Ultrafast synthesized iron-modified tungsten disulfide material and piezoelectric catalytic sterilization application method thereof

Abstract

According to the method for synthesizing the iron-modified tungsten disulfide material in a second-level ultra-fast mode, the ultrasonic treatment technology, the rotary evaporation technology and the magnetic induction heating technology are organically combined, the preparation period of the material is remarkably shortened, and meanwhile the catalytic activity and the structural uniformity of the material are improved. The method is easy and convenient to operate, high in efficiency, good in expandability and suitable for industrial-scale batch production. The prepared iron-modified tungsten disulfide material can excite excellent piezoelectric catalytic sterilization performance under weak energy conditions such as low-strength mechanical stirring, shows good stability, is widely applicable to water purification, air sterilization and disinfection and sterilization of daily living environments, and has a wide application prospect.

Description

Technical field

[0001] The present invention relates to a method for ultra-fast synthesis of iron-modified tungsten disulfide material and its piezoelectric catalytic sterilization application, and in particular to a method for rapid preparation of iron-modified tungsten disulfide piezoelectric catalytic material by magnetic induction heating and its application in the sterilization field, belonging to the field of environmental engineering technology. [Background Technology]

[0002] With the development of society and advancements in technology, bacterial infections and diseases are becoming increasingly serious. This is particularly true in the healthcare, food safety, and public environment sectors, leading to a growing demand for efficient and environmentally friendly sterilization technologies. While effective, traditional sterilization methods such as chemical disinfection and heat sterilization have drawbacks, including chemical residues, potential harm to the environment and human health, and damage to temperature-sensitive items.

[0003] In recent years, piezoelectric catalysis has garnered attention due to its high efficiency and environmental friendliness. Tungsten disulfide (WS2), a transition metal sulfide, possesses a unique layered structure and excellent catalytic properties, showing promising potential for sterilization applications. However, pure tungsten disulfide suffers from defects such as poor conductivity and a lack of active sites, limiting its catalytic efficiency.

[0004] Doping with transition metals is an effective way to enhance the performance of tungsten disulfide. Iron (Fe), due to its rich valence states and unique electronic structure, is an ideal doping element, significantly improving the material's conductivity and catalytic activity. However, existing methods for preparing iron-modified tungsten disulfide are complex and time-consuming, making rapid and economical large-scale production difficult.

[0005] This paper proposes a method for ultrafast synthesis of iron-modified tungsten disulfide in seconds. Combining ultrasonic treatment, rotary evaporation, and magnetic induction heating, this method significantly shortens preparation time and improves catalytic performance. This method is simple, efficient, and suitable for large-scale production.

[0006] Furthermore, iron-modified tungsten disulfide materials demonstrate excellent piezoelectric catalytic sterilization. The reactive species produced by the piezoelectric catalytic reaction, such as hydroxyl radicals and superoxide anions, effectively destroy bacterial cell walls and membrane structures, achieving highly effective sterilization. This material holds broad application prospects in healthcare, food safety, and public environmental protection. [Summary of the invention]

[0007] [Technical problems to be solved]

[0008] This invention aims to provide a method for the ultra-rapid synthesis of iron-modified tungsten disulfide materials and their piezoelectric catalytic sterilization applications, overcoming the complex, time-consuming, and costly preparation challenges of existing technologies. This method is simple to operate and requires minimal preparation time. The resulting iron-modified tungsten disulfide-based piezoelectric catalytic material exhibits excellent sterilization performance and stability under weak energy excitation, making it suitable for a variety of sterilization scenarios.

[0009] [Technical solution]

[0010] A method for ultra-fast synthesis of iron-modified tungsten disulfide material and its piezoelectric catalytic sterilization application, characterized in that the ultra-fast synthesis of iron-modified tungsten disulfide material comprises the following steps:

[0011] (1) Dissolve 0.2-3 g of sodium tungstate, 0.2-6 g of thiourea and 20-120 mg of ferric chloride in 10-40 mL of ethanol and treat with ultrasound for 15-40 minutes to obtain a uniform transparent solution.

[0012] (2) Add 50-200 mg of carbon black to the solution and stir thoroughly.

[0013] (3) The mixed solution was dried by rotary evaporation at a temperature of 40-60°C.

[0014] (4) Place the dried product in a vacuum oven at 50-100°C and continue drying for 6-10 hours.

[0015] (5) The dried solid was evenly spread on an iron sheet covered with 0.015-0.04 mm graphite paper. The size of the iron sheet was 3-4 cm × 3-4 cm × 0.2-0.4 mm.

[0016] (6) Place the iron sheet loaded with the sample in a quartz tube, place it on refractory bricks, and purge it with high-purity argon at a flow rate of 100-400 mL / min for 10-20 minutes.

[0017] (7) Place the quartz tube in the center of a multi-turn induction coil with a diameter of 4-6 cm and pass an induction current of 150-600 A for 10-25 seconds of magnetic induction heating.

[0018] (8) After heating, the mixture is naturally cooled to room temperature to obtain an iron-modified tungsten disulfide-based piezoelectric catalytic material.

[0019] [Beneficial Effects]

[0020] The method of this invention enables the rapid preparation of iron-modified tungsten disulfide materials in seconds, significantly improving preparation efficiency and material performance. This material performs exceptionally well in piezoelectric catalytic sterilization applications, generating reactive oxygen species that effectively destroy bacterial cells with high sterilization efficiency and excellent stability. Its environmentally friendly and highly effective sterilization properties make it suitable for widespread applications in healthcare, food safety, and environmental protection. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 : Transmission electron microscope (TEM) image showing the microstructure of the iron / WS2 piezoelectric catalytic material prepared after Example 1.

[0022] Figure 2 : Piezoelectric response current graph showing the piezoelectric catalytic current response of the iron / WS2 piezoelectric catalytic material prepared after Example 1.

[0023] Figure 3 : Effect graph showing the bactericidal effect of the iron / WS2 piezoelectric catalytic material prepared after Example 1, illustrating its application potential in multiple scenarios. DETAILED DESCRIPTION

[0024] Example 1:

[0025] (1) Take 1 gram of sodium tungstate, 2 grams of thiourea, and 0.12 grams of ferric chloride, and dissolve them in 30 milliliters of ethanol;

[0026] (2) Ultrasonic treatment for 30 minutes (frequency 40 kHz) to ensure uniform dispersion of iron ions;

[0027] (3) Transfer the solution to a rotary evaporator and evaporate at 60°C under reduced pressure to obtain dry powder;

[0028] (4) Place the dry powder in a magnetic induction heating furnace and heat for 10 seconds at a current of 500A to promote uniform doping of iron;

[0029] (5) Naturally cool down and collect the iron-modified tungsten disulfide material, analyze it using transmission electron microscopy (see Figure 1 ), and test its piezoelectric response (see Figure 2 );

[0030] (6) Disperse the material in deionized water to make a 1g / L suspension;

[0031] (7) Take 100mL of E. coli suspension (concentration 10 6 CFU / mL) and add the material suspension;

[0032] (8) Stir at 800 rpm for 30 minutes using magnetic stirring;

[0033] (9) Take 200μL of the coated culture for blank control and incubate at 37°C for 24 hours, count the colonies, and calculate the bactericidal rate.

[0034] Example 2:

[0035] (1) Take 0.5 g of sodium tungstate (Na2WO4·2H2O), 2 g of thiourea (CH4N2S) and 0.1 g of cobalt chloride hexahydrate (CoCl2·6H2O), dissolve them in 100 ml of a mixed solution of ethanol and deionized water (ethanol: water volume ratio is 1:1), and stir with a magnetic stirrer for 30 minutes to ensure that all components are fully dissolved and uniform.

[0036] (2) The above solution was placed in an ultrasonic processor, and the ultrasonic power was set to 200 W and the frequency was set to 60 kHz. The ultrasonic treatment was performed for 20 minutes to ensure that the cobalt ions were evenly dispersed and to promote the precursor reaction.

[0037] (3) The ultrasonically treated solution was transferred to a rotary evaporator, and the rotary evaporation temperature was set to 70°C and the vacuum degree was about 0.08 MPa. The reduced pressure evaporation was performed until the solvent was completely evaporated to obtain a uniformly dry powder precursor.

[0038] (4) The dried precursor powder was evenly spread on an iron sheet covered with 0.03 mm thick graphite paper (iron sheet size 3 cm × 3 cm × 0.3 mm), and then the iron sheet was placed in a quartz tube.

[0039] (5) High-purity argon gas was introduced into the quartz tube at a flow rate of 100 mL / min and purged continuously for 20 minutes to remove air and ensure an inert atmosphere.

[0040] (6) The quartz tube was placed in a multi-turn induction coil with a diameter of 5 cm, and magnetic induction heating was performed with a current set to 600 A and a heating time set to 5 seconds to ensure that the precursor was quickly converted into cobalt-doped tungsten disulfide nanomaterials.

[0041] (7) After heating, the mixture was cooled to room temperature and the product was collected.

[0042] (8) The product morphology was characterized by transmission electron microscopy (TEM), confirming that cobalt was uniformly doped and the material exhibited a well-formed layered nanostructure.

[0043] (9) The product was dispersed in deionized water to prepare a 2 g / L uniform suspension.

[0044] (10) Take 100 mL of 6 Add the bacterial solution of Escherichia coli at a concentration of 100 CFU / mL to the above suspension and mix well.

[0045] (11) The mixed solution was placed on a magnetic stirrer and stirred at 800 rpm for 30 min. During this process, no external light was applied, and the piezoelectric catalytic properties of the material were stimulated only by the mechanical energy generated by stirring.

[0046] (12) Take 200 μL of the mixed solution and spread it for culture. The incubator temperature is set at 37°C. After 24 hours of culture, observe the colony formation.

[0047] (13) Compared with the control group without cobalt-modified tungsten disulfide material, the test sterilization rate reached more than 95%, showing an excellent piezoelectric catalytic sterilization effect.

Claims

1. A method for ultra-fast synthesis of iron-modified tungsten disulfide material, comprising the following steps: (1) Dissolve 0.2-3 g of sodium tungstate, 0.2-6 g of thiourea, and 10-80 mg of ferric chloride in 10 mL to 40 mL of isopropanol and treat with ultrasound for 15 to 40 minutes to obtain a uniform transparent solution; (2) Add 30 mg to 150 mg of carbon black to the above solution and stir to mix evenly; (3) drying the mixture by rotary evaporation at a temperature of 40°C to 60°C; (4) further drying the dried product in a vacuum environment at 60° C. to 90° C. for 6 to 10 hours; (5) laying the dried solid on a copper sheet covered with graphite paper having a thickness of 0.015 mm to 0.04 mm, wherein the size of the copper sheet is 3 cm to 4 cm × 3 cm to 4 cm × 0.2 mm to 0.4 mm; (6) Place the assembly in a quartz tube, place it on refractory bricks, and introduce high-purity argon gas for purging at a flow rate of 100 mL / min to 400 mL / min for 10 to 20 minutes; (7) placing the quartz tube at the center of a multi-turn induction coil with a diameter of 4 cm to 6 cm, and performing magnetic induction heating under the condition of an induced current of 150 A to 600 A for a heating time of 10 seconds to 25 seconds; (8) cooling naturally to room temperature after heating to obtain an iron-modified tungsten disulfide-based piezoelectric catalytic material; (9) The obtained material was resuspended in 9 mL of 0.85% NaCl solution at a concentration of 800 mg / L, and after ultrasonic dispersion for 45 minutes, it was mixed with 1 mL of 10 6 CFU / mL of Escherichia coli or Staphylococcus aureus solution was mixed, and the bacterial concentration in the system after mixing was 10 5 CFU / mL; (10) The mixture was placed on a magnetic stirrer and stirred at 600 rpm for 20 min. 200 μL of the mixture was spread on an LB solid plate for culture. A blank control group was set up simultaneously. After culture at 37 °C for 24 h, the colonies were counted and the sterilization rate was calculated.

2. The method according to claim 1, wherein the magnetic induction heating method is high-frequency electromagnetic induction heating, alternating magnetic field ferromagnetic heating or infrared-assisted magnetic induction heating.

3. The method according to claim 1, wherein the frequency of the magnetic induction heating is 80 kHz to 500 kHz, the induction coil power is 2 kW to 8 kW, and the heating time is 5 seconds to 40 seconds.

4. The method according to claim 1, wherein the amount of ferric chloride added accounts for 2wt%-40wt% of the final precursor mass.

5. The method according to claim 1, wherein the molar ratio of sodium tungstate to thiourea is 1:1.5 to 1:2.

5. The method according to claim 1 , wherein the particle size of the carbon black is 20 nm to 80 nm.

7. The method according to claim 1, wherein the inert gas used for purging is argon or nitrogen, and the flow rate is controlled between 100 mL / min and 400 mL / min.

8. The method according to claim 1, wherein the surface of the copper sheet is mechanically polished and cleaned with ethanol to enhance the adhesion stability of the graphite paper.

9. The method according to claim 1, wherein the obtained iron / tungsten disulfide-based piezoelectric catalytic material can be efficiently used for bacterial inactivation and has excellent stability and reusability.

10. The method according to claim 1, wherein the piezoelectric catalytic sterilization is applicable to the fields of drinking water sterilization, industrial water sterilization and ambient air disinfection.

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