CN108380195B - Preparation method and application of molecular oxygen activation catalyst constructed based on surface oxygen defects - Google Patents

Preparation method and application of molecular oxygen activation catalyst constructed based on surface oxygen defects Download PDF

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CN108380195B
CN108380195B CN201810254535.XA CN201810254535A CN108380195B CN 108380195 B CN108380195 B CN 108380195B CN 201810254535 A CN201810254535 A CN 201810254535A CN 108380195 B CN108380195 B CN 108380195B
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surface oxygen
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CN108380195A (en
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朱建
吕品
何结红
李和兴
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Shanghai Normal University
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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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/32—Manganese, technetium or rhenium
    • B01J23/34—Manganese
    • 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
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    • C02F2101/308—Dyes; Colorants; Fluorescent agents

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Abstract

The invention discloses a preparation method and application of a molecular oxygen activation catalyst constructed based on surface oxygen defects, wherein the method comprises the following steps: 1) mixing and grinding the solid oxide and the sugar containing aldehyde groups at the normal temperature and the normal pressure according to the mixing ratio of 4: 1-1: 4, spreading the mixture in a quartz boat after fully grinding, and placing the quartz boat in a tube furnace; 2) after hydrogen-containing atmosphere is introduced into the tubular furnace, high-temperature calcination is carried out in a temperature programming mode; 3) and (3) cooling the product obtained in the step (2) by a program, taking out the product, and grinding the product into powder to obtain the carbon-coated oxide material with controllable surface oxygen defect content: c @ MOx, wherein M is Ti, Mn or Si, and the value of x is determined according to the oxidation state of the M element.

Description

Preparation method and application of molecular oxygen activation catalyst constructed based on surface oxygen defects
Technical Field
The invention relates to a preparation method and application of a molecular oxygen activation catalyst constructed based on surface oxygen defects, and belongs to the technical field of environmental materials.
Background
Molecular oxygen exists in air in a large amount and is the purest and green oxidant, but ground state oxygen molecules are stable and difficult to directly react with organic pollutant molecules. Reactive Oxygen Species (ROS) generated by molecular Oxygen activation, such as superoxide radical (. O)2 -) Hydroxyl radical (. OH) and singlet oxygen ((OH))1O2) And the like, has extremely strong oxidizing capability and can almost completely degrade most organic pollutants. Currently, there are three main ways of activating molecular oxygen: 1) in the presence of noble metals (oxides)) Adsorption and dissociation of O on specific crystal face of crystal2(ii) a The method has high cost and the synthesis of a specific crystal face is difficult to control; 2) photocatalytically activating molecular oxygen, and oxygen atom migration and exchange mechanism; this approach requires light source assistance and remains a significant controversy over the mechanism of activation; 3) adsorption and excitation of O by Surface Oxygen defects (SOVs)2(ii) a The method is a brand new technology developed in recent years, and has the characteristics of environmental protection and easy implementation. From the existing mechanism, the activation of molecular oxygen is closely related to the adsorption structure of molecular oxygen on the surface of the catalyst, the adsorption configuration determines an electron transfer path, and the atomic structure of the surface of the catalyst determines the adsorption site characteristics, so that the adsorption configuration of molecules is determined.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a molecular oxygen activation catalyst constructed based on surface oxygen defects, which removes and degrades organic pollutants in a water body by forming active oxygen species.
The technical problem to be solved can be implemented by the following technical scheme.
A preparation method of a molecular oxygen activation catalyst constructed based on surface oxygen defects is used for removing and degrading pollutants in a water body under a dark condition, and comprises the following steps:
1) mixing and grinding the solid oxide and the sugar containing aldehyde groups at the normal temperature and the normal pressure according to the mixing ratio of 4: 1-1: 4, spreading the mixture in a quartz boat after fully grinding, and placing the quartz boat in a tube furnace;
2) after hydrogen-containing atmosphere is introduced into the tubular furnace, high-temperature calcination is carried out in a temperature programming mode;
3) and (3) cooling the product obtained in the step (2) by a program, taking out the product, and grinding the product into powder to obtain the carbon-coated oxide material with controllable surface oxygen defect content: c @ MOx, wherein M is Ti, Mn or Si, and the value of x is determined according to the oxidation state of the M element.
As a further improvement of the technical scheme, the solid oxide is a metal oxide or a nonmetal oxide.
As a further improvement of the technical scheme, the sugar containing aldehyde groups is glucose, fructose or ribose.
As one of the preferred embodiments of the present invention, the metal oxide is TiO2Or MnO2(ii) a The non-metal oxide is SiO2。
Further, the TiO2The composite material is of an anatase and rutile mixed phase structure, the content of the obtained surface oxygen defects (namely the concentration of oxygen vacancies accounts for the percentage of the total oxygen element) is controlled to be 5-20%, and the thickness of the surface carbon layer is 1-5 nm.
Further, the grinding time is preferably 5 to 30 min.
As a further improvement of the technical proposal, the hydrogen-containing atmosphere is H2Or H2H accounting for 5-20% of volume2and/Ar mixed gas.
Also as a further improvement of the technical scheme, the temperature range of the programmed temperature rise is 100-1000 ℃, and the temperature rise rate is 2-20 ℃/min.
Similarly, the temperature range of the programmed cooling is 1000-100 ℃, and the cooling rate is 2-20 ℃/min; the programmed cooling atmosphere is hydrogen-containing atmosphere; the hydrogen-containing atmosphere is H2Or H2The occupied volume ratio of H is 5-20 percent (volume fraction)2and/Ar mixed gas.
By adopting the preparation method of the molecular oxygen activation catalyst constructed based on the surface oxygen defects, aiming at the molecular oxygen activation mode, a series of C @ MOx materials with controllable surface oxygen defect content are constructed by adopting a surface oxygen defect adsorption and excitation method, and active oxygen species can be generated in water: superoxide radical (. O)2 -) And singlet oxygen: (1O2) And the organic pollutants are quickly and effectively removed and degraded. The C @ MOx material with controllable surface oxygen defect content is used for activating molecular oxygen in water to form active oxygen species, and then organic pollutants in the water body are removed and degraded.
Technically, a large amount of oxygen defects are formed on the surface of the oxide by adopting high-temperature calcination reduction; meanwhile, sugar containing aldehydes is used as a precursor, so that a weak reduction atmosphere is provided, and a carbon layer is formed to stabilize and protect oxygen defects.
Another technical problem to be solved by the present invention is to provide an application of the aforementioned C @ MOx material in non-light degradation of methyl orange dye, rhodamine B dye or methylene blue dye, wherein the C @ MOx material decolorizes and removes dye molecules under adsorption and degradation of a catalyst.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of the C @ TiO2 material obtained from calcination at different temperatures. As can be seen, its TiO content2-0 is a mixed phase structure of anatase and rutile, with increasing calcination temperature (from C @ TiO)2-1 from 500 ℃ to C @ TiO2900 ℃ of-2), the peak intensity of the rutile phase in the material gradually increases, which indicates that the proportion of the rutile phase in the mixed phase structure of the material is increasing.
FIG. 2 shows the C @ TiO concentration obtained by calcination at different temperatures2Transmission Electron Microscopy (TEM) images of the material. FIG. 2 includes two views of FIG. 2a and FIG. 2b, wherein FIG. 2a is C @ TiO2-1 in a transmission electron micrograph, and FIG. 2b in a transmission electron micrograph of C @ TiO2-2 transmission electron micrograph. The C @ TiO can be seen from the figure2-1 and C @ TiO2The thickness of the carbon layer on the surface of the sample-2 is about 1-5nm, and most of the carbon layer is in a disordered structure.
FIG. 3 shows the C @ TiO concentration obtained by calcination at different temperatures2A high resolution X-ray photoelectron spectroscopy (XPS) graph of a material, in which a graph of O1s is shown, wherein a solid line represents an original graph, a dotted line represents a result after peak-splitting fitting, a short horizontal dotted line represents a base line, a dot-dashed line represents a main peak of an O1s orbit, and a short dot-dashed line represents a peak where an oxygen vacancy is located. FIG. 3 includes three views of FIG. 3a, FIG. 3b and FIG. 3c, wherein FIG. 3a is TiO2O1s binding energy spectrum of-0, FIG. 3b is C @ TiO2O1s binding energy map of-1, FIG. 3C is C @ TiO2O1s binding energy spectrum of-2. According to the calculation of the peak-splitting fitting, the oxygen defect content on the surface of the sample is 5-20% (namely the concentration of oxygen vacancies accounts for the percentage of the total oxygen element concentration).
FIG. 4 is a schematic diagram of a process in a different embodimentC @ TiO obtained by calcination at temperature2Simulated contaminant removal experimental figures for materials. It can be seen from the figure that the higher the surface oxygen defect content, the faster its contaminant removal and degradation rate.
FIG. 5 is C @ TiO2The material was tested for trapping of reactive oxygen species during a simulated contaminant (methyl orange, MO) removal experiment. As can be seen from the figure, the superoxide radical (. O)2 -) And singlet oxygen: (1O2) Is the main active species.
FIG. 6 shows the C @ TiO concentration obtained by calcination at different temperatures2An Electron Spin Resonance (ESR) spectrum of the material. FIG. 6 includes two views, FIG. 6a and FIG. 6b, in which FIG. 6a is TiO2-0、C@TiO2-1 and C @ TiO2ESR signal intensity produced by superoxide radical of-2, FIG. 6b is TiO2-0、C@TiO2-1 and C @ TiO2Singlet oxygen of-2 produces ESR signal intensity. As can be seen, the superoxide radical (. O) is generated with the increase of the surface oxygen defect content2 -) And singlet oxygen: (1O2) The strength of (A) is also increased, demonstrating that its ability to activate molecular oxygen is also gradually increased.
FIG. 7 shows the C @ TiO concentrations obtained at different precursor ratios2Simulated contaminant removal experimental figures for materials. As can be seen from the figure, the specific surface area and the adsorption capacity of the material have a certain relationship, but the specific surface area and the adsorption capacity of the material have no necessary relationship with the degradation of pollutant molecules.
FIG. 8 shows the C @ TiO concentrations obtained under different saccharide precursor calcinations2A material. As can be seen from the figure, the adsorption and removal capacity of the material prepared from different saccharide molecule precursors to pollutants is different, and C @ TiO prepared from glucose molecules as precursors in the same time2The-1 material has the best adsorption and removal effect.
Figure 9 graph of simulated contaminant removal experiments for C @ MOx materials obtained with different precursor calcinations. As can be seen from the figure, C @ MnO2And C @ SiO2The preparation method has the capability of adsorbing and removing pollutants, and proves that the preparation method has certain universality.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to specific embodiments and with reference to the drawings, but the embodiments do not limit the scope of the present invention.
Example 1:
mixing commercial Degussa P25 and glucose at a mass ratio of 1:1 at normal temperature and pressure, grinding, spreading in quartz boat, introducing H in tube furnace2Heating the mixed gas of/Ar to 500 ℃ by a program, calcining, taking out the sample after cooling, and grinding the sample into powder to obtain the C @ TiO2-1 material.
Example 2:
mixing commercial Degussa P25 and glucose at a mass ratio of 1:1 at normal temperature and pressure, grinding, spreading in quartz boat, introducing H in tube furnace2Heating the mixed gas of/Ar to 900 ℃ by a program, calcining, taking out the sample after cooling, and grinding the sample into powder to obtain the C @ TiO2-2 materials.
Example 3:
mixing commercial Degussa P25 and glucose at a mass ratio of 1:2 at normal temperature and pressure, grinding, spreading in quartz boat, introducing H in tube furnace2Heating the mixed gas of/Ar to 500 ℃ by a program, calcining, taking out the sample after cooling, and grinding the sample into powder to obtain the C @ TiO2-1/2 material.
Example 4:
mixing commercial Degussa P25 and glucose at a mass ratio of 2:1 at normal temperature and pressure, grinding, spreading in quartz boat, introducing H in tube furnace2Heating the mixed gas of/Ar to 500 ℃ by a program, calcining, taking out the sample after cooling, and grinding the sample into powder to obtain the C @ TiO2-2/1 material.
Example 5:
mixing commercial Degussa P25 and ribose at a mass ratio of 1:1 at normal temperature and pressure, grinding, spreading in a quartz boat, introducing H in a tube furnace2Carrying out temperature programming to 500 ℃ for calcination, taking out the sample after the sample is cooled, and grinding the sample into powder to obtain the C @ TiO2-4 materials.
Example 6:
grinding a certain amount of commercial Degussa P25 at normal temperature and normal pressure, spreading in a quartz boat after fully grinding, and introducing H in a tube furnace2Heating the mixed gas of/Ar to 500 ℃ by a program, calcining, taking out the sample after cooling, grinding the sample into powder to obtain the TiO2-0 material.
Example 7:
grinding a certain amount of glucose at normal temperature and normal pressure, spreading in a quartz boat after fully grinding, and introducing H in a tube furnace2And (3) carrying out programmed heating on the/Ar mixed gas to 500 ℃ for calcination, taking out the sample after the sample is cooled, and grinding the sample into powder to obtain the C-0 material.
Example 8:
mixing commercial Degussa P25 and fructose at a mass ratio of 1:1 at normal temperature and pressure, grinding, spreading in quartz boat, introducing H in tube furnace2Heating the mixed gas of/Ar to 500 ℃ by a program, calcining, taking out the sample after cooling, and grinding the sample into powder to obtain the C @ TiO2-5 materials.
Example 9:
MnO with the mass ratio of 1:1 is added at normal temperature and normal pressure2Mixing with glucose, grinding, spreading in quartz boat, introducing H in tube furnace2Heating the mixed gas of/Ar to 500 ℃ by a program, calcining, taking out the sample after cooling, and grinding the sample into powder to obtain C @ MnO2A material.
Example 10:
SiO with the mass ratio of 1:1 is added under normal temperature and normal pressure2Mixing with glucose, grinding, spreading in quartz boat, introducing H in tube furnace2Heating the mixed gas of/Ar to 500 ℃ by a program, calcining, taking out the sample after cooling, and grinding the sample into powder to obtain the C @ SiO2A material.
The method takes solid oxide and sugar containing aldehyde groups as raw materials, and obtains the C @ MOx material with controllable surface oxygen defect content by high-temperature calcination in a hydrogen-containing atmosphere. It is prepared through the combined action of high-temp calcining and reducing assistant on TiO2、MnO2Or SiO2The surface of the oxides builds up oxygen defects with different contents, and the formed carbon layer is used for stabilizing and protecting the oxygen defects. The C @ MOx material prepared by the method can directly react with dissolved Oxygen in water to generate Reactive Oxygen Species (ROS): superoxide radical (. O)2 -) And singlet oxygen: (1O2) The active oxygen species can be used for removing and degrading pollutants in water, and the composite material can be realized in the dark without additional conditions in a pollutant degradation simulation experiment, so that the composite material has a good application prospect.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (7)

1. A preparation method of a molecular oxygen activation catalyst constructed based on surface oxygen defects is characterized in that the molecular oxygen activation catalyst is used for removing and degrading pollutants in a water body under a dark condition, and comprises the following steps:
1) mixing and grinding the solid oxide and the sugar containing aldehyde groups at the normal temperature and the normal pressure according to the mixing ratio of 4: 1-1: 4, spreading the mixture in a quartz boat after fully grinding, and placing the quartz boat in a tube furnace; the solid oxide is SiO2；
2) After hydrogen-containing atmosphere is introduced into the tubular furnace, high-temperature calcination is carried out in a temperature programming mode;
3) and (3) cooling the product obtained in the step (2) by a program, taking out the product, and grinding the product into powder to obtain the carbon-coated oxide material with controllable surface oxygen defect content: c @ MOx, wherein M is an Si element, and the value of x is determined according to the oxidation state of the M element.
2. The method for preparing a molecular oxygen activating catalyst constructed based on surface oxygen defects according to claim 1, wherein the aldehyde group-containing sugar is glucose or ribose.
3. The method for preparing a molecular oxygen activating catalyst constructed based on surface oxygen defects according to claim 1, wherein the grinding time is 5-30 min.
4. The method for preparing the molecular oxygen activating catalyst constructed based on surface oxygen defects according to claim 1, wherein the hydrogen-containing atmosphere is H2Or H2H accounting for 5-20% of volume2and/Ar mixed gas.
5. The preparation method of the molecular oxygen activation catalyst constructed based on the surface oxygen defects according to claim 1, wherein the temperature range of the temperature programming is 100-1000 ℃, and the temperature rising rate is 2-20 ℃/min.
6. The preparation method of the molecular oxygen activation catalyst constructed based on the surface oxygen defects according to claim 1, wherein the temperature range of the programmed cooling is 1000-100 ℃, and the cooling rate is 2-20 ℃/min; the programmed cooling atmosphere is hydrogen-containing atmosphere; the hydrogen-containing atmosphere of the programmed temperature reduction is H2Or H2H accounting for 5-20% of volume2and/Ar mixed gas.
7. Use of a molecular oxygen-activated catalyst based on surface oxygen defects, prepared according to the preparation method of any one of claims 1 to 6, in non-illuminated degradation of methyl orange dyes, rhodamine B dyes or methylene blue dyes, characterized in that the C @ MOx material decolourizes and removes dye molecules under adsorption and degradation of the catalyst.
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CN110833865B (en) * 2019-11-21 2021-10-22 山东大学 Preparation method of high-stability catalytic membrane for generating singlet oxygen
CN111584800A (en) * 2020-01-15 2020-08-25 武汉理工大学 Oxygen-deficient titanium dioxide nanosheet modified lithium ion battery diaphragm and preparation method and application thereof
CN111634956B (en) * 2020-05-28 2022-07-05 上海大学 Method for synthesizing oxygen vacancy of oxygen-containing metal compound

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