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Graphene-based hollow cobaltous sulfide nanocrystal capable of efficiently activating persulfate and preparation method thereof

A technology for activating persulfate and graphene, which is applied in the direction of graphene, cobalt sulfide, chemical instruments and methods, etc., can solve the problem of low internal site utilization, low electrical conductivity, and the density of catalytic sites on the surface of solid cobalt sulfide Low-level problems, achieve rapid treatment of pollutants, overcome large dosage, significant environmental and economic significance

Active Publication Date: 2018-10-26
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalyst activity is still limited by the low conductivity of CoS4
Kong et al. synthesized graphene-supported solid cobalt sulfide in one step by solvothermal method for use as lithium-ion batteries and photocatalysts (Kong et al. Morphological Effect of Graphene Nanosheets on Ultrathin CoSNanosheets and Their Applications for High-Performance Li-Ion Batteries and Photocatalysis, J .Phys.Chem.C 2014,118,25355-25364), but the density of catalytic sites on the surface of solid cobalt sulfide is low, and the utilization rate of internal sites is not high

Method used

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  • Graphene-based hollow cobaltous sulfide nanocrystal capable of efficiently activating persulfate and preparation method thereof
  • Graphene-based hollow cobaltous sulfide nanocrystal capable of efficiently activating persulfate and preparation method thereof
  • Graphene-based hollow cobaltous sulfide nanocrystal capable of efficiently activating persulfate and preparation method thereof

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Experimental program
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Embodiment 1

[0031] A graphene-based hollow cobalt sulfide nanocrystal capable of efficiently activating persulfate and a preparation method thereof, the steps of which are:

[0032] a. Preparation of graphene oxide-based zeolite-type imidazolate framework 67: Graphene oxide is uniformly dispersed in water by ultrasound to obtain a graphene oxide dispersion with a concentration of 3 mg / mL, and then cobalt nitrate hexahydrate is added to it at a concentration of 12 mg / mL mL, stirred at room temperature for 0.5-2 hours to adsorb cobalt ions on the surface of graphene oxide, then added 2-methylimidazole aqueous solution with a concentration of 54 mg / mL, stirred at room temperature for 5-30 minutes, then centrifuged, washed with water, and dried to obtain Graphene oxide-based zeolitic imidazolate frameworks67.

[0033] b. Preparation of graphene oxide-based hollow cobalt tetrasulfide: the graphene oxide-based zeolite-type imidazolate framework 67 obtained in step a is uniformly dispersed in et...

Embodiment 2

[0039] With embodiment 1, difference is:

[0040] The concentration of graphene oxide dispersion in step a is 0.5mg / mL;

[0041] In step b, the concentration of the graphene oxide-based zeolite-type imidazolate framework 67 ethanol dispersion is 3mg / mL, the concentration of thioacetamide is 4.5mg / mL, the solvothermal reaction temperature is 140°C, and the reaction time is 6h;

[0042] In step c, the inert protective gas is argon, and the heating rate is 10° C. / min.

[0043] The degradation rate of the obtained catalyst to bisphenol A within 8 minutes under the same experimental conditions as in Example 1 was 88%.

Embodiment 3

[0045] With embodiment 1, difference is:

[0046] The concentration of cobalt nitrate hexahydrate in step a is 20mg / mL, and the concentration of 2-methylimidazole is 90mg / mL;

[0047] In step b, the concentration of the graphene oxide-based zeolite-type imidazolate framework 67 ethanol dispersion is 1 mg / mL, the concentration of thioacetamide is 1.5 mg / mL, the solvothermal reaction temperature is 120 ° C, and the reaction time is 3 h;

[0048] The obtained catalyst had a degradation rate of 99% to bisphenol A within 8 minutes under the same experimental conditions as in Example 1.

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Abstract

The invention belongs to the field of environmental catalyst synthesis and discloses a graphene-based hollow cobaltous sulfide nanocrystal capable of efficiently activating persulfate and a preparation method thereof. The preparation method comprises the following steps: growing a zeolite-type imidazate frame 67 on the surface of graphene oxide by a precipitation method; taking the imidazate frame67 as a self-template, taking thioacetamide as a sulfur source, and preparing cobaltosic sulfide of a hollow structure by virtue of a solvothermal reaction; and finally, calcining in an inert atmosphere, converting the cobaltosic sulfide into hollow cobaltous sulfide by virtue of desulfurization reaction, and reducing graphene oxide into graphene, thereby obtaining the graphene-based hollow cobaltous sulfide nanocrystal. The hollow cobaltous sulfide nanocrystal prepared by the method disclosed by the invention has the advantages of high catalytic activity, high free radical yield, simple recycling and the like, can achieve the effects of enhancing the conventional oxidation method, obviously shortening the reaction time and greatly reducing the usage amount of the catalyst and oxidizing agent, and has obvious technical and economic advantages.

Description

technical field [0001] The invention belongs to the field of environmental catalyst synthesis, and relates to a graphene-based hollow cobalt sulfide nanocrystal capable of efficiently activating persulfate and a preparation method thereof. Background technique [0002] The uncontrolled discharge of organic waste water from industry, life and medicine has caused more and more serious water pollution. For highly toxic and persistent organic substances, physical and chemical methods such as traditional adsorption and membrane treatment can only transfer but are difficult to reduce their toxicity. Microorganisms in biochemical methods are not very tolerant to highly toxic organic substances, and the treatment effect is not good. Advanced oxidation technology can degrade or even mineralize organic matter, can significantly reduce its toxicity and improve biodegradability, and can be placed at the front or end of the water treatment process to achieve efficient removal of organic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184C01G51/00B82Y40/00B82Y30/00B01J27/043B01J35/02C02F1/72C02F101/30B01J35/00
CPCB82Y30/00B82Y40/00C01B32/184C01G51/30C02F1/725B01J27/043C01P2004/03C01P2004/04C01P2004/64C02F2101/30B01J35/50B01J35/40
Inventor 刘福强朱长青凌晨江昊吴海德李爱民
Owner NANJING UNIV
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