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A controllable preparation method of highly dispersed nanometer metal element/carbon composite material and its electrocatalytic application

A carbon composite material and nano-metal technology, which is used in the preparation of high-dispersion metal elemental nano-particle materials and the field of high-content mesoporous carbon loading, which can solve problems such as poor shock load resistance, secondary pollution by metal ions, and complex processes. , to achieve the effect of high loading, adjustable metal content and high reactivity

Active Publication Date: 2018-12-04
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In comparison, the physical method of removing nitrate is not selective, and the pollutants are not really degraded, but only transferred or concentrated; the commonly used biological denitrification method converts nitrate into nitrogen through the reduction of microorganisms, but this method The ability to resist impact load is poor, the process is complex, and there are problems such as secondary pollution; the chemical reduction method mainly includes the reduction method of metal element, catalytic reduction and electrochemical method
The elemental metal reduction method mainly uses iron, aluminum, zinc and other metal elements as reducing agents. The problem is that the reaction product is difficult to convert into harmless nitrogen, and secondary pollution such as metal ions will be generated.
[0005] The research on the dispersion of nano-zero-valent iron with mesoporous carbon as a carrier has been reported, but a nano-zero-valent iron / mesoporous carbon material with small particles, uniform dispersion and high loading is obtained through controlled synthesis. challenge question

Method used

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  • A controllable preparation method of highly dispersed nanometer metal element/carbon composite material and its electrocatalytic application
  • A controllable preparation method of highly dispersed nanometer metal element/carbon composite material and its electrocatalytic application

Examples

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Embodiment 1

[0030]Preparation of phenolic resin and surface oxidized ordered mesoporous carbon material: first melt 12.0 g of phenol in a water bath at 40-42 °C, add 2.52 g of 20% (mass percent concentration) NaOH aqueous solution, stir for 10 minutes, and then add 20.4 g formaldehyde solution (37 wt%), reflux at 70-75°C for 1 hour, and cool to room temperature. The pH of the solution was adjusted to neutral with 0.6 M HCl. The solution system was placed in a water bath at 45°C and distilled under reduced pressure for 1-2 hours to obtain 14.1 g of phenolic resin (molecular weight 200-500). Dissolve it in 56.2 g of absolute ethanol, centrifuge to remove NaCl crystals, and prepare a light brown phenolic resin prepolymer ethanol solution with a mass fraction of 20% for later use. Add 1.6 g of nonionic surfactant polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (Pluronic F127) and 1.0 g of 0.2 M HCl to 8.0 g of ethanol at 40 °C Stirring for 1 hour gave a clear so...

Embodiment 2

[0032] Preparation of zero-valent iron-supported mesoporous carbon materials: 0.6 g surface oxidized mesoporous carbon materials were stirred and dispersed in 8.0 g ethanol; at the same time, 0.9 g Fe(NO 3 ) 3 9H 2 O was dissolved in ethanol to form a solution with a mass fraction of 20 wt%, and 0.5 mL of 0.2 M HCl was added to inhibit Fe(NO 3 ) 3 9H 2 Hydrolysis of O. Add the dissolved solution to the carbon ethanol dispersion system, continue to stir, and keep in the fume hood until the ethanol evaporates to dryness. Put the obtained composite material into a small glass tube, place the glass tube in a polytetrafluoroethylene bottle filled with 14 wt% ammonia solution, keep the sample out of direct contact with the ammonia solution, seal it and treat it at 60°C for 3 hours, cool it, and water Wash with ethanol and filter to remove soluble impurities on the surface of the sample to obtain loaded Fe(OH) 3 mesoporous carbon materials. The composite material was dried in ...

Embodiment 3

[0034] Preparation of cobalt-supported mesoporous carbon material: the preparation method is as in Example 2, the difference is that 1.0 g Co(NO 3 ) 3 9H 2 O was dissolved in ethanol to prepare a solution with a mass fraction of 20 wt%.

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Abstract

The invention relates to a method for preparing a highly dispersed nanometal element / carbon composite material and its electrocatalytic application. It synthesizes an ordered mesoporous carbon powder material with a high specific surface; and oxidizes the material to obtain a surface with hydrophilic groups and Mesoporous carbon with high specific surface area; the metal precursor is infused through the impregnation method, and converted into hydroxide by ammonia fumigation method and fixed in the mesoporous confined pores; reduced at high temperature under H2, and finally highly dispersed nanometers are obtained Metallic / mesoporous carbon composites. Taking zero-valent iron / mesoporous carbon as an example, this composite material is used as a working electrode, and a three-electrode electrochemical method is used to reduce and remove nitrate in water through electrocatalysis. The composite material obtained by the present invention has small elemental metal nanoparticles and is evenly dispersed in the pores of the carbon substrate. It is easy to control the crystallization degree and loading amount of the metal during the preparation process; after being made into an electrode sheet, the nitrate treatment efficiency is high , improved nitrogen selectivity, good stability, and no secondary pollution such as metal ion dissolution.

Description

technical field [0001] The invention provides a preparation method and application of a nanocomposite material that uses electrocatalytic reduction to remove nitrate in water, belongs to the field of pollutant control and removal, and relates to a mesoporous carbon-loaded high-content, high-dispersion metal elemental nanoparticle material method of preparation. Background technique [0002] With the rapid development of the economy, the use of a large amount of nitrogenous fertilizers, the unreasonable disposal of domestic and industrial wastewater and sludge, and the increasing nitrate content in surface water and groundwater in many countries and regions, it has become a very common and serious problem. environmental issue. The increase of nitrogen in natural water will cause eutrophication of water and the outbreak of algal blooms. At the same time, excessive intake of nitrate in drinking water will be converted into nitrite in the human body, thereby inducing methemoglo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745B01J23/75B01J35/02C02F1/461C02F1/467C02F101/16B01J35/00
CPCC02F1/461C02F1/4676B01J23/745B01J23/75C02F2101/16B01J35/50
Inventor 滕玮张伟贤范建伟冉献强杨建平吕梦华许华伟
Owner TONGJI UNIV