CN112570024B - Ag/AgCl/IL/FeOOH/AC photocatalytic material and preparation and application thereof - Google Patents
Ag/AgCl/IL/FeOOH/AC photocatalytic material and preparation and application thereof Download PDFInfo
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- 229910002588 FeOOH Inorganic materials 0.000 title claims abstract description 64
- 229910021607 Silver chloride Inorganic materials 0.000 title claims abstract description 52
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 48
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910003153 β-FeOOH Inorganic materials 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006731 degradation reaction Methods 0.000 claims abstract description 12
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 11
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002608 ionic liquid Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000015556 catabolic process Effects 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 claims abstract description 5
- HFZWRUODUSTPEG-UHFFFAOYSA-N 2,4-dichlorophenol Chemical compound OC1=CC=C(Cl)C=C1Cl HFZWRUODUSTPEG-UHFFFAOYSA-N 0.000 claims description 19
- 230000000593 degrading effect Effects 0.000 claims description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 150000002989 phenols Chemical class 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 11
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- YRGNNOABGRMUKR-UHFFFAOYSA-N Cl(=O)(=O)O.C(CCC)N1CN(C=C1)C Chemical compound Cl(=O)(=O)O.C(CCC)N1CN(C=C1)C YRGNNOABGRMUKR-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- B01J35/39—
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0277—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature
- B01J31/0292—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature immobilised on a substrate
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- 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
Abstract
The invention provides Ag/AgCl/IL/FeOOH/ACThe preparation method of the photocatalytic material is characterized by comprising the following steps of: (1) the activated carbon AC and FeCl3 react in water with the pH value of 1.5-2.0 according to the mass ratio of 2 (4-5) to prepare beta-FeOOH/AC; (2) mixing the prepared beta-FeOOH/AC with a toluene solution of N-methylimidazole type ionic liquid according to the mass ratio of (2-3) to 1, heating for reaction, repeatedly washing with acetone after the reaction is finished, and drying to obtain IL/beta-FeOOH/AC; (3) the prepared IL/beta-FeOOH/AC and AgNO are mixed 3 Mixing with phase of AgNO 3 The concentration is 0.04-0.1mol/L, IL/beta-FeOOH/AC and AgNO 3 The mass ratio of the Ag/AgCl/IL/FeOOH/AC photocatalytic material is 2 (4-5), and the Ag/AgCl/IL/FeOOH/AC photocatalytic material is obtained by xenon lamp irradiation. Compared with the prior art, the method has the advantages of high degradation efficiency, stable catalyst, reusability and good environmental significance.
Description
Technical Field
The invention relates to the technical field of chemical environment, in particular to a novel Ag/AgCl/IL/FeOOH/AC photocatalytic material and preparation and application thereof.
Technical Field
The phenolic waste water which is difficult to degrade and harmful and is ubiquitous in environmental water is a very common aromatic compound, and the traditional processes for treating the phenolic compound water comprise an adsorption method, a biological method and a chemical oxidation method. These methods often cannot degrade oxidation and even completely mineralize in a short time, and have the disadvantages of high energy consumption, easy generation of secondary pollution and the like. The photocatalytic technology has become a reliable choice for people to degrade pollutants in sewage due to its advantages of high efficiency, easy operation, relatively low cost, no toxic and harmful intermediate products in the degradation process, no harmful residues after the degradation is completed, and the like.
The currently researched photocatalysts are numerous, wherein titanium dioxide is the most widely researched photocatalytic material due to the advantages of high efficiency, stable chemical properties, low cost, no toxicity and the like, but the titanium dioxide photocatalytic technology still has many defects in the practical application process. Firstly, the light absorption wavelength range of the semiconductor is narrow, mainly in the ultraviolet region, and the ultraviolet light only accounts for 4% of the solar spectrum, so the utilization rate of solar energy is low, which greatly limits the practical application of the catalyst. Secondly, the titanium dioxide has low catalytic efficiency, and the recombination rate of electrons and holes generated by excitation is high, so that the quantum efficiency is low.
The iron hydroxide is an important compound commonly seen on the surface, has a large specific surface area, is a photocatalytic material capable of corresponding visible light, and still has a certain catalytic effect even under the condition of no light. The noble metal is deposited on the surface of the catalyst in a proper amount, which is beneficial to the effective separation of photo-generated electrons and holes, thereby greatly improving the activity of the catalyst. When the semiconductor and the metal are contacted with each other, current carriers are redistributed, electrons are transferred from the n-type semiconductor with higher Fermi level to the metal with lower Fermi level until the Fermi levels of the n-type semiconductor and the metal are the same, a Schottky barrier (Schottky barrier) is generated, the Schottky barrier becomes an effective potential well for capturing photo-generated electrons, the photo-generated electrons and holes are inhibited from being compounded, and finally the photocatalytic activity is improved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention is especially provided for overcoming the defects of high energy consumption, serious environmental pollution, easy agglomeration of a catalyst to influence the reaction performance and the like in the traditional method for degrading the phenolic compounds, especially the 2, 4-dichlorophenol.
The invention aims to provide a preparation method of a novel photocatalytic material Ag/AgCl/IL/FeOOH/AC, and specifically, the preparation method of the Ag/AgCl/IL/FeOOH/AC photocatalytic material comprises the following steps:
(1) activated carbon AC and FeCl 3 Reacting in water with pH value of 1.5-2.0 according to the mass ratio of 2 (4-5) to prepare beta-FeOOH/AC;
(2) mixing the prepared beta-FeOOH/AC with a toluene solution of N-methylimidazole type ionic liquid according to the mass ratio of (2-3) to 1, heating for reaction, repeatedly washing with acetone after the reaction is finished, and drying to obtain IL/beta-FeOOH/AC;
(3) the prepared IL/beta-FeOOH/AC and AgNO are mixed 3 Mixing with phase of AgNO 3 The concentration is 0.04-0.1mol/L, IL/beta-FeOOH/AC and AgNO 3 The mass ratio of the Ag/AgCl/IL/FeOOH/AC photocatalytic material is 2 (4-5), and the Ag/AgCl/IL/FeOOH/AC photocatalytic material is obtained by xenon lamp irradiation.
Preferably, the reaction temperature in the step (1) is 65-75 ℃, and the reaction time is 10-12 h.
Preferably, the N-methylimidazole type ionic liquid in the step (2) is 1-butyl-3-methylimidazole chlorate (BmimCl).
Preferably, the reaction temperature in the step (2) is 70-80 ℃, and the reaction time is 8-10 h.
Preferably, the xenon lamp irradiation time in the step (3) is 5-6 h.
Another objective of the invention is to provide an Ag/AgCl/IL/FeOOH/AC photocatalytic material prepared by the method.
The invention also aims to provide an application of the Ag/AgCl/IL/FeOOH/AC photocatalytic material in degrading phenolic compounds. Preferably, the application in degrading 2, 4-dichlorophenol is realized, and a specific degradation method comprises the following steps:
mixing the prepared Ag/AgCl/IL/FeOOH/AC photocatalytic material in 2,4 dichlorophenol with the initial concentration of 100mg/L, and carrying out visible light photocatalytic degradation reaction at room temperature, wherein the dosage of the Ag/AgCl/IL/FeOOH/AC photocatalytic material is 1-1.5 g/L.
More preferably, the degradation reaction time is 4 to 8 hours. When the reaction is carried out for 4 hours, the degradation rate can reach more than 80 percent, and then the degradation rate tends to be flat. More preferably, in the degradation of 2,4 dichlorophenol, the Ag/AgCl/IL/FeOOH/AC photocatalytic material can be recycled after being washed and dried, and has better stability.
The invention has the beneficial effects that:
the invention provides a novel Ag/AgCl/IL/FeOOH/AC photocatalytic material, and further provides a method for degrading 2, 4-dichlorophenol by using the novel Ag/AgCl/IL/FeOOH/AC photocatalytic material. The method overcomes the defects of high energy consumption, difficult operation and the like in the prior art for treating the 2, 4-dichlorophenol by water, also overcomes the defects of low photocatalytic efficiency and the like of the traditional catalyst, and has simple catalyst recovery process and good reusability.
Drawings
FIG. 1 is an XRD pattern of Ag/AgCl/IL/FeOOH/AC, and FeOOH/AC.
FIG. 2 is an XPS plot of Ag/AgCl/IL/FeOOH/AC.
FIG. 3 is a graph showing the effect of photocatalytic degradation of 2, 4-dichlorophenol by Ag/AgCl/IL/FeOOH/AC, IL/FeOOH/AC and FeOOH/AC under dark conditions.
FIG. 4 is a graph showing the effect of Ag/AgCl/IL/FeOOH/AC, and FeOOH/AC in photocatalytic degradation of 2, 4-dichlorophenol under xenon lamp irradiation.
FIG. 5 is a diagram showing the effect of repeated experiments of photocatalytic degradation of 2, 4-dichlorophenol by Ag/AgCl/IL/FeOOH/AC under xenon lamp irradiation.
Detailed description of the preferred embodiment
The present invention will be further explained with reference to specific embodiments and drawings, but it should be understood that the scope of the present invention is not limited thereto. In this embodiment, the equipment used in the examples of the present invention is selected from commercially available conventional chemical synthesis experimental equipment.
Example 1: preparation of Ag/AgCl/IL/FeOOH/AC photocatalytic material
(1) Activated carbon AC and FeCl 3 Reacting in water with pH value of 1.5-2.0 at a mass ratio of 2-5 at 65 ℃ for 11h to obtain beta-FeOOH/AC;
(2) mixing the prepared beta-FeOOH/AC with a toluene solution of ionic liquid BmimCl according to the mass ratio of 2:1, heating to react at the temperature of 80 ℃ for 10 hours, repeatedly washing with acetone after the reaction is finished, and drying to finally obtain IL/beta-FeOOH/AC;
(3) the prepared IL/beta-FeOOH/AC and AgNO are mixed 3 Mixing with phase of AgNO 3 The concentration is 0.08mol/L, IL/beta-FeOOH/AC and AgNO 3 The mass ratio of the Ag/AgCl/IL/FeOOH/AC photocatalytic material is 2:4, and the Ag/AgCl/IL/FeOOH/AC photocatalytic material is obtained after xenon lamp irradiation for 5 hours.
Example 2: preparation of Ag/AgCl/IL/FeOOH/AC photocatalytic material
(1) Activated carbon AC and FeCl 3 Reacting in water with pH value of 1.5-2.0 at the mass ratio of 4-5 at 70 ℃ for 10h to prepare beta-FeOOH/AC;
(2) mixing the prepared beta-FeOOH/AC with a toluene solution of ionic liquid BmimCl according to the mass ratio of 2:1, heating to react at 70 ℃ for 9 hours, repeatedly washing with acetone after the reaction is finished, and drying to finally obtain IL/beta-FeOOH/AC;
(3) the prepared IL/beta-FeOOH/AC and AgNO are mixed 3 Mixing with phase of AgNO 3 The concentration is 0.1mol/L, IL/beta-FeOOH/AC and AgNO 3 The mass ratio of the Ag/AgCl/IL/FeOOH/AC photocatalytic material is 2:4, and the Ag/AgCl/IL/FeOOH/AC photocatalytic material is obtained after xenon lamp irradiation for 5 hours.
Example 3: preparation of Ag/AgCl/IL/FeOOH/AC photocatalytic material
(1) Activated carbon AC and FeCl 3 Reacting in water with pH value of 1.5-2.0 at the mass ratio of 3-5 at 75 ℃ for 12h to obtain beta-FeOOH/AC;
(2) mixing the prepared beta-FeOOH/AC with a toluene solution of ionic liquid BmimCl according to the mass ratio of 3:1, heating to react at the temperature of 75 ℃ for 8h, repeatedly washing with acetone after the reaction is finished, and drying to finally obtain IL/beta-FeOOH/AC;
(3) the prepared IL/beta-FeOOH/AC and AgNO are mixed 3 Mixing with phase of AgNO 3 The concentration is 0.06mol/L, IL/beta-FeOOH/AC and AgNO 3 The mass ratio of the Ag/AgCl/IL/FeOOH/AC photocatalytic material is 2:5, and the Ag/AgCl/IL/FeOOH/AC photocatalytic material is obtained after xenon lamp irradiation for 5 hours.
Example 4:
the Ag/AgCl/IL/FeOOH/AC photocatalytic material prepared in example 1 was characterized:
1) structural characterization of Ag/AgCl/IL/FeOOH/AC
As can be seen from FIG. 1, the XRD patterns of the two photocatalytic materials of the loaded activated carbon FeOOH/AC and the loaded ionic liquid IL/FeOOH/AC are basically consistent. An XRD pattern of the Ag/AgCl/IL/FeOOH/AC photocatalytic material shows that an absorption peak of 44.24 corresponds to simple substance silver at 2 theta of 38.52, the silver simple substance is successfully loaded, an absorption peak appears at 2 theta of 23.74, the absorption peak is consistent with beta-FeOOH, a diffraction peak is sharp and clear, the crystallinity is better, and the prepared material is Ag/AgCl/IL/FeOOH/AC.
2) Valence state representation of Ag/AgCl/IL/FeOOH/AC
The presence of Cl, Ag, O, Fe elements in the sample can be seen in FIG. 2.
2-b, it can be known that there are two valence states of Ag in the photocatalytic material, and two peaks exist when Ag is located at 374.12 and 368.36, which correspond to the simple substance of silver and the metallic silver ion, respectively, and the existence of the simple substance of Ag and AgCl in the sample is also actually verified.
The XPS spectrum analysis of Fe 2p (FIG. 2-c) and O1s (FIG. 2-d) shows that Fe 2p2/3 has a peak with binding energy of 711.7eV, which is close to 711.8eV of FeOOH, and thus Fe element exists in the form of FeOOH. After O1s peak separation, a peak appears with a binding energy of: 531.93eV and 531.93eV are close to the binding energy 532.42eV of adsorbed oxygen, which shows that the existence of-OOH ions, 530.53eV is closer to the binding energy 530.0eV of lattice oxygen, and the structure of FeOOH is satisfied.
Example 5:
the Ag/AgCl/IL/FeOOH/AC, IL/FeOOH/AC and FeOOH/AC prepared in example 1 are respectively mixed in 2,4 dichlorophenol with the initial concentration of 100mg/L, and the catalytic degradation reaction is carried out under the condition of room temperature and light shielding, wherein the dosage of the Ag/AgCl/IL/FeOOH/AC, the IL/FeOOH/AC and the FeOOH/AC are all 1g/L, the reaction condition is that the materials are adsorbed for 0-8h under the condition of light shielding (the reaction result is shown in figure 3), the adsorption effect of the materials is researched, the measurement and calculation are carried out, and the method for degrading and removing the rate according to the absorbance in all degradation experiments is as follows:
η＝(A 0 -A)/A 0 *100％
in the formula, A 0 Is the initial absorbance of the 2,4 dichlorophenol solution; a is the absorbance of the 2,4 dichlorophenol solution under different illumination time.
Example 6:
the initial concentration of 2,4 dichlorophenol and the amount of the photocatalyst are the same as those in example 5, except that xenon lamp is added for irradiation for 0-8h (the reaction result is shown in FIG. 4), and the comparison result in FIG. 4 shows that the Ag/AgCl/IL/FeOOH/AC photocatalytic material has better effect on removing 2,4 dichlorophenol than Ag/AgCl/FeOOH/AC and FeOOH/AC under the condition of visible light. The removal rate was calculated in the same manner as in example 5.
The experimental results of example 5 and example 6 show that under the condition of visible light, the organic matter 2,4 dichlorophenol is further catalyzed and degraded. Due to the introduction of visible light, energy level transitions between conduction bands and valence bands of the three composite photocatalysts are excited, and organic matters are thoroughly degradedIs a small molecule inorganic substance such as CO 2 ，H 2 O and HCl; and the light-shielding experiment only carries out adsorption and certain Fenton-like catalysis on organic matters through the pore structure on the surface of the material.
Example 7:
the initial concentration of 2,4 dichlorophenol, the amount of the Ag/AgCl/IL/FeOOH/AC photocatalytic material and the reaction conditions were the same as those of example 6, and the Ag/AgCl/IL/FeOOH/AC photocatalytic material was reused 4 times, and the results are shown in FIG. 5, which indicates that the catalyst still has a photocatalytic degradation effect of 80% or more for 2,4 dichlorophenol after five times of use.
The AgCl can be decomposed into Ag simple substances under illumination, and the metal Ag transfers energy from the metal to the semiconductor through plasma resonance to excite an electron-hole pair of the semiconductor material; the ionic liquid can form reverse micelles on the surface of the catalyst, capture photoproduction electrons, inhibit the recombination of hole-electron pairs, and simultaneously enable Ag particles to be better diffused on the surface of the catalyst so as to improve the activity of the photocatalytic reaction of the catalyst.
Although the present invention has been described in detail, modifications within the spirit and scope of the invention will be apparent to those skilled in the art. Further, it should be understood that the various aspects recited herein, portions of different embodiments, and various features recited may be combined or interchanged either in whole or in part. In the various embodiments described above, those embodiments that refer to another embodiment may be combined with other embodiments as appropriate, as will be appreciated by those skilled in the art. Furthermore, those skilled in the art will appreciate that the foregoing description is by way of example only, and is not intended to limit the invention.
Claims (10)
1. A preparation method of Ag/AgCl/IL/FeOOH/AC photocatalytic material is characterized by comprising the following steps:
(1) activated carbon AC and FeCl 3 Reacting in water with pH value of 1.5-2.0 according to the mass ratio of 2 (4-5) to prepare beta-FeOOH/AC;
(2) mixing the prepared beta-FeOOH/AC with a toluene solution of N-methylimidazole type ionic liquid according to the mass ratio of (2-3) to 1, heating for reaction, repeatedly washing with acetone after the reaction is finished, and drying to obtain IL/beta-FeOOH/AC; the N-methylimidazole type ionic liquid is BmimCl;
(3) the prepared IL/beta-FeOOH/AC and AgNO are mixed 3 Mixing with phase of AgNO 3 The concentration is 0.04-0.1mol/L, IL/beta-FeOOH/AC and AgNO 3 The mass ratio of the Ag/AgCl/IL/FeOOH/AC photocatalytic material is 2 (4-5), and the Ag/AgCl/IL/FeOOH/AC photocatalytic material is obtained by xenon lamp irradiation.
2. The method according to claim 1, wherein the reaction temperature in the step (1) is 65 to 75 ℃ and the reaction time is 10 to 12 hours.
3. The method according to claim 1, wherein the reaction temperature in the step (2) is 70 to 80 ℃ and the reaction time is 8 to 10 hours.
4. The production method according to any one of claims 1 to 3, wherein the xenon lamp irradiation time period in the step (3) is 5 to 6 hours.
5. Ag/AgCl/IL/FeOOH/AC photocatalytic material prepared by the preparation method according to any one of claims 1 to 4.
6. The use of the Ag/AgCl/IL/FeOOH/AC photocatalytic material of claim 5 in degrading phenolic compounds.
7. Use according to claim 6 for the degradation of 2,4 dichlorophenol.
8. Use according to claim 7, characterized in that it comprises the following steps: and mixing the prepared Ag/AgCl/IL/FeOOH/AC photocatalytic material in 2,4 dichlorophenol with the initial concentration of 100mg/L, and carrying out visible light photocatalytic degradation reaction at room temperature, wherein the dosage of the Ag/AgCl/IL/FeOOH/AC photocatalytic material is 1-1.5 g/L.
9. Use according to claim 8, wherein the degradation reaction time is 4-8 h.
10. The use of claim 6, wherein the Ag/AgCl/IL/FeOOH/AC photocatalytic material is recycled after the reaction is completed, washed, and dried.
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