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CN-122013556-A - Modified nano antibacterial coating containing nano silver and preparation method thereof

CN122013556ACN 122013556 ACN122013556 ACN 122013556ACN-122013556-A

Abstract

The invention discloses a modified nano antibacterial coating containing nano silver and a preparation method thereof, belonging to the technical field of composite high polymer materials. The method comprises the steps of mixing silver nitrate, polyvinylpyrrolidone, p-phenylenediamine, isophthaloyl dichloride and ferric chloride hexahydrate according to a specific mass ratio, carrying out hydrothermal reaction and electrochemical etching, dispersing in a polyethyleneimine water solution again, dissolving polyacrylonitrile powder in N, N-dimethylformamide, carrying out electrostatic spinning, hot pressing and ethylenediamine impregnation, spraying nano silver wire sol, spin-coating a lithium fluoride solution, baking, coating a hexagonal boron nitride nano sheet and polyetherimide mixed slurry, drying, spin-coating bisphenol F type epoxy resin, curing, washing and drying after wet microetching potassium hydroxide solution. The invention improves the dispersion stability and antibacterial durability of the nano silver by surface modification and three-dimensional network construction, is suitable for the surface of a touch display module, and provides high-efficiency, durable antibacterial, high-transparency and wear-resisting performance.

Inventors

  • SI RONGMEI
  • BAO YANGUANG
  • YU NAICHUAN
  • ZHAO WENXIONG
  • HAO YANCHAO

Assignees

  • 天津宝兴威科技股份有限公司

Dates

Publication Date
20260512
Application Date
20260225

Claims (9)

  1. 1. The preparation method of the modified nano antibacterial coating containing nano silver is characterized by comprising the following steps of (1) mixing (8-15) 3-7) 1-5 (1-5) 0.05-0.2 of silver nitrate, polyvinylpyrrolidone, p-phenylenediamine, isophthaloyl chloride and ferric chloride hexahydrate according to the mass ratio, adding 100-200 parts of deionized water, carrying out hydrothermal reaction to obtain nano silver wires, carrying out electrochemical etching, then re-dispersing the etched nano silver wires in a polyethyleneimine aqueous solution with the concentration of 2-10wt%, and carrying out ultrasonic dispersion to obtain modified nano silver wire sol; (2) dissolving polyacrylonitrile powder in N, N-dimethylformamide with the mass of 6-10 times, magnetically stirring to form spinning solution, then carrying out electrostatic spinning to form nanofiber membrane, then carrying out hot pressing treatment to obtain the polyacrylonitrile nanofiber membrane, then immersing the membrane into ethylenediamine solution with the concentration of 5-15wt%, taking out, drying at low temperature, spraying modified nano silver wire sol obtained in the step (1) on the polyacrylonitrile nanofiber membrane at 0.1-0.5mL/m 2 , drying at high temperature to obtain the polyacrylonitrile membrane with the nano silver synergistic network structure, (3) dissolving lithium fluoride in ethanol to prepare solution with the concentration of 1-5wt%, spin-coating on the polyacrylonitrile membrane with the synergistic network structure obtained in the step (2), mixing hexagonal boron nitride nano-sheets and polyetherimide according to a mass ratio of 1 (0.5-2), dispersing in N-methyl pyrrolidone to prepare slurry with a concentration of 10-20wt%, coating the slurry on the spinning film obtained in the step (3), drying to obtain a spinning film containing a nano layer, spinning bisphenol F epoxy resin on the spinning film containing the nano layer obtained in the step (4) to form a coating, curing to obtain a spinning film containing a stripping layer, immersing the spinning film containing the stripping layer obtained in the step (5) into a potassium hydroxide solution with a concentration of 0.2-1wt% for wet microetching, washing with deionized water, drying with nitrogen, and drying to obtain the modified nano antibacterial coating containing nano silver.
  2. 2. The method for preparing the modified nano antibacterial coating containing nano silver according to claim 1, wherein the mass ratio of silver nitrate, polyvinylpyrrolidone, p-phenylenediamine, isophthaloyl dichloride and ferric chloride hexahydrate in the step (1) is (10-12): 4-6): 2-4): 0.1-0.15, the temperature of the hydrothermal reaction in the step (1) is 120-180 ℃ for 1-4 hours, the voltage of the electrochemical etching in the step (1) is 0.5-2V, the current density is 1-5mA/cm 2 for 10-60 seconds, the concentration of the aqueous solution of the polyethyleneimine is 4-8wt%, the power of the ultrasonic dispersion in the step (1) is 200-600W, the frequency is 20-60kHz, and the time is 30-60 minutes.
  3. 3. The preparation method of the modified nano antibacterial coating containing nano silver, which is characterized by comprising the following parameters of stirring temperature of 60-80 ℃ and rotating speed of 120-160rpm in the step (2), voltage of 10-20kV for electrostatic spinning in the step (2), flow rate of 0.5-2mL/h and receiving distance of 10-20cm, temperature of 80-120 ℃ for 5-15min for hot pressing treatment in the step (2), immersion temperature of 60-80 ℃ for 2-6h in the step (2), low-temperature drying temperature of 40-50 ℃ in the step (2) and high-temperature drying temperature of 92-98 ℃ in the step (2).
  4. 4. The method for preparing the modified nano-antibacterial coating containing nano-silver according to claim 1, wherein the spin-coating speed in the step (3) is 2000-4000rpm, the time is 30-45s, the baking temperature is 120-180 ℃ and the time is 30-60min.
  5. 5. The method for preparing the modified nano-antibacterial coating containing nano-silver according to claim 1, wherein the coating thickness in the step (4) is 0.5-1 μm, the gap is 10-50 μm and the speed is 0.1-1m/min, and the drying temperature in the step (4) is 70-80 ℃ and the time is 1-2h.
  6. 6. The method for preparing the modified nano-antibacterial coating containing nano-silver according to claim 1, wherein the spin-coating speed in the step (5) is 2000-4000rpm, the coating thickness is 60-90 μm, and the curing temperature in the step (5) is 150-200 ℃ and the time is 2-6h.
  7. 7. The method for preparing the modified nano-antibacterial coating containing nano-silver according to claim 1, wherein the microetching temperature in the step (6) is 40-60 ℃, the stirring speed is 100-200rpm, the time is 5-20min, the drying temperature in the step (6) is 50 ℃, and the drying time is 2-10min.
  8. 8. The method for preparing the modified nano-antibacterial coating containing nano-silver according to claim 1, wherein the thickness of the modified nano-antibacterial coating is 100-200 μm, the light transmittance is more than or equal to 85%, the adhesive force is more than or equal to 5B, and the hardness is more than or equal to 3H.
  9. 9. A modified nano antibacterial coating containing nano silver is characterized in that the modified nano antibacterial coating containing nano silver is obtained by the preparation method of any one of claims 1-8.

Description

Modified nano antibacterial coating containing nano silver and preparation method thereof Technical Field The invention belongs to the technical field of composite high polymer materials, and particularly relates to a modified nano antibacterial coating containing nano silver and a preparation method thereof. Background With the frequent occurrence of global public health events and the continuous promotion of health consciousness of people, the application requirements of antibacterial materials in the fields of daily life, medical treatment and electronic equipment are increasingly urgent. In particular, cross propagation of bacteria and viruses has become a potential health hazard on high-frequency contact surfaces such as touch display modules, medical instruments, public self-service terminals and the like. Traditional surface materials often lack active antibacterial capability and only rely on passive cleaning modes such as alcohol wiping or disinfectant spraying, and the methods are complex in operation and low in efficiency, and can also lead to surface corrosion, function attenuation and even secondary pollution. For this reason, the development of efficient and durable antimicrobial coatings has become a hot research direction in the field of material science. Among them, nano silver (AgNPs or AgNWs) has been paid attention to for its unique antibacterial properties, and has been widely used in antibacterial coatings. The nano silver can destroy bacterial cell membranes, inhibit DNA replication and enzyme activity by releasing silver ions (Ag +), so that a broad-spectrum sterilization effect is realized, and a high-efficiency inhibition effect on common pathogens such as staphylococcus aureus, escherichia coli and the like is realized. The prior art of nano-silver antimicrobial coatings has been developed primarily around the preparation, dispersion and coating construction of nano-silver. In terms of preparation, hydrothermal methods and polyol methods are the dominant methods. For example, silver nanowires (AgNWs) having a diameter of 20 to 50nm and a length of several tens micrometers, which have good conductivity and antibacterial properties, are synthesized by reacting silver nitrate with a reducing agent such as polyvinylpyrrolidone under high temperature and high pressure conditions, and are commonly used for antibacterial modification of transparent conductive films. Another common method is electrochemical deposition, which reduces silver ions to nanoparticles on the substrate surface to form a uniform coating. In addition, green synthesis methods, which use plant extracts (e.g., litchi rind extracts) as reducing agents to synthesize nano silver particles, have been used in antimicrobial wound dressings. These methods allow the size of the nano-silver particles to be controlled, typically in the range of 5-100nm, to optimize antimicrobial efficacy. In the aspect of coating construction, the existing nano silver antibacterial coating adopts physical methods such as spraying, spin coating or dipping to disperse nano silver in a polymer matrix. For example, nano-silver is mixed with polyacrylonitrile or polyetherimide to form a composite coating for medical implant surfaces. Another strategy is plasma polymerization, embedding nano silver into the coating, improving stability. In addition, composite coatings incorporating other nanomaterials such as titanium dioxide or boron nitride have achieved synergistic antimicrobial effects, such as a combination of photocatalysis and silver ion release, which can enhance the antimicrobial efficiency under light conditions. In the field of electronic devices, nano silver coatings are commonly used for air filters or touch screens, for example patent CN101396627a describes a coating in which nano silver is supported on a zirconium phosphate carrier for air conditioning filters, achieving durable antimicrobial. Similarly, in the field of food preservation, nano-silver coatings extend shelf life by inhibiting microbial growth (as in patent CN102057981 a). The application of nano-silver antimicrobial coatings has expanded to a number of fields. In the medical field, nano silver coatings are used in implantable devices, such as urinary catheter stents or fracture fixation devices, to prevent biofilm formation and drug-resistant bacterial infection. Research shows that the silver nano particles can effectively inhibit the formation of a biological film of methicillin-resistant staphylococcus aureus (MRSA), the inhibition rate is more than 99 percent (reference ：The antibacterial and cytotoxic effects of silver nanoparticles coated titanium implants：a narrative review,Saudi Dent J,2024）. is applied to the surface of a touch screen in the field of consumer electronics, a nano silver coating is applied to the surface of the touch screen to provide a 'touch + antibacterial' function, bacterial spread on public equipment is reduced (reference ：The antibacterial