CN115364848B - Stripe-shaped composite photocatalyst In-MoO 3 Is prepared by the preparation method of (2) - Google Patents
Stripe-shaped composite photocatalyst In-MoO 3 Is prepared by the preparation method of (2) Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 35
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000243 solution Substances 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 229910021617 Indium monochloride Inorganic materials 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 abstract description 10
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 9
- 229940043267 rhodamine b Drugs 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 229910052724 xenon Inorganic materials 0.000 abstract description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- 229910017299 Mo—O Inorganic materials 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010041 electrostatic spinning Methods 0.000 description 2
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
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- 239000002135 nanosheet Substances 0.000 description 2
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- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical group [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
Stripe-shaped composite photocatalyst In-MoO 3 Which belongs to the field of inorganic catalytic materials. The invention prepares the composite photocatalyst In-MoO by a simple one-step hydrothermal method 3 . The method has the advantages of simple preparation process, less equipment and low production cost. Prepared In-MoO 3 The photocatalytic activity is high, and under the irradiation of a simulated sunlight xenon lamp (300W), 0.03g of the prepared composite photocatalyst degrades 100mL of rhodamine B solution with the concentration of 10mg/L, and the degradation rate reaches 96.2% within 70 min. After the composite photocatalyst is recycled for four times and reused, the degradation rate of the composite photocatalyst to rhodamine B solution still reaches 91.8% under the same degradation condition, and the product prepared by the method can be widely applied to the field of photocatalytic degradation of organic pollutants.
Description
Technical Field
The invention relates to a strip-shaped composite photocatalyst In-MoO 3 Belongs to the technical field of inorganic catalytic materials.
Background
The semiconductor photocatalysis technology is favored by researchers as an efficient advanced oxidation technology due to the characteristics of mild reaction conditions, high degradation rate, relatively non-toxic products and the like. It was found that the transition metal oxide molybdenum trioxide (MoO 3 ) Has the advantages of high activity, good chemical stability, low cost and the like, and is widely applied to the field of photocatalytic degradation of wastewater. MoO (MoO) 3 There are four crystalline forms, including: orthorhombic alpha-MoO 3 Monoclinic phase beta-MoO 3 Hexagonal phase h-MoO 3 And high pressure monoclinic phase MoO 3 -ii. Wherein, alpha-MoO 3 Is a thermodynamically stable phase of molybdenum trioxide, and the main preparation methods include a hydrothermal method, a sol-gel method, a roasting method, a coprecipitation method and the like. MoO, however 3 The forbidden bandwidth of (2.9-3.5 eV) is larger, and the application and development of the catalyst in the field of photocatalysis are restricted. Doping can alter the electron and energy band structure of the photocatalyst, thereby enhancing light absorption. As a group iiia metal element, indium (In) is rich In oxidation state and d orbitals are empty, which makes it have considerable electron generation, capturing and migration ability. At present, in is widely used as a doping agent In the research of catalysts for photocatalytic degradation of dye wastewater such as Methylene Blue (MB), methyl Orange (MO) and rhodamine B (RhB), which is designed to dope MoO with In 3 The photocatalyst provides possibility for constructing a high-efficiency photodegradation RhB wastewater system.
Currently, for MoO 3 The modified research results are more. For example, "molecular science journal", month 10 of 2016, volume 32, 5 "W (V) doped MoO 3 Electrostatic spinning preparation and photocatalytic activity of micro-nano sheet, and preparation of W (V) -doped PVP/(NH) by combining electrostatic spinning technology with sol process 4 ) 6 Mo 7 O 24 ·4H 2 The precursor O is roasted by slowly controlling the temperature to obtain MoO with good crystallinity at 600 DEG C 3 Mo and Mo 0.97 W(V) 0.03 O 3－δ Micro-nano sheets. The method has the following defects: (1) The preparation process of the composite photocatalyst is complex, relates to sol preparation, self-made spinning machine preparation and high-temperature roasting treatment processes, and is not suitable for popularization and application; (2) The precursor sol is prepared by adding organic solvents such as absolute ethyl alcohol and PVP, which can increase the preparation cost and is difficult to popularize and use on a large scale. For another example, chinese patent invention discloses a method for preparing nano ribbon MOA composite photocatalyst, moO prepared by microwave hydrothermal method 3 Surface deposition of AgBr to obtain heterostructureMOA(MoO 3 /AgBr). The method has the following problems: (1) The preparation process of the compound involves the surfactants polyvinylpyrrolidone (PVP) and silver nitrate, so that the cost is high and the compound is not suitable for popularization; (2) MoO (MoO) 3 The preparation conditions of the photocatalyst are harsh, the pH and the temperature need to be strictly controlled, and the photocatalyst is not suitable for large-scale industrial application.
Disclosure of Invention
The invention is directed to MoO 3 The catalytic activity of the catalyst is not high, and an In-MoO is prepared 3 The composite photocatalyst improves the defects of a single semiconductor material in structure and performance, is beneficial to improving the catalytic activity of the composite photocatalyst and expanding MoO 3 The application of the base photocatalyst. The preparation process is simple, the used equipment is few, the cost is low, and the activity of the composite photocatalyst is high. In-MoO of the invention 3 The preparation method of the composite photocatalyst comprises the following steps:
1.5g of (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, according to the mass percentage of theoretical generated In the compound, is 3 to 20 weight percent, and the InCl is weighed 3 ·H 2 O, performing ultrasonic dissolution by 39mL of deionized water to form a mixed solution A; slowly adding the prepared 21mL of dilute nitric acid solution with the concentration of 3mol/L into the mixed solution A, and continuing to mechanically stir for 10min to obtain a uniform and transparent pale yellow precursor solution B; placing the solution B In a 100mL high-pressure reaction kettle, sealing, reacting at 180 ℃ for 20 hours, naturally cooling to room temperature, filtering, respectively carrying out suction filtration and rinsing on a filter cake with deionized water and absolute ethyl alcohol for 3 times, placing In an 80 ℃ oven for drying for 12 hours, and grinding to obtain white powdery In-MoO 3 。
The invention adopts the technical scheme and mainly has the following effects:
(1) In-MoO prepared by the method of the invention 3 The composite photocatalyst has higher photocatalytic activity. Under the irradiation of a xenon lamp simulating sunlight, 0.03g of the prepared optimal photocatalyst is dispersed in 100mL of rhodamine B solution with the concentration of 10mg/L, and the degradation rate reaches 96.2% after 70min of illumination.
(2) The invention adopts a one-step hydrothermal method for preparation, has simple preparation process, less required equipment and low cost.
(3) In-MoO prepared by the method of the invention 3 The degradation rate of the rhodamine B solution after four times of repeated use still reaches 91.8 percent after the composite photocatalyst is recovered.
Drawings
FIG. 1 is MoO 3 And In-MoO 3 Is an X-ray diffraction pattern of (2).
FIG. 2 is MoO 3 And In-MoO 3 FT-IR diagram of (c).
FIG. 3 is MoO 3 And In-MoO 3 HRTEM images of (a).
FIG. 4 is MoO 3 And In-MoO 3 Is a XPS graph of (C).
FIG. 5 is MoO 3 And In-MoO of different mass ratios 3 Degradation rate of (3).
Detailed Description
The invention will be further described with reference to the following specific embodiments.
Example 1
Stripe-shaped composite photocatalyst In-MoO 3 The preparation method comprises the following specific steps:
1.5g of (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, according to the mass percentage of theoretical generated In the compound being 3wt%, weighing InCl 3 ·H 2 O, performing ultrasonic dissolution by 39mL of deionized water to form a mixed solution A; slowly adding the prepared 21mL of dilute nitric acid solution with the concentration of 3mol/L into the mixed solution A, and continuing to mechanically stir for 10min to obtain a uniform and transparent pale yellow precursor solution B; placing the solution B In a 100mL high-pressure reaction kettle, sealing, reacting at 180 ℃ for 20 hours, naturally cooling to room temperature, filtering, respectively carrying out suction filtration and rinsing on a filter cake with deionized water and absolute ethyl alcohol for 3 times, placing In an 80 ℃ oven for drying for 12 hours, and grinding to obtain white powdery In-MoO 3 (3-IM)。
Example 2
Stripe-shaped composite photocatalyst In-MoO 3 The preparation method comprises the following specific steps:
1.5g of (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, according toThe mass percentage of the theoretically generated In the compound is 5wt percent, and the InCl is weighed 3 ·H 2 O, performing ultrasonic dissolution by 39mL of deionized water to form a mixed solution A; slowly adding the prepared 21mL of dilute nitric acid solution with the concentration of 3mol/L into the mixed solution A, and continuing to mechanically stir for 10min to obtain a uniform and transparent pale yellow precursor solution B; placing the solution B In a 100mL high-pressure reaction kettle, sealing, reacting at 180 ℃ for 20 hours, naturally cooling to room temperature, filtering, respectively carrying out suction filtration and rinsing on a filter cake with deionized water and absolute ethyl alcohol for 3 times, placing In an 80 ℃ oven for drying for 12 hours, and grinding to obtain white powdery In-MoO 3 (5-IM)。
Example 3
Stripe-shaped composite photocatalyst In-MoO 3 The preparation method comprises the following specific steps:
1.5g of (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, according to the mass percentage of theoretical generated In the compound being 10wt%, weighing InCl 3 ·H 2 O, performing ultrasonic dissolution by 39mL of deionized water to form a mixed solution A; slowly adding the prepared 21mL of dilute nitric acid solution with the concentration of 3mol/L into the mixed solution A, and continuing to mechanically stir for 10min to obtain a uniform and transparent pale yellow precursor solution B; placing the solution B In a 100mL high-pressure reaction kettle, sealing, reacting at 180 ℃ for 20 hours, naturally cooling to room temperature, filtering, respectively carrying out suction filtration and rinsing on a filter cake with deionized water and absolute ethyl alcohol for 3 times, placing In an 80 ℃ oven for drying for 12 hours, and grinding to obtain white powdery In-MoO 3 (10-IM)。
Example 4
Stripe-shaped composite photocatalyst In-MoO 3 The preparation method comprises the following specific steps:
1.5g of (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, according to the mass percentage of theoretical generated In the compound being 15wt%, weighing InCl 3 ·H 2 O, performing ultrasonic dissolution by 39mL of deionized water to form a mixed solution A; slowly adding the prepared 21mL of dilute nitric acid solution with the concentration of 3mol/L into the mixed solution A, and continuously mechanically stirring for 10min to obtain a uniform and transparent pale yellow precursorA bulk solution B; placing the solution B In a 100mL high-pressure reaction kettle, sealing, reacting at 180 ℃ for 20 hours, naturally cooling to room temperature, filtering, respectively carrying out suction filtration and rinsing on a filter cake with deionized water and absolute ethyl alcohol for 3 times, placing In an 80 ℃ oven for drying for 12 hours, and grinding to obtain white powdery In-MoO 3 (15-IM)。
Example 5
Stripe-shaped composite photocatalyst In-MoO 3 The preparation method comprises the following specific steps:
1.5g of (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, according to the mass percentage of theoretical generated In the compound being 20wt%, weighing InCl 3 ·H 2 O, performing ultrasonic dissolution by 39mL of deionized water to form a mixed solution A; slowly adding the prepared 21mL of dilute nitric acid solution with the concentration of 3mol/L into the mixed solution A, and continuing to mechanically stir for 10min to obtain a uniform and transparent pale yellow precursor solution B; placing the solution B In a 100mL high-pressure reaction kettle, sealing, reacting at 180 ℃ for 20 hours, naturally cooling to room temperature, filtering, respectively carrying out suction filtration and rinsing on a filter cake with deionized water and absolute ethyl alcohol for 3 times, placing In an 80 ℃ oven for drying for 12 hours, and grinding to obtain white powdery In-MoO 3 (20-IM)。
Experimental results
The composite photocatalyst In-MoO prepared In example 2 3 The catalytic degradation activity is optimal. For convenience of comparison, moO was prepared 3 And (3) a sample. MoO (MoO) 3 The preparation method is that in the step of the example 2, inCl is not added 3 ·H 2 O。
MoO 3 As shown in FIG. 1 (a), the diffraction peak position is consistent with JCPDS card No.05-0508, the crystal face indexes are (020), (110), (040), (021), (060), (200), (210) and (0100), and no impurity peak appears, indicating that the sample is orthorhombic phase alpha-MoO 3 。MoO 3 The infrared absorption spectrum of (a) is shown in FIG. 2 (a), 996.97cm -1 、876.95cm -1 And 552.77cm -1 The peaks at these points are respectively attributed to the tensile modes of mo=o double bond vibration, mo-O-Mo single bond vibration, and tri-coordinated oxygen (O-3 Mo), confirming the presence of MoO in the sample 3 Is a complete crystal form of (c).
XRD diffraction of the composite photocatalyst is shown In FIGS. 1 (b) - (f), in-MoO 3 The presence of MoO in the sample 3 The characteristic diffraction peak of (2) is sharp and no impurity peak appears, which indicates that the two phases in the composite sample can be well combined and stably coexist. In-MoO 3 No In was detected In the photocatalyst 2 O 3 And contain In 3+ The characteristic diffraction peak of the material is mainly derived from the fact that the doping mass proportion of In is smaller and In 3+ Ion by partial substitution of Mo 6+ Ion entry MoO 3 Is defined in the crystal lattice of (a). It was observed that the diffraction peaks slightly shifted to a small angle as the doping mass ratio increased. This is because of the ionic radius of In
Ion radius greater than Mo->
Thereby causing lattice expansion, resulting in interplanar spacing. The infrared absorption spectrum of 5-IM is shown in FIG. 2 (b), and the vibration peak-to-peak value of the single bond of Mo-O-Mo of the sample (885.66 cm) -1 ) Compared with MoO 3 Single sample (876.95 cm) -1 ) The infrared transmittance is slightly increased due to the offset. This suggests that the Mo-O bond lengths on both sides of the Mo-O-Mo bond are affected by ion doping and cause In-MoO 3 The change of the bond energy of the Mo-O bond indicates that the prepared In-MoO 3 Sample structure is stable, in 3+ Ion by partial substitution of Mo 6+ Ion entry MoO 3 Lattice, again explaining In-MoO 3 Successful synthesis of photocatalysts.
TEM and HRTEM of 5-IM are shown in FIG. 3. TEM images confirm In-MoO 3 In-MoO was detected In HRTEM image of nanoribbon structure of sample 3 The lattice spacing of the photocatalyst is 0.397nm, which is equal to MoO 3 Corresponds to the (110) crystal plane of (c). Whereas the standard spacing of the (110) crystal plane is 0.381nm, the increased lattice spacing can be interpreted as In 3+ Entering MoO 3 Inside the lattice, the lattice is expanded.
MoO 3 And 5-IM X-ray photoelectron spectroscopy (XPS) as shown In FIG. 4, the sample of FIG. 4 (a) contains Mo,O and In elements; in FIG. 4 (b), in 3d is In 3d 5/2 And In 3d 3/2 The split peaks of (a) are concentrated at 444.9eV and 452.6eV, which shows that In element is In 3+ Exists. From the viewpoint of elemental composition, description of In-MoO 3 Successful preparation of the photocatalyst.
The photocatalysis experiment result is shown in figure 5, under the irradiation of 300W Xe lamp simulated sunlight, 0.03g of prepared composite photocatalyst 5-IM has the best activity when degrading 100mL of rhodamine B solution with the concentration of 10mg/L, and the degradation rate of 70min reaches 96.2%; the degradation rate of the recycled 5-IM to rhodamine B still reaches 91.8 percent when the recycled 5-IM is used for the fourth time.
Claims (1)
1. Stripe-shaped composite photocatalyst In-MoO 3 The preparation method of (2) comprises the following steps:
1.5g of (NH) 4 ) 6 Mo 7 O 24 ·4H 2 O, according to the mass percentage of theoretical generated In the compound, is 3 to 20 weight percent, and the InCl is weighed 3 ·H 2 O, performing ultrasonic dissolution by 39mL of deionized water to form a mixed solution A; slowly adding the prepared 21mL of dilute nitric acid solution with the concentration of 3mol/L into the mixed solution A, and continuing to mechanically stir for 10min to obtain a uniform and transparent pale yellow precursor solution B; placing the solution B In a 100mL high-pressure reaction kettle, sealing, reacting at 180 ℃ for 20 hours, naturally cooling to room temperature, filtering, respectively carrying out suction filtration and rinsing on a filter cake with deionized water and absolute ethyl alcohol for 3 times, placing In an 80 ℃ oven for drying for 12 hours, and grinding to obtain white powdery In-MoO 3 。
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