CN115888782A - Co/g-C 3 N 4 Preparation method and application of composite photocatalyst - Google Patents
Co/g-C 3 N 4 Preparation method and application of composite photocatalyst Download PDFInfo
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- 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
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Abstract
The invention belongs to the technical field of composite nano material preparation and environmental protection, and discloses Co/g-C 3 N 4 A preparation method and application of the composite photocatalyst. The invention synthesizes the composite photocatalyst by a water bath method and a high-temperature calcination method. The preparation process comprises the following steps: firstly, weighing a certain amount of CoCl 2 ·6H 2 Adding deionized water into the mixture, heating and stirring the mixture until the mixture is completely dissolved, transferring the mixture into a reaction kettle for water bath reaction, washing and drying the mixture after the water bath reaction is finished, and finally calcining a dried sample to obtain Co/g-C 3 N 4 A composite photocatalyst is provided. The preparation method has the advantages of simple preparation process, mild reaction conditions, economy, energy conservation and low implementation cost. The prepared composite photocatalyst has high-efficiency photocatalytic activity and good stability, and has good application value and prospect in the field of photocatalysis.
Description
Technical Field
The invention relates to the technical field of photocatalyst material preparation and environmental protection, and relates to Co/g-C 3 N 4 A preparation method of the composite photocatalyst and application in photocatalytic degradation of 2-mercaptobenzothiazole.
Background
In recent years, water pollution has become one of the most serious environmental problems. MBT (2-mercaptobenzothiazole) is considered as a metal detection reagent and is used for synthesizing pesticides, cephalosporins and the like. Inhalation of low concentrations of MBT can cause nausea, headache, and inhalation of high concentrations of MBT can cause fatal respiratory paralysis. If the water enters the water, certain harm is caused to the water body. The traditional physical method, chemical method, biological method and the like are difficult to realize effective treatment on the wastewater, and the photocatalytic technology developed in recent years not only has strong oxidation capability, high reaction rate and no pollution, but also has lower time and economic cost, and becomes one of the important research directions for treating the wastewater. Therefore, the development of a novel high-efficiency photocatalyst is one of the best methods for solving the water body pollution.
Currently, graphitic carbon nitride (g-C) 3 N 4 ) As an important semiconductor, it has been widely studied because of its appropriate band position, ease of preparation, and good chemical stability. However, the performance of the material is still unsatisfactory due to insufficient absorption of visible light, poor specific surface area, low electron conductivity and high recombination rate of photo-generated electron-hole pairs. The photocatalytic activity of the material can be improved by enhancing the band structure, photoabsorption, charge transport, and photoinduced electron-hole pair separation. By means of synthesis technology, designing nanometer structure, regulating electronic structure and other strategies, g-C may be raised effectively 3 N 4 Photocatalytic activity of (1).
The simple substance of cobalt is often usedThe cobalt simple substance is loaded in g-C for the purpose of transferring electrons from active sites to be attracted more and more attention in photocatalysis application 3 N 4 In the above, the cobalt simple substance is used as an active site to play a role in electron aggregation, and has a certain role in improving the photocatalytic activity. So CoCl is used in this patent 2 ·6H 2 O as a cobalt source, successfully loaded to g-C 3 N 4 Above, with simple g-C 3 N 4 Compared with the prior art, the photocatalytic activity is obviously improved.
Disclosure of Invention
[ problem ] to
Aiming at the defects in the prior art, the invention aims to provide Co/g-C 3 N 4 The preparation method of the composite photocatalyst is simple and easy to implement, low in implementation cost and economical and energy-saving in reaction steps.
The invention also aims to provide the composite photocatalyst prepared by the preparation method, which has high-efficiency photocatalytic activity, can improve the adsorption effect on organic pollutants, has excellent photocatalytic degradation efficiency, greatly improves the removal and degradation of organic matters in wastewater, and has good application value and prospect in the field of photocatalysis.
[ solution ]
In order to achieve the aim, the invention provides a composite photocatalyst Co/g-C according to one embodiment of the invention 3 N 4 The preparation method of (1).
(1) CoCl was weighed in different masses (0.005g, 0.01g,0.02g,0.03g, 0.04g) 2 ·6H 2 O and 1g of melamine are placed in a beaker, 60mL of deionized water is added, the mixture is dissolved by heating in a water bath at 90 ℃, and then the solution is transferred to a 100mL reaction kettle with a polytetrafluoroethylene lining and heated at 180 ℃ for 24 hours.
(2) Cooling to room temperature, washing with deionized water and anhydrous ethanol for 3 times, and vacuum drying at 60 deg.C.
(3) Putting the powder into a tube furnace, calcining for 4h at 550 ℃, and heating at the rate of 5 ℃/min under N 2 Under an atmosphere. According to CoCl 2 ·6H 2 Quality of O will end productIn turn denoted as Co 0.005 /g-C 3 N 4 ，Co 0.01 /g-C 3 N 4 ，Co 0.02 /g-C 3 N 4 ，Co 0.03 /g-C 3 N 4 ，Co 0.04 /g-C 3 N 4 . Without adding CoCl 2 ·6H 2 In the case of O, pure g-C is prepared 3 N 4 。
In the step (1), the cobalt salt may be at least one selected from cobalt nitrate and cobalt chloride, preferably cobalt chloride; coCl 2 ·6H 2 The mass of O is 0.001-0.1 g, the volume of deionized water is 50-100 mL, the water bath dissolution temperature is 50-150 ℃, and the heating time is 16-32 h.
In the step (2), the drying temperature is 50-80 ℃.
In the step (3), the calcining temperature is 300-700 ℃, the calcining time is 2-6 h, and the heating rate is 2-7 ℃/min.
Co/g-C obtained according to the above-mentioned preparation method 3 N 4 The composite catalyst is applied to degrading MBT (2-mercaptobenzothiazole) in wastewater.
Melamine, cobalt chloride hexahydrate (CoCl) used in the present invention 2 ·6H 2 O), absolute ethanol, all analytically pure, purchased from alatin reagent limited.
[ advantageous effects ]
In conclusion, the invention has the following beneficial effects:
the invention synthesizes Co/g-C 3 N 4 The tubular catalyst is prepared by successfully using the composite catalyst as a photocatalyst for degrading MBT in wastewater, and the specific surface area of the tubular catalyst can be increased, so that reactants are more easily attached to the surface of the catalyst. Co/g-C prepared by the invention 3 N 4 The composite catalyst is excited by a xenon lamp, contacts with pollutant molecules and interacts with the pollutant molecules to realize a special catalytic or conversion effect, so that ambient oxygen and water molecules are excited into free negative ions with strong oxidizing power, and the aim of degrading MBT in environmental wastewater is fulfilledThe method is low in cost and is an environment-friendly high-efficiency treatment technology.
Description of the drawings:
FIG. 1 shows g-C 3 N 4 And Co/g-C 3 N 4 XRD pattern of the composite photocatalyst.
FIG. 2 is an FT-IR diagram of the Co/g-C3N4 composite photocatalyst.
FIG. 3 is Co 0.01 /g-C 3 N 4 SEM and TEM images of the composite photocatalyst.
FIG. 4 shows Co 0.01 /g-C 3 N 4 And degrading the MBT absorbance graph and the degradation rate graph by the composite photocatalyst under visible light.
FIG. 5 shows Co/g-C 3 N 4 Fluorescence spectrum and electrochemical impedance diagram of the composite photocatalyst.
FIG. 6 shows Co 0.01 /g-C 3 N 4 Four-cycle experimental diagram of composite photocatalyst degradation MBT.
Detailed Description
The invention is further illustrated by the following examples.
Evaluation of adsorption activity of the photocatalyst prepared in the present invention: the method is carried out in a CEL-LB70 type photochemical reactor, but without a light source, 100mL of MBT simulated wastewater is added into the reactor, the initial value of the MBT simulated wastewater is measured, then 0.1g of photocatalyst is added, the magnetic stirring is started without turning on the lamp, the air is not ventilated, sampling analysis is carried out at intervals of 10min, and supernatant liquid is taken after centrifugation and is counted in by ultraviolet spectrophotometry. The concentration was determined at λ =310nm and was determined by the formula: q = (C) 0 C) V/m calculating the adsorption Q, where C 0 The initial concentration of MBT solution, C the concentration of MBT solution at equilibrium of adsorption, V the volume of solution, and m the mass of catalyst added.
Photocatalytic activity evaluation of the photocatalyst prepared in the present invention: performing in CEL-LB70 type photochemical reaction instrument (purchased from Ching Tanji-Ching-Tanji-Tech Co., ltd.) under irradiation of xenon lamp, adding 100mL MBT simulated wastewater into the reactor, measuring initial value, adding the prepared photocatalyst, magnetically stirring, starting aeration device, introducing air to keep the catalyst in suspension or floating stateAnd (3) sampling and analyzing at an interval of 10min in the illumination process, taking supernatant after centrifugal separation, measuring absorbance at a position lambda max =310nm of a spectrophotometer, and passing the formula: dr = (C-C) 0 )/C 0 X 100% calculating the degradation efficiency Dr, where C 0 To reach the concentration after adsorption equilibrium, C is the concentration of MBT solution measured at time t, and t is the reaction time.
In order that those skilled in the art may more clearly understand the present invention, the present invention will be further described in detail with reference to the following examples, but it should be understood that the following examples are only preferred embodiments of the present invention, and the scope of the present invention as claimed should not be limited thereto.
< example >
Example 1
Co/g-C according to the invention was prepared by the following method 3 N 4 The composite photocatalyst comprises:
(1) Weighing CoCl with different masses 2 ·6H 2 O and 1g of melamine are placed in a beaker, 60mL of deionized water is added, the mixture is dissolved by heating in a water bath at 90 ℃, and then the solution is transferred to a 100mL reaction kettle with a polytetrafluoroethylene lining and heated at 180 ℃ for 24 hours.
(2) Cooling to room temperature, washing with deionized water and anhydrous ethanol for 3 times, and vacuum drying at 60 deg.C.
(3) Putting the powder into a tube furnace, calcining for 4h at 550 ℃, and heating at the rate of 5 ℃/min under N 2 Under an atmosphere. According to CoCl 2 ·6H 2 The quality of O marks the final product as Co 0.005 /g-C 3 N 4 ，Co 0.01 /g-C 3 N 4 ，Co 0.02 /g-C 3 N 4 ，Co 0.03 /g-C 3 N 4 ，Co 0.04 /g-C 3 N 4 。
Example 2
The same procedure was followed as in example 1, except that 0.005g of CoCl was weighed in (1) 2 ·6H 2 O，Co 0.005 /g-C 3 N 4 Photo-catalysis in photochemical reaction instrumentAnd (3) a chemical degradation test shows that the degradation efficiency of the photocatalyst on the MBT solution reaches 93% within 70 min.
Example 3
The same procedure was followed as in example 1, except that 0.01g of CoCl was weighed in (1) 2 ·6H 2 O，Co 0.01 /g-C 3 N 4 A photocatalytic degradation test is carried out in a photochemical reactor, and the degradation efficiency of the photocatalyst on the MBT solution is measured to reach 98% within 70 min.
Example 4
The same procedure was followed as in example 1, except that 0.02g of CoCl was weighed in (1) 2 ·6H 2 O，Co 0.02 /g-C 3 N 4 A photocatalytic degradation test is carried out in a photochemical reactor, and the degradation efficiency of the photocatalyst on MBT solution is measured to reach 91% within 70 min.
Example 5
The same procedure was followed as in example 1, except that 0.03g of CoCl was weighed in (1) 2 ·6H 2 O，Co 0.03 /g-C 3 N 4 A photocatalytic degradation test is carried out in a photochemical reactor, and the degradation efficiency of the photocatalyst to the MBT solution is measured to reach 83 percent within 70min
Example 6
The same procedures as in example 1 were carried out except that 0.04g of CoCl was weighed in (1) 2 ·6H 2 O，Co 0.04 /g-C 3 N 4 A photocatalytic degradation test is carried out in a photochemical reactor, and the degradation efficiency of the photocatalyst on the MBT solution is measured to reach 80% within 70 min.
It can be seen from XRD in FIG. 1 (a) that the composite photocatalyst Co/g-C is prepared 3 N 4 There are distinct absorption peaks at 13.1 ℃ and 27.3 ℃ corresponding to g-C, respectively 3 N 4 The (100) and (002) crystal planes of (2) and (002) are clear, and the absorption peak of 27.3 degrees is obvious due to the (002) crystal lattice plane layer spacing stacking diffraction of the graphite-like structure. As the amount of Co supported increases, 27The gradual broadening of the diffraction peak at 3 ℃ indicates that Co and g-C 3 N 4 There is a strong attraction between them. By observation, g-C 3 N 4 The diffraction peak of (A) is not shifted, which shows that the Co simple substance is only loaded in g-C 3 N 4 On the surface, there is no access to the crystal structure. In addition, no other characteristic impurity peaks were detected in these samples, indicating that they are pure phases with the same crystal structure. Since the morphology of Co is unknown from FIG. 1 (a), there is a possibility that CoCl is introduced 2 ·6H 2 The amount of O is too small, so that CoCl is increased 2 ·6H 2 O in an amount of 0.5g as the cobalt source, thereby obtaining FIG. 1 (b), and it can be seen that three diffraction peaks at 45.9 DEG, 53.5 DEG and 79.1 DEG, respectively, are obtained except for 27.3 DEG, and that these three diffraction peaks are classified into Co simple substance as can be seen from XRD standard card Co PDF-88-2325, from which Co/g-C 3 N 4 The composite photocatalyst is successfully prepared.
All samples made from the FT-IR spectrum of FIG. 2 were at 810cm -1 Has characteristic peak belonging to the respiratory vibration of triazine unit and ranging from 1200 cm to 1700cm -1 Several peaks in between are typical stretching vibration of CN heterocyclic ring, 3100cm -1 The vicinity belongs to the stretching vibration of N-H. Thus, co/g-C 3 N 4 The preparation of the composite photocatalyst is successful.
The composite Co can be seen from the SEM image in FIG. 3 (a) 0.01 /g-C 3 N 4 The surface of the hollow pipe-shaped structure is smooth, and Co particles with different sizes are dispersed on the surface. As can be further seen from the TEM image of FIG. 3 (b), co particles are attached to g-C 3 N 4 Above, description of Co/g-C 3 N 4 The photocatalytic material is successfully compounded.
FIG. 4 (a) shows a composite photocatalyst Co under visible light 0.01 /g-C 3 N 4 Absorbance pattern of degraded MBT solution. It can be seen that the characteristic peak at 310nm corresponding to MBT gradually decreases with time, indicating that the MBT molecule is obviously degraded and destroyed. As can be seen more visually from FIG. 4 (b), the degradation efficiency of the six catalysts under the same conditions, where Co is present 0.01 /g-C 3 N 4 The degradation effect of (2) is the best, and blank experiments prove that the influence of photosensitization on MBT is eliminated.
As can be seen in FIG. 5 (a), with a single g-C 3 N 4 Catalyst phase, co 0.01 /g-C 3 N 4 The composite photocatalyst has low fluorescence intensity, which indicates that the composite photocatalyst has low recombination rate of photo-generated carriers, thereby improving the photocatalytic activity. As can be seen from FIG. 5 (b), with a single g-C 3 N 4 Catalyst phase, co 0.01 /g-C 3 N 4 The composite photocatalyst has smaller radius, which shows that the composite photocatalyst has better interface charge transfer characteristic and is more beneficial to the separation and migration of current carriers, thereby improving the photocatalytic performance.
As can be seen from FIG. 6, after four photocatalytic experiments, co 0.01 /g-C 3 N 4 The composite photocatalyst shows relative stability when degrading tetracycline under visible light, and the number of the subsequent two times is slightly reduced, mainly because after each experiment is finished, a sample has certain loss in the washing and drying processes.
Claims (7)
1. Co/g-C 3 N 4 The preparation method of the composite photocatalyst is characterized by comprising the following steps:
(1) CoCl was weighed in different masses (0.005g, 0.01g,0.02g,0.03g, 0.04g) 2 ·6H 2 And (3) putting the O and the melamine into a beaker, adding deionized water, heating and dissolving in a water bath, and then transferring the solution into a reaction kettle with a 100mL polytetrafluoroethylene lining for hydrothermal reaction.
(2) Cooling to room temperature, washing with deionized water and anhydrous ethanol for 3 times, and oven drying.
(3) Placing the powder in a tube furnace, calcining in N 2 Under an atmosphere. Thereby obtaining said Co/g-C 3 N 4 A composite photocatalyst is provided.
2. The method of claim 1, wherein the step of preparing is carried out in the presence of a catalyst(1) In, coCl 2 ·6H 2 The mass of O is 0.005-0.04 g, and the volume of deionized water is 50-100 mL.
3. The method according to claim 1, wherein the step (1) is: the water bath stirring temperature of the mixed solution is 80-100 ℃.
4. The method of claim 1, wherein the step (1) further comprises: the hydrothermal reaction temperature is 150-220 ℃, and the heating time is 20-28 h.
5. The production method according to claim 1, wherein in the step (2), the drying temperature is 50 to 80 ℃.
6. The preparation method according to claim 1, wherein in the step (3), the calcination temperature is 450-650 ℃, the calcination time is 3-6 h, and the temperature rise rate is 5-10 ℃/min.
7. Co/g-C prepared by the synthesis method of claim 1 3 N 4 The composite photocatalyst is applied to efficient removal of 2-Mercaptobenzothiazole (MBT) in the environment.
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| Publication number | Priority date | Publication date | Assignee | Title |
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