Co3O4/three-dimensional nitrogen-doped graphene hydrogel catalyst for activating persulfate as well as preparation and use methods of catalyst

A technology of nitrogen-doped graphene and activated persulfate, applied in physical/chemical process catalysts, chemical instruments and methods, oxidized water/sewage treatment, etc., can solve solid-liquid separation problems, limited applications, catalytic activity and stability In order to achieve the effects of high catalytic activity and stability, enhanced catalytic synergy, and a wide range of pH applications

Active Publication Date: 2019-03-22
UNIV OF SCI & TECH LIAONING
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Problems solved by technology

Existing research results show that two-dimensional graphene materials have a certain catalytic synergistic effect, but the supported catalysts prepared as catalyst support materials have certain disadvantages, mainly in: (1) the catalytic performance of two-dimensional graphene materials itself The stability is poor, mainly because there are strong π-π interactions and van der Waals forces between graphene sheets, which can easily lead to agglomeration, resulting in changes in the chemical composition and morphology of the surface.
(2) The nanoscale size of two-dimensional graphene will also bring difficulties to solid-liquid separation; the above defects limit the practical application of this material
At present, the commonly used nitrogen sources for nitrogen doping of graphene materials mainly include ammonium carbonate, urea, melamine, etc., which only play the role of nitrogen doping, and often use a two-step method, which requires a separate heat treatment to complete the formation of structured nitrogen. , the process is cumbersome
Not only that, the preparation method of conventional graphene-based composite catalysts has defects such as uneven distribution of active components on the carrier, large particle size, and low catalytic activity.
[0007] For example, patent CN 104681823 A discloses a kind of nitrogen-doped graphene and Co 3 o 4 Hollow nanosphere composite material and its preparation method and application. The nitrogen source used in the preparation method is melamine, and its function is also only to realize the nitrogen doping of graphene materials. In the preparation method, nitrogen doped graphene materials and supported catalysts The preparation process is relatively cumbersome, and the prepared catalyst is based on nitrogen-doped two-dimensional graphene as a carrier, with Co 3 o 4 Hollow spheres are active components, which have the disadvantages of poor catalytic activity and stability

Method used

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  • Co3O4/three-dimensional nitrogen-doped graphene hydrogel catalyst for activating persulfate as well as preparation and use methods of catalyst
  • Co3O4/three-dimensional nitrogen-doped graphene hydrogel catalyst for activating persulfate as well as preparation and use methods of catalyst
  • Co3O4/three-dimensional nitrogen-doped graphene hydrogel catalyst for activating persulfate as well as preparation and use methods of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Preparation of graphite oxide: Measure 40 mL of concentrated sulfuric acid into a three-necked flask, place in a constant temperature water bath at 4°C, and stir. Weigh 2g natural graphite powder, 1gNaNO 3 and 6gKMnO 4 , were added to the three-neck flask in turn. Then adjust the temperature of the water bath to 20°C, react for 2 hours, then raise the temperature to 35°C, and react for 30 minutes. Then slowly add 90mL of deionized water, control the reaction temperature at 95°C for 20min, remove the flask from the constant temperature water bath, and add 300mL of deionized water and 50mL of H 2 o 2 , and then centrifuged with 10% HCl, then centrifuged with deionized water until no metal ions, SO 4 2- , Cl - , and is neutral. The obtained solid was again filtered through a 300 μm sieve, a polyester fiber column, and centrifuged in a high-speed centrifuge (4000 rpm) for 4 hours to remove a small amount of unoxidized graphite particles. Finally, the obtained vi...

Embodiment 2

[0074] The preparation of graphite oxide was the same as in Example 1, and then 0.2 g of graphite oxide was weighed in 100 mL of deionized water, and ultrasonically dispersed for 1 h to obtain a graphene oxide dispersion; Cobalt was dissolved in 2.5 mL of deionized water, and the pH was adjusted to 8 with ammonia water, then 12.5 mL of the above-mentioned graphene oxide dispersion was added, and the mixture was sonicated for 60 min. Then, the above mixed solution was put into a 25mL high-pressure hydrothermal reactor, and reacted at 180°C for 12h to form Co 3 o 4 / 3D N-GN hydrogel. Finally, the prepared hydrogel was washed 3 to 5 times with deionized water to completely remove impurities.

[0075] After testing, the Co obtained in this example 3 o 4 / 3D N-GN hydrogel, Co 3 o 4 Accounting for 15.0% of the total mass, the nitrogen-doped three-dimensional graphene accounts for 85.0% of the total mass; the mass percentage of nitrogen in the nitrogen-doped three-dimensional g...

Embodiment 3

[0080] The preparation of graphite oxide was the same as in Example 1, and then weighed 0.3g of graphite oxide in 100mL of deionized water, ultrasonically dispersed for 1h, and dissolved 0.038g of acrylamide, 0.3mg of ammonium persulfate and 0.027g of cobalt nitrate hexahydrate in 2.5mL of deionized In water, adjust the pH to 8 with ammonia water, then add 12.5 mL of the above-mentioned graphene oxide dispersion, and sonicate for 60 min. Then, the above mixed solution was put into a high-pressure hydrothermal reactor, and reacted at 200°C for 14 hours to form Co 3 o 4 / 3D N-GN hydrogel. Finally, the prepared hydrogel was washed 3 to 5 times with deionized water to completely remove impurities.

[0081] After testing, the Co obtained in this example 3 o 4 / 3D N-GN hydrogel, Co 3 o 4 Accounting for 9.0% of the total mass, nitrogen-doped three-dimensional graphene accounts for 91.0% of the total mass; the mass percentage of nitrogen in nitrogen-doped three-dimensional graph...

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Abstract

The inventions aims at solving the problem of a supported Co3O4 catalyst for treating nitrobenzene wastewater, provides a Co3O4 / three-dimensional nitrogen-doped graphene hydrogel catalyst for activating persulfate as well as preparation and use methods of the catalyst, and belongs to the technical field of nitrobenzene wastewater treatment. The catalyst is high in catalytic activity, long in service life and easy to separate and recover, and can permanently and efficiently activate the persulfate. According a preparation method of the catalyst, the catalyst is prepared with a hydrothermal method by taking cobalt nitrate as a precursor, natural graphite powder as a main raw material and acrylamide as a nitrogen source. The method is simple, convenient and efficient. By means of polyacrylamide formed by the polymerization of the acrylamide, the nitrogen doping of three-dimensional graphene and the formation and uniform loading of fine-grained Co3O4 by one-step reaction are realized synchronously, so that not only is the catalytic synergy of pyridine nitrogen enhanced carriers fully utilized, but also the catalytic action of Co3O4 is enhanced, and the catalytic performance of the overall catalyst is significantly improved.

Description

technical field [0001] The invention belongs to the technical field of nitrobenzene wastewater treatment, in particular to a heterogeneous loaded catalyst Co 3 o 4 / Three-dimensional nitrogen-doped graphene hydrogel and methods of making and using the same. Background technique [0002] Nitrobenzene (NB), also known as dense spot oil and bitter almond oil, is a colorless or apricot-yellow oily liquid with a bitter almond flavor. It is often used in the production of explosives, dyes, spices and other organic synthesis industries. Nitrobenzene has high stability and biological toxicity in water, and is extremely harmful to humans and animals. It has been listed as one of the priority environmental pollutants in my country. Nitrobenzene is a kind of refractory organic compound. It is difficult to achieve the ideal removal effect by common wastewater treatment methods, such as adsorption method and biological method, so it must be treated in depth. [0003] At present, advan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C02F1/72C02F101/38
CPCB01J27/24B01J35/0013C02F1/725C02F2101/38
Inventor 李丽华陶永康任立兄王鑫梁玉高鑫宇
Owner UNIV OF SCI & TECH LIAONING
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