阅读说明：本技术 一种钽氧氮/泡沫镍光催化接触氧化膜的制备方法和应用 (Preparation method and application of tantalum oxygen nitrogen/foamed nickel photocatalytic contact oxide film ) 是由 王少莽 关媛 于 2019-10-09 设计创作，主要内容包括：本发明属于光催化环境污染物治理领域,公开了一种钽氧氮/泡沫镍光催化接触氧化膜的制备方法和应用。以五氧化二钽为原料,置于管式炉中,在NH<Sub>3</Sub>气氛中氮化,冷却获得钽氧氮。将钽氧氮粉体分散在丙酮中,加入碘单质,超声形成带电悬浮TaON粒子。用两片洗净后的泡沫镍分别作为电极正极和负极,在直流电压的作用下电沉积,干燥取出获得钽氧氮/泡沫镍光催化接触氧化膜。将其光催化处理品红溶液结果显示,担载量为60mg钽氧氮/泡沫镍接触氧化膜光催化活性最高。在72W白色LED光源照射5h后,能够将50mL、10mg/L品红溶液中约80％的品红降解。循环三次使用该光催化接触氧化膜降解品红,其活性并没有明显地下降。(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 NH 3 Nitriding 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.)

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.

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: