CN114505087B - Preparation of copper monatomic catalyst and application of copper monatomic catalyst in degradation of organic pollutants - Google Patents

Preparation of copper monatomic catalyst and application of copper monatomic catalyst in degradation of organic pollutants Download PDF

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CN114505087B
CN114505087B CN202210418419.3A CN202210418419A CN114505087B CN 114505087 B CN114505087 B CN 114505087B CN 202210418419 A CN202210418419 A CN 202210418419A CN 114505087 B CN114505087 B CN 114505087B
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copper
catalyst
nitrogen
graphene
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CN114505087A (en
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李杨
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Beijing Single Atom Catalysis Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B01J37/088—Decomposition of a metal salt
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/722—Oxidation by peroxides
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C02F2101/345—Phenols
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant
    • C02F2305/026—Fenton's reagent
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention provides a preparation method of a copper monatomic catalyst and application of the copper monatomic catalyst in degradation of organic pollutants. According to the invention, a copper monoatomic/nitrogen-doped graphene catalyst is used for activating peroxodisulfate so as to degrade organic pollutants in water. In the catalyst, Cu is loaded on aza-graphene in a single atomic site state, the loading amount of Cu is 0.2-6wt% based on the total weight of the catalyst, and the balance is carrier nitrogen-doped graphene.

Description

Preparation of copper monatomic catalyst and application of copper monatomic catalyst in degradation of organic pollutants
Technical Field
The invention relates to the technical field of using a monatomic catalyst for removing organic matters in water, and belongs to the technical field of sewage treatment.
Background
Water is the source of life, and people's life is closely related to water resources. However, with the growth of the population and the development of industrialization, the problems of shortage of water resources and pollution become more serious. Among them, organic pollutants in high-concentration organic wastewater are difficult to be removed by physical means, and thus development of efficient chemical means for removing organic pollutants in water has received much attention from researchers. The high-concentration organic wastewater generally refers to wastewater with COD of more than 2000 mg/L discharged by industries such as papermaking, leather, food and the like. The wastewater is mainly classified into three types according to the nature and source of the wastewater: (1) the high-concentration organic wastewater which does not contain harmful substances and is easy to biodegrade is generally derived from industrial wastewater which takes agricultural and pastoral products as raw materials, such as food industrial wastewater, (2) the high-concentration organic wastewater which contains harmful substances and is easy to biodegrade is mainly derived from light industry, metallurgical industry and the like, such as pharmaceutical industry wastewater, and (3) the high-concentration organic wastewater which contains harmful substances and is difficult to biodegrade. It is mainly from organic synthesis chemical industry, pesticide production industry and the like, such as pesticide wastewater. The pollutant components in the high-concentration organic wastewater are complex, and the high-concentration organic wastewater poses serious threats to human health and ecological environment after being discharged into a human water body. Therefore, how to effectively treat, recycle and reuse the wastewater is an important issue.
Advanced Oxidation Processes (AOPs) have attracted considerable attention in recent years as a powerful technique for the removal of refractory organic contaminants. Wherein, the persulfate is used as the oxidant to catalyze and degrade the organic pollutants, which shows attractive application prospect, and mainly comprises peroxymonosulfate (PMS, HSO) 5 - ) And peroxodisulfates (PDS, S) 2 O 8 2- ). They are promising AOP oxidizing agents due to their simplicity of operation as oxidizing agents and the variety of organic species that can be removed. However, since persulfate needs catalytic activation in the catalysis process to degrade organic pollutants, how to activate persulfate with high efficiency is a key factor for degrading organic pollutants. Recently, due to its unique structural characteristics, monatomic catalyst has attracted much attention in activating persulfate to degrade pollutants: (Angew. Chem. Int. Ed. 2021, 60, 21751-21755; J. Am. Chem. Soc. 2018, 140, 12469-12475;Angew. Chem. Int. Ed. 2021, 60, 4588-4593; Angew. Chem. Int. Ed.2021, 60, 22513-22521.). However, the studies on the monatomic activation of persulfate are still in the preliminary stage, and the monatomic catalyst reported so far is mainly used for the activation of PMS, and the monatomic catalyst for the activation of PDS is rarely reported. However, it is noted that PDS has more advantages than PMS, such as cheaper price (0.16 USD/mol for PDS vs. 1.36 USD/mol for PMS) ((PMS))Environ. Sci. Technol.2014, 48, 5868-Chem. Eng. J.2017, 330, 44-62.). Therefore, SAC with appropriate active sites needs to be designed to activate PDS for effective organic contaminant removal.
Disclosure of Invention
The invention discloses a method for degrading organic pollutants in water, which is characterized in that copper monoatomic/nitrogen-doped graphene (Cu) is used 1 Perperoxodisulfate (PDS) is used in the presence of catalysts of the structure/NG) for degrading organic pollutants in water. In the presence of a catalyst comprising a metal oxide,cu is loaded on aza-graphene in a single atomic site state, the loading amount of Cu is 0.2-6wt%, preferably 2-4wt% based on the total weight of the catalyst, and the balance is carrier nitrogen-doped graphene.
Cu 1 in/NG, the subscript 1 of Cu indicates that copper is present in a monoatomic state, and/NG indicates that copper is supported on an NG carrier.
The organic pollutants are phenolic compounds which are easily oxidized and degraded, and oxygen-containing or nitrogen-containing heterocyclic compounds, and comprise: bisphenol A (BPA), phenol, 2, 4-Dichlorophenol (DCP), Ciprofloxacin (CIP) or rhodamine B (RhB) and other compounds.
The peroxodisulfate is selected from potassium peroxodisulfate or sodium peroxodisulfate.
The invention discovers that when the Cu loading is between 2 and 4 weight percent, the catalytic activation PDS has the highest activity of degrading pollutants in water, and the higher loading or the lower loading reduces the PDS degradation activity.
The invention also discloses the copper monoatomic/nitrogen-doped graphene (Cu) 1 A method for producing a catalyst of the structure/NG), characterized in that the method comprises:
s1: mixing and stirring graphene and copper-containing salt solution, and removing a solvent to obtain a mixture;
s2: respectively placing the obtained mixture and the nitrogen-releasing small molecular compound in devices with the same reaction space for calcination to obtain the catalyst;
wherein the content of the first and second substances,
in the step S1, the copper salt in the copper-containing salt solution is soluble copper salt selected from copper chloride, copper nitrate, copper sulfate, copper acetate and copper ammonia complex, and the solvent is selected from water and/or C 1-4 An alcohol solvent, preferably methanol or ethanol; the solvent removal can be carried out by common means, including but not limited to evaporation, heating evaporation, vacuum evaporation; evaporation by heating to remove the solvent is preferred.
In the step S2, the nitrogen-releasing small molecule compound is selected from one or more of dicyandiamide, urea or melamine; the calcination is carried out at the temperature of 400-800 ℃, the calcination atmosphere is nitrogen or argon, and the calcination time is 2-8 hours; the device with the same reaction space comprises a tube furnace, a muffle furnace or a high-temperature kiln.
Further, in the S1 step, graphene may be dispersed in C in advance 1-4 Among alcohols, methanol or ethanol is preferred; the stabilizer can be added during the mixing and stirring, and the stabilizer is selected from polyvinylpyrrolidone.
In the step S2, the calcination may be performed with flowing nitrogen gas, and the nitrogen-releasing small molecule compound may be placed upstream of the gas flow and the mixture obtained in the corresponding step S1 may be placed downstream.
The invention further discloses an application of the copper monatomic/nitrogen-doped graphene catalyst, which comprises the step of activating peroxodisulfate to degrade organic pollutants in water by using the copper monatomic/nitrogen-doped graphene prepared by the method as the catalyst, wherein the peroxodisulfate is selected from potassium peroxodisulfate or sodium peroxodisulfate.
The noun explains:
and (2) PDS: peroxodisulfate (S2O 82-).
PMS: peroxymonosulfate (HSO) 5 - ）。
NG: and (3) nitrogen-doped graphene.
Fenton reaction: and (4) performing Fenton reaction.
Has the advantages that:
compared with the prior art, the catalyst provided by the invention can efficiently activate PDS to degrade organic pollutants in water, and compared with PMS, the catalyst provided by the invention has the advantages that the use cost is reduced, and the degradation efficiency is improved. In addition, the method can degrade various organic matters such as bisphenol A (BPA), phenol, 2, 4-Dichlorophenol (DCP), Ciprofloxacin (CIP) and rhodamine B (RhB), and has wide application in various industrial scenes.
Drawings
FIG. 1 shows Cu in example 1 of the present invention 1 High angle annular dark field scanning transmission electron microscope (HAADF-STEM) image of/NG monatomic catalyst.
FIG. 2 shows Cu in example 1 of the present invention 1 Spherical aberration corrected high angle annular dark field scanning Transmission Electron microscopy (AC-HAADF-STEM) images of NG monatomic catalysts.
FIG. 3 shows the results of example 1 of the present inventionCu 1 K-edge Fourier transform extended absorption fine structure (EXAFS) spectrum of/NG monatomic catalyst Cu.
FIG. 4 shows Cu in example 1 of the present invention 1 Performance diagram of degrading pollutant bisphenol A in water by activating PDS through NG monatomic catalyst.
FIG. 5 is a graph showing the performance of Cu1/NG monatomic catalyst activated PDS in examples 1-4 of the present invention in degrading bisphenol A as a contaminant in water.
FIG. 6 is a performance diagram of the Cu1/NG monatomic catalyst activated PDS degrading pollutants bisphenol A, phenol, 2, 4-Dichlorophenol (DCP), Ciprofloxacin (CIP) and rhodamine B (RhB) in water in example 1 of the invention.
FIG. 7 is a graph showing the degradation of bisphenol A as a contaminant in water by the activated PDS of example 1 and comparative examples 1-3.
Detailed Description
Example 1
Cu 1 The synthesis procedure for a monatomic catalyst with a NG loading of 2.9 wt.% was as follows: firstly, 60 mg of graphene is dispersed in 15 mL of ethanol, and then 9.75 mg of CuCl is added under the stirring condition 2 · 4H 2 O in 5 mL ethanol and 120 mg polyvinylpyrrolidone (PVP). After that, the resulting mixture solution was stirred at 75 ℃ until the ethanol was evaporated to dryness. Then, the resultant mixture and 5.0 g of dicyandiamide were respectively placed in two porcelain burners located in the downstream and upstream directions, respectively, in a tube furnace. The tube furnace was heated to 700 ℃ at a heating rate of 3 ℃ per min under flowing nitrogen and held at 700 ℃ for 2 hours. After the reaction is finished, Cu can be obtained under the tube furnace 1 /NG-2.9 wt%。
Example 2
The specific implementation conditions are the same as example 1, except that the amount of copper added in the catalyst synthesis process is changed to 3.36 mg, and Cu is obtained 1 A monatomic catalyst with a NG loading of 1 wt%.
Example 3
The specific implementation conditions are the same as example 1, except that the addition amount of copper is changed to 0.68mg during the catalyst synthesis process, and Cu is obtained 1 A monatomic catalyst with a NG loading of 0.2 wt%.
Example 4
The specific implementation conditions are the same as example 1, except that the amount of copper added in the catalyst synthesis process is changed to 16.9mg, and Cu is obtained 1 A monatomic catalyst with a NG loading of 5 wt%.
Comparative example 1
CuCl purchased from Chinese medicine 2 · 4H 2 O is used as a catalyst.
Comparative example 2
CuO was purchased as a catalyst.
Comparative example 3
Referring to the method of example 1, nitrogen-doped graphene NG was prepared without adding metal.
Application test experiments
The Fenton reaction performance of the samples was evaluated in a 100 mL beaker at 25. + -. 0.2 ℃ with a magnetic stirring speed of 500 rpm. In a typical experiment, 5 mg of catalyst was first dispersed in 50 mL of a solution containing 20 mg/L of organics and 10 mM Phosphate Buffered Saline (PBS), pH 7.2. Then, an oxidant (potassium peroxodisulfate, PDS, 0.5 mM) was added to the solution to start the catalytic degradation experiment. At predetermined time intervals, 0.5 mL of liquid sample was collected and rapidly filtered through a 0.22 μm polyethersulfone filter, and then detected by HPLC (LC-20A, Shimadzu, Japan) and UV-vis detector.
The organics were tested separately: bisphenol a (bpa), phenol, 2, 4-Dichlorophenol (DCP), Ciprofloxacin (CIP) and rhodamine b (rhb), the test results are shown in fig. 6.
Catalyst test example 1 Cu loading of 2.9wt% Cu 1 /NG catalyst, example 2 Cu loading of 1wt% Cu 1 NG catalyst and CuCl 2 (comparative example 1), CuO (comparative example 2), NG (comparative example 3) several catalysts or comparative catalysts. The results of the correlation measurements are shown in FIG. 7.
And (4) conclusion:
FIGS. 1 and 2 are TEM photographs of the catalyst of example 1, and FIG. 3 is an EXAFS spectrum of the catalyst of example 1. The above map shows that: the copper atom of example 1 is present in a monoatomic state.
As shown in FIG. 4, the catalyst of example 1 is better for activating the degradation of bisphenol A in water by PDS.
As shown in fig. 5, the effect of activating PDS degradation is different for catalysts with different Cu loading, and the results show that the loading has a large influence on the activation performance of PDS. Especially Cu with a loading of 2.9wt% 1 The catalytic effect of/NG was stronger than the lower loading of 1wt% and the higher loading of 5wt% catalyst.
As shown in FIG. 6, the catalyst of the present invention has a good catalytic effect on Fenton reactions of different organic substances, and can activate PDS to remove corresponding organic pollutants.
As shown in FIG. 7, the results of the comparative experiment showed that Cu 1 The catalytic effect of the/NG is better than that of pure Cu 2+ NG and CuO.

Claims (10)

1. A method for degrading organic pollutants in water, characterized in that peroxodisulfate is used to degrade the organic pollutants in water in the presence of a catalyst of copper monatomic/nitrogen-doped graphene, wherein Cu is supported on aza-graphene in a monatomic site state, the Cu loading is 2-6wt% based on the total weight of the catalyst, and the balance is carrier nitrogen-doped graphene, and the peroxodisulfate is selected from potassium peroxodisulfate or sodium peroxodisulfate.
2. The method of claim 1, wherein the loading of Cu is 2 to 4wt% based on the total weight of the catalyst, with the remainder being supported nitrogen-doped graphene.
3. The method of claim 1 or 2, wherein the organic contaminant is a phenolic compound or an oxygen-or nitrogen-containing heterocyclic compound susceptible to oxidative degradation.
4. The method of claim 3, wherein the organic contaminant is bisphenol A, phenol, 2, 4-dichlorophenol, ciprofloxacin, or rhodamine B.
5. A method for preparing a catalyst for copper monatomic/nitrogen-doped graphene used in claim 1 or 2, wherein the method comprises:
s1: mixing and stirring graphene and copper-containing salt solution, and removing a solvent to obtain a mixture;
s2: respectively placing the obtained mixture and the nitrogen-releasing small molecular compound in devices with the same reaction space for calcination to obtain the catalyst;
wherein the content of the first and second substances,
the copper salt in the copper-containing salt solution is soluble copper salt; the solvent is selected from water and/or C 1-4 An alcohol solvent; the nitrogen-releasing small molecular compound is selected from one or more of dicyandiamide, urea or melamine; the device with the same reaction space comprises a tubular furnace, a muffle furnace or a high-temperature kiln.
6. The method according to claim 5, wherein in the step S1, the copper salt is selected from one or more of copper chloride, copper nitrate, copper sulfate, copper acetate, and copper ammonia complex.
7. The method as claimed in claim 5, wherein in the step S2, the calcination is performed at 400-800 ℃, the calcination atmosphere is nitrogen or argon, and the calcination time is 2-8 hours.
8. The method of claim 5, wherein in the step of S1, the graphene is pre-dispersed in C 1-4 In alcohol; and adding a stabilizer during mixing and stirring, wherein the stabilizer is polyvinylpyrrolidone.
9. The method of claim 5, wherein the calcining in the flowing nitrogen gas is performed in S2, and the nitrogen-releasing small molecule compound is placed upstream of the gas flow and the mixture obtained in the corresponding S1 is placed downstream.
10. Use of the catalyst prepared according to any one of claims 5 to 9, wherein said use comprises the activation of peroxodisulphates selected from potassium peroxodisulphate or sodium peroxodisulphate in order to degrade organic pollutants in water, using said copper monatomic/nitrogen doped graphene catalyst.
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