CN115957769A - MoO 2 @ CoFe LDHs photocatalyst and application thereof in degrading tetracycline with persulfate in synergy mode - Google Patents
MoO 2 @ CoFe LDHs photocatalyst and application thereof in degrading tetracycline with persulfate in synergy mode Download PDFInfo
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- 239000004098 Tetracycline Substances 0.000 title claims abstract description 24
- 229960002180 tetracycline Drugs 0.000 title claims abstract description 24
- 229930101283 tetracycline Natural products 0.000 title claims abstract description 24
- 235000019364 tetracycline Nutrition 0.000 title claims abstract description 24
- 150000003522 tetracyclines Chemical class 0.000 title claims abstract description 24
- 229910003321 CoFe Inorganic materials 0.000 title claims abstract description 20
- 239000011941 photocatalyst Substances 0.000 title claims description 7
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 title abstract description 14
- 230000000593 degrading effect Effects 0.000 title description 8
- 238000006731 degradation reaction Methods 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 230000015556 catabolic process Effects 0.000 claims abstract description 17
- 230000001699 photocatalysis Effects 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 49
- 238000003756 stirring Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 6
- 229910017855 NH 4 F Inorganic materials 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims description 4
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012456 homogeneous solution Substances 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229910016870 Fe(NO3)3-9H2O Inorganic materials 0.000 claims 1
- 230000032683 aging Effects 0.000 claims 1
- 230000001678 irradiating effect Effects 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000003344 environmental pollutant Substances 0.000 abstract description 11
- 231100000719 pollutant Toxicity 0.000 abstract description 11
- 239000003242 anti bacterial agent Substances 0.000 abstract description 7
- 229940088710 antibiotic agent Drugs 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 229960001545 hydrotalcite Drugs 0.000 abstract description 5
- 229910001701 hydrotalcite Inorganic materials 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 4
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 abstract description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- -1 hydrotalcite compound Chemical class 0.000 abstract 2
- 230000000694 effects Effects 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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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 discloses a hydrotalcite compound and application thereof as a photocatalytic material to degradation of tetracycline in cooperation with persulfate. The hydrotalcite composite product is MoO 2 @ CoFe LDH, and discloses the application of the hydrotalcite compound and persulfate which are used for photocatalytic degradation of antibiotics under the combined action, the reaction condition is mild,the pollutant removal rate is high, the speed is high, and the material after catalytic degradation is easy to recycle.
Description
Technical Field
The invention relates to the field of photocatalytic degradation, and in particular relates to a novel hydrotalcite-based composite material and application thereof as a photocatalytic material to synergistically degrade antibiotics in water with persulfate.
Background
Most organic pollutants contained in the industrial wastewater, such as dyes, phenols, antibiotics and the like, are stable in structure and difficult to degrade. Antibiotics are widely used in the fields of medicine, health, agriculture, biology, etc., but in recent years, due to inappropriate use in medicine, livestock raising, etc., the threats to environmental safety, ecosystem, and human health have been increasing. Tetracycline serving as one of antibiotics cannot be completely absorbed by a human body and can enter the environment through urine and excrement, and is not easy to degrade and has high chemical stability. Therefore, degradation of tetracycline in aqueous systems is essential. The mainstream treatment technologies include chemical catalytic oxidation, physical adsorption and biodegradation, but the methods have secondary pollution, long period and high cost respectively, and the limited photocatalysis technologies become research hotspots in the aspects of energy, environment and the like due to the characteristics of environmental protection, simple operation and high efficiency
Compared with other methods, photocatalysis has the advantages of mild reaction conditions, simple equipment, less secondary pollution, utilization of sunlight as the only external energy input and the like, and is a promising pollution control technology.
Semiconductor photocatalysis has been widely studied, and in a system based on a semiconductor catalyst, a Layered Double Hydroxide (LDHs) based material has a special layered structure and has the advantages of good dispersion of contained substances, high specific surface area, small grain size, proper acidity and alkalinity, high thermal stability and the like. Under the excitation of visible light, the LDHs material can generate a large amount of photo-generated electrons and holes for degrading pollutants. However, single-phase LDHs still have many limitations, the electron transmission rate is slow, and the problems of electron-hole pair recombination annihilation and the like inhibit the photocatalytic performance of the LDHs. In order to solve the problem, different semiconductor materials can be utilized for compounding to construct a heterojunction, a built-in electric field is formed, and electron transfer is promoted, so that the compounding of electrons and holes is inhibited. On one hand, the electrons and the holes are accumulated at a higher energy level, and the redox capacity is stronger; on the other hand, more electrons and holes are used for generating active free radicals to act on subsequent degradation reactions. In addition, although the photocatalytic process has a good effect of degrading pollutants, the photocatalytic process has low light energy utilization efficiency and generates limited active free radicals, so the process is slow. Are currently based on SO 4 · - The photocatalytic method of (2) is widely applied to degradation of organic pollutants. SO (SO) 4 · - Persulfate salts can be generally activated and generated by light, microwaves, ultrasound, heat, transition metal ions, metal and metal-free catalysts, and the like. Wherein the SO is activated by light energy and a semiconductor 4 · — The secondary pollution can not be caused, extra energy is not provided manually, and the cost for degrading pollutants is greatly saved. PS has high electron affinity, and photo-generated electrons generated by the semiconductor can be rapidly captured by the PS to form SO4 with strong oxidizing property — The degradation effect on pollutants in water is very obvious, the time is shortened to one fourth of the original time, and the degradation efficiency is greatly improved.
Therefore, an LDHs/persulfate system is coupled with photocatalysis to construct a multi-reaction coupled advanced oxidation system for efficiently degrading waterOrganic contaminants are the hot spot of current research. The patent successfully prepares the novel MoO 2 The material is a @ LDHs composite material, and a multi-reaction coupling type advanced oxidation system (photocatalysis + persulfate activation) is constructed by coupling persulfate.
Disclosure of Invention
The invention aims to provide novel MoO 2 The composite material is used as a photocatalytic material and is applied to degrading antibiotics and azo dyes in cooperation with persulfate.
The technical scheme adopted by the invention is as follows:
MoO of the invention 2 @ CoFe LDHs are generally prepared as follows:
(1)MoO 2 preparation of
Weighing 1.0-1.5 g of ammonium molybdate tetrahydrate, dispersing in 30-50 mL of deionized water, stirring for 30-60 min at room temperature until the solution becomes transparent, and marking as solution A; weighing 0.1-0.15 CTAB (cetyl trimethyl ammonium bromide) and dissolving in ethanol, wherein the amount of the ethanol is about 3-5 ml, and forming a homogeneous solution which is marked as solution B; solution B was added dropwise to solution a with constant stirring. Concentrated HNO 3 Was added dropwise to the mixed solution to adjust the pH to 1.5. Pouring the solution into a 100mL Teflon stainless steel high-pressure reaction kettle, and heating for 48h at 180 ℃; after the reaction is finished, the reaction kettle is cooled to room temperature. Washing with ethanol and distilled water for 3 times, and drying at 50-60 deg.C.
(2)MoO 2 Preparation of @ LDHs:
taking Co (NO) 3 ) 2 6H 2 O 4mmol，Fe(NO 3 ) 3 9H 2 O2 mmol, a certain amount of MoO 2 Dissolving in 50ml water, magnetically stirring for 30min to obtain a uniform solution, and adding 15mmol NH 4 F, stirring for 30min again to mix uniformly, and marking as a solution A; 21mmol NaOH,3mmol Na are taken 2 CO 3 Dissolved in 50ml of distilled water and marked as solution B; solution B was added dropwise to solution A with constant stirring, the pH was adjusted to 9.5, and stirring was further continued for 5h. The precipitate was then aged at room temperature for 12h. Washing with ethanol and distilled water for 3 times, and drying at 50-60 deg.C.
The present invention provides a MoO 2 The combination of @ CoFe LDHs and persulfate can be applied to the degradation of antibiotics, and more particularly, tetracycline.
Further, the method of the present invention comprises: 5-30 mg of MoO 2 @ LDHs and 0.01-1 g of sodium persulfate are placed in an organic matter aqueous solution, irradiated under a xenon lamp for 0.5-2 h, and stirred to degrade pollutants; the initial mass concentration of the pollutants is 10-100 mg/L respectively.
The MoO provided by the invention 2 The energy gap and the grain size of the @ CoFe LDHs are both small, and the electronic-hole pairs with catalytic activity can be generated under the proper illumination, when pollutants (tetracycline) are adsorbed on the surface of hydrotalcite, the electronic-hole pairs can be captured, sulfate radicals are activated, and the pollutants are degraded, so that the aim of purifying the wastewater is fulfilled.
The MoO of the invention 2 The method is adopted to calculate the degradation rate of the @ CoFe LDHs and the co-degradation of pollutants in water by using the @ CoFe LDHs as a photocatalytic material and persulfate, the reaction condition is mild, the degradation efficiency is high, the effect is obvious, and the material after catalytic degradation is easy to recycle.
Drawings
FIG. 1 shows MoO in example 1 2 ，CoFe LDH，MoO 2 X-ray diffraction pattern of @ CoFe LDHs;
FIG. 2 is a graph of the degradation rate of the tetracycline of example 2;
FIG. 3 is a standard graph of the tetracycline of example 3.
Detailed Description
The invention will be further illustrated by the following specific examples, without limiting the scope of the invention thereto.
Example 1: the preparation method of the photocatalyst comprises the following steps:
(1)MoO 2 preparation of
Weighing 1.0-1.5 g of ammonium molybdate tetrahydrate, dispersing in 30-50 mL of deionized water, stirring for 30-60 min at room temperature until the solution becomes transparent, and marking as solution A; weighing 0.1-0.15 CTAB (cetyl trimethyl ammonium bromide) and dissolving in ethanol, wherein the amount of the ethanol is about 3-5 ml, and forming a homogeneous solution which is marked as solution B; dropwise adding the solution B into the solutionSolution a and stirring was continued. Concentrated HNO 3 Was added dropwise to the mixed solution to adjust the pH to 1.5. Pouring the solution into a 100mL Teflon stainless steel high-pressure reaction kettle, and heating for 48h at 180 ℃; after the reaction is finished, the reaction kettle is cooled to room temperature. Washing with ethanol and distilled water for 3 times, drying at 50-60 deg.C to obtain MoO 2 。
(2) Preparation of CoFe LDH:
taking Co (NO) 3 ) 2 6H 2 O 4mmol，Fe(NO 3 ) 3 9H 2 O2 mmol, magnetically stirring for 30min to form a homogeneous solution, and adding 15mmol NH 4 F, stirring for 30min again to mix uniformly, and marking as a solution A; 21mmol NaOH and 3mmol Na are taken 2 CO 3 Dissolved in 50ml of distilled water and marked as solution B; solution B was added dropwise to solution A with constant stirring, the pH was adjusted to 9.5, and stirring was further continued for 5h. The precipitate was then aged at room temperature for 12h. Washing with ethanol and distilled water for 3 times, and drying at 50-60 deg.C.
(3)MoO 2 Preparation of @ LDHs:
taking Co (NO) 3 ) 2 ·6H 2 O 4mmol，Fe(NO 3 ) 3 ·9H 2 O2 mmol, a certain amount of MoO 2 Dissolving in 50ml water, magnetically stirring for 30min to obtain a uniform solution, and adding 15mmol NH 4 F, stirring for 30min again to mix uniformly, and marking as a solution A; 21mmol NaOH and 3mmol Na are taken 2 CO 3 Dissolved in 50ml of distilled water and marked as solution B; solution B was added dropwise to solution A with constant stirring, the pH was adjusted to 9.5, and stirring was further continued for 5h. The precipitate was then aged at room temperature for 12h. Washing with ethanol and distilled water for 3 times, drying at 50-60 deg.C to obtain MoO 2 @CoFe LDHS。
Example 2: photocatalytic experiment
The method adopts simulated sunlight to degrade tetracycline as a model reaction, and determines the relative concentration of tetracycline solution at 357nm through measuring the absorbance of the tetracycline solution by an ultraviolet-visible spectrophotometer, so as to evaluate the photocatalytic performance of the material. The light source is a 300W xenon lamp (adopting a filter to filter out ultraviolet light and retain 400nm<λ<Visible light of 800 nm), light source distanceThe reaction solution was 25cm. At a temperature and pH, 10mg of catalytic material was added to a two-layer quartz reaction tube containing 100mL of 40mg/L tetracycline solution, followed by 0.0238g of sodium persulfate. The xenon lamp was then turned on to perform the photocatalytic experiment under continuous light and magnetic stirring. After the reaction, samples were taken every 5min, filtered through a 0.22 μm organic filter membrane, and then the absorbance of the filtrate at 357nm was measured using an ultraviolet-visible spectrophotometer, and converted to the relative mass concentration C (mg/L) of tetracycline according to a standard curve. According to C/C 0 Calculating the degradation rate (. Eta.%) of tetracycline C 0 (mg/L) is the starting mass concentration of tetracycline.
η＝C/C 0 (1)
In the experiment, respectively do
1. Blank experiment (no catalyst);
2. addition of catalyst MoO alone 2 、MoO 2 @LDHs；
3. Adding catalyst MoO 2 、CoFe-LDH MoO 2 @ LDHs and persulfate Na 2 S 2 O 8 ；
4. Addition of catalyst MoO in the absence of light 2 @ LDHs and persulfate Na 2 S 2 O 8 。
The degradation rate curve is shown in figure 2. As can be seen from the figure, the catalyst has no degradation effect on tetracycline in no light, and is only Na 2 S 2 O8 is activated slightly under illumination, and has a weak effect of degrading tetracycline, namely about 20%. Single-phase MoO 2 The material has a certain promotion effect under illumination, but the activation effect on the peroxydisulfate is not obvious, and the degradation rate is 48%. But CoFe LDHs and MoO are co-precipitated 2 The effect is obviously improved by compounding, and the degradation rate is improved to 85-90% in 30 min. Compared with the conventional photodegradation, the method has shorter time for treating the pollutants and reduces the consumption of energy.
Example 3 preparation of a Standard Curve
Based on a tetracycline solution with an initial concentration of 100mg/L, solutions with concentrations of 5.00mg/L, 10.00mg/L, 20.00mg/L, 30.00mg/L, 40.00mg/L and 50.00mg/L are prepared, deionized water is used as a blank reference, an Shimadzu 2550 type ultraviolet-visible spectrophotometer is used for measuring the absorbance of each solution at 357nm, and a standard curve of the absorbance A-the concentration C of the tetracycline solution is obtained by linear fitting, as shown in FIG. 3.
Claims (5)
1. MoO 2 The @ CoFe LDHs photocatalyst is characterized by being prepared by the following method:
(1)MoO 2 the preparation of (1):
MoO was obtained by reacting ammonium molybdate tetrahydrate with CTAB (cetyltrimethylammonium bromide) 2 ；
(2)MoO 2 Preparation of @ CoFe LDHs:
taking Co (NO) 3 ) 2 6H 2 O、Fe(NO 3 ) 3 9H 2 O', moO obtained in step (1) 2 Dissolving in water, magnetically stirring to obtain uniform solution, and adding NH 4 F, mixing uniformly and marking as a solution A;
taking NaOH and Na 2 CO 3 Dissolving in 50ml of distilled water, and marking as solution B;
dropwise adding the solution B into the solution A under continuous stirring, adjusting the pH to 8-11, further stirring, aging the precipitate at room temperature, washing, and drying to obtain MoO 2 @ CoFe LDHs photocatalyst.
2. The MoO of claim 1 2 The @ CoFe LDHs photocatalyst is characterized in that MoO is obtained in the step (1) 2 The preparation method comprises the following steps: weighing 1.0-1.5 g of ammonium molybdate tetrahydrate, dispersing in 30-50 mL of deionized water, stirring at room temperature for 30-60 min until the solution becomes transparent, and marking as solution A; weighing 0.1-0.15 CTAB (cetyl trimethyl ammonium bromide) and dissolving in ethanol with the amount of about 3-5 ml to form a homogeneous solution, recording as the solution B, dropwise adding the solution B into the solution A and continuously stirring; concentrated HNO 3 Dropwise adding the mixture into the mixed solution, and adjusting the pH value to 1.5; pouring the solution into a high-pressure reaction kettle, and heating for 48 hours at 180 ℃; after the reaction is finished, the reaction kettle is cooled to room temperature. Washing with ethanol and distilled water for 3 times, 5 times respectivelyDrying at 0-60 deg.c.
3. The MoO of claim 2 2 The @ CoFe LDHs photocatalyst is characterized in that MoO is obtained in the step (2) 2 The preparation method of the @ CoFe LDHs comprises the following steps: taking Co (NO) 3 ) 2 6H 2 O 4mmol，Fe(NO 3 ) 3 9H 2 O2 mmol, a certain amount of MoO 2 Dissolving in 50ml water, magnetically stirring for 30min to obtain a uniform solution, and adding 15mmol NH 4 F, stirring for 30min again to mix uniformly, and marking as a solution A; 21mmol NaOH and 3mmol Na are taken 2 CO 3 Dissolved in 50ml of distilled water and marked as solution B; solution B was added dropwise to solution A with constant stirring, the pH was adjusted to 9.5, stirring was further carried out for 5h, and the precipitate was aged at room temperature for 12h. Washing with ethanol and distilled water for 3 times, and drying at 50-60 deg.C.
4. The MoO of any of claims 1-3 2 The application of @ CoFe LDHs in cooperation with sodium persulfate as a tetracycline degradation photocatalytic material.
5. Use according to claim 4, characterized in that: 10-100 mg of MoO 2 Putting @ LDHs and 0.01-1 g of sodium persulfate into the tetracycline aqueous solution, irradiating for 0.5-2 h under a xenon lamp, and stirring to degrade the tetracycline; the initial mass concentration of the tetracycline is 10-100 mg/L respectively.
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| CN118527138A (en) * | 2024-07-25 | 2024-08-23 | 中国科学院合肥物质科学研究院 | Mo/BNS catalyst and preparation method and application thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107774283A (en) * | 2017-10-24 | 2018-03-09 | 中南大学 | A kind of molybdenum disulfide hybrid hydrotalcite composite material and its preparation method and application |
| CN108435191A (en) * | 2018-04-26 | 2018-08-24 | 济南大学 | A kind of SnNb2O6/ CoFe-LDH piece piece composite magnetic heterojunction structure catalyst and its preparation method and application |
| CN108786881A (en) * | 2018-09-06 | 2018-11-13 | 江苏大学 | Visible light-responded molybdenum dioxide nanometer sheet/class graphene carbonitride catalysis material and its preparation method and application |
| CN110801839A (en) * | 2019-11-21 | 2020-02-18 | 中国科学技术大学 | Co2FeAl-LDH, preparation method thereof and method for degrading pollutants |
| CN111054395A (en) * | 2019-12-10 | 2020-04-24 | 中国环境科学研究院 | Visible-light-driven photocatalyst, and preparation method and application thereof |
| CN111135818A (en) * | 2019-12-13 | 2020-05-12 | 上海电力大学 | MoO (MoO)3Preparation method of/ZnAl layered double hydroxide composite material, product and application thereof |
| CN113972076A (en) * | 2021-10-26 | 2022-01-25 | 南京信息工程大学 | Molybdenum-based electrode material and preparation method and application thereof |
| CN113998758A (en) * | 2021-10-08 | 2022-02-01 | 东北大学 | Method for degrading antibiotics by activating persulfate through photoelectric synergistic graphite-phase carbon nitride |
| CN114956194A (en) * | 2022-04-22 | 2022-08-30 | 浙江华源颜料股份有限公司 | Iron oxyhydroxide and application thereof in cooperative degradation of antibiotics with persulfate |
| CN115245839A (en) * | 2021-04-28 | 2022-10-28 | 长春理工大学 | Preparation method of phosphomolybdic acid intercalated 3D-LDHs photo-Fenton catalyst |
-
2022
- 2022-11-21 CN CN202211455135.8A patent/CN115957769A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107774283A (en) * | 2017-10-24 | 2018-03-09 | 中南大学 | A kind of molybdenum disulfide hybrid hydrotalcite composite material and its preparation method and application |
| CN108435191A (en) * | 2018-04-26 | 2018-08-24 | 济南大学 | A kind of SnNb2O6/ CoFe-LDH piece piece composite magnetic heterojunction structure catalyst and its preparation method and application |
| CN108786881A (en) * | 2018-09-06 | 2018-11-13 | 江苏大学 | Visible light-responded molybdenum dioxide nanometer sheet/class graphene carbonitride catalysis material and its preparation method and application |
| CN110801839A (en) * | 2019-11-21 | 2020-02-18 | 中国科学技术大学 | Co2FeAl-LDH, preparation method thereof and method for degrading pollutants |
| CN111054395A (en) * | 2019-12-10 | 2020-04-24 | 中国环境科学研究院 | Visible-light-driven photocatalyst, and preparation method and application thereof |
| CN111135818A (en) * | 2019-12-13 | 2020-05-12 | 上海电力大学 | MoO (MoO)3Preparation method of/ZnAl layered double hydroxide composite material, product and application thereof |
| CN115245839A (en) * | 2021-04-28 | 2022-10-28 | 长春理工大学 | Preparation method of phosphomolybdic acid intercalated 3D-LDHs photo-Fenton catalyst |
| CN113998758A (en) * | 2021-10-08 | 2022-02-01 | 东北大学 | Method for degrading antibiotics by activating persulfate through photoelectric synergistic graphite-phase carbon nitride |
| CN113972076A (en) * | 2021-10-26 | 2022-01-25 | 南京信息工程大学 | Molybdenum-based electrode material and preparation method and application thereof |
| CN114956194A (en) * | 2022-04-22 | 2022-08-30 | 浙江华源颜料股份有限公司 | Iron oxyhydroxide and application thereof in cooperative degradation of antibiotics with persulfate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118527138A (en) * | 2024-07-25 | 2024-08-23 | 中国科学院合肥物质科学研究院 | Mo/BNS catalyst and preparation method and application thereof |
| CN118527138B (en) * | 2024-07-25 | 2024-09-27 | 中国科学院合肥物质科学研究院 | Mo/BNS catalyst and preparation method and application thereof |
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