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Preparing method of Nitorgen-doped carbon nano-material modified by metal cobalt

A nitrogen-doped carbon and nanomaterial technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve problems such as cumbersome steps, large differences in structure and performance between batches, and complicated operations. To achieve the effect of simple operation, stable structure and performance, and easy realization

Active Publication Date: 2017-05-24
美迪森(荆门)生物医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This conventional preparation method has cumbersome steps and complex operations, and the obtained catalysts have large differences in structure and performance between batches due to factors such as preparation conditions and environmental changes. Therefore, a simple and easy-to-realize metal modification The preparation method of nitrogen-doped carbon nanomaterials is of great significance

Method used

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  • Preparing method of Nitorgen-doped carbon nano-material modified by metal cobalt
  • Preparing method of Nitorgen-doped carbon nano-material modified by metal cobalt
  • Preparing method of Nitorgen-doped carbon nano-material modified by metal cobalt

Examples

Experimental program
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Effect test

Embodiment 1

[0029] A method for preparing a metal cobalt-modified nitrogen-doped carbon nanomaterial, the steps of which are:

[0030] A. Add 4g EDTA as a carbon source to a 250mL beaker and add 50mL water;

[0031] B. Stir and adjust the pH value to 7.0 with 10% (m / m, the same below) ammonia solution, at which point the EDTA is completely dissolved;

[0032] C, and then 0.7g of Co(NO 3 ) 2 ·6H 2 O was dissolved in 10 mL of water as a cobalt source and added to the EDTA solution;

[0033] D. After stirring, adjust the pH value to 7.0 with 10% (m / m, the same below) ammonia water again, and place the prepared solution in a rotary evaporator to spin out the water;

[0034] E. Put it in an electric blast drying oven with a temperature of 80°C for 18 hours until a pink granular solid is obtained;

[0035] F. Grind the obtained pink granular solid into a fine powder, put it into a porcelain boat, place it in a vacuum tube type high-temperature sintering furnace for heating and roasting und...

Embodiment 2

[0040] A method for preparing a metal cobalt-modified nitrogen-doped carbon nanomaterial, the steps of which are:

[0041] Add 7g of EGTA as a carbon source into a 250mL beaker, add 80mL of water, stir and adjust the pH value to 7.5 with 7% triethylamine aqueous solution, at this time EGTA is completely dissolved, and then add 1.2g of Co(NO 3 ) 2 ·6H 2 O is used as a cobalt source and dissolved in 10mL of water, and then added to the EGTA solution. After stirring, the pH value is adjusted to 7.5 with 7% triethylamine aqueous solution again. The prepared solution is placed in a rotary evaporator to spin out the water, and then placed at It was placed in an electric blast drying oven at 85°C for 12 hours until a pink granular solid was obtained. The obtained pink granular solid was ground to a fine powder and put into a porcelain boat, and placed in a vacuum tube type high-temperature sintering furnace for heating and roasting under nitrogen protection at a flow rate of 35 mL / ...

Embodiment 3

[0046] A method for preparing a metal cobalt-modified nitrogen-doped carbon nanomaterial, the steps of which are:

[0047] Add 5g EGTA as a carbon source into a 250mL beaker, add 70mL water, stir and adjust the pH value to 7.2 with 9% ethylenediamine solution. At this time, EGTA is completely dissolved, and then 0.8g Co(NO 3 ) 2 ·6H 2 Add O as the cobalt source, add 10mL water to dissolve it, add it to the EGTA solution, adjust the pH value to 7.2 with 9% ethylenediamine solution after stirring, put the prepared solution in a rotary evaporator to spin out the water, and then place it at temperature It was placed in an electric blast drying oven at 82°C for 14 hours until a pink granular solid was obtained. The obtained pink granular solid was ground to a fine powder and put into a porcelain boat, and placed in a vacuum tube type high-temperature sintering furnace for heating and roasting under nitrogen protection at a flow rate of 40 mL / min. During the calcination process, ...

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Abstract

The invention discloses a preparing method of Nitrogen-doped carbon nano-material modified by metal cobalt. The preparing method comprises the first step of adopting Ethylene glycol-bis-(2-aminoethylether)-N,N,N',N'-tetraacetic acid or ethylenediaminetetraacetic acid as a carbon source and adding the carbon source into a beaker; the second step of stirring the carbon source and using a nitrogen source to adjust the ph value of a solution to be neutral till the carbon source is completely dissolved; the third step of adding water into cobalt nitrate or cobalt acetate to dissolve cobalt nitrate or cobalt acetate, putting dissolved cobalt nitrate or cobalt acetate into the solution of which the pH value is already adjusted; the fourth step of stirring the solution and afterwards again adjusting the pH value to be neutral, and putting the prepared solution into a rotary evaporator to spin out moisture; the fifth step of placing the solution to an electrothermal blowing dry box to dry the solution and obtaining a solid body; the sixth step of grinding the obtained solid body into fine powder and placing the fine powder into a porcelain boat, under the condition of the protection of nitrogen, placing the porcelain boat in a vacuum tube type high-temperature sintering furnace to be subjected to heating and roasting to prepare the Nitrogen-doped carbon nano-material modified by metal cobalt. According to the preparing method of the Nitrogen-doped carbon nano-material modified by metal cobalt, the steps of synthesis of carbon nano-materials, doping of nitrogen, and modification of metal ion cobalt are integrated into one, thus the obtained catalyst is large in superficial area, stable in structure and property, and is applicable to heterogeneous catalysis such as epoxidation of alkene.

Description

technical field [0001] The invention belongs to the technical field of nitrogen-doped carbon nanomaterials, and more specifically relates to a preparation method of metal cobalt-modified nitrogen-doped carbon nanomaterials. Nitrogen atoms are introduced into the skeleton of carbon materials, causing dislocation, bending, dislocation, etc. between graphite layers in the carbon layer, and there are defect positions of unpaired electrons. At the same time, the introduction of nitrogen atoms can form local functional groups on the surface of carbon materials, so that the surface of carbon materials has a certain degree of alkalinity, and nitrogen atoms can provide a pair of extranuclear electrons, which can enhance its electrical conductivity, improve the polarity of the material and electron transport. performance etc. Compared with pure materials, nitrogen-doped carbon materials have higher activity and can be used as heterogeneous catalysts by themselves; on the other hand, th...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07D301/04C07D303/04
CPCC07D301/04C07D303/04B01J27/24B01J35/40
Inventor 詹红菊康颖马雪涛沈艳施红杨文豪安梦奇
Owner 美迪森(荆门)生物医药科技有限公司
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