CN115465881A - Synthesis method of electron-rich n-CuO material rich in oxygen vacancies - Google Patents

Synthesis method of electron-rich n-CuO material rich in oxygen vacancies Download PDF

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CN115465881A
CN115465881A CN202210949731.5A CN202210949731A CN115465881A CN 115465881 A CN115465881 A CN 115465881A CN 202210949731 A CN202210949731 A CN 202210949731A CN 115465881 A CN115465881 A CN 115465881A
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electron
cuo
cuo material
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CN115465881B (en
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李发堂
刘宇萌
宁萌
郝影娟
王晓静
刘瑞红
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Hebei University of Science and Technology
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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
    • 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
    • B01J35/39—
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00—Compounds of copper
    • C01G3/02—Oxides; Hydroxides
    • 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
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
    • 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
    • C02F2101/36—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
    • C02F2305/10—Photocatalysts

Abstract

The invention provides a preparation method of an electron-rich n-CuO material rich in oxygen vacancies, belonging to the field of material synthesis and photocatalysis. Uniformly mixing copper nitrate trihydrate, ammonium salt, urea or aminoacetic acid, then placing the mixture on an electronic furnace, heating the mixture, continuously stirring the mixture until a solution is formed, then carrying out combustion reaction to form a catalyst precursor rich in oxygen vacancies, and calcining the obtained precursor in a muffle furnace at the temperature of 300-700 ℃ to remove residual impurities, thus obtaining the pure n-CuO material. Compared with the prior art, the method provided by the invention has the advantages that the intrinsic defect of CuO is regulated and controlled by creating a reducing atmosphere through fuel combustion, and the electron-rich n-CuO material with the oxygen vacancy-rich structure is successfully prepared. Under visible light, the synthesized electron-rich n-CuO material rich in oxygen vacancies has higher tetracycline hydrochloride degradation capability.

Description

Synthesis method of electron-rich n-CuO material rich in oxygen vacancies
Technical Field
The invention relates to a method for synthesizing an electron-rich n-CuO material rich in oxygen vacancies, belonging to the technical field of material synthesis and environmental protection.
Background
Copper oxide (CuO) is structurally stable, relatively low cost, non-toxic, and one of the materials that has attracted attention in recent decades (george et al. Mater lett.281 (2020) 128603). CuO itself contains metal defects, so CuO prepared in most cases is a p-type semiconductor (Bae et al. Nat. Commun.8 (2017) 1-8). For p-type semiconductors, in the application of photocatalytic degradation of pollutants, many molecules are holes, and the holes have certain oxidizing power and can be used for oxidizing pollutants, however, the band gap of the conventional p-CuO is narrow, the valence band is usually between 0.50V and 2.00V (Qamar et al acs appl. Mater. Interfaces 7 (2015) 8757-8769), the valence band is low, and the oxidizing power is weak, so that the p-CuO cannot achieve a good pollutant degradation effect. Therefore, researchers have adopted microwave methods, hydrothermal methods and the like to control the shape and the size of the p-CuO so as to further improve the photocatalytic degradation activity of the p-CuO (Bhattacharjee et al. J Photoshop Photobiolo A353 (2017) 215-228). However, these methods are not only complicated to operate, but also have limited improvement effects because they fail to degrade contaminant radicals.
Disclosure of Invention
The invention aims to solve the problems in the prior art, provides a simple and convenient method for synthesizing an electron-rich n-CuO material rich in oxygen vacancies, and aims to solve the problems that the traditional p-CuO has poor photocatalytic degradation performance, and the traditional modification method is complex and is not beneficial to large-scale production.
The idea of the invention is as follows: from the viewpoint of radical activation, if an electron-rich n-type CuO semiconductor can be synthesized, it is undoubtedly beneficial to improve the degradation ability of the electron-activated molecular oxygen by generating active oxidation species such as superoxide anion, hydroxyl radical and the like. The technical scheme of the invention is that through a solution combustion method, the type and the dosage of fuel are designed and regulated to enable combustion to generate reducing atmosphere, oxygen atoms on the surface of CuO are induced to escape to change intrinsic defects of the material, cuO oxygen vacancies rich in oxygen vacancies are prepared, cuO can exist in an n-type semiconductor mode, and the traditional free radical degradation way is changed.
The technical scheme adopted by the invention is as follows:
a method for synthesizing an electron-rich n-CuO material rich in oxygen vacancies comprises the following steps:
a. uniformly mixing raw materials of copper nitrate trihydrate, ammonium salt and urea or aminoacetic acid, putting the raw materials into an electronic universal furnace for heating, continuously stirring, and gradually melting the raw materials to form a solution;
b. and continuously heating the solution, carrying out self-combustion reaction on the solution to form catalyst precursor powder rich in oxygen vacancies, cooling the catalyst precursor powder to room temperature, placing the cooled catalyst precursor powder in a muffle furnace, and calcining the cooled catalyst precursor powder to obtain the electron-rich n-CuO material rich in oxygen vacancies.
Preferably, in the step a, the molar ratio of copper nitrate trihydrate, ammonium salt, urea or glycine is 1.0: (0 to 0.75): (0.125-2.0).
Further preferably, in the step a, the molar ratio of copper nitrate trihydrate, ammonium salt, urea or glycine is 1.0: (0.1-0.75): (0.67-1.5).
In the step a, the ammonium salt is one or a compound of 2-bromoethylamine hydrobromide, diethylamine hydrochloride, tetrabutylammonium bromide, tetramethylammonium iodide and tetraethylammonium iodide.
And in the step b, the muffle furnace calcining temperature is 300-700 ℃, and the temperature is kept for 1-6 hours continuously.
Preferably, in the step b, the muffle furnace calcination temperature is 400-550 ℃, and the heat preservation is continuously carried out for 3-4 hours.
Preferably, the method for synthesizing the electron-rich n-CuO material rich in oxygen vacancies comprises the following specific steps:
uniformly mixing copper nitrate trihydrate, tetramethylammonium iodide and glycine according to a molar ratio (1;
the solution is subjected to spontaneous combustion reaction, is cooled to room temperature and then is placed in a muffle furnace, and the temperature is kept at 400 ℃ for 4 hours, so that the electron-rich n-CuO material rich in oxygen vacancies is obtained.
Preferably, the method for synthesizing the electron-rich n-CuO material rich in oxygen vacancies comprises the following specific steps:
the molar ratio of 1.0:2.0 taking copper nitrate trihydrate and urea, uniformly mixing, heating in an electronic universal furnace, and gradually melting the raw materials to form a solution;
and (3) carrying out spontaneous combustion reaction on the solution, cooling to room temperature, placing in a muffle furnace, keeping the temperature at 550 ℃ for 3 hours to obtain the oxygen vacancy-rich electron-rich n-CuO material.
Compared with the prior art, the invention has the outstanding effects that:
the n-CuO photocatalyst is synthesized based on the idea of generating oxygen vacancies induced by reducing atmosphere, the prepared n-CuO photocatalyst has the structure rich in electrons, and is more favorable for activating electron acceptors, and the existence of the oxygen vacancies is favorable for adsorbing reactant molecules and improving the carrier separation efficiency, so that the capability and the effect of degrading pollutants are improved.
The preparation method of the electron-rich n-CuO material rich in oxygen vacancies provided by the invention is simple, rapid and low in cost.
The product of the invention is applied to degrading pollutants, has wide application prospect in the technical field of environmental protection, and can be produced in large scale.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of n-CuO prepared in examples 1 to 6.
FIG. 2 is a UV-visible Diffuse Reflectance (DRS) spectrum of n-CuO prepared in examples 1-6.
FIG. 3 is an electron spin resonance (EPR) spectrum of n-CuO prepared in examples 1-6.
FIG. 4 is a graph showing tetracycline hydrochloride degradation of n-CuO prepared in examples 1 to 6.
Detailed Description
The invention is further illustrated by the accompanying drawings and the detailed description.
Table 1 below shows Hall Effect test tables for preparing n-CuO in examples 1 to 6.
TABLE 1
Figure BDA0003788682730000041
Example 1:
5.436g of copper nitrate trihydrate, 0.725g of tetrabutylammonium bromide and 0.45g of urea (1.0. And (3) carrying out spontaneous combustion reaction on the solution, cooling to room temperature, placing in a muffle furnace, keeping the temperature at 300 ℃ for 6 hours to obtain the oxygen vacancy-rich electron-rich n-CuO material.
XRD, DRS, EPR, tetracycline hydrochloride degradation and hall effect tests were performed on the samples as shown in fig. 1, fig. 2, fig. 3, fig. 4 and table 1, respectively.
The XRD pattern in figure 1 shows that the diffraction peak of the prepared n-CuO material is well matched with the monoclinic CuO crystal face, which indicates that the prepared sample is a pure monoclinic n-CuO material.
The sample has strong visible light absorption as shown by the DRS profile of figure 2.
The n-CuO material is enriched in oxygen vacancies as shown by the EPR test in accordance with figure 3.
According to a tetracycline hydrochloride degradation test shown in FIG. 4, the degradation performance of the n-CuO material is better than that of commercial p-CuO, which proves that the prepared electron-rich n-CuO material rich in oxygen vacancies is beneficial to the improvement of photocatalytic activity.
According to the Hall effect calculation result in the table 1, the Hall coefficient is negative, and the successful preparation of the oxygen vacancy enriched electron enriched n-CuO material is proved.
Example 2
5.436g of copper nitrate trihydrate, 2.703g of diethylamine hydrochloride, and 0.9g of urea (1.0.
The solution is subjected to spontaneous combustion reaction, is cooled to room temperature and then is placed in a muffle furnace, and is kept at 450 ℃ for 4 hours, so that the electron-rich n-CuO material rich in oxygen vacancies is obtained.
XRD, DRS, EPR, tetracycline hydrochloride degradation and hall effect tests were performed on the samples as shown in fig. 1, fig. 2, fig. 3, fig. 4 and table 1, respectively.
The XRD spectrum in figure 1 shows that the diffraction peak of the prepared n-CuO material is well matched with the monoclinic CuO crystal face, which indicates that the prepared sample is a pure monoclinic n-CuO material.
The sample has strong visible light absorption as shown by the DRS profile of figure 2.
The n-CuO material is enriched in oxygen vacancies as shown by the EPR test of FIG. 3.
According to a tetracycline hydrochloride degradation test shown in FIG. 4, the degradation performance of the n-CuO material is better than that of commercial p-CuO, which proves that the prepared electron-rich n-CuO material rich in oxygen vacancies is beneficial to the improvement of photocatalytic activity.
According to the Hall effect calculation result in the table 1, the Hall coefficient is negative, and the successful preparation of the oxygen vacancy enriched electron enriched n-CuO material is proved.
Example 3
4.832g of copper nitrate trihydrate and 2.402g of urea (1.0. The solution is subjected to spontaneous combustion reaction, is cooled to room temperature and then is placed in a muffle furnace, and the temperature is kept at 550 ℃ for 3 hours, so that the electron-rich n-CuO material rich in oxygen vacancies is obtained.
XRD, DRS, EPR, tetracycline hydrochloride degradation and hall effect tests were performed on the samples as shown in fig. 1, fig. 2, fig. 3, fig. 4 and table 1, respectively.
The XRD pattern in figure 1 shows that the diffraction peak of the prepared n-CuO material is well matched with the monoclinic CuO crystal face, which indicates that the prepared sample is a pure monoclinic n-CuO material.
The sample has strong visible light absorption as shown by the DRS profile of figure 2.
The n-CuO material is enriched in oxygen vacancies as shown by the EPR test of FIG. 3.
According to the tetracycline hydrochloride degradation test shown in FIG. 4, the degradation performance of the n-CuO material is better than that of the commercial p-CuO, which proves that the prepared electron-rich n-CuO material rich in oxygen vacancies is beneficial to the improvement of the photocatalytic activity.
According to the Hall effect calculation result in the table 1, the Hall coefficient is negative, and the successful preparation of the oxygen vacancy enriched electron enriched n-CuO material is proved.
Example 4
5.436g of copper nitrate trihydrate, 3.375g of tetramethylammonium iodide, and 0.18g of urea (1. The solution is subjected to spontaneous combustion reaction, is cooled to room temperature and then is placed in a muffle furnace, and the temperature is kept at 700 ℃ for 1 hour, so that the electron-rich n-CuO material rich in oxygen vacancies is obtained.
XRD, DRS, EPR, tetracycline hydrochloride degradation and hall effect tests were performed on the samples as shown in fig. 1, fig. 2, fig. 3, fig. 4 and table 1, respectively.
The XRD spectrum in figure 1 shows that the diffraction peak of the prepared n-CuO material is well matched with the monoclinic CuO crystal face, which indicates that the prepared sample is a pure monoclinic n-CuO material.
The sample has strong visible light absorption as shown by the DRS profile of figure 2.
The n-CuO material is enriched in oxygen vacancies as shown by the EPR test in accordance with figure 3.
According to a tetracycline hydrochloride degradation test shown in FIG. 4, the degradation performance of the n-CuO material is better than that of commercial p-CuO, which proves that the prepared electron-rich n-CuO material rich in oxygen vacancies is beneficial to the improvement of photocatalytic activity.
According to the Hall effect calculation result in the table 1, the Hall coefficient is negative, and the successful preparation of the oxygen vacancy rich electron rich n-CuO material is proved.
Example 5
5.436g of copper nitrate trihydrate, 3.015g of tetramethylammonium iodide, and 1.125g of glycine (1. The solution is subjected to spontaneous combustion reaction, is cooled to room temperature and then is placed in a muffle furnace, and is kept at 400 ℃ for 4 hours to obtain the oxygen vacancy-rich electron-rich n-CuO material.
XRD, DRS, EPR, tetracycline hydrochloride degradation and hall effect tests were performed on the samples as shown in fig. 1, fig. 2, fig. 3, fig. 4 and table 1, respectively.
The XRD pattern in figure 1 shows that the diffraction peak of the prepared n-CuO material is well matched with the monoclinic CuO crystal face, which indicates that the prepared sample is a pure monoclinic n-CuO material.
The sample has strong visible light absorption as shown by the DRS profile of figure 2.
The n-CuO material is enriched in oxygen vacancies as shown by the EPR test in accordance with figure 3.
According to a tetracycline hydrochloride degradation test shown in FIG. 4, the degradation performance of the n-CuO material is better than that of commercial p-CuO, which proves that the prepared electron-rich n-CuO material rich in oxygen vacancies is beneficial to the improvement of photocatalytic activity.
According to the Hall effect calculation result in the table 1, the Hall coefficient is negative, and the successful preparation of the oxygen vacancy enriched electron enriched n-CuO material is proved.
Example 6
5.436g of copper nitrate trihydrate, 2.701g of diethylamine hydrochloride, and 2.518g of glycine (1. The solution is subjected to spontaneous combustion reaction, is cooled to room temperature and then is placed in a muffle furnace, and the temperature is kept at 600 ℃ for 5 hours, so that the electron-rich n-CuO material rich in oxygen vacancies is obtained.
XRD, DRS, EPR, tetracycline hydrochloride degradation and hall effect tests were performed on the samples as shown in fig. 1, fig. 2, fig. 3, fig. 4 and table 1, respectively.
The XRD pattern in figure 1 shows that the diffraction peak of the prepared n-CuO material is well matched with the monoclinic CuO crystal face, which indicates that the prepared sample is a pure monoclinic n-CuO material.
The sample has strong visible light absorption as shown by the DRS profile of figure 2.
The n-CuO material is enriched in oxygen vacancies as shown by the EPR test in accordance with figure 3.
According to a tetracycline hydrochloride degradation test shown in FIG. 4, the degradation performance of the n-CuO material is better than that of commercial p-CuO, which proves that the prepared electron-rich n-CuO material rich in oxygen vacancies is beneficial to the improvement of photocatalytic activity.
According to the Hall effect calculation result in the table 1, the Hall coefficient is negative, and the successful preparation of the oxygen vacancy enriched electron enriched n-CuO material is proved.

Claims (8)

1. A method for synthesizing an electron-rich n-CuO material rich in oxygen vacancies is characterized by comprising the following steps:
a. uniformly mixing raw materials of copper nitrate trihydrate, ammonium salt and urea or aminoacetic acid, placing the raw materials in an electronic universal furnace for heating, continuously stirring, and gradually melting the raw materials to form a solution;
b. and continuously heating the solution, carrying out self-combustion reaction on the solution to form catalyst precursor powder rich in oxygen vacancies, cooling the catalyst precursor powder to room temperature, placing the cooled catalyst precursor powder in a muffle furnace, and calcining to obtain the electron-rich n-CuO material rich in oxygen vacancies.
2. The method for synthesizing an oxygen vacancy enriched electron rich n-CuO material of claim 1, wherein in step a, the molar ratio of copper nitrate trihydrate, ammonium salt, urea or glycine is 1.0: (0 to 0.75): (0.125-2.0).
3. The method for synthesizing an oxygen vacancy rich, electron rich, n-CuO material of claim 2, wherein in step a, the molar ratio of copper nitrate trihydrate, ammonium salt, urea or glycine is 1.0: (0.1-0.75): (0.67-1.5).
4. The method for synthesizing an electron rich n-CuO material rich in oxygen vacancies of claim 1, wherein in the step a, the ammonium salt is one or a combination of 2-bromoethylamine hydrobromide, diethylamine hydrochloride, tetrabutylammonium bromide, tetramethylammonium iodide and tetraethylammonium iodide.
5. The method for synthesizing an electron rich n-CuO material rich in oxygen vacancies as claimed in claim 1, wherein the step b, the muffle calcination temperature is 300-700 ℃ and the holding time is 1-6 hours.
6. The method for synthesizing an electron rich n-CuO material rich in oxygen vacancies as claimed in claim 5, wherein in the step b, the muffle calcination temperature is 400-550 ℃ and the temperature is kept for 3-4 hours.
7. The method for synthesizing an oxygen vacancy rich electron-rich n-CuO material of claim 1, comprising the steps of:
uniformly mixing copper nitrate trihydrate, tetramethylammonium iodide and glycine according to a molar ratio (1;
the solution is subjected to spontaneous combustion reaction, is cooled to room temperature and then is placed in a muffle furnace, and is kept at 400 ℃ for 4 hours to obtain the oxygen vacancy-rich electron-rich n-CuO material.
8. The method for synthesizing an oxygen vacancy rich electron-rich n-CuO material of claim 1, comprising the steps of:
the molar ratio of 1.0:2.0 taking copper nitrate trihydrate and urea, uniformly mixing, heating in an electronic universal furnace, and gradually melting raw materials to form a solution;
and (3) carrying out spontaneous combustion reaction on the solution, cooling to room temperature, placing in a muffle furnace, keeping the temperature at 550 ℃ for 3 hours to obtain the oxygen vacancy-rich electron-rich n-CuO material.
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