CN113443695B - Molybdenum carbide auxiliary agent, preparation method thereof and application thereof in Fenton reaction degradation of organic pollutants - Google Patents
Molybdenum carbide auxiliary agent, preparation method thereof and application thereof in Fenton reaction degradation of organic pollutants Download PDFInfo
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Abstract
The invention belongs to the field of heterogeneous catalysis and water pollutant treatment, and particularly relates to a molybdenum carbide catalytic material, a preparation method thereof and application thereof in catalyzing hydrogen peroxide to degrade organic pollutants by a Fenton method. The method takes molybdenum carbide as a cocatalyst and hydrogen peroxide as an oxidant, and organic pollutants are degraded under the existence of Fenton main catalyst. The method has the advantages of simple operation, mild reaction conditions, short degradation time, high repeatability, easy synthesis of the auxiliary agent, simple equipment requirement and certain industrial application prospect. The invention accelerates the circulation rate of Fe (III)/Fe (II) in Fenton reaction by utilizing the electron-rich characteristic of molybdenum carbide, and inhibits the ineffective decomposition of hydrogen peroxide, thereby improving the Fenton reaction efficiency. The invention provides a using method for developing a low-cost, stable and efficient supported catalyst, and has potential application prospect.
Description
Technical Field
The invention belongs to the field of heterogeneous catalysis and water pollutant treatment, and particularly relates to a molybdenum carbide catalytic material, a preparation method thereof and application thereof in catalyzing hydrogen peroxide to degrade organic pollutants by a Fenton method.
Background
With the continuous development of the industrial level in China, the environmental problems are increasingly prominent, wherein the problem of organic pollutant emission of water bodies is more serious. Fenton oxidation technology refers to catalytic decomposition of H by a catalyst 2 O 2 The reaction generates a large number of hydroxyl free radicals with strong oxidability and no selectivity, and realizes the process of oxidative degradation of organic pollutants in water. Fenton reaction efficiency is limited mainly by the following two aspects: 1. in the catalytic process, the reduction rate of the high-valence metal in the catalyst is slower, so that the rate of the whole Fenton process is inhibited. 2. The reduction step of the metal is accompanied by the generation of oxygen, which is regarded as ineffective decomposition of hydrogen peroxide, reducing the utilization of hydrogen peroxide. Therefore, how to promote the electron circulation process of the catalyst, promote the oxidation step-by-step rate of hydrogen peroxide and inhibit the generation of oxygen is a key to improving the Fenton reaction efficiency.
Disclosure of Invention
The invention aims to provide a preparation method and application of molybdenum carbide, which utilize the electron-rich characteristic of the prepared molybdenum carbide to promote the electron circulation rate of a main catalyst in Fenton reaction, inhibit the ineffective decomposition of hydrogen peroxide and improve the degradation efficiency of pollutants. The method is simple in synthesis and easy to operate, shows excellent auxiliary catalytic effect in Fenton reaction, and has potential application value.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the molybdenum carbide auxiliary agent comprises the following specific scheme:
(1) Preparing a molybdenum precursor solution (solution A) and a carbon precursor solution (solution B) respectively, dropwise adding the solution A into the solution B under the stirring condition, uniformly stirring, and evaporating the solvent to obtain a solid C.
(2) And (3) placing the solid C in a tube furnace for calcination under the protection of inert gas to obtain the molybdenum carbide.
Further, in the step (1), the solvent in the molybdenum precursor solution or the carbon precursor solution is water or ethanol.
Further, in step (1), the molybdenum precursor includes one of ammonium molybdate, sodium molybdate, and molybdenum chloride. The carbon precursor comprises one or more of dicyandiamide, melamine, urea, glucose, and pramipexole F127. Wherein the mass ratio of the molybdenum-containing precursor to the carbon-containing precursor is 0.2-1: 1.
further, the stirring temperature in the step (1) is 25-80 ℃, and the stirring time is 1-4 h.
Further, in the step (2), the inert atmosphere comprises one of argon and nitrogen, the annealing temperature is 700-900 ℃, and the time is 2-4 hours.
The invention also discloses application of the molybdenum carbide promoter: molybdenum carbide is used as a cocatalyst, and hydrogen peroxide is used as an oxidant to degrade common water organic pollutants in a multiphase Fenton oxidation system.
Further, the Fenton oxidation system catalyst is one of ferrous sulfate, nano zero-valent iron and carbon-coated iron nanospheres.
Further, the organic pollutant comprises rhodamine B, golden orange II and bisphenol A.
Further, the Fenton system temperature is 25-60 ℃ and the degradation time is 5-30 min.
Further, the mass ratio of the hydrogen peroxide to the pollutant is 1-20.
Compared with the prior art, the invention has the following advantages:
(1) The invention discloses a preparation method of molybdenum carbide, and the molybdenum carbide is introduced into Fenton reaction. By utilizing the electron-rich characteristic of molybdenum carbide, the electron circulation process of the catalyst in the Fenton reaction is accelerated, the ineffective decomposition of hydrogen peroxide is inhibited, and the Fenton reaction efficiency is improved. Experimental results show that the Fenton reaction system added with the molybdenum carbide auxiliary agent has higher pollutant degradation efficiency.
(2) The invention has simple process, low cost and strong stability, and is beneficial to large-scale industrialized production and application.
Drawings
FIG. 1 is an XRD pattern of carbon-coated molybdenum carbide a in example 1 of the present invention;
FIG. 2 is a Raman spectrum of carbon-coated molybdenum carbide a in example 1 of the present invention;
FIG. 3 is an SEM image of carbon-coated molybdenum carbide a prepared according to example 1 of the invention;
FIG. 4 is a graph of the degradation of RhB by carbon coated molybdenum carbide-ferrous sulfate in example 4 of the present invention;
FIG. 5 is a graph of carbon coated molybdenum carbide-nano zero valent iron degradation RhB in example 5 of the present invention;
FIG. 6 is a graph showing the degradation of RhB by carbon-coated molybdenum carbide-carbon-coated iron nanospheres in example 6 of the present invention.
Detailed Description
In order to make the contents of the present invention more easily understood, the technical scheme of the present invention will be further described with reference to the specific embodiments, but the present invention is not limited thereto.
Example 1
Molybdenum carbide a (carbon-coated molybdenum carbide, mo) 2 C@C) preparation:
at room temperature, 0.5g of molybdenum pentachloride was dissolved in 10mL of ethanol to form solution A, and 1g of urea was dissolved in 10mL of ethanol to form solution B. Solution A was added dropwise to solution B, and 0.5g glucose was added, stirred in a 25℃water bath for 2h, stirred well and then warmed to 80℃and the solvent evaporated. And (3) heating to 800 ℃ in a tube furnace at a heating rate of 5 ℃/min by taking nitrogen as a shielding gas, and preserving heat for 3 hours to obtain the molybdenum carbide a.
The molybdenum carbide a is characterized in that the molybdenum carbide is coated by in-situ grown carbon, and the stability of the molybdenum carbide can be maintained under more extreme reaction conditions.
Example 2
Molybdenum carbide b (porous molybdenum carbide, porus-Mo) 2 C) Is prepared from the following steps:
at normal temperature, 0.5g of molybdenum pentachloride was dissolved in 5mL of ethanol to form solution A, and 1g of urea was dissolved in 5mL of ethanol to form solution B. Solution a was added dropwise to solution B to form solution C. 1.5g of Pranik F127 was dissolved in 10mL of ethanol to form solution D, solution C was added dropwise to solution D, stirred in a water bath at 25℃for 2h, then warmed to 80℃and the solvent evaporated. And (3) heating to 300 ℃ at a heating rate of 2 ℃/min in a tube furnace by taking nitrogen as a shielding gas, preserving heat for 3h, heating to 800 ℃ at a heating rate of 5 ℃/min, and preserving heat for 3h to obtain the molybdenum carbide b.
The molybdenum carbide a is characterized in that F127 is used as a soft template agent to induce the molybdenum carbide to form a porous structure, thereby increasing the specific surface area and improving the catalytic activity.
Example 3
Molybdenum carbide c (mesoporous molybdenum carbide mes-Mo 2 C) Is prepared from the following steps:
0.5g of ammonium molybdate was dissolved in water at 80℃in an oil bath to form solution A and 1g of dicyandiamide was dissolved in water to form solution B. Solution A was added dropwise to solution B, stirred in a water bath at 25℃for 2h, then warmed to 80℃and the solvent evaporated. Heating to 550 ℃ in a tube furnace at a heating rate of 5 ℃/min by taking nitrogen as a protective gas, preserving heat for 2h, heating to 750 ℃ and preserving heat for 2h to obtain molybdenum carbide c.
The molybdenum carbide c is characterized in that in the annealing process, the material passes through MoO x @C 3 N 4 And in the middle process, finally forming mesoporous molybdenum carbide.
Example 4
Activity test of ferrous sulfate-molybdenum carbide Fenton method for degrading rhodamine B (RhB)
10mg of molybdenum carbide a was dispersed in 50mL of a solution containing 20ppm of rhodamine B, and 2mg of FeSO was added 4 ·6H 2 O, stirring for 15min to reach adsorption and desorption equilibrium, taking 1.5mL of solution, filtering, and marking as a sample No. 0. 100 μL 3%H is added 2 O 2 The solution (60 ppm concentration in the system) was then sampled every two minutes until the tenth minute sampling was completed. Each sample was tested for absorbance at 554nm using an ultraviolet-visible spectrophotometer and the absorbance of each sample was recorded (C x ) Absorbance with sample No. 0 (C 0 ) The ratio is marked as C x /C 0 A graph of rhodamine B versus time was recorded.
Example 5
Nanometer zero-valent iron-molybdenum carbide Fenton method rhodamine B (RhB) degradation activity test
Dispersing 10mg of molybdenum carbide a in 50mL of solution containing 20ppm of rhodamine B, adding 4mg of nano zero-valent iron, stirring for 15min to reach adsorption and desorption equilibrium, and taking 1.5mL of solution at the momentFiltration was performed and designated as sample No. 0. 100 μL 3%H is added 2 O 2 The solution (60 ppm concentration in the system) was then sampled every two minutes until the tenth minute sampling was completed. Each sample was tested for absorbance at 554nm using an ultraviolet-visible spectrophotometer and the absorbance of each sample was recorded (C x ) Absorbance with sample No. 0 (C 0 ) The ratio is marked as C x /C 0 A graph of rhodamine B versus time was recorded.
Example 6
Carbon-coated iron nanosphere-molybdenum carbide Fenton method rhodamine B (RhB) degradation activity test
10mg of molybdenum carbide a is dispersed in 50mL of solution containing 20ppm of rhodamine B, 4mg of carbon-coated iron nanospheres are added, and stirring is carried out for 15min to reach adsorption and desorption equilibrium, at the moment, 1.5mL of solution is taken, and the solution is filtered and marked as a sample No. 0. 100 μL 3%H is added 2 O 2 The solution (60 ppm concentration in the system) was then sampled every two minutes until the tenth minute sampling was completed. Each sample was tested for absorbance at 554nm using an ultraviolet-visible spectrophotometer and the absorbance of each sample was recorded (C x ) Absorbance with sample No. 0 (C 0 ) The ratio is marked as C x /C 0 A graph of rhodamine B versus time was recorded.
Fig. 1 is an XRD pattern of molybdenum carbide a, in which diffraction peaks of 2θ=36.6° and 42.6 ° correspond to (111) and (200) crystal planes of molybdenum carbide, respectively,
FIG. 2 is a Raman spectrum of molybdenum carbide a, whose peaks at 1300cm-1 and 1580cm-1 correspond to carbon in amorphous and graphitic states, respectively, demonstrating the presence of elemental carbon in molybdenum carbide a.
Fig. 3 is an SEM image of molybdenum carbide, and it can be seen that the surface of molybdenum carbide a has a smooth-surfaced lamellar structure.
Fig. 4 is a graph of degradation of RhB by carbon-coated molybdenum carbide-ferrous sulfate in example 4 of the present invention, showing that molybdenum carbide itself does not have fenton activity, but it significantly improves the degradation efficiency of iron sulfate to dyes.
Fig. 5 is a graph of carbon-coated molybdenum carbide-nano zero-valent iron degradation RhB in example 5 of the present invention, illustrating that molybdenum carbide itself does not have fenton activity, but it significantly improves the efficiency of nano zero-valent iron degradation to dyes.
Fig. 6 is a graph of degradation of RhB by the carbon-coated molybdenum carbide-carbon-coated iron nanospheres in example 6 of the present invention, showing that molybdenum carbide itself does not have fenton activity, but it significantly improves the degradation efficiency of the carbon-coated iron nanospheres to dyes.
Claims (4)
1. The application of the molybdenum carbide auxiliary agent in Fenton method degradation of organic pollutants is characterized in that: the molybdenum carbide auxiliary agent performs Fenton reaction in a Fenton reaction main catalyst-pollutant-hydrogen peroxide system;
the preparation method of the molybdenum carbide auxiliary agent comprises the following steps:
(1) Dissolving a carbon-containing precursor in water or ethanol to obtain a solution A;
(2) Dissolving a molybdenum-containing precursor in water or ethanol to obtain a solution B;
(3) Dropwise adding the solution B into the solution A under the heating condition, uniformly stirring, evaporating the solvent to obtain a white solid, and placing the white solid in a tube furnace for annealing and calcining under the protection of inert atmosphere to obtain a molybdenum carbide auxiliary product;
the carbon-containing precursor is urea and glucose, and the molybdenum-containing precursor is molybdenum pentachloride;
the annealing temperature in the step (3) is 700-900 ℃ and the time is 2-4 hours;
in the solution in the step (3), the mass ratio of the molybdenum-containing precursor to the carbon-containing precursor is 0.2-1: 1.
2. the use according to claim 1, characterized in that: in the step (3), the stirring temperature is 25-80 o And C, stirring for 1-4 hours.
3. The use according to claim 1, characterized in that: the Fenton reaction main catalyst comprises one of ferrous sulfate, nano zero-valent iron and nano carbon coated iron, the concentration of pollutants is 10-50 ppm, the pollutants comprise one of rhodamine B, bisphenol A and gold orange II, and the concentration of hydrogen peroxide is 100-300 ppm.
4. The use according to claim 1, characterized in that: the Fenton reaction temperature is 25-60 ℃, and the reaction time is 5-30 min.
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| JP2004337798A (en) * | 2003-05-19 | 2004-12-02 | Nomura Plating Co Ltd | Oxide catalyst and detoxification method of organic matter-containing wastewater using the same |
| CN112121844A (en) * | 2020-10-26 | 2020-12-25 | 江西科技师范大学 | Preparation method of molybdenum disulfide carbide/sulfur-doped carbon nitride heterojunction and application of molybdenum disulfide carbide/sulfur-doped carbon nitride heterojunction in degradation of organic pollutant rhodamine B |
| CN112194136A (en) * | 2020-10-22 | 2021-01-08 | 哈尔滨工业大学 | Preparation method of three-dimensional bouquet structure alpha-molybdenum carbide @ carbon with efficient photo-thermal conversion characteristic |
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| KR101481111B1 (en) * | 2013-02-05 | 2015-01-15 | 한국과학기술연구원 | Method for Synthesis of Molybdenum carbide catalyst for Hydrodeoxygenation |
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| JP2004337798A (en) * | 2003-05-19 | 2004-12-02 | Nomura Plating Co Ltd | Oxide catalyst and detoxification method of organic matter-containing wastewater using the same |
| CN112194136A (en) * | 2020-10-22 | 2021-01-08 | 哈尔滨工业大学 | Preparation method of three-dimensional bouquet structure alpha-molybdenum carbide @ carbon with efficient photo-thermal conversion characteristic |
| CN112121844A (en) * | 2020-10-26 | 2020-12-25 | 江西科技师范大学 | Preparation method of molybdenum disulfide carbide/sulfur-doped carbon nitride heterojunction and application of molybdenum disulfide carbide/sulfur-doped carbon nitride heterojunction in degradation of organic pollutant rhodamine B |
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