Ultrafast synthesized nickel modified molybdenum disulfide material and piezoelectric catalytic sterilization application method thereof

Abstract

The invention provides an ultra-fast synthesized nickel-doped molybdenum disulfide material and an application method thereof in piezoelectric catalytic sterilization. According to the method, a solid-phase reaction is combined with a magnetic induction heating technology, so that the problems of harsh synthesis conditions, long time consumption, low yield and the like of a traditional hydrothermal method are effectively solved. The method is simple and convenient in process and rapid in reaction, and the nickel-doped molybdenum disulfide material with high doping uniformity and excellent piezoelectric property can be synthesized within tens of seconds. The prepared material shows excellent piezoelectric catalytic sterilization performance and long-term stability under excitation of low energy such as stirring, is suitable for various application scenes such as water purification, air sterilization and medical treatment and public health, and has wide practical popularization value.

Description

Technical field

[0001] The present invention relates to a method for rapid synthesis of nickel-doped molybdenum disulfide composite materials and their application in piezoelectric catalytic sterilization, in particular to a method for preparing Ni-MoS2 piezoelectric catalytic materials based on magnetic induction heating technology and using them for efficient antibacterial treatment, belonging to the interdisciplinary field of environmental governance and materials chemistry. [Background Technology]

[0002] With increasing emphasis on environmental safety and public health, the infection risks posed by microbial contamination are becoming a growing concern. While traditional sterilization methods, such as ultraviolet radiation, heat sterilization, or chemical disinfection, are effective, they are limited in terms of energy consumption, safety, and material compatibility. This has led to extensive research into new, green, efficient, and non-destructive sterilization technologies.

[0003] Piezoelectric catalysis is a green catalytic method that relies on materials to generate charges under mechanical stress and then drive interfacial reactions. It can complete sterilization without additional energy consumption. Molybdenum disulfide (MoS2) has potential application prospects in the field of piezoelectric catalysis due to its layered structure and good flexibility. However, its poor intrinsic conductivity and weak piezoelectric response still limit its catalytic activity. Metal doping is considered to be an effective strategy to improve its electronic structure and reaction activity. Among them, nickel has become an ideal modification element due to its good conductivity and electronic synergy.

[0004] Traditional nickel-doped MoS2 synthesis methods, such as hydrothermal and high-temperature atmosphere pyrolysis, generally suffer from long synthesis cycles, high equipment requirements, and low doping efficiency. To address this, the present invention proposes a novel rapid synthesis pathway that combines ultrasound-assisted dispersion, rotary evaporation, and magnetic induction heating. This significantly shortens the preparation cycle, improves doping uniformity, and enhances catalytic activity. The resulting material can achieve efficient sterilization under conventional stirring and is suitable for broad-spectrum removal of microorganisms in water, surfaces, and air.

[0005] With the continuous development of society and technology, bacterial infections and diseases are becoming increasingly serious. This is particularly true in areas such as healthcare, food safety, and the public environment, where the demand for efficient sterilization technologies is urgent. While effective, traditional sterilization methods such as chemical disinfection and thermal sterilization have limitations. Chemical disinfectants can leave residues, potentially harming the environment and humans, while thermal sterilization can damage temperature-sensitive items. Therefore, the development of new, efficient, and environmentally friendly sterilization technologies is a pressing need. [Summary of the invention]

[0006] [Technical problems to be solved]

[0007] The present invention aims to provide an efficient and convenient method for rapidly preparing nickel-doped MoS2 composite materials, addressing the high energy consumption, cumbersome procedures, and poor material properties inherent in traditional processes. Furthermore, the invention aims to expand its application in piezoelectric catalytic sterilization, by driving the production of highly active reactive species through simple mechanical perturbations, achieving efficient, broad-spectrum sterilization with practical environmental adaptability and reusability.

[0008] [Technical solution]

[0009] A method for ultra-fast synthesis of nickel-modified molybdenum disulfide material and its piezoelectric catalytic sterilization application, characterized in that the ultra-fast synthesis of nickel-modified molybdenum disulfide material comprises the following steps:

[0010] (1) Dissolve 100-400 mg of ammonium molybdate, 100-400 mg of sodium thiosulfate, and 5-80 mg of nickel nitrate in 10 mL to 40 mL of isopropanol and treat under ultrasonication for 15 to 30 minutes to obtain a transparent and uniform precursor solution.

[0011] (2) Add 50-150 mg of graphene oxide powder to the above precursor solution and stir thoroughly.

[0012] (3) The mixed solution is concentrated to dryness by rotary evaporation to obtain a solid precursor.

[0013] (4) Dry the precursor in a vacuum drying oven at 60°C to 90°C for 6 to 10 hours.

[0014] (5) The dried material is evenly dispersed and pressed onto the surface of a copper sheet covered with a graphite film with a thickness of 0.02 mm to 0.04 mm. The size of the copper sheet is 3 cm to 4 cm × 3 cm to 4 cm × 0.2 mm to 0.4 mm.

[0015] (6) Place the assembly on a refractory tray in a quartz tube and purge it with high-purity argon for 10 to 25 minutes to remove air.

[0016] (7) Place the quartz tube in an induction coil with a diameter of 4 cm to 6 cm, pass a current of 100 A to 600 A, and perform magnetic induction heating treatment for 10 to 45 seconds.

[0017] (8) After magnetic induction heating, the mixture was allowed to cool to room temperature to obtain a nickel-doped MoS2 composite material.

[0018] [Beneficial Effects]

[0019] The method of the present invention can achieve efficient doping and crystallization in less than one minute, greatly improving preparation efficiency and simplifying the process steps. The prepared Ni-MoS2 material exhibits good piezoelectric response and bactericidal properties. The bactericidal reaction can be stimulated under stirring or slight perturbation. It has a high bactericidal rate, strong adaptability, and good cyclic stability. It is suitable for various scenarios such as medical and health care, drinking water purification, and air microbial removal.

Brief Description of the Drawings

[0020] Figure 1 : TEM image of Ni / MoS2 piezoelectric catalytic material, showing its microstructure.

[0021] Figure 2 : The effect diagram of the nickel / MoS2 piezoelectric catalytic material prepared after Example 1 in sterilization is displayed, illustrating its application potential in sterilization in multiple scenarios. [Specific implementation method]

[0022] Example 1:

[0023] (1) 200 mg of ammonium molybdate, 200 mg of sodium thiosulfate, and 20 mg of nickel nitrate were dissolved in 20 mL of isopropanol and ultrasonically treated in an ultrasonic cleaner for 20 minutes to obtain a transparent and uniform precursor solution.

[0024] (2) Add 100 mg of graphene oxide powder to the precursor solution and stir magnetically for 15 minutes to mix thoroughly.

[0025] (3) The mixed solution was poured into a rotary evaporation bottle and rotary evaporated in a 60°C water bath until the solvent was completely removed to obtain a solid precursor.

[0026] (4) The obtained precursor was placed in a vacuum drying oven at 70°C and dried for 8 hours to obtain dry powder.

[0027] (5) The dried powder was evenly dispersed and pressed onto the surface of a pre-cut copper sheet covered with a 0.03 mm thick graphite film. The size of the copper sheet was 3 cm × 3 cm × 0.3 mm.

[0028] (6) Place the assembled copper sheet in a quartz tube and introduce high-purity argon gas at a flow rate of 400 mL / min for 20 minutes to complete the atmosphere replacement.

[0029] (7) Place the quartz tube in the center of a magnetic induction coil with a diameter of 5 cm, apply a 300A current for magnetic induction heating, keep it for 20 seconds, then turn off the power and let the quartz tube cool naturally to room temperature.

[0030] (8) Take out the copper sheet and scrape off the black powder generated on the surface to obtain nickel-doped MoS2 piezoelectric catalytic material.

[0031] (9) Weigh 9 mg of the above materials, disperse them in 9 mL of 0.85% NaCl solution, and ultrasonically disperse them for 30 minutes.

[0032] (10) Add 1 mL of 10 5 CFU / mL of E. coli suspension to make the material concentration 800 mg / L.

[0033] (11) The mixed solution was placed on a magnetic stirrer with a stirring rate of 600 rpm. The reaction times were 20 min, 60 min, 180 min, and 300 min, respectively.

[0034] (12) After each reaction, 200 μL of the mixture was taken for plate culture, and a blank control was set up. The culture was carried out at 37°C for 24 hours, and the number of colonies was counted to calculate the sterilization rate. The results showed that the sterilization rate was as high as 98% after 300 minutes of reaction. Figure 2 .

[0035] Example 2:

[0036] (1) 300 mg of ammonium molybdate, 150 mg of sodium thiosulfate, and 10 mg of nickel nitrate were dissolved in 30 mL of isopropanol and ultrasonicated for 30 minutes to obtain a precursor solution.

[0037] (2) Add 70 mg of graphene oxide powder and mix under magnetic stirring for 15 minutes.

[0038] (3) After removing the solvent by rotary evaporation, dry in a vacuum drying oven at 80°C for 6 hours.

[0039] (4) The dried product was pressed onto a copper sheet with a size of 4 cm × 4 cm × 0.4 mm and a graphite film with a thickness of 0.04 mm attached to the surface.

[0040] (5) Place the tube in a quartz tube and purge it under a high-purity argon atmosphere for 25 minutes.

[0041] (6) Apply 500A current for magnetic induction heating for 15 seconds and then cool naturally.

[0042] (7) The collected materials were used for the Staphylococcus aureus sterilization experiment, and the experimental conditions were consistent with those in Example 1.

[0043] (8) After stirring and reacting for 300 minutes, the plate count sterilization rate reached more than 93%.

Claims

1. A method for ultra-fast synthesis of nickel-modified molybdenum disulfide material, comprising the following steps: (1) Dissolve 100-400 mg of ammonium molybdate, 100-400 mg of sodium thiosulfate, and 5-80 mg of nickel nitrate in 10 mL to 40 mL of isopropanol and ultrasonicate for 15 to 30 minutes to obtain a clear solution; (2) Add 50 mg to 150 mg of graphene oxide powder to the above solution and stir to mix evenly; (3) concentrating the resulting mixed solution by rotary evaporation to obtain a solid precursor; (4) drying the precursor in a vacuum drying oven at 60°C to 90°C for 6 to 10 hours; (5) The dried material is evenly dispersed and pressed onto the surface of a copper sheet covered with a graphite film having a thickness of 0.02 mm to 0.04 mm, wherein the copper sheet has a size of 3 cm to 4 cm × 3 cm to 4 cm × 0.2 mm to 0.4 mm; (6) Place the above components on a high-temperature resistant ceramic support in a quartz tube and purge with high-purity argon gas for 10 to 25 minutes to remove residual air; (7) placing the quartz tube in a multi-turn induction coil with an inner diameter of 4 cm to 6 cm and performing magnetic induction heating treatment for 10 seconds to 45 seconds at a current of 100 A to 600 A; (8) After magnetic induction heating, the mixture is naturally cooled to room temperature to obtain a nickel-doped molybdenum disulfide piezoelectric catalytic material; (9) The obtained material was resuspended in 9 mL of 0.85% NaCl solution, and after ultrasonication for 30 minutes, 1 mL of 10% NaCl was added. s CFU / mL of Escherichia coli or Staphylococcus aureus suspension, so that the material concentration in the system is 800 mg / L; (10) The mixed system was placed on a magnetic stirrer and stirred at 600 rpm for 20, 60, 180, and 300 minutes. 200 μL of sample solution was taken at each time point for plate smear culture. At the same time, an untreated bacterial solution was set as a control and cultured in a constant temperature box for 24 hours. The sterilization rate was calculated based on the number of colonies.

2. The method according to claim 1, wherein the magnetic induction heating method is electromagnetic induction heating, eddy current heating or microwave-assisted magnetic induction heating.

3. The method according to claim 1, wherein the magnetic induction heating frequency is 80 kHz to 800 kHz, the induction coil power is 2 kW to 8 kW, and the heating time is 5 seconds to 50 seconds.

4. The method according to claim 1, wherein the amount of nickel nitrate added is 2 wt% to 40 wt% of the total mass of the material.

5. method according to claim 1, wherein the molar ratio of ammonium molybdate to sodium thiosulfate is 1:1 to 1:

2.

6. The method according to claim 1, wherein the flake diameter of the graphene oxide powder is 50 nm to 200 nm.

7. The method according to claim 1, wherein the flow rate of argon in step (6) is 80 mL / min to 400 mL / min. The method according to claim 1 , wherein the copper sheet is subjected to a surface roughening treatment to enhance adhesion of the graphite film.

9. The method according to claim 1, wherein the prepared nickel / molybdenum disulfide composite material exhibits excellent sterilization efficiency and cycle stability during the piezoelectric catalytic sterilization process.

10. The method according to claim 1, wherein the molybdenum disulfide-based piezoelectric material is applicable to a variety of sterilization scenarios, including water purification, medical surface treatment, and removal of microorganisms in the air.

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