Antibacterial non-woven fabric and preparation process thereof
By using intelligent microcapsule complexes and photosensitive grafting technology, combined with high-pressure hydroentangling and electrospinning, the problems of poor antibacterial durability and unsatisfactory physical properties of nonwoven fabrics have been solved, achieving the synergistic effect of multiple protection mechanisms and intelligent response capabilities.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- JINAN HAOXIN IND
- Filing Date
- 2026-01-09
- Publication Date
- 2026-04-17
AI Technical Summary
Existing nonwoven fabrics have poor antibacterial durability, undesirable physical properties, and limited functional dimensions. Traditional methods cannot achieve long-lasting, sustained-release, and multi-mechanism synergistic antibacterial effects.
By employing intelligent microcapsule composites and photosensitive grafting technology, and activating the fiber surface through low-temperature plasma, combined with high-pressure hydroentangling and electrospinning technology, a multi-protection mechanism is constructed to achieve controlled release of antibacterial components and improved fiber mechanical properties.
It improves the durability and physical properties of antibacterial nonwoven fabrics, achieves the synergistic effect of multiple protection mechanisms, and enhances the intelligent response capability of materials.
Smart Images

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Abstract
Description
Technical Field
[0001] This invention relates to the field of textile technology, and more specifically, to an antibacterial nonwoven fabric and its preparation process. Background Technology
[0002] Nonwoven fabrics, as a type of nonwoven material, are widely used in medical supplies, personal care, home filtration and packaging due to their advantages of short production process, low cost and strong designability. In these applications, nonwoven fabrics often become a medium for the growth and spread of microorganisms, so endowing nonwoven fabrics with antibacterial properties is of great practical significance.
[0003] Nonwoven fabrics in related technologies include main fibers, adhesives, functional additives, and finishing agents. The main fibers are generally polypropylene (PP) or polyester (PET), used to form the basic skeleton of the nonwoven fabric, providing the material with mechanical strength, shape, and main physical properties. Adhesives are generally acrylates, used in chemical or thermal bonding processes to fix the fiber network, giving the nonwoven fabric a certain structural stability and wet / dry strength. Functional additives are generally such as color masterbatches and whitening agents, mainly used to change the color or appearance of the product to meet different visual needs; they themselves do not possess bioactive functions. Finishing agents are applied in the post-processing stage of the finished product to improve the feel, eliminate static electricity, etc., but these agents have relatively weak bonding strength with the fibers.
[0004] However, it still has some drawbacks in practical use, such as poor antibacterial durability. By soaking or spraying antibacterial agents in the finishing process, the antibacterial components only physically adhere to the fiber surface and are easily and quickly lost during use and washing, resulting in a rapid decline in antibacterial effect. Poor physical properties. Adding a large amount of inorganic antibacterial powder before melt spinning will interfere with the rheological properties of the polymer melt, leading to difficulties in fiber forming, increased filament breakage, and damage to the uniformity, softness, and mechanical strength of the nonwoven fabric. Single functional dimension. Traditional methods are usually only effective for contact sterilization and lack a systematic structural design for long-lasting, sustained-release, and multi-mechanism synergistic antibacterial effects. Summary of the Invention
[0005] To improve the above-mentioned problems and reduce the issues of poor antibacterial durability, poor physical properties, and limited functional dimensions of nonwoven fabrics in related technologies, this invention provides an antibacterial nonwoven fabric and its preparation process to solve the problems mentioned in the background art.
[0006] To achieve the above objectives, the present invention provides the following technical solution: A process for preparing an antibacterial nonwoven fabric includes the following steps: S1. Polyester and nylon fibers are fed into an opening machine for initial opening, followed by the addition of aramid precipitated fibers. The mixed fibers are placed in a low-temperature plasma treatment device, and a mixed gas is introduced as the treatment atmosphere. The mixture is continuously treated at a radio frequency power of 250-450W for 60-120s to obtain surface-activated modified mixed fibers. S2. The activated mixed fibers obtained in S1 are fed into a carding machine and carded into single fibers by a cylinder and a doffer. The fibers are then laid up by a cross-laying machine to form a fiber web. The fiber web is then passed through a low-pressure hydroentanglement zone and pre-entangled and reinforced by a hydroentanglement head at a hydroentanglement pressure of 45 bar to obtain a fiber web substrate. S3. The fiber web substrate obtained in S2 is passed through an impregnation tank containing antibacterial precursor solution at a speed of 2 m / min, and squeezed by a pair of rollers to control its liquid content to 80%; then the impregnated wet fiber web is immediately introduced into an ultraviolet curing chamber filled with high-purity nitrogen gas, using an ultraviolet light-emitting diode array light source with a main wavelength of 365nm, at a light intensity of 80-150 nm. Irradiate for 2-5 minutes under the specified conditions to obtain a photocured fiber web; S4. The photocured fiber web obtained in S3 is sent into a multi-stage high-pressure hydroentanglement reinforcement system. Hydroentanglement is performed under the conditions that the first stage hydroentanglement pressure is 80 bar, the second and third stage hydroentanglement pressures are increased to 120 bar, and the hydroentangled web conveying speed is 4 m / min. Then, it is dried at a temperature of 110℃ to obtain a non-woven fabric substrate. S5. The nonwoven fabric substrate obtained in S4 is wrapped on a rotating drum receiver. The mixed spinning solution is injected into an electrospinning device and continuously spun for 30 minutes at a voltage of 150-250V, a spinneret distance of 15cm, a drum speed of 100r / min, and a relative humidity of 30%. Then the substrate is transferred into a vapor deposition chamber, perfluorooctyltriethoxysilane vapor is introduced, and it is treated at a temperature of 100-140℃ for 3-8 minutes to obtain the treated nonwoven fabric substrate. S6. The nonwoven fabric substrate obtained in S5 is subjected to instantaneous light-setting and shaping treatment through a hot rolling mill at an upper roll temperature of 150℃, a lower roll temperature of 145℃, a linear pressure of 1MPa, and a rolling speed of 10m / min. After cooling, edge trimming, and winding, antibacterial nonwoven fabric is obtained.
[0007] Preferably, the antibacterial nonwoven fabric is prepared by fiber web reinforcement, antibacterial precursor liquid impregnation and photografting, high-pressure hydroentangling bonding, and electrospinning with mixed spinning solution from polyester fiber, nylon fiber and aramid precipitated fiber. The raw materials for preparation include: 45-65 parts of polyester fiber, 25-40 parts of nylon fiber and 10-20 parts of aramid precipitated fiber.
[0008] Preferably, the preparation method of the antibacterial precursor solution includes the following steps: C1. Using a microfluidic chip device, a pH-sensitive polymer is used as the wall material to encapsulate a composite antibacterial agent, and capsules A with a particle size distribution of 2 μm are prepared. C2. Microcapsules B with a particle size of 4 μm were prepared by using cationic chitosan as the wall material to encapsulate polylysine and zinc-doped zeolite powder through complex coagulation method. C3. Place the microcapsule A obtained in C1 and the microcapsule B obtained in C2 in a low-speed mixer and mix for 60 min at a speed of 30 r / min to obtain the microcapsule complex. C4. Dimethylaminoethyl methacrylate and a crosslinking agent are dissolved together in deionized water, followed by the addition of benzophenone. The mixture is stirred at 35-45℃ and 400-600 r / min until completely dissolved to prepare a pre-grafted solution. Then, the microcapsule complex obtained in S3 is added, and the mixture is treated with an ultrasonic disperser at 300-500W for 20-40 min to obtain an antibacterial precursor solution.
[0009] Preferably, the raw materials for preparing the antibacterial precursor solution and their weight proportions are as follows: 12-22 parts of pH-sensitive polymer, 5-12 parts of composite antibacterial agent, 5-10 parts of polylysine, 8-15 parts of zinc-doped zeolite powder, 10-20 parts of cationic chitosan, 100 parts of dimethylaminoethyl methacrylate, 8-18 parts of crosslinking agent, and 1.08-1.18 parts of benzophenone.
[0010] Preferably, the pH-sensitive polymer is a copolymer of polyacrylic acid and ethylene glycol dimethacrylate; Polylysine is specifically - Polylysine; The crosslinking agent is specifically N,N'-bis(acryloyloxyethyl)ethylenediamine-N,N'-diacetic acid tetrasodium salt.
[0011] Preferably, the composite antibacterial agent is prepared by silver sulfadiazine and hexadecyltrimethylammonium bromide in a mass ratio of 1:2.
[0012] Preferably, the zeolite carrier in the zinc-doped zeolite powder is ZSM-5 type zeolite with a silicon-aluminum molar ratio of 50:1, and the mass fraction of zinc is 5.0%.
[0013] Preferably, the mass fraction of the pre-grafted solution is 10-20%.
[0014] Preferably, the mixed gas is composed of argon and oxygen in a volume ratio of 9:1.
[0015] Preferably, the mixed spinning solution is composed of thermoplastic polyurethane particles, N,N-dimethylformamide solvent, quaternized chitosan, and deionized water in a weight ratio of 7.2-8.5:91.15-92.0:0.2-0.8:9.2-9.8.
[0016] 1. This invention constructs an intelligent microcapsule composite and combines it with photosensitive grafting technology. By using photo-initiated polymerization to form a stable three-dimensional polymer network in situ on the fiber surface, the antibacterial components can be released in a controlled manner through the dual mechanisms of sustained release from the microcapsules and pH response of the polymer network, thereby improving the antibacterial performance. 2. In this invention, after activating the fiber surface with low-temperature plasma, in-situ optical grafting is performed on the formed fiber web substrate, and then a high-pressure hydroentangling process is used to promote deep bonding between the functional layer and the fiber, thereby enhancing the mechanical properties of the fiber. 3. This invention, by designing a pH-sensitive polymer wall material and an intelligent responsive crosslinking network, endows the material with the ability to keenly sense and respond to the acidity and alkalinity of the environment. Combined with the surface electrospinning construction, it realizes the synergy of multiple protection mechanisms and improves its intelligent protection capabilities. Detailed Implementation
[0017] The present invention will be further described in detail below with reference to the embodiments of the present invention. Unless otherwise specified below, the raw materials used in the various examples and embodiments of the present invention are all commercially available common materials. Preparation Examples 1-5 An antibacterial precursor solution, the components of which and their corresponding proportions are shown in the table below, is prepared using the following method: C1. Using a microfluidic chip device, a pH-sensitive polymer is used as the wall material to encapsulate a composite antibacterial agent, and capsules A with a particle size distribution of 2 μm are prepared. The pH-sensitive polymer is specifically a copolymer of polyacrylic acid and ethylene glycol dimethacrylate. The composite antibacterial agent is prepared by mixing silver sulfadiazine and hexadecyltrimethylammonium bromide in a mass ratio of 1:2. C2. Microcapsules B with a particle size of 4 μm were prepared by using cationic chitosan as the wall material to encapsulate polylysine and zinc-doped zeolite powder through complex coagulation method. Polylysine specifically refers to - Polylysine; The zinc-doped zeolite powder uses ZSM-5 type zeolite with a silicon-aluminum molar ratio of 50:1 as the zeolite carrier, and the mass fraction of zinc is 5.0%. C3. Place the microcapsule A obtained in C1 and the microcapsule B obtained in C2 in a low-speed mixer and mix for 60 min at a speed of 30 r / min to obtain the microcapsule complex. C4. Dimethylaminoethyl methacrylate and crosslinking agent are dissolved together in deionized water, then benzophenone is added, and the mixture is stirred at 40°C and 500 r / min until completely dissolved to prepare a pre-grafted solution. Then the microcapsule complex obtained in S3 is added, and the mixture is treated with an ultrasonic disperser at 400W for 30 min to obtain an antibacterial precursor solution.
[0018] The mass fraction of the pre-grafted solution was 15%. The crosslinking agent is specifically N,N'-bis(acryloyloxyethyl)ethylenediamine-N,N'-diacetic tetrasodium salt; Table: Components and their mass ratios (g) of the raw materials used in Preparation Examples 1-5 Preparation Example 6 An antibacterial precursor solution, differing from Preparation Example 1 in that its preparation method is as follows: C1. Using a microfluidic chip device, a pH-sensitive polymer is used as the wall material to encapsulate a composite antibacterial agent, and capsules A with a particle size distribution of 2 μm are prepared. C2. Microcapsules B with a particle size of 4 μm were prepared by using cationic chitosan as the wall material to encapsulate polylysine and zinc-doped zeolite powder as an antibacterial agent. C3. Place the microcapsule A obtained in C1 and the microcapsule B obtained in C2 in a low-speed mixer and mix for 60 min at a speed of 30 r / min to obtain the microcapsule complex. C4. Dimethylaminoethyl methacrylate and crosslinking agent were dissolved together in deionized water, and then benzophenone was added. The mixture was stirred at 35°C and 400 r / min until completely dissolved to prepare a pre-grafted solution. Then the microcapsule complex obtained in S3 was added and treated with an ultrasonic disperser at 300W for 20 min to obtain an antibacterial precursor solution.
[0019] Preparation Example 7 An antibacterial precursor solution, differing from Preparation Example 1 in that its preparation method is as follows: C1. Using a microfluidic chip device, a pH-sensitive polymer is used as the wall material to encapsulate a composite antibacterial agent, and capsules A with a particle size distribution of 2 μm are prepared. C2. Microcapsules B with a particle size of 4 μm were prepared by using cationic chitosan as the wall material to encapsulate polylysine and zinc-doped zeolite powder as an antibacterial agent. C3. Place the microcapsule A obtained in C1 and the microcapsule B obtained in C2 in a low-speed mixer and mix for 60 min at a speed of 30 r / min to obtain the microcapsule complex. C4. Dimethylaminoethyl methacrylate and crosslinking agent were dissolved together in deionized water, and then benzophenone was added. The mixture was stirred at 45°C and 600 r / min until completely dissolved to prepare a pre-grafted solution. Then the microcapsule complex obtained in S3 was added, and the mixture was treated with an ultrasonic disperser at 500W for 40 min to obtain an antibacterial precursor solution.
[0020] Preparation Example 8 An antibacterial precursor solution, which differs from Preparation Example 1 in that the pre-grafted solution has a mass fraction of 10%.
[0021] Preparation Example 9 An antibacterial precursor solution, which differs from Preparation Example 1 in that the pre-grafted solution has a mass fraction of 20%.
[0022] Preparation Examples 10-14 An antibacterial nonwoven fabric, the components of which and their corresponding proportions are shown in the table below, is prepared using the following method: S1. Polyester and nylon fibers are fed into an opening machine for initial opening, followed by the addition of aramid precipitated fibers. The mixed fibers are placed in a low-temperature plasma treatment device, and a mixed gas is introduced as the treatment atmosphere. The mixture is continuously treated at a radio frequency power of 350W for 90 seconds to obtain surface-activated modified mixed fibers. The mixed gas is composed of argon and oxygen in a volume ratio of 9:1. Specifically, the polyester fiber is a staple polyester fiber with a fineness range of 1.0-3.0 dtex, a length range of 38-51 mm, and a single filament strength ≥5.0 cN / dtex; Specifically, nylon fiber refers to nylon staple fiber with a surface amino content ≥35mmol / kg, a breaking elongation range of 30-50%, and an elastic recovery rate ≥90%. The aramid precipitated fibers are specifically aramid precipitated fibers with a length range of 0.5-3.0 mm, a diameter range of 10-20 μm, and a modulus ≥100 GPa. S2. The activated mixed fibers obtained in S1 are fed into a carding machine and carded into single fibers by a cylinder and a doffer. The fibers are then laid up by a cross-laying machine to form a fiber web. The fiber web is then passed through a low-pressure hydroentanglement zone and pre-entangled and reinforced by a hydroentanglement head at a hydroentanglement pressure of 45 bar to obtain a fiber web substrate. S3. The fiber web substrate obtained in S2 is passed through an impregnation tank containing antibacterial precursor solution at a speed of 2 m / min, and squeezed by a pair of rollers to control its liquid content to 80%; then the impregnated wet fiber web is immediately introduced into an ultraviolet curing chamber filled with high-purity nitrogen gas, using an ultraviolet light-emitting diode array light source with a main wavelength of 365nm, at a light intensity of 120 Irradiated for 3 minutes under the specified conditions to obtain a photocured fiber web; The antibacterial precursor solution was prepared in Preparation Example 1; S4. The photocured fiber web obtained in S3 is sent into a multi-stage high-pressure hydroentanglement reinforcement system. Hydroentanglement is performed under the conditions that the first stage hydroentanglement pressure is 80 bar, the second and third stage hydroentanglement pressures are increased to 120 bar, and the hydroentangled web conveying speed is 4 m / min. Then, it is dried at a temperature of 110℃ to obtain a non-woven fabric substrate. S5. The nonwoven fabric substrate obtained in S4 is wrapped on a rotating drum receiver. The mixed spinning solution is injected into an electrospinning device and continuously spun for 30 minutes at a voltage of 200V, a spinneret distance of 15cm, a drum speed of 100r / min, and a relative humidity of 30%. Then the substrate is transferred into a vapor deposition chamber, perfluorooctyltriethoxysilane vapor is introduced, and it is treated at a temperature of 120℃ for 5 minutes to obtain the treated nonwoven fabric substrate. The mixed spinning solution is composed of thermoplastic polyurethane particles, N,N-dimethylformamide solvent, quaternized chitosan, and deionized water in a weight ratio of 8.5:91.15:0.2:9.8. S6. The nonwoven fabric substrate obtained in S5 is subjected to instantaneous light-setting and shaping treatment through a hot rolling mill at an upper roll temperature of 150℃, a lower roll temperature of 145℃, a linear pressure of 1MPa, and a rolling speed of 10m / min. After cooling, edge trimming, and winding, antibacterial nonwoven fabric is obtained.
[0023] Table: Components and their mass ratios (g) of the raw materials used in Preparation Examples 10-14 Preparation Example 15 An antibacterial nonwoven fabric, which differs from preparation example 10 in that its preparation method is as follows: S1. Polyester and nylon fibers are fed into an opening machine for initial opening, followed by the addition of aramid precipitated fibers. The mixed fibers are placed in a low-temperature plasma treatment device, and a mixed gas is introduced as the treatment atmosphere. The mixture is continuously treated at a radio frequency power of 250W for 60s to obtain surface-activated modified mixed fibers. S2. The activated mixed fibers obtained in S1 are fed into a carding machine and carded into single fibers by a cylinder and a doffer. The fibers are then laid up by a cross-laying machine to form a fiber web. The fiber web is then passed through a low-pressure hydroentanglement zone and pre-entangled and reinforced by a hydroentanglement head at a hydroentanglement pressure of 45 bar to obtain a fiber web substrate. S3. The fiber web substrate obtained in S2 is passed through an impregnation tank containing antibacterial precursor solution at a speed of 2 m / min, and squeezed by a pair of rollers to control its liquid content to 80%; then the impregnated wet fiber web is immediately introduced into an ultraviolet curing chamber filled with high-purity nitrogen gas, using an ultraviolet light-emitting diode array light source with a main wavelength of 365nm, at a light intensity of 120 Irradiated for 3 minutes under the specified conditions to obtain a photocured fiber web; S4. The photocured fiber web obtained in S3 is sent into a multi-stage high-pressure hydroentanglement reinforcement system. Hydroentanglement is performed under the conditions that the first stage hydroentanglement pressure is 80 bar, the second and third stage hydroentanglement pressures are increased to 120 bar, and the hydroentangled web conveying speed is 4 m / min. Then, it is dried at a temperature of 110℃ to obtain a non-woven fabric substrate. S5. The nonwoven fabric substrate obtained in S4 is wrapped on a rotating drum receiver. The mixed spinning solution is injected into an electrospinning device and continuously spun for 30 minutes at a voltage of 200V, a spinneret distance of 15cm, a drum speed of 100r / min, and a relative humidity of 30%. Then the substrate is transferred into a vapor deposition chamber, perfluorooctyltriethoxysilane vapor is introduced, and it is treated at a temperature of 120℃ for 5 minutes to obtain the treated nonwoven fabric substrate. S6. The nonwoven fabric substrate obtained in S5 is subjected to instantaneous light-setting and shaping treatment through a hot rolling mill at an upper roll temperature of 150℃, a lower roll temperature of 145℃, a linear pressure of 1MPa, and a rolling speed of 10m / min. After cooling, edge trimming, and winding, antibacterial nonwoven fabric is obtained.
[0024] Preparation Example 16 An antibacterial nonwoven fabric, which differs from preparation example 10 in that its preparation method is as follows: S1. Polyester and nylon fibers are fed into an opening machine for initial opening, followed by the addition of aramid precipitated fibers. The mixed fibers are placed in a low-temperature plasma treatment device, and a mixed gas is introduced as the treatment atmosphere. The mixture is continuously treated at a radio frequency power of 450W for 120s to obtain surface-activated modified mixed fibers. S2. The activated mixed fibers obtained in S1 are fed into a carding machine and carded into single fibers by a cylinder and a doffer. The fibers are then laid up by a cross-laying machine to form a fiber web. The fiber web is then passed through a low-pressure hydroentanglement zone and pre-entangled and reinforced by a hydroentanglement head at a hydroentanglement pressure of 45 bar to obtain a fiber web substrate. S3. The fiber web substrate obtained in S2 is passed through an impregnation tank containing antibacterial precursor solution at a speed of 2 m / min, and squeezed by a pair of rollers to control its liquid content to 80%; then the impregnated wet fiber web is immediately introduced into an ultraviolet curing chamber filled with high-purity nitrogen gas, using an ultraviolet light-emitting diode array light source with a main wavelength of 365nm, at a light intensity of 120 Irradiated for 3 minutes under the specified conditions to obtain a photocured fiber web; S4. The photocured fiber web obtained in S3 is sent into a multi-stage high-pressure hydroentanglement reinforcement system. Hydroentanglement is performed under the conditions that the first stage hydroentanglement pressure is 80 bar, the second and third stage hydroentanglement pressures are increased to 120 bar, and the hydroentangled web conveying speed is 4 m / min. Then, it is dried at a temperature of 110℃ to obtain a non-woven fabric substrate. S5. The nonwoven fabric substrate obtained in S4 is wrapped on a rotating drum receiver. The mixed spinning solution is injected into an electrospinning device and continuously spun for 30 minutes at a voltage of 200V, a spinneret distance of 15cm, a drum speed of 100r / min, and a relative humidity of 30%. Then the substrate is transferred into a vapor deposition chamber, perfluorooctyltriethoxysilane vapor is introduced, and it is treated at a temperature of 120℃ for 5 minutes to obtain the treated nonwoven fabric substrate. S6. The nonwoven fabric substrate obtained in S5 is subjected to instantaneous light-setting and shaping treatment through a hot rolling mill at an upper roll temperature of 150℃, a lower roll temperature of 145℃, a linear pressure of 1MPa, and a rolling speed of 10m / min. After cooling, edge trimming, and winding, antibacterial nonwoven fabric is obtained.
[0025] Preparation Example 17 An antibacterial nonwoven fabric, which differs from preparation example 10 in that its preparation method is as follows: S1. Polyester and nylon fibers are fed into an opening machine for initial opening, followed by the addition of aramid precipitated fibers. The mixed fibers are placed in a low-temperature plasma treatment device, and a mixed gas is introduced as the treatment atmosphere. The mixture is continuously treated at a radio frequency power of 350W for 90 seconds to obtain surface-activated modified mixed fibers. S2. The activated mixed fibers obtained in S1 are fed into a carding machine and carded into single fibers by a cylinder and a doffer. The fibers are then laid up by a cross-laying machine to form a fiber web. The fiber web is then passed through a low-pressure hydroentanglement zone and pre-entangled and reinforced by a hydroentanglement head at a hydroentanglement pressure of 45 bar to obtain a fiber web substrate. S3. The fiber web substrate obtained in S2 is passed through an impregnation tank containing antibacterial precursor solution at a speed of 2 m / min, and squeezed by a pair of rollers to control its liquid content to 80%; then the impregnated wet fiber web is immediately introduced into an ultraviolet curing chamber filled with high-purity nitrogen, using an ultraviolet light-emitting diode array light source with a main wavelength of 365 nm and a light intensity of 80. Irradiated for 2 minutes under the specified conditions to obtain a photocured fiber web; S4. The photocured fiber web obtained in S3 is sent into a multi-stage high-pressure hydroentanglement reinforcement system. Hydroentanglement is performed under the conditions that the first stage hydroentanglement pressure is 80 bar, the second and third stage hydroentanglement pressures are increased to 120 bar, and the hydroentangled web conveying speed is 4 m / min. Then, it is dried at a temperature of 110℃ to obtain a non-woven fabric substrate. S5. The nonwoven fabric substrate obtained in S4 is wrapped on a rotating drum receiver. The mixed spinning solution is injected into an electrospinning device and continuously spun for 30 minutes at a voltage of 200V, a spinneret distance of 15cm, a drum speed of 100r / min, and a relative humidity of 30%. Then the substrate is transferred into a vapor deposition chamber, perfluorooctyltriethoxysilane vapor is introduced, and it is treated at a temperature of 120℃ for 5 minutes to obtain the treated nonwoven fabric substrate. S6. The nonwoven fabric substrate obtained in S5 is subjected to instantaneous light-setting and shaping treatment through a hot rolling mill at an upper roll temperature of 150℃, a lower roll temperature of 145℃, a linear pressure of 1MPa, and a rolling speed of 10m / min. After cooling, edge trimming, and winding, antibacterial nonwoven fabric is obtained.
[0026] Preparation Example 18 An antibacterial nonwoven fabric, which differs from preparation example 10 in that its preparation method is as follows: S1. Polyester and nylon fibers are fed into an opening machine for initial opening, followed by the addition of aramid precipitated fibers. The mixed fibers are placed in a low-temperature plasma treatment device, and a mixed gas is introduced as the treatment atmosphere. The mixture is continuously treated at a radio frequency power of 350W for 90 seconds to obtain surface-activated modified mixed fibers. S2. The activated mixed fibers obtained in S1 are fed into a carding machine and carded into single fibers by a cylinder and a doffer. The fibers are then laid up by a cross-laying machine to form a fiber web. The fiber web is then passed through a low-pressure hydroentanglement zone and pre-entangled and reinforced by a hydroentanglement head at a hydroentanglement pressure of 45 bar to obtain a fiber web substrate. S3. The fiber web substrate obtained in S2 is passed through an impregnation tank containing antibacterial precursor solution at a speed of 2 m / min, and squeezed by a pair of rollers to control its liquid content to 80%; then the impregnated wet fiber web is immediately introduced into an ultraviolet curing chamber filled with high-purity nitrogen gas, using an ultraviolet light-emitting diode array light source with a main wavelength of 365nm, at a light intensity of 150 Under the condition of irradiation for 5 minutes, a photocured fiber web was obtained; S4. The photocured fiber web obtained in S3 is sent into a multi-stage high-pressure hydroentanglement reinforcement system. Hydroentanglement is performed under the conditions that the first stage hydroentanglement pressure is 80 bar, the second and third stage hydroentanglement pressures are increased to 120 bar, and the hydroentangled web conveying speed is 4 m / min. Then, it is dried at a temperature of 110℃ to obtain a non-woven fabric substrate. S5. The nonwoven fabric substrate obtained in S4 is wrapped on a rotating drum receiver. The mixed spinning solution is injected into an electrospinning device and continuously spun for 30 minutes at a voltage of 200V, a spinneret distance of 15cm, a drum speed of 100r / min, and a relative humidity of 30%. Then the substrate is transferred into a vapor deposition chamber, perfluorooctyltriethoxysilane vapor is introduced, and it is treated at a temperature of 120℃ for 5 minutes to obtain the treated nonwoven fabric substrate. S6. The nonwoven fabric substrate obtained in S5 is subjected to instantaneous light-setting and shaping treatment through a hot rolling mill at an upper roll temperature of 150℃, a lower roll temperature of 145℃, a linear pressure of 1MPa, and a rolling speed of 10m / min. After cooling, edge trimming, and winding, antibacterial nonwoven fabric is obtained.
[0027] Preparation Example 19 An antibacterial nonwoven fabric, which differs from preparation example 10 in that its preparation method is as follows: S1. Polyester and nylon fibers are fed into an opening machine for initial opening, followed by the addition of aramid precipitated fibers. The mixed fibers are placed in a low-temperature plasma treatment device, and a mixed gas is introduced as the treatment atmosphere. The mixture is continuously treated at a radio frequency power of 350W for 90 seconds to obtain surface-activated modified mixed fibers. S2. The activated mixed fibers obtained in S1 are fed into a carding machine and carded into single fibers by a cylinder and a doffer. The fibers are then laid up by a cross-laying machine to form a fiber web. The fiber web is then passed through a low-pressure hydroentanglement zone and pre-entangled and reinforced by a hydroentanglement head at a hydroentanglement pressure of 45 bar to obtain a fiber web substrate. S3. The fiber web substrate obtained in S2 is passed through an impregnation tank containing antibacterial precursor solution at a speed of 2 m / min, and squeezed by a pair of rollers to control its liquid content to 80%; then the impregnated wet fiber web is immediately introduced into an ultraviolet curing chamber filled with high-purity nitrogen gas, using an ultraviolet light-emitting diode array light source with a main wavelength of 365nm, at a light intensity of 120 Irradiated for 3 minutes under the specified conditions to obtain a photocured fiber web; S4. The photocured fiber web obtained in S3 is sent into a multi-stage high-pressure hydroentanglement reinforcement system. Hydroentanglement is performed under the conditions that the first stage hydroentanglement pressure is 80 bar, the second and third stage hydroentanglement pressures are increased to 120 bar, and the hydroentangled web conveying speed is 4 m / min. Then, it is dried at a temperature of 110℃ to obtain a non-woven fabric substrate. S5. The nonwoven fabric substrate obtained in S4 is wrapped on a rotating drum receiver. The mixed spinning solution is injected into an electrospinning device and continuously spun for 30 minutes at a voltage of 150V, a spinneret distance of 15cm, a drum speed of 100r / min, and a relative humidity of 30%. Then the substrate is transferred into a vapor deposition chamber, perfluorooctyltriethoxysilane vapor is introduced, and it is treated at a temperature of 100℃ for 3 minutes to obtain the treated nonwoven fabric substrate. S6. The nonwoven fabric substrate obtained in S5 is subjected to instantaneous light-setting and shaping treatment through a hot rolling mill at an upper roll temperature of 150℃, a lower roll temperature of 145℃, a linear pressure of 1MPa, and a rolling speed of 10m / min. After cooling, edge trimming, and winding, antibacterial nonwoven fabric is obtained.
[0028] Preparation Example 20 An antibacterial nonwoven fabric, which differs from preparation example 10 in that its preparation method is as follows: S1. Polyester and nylon fibers are fed into an opening machine for initial opening, followed by the addition of aramid precipitated fibers. The mixed fibers are placed in a low-temperature plasma treatment device, and a mixed gas is introduced as the treatment atmosphere. The mixture is continuously treated at a radio frequency power of 350W for 90 seconds to obtain surface-activated modified mixed fibers. S2. The activated mixed fibers obtained in S1 are fed into a carding machine and carded into single fibers by a cylinder and a doffer. The fibers are then laid up by a cross-laying machine to form a fiber web. The fiber web is then passed through a low-pressure hydroentanglement zone and pre-entangled and reinforced by a hydroentanglement head at a hydroentanglement pressure of 45 bar to obtain a fiber web substrate. S3. The fiber web substrate obtained in S2 is passed through an impregnation tank containing antibacterial precursor solution at a speed of 2 m / min, and squeezed by a pair of rollers to control its liquid content to 80%; then the impregnated wet fiber web is immediately introduced into an ultraviolet curing chamber filled with high-purity nitrogen gas, using an ultraviolet light-emitting diode array light source with a main wavelength of 365nm, at a light intensity of 120 Irradiated for 3 minutes under the specified conditions to obtain a photocured fiber web; S4. The photocured fiber web obtained in S3 is sent into a multi-stage high-pressure hydroentanglement reinforcement system. Hydroentanglement is performed under the conditions that the first stage hydroentanglement pressure is 80 bar, the second and third stage hydroentanglement pressures are increased to 120 bar, and the hydroentangled web conveying speed is 4 m / min. Then, it is dried at a temperature of 110℃ to obtain a non-woven fabric substrate. S5. The nonwoven fabric substrate obtained in S4 is wrapped on a rotating drum receiver. The mixed spinning solution is injected into an electrospinning device and continuously spun for 30 minutes at a voltage of 250V, a spinneret distance of 15cm, a drum speed of 100r / min, and a relative humidity of 30%. Then the substrate is transferred into a vapor deposition chamber, perfluorooctyltriethoxysilane vapor is introduced, and it is treated at a temperature of 140℃ for 8 minutes to obtain the treated nonwoven fabric substrate. S6. The nonwoven fabric substrate obtained in S5 is subjected to instantaneous light-setting and shaping treatment through a hot rolling mill at an upper roll temperature of 150℃, a lower roll temperature of 145℃, a linear pressure of 1MPa, and a rolling speed of 10m / min. After cooling, edge trimming, and winding, antibacterial nonwoven fabric is obtained.
[0029] Preparation Example 21 An antibacterial nonwoven fabric, which differs from Preparation Example 10, is provided in that the mixed spinning solution is composed of thermoplastic polyurethane particles, N,N-dimethylformamide solvent, quaternized chitosan, and deionized water in a weight ratio of 7.2:92.0:0.8:9.2.
[0030] Preparation Example 22 An antibacterial nonwoven fabric, which differs from Preparation Example 10, is provided in that the mixed spinning solution is composed of thermoplastic polyurethane particles, N,N-dimethylformamide solvent, quaternized chitosan, and deionized water in a weight ratio of 7.8:91.82:0.5:9.5.
[0031] Preparation Examples 23-30 An antibacterial nonwoven fabric differs from Preparation Example 10 in that the antibacterial precursor liquid used in its components is used differently, as shown in the table below.
[0032] Table: Comparison of the use of antibacterial precursor solutions in Preparation Examples 23-30 Performance testing The antibacterial nonwoven fabrics prepared in each embodiment were selected for testing. The test subjects were 210 samples of antibacterial nonwoven fabrics, with 10 samples in each group. Their physical properties, antibacterial properties, and intelligent response function were tested. The specific testing steps are as follows: Physical properties: First, samples were taken from the antibacterial nonwoven fabric prepared in the examples. Using the strip method, the samples and pure fiber nonwoven fabric were stretched to break on a constant speed elongation testing machine under conditions of 50 mm width, 200 mm clamping distance, and 100 mm / min. The breaking strength was tested, and the breaking strength retention rate was calculated to characterize the physical properties of the antibacterial nonwoven fabric. The test results and evaluation criteria are as follows: Fracture strength retention rate > 90% (considered as having strong physical properties); Fracture strength retention rate <90% (considered as weak physical properties).
[0033] Antibacterial properties: First, samples of the antibacterial nonwoven fabric prepared in the examples were taken and subjected to 20 standard simulated washes under A1M conditions. The antibacterial rate against Staphylococcus aureus was then determined using the shaking method to characterize the antibacterial performance of the nonwoven fabric. The test results and evaluation criteria are as follows: Antibacterial rate > 90% (considered as having strong antibacterial properties); Antibacterial rate <90% (considered as weak antibacterial performance).
[0034] Smart Response Feature: First, samples of the antibacterial nonwoven fabric prepared in the examples were taken and placed in buffer solutions of different pH values for isothermal shaking release. The cumulative release of zinc ions within a specific time window was determined by ICP-MS, and its intelligent release response ratio was calculated; this was used to characterize the basic function of the antibacterial nonwoven fabric; the test results and evaluation criteria are as follows: Smart release response ratio > 3.0 (considered as strong smart response function); A smart release response ratio of <3.0 is considered a weak smart response function.
[0035] It should be specifically noted that the antibacterial nonwoven fabric obtained above is produced using normal production methods. Any defective antibacterial nonwoven fabric produced is disregarded.
[0036] Examples 1-5 The corresponding relationship of the preparation methods used for an antibacterial nonwoven fabric is shown in the table below.
[0037] Table: Comparison of the use of antibacterial nonwoven fabrics in Examples 1-5 Extract the antibacterial nonwoven fabrics from Examples 1-5 above, and test their breaking strength retention rate, antibacterial rate, and intelligent release response ratio according to the above measurement steps and standards. The average value of the test results is recorded in the table below.
[0038] Table: Performance test results of tensile strength retention rate, antibacterial rate, and smart release response ratio in Examples 1-5 As can be seen from the table above, the antibacterial nonwoven fabric preparation processes in Examples 1-5 all effectively improve the production efficiency of antibacterial nonwoven fabrics. Polyester and nylon fibers constitute the main fiber network, providing a rigid skeleton and elastic flexibility respectively, laying the foundation for the material's basic physical properties. Aramid precipitated fibers are dispersed as a reinforcing phase, significantly improving the tear strength and dimensional stability of the nonwoven fabric through their high modulus characteristics. The pH-sensitive polymer, as the wall material of microcapsule A, causes its molecular chains to swell or break in a slightly acidic environment, thereby intelligently regulating the release rate of the silver ion and quaternary ammonium salt composite antibacterial agent, realizing a response mechanism that triggers accelerated release in the infected microenvironment. Microcapsule B uses cationic chitosan as the wall material, which has antibacterial activity and good biocompatibility. It can gently encapsulate and slowly release the composite antibacterial agent of polylysine and zinc-doped zeolite powder. The continuous release of zinc ions and the membrane-breaking effect of polylysine produce a synergistic antibacterial effect. Dimethylaminoethyl methacrylate, as the main monomer of the photosensitive grafting reaction, has double bonds and tertiary amine groups in its molecule under the influence of the photoinitiator diphenylmethyl methacrylate. Under the influence of ketones, free radical polymerization and grafting occur on the fiber surface, forming a robust polymer coating. Simultaneously, a pH-sensitive crosslinking agent with double bonds participates in copolymerization, constructing an environmentally responsive three-dimensional network within the coating. This not only firmly fixes the two types of intelligent microcapsules through a dual mechanism of chemical bonding and physical encapsulation, preventing physical loss, but also endows the entire functional layer with release regulation capabilities. The resulting antibacterial precursor solution, after UV curing, is then driven by the physical energy of high-pressure hydroentangling, causing unreacted monomers to undergo deep secondary crosslinking at the fiber interlacing points. This achieves a high degree of integration between the functional layer and the substrate in three-dimensional space, fundamentally ensuring functional durability. Finally, the thermoplastic polyurethane in the mixed spinning solution forms a continuous and tough nanofiber framework, while quaternized chitosan endows it with rapid contact sterilization capabilities. The nanofiber membrane formed by the co-spun materials is then modified by vapor deposition, constructing a biomimetic barrier surface that is internally hydrophilic and antibacterial, and externally superhydrophobic, comprehensively enhancing the material's immediate protection and anti-pollution capabilities. This achieves the goal of improving the production efficiency of antibacterial nonwoven fabrics. Its tensile strength retention rate is 92.6-98.8%, which is considered to be strong physical properties; its antibacterial rate is 91.2-95.2%, which is considered to be strong antibacterial properties; and its intelligent release response ratio is 3.8-4.7, which is considered to be strong intelligent response function. It is evident that, given a fixed amount of raw materials, the production effect of antibacterial nonwoven fabric can be increased by adjusting the proportions of the raw materials. Based on the data in the table above, it is clear that the antibacterial nonwoven fabric prepared using 45 parts polyester fiber, 35 parts nylon fiber, and 20 parts aramid precipitated fiber exhibits the strongest physical properties. This is because the high proportion of aramid precipitated fiber forms a continuous and dense reinforcing network skeleton. The excellent specific strength and high modulus of aramid fiber make it the main stress-bearing unit in the fiber web, effectively distributing and dispersing the load under stress, thereby greatly improving the overall breaking strength and tear resistance of the nonwoven fabric. Simultaneously, polyester fiber, as a rigid matrix, provides stable structural support, while nylon fiber, with its good toughness, acts as a buffer and toughening agent, exhibiting the strongest physical and mechanical properties, as shown in Examples 1-5.
[0039] It is evident that, given a fixed amount of raw materials, the production effect of antibacterial nonwoven fabric can be increased by adjusting the proportion of raw materials used in preparation. Based on the data in the table above, it is clear that the antibacterial nonwoven fabric prepared using 50 parts polyester fiber, 40 parts nylon fiber, and 10 parts aramid precipitated fiber exhibits the strongest antibacterial performance and intelligent response function. This is because the high proportion of nylon fiber significantly enhances the surface polarity and chemical reactivity of the fiber aggregate. The abundant polar amide groups in the nylon molecular chain provide more active sites for subsequent photografting polymerization reactions, enabling the functional monomers and crosslinking agents in the antibacterial precursor solution to form a more uniform, dense, and firmly bonded intelligent polymer network on the fiber surface. This network not only chemically encapsulates pH-responsive antibacterial microcapsules, greatly inhibiting loss during use and ensuring long-lasting antibacterial efficacy, but its own stereo-responsive structure can more sensitively sense changes in environmental acidity and alkalinity and precisely regulate the release behavior of antibacterial factors, as obtained from Examples 1-5.
[0040] Examples 14-21 The corresponding relationship of the preparation methods used for an antibacterial nonwoven fabric is shown in the table below.
[0041] Table: Comparison of Antibacterial Nonwoven Fabric Usage in Examples 14-21 Extract the antibacterial nonwoven fabrics from Examples 14-21 above, and test their tensile strength retention rate, antibacterial rate, and intelligent release response ratio according to the above measurement steps and standards. The average value of the test results is recorded in the table below.
[0042] Table: Performance test results of tensile strength retention rate, antibacterial rate, and smart release response ratio in Examples 1, 14-21 As can be seen from the table above, the antibacterial nonwoven fabric preparation processes in Examples 1 and 14-21 all effectively improve the production efficiency of antibacterial nonwoven fabrics. Polyester and nylon fibers constitute the main fiber network, providing a rigid skeleton and elastic flexibility respectively, laying the foundation for the basic physical properties of the material. Aramid precipitated fibers are dispersed as a reinforcing phase, significantly improving the tear strength and dimensional stability of the nonwoven fabric through their high modulus characteristics. The pH-sensitive polymer is used as the wall material of microcapsule A. Its molecular chains swell or break in a slightly acidic environment, thereby intelligently regulating the release rate of the silver ion and quaternary ammonium salt composite antibacterial agent, realizing the response mechanism of accelerated release triggered by the infection microenvironment. Microcapsule B uses cationic chitosan as the wall material. It has antibacterial activity and good biocompatibility, and can gently encapsulate and slowly release the composite antibacterial agent of polylysine and zinc-doped zeolite powder. The continuous release of zinc ions and the membrane-breaking effect of polylysine produce a synergistic antibacterial effect. Dimethylaminoethyl methacrylate is the main monomer of the photosensitive grafting reaction. The double bond and tertiary amine group in its molecule are activated by the photoinitiator. Benzophenone facilitates free radical polymerization and grafting on the fiber surface, forming a robust polymer coating. Simultaneously, a pH-sensitive crosslinking agent with double bonds participates in copolymerization, constructing an environmentally responsive three-dimensional network within the coating. This not only firmly fixes the two types of intelligent microcapsules through a dual mechanism of chemical bonding and physical encapsulation, preventing physical loss, but also endows the entire functional layer with release regulation capabilities. The resulting antibacterial precursor solution, after UV curing, is then driven by the physical energy of high-pressure hydroentangling, causing unreacted monomers to undergo deep secondary crosslinking at the fiber interlacing points. This achieves a high degree of integration between the functional layer and the substrate in three-dimensional space, fundamentally ensuring functional durability. Finally, the thermoplastic polyurethane in the mixed spinning solution forms a continuous and tough nanofiber framework, while quaternized chitosan endows it with rapid contact sterilization capabilities. The nanofiber membrane formed by the co-spun nanofibers is then modified by vapor deposition, constructing a biomimetic barrier surface that is internally hydrophilic and antibacterial, and externally superhydrophobic, comprehensively enhancing the material's immediate protection and anti-fouling capabilities. This achieves the goal of improving the production efficiency of antibacterial nonwoven fabrics. Its tensile strength retention rate is 93.3-95.9%, which is considered to be strong physical properties; its antibacterial rate is 94.0-96.2%, which is considered to be strong antibacterial properties; and its intelligent release response ratio is 4.0-4.5, which is considered to be strong intelligent response function. It is evident that, given a fixed amount of raw materials, the production effect of antibacterial nonwoven fabrics can be increased by adjusting the preparation conditions. Based on the data in the table above, it is clear that when preparing antibacterial nonwoven fabrics, increasing the radio frequency power and duration of the fiber pretreatment process, the light intensity and duration of the photografting process, and the applied voltage, deposition temperature, and duration of the electrospinning process all result in the physical properties, antibacterial properties, and intelligent response function of the prepared antibacterial nonwoven fabric initially becoming stronger and then weaker. Specifically, the fiber pretreatment process at a radio frequency power of 350W for 90s, and the photografting process at a light intensity of 120W... Irradiation for 3 minutes under the following conditions, electrospinning at 200V, and vapor deposition at 120℃ for 5 minutes resulted in the antibacterial nonwoven fabric exhibiting the strongest physical properties, antibacterial properties, and intelligent response function. The reason for this is that the appropriate radio frequency power and processing time are sufficient to generate a large number of oxygen- and nitrogen-containing active free radicals and polar groups on the surface of polyester, nylon, and aramid fibers through plasma bombardment, providing sufficient and uniform reaction sites for subsequent photografting. Excessive power or excessive time would lead to excessive etching of the fiber surface or even damage to the fiber itself, thus weakening the substrate strength. Within this optimized window, the light intensity and duration of the photografting stage ensure that the photoinitiator benzophenone effectively decomposes to generate sufficient free radicals, driving the dimethylaminoethyl methacrylate monomer and crosslinking agent to undergo sufficient and deep graft copolymerization at the active sites of the fiber, forming a smart polymer layer of moderate thickness and uniform crosslinking network. The antibacterial microcapsules are firmly embedded and achieve excellent pH responsiveness. If the light intensity is too low or the time is too short, the grafting layer will be incomplete and the function will be weak. If the light intensity is too high or the time is too long, it may cause excessive cross-linking and brittleness of the surface polymer or homopolymerization of the monomer, reducing the interfacial bonding force and response sensitivity. The voltage used in the electrospinning process can form a sufficiently strong and stable electric field between the spinneret and the receiving roller, which promotes the full stretching of the mixed spinning solution to form a uniform diameter, continuous and dense nanofiber membrane with good adhesion to the substrate, providing a high specific surface area loading platform for quaternized chitosan. The subsequent vapor deposition temperature can enable the perfluorooctyltriethoxysilane molecules to have sufficient kinetic energy and reactivity, so that they can be fully spread on the nanofiber surface and chemically bonded to form a low surface energy modification layer, achieving long-lasting superhydrophobic properties. However, if the temperature is too low, the reaction will be incomplete, and if it is too high, it may cause silane decomposition or nanofiber deformation, as obtained from Examples 1 and 6-11.
[0043] It is evident that, given a fixed amount of raw materials, the production effect of antibacterial nonwoven fabrics can be increased by adjusting the preparation conditions. Based on the data in the table above, it is clear that when preparing antibacterial nonwoven fabrics, the mixed spinning solution prepared with 8.5 parts thermoplastic polyurethane particles, 91.15 parts N,N-dimethylformamide solvent, 0.2 parts quaternized chitosan, and 9.8 parts deionized water yields the antibacterial nonwoven fabric with the strongest physical properties and intelligent response function. This is because the higher proportion of thermoplastic polyurethane ensures that the spinning solution has excellent fiber-forming properties, enabling the formation of a continuous, uniform, dense, and mechanically strong nanofiber film during electrospinning, thus improving the material's properties. The overall mechanical properties effectively protect the underlying intelligent antibacterial functional layer constructed through photografting technology, preventing it from being damaged by external mechanical friction and physical erosion. At the same time, the relatively low quaternized chitosan content avoids excessive swelling or loose structure of the nanofiber membrane due to the introduction of too many hydrophilic components, thus maintaining the stable physical barrier function of the film. This stable and dense surface structure provides a protected and controllable microenvironment for the underlying pH-sensitive polymer network and microcapsules, enabling the intelligent antibacterial system to more accurately sense changes in environmental acidity and alkalinity and perform controlled release without being disturbed by unstable factors on the surface, as obtained in Examples 1 and 12-13.
[0044] It is evident that, given a fixed amount of raw materials, the production effect of antibacterial nonwoven fabric can be increased by adjusting the preparation conditions. Based on the data in the table above, it is clear that the antibacterial nonwoven fabric prepared using a mixed spinning solution consisting of 7.2 parts thermoplastic polyurethane particles, 92.0 parts N,N-dimethylformamide solvent, 0.8 parts quaternized chitosan, and 9.2 parts deionized water exhibits the strongest antibacterial properties. This is because the significantly increased relative content of quaternized chitosan allows it to accumulate in the nanofiber membrane formed by electrospinning and be fully exposed on the fiber surface. These surface-enriched quaternized chitosan molecules carry high density... The positive charge can quickly capture and firmly bind to the cell membranes of negatively charged bacteria and other microorganisms through strong electrostatic adsorption, thereby effectively destroying their membrane structure, causing leakage of cell contents and death, thus giving the nonwoven fabric surface a strong contact killing ability; at the same time, the appropriately reduced proportion of thermoplastic polyurethane ensures that the viscosity of the spinning solution is suitable, so that the high content of quaternized chitosan can still be smoothly fiberized and evenly distributed, avoiding the impact of excessive agglomeration on the function. This strong antibacterial mechanism dominated by rapid contact killing on the surface, together with the underlying intelligent slow-release antibacterial system, forms a highly efficient complement and dual guarantee, as obtained from Examples 1 and 12-13.
[0045] Examples 14-21 The corresponding relationship of the preparation methods used for an antibacterial nonwoven fabric is shown in the table below.
[0046] Table: Comparison of Antibacterial Nonwoven Fabric Usage in Examples 14-21 Extract the antibacterial nonwoven fabrics from Examples 14-21 above, and test their tensile strength retention rate, antibacterial rate, and intelligent release response ratio according to the above measurement steps and standards. The average value of the test results is recorded in the table below.
[0047] Table: Performance test results of tensile strength retention rate, antibacterial rate, and smart release response ratio in Examples 1, 14-21 As can be seen from the table above, the antibacterial nonwoven fabric preparation processes in Examples 1 and 14-21 all effectively improve the production efficiency of antibacterial nonwoven fabrics. Polyester and nylon fibers constitute the main fiber network, providing a rigid skeleton and elastic flexibility respectively, laying the foundation for the basic physical properties of the material. Aramid precipitated fibers are dispersed as a reinforcing phase, significantly improving the tear strength and dimensional stability of the nonwoven fabric through their high modulus characteristics. The pH-sensitive polymer is used as the wall material of microcapsule A. Its molecular chains swell or break in a slightly acidic environment, thereby intelligently regulating the release rate of the silver ion and quaternary ammonium salt composite antibacterial agent, realizing the response mechanism of accelerated release triggered by the infection microenvironment. Microcapsule B uses cationic chitosan as the wall material. It has antibacterial activity and good biocompatibility, and can gently encapsulate and slowly release the composite antibacterial agent of polylysine and zinc-doped zeolite powder. The continuous release of zinc ions and the membrane-breaking effect of polylysine produce a synergistic antibacterial effect. Dimethylaminoethyl methacrylate is the main monomer of the photosensitive grafting reaction. The double bond and tertiary amine group in its molecule are activated by the photoinitiator. Benzophenone facilitates free radical polymerization and grafting on the fiber surface, forming a robust polymer coating. Simultaneously, a pH-sensitive crosslinking agent with double bonds participates in copolymerization, constructing an environmentally responsive three-dimensional network within the coating. This not only firmly fixes the two types of intelligent microcapsules through a dual mechanism of chemical bonding and physical encapsulation, preventing physical loss, but also endows the entire functional layer with release regulation capabilities. The resulting antibacterial precursor solution, after UV curing, is then driven by the physical energy of high-pressure hydroentangling, causing unreacted monomers to undergo deep secondary crosslinking at the fiber interlacing points. This achieves a high degree of integration between the functional layer and the substrate in three-dimensional space, fundamentally ensuring functional durability. Finally, the thermoplastic polyurethane in the mixed spinning solution forms a continuous and tough nanofiber framework, while quaternized chitosan endows it with rapid contact sterilization capabilities. The nanofiber membrane formed by the co-spun nanofibers is then modified by vapor deposition, constructing a biomimetic barrier surface that is internally hydrophilic and antibacterial, and externally superhydrophobic, comprehensively enhancing the material's immediate protection and anti-fouling capabilities. This achieves the goal of improving the production efficiency of antibacterial nonwoven fabrics. Its tensile strength retention rate is 92.7-96.7%, which is considered to be strong physical properties; its antibacterial rate is 91.8-95.2%, which is considered to be strong antibacterial properties; and its intelligent release response ratio is 3.6-4.8, which is considered to be strong intelligent response function. It is evident that when the raw materials are constant, the production effect of antibacterial nonwoven fabric can be increased by adjusting the proportions of the raw materials. Based on the data in the table above, it is clear that when preparing the antibacterial precursor solution, the antibacterial nonwoven fabric prepared using 12 parts of a pH-sensitive polymer, 12 parts of a composite antibacterial agent, 10 parts of polylysine, 10 parts of zinc-doped zeolite powder, 10 parts of cationic chitosan, 100 parts of dimethylaminoethyl methacrylate, 15 parts of a crosslinking agent, and 1.15 parts of benzophenone exhibits the strongest physical properties, antibacterial performance, and intelligent response function. This is because the high proportion of silver ion composite antibacterial agent reacts with polylysine and zinc-doped zeolite powder to form an inorganic... The potent antibacterial combination of synergistic and complementary mechanisms ensures ample antibacterial agent reserves and broad-spectrum, highly efficient bactericidal potential. The high proportion of crosslinking agent, under photoinitiation, promotes the formation of an extremely dense and robust three-dimensional polymer network of dimethylaminoethyl methacrylate monomers. This network anchors the antibacterial components firmly to the fiber surface through both chemical bonding and physical encapsulation, greatly improving the mechanical strength and washability of the functional layer. This ensures excellent physical property retention and antibacterial durability. Meanwhile, the pH-sensitive units rich in this highly crosslinked network can tightly lock in antibacterial ions under normal conditions to achieve low leakage, as obtained in Examples 1 and 14-17.
[0048] It is evident that, given a fixed amount of raw materials, the production effect of antibacterial nonwoven fabrics can be increased by adjusting the preparation conditions. Based on the data in the table above, it is clear that when preparing the antibacterial precursor solution, increasing the stirring speed and duration during the preparation process, as well as the power and duration of the ultrasonic dispersion process, initially strengthens and then weakens the physical properties, antibacterial properties, and intelligent response function of the prepared antibacterial nonwoven fabric, but the changes are not significant. The antibacterial nonwoven fabric with the strongest physical properties, antibacterial properties, and intelligent response function is obtained when stirring at 45℃ and 600 r / min, and treating with 500W power for 40 min. This is because sufficient but not excessive stirring ensures that the dimethylaminoethyl methacrylate monomer, crosslinking agent, and photoinitiator achieve uniform molecular-level distribution and full activation in the solution, laying the reaction foundation for the subsequent formation of a uniform and appropriately crosslinked intelligent polymer network. Simultaneously, gentle heating promotes… The dissolution process was eliminated while premature polymerization of monomers was avoided. Appropriate ultrasonic power and time were sufficient to overcome the van der Waals forces and electrostatic interactions between microcapsule particles, enabling them to achieve highly monodisperse and stable suspension in the pre-grafted solution. This ensured that during subsequent impregnation and photocuring, the microcapsules were uniformly loaded onto the fiber surface and completely coated by the polymer network, forming a strong and uniform functional composite layer. Insufficient stirring or ultrasonic intensity could lead to uneven solution or microcapsule aggregation, resulting in discontinuity in the photografted network and weak microcapsule fixation, ultimately weakening the overall performance of the material. Conversely, excessive stirring or prolonged ultrasonic time and power could cause local prepolymerization of monomers, abnormally high solution viscosity, or even damage to the structural integrity or surface properties of the microcapsules, affecting their dispersion stability and bonding strength in the polymer network, leading to defects in the functional layer, as seen in Examples 1 and 18-19.
[0049] It is evident that when the raw materials are fixed, the production effect of antibacterial nonwoven fabric can be increased by adjusting the preparation conditions. Based on the data in the table above, it is easy to see that when the mass fraction of the pre-grafted solution prepared when preparing the antibacterial precursor liquid is 15%, the physical properties, antibacterial properties, and intelligent response function of the obtained antibacterial nonwoven fabric are the strongest, as obtained from Examples 1 and 20-21.
[0050] This specific embodiment is merely an explanation of the present invention and not a limitation thereof. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but as long as they are within the scope of the claims of the present invention, they are protected by patent law.
Claims
1. An antibacterial nonwoven fabric, characterized in that, By weight, the antibacterial nonwoven fabric is prepared from polyester fibers, nylon fibers, and aramid precipitated fibers through web reinforcement, antibacterial precursor solution impregnation and photografting, high-pressure hydroentangling bonding, and electrospinning with a mixed spinning solution. The raw materials for its preparation include: 45-65 parts polyester fiber, 25-40 parts nylon fiber, and 10-20 parts aramid precipitated fiber.
2. The antibacterial nonwoven fabric according to claim 1, characterized in that: The preparation method of the antibacterial precursor solution includes the following steps: C1. Using a microfluidic chip device, a pH-sensitive polymer is used as the wall material to encapsulate a composite antibacterial agent, and capsules A with a particle size distribution of 2 μm are prepared. C2. Microcapsules B with a particle size of 4 μm were prepared by using cationic chitosan as the wall material to encapsulate polylysine and zinc-doped zeolite powder through complex coagulation method. C3. Place the microcapsule A obtained in C1 and the microcapsule B obtained in C2 in a low-speed mixer and mix for 60 min at a speed of 30 r / min to obtain the microcapsule complex. C4. Dimethylaminoethyl methacrylate and a crosslinking agent are dissolved together in deionized water, followed by the addition of benzophenone. The mixture is stirred at 35-45℃ and 400-600 r / min until completely dissolved to prepare a pre-grafted solution. Then, the microcapsule complex obtained in S3 is added, and the mixture is treated with an ultrasonic disperser at 300-500W for 20-40 min to obtain an antibacterial precursor solution.
3. The antibacterial nonwoven fabric according to claim 1, characterized in that: The components and weight proportions of the raw materials for preparing the antibacterial precursor solution are as follows: 12-22 parts of pH-sensitive polymer, 5-12 parts of composite antibacterial agent, 5-10 parts of polylysine, 8-15 parts of zinc-doped zeolite powder, 10-20 parts of cationic chitosan, 100 parts of dimethylaminoethyl methacrylate, 8-18 parts of crosslinking agent, and 1.08-1.18 parts of benzophenone.
4. The antibacterial nonwoven fabric according to claim 1, characterized in that: The pH-sensitive polymer is specifically a copolymer of polyacrylic acid and ethylene glycol dimethacrylate. Polylysine is specifically - Polylysine; The crosslinking agent is specifically N,N'-bis(acryloyloxyethyl)ethylenediamine-N,N'-diacetic acid tetrasodium salt.
5. The antibacterial nonwoven fabric according to claim 1, characterized in that: The composite antibacterial agent is prepared by mixing silver sulfadiazine and hexadecyltrimethylammonium bromide in a mass ratio of 1:
2.
6. The antibacterial nonwoven fabric according to claim 4, characterized in that: The zinc-doped zeolite powder contains ZSM-5 type zeolite with a silicon-aluminum molar ratio of 50:1 and a zinc element mass fraction of 5.0%.
7. The antibacterial nonwoven fabric according to claim 1, characterized in that: The pre-grafted solution has a mass fraction of 10-20%.
8. The preparation process of the antibacterial nonwoven fabric according to any one of claims 1-7, characterized in that, The preparation process of the antibacterial nonwoven fabric includes the following steps: S1. Polyester and nylon fibers are fed into an opening machine for initial opening, followed by the addition of aramid precipitated fibers. The mixed fibers are placed in a low-temperature plasma treatment device, and a mixed gas is introduced as the treatment atmosphere. The mixture is continuously treated at a radio frequency power of 250-450W for 60-120s to obtain surface-activated modified mixed fibers. S2. The activated mixed fibers obtained in S1 are fed into a carding machine and carded into single fibers by a cylinder and a doffer. The fibers are then laid up by a cross-laying machine to form a fiber web. The fiber web is then passed through a low-pressure hydroentanglement zone and pre-entangled and reinforced by a hydroentanglement head at a hydroentanglement pressure of 45 bar to obtain a fiber web substrate. S3. The fiber web substrate obtained in S2 is passed through an impregnation tank containing antibacterial precursor solution at a speed of 2 m / min, and squeezed by a pair of rollers to control its liquid content to 80%; then the impregnated wet fiber web is immediately introduced into an ultraviolet curing chamber filled with high-purity nitrogen gas, using an ultraviolet light-emitting diode array light source with a main wavelength of 365nm, at a light intensity of 80-150 nm. Irradiate for 2-5 minutes under the specified conditions to obtain a photocured fiber web; S4. The photocured fiber web obtained in S3 is sent into a multi-stage high-pressure hydroentanglement reinforcement system. Hydroentanglement is performed under the conditions that the first stage hydroentanglement pressure is 80 bar, the second and third stage hydroentanglement pressures are increased to 120 bar, and the hydroentangled web conveying speed is 4 m / min. Then, it is dried at a temperature of 110℃ to obtain a non-woven fabric substrate. S5. The nonwoven fabric substrate obtained in S4 is wrapped on a rotating drum receiver. The mixed spinning solution is injected into an electrospinning device and continuously spun for 30 minutes at a voltage of 150-250V, a spinneret distance of 15cm, a drum speed of 100r / min, and a relative humidity of 30%. Then the substrate is transferred into a vapor deposition chamber, perfluorooctyltriethoxysilane vapor is introduced, and it is treated at a temperature of 100-140℃ for 3-8 minutes to obtain the treated nonwoven fabric substrate. S6. The nonwoven fabric substrate obtained in S5 is subjected to instantaneous light-setting and shaping treatment through a hot rolling mill at an upper roll temperature of 150℃, a lower roll temperature of 145℃, a linear pressure of 1MPa, and a rolling speed of 10m / min. After cooling, edge trimming, and winding, antibacterial nonwoven fabric is obtained.
9. The preparation process of an antibacterial nonwoven fabric according to claim 8, characterized in that: The mixed gas is composed of argon and oxygen in a volume ratio of 9:
1.
10. The preparation process of an antibacterial nonwoven fabric according to claim 8, characterized in that: The mixed spinning solution is composed of thermoplastic polyurethane particles, N,N-dimethylformamide solvent, quaternized chitosan, and deionized water in a weight ratio of 7.2-8.5:91.15-92.0:0.2-0.8:9.2-9.8.