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An iron-nitrogen-carbon composite material containing a single-atom active site, and its preparation and application method

A composite material and active site technology, applied in chemical instruments and methods, physical/chemical process catalysts, oxidized water/sewage treatment, etc., can solve the problem of increasing the amount of slag at the end of water treatment, poor activation effect of persulfate, etc. problem, to achieve the effect of less iron dissolution, low equipment requirements, and improved degradation efficiency

Active Publication Date: 2022-03-08
CENT SOUTH UNIV
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Problems solved by technology

[0005] The main purpose of the present invention is to provide an iron-nitrogen-carbon composite material containing a single-atom active site, and its preparation and application methods, aiming to solve the problem of poor activation of persulfate in the prior art and increased water treatment Technical problems of back-end slag volume

Method used

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  • An iron-nitrogen-carbon composite material containing a single-atom active site, and its preparation and application method
  • An iron-nitrogen-carbon composite material containing a single-atom active site, and its preparation and application method
  • An iron-nitrogen-carbon composite material containing a single-atom active site, and its preparation and application method

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preparation example Construction

[0047] In order to obtain a substance capable of efficiently activating peroxymonosulfate, the present invention also provides a preparation method, which can be used to prepare the iron-nitrogen-carbon composite material as described in any of the above-mentioned embodiments, and the preparation method includes steps:

[0048] S1, dissolving a nitrogen-containing carbon source in an ethanol solution to obtain a solution A; wherein, the nitrogen-containing carbon source includes: one or more of melamine, dicyandiamide, and urea.

[0049] In addition, as another expanded option, the nitrogen-containing carbon source may also include: one or more of the melamine, the dicyandiamide, and the urea formed with glucose and / or sucrose The mixture, that is: the mixture formed after one or more of the melamine, the dicyandiamine, and the urea are selected and then mixed with glucose and / or sucrose can also be used as the present invention nitrogenous carbon source.

[0050] S2, dispers...

Embodiment 1

[0072] A method for preparing an iron-nitrogen-carbon composite material containing a single-atom active site, the specific steps are as follows:

[0073] 1. Weigh 10g of dicyandiamide and place it in 500ml of 75% alcohol solution, raise the temperature to 60°C, and ultrasonicate for 1 hour to prepare solution A.

[0074] 2. Weigh 200 mg of hemin and place it in solution A, and disperse it by ultrasonic for 3 hours; then evaporate at 60°C to complete dryness to obtain the mixed substance B.

[0075] 3. Grind the mixed substance B evenly, raise the temperature to 350°C at a heating rate of 3°C / min, keep at this temperature for 3 hours, continue to raise the temperature to 650°C at the same heating rate, and keep it for 5 hours. The temperature was lowered to room temperature, and then the cooled material was pickled, and finally the product was washed with deionized water to neutrality, and dried at 60°C to obtain an iron-nitrogen-carbon composite material containing a single-a...

Embodiment 2

[0087] According to the method of Example 1, the only difference is that the amount of hemin in step 2 is changed to 100 mg.

[0088] The material obtained by the above method is denoted as Fe SA(100)-g-C 3 N 4 , which contains a graphite-like carbon nitride support and iron single atoms combined with the support.

[0089] Such as figure 1 as shown, figure 1 Middle curve is Fe SA-g-C prepared in embodiment 1, embodiment 2, embodiment 3 3 N 4 powder diffraction (XRD) spectrum.

[0090] Depend on figure 1 It can be seen that the Fe SA(100)-g-C synthesized in Example 2 3 N 4 Only the peak of graphitic phase carbon nitride appears in the XRD spectrum of XRD, indicating that Fe is highly dispersed in it, and there is no Fe element or its compound nanoparticles, thereby forming and improving the activation of persulfate.

[0091] Furthermore, by the ICP-OES method, Fe SA(100)-g-C could be detected 3 N 4 In , the loading of Fe atoms is 1.32wt%.

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Abstract

The invention provides an iron-nitrogen-carbon composite material containing a single-atom active site, including a support containing graphite-like carbon nitride, and a single iron atom combined with the support, thereby improving the catalysis of peroxymonosulfate Active, and avoid a large amount of metal ion dissolution. The preparation method includes the step: S1, dissolving the nitrogen-containing carbon source in an ethanol solution to obtain solution A; wherein, the nitrogen-containing carbon source includes: one or more of melamine, dicyandiamide, and urea Kind; S2, disperse the iron-containing metal precursor in the solution A, and then evaporate to dryness to obtain a mixed substance B; wherein, the iron-containing metal precursor includes hemin and iron phthalocyanine one or both; S3, the mixed material B is sequentially subjected to grinding and mixing treatment, pyrolysis treatment, and cooling treatment, and the material obtained after the cooling treatment is sequentially subjected to pickling treatment, water washing treatment, and drying treatment , to obtain the iron-nitrogen-carbon composite material.

Description

technical field [0001] The invention relates to the technical field of advanced oxidation, in particular to an iron-nitrogen-carbon composite material containing a single-atom active site, and a preparation and application method thereof. Background technique [0002] For the emerging trace organic pollutants in water bodies, such as antibiotics, endocrine disruptors, pharmaceuticals and personal care products, the commonly used biological treatment technology cannot handle them well, so it is necessary to develop pretreatment and subsequent treatment Technology, combined with biological treatment technology can achieve good treatment effect. [0003] Persulfate is a stable solid at room temperature, which is convenient for transportation and storage. It is a green oxidant and has been officially included in the catalog of drinking water disinfectants by the country. It can be activated by heat, alkali, transition metals, and microwaves. It can be activated to efficiently d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24C02F1/72
CPCB01J27/24C02F1/725
Inventor 刘恢赵飞平付迎雪柴立元闵小波向开松唐崇俭沈锋华柯勇
Owner CENT SOUTH UNIV
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