CN108380195A - A kind of preparation method and applications of the RAPD check catalyst based on surface oxygen defect structure - Google Patents
A kind of preparation method and applications of the RAPD check catalyst based on surface oxygen defect structure Download PDFInfo
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- CN108380195A CN108380195A CN201810254535.XA CN201810254535A CN108380195A CN 108380195 A CN108380195 A CN 108380195A CN 201810254535 A CN201810254535 A CN 201810254535A CN 108380195 A CN108380195 A CN 108380195A
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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
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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
- B01J23/16—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
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- 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
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- 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
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Abstract
The invention discloses a kind of preparation method and applications of the RAPD check catalyst based on surface oxygen defect structure, wherein this approach includes the following steps：1), under room temperature, normal pressure, by soild oxide and sugar in mass ratio 4 containing aldehyde radical:1~1:4 mixed proportion carries out mixed grinding, is laid in quartz boat after being fully ground, and quartz boat is placed in tube furnace；2) after, being passed through hydrogeneous atmosphere in tube furnace, high-temperature calcination is carried out by the way of temperature programming；3) it, takes out and is ground into powder after program cooling down after the product that step 2) obtains, obtain the oxide material of the controllable carbon package of surface oxygen defect content：C@MOx, wherein the value of M Ti, Mn or Si elements, x is determined according to the oxidation state of M element.
Description
Technical field
The present invention relates to it is a kind of based on surface oxygen defect structure RAPD check catalyst preparation method and applications,
Belong to environmentally conscious materials technical field.
Background technology
Molecular oxygen is largely present in air, is most pure and green oxidant, but the oxygen molecule of ground state is very stable, difficult
Directly to be reacted with organic pollutant molecule.And active oxygen species (ROS, the Reactive generated by RAPD check
Oxygen Species), such as superoxide radical (O2 -), hydroxyl radical free radical (OH) and singlet oxygen (1O2) etc., then there is pole
Strong oxidability, almost being capable of degradable majority of organic pollutants.Currently, to the activation of molecular oxygen, there are mainly three types of sides
Formula：1) dissociation O is adsorbed in noble metal (oxide) crystal particular crystal plane2；Which cost is higher and the synthesis of particular crystal plane
It is difficult to control；2) photo catalytic activation molecular oxygen, oxygen atom migrate exchange mechanism；Which needs light source and the machine to activation
Reason still has prodigious dispute；3) surface oxygen defect (SOVs, Surface Oxygen Vacancies) is utilized to adsorb and swash
Send out O2；This method is the completely new skill developed in recent years, is had the characteristics that environmentally protective and easy to implement.From at present it is existing
For in mechanism, the activation of molecular oxygen is closely related with its adsorption structure in catalyst surface, and adsorptive behavior determines electronics
Transfer path, and the atomic structure of catalyst surface determines adsorption site feature, to determine the adsorptive behavior of molecule.
Invention content
Technical problem to be solved by the present invention lies in a kind of RAPD checks based on surface oxygen defect structure of offer to urge
The preparation method of agent by forming active oxygen species, and then is removed and degrades to the organic pollution in water body.
Its technical problem to be solved can be implemented by the following technical programs.
A kind of preparation method of the RAPD check catalyst based on surface oxygen defect structure, includes the following steps：
1), under room temperature, normal pressure, by soild oxide and sugar in mass ratio 4 containing aldehyde radical:1~1:4 mixed proportion into
Row mixed grinding is laid in quartz boat after being fully ground, and quartz boat is placed in tube furnace；
2) after, being passed through hydrogeneous atmosphere in tube furnace, high-temperature calcination is carried out by the way of temperature programming；
3) it, takes out and is ground into powder after program cooling down after the product that step 2) obtains, obtain surface oxygen defect
The oxide material of the controllable carbon package of content：C@MOx, wherein M Ti, Mn or Si elements, the value of x is according to the oxidation of M element
State determines.
As being further improved for the technical program, the soild oxide is metal oxide or nonmetal oxide.
Also being further improved as the technical program, the sugar containing aldehyde radical are glucose, fructose or ribose.
As one of the preferred embodiment of the present invention, the metal oxide is TiO2Or MnO2；The nonmetal oxide
For SiO2。
Further, the TiO2For anatase and rutile mixed phase structure, (i.e. oxygen is empty for obtained surface oxygen defect content
The concentration of position accounts for the percentage of the concentration of total oxygen element) 5~20%, the thickness of carbon layer on surface is 1-5nm for control.
In addition, the milling time is preferably 5-30min.
Also being further improved as the technical program, the hydrogeneous atmosphere are H2Or H2Shared volume ratio is 5%-
20% H2/ Ar gaseous mixtures.
The temperature range of same being further improved as the technical program, described program heating rises at 100~1000 DEG C
Warm rate is in 2-20 DEG C/min.
Likewise, the temperature range of described program cooling is at 1000~100 DEG C, rate of temperature fall is in 2-20 DEG C/min；Program
The atmosphere of cooling is hydrogeneous atmosphere；The hydrogeneous atmosphere is H2Or H2Shared volume ratio is 5%-20%'s (volume fraction)
H2/ Ar gaseous mixtures.
Using the preparation method of RAPD check catalyst of the above-mentioned technical proposal based on surface oxygen defect structure, for
The mode of RAPD check, the method adsorbed and excited using surface oxygen defect, constructing a series of surface oxygen defect contents can
The C@MOx materials of control, can generate active oxygen species in water：Superoxide radical (O2 -) and singlet oxygen (1O2), and to having
Machine pollutant carries out rapid effective removal and degradation.By in the controllable C MOx material activated waters of surface oxygen defect content
Molecular oxygen formed active oxygen species, and then realize the organic pollution in water body is removed and is degraded.
It is technically restored by using high-temperature calcination, a large amount of oxygen defects is formed in oxide surface；Aldehyde-containing type is used simultaneously
Sugar as presoma, provide faint reduction atmosphere, and form that carbon-coating is stable and protection oxygen defect.
Another technical problem to be solved by this invention is to provide a kind of aforementioned C@MOx materials in methyl orange dye, sieve
Application in the no light degradation of red bright B dyestuffs or methylene blue dye, wherein the C@MOx materials make dye molecule urge
The lower decoloration removal of absorption and degradation of agent.
Description of the drawings
Fig. 1 is X-ray diffraction (XRD) figure of the C@TiO2 materials obtained under different temperatures calcining.As seen from the figure,
TiO2- 0 is anatase and rutile mixed phase structure, as the raising of calcination temperature is (from C@TiO2500 DEG C of -1 arrive C@TiO2-2
900 DEG C), the peak intensity of Rutile Type gradually increases in material, illustrates that the Rutile Type ratio in its mixed phase structure is increasing.
Fig. 2 is the C@TiO obtained under different temperatures calcining2Transmission electron microscope (TEM) figure of material.Fig. 2 include Fig. 2 a and
Two figures of Fig. 2 b, wherein Fig. 2 a are C@TiO2- 1 transmission electron microscope picture, Fig. 2 b are C@TiO2- 2 transmission electron microscope picture.As seen from the figure
C@TiO2- 1 and C@TiO2In -2 samples, the thickness of carbon layer on surface most of is in unordered knot all in 1-5nm or so
Structure.
Fig. 3 is the C@TiO obtained under different temperatures calcining2The high-resolution X-ray photoelectron spectroscopic analysis of material
(XPS) figure is the collection of illustrative plates of O 1s in figure, and wherein solid line represents original figure spectrum, and dotted line is after swarming is fitted as a result, hyphen
Dotted line represents baseline, and pecked line represents the main peak of O1s tracks, and short pecked line represents the peak where Lacking oxygen.Fig. 3 include Fig. 3 a,
Tri- figures of Fig. 3 b and Fig. 3 c, wherein Fig. 3 a are TiO2It is C@TiO that -0 O1s, which combines energy collection of illustrative plates, Fig. 3 b,2- 1 O1s combinations can be schemed
Spectrum, Fig. 3 c are C@TiO2- 2 O1s is combined can collection of illustrative plates.According to the calculating that swarming is fitted, sample surfaces oxygen defect content 5~
Between 20% (i.e. the concentration of Lacking oxygen accounts for the percentage of the concentration of total oxygen element).
Fig. 4 is the C@TiO obtained under different temperatures calcining2The simulating pollution object of material removes lab diagram.It can from figure
To find out, surface oxygen defect content is higher, faster to the removal and degradation rate of pollutant.
Fig. 5 is C@TiO2Material is in simulating pollution object (methyl orange, MO) removes experimentation, the capture of active oxygen species
Experiment.It can be seen from the figure that superoxide radical (O2 -) and singlet oxygen (1O2) it is main active specy.
Fig. 6 is the C@TiO obtained under different temperatures calcining2Electron spin resonance (ESR) collection of illustrative plates of material.Fig. 6 includes
Two figures of Fig. 6 a and Fig. 6 b, wherein Fig. 6 a are TiO2-0、C@TiO2- 1 and C@TiO2It is strong that -2 superoxide radical generates ESR signals
Degree, Fig. 6 b are TiO2-0、C@TiO2- 1 and C@TiO2- 2 singlet oxygen generates ESR signal strengths.Root as seen from the figure, with table
The raising of face oxygen defect content generates superoxide radical (O2 -) and singlet oxygen (1O2) intensity also improve therewith, it was demonstrated that
It also steps up the ability of RAPD check.
Fig. 7 is the C@TiO obtained under different presoma ratios2The simulating pollution object of material removes lab diagram.By scheming
As it can be seen that specific surface area and the adsorption capacity of material have certain relationship, but there is no necessarily relationships to the degradation of contaminant molecule.
Fig. 8 is the C@TiO obtained under different carbohydrate presoma calcinings2Material.It can be seen from the figure that different carbohydrates
Material prepared by molecular precursor is different to the ability of pollutant absorption with removal, interior at the same time, by grape sugar
The C@TiO that son is prepared as presoma2- 1 material has best absorption and removal effect.
The simulating pollution object for the C@MOx materials that Fig. 9 is obtained under being calcined using different presomas removes lab diagram.It can from figure
To find out, C@MnO2With C@SiO2With the ability adsorbed and removed to pollutant, it was demonstrated that preparation method of the invention has
Certain universality.
Specific implementation mode
Technical scheme of the present invention, but the reality are described in further detail below in conjunction with specific embodiment and with reference to each attached drawing
Example is applied not limit the scope of the invention.
Embodiment 1：
It is 1 by mass ratio under room temperature, normal pressure:1 commercial Degussa P25 and glucose mixed grinding, is fully ground
After be laid in quartz boat, be passed through H with tube furnace2/ Ar gaseous mixtures carry out temperature programming to 500 DEG C of calcinings, after sample cooling
Taking-up is ground into powder to get to C@TiO2- 1 material.
Embodiment 2：
It is 1 by mass ratio under room temperature, normal pressure:1 commercial Degussa P25 and glucose mixed grinding, is fully ground
After be laid in quartz boat, be passed through H with tube furnace2/ Ar gaseous mixtures carry out temperature programming to 900 DEG C of calcinings, after sample cooling
Taking-up is ground into powder to get to C@TiO2- 2 materials.
Embodiment 3：
It is 1 by mass ratio under room temperature, normal pressure:2 commercial Degussa P25 and glucose mixed grinding, is fully ground
After be laid in quartz boat, be passed through H with tube furnace2/ Ar gaseous mixtures carry out temperature programming to 500 DEG C of calcinings, after sample cooling
Taking-up is ground into powder to get to C@TiO2- 1/2 material.
Embodiment 4：
It is 2 by mass ratio under room temperature, normal pressure:1 commercial Degussa P25 and glucose mixed grinding, is fully ground
After be laid in quartz boat, be passed through H with tube furnace2/ Ar gaseous mixtures carry out temperature programming to 500 DEG C of calcinings, after sample cooling
Taking-up is ground into powder to get to C@TiO2- 2/1 material.
Embodiment 5：
It is 1 by mass ratio under room temperature, normal pressure:1 commercial Degussa P25 and ribose mixed grinding, after being fully ground
It is laid in quartz boat, H is passed through with tube furnace2Temperature programming is carried out to 500 DEG C of calcinings, takes out and pulverizes after sample cooling
Last shape is to get to C@TiO2- 4 materials.
Embodiment 6：
Under room temperature, normal pressure, a certain amount of commercialization Degussa P25 are ground, are laid in quartz boat after being fully ground, used
Tube furnace is passed through H2/ Ar gaseous mixtures carry out temperature programming to 500 DEG C of calcinings, take out and are ground into powder after sample cooling, i.e.,
Obtain TiO2- 0 material.
Embodiment 7：
Under room temperature, normal pressure, a certain amount of glucose is ground, is laid in quartz boat after being fully ground, it is logical with tube furnace
Enter H2/ Ar gaseous mixtures carry out temperature programming and calcine to 500 DEG C, take out and are ground into powder to get to C-0 materials after sample cooling
Material.
Embodiment 8：
It is 1 by mass ratio under room temperature, normal pressure:1 commercial Degussa P25 and fructose mixed grinding, after being fully ground
It is laid in quartz boat, H is passed through with tube furnace2/ Ar gaseous mixtures carry out temperature programming to 500 DEG C of calcinings, are taken after sample cooling
Go out to be ground into powder to get to C@TiO2- 5 materials.
Embodiment 9：
It is 1 by mass ratio under room temperature, normal pressure:1 MnO2With glucose mixed grinding, stone is laid in after being fully ground
Ying Zhouzhong is passed through H with tube furnace2/ Ar gaseous mixtures carry out temperature programming to 500 DEG C of calcinings, take out and are ground into after sample cooling
It is powdered to get to C@MnO2Material.
Embodiment 10：
It is 1 by mass ratio under room temperature, normal pressure:1 SiO2With glucose mixed grinding, stone is laid in after being fully ground
Ying Zhouzhong is passed through H with tube furnace2/ Ar gaseous mixtures carry out temperature programming to 500 DEG C of calcinings, take out and are ground into after sample cooling
It is powdered to get to C@SiO2Material.
Sugar of the present invention with soild oxide and containing aldehyde radical is raw material, by obtaining surface containing the high-temperature calcination under hydrogen atmosphere
The controllable C@MOx materials of oxygen defect content.It is by high-temperature calcination and the collective effect for restoring auxiliary agent, in TiO2、MnO2Or SiO2
The surface construction of the oxides different oxygen defect of content is waited, and using the carbon-coating of formation stabilization and protects these oxygen defects.With
C@MOx materials made from the method for the present invention can directly react with dissolved oxygen in water, generation active oxygen species (ROS,
Reactive Oxygen Species)：Superoxide radical (O2 -) and singlet oxygen (1O2), and these active oxygen species are available
The removal and degradation of pollutant in water body, the composite material are not necessarily to additional condition, black in simulating pollution thing degradation experiment
It can be realized, have a good application prospect in the dark.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although with reference to compared with
Good embodiment describes the invention in detail, it will be understood by those of ordinary skill in the art that, it can be to the technology of invention
Scheme is modified or replaced equivalently, and without departing from the spirit of the technical scheme of the invention and range, should all be covered in this hair
In bright right.
Claims (10)
1. a kind of preparation method of the RAPD check catalyst based on surface oxygen defect structure, which is characterized in that including following
Step：
1), under room temperature, normal pressure, by soild oxide and sugar in mass ratio 4 containing aldehyde radical:1~1:4 mixed proportion is mixed
Grinding is closed, is laid in quartz boat after being fully ground, and quartz boat is placed in tube furnace；
2) after, being passed through hydrogeneous atmosphere in tube furnace, high-temperature calcination is carried out by the way of temperature programming；
3) it, takes out and is ground into powder after program cooling down after the product that step 2) obtains, obtain surface oxygen defect content
The oxide material of controllable carbon package：C@MOx, wherein the value of M Ti, Mn or Si elements, x is determined according to the oxidation state of M element
It is fixed.
2. the preparation method of the RAPD check catalyst according to claim 1 based on surface oxygen defect structure, feature
It is, the soild oxide is metal oxide or nonmetal oxide.
3. the preparation method of the RAPD check catalyst according to claim 1 based on surface oxygen defect structure, feature
It is, the sugar containing aldehyde radical is glucose, fructose or ribose.
4. the preparation method of the RAPD check catalyst according to claim 2 based on surface oxygen defect structure, feature
It is, the metal oxide is TiO2Or MnO2；The nonmetal oxide is SiO2。
5. the preparation method of the RAPD check catalyst according to claim 4 based on surface oxygen defect structure, feature
It is, the TiO2For anatase and rutile mixed phase structure, obtained surface oxygen defect content control is 5~20%, surface
The thickness of carbon-coating is 1-5nm.
6. the preparation method of the RAPD check catalyst according to claim 1 based on surface oxygen defect structure, feature
It is, milling time 5-30min.
7. the preparation method of the RAPD check catalyst according to claim 1 based on surface oxygen defect structure, feature
It is, the hydrogeneous atmosphere is H2Or H2Shared volume ratio is the H of 5%-20%2/ Ar gaseous mixtures.
8. the preparation method of the RAPD check catalyst according to claim 1 based on surface oxygen defect structure, feature
It is, the temperature range of described program heating is at 100~1000 DEG C, and heating rate is in 2-20 DEG C/min.
9. the preparation method of the RAPD check catalyst according to claim 1 based on surface oxygen defect structure, feature
It is, the temperature range of described program cooling is at 1000~100 DEG C, and rate of temperature fall is in 2-20 DEG C/min；The atmosphere of program cooling
For hydrogeneous atmosphere；The hydrogeneous atmosphere is H2Or H2Shared volume ratio is the H of 5%-20%2/ Ar gaseous mixtures.
10. C@MOx materials described in any claim are in methyl orange dye, rhdamine B or methylene in claim 1-9
Application in the no light degradation of blue dyestuff, the C@MOx materials make dye molecule decolourize under the absorption and degradation of catalyst
Removal.
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| CN111634956A (en) * | 2020-05-28 | 2020-09-08 | 上海大学 | Method for synthesizing oxygen vacancy of oxygen-containing metal compound |
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