Method for preparing tungsten disulfide-based piezoelectric catalytic material at second-level ultra-fast speed and water treatment application of tungsten disulfide-based piezoelectric catalytic material

Abstract

The invention discloses a second-level ultrafast preparation method of a tungsten disulfide-based piezoelectric catalytic material, which overcomes the problems of complexity and high cost in the traditional method by combining ultrasonic treatment, rotary evaporation and magnetic induction heating. The method is simple to operate and short in preparation time, and the efficient tungsten disulfide-based piezoelectric catalytic material can be prepared in a short time. Meanwhile, the material has excellent catalytic performance and stability and can be widely applied to the fields of electro-catalysis hydrogen evolution reaction, water treatment and the like.

Description

[Technical field]

[0001] The present invention relates to a method for preparing a tungsten disulfide-based piezoelectric catalytic material ultra-fast in seconds, in particular to a method for preparing a tungsten disulfide-based piezoelectric catalytic material by ultrasonic treatment, rotary evaporation and magnetic induction heating, and an application of the method in water treatment, belonging to the field of material science and environmental engineering technology. [Background technology]

[0002] Tungsten disulfide (WS2) is a layered transition metal disulfide with unique physical and chemical properties similar to molybdenum disulfide. It has broad application prospects in catalysis, optoelectronics, sensing and other fields. Especially in the electrocatalytic hydrogen evolution reaction (HER), WS2 is also considered to be a potential high-efficiency catalyst to replace platinum. In recent years, with the increase in energy demand and the intensification of environmental problems, the development of efficient and low-cost catalytic materials to replace precious metal catalysts has become a research hotspot. WS2 has received widespread attention due to its efficient catalytic performance, stability and abundant resources.

[0003] At present, the preparation methods of WS2 mainly include hydrothermal / solvothermal method, chemical vapor deposition (CVD) method, liquid phase exfoliation method, etc. These methods have made certain progress in controlling the morphology and performance of the product, but generally have problems such as complex preparation process, long time consumption, and high cost. In addition, it is difficult to achieve large-scale production during the preparation process, which also limits the promotion of WS2 in practical applications.

[0004] In order to improve the catalytic performance of WS2, researchers have introduced a variety of modification methods during the preparation process. For example, by doping different elements (such as nitrogen, phosphorus, etc.) or introducing defect structures, the electrocatalytic performance of WS2 can be significantly improved. At the same time, compounding WS2 with conductive materials (such as graphene, carbon nanotubes, etc.) can improve its conductivity and stability, and further improve its catalytic performance. However, these modification methods still face challenges in practical applications, such as complex processes and high costs.

[0005] Magnetic induction heating (MIH) is an emerging heating technology with the advantages of fast heating speed, concentrated energy, and strong controllability. It has been gradually applied to the field of material preparation in recent years. MIH can achieve high-temperature heating in a short time, effectively avoiding the temperature gradient problem caused by heat diffusion in traditional heating methods, thereby achieving precise control of the material microstructure.

[0006] Patent CN201811280601.7 discloses a method for preparing a three-dimensional self-assembled flower-shaped tungsten disulfide material, wherein sodium tungstate dihydrate is added to a mixed solution of deionized water and ethanol, stirred until dissolved to form a transparent solution A, then ammonium acetate is added and stirred evenly, then oleic acid is added, mixed evenly, the pH value is adjusted to 1.3-1.7, and the hydrothermal reaction is carried out at 160-180°C for 12-24h, centrifuged, and dried to obtain WO3·0.33H2O powder; the WO3·0.33H2O powder is mixed with thioacetamide at a molar ratio of 1:20, and calcined to obtain a three-dimensional self-assembled flower-shaped tungsten disulfide material. Patent CN201410379340.X discloses a method for preparing tungsten disulfide nanorods, comprising the following steps: adding tungsten disulfide powder to a mixed solvent of water and ethanol to perform a hydrothermal synthesis reaction; then ultrasonicating and centrifuging the solution after the reaction to obtain tungsten disulfide nanorods. [Summary of the invention]

[0007] [Technical issues to be solved]

[0008] The purpose of the present invention is to provide a method for preparing tungsten disulfide-based piezoelectric catalytic materials in seconds, which overcomes the complexity and high cost problems existing in traditional methods by combining ultrasonic treatment, rotary evaporation and magnetic induction heating. The method is simple to operate and has a short preparation time, and can prepare efficient tungsten disulfide-based piezoelectric catalytic materials in a short time. At the same time, the material has excellent catalytic performance and stability, and can be widely used in the fields of electrocatalytic hydrogen evolution reaction and water treatment.

[0009] [Technical solution]

[0010] A method for preparing a tungsten disulfide-based piezoelectric catalytic material ultra-fast in seconds and a water treatment application thereof, characterized in that the method comprises the following steps:

[0011] (1) 100 mg of tungsten trioxide (WO3) and 500 mg of thiourea were dissolved in 10 mL of ethanol and treated with ultrasound for 20 minutes to obtain a transparent solution.

[0012] (2) Add 50 mg of carbon black to the above transparent solution and mix well.

[0013] (3) The mixture was dried by rotary evaporation at 40°C.

[0014] (4) The dried mixture was further dried in a vacuum oven at 60°C for 8 hours.

[0015] (5) The dried material was loaded onto an iron sheet covered with a piece of graphite paper with a thickness of 0.01 mm. The size of the iron sheet was 2.5 cm×2.5 cm×0.2 mm.

[0016] (6) Place the above assembly at the center of the refractory brick in a quartz tube and purge it with high-purity argon gas (flow rate of 100 mL / min) for 10 minutes.

[0017] (7) The quartz tube was placed in a four-turn induction coil with a diameter of 5 cm and subjected to magnetic induction heating for 10 seconds under a controlled current (200 A).

[0018] (8) After magnetic induction heating, the sample is allowed to cool naturally to room temperature to obtain a tungsten disulfide-based piezoelectric catalytic material.

[0019] (9) The prepared piezoelectric catalyst material was added to a water sample containing 10 mg / L of organic pollutants such as rhodamine b at a mass concentration of 10 mg / L. The removal rate of the pollutants was measured after ultrasonic treatment for 5 minutes to evaluate the piezoelectric catalytic efficiency of the material.

[0020] [Beneficial Effects]

[0021] The tungsten disulfide-based piezoelectric catalytic material prepared by this method not only exhibits excellent catalytic performance in the electrocatalytic hydrogen evolution reaction, but also shows good results in water treatment applications. This provides new ideas and methods for the promotion of WS2-based materials in practical applications, and has important research value and application prospects.

Brief Description of the Drawings

[0022] Figure 1 : A transmission electron microscope (TEM) image of the WS2 piezoelectric catalytic material prepared after Example 1 is shown, showing its microstructure.

[0023] Figure 2 : The Raman spectrum (Raman) of the WS2 piezoelectric catalytic material prepared after Example 1 is shown, reflecting its chemical composition and structural characteristics.

[0024] Figure 3 :The effect diagram of the WS2 piezoelectric catalytic material prepared after Example 1 in the degradation of rhodamine b organic pollutant is shown, illustrating its application potential in water treatment. [Specific implementation method]

[0025] Embodiment 1:

[0026] (1) 100 mg of tungsten trioxide (WO3) and 500 mg of thiourea were dissolved in 10 mL of ethanol and treated with ultrasound for 20 minutes to obtain a transparent solution.

[0027] (2) Add 50 mg of carbon black to the above transparent solution and mix well.

[0028] (3) The mixture was dried by rotary evaporation at 40°C.

[0029] (4) The dried mixture was further dried in a vacuum oven at 60°C for 8 hours.

[0030] (5) The dried material was loaded onto an iron sheet covered with a piece of graphite paper with a thickness of 0.01 mm. The size of the iron sheet was 2.5 cm×2.5 cm×0.2 mm.

[0031] (6) Place the above assembly at the center of the refractory brick in a quartz tube and purge it with high-purity argon gas (flow rate of 100 mL / min) for 10 minutes.

[0032] (7) The quartz tube was placed in a four-turn induction coil with a diameter of 5 cm and subjected to magnetic induction heating for 10 seconds under a controlled current (200 A).

[0033] (8) After magnetic induction heating, the sample is allowed to cool naturally to room temperature to obtain a tungsten disulfide-based piezoelectric catalytic material.

[0034] (9) The prepared piezoelectric catalyst material was added to a water sample containing 10 mg / L of organic pollutants such as rhodamine b at a mass concentration of 10 mg / L. The removal rate of the pollutants was measured after ultrasonic treatment for 5 minutes to evaluate the piezoelectric catalytic efficiency of the material.

[0035] Embodiment 2:

[0036] (1) 200 mg of tungsten trioxide (WO3) and 200 mg of thiourea were dissolved in 10 mL of ethanol, 5 wt% of ferric chloride was added, and ultrasonic treatment was performed for 20 minutes to obtain a transparent solution.

[0037] (2) Add 50 mg of carbon black to the above transparent solution and mix well.

[0038] (3) The mixture was dried by rotary evaporation at 40°C.

[0039] (4) The dried mixture was further dried in a vacuum oven at 60°C for 8 hours.

[0040] (5) The dried material was loaded onto an iron sheet covered with a piece of graphite paper with a thickness of 0.01 mm. The size of the iron sheet was 2.5 cm×2.5 cm×0.2 mm.

[0041] (6) Place the above assembly at the center of the refractory brick in a quartz tube and purge it with high-purity argon gas (flow rate of 100 mL / min) for 10 minutes.

[0042] (7) The quartz tube was placed in a four-turn induction coil with a diameter of 5 cm and subjected to magnetic induction heating for 10 seconds under a controlled current (200 A).

[0043] (8) After magnetic induction heating, the sample is allowed to cool naturally to room temperature to obtain an iron-modified tungsten disulfide-based piezoelectric catalytic material.

[0044] (9) The prepared iron-modified tungsten disulfide-based piezoelectric catalyst material was added to a water sample containing 10 mg / L of organic pollutants such as rhodamine b at a mass concentration of 10 mg / L. The removal rate of the pollutants was measured after stirring for 30 minutes to evaluate the piezoelectric catalytic efficiency of the material.

Claims

1. A method for preparing tungsten disulfide-based piezoelectric catalytic materials ultra-fast in seconds, comprising the following steps: (1) Dissolve 200 mg to 500 mg of tungsten trioxide (WO3) and 200 mg to 500 mg of thiourea in 5 mL to 50 mL of ethanol, add 0-20 wt% of ferric chloride, and obtain a transparent solution by ultrasonic treatment; (2) Add 50 mg to 200 mg of carbon black to the above transparent solution and mix well; (3) drying the mixture by rotary evaporation; (4) the dried mixture is further dried in a vacuum oven at 50° C. to 100° C. for 4 to 12 hours; (5) loading the dried substance onto an iron sheet covered with a graphite paper having a thickness of 0.01 mm to 0.05 mm, wherein the size of the iron sheet is 2 cm to 5 cm×2 cm to 5 cm×0.1 mm to 0.5 mm; (6) placing the above assembly in a refractory brick in a quartz tube and purging with high-purity inert gas for 5 to 30 minutes; (7) placing the quartz tube in a multi-turn induction coil with a diameter of 3 cm to 7 cm and performing magnetic induction heating for 5 seconds to 30 seconds under a controlled current (X = 50 to 800 A); (8) After magnetic induction heating, the sample is allowed to cool naturally to room temperature, and finally a tungsten disulfide-based piezoelectric catalytic material is obtained for water treatment applications. (9) The prepared piezoelectric catalyst material was added to a water sample containing organic pollutants at a mass concentration of 10-1000 mg / L, and the removal rate of the pollutants was measured after ultrasonic treatment for 1-60 minutes or stirring for 0.1-6 hours to evaluate the piezoelectric catalytic efficiency of the material.

2. The method according to claim 1, wherein the inert gas is argon, nitrogen or helium, and the flow rate of the inert gas is 50 mL / min to 500 mL / min.

3. The method according to claim 1, wherein the frequency of the magnetic induction heating is 50 kHz to 1 MHz, the time of the magnetic induction heating is 5 seconds to 60 seconds, and the power of the induction coil is 1 kW to 10 kW.

4. The method according to claim 1, wherein the conductivity of the graphite paper is 10 S / cm to 1000 S / cm.

5. The method according to claim 1, wherein the molar ratio of tungsten trioxide (WO3) to thiourea is 1:1 to 1:

3. The method according to claim 1 , wherein the particle size of the carbon black is 20 nm to 100 nm.

7. The method according to claim 1, wherein the surface of the iron sheet is pretreated to improve the adhesion of the graphite paper.

8. The method according to claim 1, wherein the obtained tungsten disulfide-based piezoelectric catalytic material is used for piezoelectric catalytic degradation of organic matter in water and has high catalytic performance and stability.

9. The method according to claim 1, wherein the tungsten disulfide-based piezoelectric catalytic material has a morphology of nanosheets or nanowires.

10. The method of claim 1, wherein the tungsten disulfide-based piezoelectric catalytic material is used in water treatment applications, including but not limited to water purification and sewage treatment.

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