阅读说明：本技术 一种抗菌纳米纤维的制备方法 (Preparation method of antibacterial nanofiber ) 是由 张丽娜 惠林涛 金夏伟 邵礼滨 张鲁燕 张云兵 王龙飞 于 2021-07-22 设计创作，主要内容包括：本发明公开了一种抗菌纳米纤维的制备方法。方法包括：将聚乙烯醇加入水中,加热条件下搅拌至完全溶解,加入抗菌试剂,室温条件搅拌得到混合纺丝液,通过静电纺丝的工艺制备纳米纤维,最终将纳米纤维通过交联反应处理成非水溶性的纳米材料。所述的纳米纤维为负载有抗菌成分的纳米纤维。本发明所得到的抗菌纳米纤维除了具有高效的空气过滤性能,还具有广谱的抗菌功能。整个纤维制备工艺流程短,操作简单,原料选择环保。所述的抗菌纳米纤维具有良好的应用前景,可以作为口罩、空气过滤器、呼吸机等空气过滤装置和设备的过滤层,能够高效地吸附和杀灭空气中的细菌等有害物质。(The invention discloses a preparation method of antibacterial nano-fibers. The method comprises the following steps: adding polyvinyl alcohol into water, stirring under heating to completely dissolve, adding an antibacterial agent, stirring at room temperature to obtain a mixed spinning solution, preparing nanofibers through an electrostatic spinning process, and finally treating the nanofibers into water-insoluble nanomaterials through a crosslinking reaction. The nano-fiber is loaded with antibacterial components. The antibacterial nanofiber obtained by the invention has high-efficiency air filtering performance and broad-spectrum antibacterial function. The whole fiber preparation process is short in flow, simple to operate and environment-friendly in raw material selection. The antibacterial nanofiber has a good application prospect, can be used as a filtering layer of air filtering devices and equipment such as a mask, an air filter and a breathing machine, and can efficiently adsorb and kill harmful substances such as bacteria in the air.)

1. A method for preparing antibacterial nano-fibers comprises the following steps:

(1) dispersing polyvinyl alcohol in water, and stirring and dissolving under a heating condition to obtain a polyvinyl alcohol solution;

(2) adding an antibacterial agent into the polyvinyl alcohol solution, and uniformly stirring at room temperature;

(3) carrying out electrostatic spinning on the mixed spinning solution prepared in the step (2) to obtain drug-loaded nano fibers;

(4) and (4) completing a crosslinking reaction on the nanofiber obtained in the step (3), and treating to obtain the water-insoluble nanofiber.

2. The method for preparing antibacterial nano-fiber according to claim 1, characterized in that: the main antibacterial component is quaternary ammonium salt derivative.

3. The method for preparing antibacterial nano-fiber according to claim 1, characterized in that: the polymerization degree of the polyvinyl alcohol in the step (1) is 1700-2200, and the alcoholysis degree is not less than 95%.

4. The method for preparing antibacterial nano-fiber according to claim 1, characterized in that: the concentration of the polyvinyl alcohol solution in the step (1) is 8-15 wt%.

5. The method for preparing antibacterial nano-fiber according to claim 1, characterized in that: the mass fraction of the antibacterial agent in the solution in the step (2) is 1-20 wt%, and the stirring time is 3-5 h.

6. The method for preparing antibacterial nano-fiber according to claim 1, characterized in that: the electrostatic spinning parameters in the step (3) are as follows: the electrostatic spinning applied voltage is 12-20KV, the receiving distance is 12-22cm, and the solution flow rate is 0.4-1.2 mL/h.

7. The method for preparing antibacterial nano-fiber according to claim 1, characterized in that: the electrostatic spinning conditions were: 20-25 ℃; the relative humidity is 30-50%.

8. The method for preparing antibacterial nanofiber as claimed in claim 1, wherein the cross-linking agent in step (4) is glutaraldehyde, and the solvent is acetone or absolute ethanol.

9. The method for preparing antibacterial nano-fiber according to claim 1, characterized in that: the antibacterial nanofiber can be used as a filter layer of air filtering devices and equipment such as a mask, an air filter and a breathing machine, and can efficiently adsorb and kill harmful substances such as bacteria in the air.

Technical Field

The invention belongs to the field of nanofiber materials and preparation thereof, and particularly relates to a preparation method of antibacterial nanofibers.

Background

The electrostatic spinning is one of the most effective modes for preparing the nanofiber material at present, and the method has the advantages of simplicity in operation, short preparation flow, wide material selection and the like. The nanofibers can be used as air filtration materials, generally, the filtration efficiency of the filtration materials increases with the decrease of the diameter of the filtration fibers, and the nanomaterials prepared by the electrospinning technology are generally distributed in the diameter range from a few nanometers to hundreds of nanometers. In addition, the nano material prepared by electrostatic spinning generally has higher porosity and excellent air permeability, and is very suitable for being used as an air filter material.

The nano fiber is usually used as a drug carrier in a drug controlled release system, the nano fiber has the excellent characteristics of high porosity, large specific surface area and the like, the drug effect can be better exerted, the nano fiber drug-loaded system can also avoid the drug burst release in the release process of the drug, and the drug effect can be continuously and efficiently provided. If the antibacterial agent is loaded on the nano-fiber, and then the nano-fiber is applied to the filter material of the mask, the filtering effect of the mask on harmful substances in the air can be further improved.

Disclosure of Invention

The invention relates to a preparation method of antibacterial nanofibers, and aims to solve the technical problem of providing antibacterial nanofibers and a preparation method thereof aiming at a single physical filtration mechanism of the traditional mask filter material. The invention has simple operation and environment-friendly and nontoxic materials, kills harmful substances such as bacteria and the like in the air by a chemical method and provides a double filtering mechanism. The invention discloses a preparation method of antibacterial nano-fibers, which comprises the following steps:

(1) adding polyvinyl alcohol into water, and stirring and dissolving under a heating condition to obtain a polyvinyl alcohol solution;

(2) adding an antibacterial agent into the polyvinyl alcohol solution, and uniformly stirring at room temperature;

(3) carrying out electrostatic spinning on the mixed spinning solution prepared in the step (2) to obtain antibacterial component-loaded nano fibers;

(4) and (4) completing a crosslinking reaction on the nanofiber obtained in the step (3), and treating to obtain the water-insoluble nanofiber.

The polymerization degree of the polyvinyl alcohol in the step (1) is 1700-2200, and the alcoholysis degree is more than or equal to 95 percent;

the concentration of the polyvinyl alcohol solution in the step (1) is 8-15 wt%;

the antibacterial component in the step (2) is a quaternary ammonium salt derivative;

the mass fraction of the antibacterial agent in the solution in the step (2) is 1-20 wt%, and the stirring time is 3-5 h;

the nano-fibers in the step (3) are nano-fibers loaded with antibacterial components;

the electrostatic spinning parameters in the step (3) are as follows: the electrostatic spinning applied voltage is 12-20KV, the receiving distance is 12-22cm, the solution flow rate is 0.4-1.2mL/h, and the electrostatic spinning conditions are as follows: 20-25 ℃; relative humidity is 30-50%;

in the step (4), the cross-linking agent is glutaraldehyde, and the solvent is acetone or absolute ethyl alcohol;

the antibacterial nanofiber in the step (4) can be used as a filter layer of air filtering devices and equipment such as a mask, an air filter and a breathing machine, and can efficiently adsorb and kill harmful substances such as bacteria in the air.

In the invention, the quaternary ammonium salt derivative is added into the polyvinyl alcohol solution, wherein the quaternary ammonium salt derivative is selected because the quaternary ammonium salt derivative is a broad-spectrum antibacterial agent, the sterilization mechanism of the quaternary ammonium salt derivative is mainly that cations with sterilization effect are effectively attached to the surface of bacteria, and the biological active enzyme and metabolic intermediate products in the bacteria overflow by destroying the cell membrane of thalli, thereby achieving the effects of sterilization and bacteriostasis. The quaternary ammonium salt derivative is a water-soluble substance, can have better compatibility with polyvinyl alcohol solution, and the quaternary ammonium salt component can be uniformly distributed in the finally obtained antibacterial nanofiber.

Advantageous effects

(1) The whole preparation process related by the invention has short flow, simple operation, environment-friendly raw material selection and low requirements on equipment and treatment environment;

(2) the antibacterial nanofiber obtained by the invention has high-efficiency air filtering performance and also has a broad-spectrum antibacterial function.

Drawings

Fig. 1 is an antibacterial nanofiber SEM.

Detailed Description

The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it will be appreciated that various changes and modifications may be made by those skilled in the art after reading the teachings herein, and such equivalents may fall within the scope of the invention as defined in the appended claims.

Example 1

(1) Adding 10g of polyvinyl alcohol into 80g of water, and stirring and dissolving under the heating condition of 80 ℃ to obtain a polyvinyl alcohol solution;

(2) adding 10g of antibacterial agent into the polyvinyl alcohol solution, and uniformly stirring at room temperature;

(3) and (3) carrying out electrostatic spinning on the mixed spinning solution prepared in the step (2) to obtain the antibacterial component-loaded nano fiber, wherein the spinning conditions are as follows: the spinning voltage is 15KV, the receiving distance is 12cm, and the solution flow rate is 0.8 ml/h.

(4) Preparing a cross-linking agent solution: 5 wt% glutaraldehyde (25% aqueous solution) was added to acetone, followed by 2ml of dilute hydrochloric acid and mixed well.

(5) And (4) flatly immersing the prepared nanofiber membrane into the cross-linking agent solution in the step (4), standing for 3 hours, taking out and washing for 5 times, and putting into a drying oven at 40 ℃ for drying. The prepared nanofiber membrane has the bacteriostasis rate of over 99 percent on escherichia coli, staphylococcus aureus and candida albicans.

Example 2

(1) Adding 10g of polyvinyl alcohol into 70g of water, and stirring and dissolving under the heating condition of 80 ℃ to obtain a polyvinyl alcohol solution;

(2) adding 20g of antibacterial agent into the polyvinyl alcohol solution, and uniformly stirring at room temperature;

(3) and (3) carrying out electrostatic spinning on the mixed spinning solution prepared in the step (2) to obtain the antibacterial component-loaded nano fiber, wherein the spinning conditions are as follows: the spinning voltage is 15KV, the receiving distance is 12cm, and the solution flow rate is 0.8 ml/h.

(4) Preparing a cross-linking agent solution: 5 wt% glutaraldehyde (25% aqueous solution) was added to acetone, followed by 2ml of dilute hydrochloric acid and mixed well.

(5) And (4) flatly immersing the prepared nanofiber membrane into the cross-linking agent solution in the step (4), standing for 3 hours, taking out and washing for 5 times, and putting into a drying oven at 40 ℃ for drying. The prepared nanofiber membrane has the bacteriostasis rate of over 99 percent on escherichia coli, staphylococcus aureus and candida albicans.