transition metal and nanoparticle technology, used in catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of high nanoparticle dispersion and small particle size, and achieve good activity and selectivity. Effect

Inactive Publication Date: 2018-08-03
NANTONG LONGXIANG NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are almost no reports on the preparation of nitrogen-doped ordered mesoporous carbon-supported transition metal nanoparticle catalysts using 1,10-phenanthroline as a nitrogen source in one step, and this method can obtain small particle size (<30nm), nanoparticle Catalyst with high dispersion and good stability

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  • Preparation method of nitrogen-doped ordered mesoporous carbon supported transition metal nanoparticle catalyst

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Embodiment 1

[0018] see Figure 1-4 , the present invention provides the following technical scheme: a preparation method of a nitrogen-doped ordered mesoporous carbon-supported transition metal nanoparticle catalyst, comprising the following steps:

[0019] A. Put 10g of phenol into a round-bottomed flask, add 2.13g of 20wt% NaOH solution in a water bath at 40°C, stir for 10min-13min, then add 17g of 37wt% formaldehyde solution dropwise, and then heat up to 70°C-80°C Stir the reaction for 1 h, cool to room temperature, then drop in 0.6 mol / L HCl to adjust the pH value of the reaction system to 7.0, then remove water by rotary evaporation, and dilute the obtained yellow oily product to 20 wt% phenolic resin with absolute ethanol Ethanol solution for standby;

[0020] B. Dissolve 1.6g F127 in 8g absolute ethanol at 42°C, stir until F127 is completely dissolved, add 5.0g 20wt% phenolic resin ethanol solution, then add 3g dissolved in 0.15g nickel nitrate hexahydrate, cobalt nitrate hexahydr...

Embodiment 2

[0025] A method for preparing a nitrogen-doped ordered mesoporous carbon-supported transition metal nanoparticle catalyst, comprising the following steps:

[0026] A. Put 10g of phenol into a round-bottomed flask, add 2.13g of 20wt% NaOH solution in a water bath at 42°C, stir for 13min, then add 17g of 37wt% formaldehyde solution dropwise, then heat up to 80°C, stir for 1h, and cool to room temperature, then drop 0.6mol / L of HCl to adjust the pH value of the reaction system to 7.0, then remove water by rotary evaporation, and dilute the obtained yellow oily product with absolute ethanol to 20wt% phenolic resin ethanol solution for subsequent use;

[0027] B. Dissolve 1.6g F127 in 8g absolute ethanol at 42°C, stir until F127 is completely dissolved, add 5.0g 20wt% phenolic resin ethanol solution, then add 3g dissolved in 0.15g nickel nitrate hexahydrate, cobalt nitrate hexahydrate, nitric acid nonahydrate Any one of iron, 0.1g acetylacetone and 0.10gl, 10-phenanthroline ethanol...

Embodiment 3

[0032] A method for preparing a nitrogen-doped ordered mesoporous carbon-supported transition metal nanoparticle catalyst, comprising the following steps:

[0033] A. Put 10g of phenol into a round-bottomed flask, add 2.13g of 20wt% NaOH solution in a water bath at 41°C, stir for 12min, then add 17g of 37wt% formaldehyde solution dropwise, then raise the temperature to 75°C, stir for 1h, and cool to room temperature, then drop 0.6mol / L of HCl to adjust the pH value of the reaction system to 7.0, then remove water by rotary evaporation, and dilute the obtained yellow oily product with absolute ethanol to 20wt% phenolic resin ethanol solution for subsequent use;

[0034] B. Dissolve 1.6g F127 in 8g absolute ethanol at 42°C, stir until F127 is completely dissolved, add 5.0g 20wt% phenolic resin ethanol solution, then add 3g dissolved in 0.15g nickel nitrate hexahydrate, cobalt nitrate hexahydrate, nitric acid nonahydrate Any one of iron, 0.2g acetylacetone and 0.2gl, 10-phenanthr...

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Abstract

The invention discloses a preparation method of a nitrogen-doped ordered mesoporous carbon supported transition metal nanoparticle catalyst. In the preparation method, the nitrogen-doped ordered mesoporous carbon supported transition metal nanoparticle catalyst is prepared from acetylacetone and 1,10-phenanthroline as complexing agents as well as a nitrogen source with a one-step method for the first time. The catalyst is good in dispersity and uniform in nanoparticle size distribution. The catalyst has good activity and selectivity for hydrogenation of aromatic nitro-compounds in aqueous solutions.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic nanometer materials, in particular to a preparation method of a nitrogen-doped ordered mesoporous carbon-loaded transition metal nanoparticle catalyst. Background technique [0002] According to the definition of porous materials given by the International Union of Pure and Applied Chemistry (IUPAC), according to the size of their pore diameters, they can be divided into three categories: microporous materials with a pore size less than 2 nm; mesoporous materials with a pore size of 2 nm. -50nm; the pore diameter of the macroporous material is greater than 50nm. Mesoporous materials have the characteristics of extremely high specific surface area, regular and orderly pore structure, narrow pore size distribution, and continuously adjustable pore size, making it suitable for the adsorption and separation of macromolecules that are difficult for many microporous zeolite molecular si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/02B01J37/08B01J35/00
CPCB01J27/24B01J37/082B01J37/084B01J35/23B01J35/40
Inventor 倪伟汪学广盛瑶邹秀晶尚兴付
Owner NANTONG LONGXIANG NEW MATERIALS TECH CO LTD
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