CN110605138A - Preparation method and application of tantalum oxygen nitrogen/foamed nickel photocatalytic contact oxide film - Google Patents
Preparation method and application of tantalum oxygen nitrogen/foamed nickel photocatalytic contact oxide film Download PDFInfo
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- CN110605138A CN110605138A CN201910952244.2A CN201910952244A CN110605138A CN 110605138 A CN110605138 A CN 110605138A CN 201910952244 A CN201910952244 A CN 201910952244A CN 110605138 A CN110605138 A CN 110605138A
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- taon
- oxide film
- foamed nickel
- nickel
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 193
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 96
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 44
- NRYVNQQMPSBVQK-UHFFFAOYSA-N [N].[O].[Ta] Chemical compound [N].[O].[Ta] NRYVNQQMPSBVQK-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000006260 foam Substances 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 42
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 28
- AXDJCCTWPBKUKL-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-imino-3-methylcyclohexa-2,5-dien-1-ylidene)methyl]aniline;hydron;chloride Chemical compound Cl.C1=CC(=N)C(C)=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 AXDJCCTWPBKUKL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 16
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 14
- 239000011630 iodine Substances 0.000 claims abstract description 14
- 230000009471 action Effects 0.000 claims abstract description 12
- 238000005121 nitriding Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 230000000593 degrading effect Effects 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 7
- 230000015556 catabolic process Effects 0.000 claims description 6
- 238000006731 degradation reaction Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000002835 absorbance Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims 2
- 239000000725 suspension Substances 0.000 claims 2
- 230000008021 deposition Effects 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910003071 TaON Inorganic materials 0.000 abstract description 60
- 238000001035 drying Methods 0.000 abstract description 20
- 229910052715 tantalum Inorganic materials 0.000 abstract description 13
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 10
- 239000003344 environmental pollutant Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 238000005286 illumination Methods 0.000 abstract description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 36
- 238000004070 electrodeposition Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000011068 loading method Methods 0.000 description 10
- 238000005520 cutting process Methods 0.000 description 9
- 238000002791 soaking Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- 238000005303 weighing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000985 reflectance spectrum Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910003893 H2WO4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000036962 time dependent Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
Abstract
The invention belongs to the field of photocatalytic environmental pollutant treatment, and discloses a preparation method and application of a tantalum oxynitride/foamed nickel photocatalytic contact oxide film. Tantalum pentoxide is used as raw material, put into a tube furnace, and put into NH3Nitriding in atmosphere, and cooling to obtain tantalum oxygen nitrogen. Dispersing tantalum oxygen-nitrogen powder in acetone, adding an iodine simple substance, and performing ultrasonic treatment to form charged suspended TaON particles. And (3) using two pieces of cleaned nickel foam as the anode and the cathode of the electrode respectively, electrodepositing under the action of direct current voltage, drying and taking out to obtain the tantalum oxynitride/nickel foam photocatalytic contact oxide film. The result of the photocatalytic treatment of the fuchsin solution shows that the supported tantalum oxygen nitrogen/foamed nickel contact oxide film with the load of 60mg has the highest photocatalytic activity. Approximately 80% of the magenta in a 50mL,10mg/L magenta solution was degraded after 5h illumination with a 72W white LED light source. Circulation typeThe activity of the degraded fuchsin is not obviously reduced by using the photocatalytic contact oxide film for three times.
Description
Technical Field
The invention belongs to the technical field of photocatalytic environmental pollutant purification, and particularly relates to a preparation method of a tantalum oxynitride/foamed nickel photocatalytic contact oxide film and application of the tantalum oxynitride/foamed nickel photocatalytic contact oxide film in water body purification.
Background
The photocatalysis technology degrades pollutants in the environment, is expected to utilize solar energy, has mild reaction conditions, can be popularized and applied on a large scale, and is widely concerned.
The currently developed photocatalysisAgent, high activity TiO with mainly ultraviolet response2ZnO, BiOCl and the like, but the utilization rate of the light energy of the ultraviolet light response photocatalysis material is lower. Therefore, there is a need to develop a highly efficient photocatalytic material for visible light absorption.
In recent years, TaON has become a hot research point as a photocatalytic material. TaON has a band gap of about 2.3eV and absorbs photons with a wavelength of 550nm at their maximum. In addition, TaON has conduction band potentials of-0.3V and 2.1V respectively, and has good oxidation-reduction performance. However, the TaON powder applied to photocatalytic water purification has the problems of easy agglomeration and loss, difficult recovery, low recycling stability and the like, and the practical application of the TaON powder photocatalyst in the purification of environmental pollutants is greatly limited by the defects.
Disclosure of Invention
In order to solve the defects that the TaON powder photocatalyst is easy to agglomerate and run off, difficult to recover, low in recycling stability and the like, the TaON powder is fixedly supported on the foamed nickel by utilizing an electrodeposition technology, and a novel high-performance tantalum oxynitride/foamed nickel photocatalytic contact oxide film is obtained.
A preparation method of a tantalum oxygen nitrogen/nickel foam photocatalytic contact oxide film comprises the following steps:
(1) weighing 1g of Ta2O5Placing the mixture into an alumina crucible, placing the alumina crucible into a tube furnace, and introducing NH at the flow rate of 100-200mL/min3And heating the furnace temperature to 850-950 ℃ at the heating rate of 10 ℃/min, nitriding for 2-4h, and cooling to room temperature to obtain TaON powder.
(2) Cutting the foam nickel screen into 3cm multiplied by 3cm square blocks, soaking with 2mol/L hydrochloric acid, performing ultrasonic treatment for 10min, taking out, washing with distilled water for three times to be neutral, and drying for later use.
(3) Weighing 100-200mg TaON powder, putting the powder into a 50mL beaker, adding 5-15mg of ground iodine simple substance and 30-50mL of acetone, and carrying out sealed ultrasonic treatment for 0.5h to form the charged suspended TaON particles.
(4) Taking two pieces of spare foamed nickel as a cathode and an anode, and electrodepositing for 3-5min under the action of 12-15V direct current voltage. And taking out the foamed nickel, and drying at 120 ℃ to obtain the tantalum oxygen nitrogen/foamed nickel photocatalytic contact oxide film with the carrying capacity of 30mg, 40mg, 50mg, 60mg and 70 mg.
NH of said step 1)3The flow rate is preferably 175mL/min, the nitriding temperature is 900 ℃ and the nitriding time is 3 h.
The iodine in the step 3) is preferably 10mg, and the acetone is 40 mL.
The direct current voltage in the step 4) is preferably 15V.
The tantalum oxygen nitrogen/foamed nickel photocatalytic contact oxide film prepared by the method is applied to dye wastewater treatment.
The method is specifically used for degrading the fuchsin dye wastewater, and the specific method comprises the following steps: preparing 50mL of 10mg/L fuchsin aqueous solution, pouring the solution into a 100mL photocatalytic reactor, placing the reactor on a magnetic stirrer with 4 white LED light source plates (18W/LED light source plate multiplied by 4: 72W), suspending the prepared TaON/foamed nickel above the solution, magnetically stirring the solution in a dark place for 1h, turning on a light source, carrying out photocatalytic degradation reaction, taking 4mL of the solution every 1h, measuring the absorbance of the solution by using a photometer, and calculating the degradation rate of the fuchsin.
The beneficial effects are as follows:
the invention utilizes the electrodeposition technology to immobilize the powder TaON on the foamed nickel, and obtains a photocatalytic film with application prospect in the practical production of water treatment. The problems that the catalyst efficiency is low in the existing photocatalysis technology, TaON powder is applied to photocatalytic water purification, and the problems of easy agglomeration and loss, difficulty in recovery, low recycling stability and the like exist.
The tantalum oxygen nitrogen/foamed nickel photocatalytic contact oxide film prepared by the method effectively avoids agglomeration and loss of TaON powder in actual use, is convenient to recover, and has good recycling stability. In addition, the treated water does not need to be filtered to remove the catalyst powder.
The tantalum oxygen nitrogen/foamed nickel photocatalytic contact oxide film prepared by the invention has the advantages of simple preparation method, low cost and easy industrial production and application.
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
Drawings
FIG. 1 is an X-ray diffraction pattern of a TaON sample;
FIG. 2 is a graphical representation of the morphology of TaON samples and TaON/nickel foam films;
FIG. 3 is a UV-VIS diffuse reflectance spectrum of a TaON sample;
FIGS. 4 and 5 are graphs showing the effect of TaON powder and TaON/foam nickel film degrading fuchsin solution;
FIG. 6 is a diagram showing the effect of TaON powder and TaON/foam nickel film on cyclic degradation of magenta solution;
FIG. 7 is TaON/Nickel foam, WO3The effect of the fuchsin solution for degrading the foamed nickel film.
Detailed Description
The invention is described in more detail below with reference to the following examples:
example 1
(1) 100mg of TaON powder was weighed into a 50mL beaker, and 10mg of ground elemental iodine and 40mL of acetone were added thereto, and sealed and sonicated for 0.5 h.
(2) Taking two pieces of standby foamed nickel as a cathode and an anode, performing electrodeposition for 3min under the action of 15V direct current voltage, taking out the cathode foamed nickel, and drying at 120 ℃ to obtain the tantalum oxynitride/foamed nickel photocatalytic contact oxide film with the loading capacity of about 60 mg.
The foam nickel is as follows: cutting the foam nickel screen into 3cm multiplied by 3cm square blocks, soaking with 2mol/L hydrochloric acid, performing ultrasonic treatment for 10min, taking out, washing with distilled water for three times to be neutral, and drying for later use.
TaON powder was prepared in the same manner as in comparative example 1.
The specific method for degrading the fuchsin solution comprises the following steps: preparing 50mL of 10mg/L fuchsin aqueous solution, pouring the solution into a 100mL photocatalytic reactor, placing the reactor on a magnetic stirrer with 4 white LED light source plates (18W/LED light source plate multiplied by 4: 72W), suspending the prepared TaON/foamed nickel above the fuchsin aqueous solution, magnetically stirring the solution in a dark place for 1h, turning on a light source, carrying out photocatalytic degradation reaction, taking 4mL of solution every 1h, measuring the absorbance of the solution by using a photometer, and calculating the degradation rate of the fuchsin.
Example 2
(1) 100mg of TaON powder was weighed into a 50mL beaker, and 10mg of ground elemental iodine and 40mL of acetone were added thereto, and sealed and sonicated for 0.5 h.
(2) Taking two pieces of spare foamed nickel as a cathode and an anode, and electrodepositing for 5min under the action of 15V direct current voltage.
(3) And (3) after the residual solution is subjected to ultrasonic treatment for 15min, using new nickel foam as a cathode, performing electrodeposition for 5min under the voltage of 15V, taking out the cathode, and drying at 120 ℃ to obtain the tantalum oxynitride/nickel foam photocatalytic contact oxide film with the loading capacity of about 30 mg.
The foam nickel is as follows: cutting the foam nickel screen into 3cm multiplied by 3cm square blocks, soaking with 2mol/L hydrochloric acid, performing ultrasonic treatment for 10min, taking out, washing with distilled water for three times to be neutral, and drying for later use.
TaON powder was prepared by the method of comparative example 1.
The procedure for degrading the magenta solution was the same as in example 1.
Example 3
(1) 150mg of TaON powder was weighed into a 50mL beaker, and 10mg of ground elemental iodine and 40mL of acetone were added thereto, and sealed and sonicated for 0.5 h.
(2) Taking two pieces of spare foamed nickel as a cathode and an anode, and electrodepositing for 5min under the action of 15V direct current voltage.
(3) And (3) after the residual solution is subjected to ultrasonic treatment for 15min, using new nickel foam as a cathode, performing electrodeposition for 5min under the voltage of 15V, taking out the cathode, and drying at 120 ℃ to obtain the tantalum oxynitride/nickel foam photocatalytic contact oxide film with the loading amount of about 40 mg.
The foam nickel is as follows: cutting the foam nickel screen into 3cm multiplied by 3cm square blocks, soaking with 2mol/L hydrochloric acid, performing ultrasonic treatment for 10min, taking out, washing with distilled water for three times to be neutral, and drying for later use.
TaON powder was prepared by the method of comparative example 1.
The procedure for degrading the magenta solution was the same as in example 1.
Example 4
(1) 150mg of TaON powder was weighed into a 50mL beaker, and 10mg of ground elemental iodine and 40mL of acetone were added thereto, and sealed and sonicated for 0.5 h.
(2) Taking two pieces of spare foamed nickel as a cathode and an anode, and electrodepositing for 3min under the action of 15V direct current voltage.
(3) And (3) after the residual solution is subjected to ultrasonic treatment for 15min, using new nickel foam as a cathode, performing electrodeposition for 3min under the voltage of 15V, taking out the cathode, and drying at 120 ℃ to obtain the tantalum oxynitride/nickel foam photocatalytic contact oxide film with the loading capacity of about 50 mg.
The foam nickel is as follows: cutting the foam nickel screen into 3cm multiplied by 3cm square blocks, soaking with 2mol/L hydrochloric acid, performing ultrasonic treatment for 10min, taking out, washing with distilled water for three times to be neutral, and drying for later use.
TaON powder was prepared by the method of comparative example 1.
The procedure for degrading the magenta solution was the same as in example 1.
Example 5
(1) 100mg of TaON powder was weighed into a 50mL beaker, and 10mg of ground elemental iodine and 40mL of acetone were added thereto, and sealed and sonicated for 0.5 h.
(2) Taking two pieces of standby foamed nickel as a cathode and an anode, performing electrodeposition for 5min under the action of 15V direct current voltage, taking out the cathode, and drying at 120 ℃ to obtain the tantalum oxynitride/foamed nickel photocatalytic contact oxide film with the loading amount of about 70 mg.
The foam nickel is as follows: cutting the foam nickel screen into 3cm multiplied by 3cm square blocks, soaking with 2mol/L hydrochloric acid, performing ultrasonic treatment for 10min, taking out, washing with distilled water for three times to be neutral, and drying for later use.
TaON powder was prepared by the method of comparative example 1.
The procedure for degrading the magenta solution was the same as in example 1.
Example 6
(1) 100mg of TaON powder was weighed into a 50mL beaker, and 5mg of ground elemental iodine and 40mL of acetone were added thereto, and sealed and sonicated for 0.5 h.
(2) Taking two pieces of standby foamed nickel as a cathode and an anode, performing electrodeposition for 3min under the action of 15V direct current voltage, taking out the cathode foamed nickel, and drying at 120 ℃ to obtain the tantalum oxynitride/foamed nickel photocatalytic contact oxide film with the loading capacity of about 60 mg.
The foam nickel is as follows: cutting the foam nickel screen into 3cm multiplied by 3cm square blocks, soaking with 2mol/L hydrochloric acid, performing ultrasonic treatment for 10min, taking out, washing with distilled water for three times to be neutral, and drying for later use.
TaON powder was prepared in the same manner as in comparative example 1.
The procedure for degrading the magenta solution was the same as in example 1.
Example 7
(1) 100mg of TaON powder was weighed into a 50mL beaker, and 15mg of ground elemental iodine and 40mL of acetone were added thereto, and sealed and sonicated for 0.5 h.
(2) Taking two pieces of standby foamed nickel as a cathode and an anode, performing electrodeposition for 3min under the action of 15V direct current voltage, taking out the cathode foamed nickel, and drying at 120 ℃ to obtain the tantalum oxynitride/foamed nickel photocatalytic contact oxide film with the loading capacity of about 60 mg.
The foam nickel is as follows: cutting the foam nickel screen into 3cm multiplied by 3cm square blocks, soaking with 2mol/L hydrochloric acid, performing ultrasonic treatment for 10min, taking out, washing with distilled water for three times to be neutral, and drying for later use.
TaON powder was prepared in the same manner as in comparative example 1.
The procedure for degrading the magenta solution was the same as in example 1.
Example 8
(1) 100mg of TaON powder was weighed into a 50mL beaker, and 10mg of ground elemental iodine and 40mL of acetone were added thereto, and sealed and sonicated for 0.5 h.
(2) Taking two pieces of standby foamed nickel as a cathode and an anode, performing electrodeposition for 3min under the action of 12V direct current voltage, taking out the cathode foamed nickel, and drying at 120 ℃ to obtain the tantalum oxynitride/foamed nickel photocatalytic contact oxide film with the loading capacity of about 60 mg.
The foam nickel is as follows: cutting the foam nickel screen into 3cm multiplied by 3cm square blocks, soaking with 2mol/L hydrochloric acid, performing ultrasonic treatment for 10min, taking out, washing with distilled water for three times to be neutral, and drying for later use.
TaON powder was prepared in the same manner as in comparative example 1.
The procedure for degrading the magenta solution was the same as in example 1.
Comparative example 1
Weighing 1g of Ta2O5Placing into an alumina crucible, placing into a tube furnace, and introducing NH at a flow rate of 175mL/min3And heating the furnace temperature to 900 ℃ at the heating rate of 10 ℃/min, nitriding for 3h, and cooling to room temperature to obtain TaON powder.
Comparative example 2
Weighing 1g H2WO4Placing into an alumina crucible, placing into a tubular furnace, heating to 500 deg.C at a heating rate of 10 deg.C/min, roasting for 3 hr, and cooling to room temperature to obtain WO3And (3) powder.
Weighing the milled WO3100mg, put into a 50mL beaker, and 10mg of ground elemental iodine and 40mL of acetone are added thereto, and sealed and sonicated for 0.5 h. Taking two pieces of standby foamed nickel as a cathode and an anode, performing electrodeposition for 3min under the action of 15V direct current voltage, taking out the cathode foamed nickel, and drying at 120 ℃ to obtain WO with the loading capacity of about 60mg3Foam nickel photocatalytic contact oxide film.
FIG. 1 is an X-ray diffraction pattern of a TaON sample. As can be seen from FIG. 1, the diffraction peaks of the TaON sample were consistent with the monoclinic phase (PDF #70-1193) with no other peaks present, indicating that Ta was used2O5At NH3The pure TaON powder can be prepared with the flow of 175mL/min, the temperature of 900 ℃ and the nitriding time of 3 h.
FIG. 2 is a morphology chart of a TaON sample and a TaON/foam nickel film. As can be seen from FIG. 2, the TaON sample synthesized was pale yellow, the particles of the sample had a cobblestone shape, and the surface had small pores corroded by ammonia gas, and the particles had an average length of about 500nm and a width of about 250 nm. The TaON powder is uniformly fixed on the foamed nickel to form a TaON/foamed nickel film.
FIG. 3 is a UV-VIS diffuse reflectance spectrum of a TaON sample. As shown in FIG. 3, the prepared TaON has a wide light absorption range, a maximum absorption wavelength of 550nm and a band gap value of about 2.3eV, which proves that the TaON has good visible light absorption properties.
FIG. 4 is a graph showing the time-dependent change of absorbance of TaON powder and TaON/foam nickel film degradation fuchsin solutions with different solid loading amounts, and FIG. 5 is a graph showing the actual effect of 60 mgTaON/foam nickel film degradation fuchsin. As is clear from FIG. 4, 50mg TaON powder and 30, 40, 50, 60, and 70mg TaON/foam nickel thin films were used, and 50mL and 10mg/L magenta solutions were degraded under 72W white LED light source, and the magenta concentration gradually decreased with the increase of light irradiation time. The supported amount of 60 mgTaON/nickel foam film had the highest activity compared to other films. After 5h of LED illumination, it was able to degrade about 80% of the magenta.
The degrading activity of TaON powder to fuchsin at 1 st time is slightly higher than that of a 60 mgTaON/nickel foam film, but the degrading effect to fuchsin in the 2 nd and 3 rd cycle use is obviously lower than that of the 60 mgTaON/nickel foam film (figure 6).
FIG. 7 is TaON/Nickel foam, WO3The effect of the fuchsin solution for degrading the foamed nickel film. As can be seen from FIG. 7, the activity ratio WO of the supported amount of 60 mgTaON/nickel foam film3The/foamed nickel film is high. After 5h of LED illumination, TaON/foam Ni film can degrade about 80% of magenta, while WO3The nickel foam film degraded approximately 60% magenta.
Claims (6)
1. A preparation method of a tantalum oxygen nitrogen (TaON)/foamed nickel photocatalytic contact oxide film is characterized by comprising the following steps: and putting the prepared TaON powder into an acetone and iodine simple substance solution, ultrasonically forming a suspension, and depositing the suspension on clean foamed nickel under the action of direct current voltage to obtain the TaON/foamed nickel photocatalytic contact oxidation film.
2. The method for preparing the tantalum oxygen nitrogen/nickel foam photocatalytic contact oxide film according to claim 1, wherein the method for preparing TaON powder comprises the following steps: mixing Ta2O5The powder is put into an alumina crucible and put into a tube furnace, NH is introduced at the flow rate of 100 plus 200mL/min3And heating the furnace temperature to 850-950 ℃ at the heating rate of 10 ℃/min, nitriding for 2-4h, and cooling to room temperature to obtain TaON powder.
3. The preparation method of the tantalum oxygen nitrogen/nickel foam photocatalytic contact oxide film as claimed in claim 1, wherein the mass ratio of TaON powder to iodine is 20-40: 1-3, the volume of the acetone solution is 30-50mL, and the ultrasonic treatment is carried out for 0.5 h.
4. The method for preparing the tantalum oxygen nitrogen/foamed nickel photocatalytic contact oxide film as claimed in claim 1, wherein the voltage is 12-15V, the deposition time is 3-5min, the size of the foamed nickel is 3cm x 3cm, the foamed nickel needs to be soaked with 2mol/L hydrochloric acid before use, ultrasonic treatment is carried out for 10min, the foamed nickel is taken out and washed with distilled water for three times until the foamed nickel is neutral, and the foamed nickel is dried for later use.
5. The application of the tantalum oxygen nitrogen/nickel foam photocatalytic contact oxide film in water body purification according to claim 1.
6. The application of the tantalum oxygen nitrogen/foamed nickel photocatalytic contact oxide film in water body purification, which is characterized in that the oxide film is used for degrading magenta dye wastewater, and the specific method comprises the following steps: preparing 50mL of 10mg/L fuchsin aqueous solution, pouring the solution into a 100mL photocatalytic reactor, placing the reactor on a magnetic stirrer with 4 white LED light source plates (18W/LED light source plate multiplied by 4: 72W), suspending the prepared TaON/foamed nickel above the solution, magnetically stirring the solution in a dark place for 1h, turning on a light source, carrying out photocatalytic degradation reaction, taking 4mL of the solution every 1h, measuring the absorbance of the solution by using a photometer, and calculating the degradation rate of the fuchsin.
Priority Applications (1)
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