CN106492817B - A kind of porous Fe VO4Nanometer rods class Fenton photochemical catalyst and its preparation method and application - Google Patents

A kind of porous Fe VO4Nanometer rods class Fenton photochemical catalyst and its preparation method and application Download PDF

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CN106492817B
CN106492817B CN201611156627.1A CN201611156627A CN106492817B CN 106492817 B CN106492817 B CN 106492817B CN 201611156627 A CN201611156627 A CN 201611156627A CN 106492817 B CN106492817 B CN 106492817B
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夏杰祥
曾洁
陈志刚
李华明
狄俊
季梦夏
尹盛
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Jiangsu University
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Abstract

The present invention provides a kind of porous Fe VO4Nanometer rods class Fenton photochemical catalyst and its preparation method and application, preparation method include the following steps: (1) by [Omim] FeCl4It is dissolved in distilled water and obtains solution A, by NH4VO4It is dissolved in hot water and obtains solution B, then solution A is added dropwise in B solution, after being added dropwise, be placed in stirring at normal temperature on magnetic stirring apparatus, obtain suspension;Step 2, the suspension for obtaining step 1 are transferred in autoclave, and hydro-thermal reaction is carried out in baking oven, after completion of the reaction, are washed with deionized water and dehydrated alcohol, obtain presoma FeVO after drying4·1.1H2O nano-bar material;Step 3, by presoma FeVO4·1.1H2O nano-bar material is calcined to arrive the porous Fe VO in tube furnace4Nanometer rods class Fenton photochemical catalyst.Porous Fe VO of the invention4Preparation method is simple for nano-bar material, at low cost, and synthesis condition is mild, is conducive to large-scale promotion.

Description

A kind of porous Fe VO4Nanometer rods class Fenton photochemical catalyst and its preparation method and application
Technical field
The present invention relates to catalysis material, porous Fe VO in ionic liquid is refered in particular to4The system of nanometer rods class Fenton photochemical catalyst Preparation Method and purposes belong to photocatalysis technology field in material and environmental improvement.
Background technique
Since 1970s Fujishima has found photocatalytic water phenomenon, Photocatalitic Technique of Semiconductor is as a kind of high Effect, environmental protection, energy-efficient emerging green technology, receive the concern of more and more energy and environmental area researcher.TiO2、 ZnO is the material of most study so far, but since their forbidden bandwidths are larger as traditional catalysis material on basis, There can only be response to UV light region, can not effectively utilize solar energy, and their quantum efficiency is unable to get significantly It is promoted, this strongly limits their industrial applications.To seek, spectral response range is wider and the higher light of quantum efficiency is urged Change material, exploitation novel visible response semiconductor catalysis material is essential.The design of novel photocatalysis material with Exploitation is unfolded based on typical (compound) metal oxide, a kind of possible reduction metal-oxide semiconductor (MOS) forbidden bandwidth Method be to pass through compound being modified to O 2p valence band with transition metal track (such as: Bi 6s, Ag 4d, V 3d etc.), it is real Now enhance the purpose of visible absorption.Therefore, people increasingly increase the research of metal composite oxide.
FeVO4It is wolframite type (ABO4) metal composite oxide, multi-functional compounds are used as, in luminescent material, gas The fields such as quick material, lithium electricity electrode material have a wide range of applications.In recent years, FeVO4As novel n-type semiconductor material Material, photocatalysis performance also start gradually to be seen in report.Three oblique type FeVO of Wang Min et al. research preparation4Nano particle is ultraviolet There is certain photocatalysis effect to methyl orange under light;Zhao Yi et al. has synthesized the orthorhombic phase FeVO of [010] crystal face exposure4Nanometer Piece, the material not only have the air-sensitive performance of micro ethanol gas in detection air, also under visible light there is excellent light to urge Change the ability of degradation methyl orange.Meanwhile FeVO4Middle Fe3+And V5+Simultaneously and cooperate with activation H2O2, form dual class Fenton's reaction body System, can greatly accelerate the process of catalyst degradation pollutant.Deng Jingheng et al. is with FeVO4As visible light class fenton catalyst, Visible light is introduced in the system, so that the yield of OH free radical obviously increases in system;Ozturk et al. has synthesized surface The modified FeVO of activating agent4Nano particle, research have found H2O2In the presence of, modified FeVO4Nano particle Pyrogentisinic Acid's Photocatalytic activity is significantly promoted.Therefore, by FeVO4In conjunction with H2O2Class Fenton photocatalytic system is constructed to be applied at sewage Reason has certain research significance.
Ionic liquid refers in room temperature or the nearly liquid being made of completely zwitterion at room temperature, is a kind of physical chemistry Good green solvent, catalyst and composite functional material of fine quality.The own ionic environment of ionic liquid can provide one for material Unique growing environment, existing research show that material property synthesized by ionic liquid auxiliary hydrothermal system is generally preferred over tradition Material synthesized by hydrothermal system.Currently, although publication number CN101284236A reports solid acid FexVyOzAs class Fenton The application of catalysts, but its synthetic method also compares shortcoming in material morphology control, is the inhomogenous nanometer of pattern Particle.And ionic liquid assists porous Fe VO in hydrothermal system4The preparation of nanometer rods class Fenton photochemical catalyst and performance study It has not been reported.Therefore the advantages of the present invention is based on ionic liquids, provides a kind of porous Fe VO4Nanometer rods class Fenton photocatalysis The preparation method of agent, the purpose is to the ionic environments being had by oneself using ionic liquid to provide a unique growing environment for material, To regulate and control its pattern and promote its photocatalysis performance.
Summary of the invention
The object of the present invention is to provide porous Fe VO in ionic liquid4The preparation method of nanometer rods class Fenton photochemical catalyst, The uniform porous Fe VO of pattern can be obtained by simple synthetic method by realizing4Photochemical catalyst solves existing FeVO4Light is urged Agent the problems such as pattern is not easy to control after firing.
The technical solution for realizing the aim of the invention is as follows: porous Fe VO in ionic liquid4Nanometer rods class Fenton photocatalysis The preparation method of agent, [Omim] FeCl for being 1:1 by molar ratio4And NH4VO4Two steps of hydro-thermal and calcining are assisted by ionic liquid Method is made;Ionic liquid [Omim] FeCl4It is by [Omim] Cl and FeCl3Oil bath reaction is made, reaction equation such as following formula I It is shown:
Concrete scheme is as follows:
A kind of porous Fe VO4Nanometer rods class Fenton photochemical catalyst, the porous Fe VO4Nanometer rods class Fenton photochemical catalyst is The monodimension nanometer material that length is 2~3 μm, width 100nm, aperture are about 20~50nm.
A kind of porous Fe VO4The preparation method of nanometer rods class Fenton photochemical catalyst, steps are as follows:
Step 1, by [Omim] FeCl4It is dissolved in distilled water and obtains solution A, by NH4VO4It is dissolved in hot water and obtains solution B, then will Solution A is added dropwise in B solution, after being added dropwise, is placed in stirring at normal temperature on magnetic stirring apparatus, obtains suspension;
Step 2, the suspension for obtaining step 1 are transferred in autoclave, and hydro-thermal reaction is carried out in baking oven, reaction After, it is washed with deionized water and dehydrated alcohol, obtains presoma FeVO after drying4·1.1H2O nano-bar material;
Step 3, by presoma FeVO4·1.1H2O nano-bar material is calcined in tube furnace to get to described porous FeVO4Nanometer rods class Fenton photochemical catalyst.
In step 1, in the solution A, [Omim] FeCl4Concentration be 0.1mol/L;In the solution B, NH4VO4It is dense Degree is 0.1mol/L;The volume ratio of the solution A and solution B is 1:1;The stirring at normal temperature time is 20~30 minutes.
In step 2, the temperature of the hydro-thermal reaction is 180 DEG C, and the hydro-thermal reaction time is 24 hours.
In step 3, the calcination temperature in the tube furnace is 500 DEG C, and calcination time is 4 hours.
The porous Fe VO4Nanometer rods class Fenton photochemical catalyst is used for rhodamine B degradation or tetracycline under excited by visible light.
The utility model has the advantages that
Compared with prior art, the present invention its remarkable advantage: assisting hydro-thermal and calcining two-step method that can obtain by ionic liquid The micropore FeVO uniform to pattern4Nano-bar material, photocatalytic activity can be by being added H2O2Form class Fenton light reaction system And it is greatly enhanced;Secondly porous Fe VO of the invention4Preparation method is simple for nano-bar material, at low cost, Synthesis condition is mild, is conducive to large-scale promotion.
Detailed description of the invention
Fig. 1 is porous Fe VO obtained by embodiment 14The XRD diagram of nano-rod photo-catalyst;
Fig. 2 is presoma FeVO obtained by embodiment 14·1.1H2The SEM of O nanometer rods schemes;
Fig. 3 is porous Fe VO obtained by embodiment 14The TEM of nano-rod photo-catalyst schemes;
In Fig. 4, figure a is porous Fe VO obtained by embodiment 14The DRS spectrogram of nano-rod photo-catalyst;It is real for scheming b Apply porous Fe VO obtained by example 14The forbidden bandwidth map of nano-rod photo-catalyst;
Fig. 5 is porous Fe VO obtained by embodiment 14Nano-rod photo-catalyst is under different visible light irradiation time to dense Degree is the rhodamine B Fenton photocatalytic degradation curve graph of 10mg/L;
Fig. 6 is porous Fe VO obtained by embodiment 14Nano-rod photo-catalyst is under different visible light irradiation time to dense Degree is the Tetracyclines Fenton photocatalytic degradation curve graph of 50mg/L.
Specific embodiment
In order to further illustrate the present invention, below with reference to example and attached drawing, the present invention will be described in detail:
Embodiment 1: porous Fe VO in ionic liquid of the invention4The preparation method of nanometer rods class Fenton photochemical catalyst, tool Body the following steps are included:
The first step, by 1mmol [Omim] FeCl4Ionic liquid is placed in 50mL beaker, is dissolved in distilled water (10mL) and being obtained Solution A, by 1mmol NH4VO4Solid particle is placed in 50mL beaker, is dissolved in hot water (10mL) obtaining solution B, then by solution A by Be added dropwise in B solution to obtain crocus suspension (suspension pH value is 2), place it in stirring at normal temperature 20 on magnetic stirring apparatus~ 30min;
The suspension that stirring terminates is transferred in autoclave by second step, and hydro-thermal reaction (baking oven is carried out in baking oven 180 DEG C of temperature, the time is about for 24 hours), then washed with deionized water and dehydrated alcohol, then move it to drying (baking oven temperature in baking oven 60 DEG C of degree, time about 8h), presoma FeVO can be obtained4·1.1H2O nanometer rods;
Third step, by presoma FeVO4·1.1H2O calcines that (tubular type furnace temperature is 500 DEG C, and the time is in tube furnace 4h) to get arrive the photochemical catalyst.
Embodiment 2: porous Fe VO of the invention4The application of nanometer rods class Fenton photocatalyst for degrading RhB, specifically include with Lower step: 100mL RhB solution (10mg/L) and 0.1g FeVO is added simultaneously into glass reaction bottle4, then to place it in light anti- Ying Yizhong is passed through air, reaches adsorption-desorption balance after magnetic agitation 30min under dark surrounds, then by 1mL H2O2It is added It in reaction system, and turns on light simultaneously (xenon lamp of 300W), is taken in 4mL solution and test tube every 20min, be centrifuged and take supernatant. It is measured at 553nm with ultraviolet specrophotometer (UV-2450), records data.
Embodiment 3: porous Fe VO of the invention4The application of nanometer rods class Fenton photocatalyst for degrading tetracycline, it is specific to wrap It includes following steps: into glass reaction bottle while 100mL tetracycline (50mg/L) and 0.05g FeVO is added4, then by its It is placed in light reaction instrument, is passed through air, reach adsorption-desorption balance after magnetic agitation 30min under dark surrounds, then by 4mL H2O2It is added in reaction system, and turns on light simultaneously (xenon lamp of 300W), taken in 4mL solution and test tube every 20min, be centrifuged and take Supernatant.It is measured at 356nm with ultraviolet specrophotometer (UV-2450), records data.
Fig. 1 is porous Fe VO prepared by the present invention4The X-ray diffracting spectrum of nanometer rods visible light catalyst, in figure FeVO4Diffraction maximum and its standard card it is completely corresponding, without any other miscellaneous phase exist, diffraction maximum is sharp, and crystallinity is preferable; Fig. 2 is presoma FeVO prepared by the present invention4·1.1H2The scanning electron microscope diagram of O nanometer rods, it can be seen that Gained presoma FeVO4·1.1H2O pattern is uniform and smooth surface monodimension nano stick, and length is about 2-3 μm, and width is about For 100nm;Fig. 3 is porous Fe VO prepared by the present invention4The transmission electron microscope figure of nanometer rods visible light catalyst, It can be seen that it is about 2-3 μm that resulting materials pattern, which is length, the nanometer rods that width is about 100nm, and be distributed in nanometer rods There is a large amount of hole.In Fig. 4, figure a is porous Fe VO prepared by the present invention4The uv drs of nanometer rods visible light catalyst Map, Cong Tuzhong it can be concluded that, absorption of the catalyst in Uv and visible light area is stronger, and light absorption band edge may extend to 560 nm;Scheming b is that above-mentioned uv drs spectrum data calculates conversion gained forbidden bandwidth map, can obtain the band gap width of the catalyst About 2.35eV;Fig. 5 is porous Fe VO prepared by the present invention4Nanometer rods visible light catalyst is under visible light conditions to sieve Red bright B (10mg/L) photocatalytic degradation curve graph, it can be seen from the figure that in H2O2In the presence of, such Fenton photochemical catalyst exists 90% is reached to the degradation rate of rhodamine B after radiation of visible light 120min.When no light, such Fenton catalyst system is to rhodamine The degradation rate of B is about 75%.And only H2O2In the presence of, the photocatalytic activity to rhodamine B is about 50%;Fig. 6 is this hair Bright prepared porous Fe VO4Nanometer rods visible light catalyst is under visible light conditions to tetracycline (50mg/L) class Fenton Photocatalytic degradation curve graph, it can be seen from the figure that the photochemical catalyst is after radiation of visible light 10min to the degradation rate of tetracycline Reach 75%, it will be seen that tetracycline degradation rate is 80% after light irradiation time extends to 100min.Only H2O2In the presence of, it is right The photocatalytic activity of tetracycline is about 23%.So under visible light illumination, porous Fe VO4Nanometer rods combination H2O2It is formed Class Fenton photocatalytic system have maximum catalytic degradation efficiency, there is ideal light to urge rhodamine B and tetracycline Change degradation effect.

Claims (4)

1. a kind of porous Fe VO4The preparation method of nanometer rods class Fenton photochemical catalyst, which is characterized in that steps are as follows:
Step 1, by [Omim] FeCl4It is dissolved in distilled water and obtains solution A, by NH4VO4It is dissolved in hot water obtaining solution B, then by solution A It is added dropwise in B solution, after being added dropwise, is placed in stirring at normal temperature on magnetic stirring apparatus, obtains suspension;
Step 2, the suspension for obtaining step 1 are transferred in autoclave, and hydro-thermal reaction, end of reaction are carried out in baking oven Afterwards, it is washed with deionized water and dehydrated alcohol, obtains presoma FeVO after drying4·1.1H2O nano-bar material;The hydro-thermal The temperature of reaction is 180 DEG C, and the hydro-thermal reaction time is 24 hours;
Step 3, by presoma FeVO4·1.1H2O nano-bar material is calcined to arrive the porous Fe VO in tube furnace4 Nanometer rods class Fenton photochemical catalyst, the calcination temperature in the tube furnace are 500 DEG C, and calcination time is 4 hours.
2. a kind of porous Fe VO according to claim 14The preparation method of nanometer rods class Fenton photochemical catalyst, feature exist In, in step 1, in the solution A, [Omim] FeCl4Concentration be 0.1mol/L;In the solution B, NH4VO4Concentration be 0.1mol/L;The volume ratio of the solution A and solution B is 1:1;The stirring at normal temperature time is 20~30 minutes.
3. porous Fe VO according to claim 14The catalyst of the preparation method preparation of nanometer rods class Fenton photochemical catalyst, It is characterized in that, the porous Fe VO4Nanometer rods class Fenton photochemical catalyst be length be 2~3 μm, width 100nm, aperture about For the monodimension nanometer material of 20~50nm, light absorption band edge of the nano material in Uv and visible light area extends to 560nm, Band gap width is 2.35eV.
4. porous Fe VO as claimed in claim 34The purposes of nanometer rods class Fenton photochemical catalyst, which is characterized in that described porous FeVO4Nanometer rods class Fenton photochemical catalyst is used for rhodamine B degradation or tetracycline under excited by visible light.
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CN111841606B (en) * 2020-07-23 2021-03-12 中国环境科学研究院 Heterogeneous FeVO4Catalytic material, preparation method and application thereof
CN111924928A (en) * 2020-08-05 2020-11-13 河北北方学院 FeVO4Method for preparing porous nano rod
CN114538523A (en) * 2022-02-17 2022-05-27 华南协同创新研究院 Iron vanadate material and preparation method and application thereof
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