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Controllable high-dispersion nano simple-substance metal/carbon composite material preparation method and electrical catalytic application thereof

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

Active Publication Date: 2016-10-26
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

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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  • Controllable high-dispersion nano simple-substance metal/carbon composite material preparation method and electrical catalytic application thereof
  • Controllable high-dispersion nano simple-substance metal/carbon composite material preparation method and electrical catalytic application thereof

Examples

Experimental program
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Effect test

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-loaded mesoporous carbon material: the preparation method is as in Example 2, the difference is that 1.0g 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 controllable high-dispersion nano simple-substance metal / carbon composite material preparation method and electrical catalytic application thereof. An ordered mesoporous carbon powder material having high specific area is synthesized; the material is subjected to oxidation treatment to obtain mesoporous carbon provided with hydrophilic groups on the surface and having high specific area; metal precursor perfusion is performed by adopting an impregnation method, the mesoporous carbon is converted into hydroxide by adopting an ammonia fumigation method, and the hydroxide is fixed in mesoporous confined pore channels; reduction is performed at high temperature in the presence of H2, and finally a high-dispersion nano metal simple-substance / carbon composite material is obtained. With zero-valent iron / mesoporous carbon as an example, the composite material serves as a working electrode, a three-electrode electrochemical method is adopted to remove nitrate in a water body through electrical catalytic reduction. The composite material prepared by adopting the preparation method contains small simple-substance metal nanoparticles which are evenly dispersed in the pore channels of a carbon substrate, and the metal crystallization degree and supporting amount are easy to control in the preparation process. After electrode slices are produced, the nitrate treatment efficiency is high, the nitrogen selectivity is improved, the stability is good, and secondary pollution such as metal ion dissolution is not caused.

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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IPC IPC(8): B01J23/745B01J23/75B01J35/02C02F1/461C02F1/467C02F101/16
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
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