Fiber material with antibacterial function and preparation method thereof

Through an integrated preparation method, titanium source and polymer particles are reacted under high temperature and high pressure to form nano-flower-like TiO2, which solves the problems of complex preparation and poor antibacterial effect of existing antibacterial fiber materials, and realizes the rapid, low-cost preparation of high-efficiency antibacterial fiber materials.

CN118932522BActive Publication Date: 2025-09-16DONGHUA UNIV +1
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Patent Information

Application Number
CN202411224059.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-02
Publication Date
2025-09-16
Estimated Expiration
2044-09-02

AI Technical Summary

Technical Problem

The preparation process of existing antibacterial fiber materials is complicated, time-consuming and labor-intensive, and has poor antibacterial effect.

Method used

An integrated preparation method is adopted to mix titanium source, alkyl alcohol solvent, chemical reactants, cosolvent and polymer particles, and react them under high temperature and high pressure conditions to form nanoflower-like TiO2, and then the antibacterial fiber material is prepared through a spinning process.

Benefits of technology

The rapid preparation of antibacterial fiber materials is achieved, which reduces production costs and time, while improving antibacterial properties and durability.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides a fiber material with antibacterial function and a preparation method thereof, relating to the technical field of antibacterial materials. The present invention combines multiple processes, such as antibacterial agent synthesis, polymer dissolution, and uniform dispersion of the antibacterial agent in the polymer, into one process, which can be completed in the same reactor. This conveniently utilizes the same solvent to achieve in-situ preparation of the antibacterial agent and polymer dissolution, saving time and effort. The nonwoven material prepared by the present invention has good air permeability of 200 to 400 mm / s, a longitudinal breaking strength of greater than 200 N, and a transverse breaking strength of greater than 150 N. It exhibits excellent antibacterial effects, with an inhibition rate against Escherichia coli, Staphylococcus aureus, and Helicobacter pylori exceeding 99.8%. Its antiviral activity against the RNA virus H1N1 reaches 98.24%.
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Description

Technical Field

[0001] The present invention relates to the technical field of antibacterial materials, and in particular to a fiber material with antibacterial function and a preparation method thereof. Background Art

[0002] In the field of antibacterial materials, protective materials such as masks and protective clothing intercept carriers containing bacteria or viruses outside the body through physical isolation, avoiding physical damage caused by subsequent infection. Protective equipment is currently mainly made of microfiber textile materials, which do not have bactericidal and antiviral properties. Combining antibacterial agents with protective materials is the key to achieving the transformation of protective materials from physical protection to active antibacterial and bactericidal protection. The metal oxide titanium dioxide has the characteristics of stability, low cost, strong heat resistance and semiconductor properties. Under solar radiation, photoelectrons with energy greater than the band gap are captured, generating photogenerated electron and hole pairs with redox properties. The two migrate to the surface of the metal oxide and undergo oxidation or reduction reactions with external water molecules or oxygen to generate active substances. The active substances further react with the bacterial cell wall to kill the bacteria.

[0003] The conventional approach to combining antimicrobial agents with textile materials is to first prepare the antimicrobial agent, and then prepare it into an antimicrobial nonwoven material through physical blending, surface coating, plasma treatment, or post-textile processing. The preparation process is divided into multiple discontinuous steps, which is time-consuming, labor-intensive, and requires multiple sets of equipment. Summary of the Invention

[0004] In view of this, the purpose of the present invention is to provide a fiber material with antibacterial function and a preparation method thereof. The present invention combines multiple steps into one, greatly saving production and labor costs, and the prepared fiber material has the advantages of strong antibacterial properties and long-lasting antibacterial properties.

[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0006] The present invention provides a method for preparing a fiber material with antibacterial function, comprising the following steps:

[0007] A titanium source, an alkyl alcohol solvent, a chemical reactant, a cosolvent, and polymer particles are mixed, and the resulting mixture is heated to 170-200° C. in a sealed and first stirring condition and reacted for 5-10 hours, wherein the titanium source and the alkyl alcohol solvent form a titanium alcohol complex, which is then dehydrated under the action of the chemical reactant to form TiO2; the chemical reactant includes at least one of N,N-dimethylformamide and N,N-dimethylacetamide;

[0008] The obtained reaction system is pressurized to 7-15 MPa, the stirring rate is increased, and a second stirring is performed for 1-1.5 hours. The polymer particles become fluid and impact TiO2 together with the alkyl alcohol solvent to form nanoflower-like TiO2, thereby obtaining a spinning solution. The spinning solution is then ejected through the spinneret by releasing the pressure, and the solvent evaporates to form polymer fibers, thereby obtaining a fiber material with antibacterial function.

[0009] Preferably, the titanium source is one or more of tetrabutyl titanate, titanium tetrachloride and titanium sulfate.

[0010] Preferably, the alkyl alcohol solvent has no more than 5 carbon atoms.

[0011] Preferably, the polymer particles include one or more of polyethylene particles, polypropylene particles, polyester particles and polyamide particles.

[0012] Preferably, the co-solvent comprises at least one of dichloroethane and dichloromethane.

[0013] Preferably, based on 100% of the raw material mass, the titanium source accounts for 5-8%, the chemical reactant accounts for 25-35%, the alkyl alcohol solvent accounts for 30-37%, the cosolvent accounts for 10-15%, and the polymer particles account for 5-30%.

[0014] Preferably, the first stirring rate is 20-40 r / min; the second stirring rate is 100-200 r / min.

[0015] Preferably, the gas used for pressurization is one or more of argon, nitrogen and carbon dioxide.

[0016] Preferably, after the polymer fibers are formed, the process further comprises air-opening the polymer fibers and collecting the opened fibers with a conveyor belt.

[0017] The present invention provides a fiber material with antibacterial function prepared by the preparation method described in the above scheme, which is composed of polymer fibers, and nano-flower-shaped TiO2 is distributed on the surface of the polymer fibers.

[0018] The present invention provides a preparation method of a fiber material with antibacterial function, comprising the following steps: mixing a titanium source, an alkyl alcohol solvent, a chemical reactant, a cosolvent and polymer particles, heating the obtained mixture to 170-200°C under closed and first stirring conditions for reaction for 5-10 hours, wherein the titanium source and the alkyl alcohol solvent form a titanium alcohol complex, which is then dehydrated to form TiO2 under the action of the chemical reactant; the chemical reactant includes at least one of N,N-dimethylformamide and N,N-dimethylacetamide; pressurizing the obtained reaction system to 7-15 MPa, increasing the stirring rate, and performing a second stirring for 1-1.5 hours, wherein the polymer particles become a fluid state and impact the TiO2 together with the alkyl alcohol solvent to form nanoflower-shaped TiO2, thereby obtaining a spinning solution, and then releasing the pressure to spray out the spinning solution through a spinneret, wherein the solvent evaporates to form polymer fibers, thereby obtaining a fiber material with antibacterial function.

[0019] The present invention mixes the raw materials and heats them to 170-200°C. The titanium source is evenly dispersed in the solvent to form a titanium alcohol complex with the solvent. Then, under the action of a chemical reactant, a dehydration reaction occurs to generate TiO2. Under a critical state, the polymer particles become fluid. Due to the viscosity difference with the solvent, the titanium dioxide is repeatedly and irregularly impacted by the solvent and the polymer fluid, forming flow marks on the surface of the TiO2 particles, which are similar to the surface of shellfish in a tidal area (where sand and seawater are washed together). At the same time, it is ensured that there will be no serious collision with other titanium dioxide particles, and its morphology finally appears as a nanoflower.

[0020] The present invention combines multiple processes such as antimicrobial agent synthesis, polymer dissolution, and uniform dispersion of the antimicrobial agent in the polymer into one process during the entire preparation process, which can be completed in the same reactor. The same solvent is used to cleverly achieve in-situ preparation of the antimicrobial agent and polymer dissolution, which has the advantage of saving time and labor.

[0021] The fiber material prepared by the present invention has an antibacterial agent loaded with titanium dioxide in the form of a nanoflower, which has the characteristics of a large specific surface area. Firstly, it can fully contact and absorb natural light, generate active oxygen (hydroxyl radicals, superoxide radicals and photogenerated holes) substances, destroy the activity of bacteria, and thus inhibit bacteria and kill bacteria; secondly, the irregular shape of the surface makes it easy for the antibacterial agent to be embedded in the polymer surface, has a strong interfacial bonding force with the polymer, and is not easy to fall off, thereby achieving a long-lasting antibacterial effect of the fiber material.

[0022] The fiber material prepared by the present invention can be in the form of individual fibers, or in the form of non-woven materials after being opened and collected.

[0023] After the polymer fibers are formed, the present invention further opens the fibers through air flow, and the spinning solution is subjected to tension to form microfibers, so that the obtained non-woven material has good air permeability while maintaining good antibacterial properties and is comfortable to wear. The protective clothing prepared with the non-woven material can be used for a long time in scenarios such as preventing hospital bacterial infections and treating special medical accidents.

[0024] The fiber material of the present invention has a short preparation process, a simple preparation method, is easy to implement, has strong applicability, can be quickly and mass-produced, and can be used as raw materials for protective clothing, masks or other protective devices to respond to sudden health and safety accidents.

[0025] The results of the examples show that the nonwoven material prepared by the present invention has an air permeability of 200-400 mm / s, a longitudinal breaking strength of >200 N, and a transverse breaking strength of >150 N. It has excellent antibacterial effect, with the inhibition rates against Escherichia coli, Staphylococcus aureus and Helicobacter pylori being greater than 99.8%; and the antiviral activity rate against RNA virus H1N1 reaches 98.24%. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 Schematic diagram of the device used to prepare the antibacterial nonwoven material in the examples and comparative examples of the present invention, wherein 1 is a stirring device, 2 is a feeding hole, 3 is a stirring device, 4 is a spinneret hole, 5 is an air fiber opening device, 6 is a collecting device, and 7 is a nonwoven material;

[0027] Figure 2 The morphology of the nonwoven material of Example 1, wherein a is the surface morphology of the nonwoven material, and b is the microfiber morphology;

[0028] Figure 3 The morphology of the antimicrobial agent in Example 2, where a is the aggregated state of the antimicrobial agent and b is the surface morphology of the antimicrobial agent;

[0029] Figure 4 The morphology of the antibacterial nonwoven material of Example 2, wherein a is the surface morphology of the antibacterial nonwoven material, the inset is the enlarged view of the area, and b is the microfiber morphology;

[0030] Figure 5 The mechanical properties of the nonwoven materials of Examples 1 to 2 and Comparative Example 1, a is Example 1, b is Example 2, and c is Comparative Example 1;

[0031] Figure 6 The electron paramagnetic resonance spectra of the nonwoven material in comparative example 1 and the antibacterial nonwoven material in example 2 under light irradiation are shown in FIG. 3 , wherein the spin trapping agents are ·OH(a), h + (b) and O2 - (c);

[0032] Figure 7The antibacterial performance diagram of the antibacterial nonwoven material of Example 2, wherein a is a blank control sample, b to d are diagrams of the inhibition effect on Escherichia coli colonies at different concentrations, specifically, b is 0.075 mg / mL, c is 0.1 mg / mL, d is 0.125 mg / mL, e is 0.15 mg / mL, and f is 0.175 mg / mL. DETAILED DESCRIPTION

[0033] The present invention provides a method for preparing a fiber material with antibacterial function, comprising the following steps:

[0034] A titanium source, an alkyl alcohol solvent, a chemical reactant, a cosolvent, and polymer particles are mixed, and the resulting mixture is heated to 170-200° C. in a sealed and first stirring condition and reacted for 5-10 hours, wherein the titanium source and the alkyl alcohol solvent form a titanium alcohol complex, which is then dehydrated under the action of the chemical reactant to form TiO2; the chemical reactant includes at least one of N,N-dimethylformamide and N,N-dimethylacetamide;

[0035] The obtained reaction system is pressurized to 7-15 MPa, the stirring rate is increased, and a second stirring is performed for 1-1.5 hours. The polymer particles become fluid and impact TiO2 together with the alkyl alcohol solvent to form nanoflower-like TiO2, thereby obtaining a spinning solution. The spinning solution is then ejected through the spinneret by releasing the pressure, and the solvent evaporates to form polymer fibers, thereby obtaining a fiber material with antibacterial function.

[0036] In the present invention, unless otherwise specified, all raw materials used are commercially available products well known in the art.

[0037] The present invention mixes a titanium source, an alkyl alcohol solvent, a chemical reactant, a cosolvent and polymer particles.

[0038] In the present invention, the titanium source is preferably one or more of tetrabutyl titanate, titanium tetrachloride and titanium sulfate; the number of carbon atoms of the alkyl alcohol solvent is preferably not more than 5, and is more preferably isopropyl alcohol, ethylene glycol, n-propyl alcohol or a mixture thereof; in the present invention, the alkyl alcohol solvent has two functions: one is to form a titanium alcohol complex with the titanium source, and the other is to reduce the interfacial tension of the polymer in the solvent under high temperature and high pressure conditions.

[0039] In the present invention, the chemical reactant comprises at least one of N,N-dimethylformamide and N,N-dimethylacetamide; the cosolvent preferably comprises at least one of dichloroethane and dichloromethane; and the cosolvent functions to increase the cloud point pressure of the spinning solution. In the present invention, the polymer particles preferably comprise one or more of polyethylene particles, polypropylene particles, polyester particles, and polyamide particles; and the polymer viscosity preferably ranges from 1,000 to 45,000 mPa·s (measured using a capillary viscometer at atmospheric pressure and 25°C, using GB / T 1632.1-2008 for testing dilute polymer solution viscosity).

[0040] In the present invention, based on 100% raw material mass, the titanium source is preferably 5-8%, more preferably 6-7%; the chemical reactant is preferably 25-35%, more preferably 28-32%; the alkyl alcohol solvent is preferably 30-37%, more preferably 32-35%; the cosolvent is preferably 10-15%, more preferably 12-14%; the polymer particles are preferably 5-30%, more preferably 10-25%, and further preferably 15-20%.

[0041] In the present invention, the polymer particles are preferably dried before mixing. The present invention has no special requirements for the drying temperature, and any drying temperature known in the art can be used. In the embodiment of the present invention, the drying temperature is 60°C.

[0042] In the present invention, the mixing preferably includes: firstly adding the titanium source, alkyl alcohol solvent, chemical reactants and co-solvent into a reaction kettle, stirring evenly, and then adding the polymer particles.

[0043] After the mixing is completed, the present invention heats the obtained mixture to 170-200° C., preferably 180-190° C., under closed and first stirring conditions, and reacts for 5-10 hours, preferably 6-8 hours.

[0044] In the present invention, the first stirring rate is preferably 20-40 r / min. In the reaction process of the present invention, the titanium source and the alkyl alcohol solvent form a titanium alcohol complex, which is then dehydrated to form TiO2 under the action of chemical reactants, while the polymer is partially dissolved.

[0045] After the reaction is completed, the present invention pressurizes the resulting reaction system to 7-15 MPa, increases the stirring rate, and stirs for a second time for 1-1.5 hours. The polymer particles become fluid and impact the TiO2 with the alkyl alcohol solvent to form nanoflower-shaped TiO2, obtaining a spinning solution. The spinning solution is then released through the spinneret to release the pressure, and the solvent evaporates to form polymer fibers, thereby obtaining a fiber material with antibacterial function. Under the critical state, there is a viscosity difference between the polymer and the solvent. Subsequently, under the impact of the fluid, flow marks are formed on the surface of the TiO2 particles, and the morphology thereof ultimately manifests as nanoflower-shaped.

[0046] In the present invention, the gas used for pressurization is preferably one or more of argon, nitrogen and carbon dioxide; the pressure is increased to 7-15 MPa, preferably 9-13 MPa; the second stirring rate is preferably 100-200 r / min, more preferably 120-180 r / min.

[0047] The present invention promotes the polymer to become a fluid state through high temperature and high pressure. Due to the viscosity difference with the solvent, titanium dioxide is repeatedly subjected to irregular impacts of the solvent and polymer fluid, forming flow marks on the surface of TiO2 particles, similar to the surface of shellfish in a tidal area (sand and seawater are washed together), and its morphology eventually appears as a nanoflower. After the second stirring is completed, a spinning solution is obtained.

[0048] The present invention releases the pressure instantaneously to eject the spinning solution. In the present invention, the diameter of the spinneret is preferably 10 to 50 cm.

[0049] After the polymer fibers are formed, the present invention preferably further comprises air-opening the polymer fibers, collecting the opened fibers with a conveyor belt, and obtaining a fiber material with antibacterial function. In this case, the fiber material is an antibacterial nonwoven material.

[0050] In the present invention, the opening speed is preferably 20 to 200 m / s, more preferably 50 to 150 m / s. In the present invention, the spinning solution is subjected to tension to form fine fibers through airflow opening, resulting in a nonwoven material that maintains good antibacterial properties while also having good air permeability. In the present invention, the diameter of the polymer fibers after airflow opening is preferably 0.5 to 2 μm.

[0051] The present invention provides a fiber material with antibacterial function prepared by the preparation method described in the above scheme, which is composed of polymer fibers, and nano-flower-shaped TiO2 is distributed on the surface of the polymer fibers.

[0052] Nanoflower-like TiO2 has the characteristics of large specific surface area. First, it can fully contact and absorb natural light, produce active oxygen (hydroxyl radicals, superoxide radicals and photogenerated holes) substances, destroy the activity of bacteria, and thus inhibit bacteria and kill bacteria; second, the irregular shape of the surface makes it easy for the antibacterial agent to be embedded in the polymer surface, and has a strong interfacial bonding force with the polymer, which is not easy to fall off, thereby achieving a long-lasting antibacterial effect of the fiber material.

[0053] In the present invention, when the fiber material is an antibacterial nonwoven material, the antibacterial nonwoven material is composed of polymer fibers, the diameter of the polymer fibers is preferably 0.5 to 2 μm, the polymer fibers are densely arranged, the longitudinal breaking strength is greater than 200N, the transverse breaking strength is greater than 150N, and the air permeability is 200 to 400 mm / s.

[0054] The fiber material with antibacterial function and the preparation method thereof provided by the present invention are described in detail below with reference to the examples, but they should not be construed as limiting the scope of protection of the present invention.

[0055] Example 1

[0056] Use Figure 1 The antibacterial non-woven material was prepared using an experimental device with a reactor capacity of 10 L. Tetrabutyl titanate was used as the titanium source, N,N-dimethylformamide was used as the chemical reactant, isopropyl alcohol was used as the solvent, dichloroethane was used as the cosolvent, polyethylene particles were used as the polymer particles, and nitrogen was used as the protective gas.

[0057] 1500g of polyethylene granules were dried in an oven at 60°C. 250g of tetrabutyl titanate, 1250g of N,N-dimethylformamide, 1500g of isopropyl alcohol, and 500g of ethylene dichloride were then added to the reactor through the reactor feed port. Mechanical stirring was performed for 5 minutes at a speed of 20 r / min. The dried polymer granules were added to the reactor, the temperature was raised to 180°C, and stirring was continued for 8 hours. Carbon dioxide gas was injected into the reactor, and the pressure was increased to 7MPa. The stirring speed was slowly increased to 100 r / min. After stirring for 1 hour, the pressure was released, and the solvent in the polymer solution evaporated, forming microfiber bundles. These were then passed through an air opening device for air opening at a speed of 150m / s. Finally, the fibers were collected on a conveyor belt to form an antibacterial nonwoven material.

[0058] Through testing and analysis, the average fiber diameter is 1.2μm, the fiber transverse breaking strength is 160N, the longitudinal breaking strength is 209N, and the air permeability is 291mm / s (refer to the national standard GB / T15453-1997, analyzed using a differential pressure flowmeter, the same below). When the concentration of the non-woven material is 0.15mg / mL, the antibacterial rate against Escherichia coli is 99.8%, and the antiviral activity rate against RNA virus H1N1 reaches 98.35%.

[0059] Figure 2 The morphology of the nonwoven material of Example 1 is shown in Figure 1, where a is the surface morphology of the nonwoven material and b is the microfiber morphology. Figure 2 It can be seen that non-woven materials are composed of polymer microfibers with a diameter of 0.5 to 2 μm. The fibers are stacked on each other, leaving pores and having good air permeability.

[0060] Example 2

[0061] Use Figure 1The antibacterial non-woven material was prepared using an experimental device with a reactor capacity of 10 L. Tetrabutyl titanate was used as the titanium source, N,N-dimethylformamide was used as the chemical reactant, ethylene glycol was used as the solvent, chloroform was used as the cosolvent, polyester particles were used as the polymer particles, and argon was used as the protective gas.

[0062] 1500g of polyester granules were dried in an oven at 80°C. 250g of tetrabutyl titanate, 1250g of N,N-dimethylformamide, 1500g of ethylenedipropylene glycol, and 500g of chloroform were then added to the reactor through the reactor feed port. Mechanical stirring was continued for 5 minutes at a speed of 20 r / min. The dried polymer granules were added to the reactor, the temperature was raised to 180°C, and stirring was continued for 8 hours. Argon was injected into the reactor, the pressure within the reactor was increased to 8MPa, and the stirring speed was slowly increased to 100 r / min. After stirring for 1 hour, the pressure was released, and the solvent in the polymer solution evaporated, forming microfiber bundles. These were then passed through an air opening device for air opening at a speed of 200m / s. Finally, the fibers were collected on a conveyor belt to form an antibacterial nonwoven material.

[0063] Through testing and analysis, the average fiber diameter is 1.0μm, the fiber transverse breaking strength is 163N, the longitudinal breaking strength is 211N, the air permeability is 298mm / s, and when the concentration of the non-woven material is 0.15mg / mL, the antibacterial rate against Escherichia coli is 99.8%, and the antiviral activity rate against RNA virus H1N1 reaches 98.57%.

[0064] Figure 3 The morphology of the antibacterial agent in Example 2, wherein a is the aggregated state of the antibacterial agent and b is the surface morphology of the antibacterial agent. Figure 3 It can be seen that the antibacterial agent particles are uniform in size, at the micro-nano level, and the surface is similar to the shape of petals.

[0065] Figure 4 The morphology of the antibacterial nonwoven material of Example 2 is shown in Figure a, where a is the surface morphology of the antibacterial nonwoven material, the embedded image is the enlarged image of the region, and b is the microfiber morphology. Figure 4 It can be seen that the antimicrobial agent is evenly dispersed on the surface of the nonwoven material and the fiber, and the surface petal-like morphology is embedded on the fiber surface, which improves the antimicrobial durability of the fiber.

[0066] Figure 7 The antibacterial performance of the antibacterial nonwoven material of Example 2 was tested by the oscillation method, wherein a is a blank control sample, b to d are the inhibition effects on E. coli colonies at different nonwoven material concentrations, specifically, b is 0.075 mg / mL, c is 0.1 mg / mL, d is 0.125 mg / mL, e is 0.15 mg / mL, and f is 0.175 mg / mL. Figure 7 It can be seen that the antibacterial nonwoven material of Example 2 exhibits a good antibacterial effect on Escherichia coli.

[0067] Comparative Example 1

[0068] Use Figure 1 The antibacterial non-woven material was prepared using an experimental device with a reactor capacity of 10 L, N,N-dimethylformamide as the chemical reactant, isopropyl alcohol as the solvent, dichloroethane as the cosolvent, polyethylene particles as the polymer particles, and nitrogen as the protective gas.

[0069] 1500g of polyethylene granules were dried in an oven at 60°C. 1250g of N,N-dimethylformamide, 1500g of isopropyl alcohol, and 500g of ethylene dichloride were then added to the reactor through the reactor feed port. The mixture was mechanically stirred for 5 minutes at a speed of 20 r / min. The dried polymer granules were added to the reactor, heated to 180°C, and stirred for 8 hours. Nitrogen was injected into the reactor, and the pressure was increased to 15MPa. The stirring speed was slowly increased to 100 r / min. After stirring for 1 hour, the pressure was released, and the solvent in the polymer solution evaporated, forming microfiber bundles. These were then passed through an air opening device and opened by airflow at a speed of 150m / s. Finally, the fibers were collected on a conveyor belt to form an antibacterial nonwoven material.

[0070] Through testing and analysis, the average fiber diameter is 0.9μm, the fiber transverse breaking strength is 157N, the longitudinal breaking strength is 201N, the air permeability is 292mm / s, and the antibacterial rate against Escherichia coli is 0.12% when the concentration of non-woven material is 0.15mg / mL; the antiviral activity rate against RNA virus H1N1 reaches 5.24%.

[0071] Figure 5 The mechanical properties of the nonwoven materials of Examples 1 to 2 and Comparative Example 1 are shown in Figures a and b, respectively. Figure 5 It can be seen that the longitudinal breaking strength of the nonwoven fabrics prepared in Examples 1 to 2 and Comparative Example 1 is greater than 200N, and the transverse breaking strength is greater than 150N.

[0072] Figure 6 For the nonwoven material in Comparative Example 1 (i.e. Figure 6 The non-woven fabric in Example 2) and the antibacterial non-woven material in Example 2 (ie Figure 6 Electron paramagnetic resonance spectra of the antibacterial nonwoven fabric) under light irradiation, the spin trapping agents are OH(a), h + (b) and O2 - (c) By Figure 6 It can be seen that the nonwoven material of the present invention can generate active oxygen species (hydroxyl radicals, superoxide radicals and photogenerated holes) under light conditions, has strong oxidizing properties, and can be used to oxidize and kill bacteria.

[0073] Based on Examples 1 to 2 and Comparative Example 1, the following conclusions can be drawn: (1) The antibacterial nonwoven material is simplifies the manufacturing process by adopting the in-situ synthesis of antibacterial agents and the instantaneous pressure release method. Compared with the traditional preparation process, the production cost and production time are reduced and shortened; (2) It can be seen from the results of Examples 1 to 2 that the antibacterial nonwoven material prepared by the present invention has the characteristics of good antibacterial property, high breaking strength and strong air permeability; (3) It can be seen from Examples 1 to 2 and Comparative Example 1 that in the absence of a titanium source, a nonwoven material composed of fine fibers can still be prepared. The titanium source is the precursor of the main antibacterial agent and is the key component that gives the nonwoven material the antibacterial function.

[0074] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A method for preparing a fiber material with antibacterial function, characterized in that: The following steps are involved: A titanium source, an alkyl alcohol solvent, a chemical reactant, a cosolvent, and polymer particles are mixed, and the resulting mixture is heated to 170-200° C. in a sealed and first stirring condition and reacted for 5-10 hours, wherein the titanium source and the alkyl alcohol solvent form a titanium alcohol complex, which is then dehydrated under the action of the chemical reactant to form TiO2; the chemical reactant includes at least one of N,N-dimethylformamide and N,N-dimethylacetamide; The obtained reaction system is pressurized to 7-15 MPa, the stirring rate is increased, and a second stirring is performed for 1-1.5 hours. The polymer particles become fluid and impact TiO2 together with the alkyl alcohol solvent to form nanoflower-like TiO2, thereby obtaining a spinning solution. The spinning solution is then ejected through the spinneret by releasing the pressure, and the solvent evaporates to form polymer fibers, thereby obtaining a fiber material with antibacterial function.

2. The preparation method according to claim 1, characterized in that The titanium source is one or more of tetrabutyl titanate, titanium tetrachloride and titanium sulfate.

3. The preparation method according to claim 1, characterized in that The carbon number of the alkyl alcohol solvent is no more than 5.

4. The preparation method according to claim 1, characterized in that The polymer particles include one or more of polyethylene particles, polypropylene particles, polyester particles and polyamide particles.

5. The preparation method according to claim 1, characterized in that The co-solvent includes at least one of dichloroethane and dichloromethane.

6. The preparation method according to any one of claims 1 to 5, characterized in that Based on 100% of the raw material mass, the titanium source accounts for 5-8%, the chemical reactant accounts for 25-35%, the alkyl alcohol solvent accounts for 30-37%, the cosolvent accounts for 10-15%, and the polymer particles account for 5-30%.

7. The preparation method according to claim 1, characterized in that The first stirring rate is 20-40 r / min; the second stirring rate is 100-200 r / min.

8. The preparation method according to claim 1, characterized in that The gas used for pressurization is one or more of argon, nitrogen and carbon dioxide.

9. The preparation method according to claim 1, characterized in that After the polymer fibers are formed, the method further includes air-opening the polymer fibers and collecting the opened fibers with a conveyor belt.

10. The fiber material with antibacterial function prepared by the preparation method according to any one of claims 1 to 9, comprising polymer fibers, wherein nano-flower-like TiO2 is distributed on the surface of the polymer fibers.

Citation Information

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