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Preparation method and application of nitrogen-sulfur co-doped graphene for persulfate activation

A technology of activating persulfate and nitrogen-sulfur co-doping, which is applied in the field of graphene to achieve the effect of large specific surface area, less dosage and cost reduction

Inactive Publication Date: 2019-07-05
JIAXING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are no literature and patent reports on nitrogen-sulfur co-doped graphene prepared from graphene (reduced graphene oxide) to activate persulfate oxidation to remove pollutants in water

Method used

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  • Preparation method and application of nitrogen-sulfur co-doped graphene for persulfate activation
  • Preparation method and application of nitrogen-sulfur co-doped graphene for persulfate activation
  • Preparation method and application of nitrogen-sulfur co-doped graphene for persulfate activation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take a certain amount of commercial graphene (IrGO) and thiourea, mix them evenly, and put them into nitrogen gas (N 2 ) Calcined at 350°C in a tube furnace for 30min. The calcination time was 60min at different times, and the heating rate was chosen to be 10°C / min for multiple tests. After cooling to room temperature under a nitrogen atmosphere, the obtained samples were washed three times with ultrapure water and then three times with ethanol. The vacuum drying temperature was 60°C and the drying time was 12h, and finally the test sample IrGO-NS was obtained.

[0038] For the test samples, Quanta400FEG scanning electron microscope (SEM) (FEI, USA) and JEM-2100F high-resolution transmission electron microscope (HRTEM) (JEOL, Japan) were used for morphological analysis of the samples. Surface elemental composition was analyzed using an ESCALAB250XIX-ray photoelectron spectroscopy (XPS) system (ThermoFisher Scientific, USA). Nitrogen adsorption–desorption isotherms, s...

Embodiment 2

[0045]The test sample prepared in Example 1 was taken for the experiment of degrading the preservative methylparaben (MP). In the 15 mg / LMP solution, 20 mg / L IrGO-NS and 307 mg / L PMS were added, and samples were taken at regular intervals, filtered to remove IrGO-NS, and methanol was added to terminate the reaction, and the concentration of MP in the reaction solution was analyzed by HPLC.

[0046] As a comparison, conventional GO and its N-doped samples or classical metal catalysts (nano-Co 3 o 4 and Fe 3 o 4 ) as a catalyst, other conditions are the same as above.

[0047] IrGO-NS was added alone without PMS, and the other conditions were the same as above.

[0048] Add PMS alone, without IrGO-NS, other conditions are the same as above.

[0049] Such as Figure 6 As shown, in the case of less amount of catalyst and oxidant, conventional GO and its N-doped samples or classical metal catalyst (nano-Co 3 o 4 and Fe 3 o 4 ) cannot effectively activate PMS to remove MP....

Embodiment 3

[0051] The test sample prepared in Example 1 was taken to conduct the mineralization effect test of the preservative methylparaben (MP). In the 15 mg / L MP solution, 20 mg / L IrGO-NS and 307 mg / L PMS were added, and samples were taken at regular intervals, filtered to remove IrGO-NS, and the TOC change of the reaction solution was analyzed. Such as Figure 7 It can be seen that 70% TOC can be removed after 30 min. It can be seen that under the experimental conditions, IrGO-NS and PMS have a good mineralization effect on MP.

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Abstract

The invention provides preparation and application of nitrogen-sulfur co-doped graphene for persulfate activation. The preparation comprises the following steps: step 1, selecting raw materials: selecting commercial graphene, thiourea, ultrapure water and ethanol; step 2, performing mixing: uniformly mixing the commercial graphene and the thiourea; step 3, performing calcination: placing the commercial graphene and the thiourea uniformly mixed in the step 2 into a tubular furnace under a nitrogen atmosphere, controlling the temperature at 350-800 DEG C, performing calcination, wherein the heating speed is controlled at 8-12 DEG C / min, performing constant-temperature treatment for 40-80 min, and performing cooling to a room temperature in a nitrogen atmosphere; step 4, performing washing: washing the sample obtained in the step 3 by using the ultrapure water and the ethanol; and step 5, performing drying: placing the sample obtained in the step 4 in a vacuum environment, and performingdrying for 20-28 h to obtain the nitrogen-sulfur co-doped graphene. The invention also provides the application of the prepared nitrogen-sulfur co-doped graphene in water treatment.

Description

technical field [0001] The invention relates to the field of graphene, in particular to a preparation method and application of nitrogen-sulfur co-doped graphene with activated persulfate. Background technique [0002] Traditional water treatment technology is difficult to effectively remove new pollutants in water, and advanced oxidation technology is highly efficient, thorough and economical for the removal of these organic pollutants, so it is widely used in the field of water treatment. In recent years, advanced oxidation technology based on persulfate activation has attracted much attention due to its strong oxidation ability and degradation efficiency. Nanocarbons (such as carbon nanotubes (CNTs), graphene oxide (GO)) have been used as alternative metal-based catalysts for persulfate activation, and heteroatom doping can further enhance their catalytic activity. The oxidation process based on heteroatom-doped carbon materials does not require energy supply and can avo...

Claims

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Application Information

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IPC IPC(8): B01J27/24C02F1/72C02F101/34
CPCB01J27/24C02F1/725C02F2101/34C02F2101/345
Inventor 刘辉孙萍翟志才郭黎吴强施德剑林驰浩方应森吴家强
Owner JIAXING UNIV
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