阅读说明：本技术 一种抗菌纤维及其制备方法、抗菌产品 (Antibacterial fiber, preparation method thereof and antibacterial product ) 是由 欧阳申珅 陈妙金 陆龙喜 陈鹏 刘明 于 2021-10-29 设计创作，主要内容包括：本发明涉及一种抗菌纤维的制备方法,包括以下步骤：提供PVA水溶液,其中,PVA水溶液中PVA的质量分数为8％-15％；向PVA水溶液中加入纳米TiO-(2)颗粒和分散剂,并进行超声分散,得到纺丝液,其中,PVA水溶液与纳米TiO-(2)颗粒的质量比为100:1-100:15,纺丝液的Zeta电位的绝对值为10mV-40mV；将纺丝液进行静电纺丝,得到抗菌纤维。本发明还涉及一种由所述制备方法制备得到的抗菌纤维以及由所述的抗菌纤维制成的抗菌产品。本发明的制备工艺简单,且获得的抗菌纤维具有优异的抗菌性能,同时,纳米TiO-(2)颗粒不易脱落,循环洗涤50次后,抑菌率下降均不超过5％,因此,采用本发明抗菌纤维制成的纺丝品、过滤材料、包装材料和医药卫生材料等抗菌产品具有优异的抗菌和抑菌性能,且效果持久。(The invention relates to a preparation method of an antibacterial fiber, which comprises the following steps: providing a PVA aqueous solution, wherein the mass fraction of PVA in the PVA aqueous solution is 8-15%; adding nano TiO into PVA water solution 2 Carrying out ultrasonic dispersion on the particles and a dispersing agent to obtain a spinning solution, wherein the PVA aqueous solution and the nano TiO 2 The mass ratio of the particles is 100:1-100:15, and the absolute value of the Zeta potential of the spinning solution is 10mV-40 mV; and (4) carrying out electrostatic spinning on the spinning solution to obtain the antibacterial fiber. The invention also relates to the antibacterial fiber prepared by the preparation method and an antibacterial product prepared from the antibacterial fiber. The preparation process is simple, and the obtained antibacterial fiber has excellent antibacterial performance and nano TiO 2 The particles are not easy to fall off, and the bacteriostasis rate is not reduced by more than 5 percent after the circulation washing for 50 times, so that the spinning product, the filtering material, the packaging material and the medicine made of the antibacterial fiber are adoptedThe antibacterial products such as the medical and sanitary materials have excellent antibacterial and bacteriostatic properties and lasting effect.)

1. A preparation method of antibacterial fiber is characterized by comprising the following steps: the preparation method comprises the following steps:

providing a PVA aqueous solution, wherein the mass fraction of PVA in the PVA aqueous solution is 8-15%;

adding nano titanium dioxide particles and a dispersing agent into the PVA aqueous solution, and performing ultrasonic dispersion to obtain a spinning solution, wherein the mass ratio of the PVA aqueous solution to the nano titanium dioxide particles is 100:1-100:15, and the absolute value of the Zeta potential of the spinning solution is 10mV-40 mV; and

and (3) carrying out electrostatic spinning on the spinning solution to obtain the antibacterial fiber.

2. The method for producing an antibacterial fiber according to claim 1, characterized in that: the dispersant is selected from stearic acid.

3. The method for producing an antibacterial fiber according to claim 1 or 2, characterized in that: the mass of the dispersing agent is 0.1-1% of the mass of the nano titanium dioxide particles.

4. The method for producing an antibacterial fiber according to claim 1, characterized in that: the particle size of the nano titanium dioxide particles is 3nm-50 nm.

5. The method for producing an antibacterial fiber according to claim 4, characterized in that: the particle size of the nano titanium dioxide particles is 5nm-20nm, and the mass ratio of the PVA aqueous solution to the nano titanium dioxide particles is 100:5-100: 10.

6. The method for producing an antibacterial fiber according to claim 1, characterized in that: the absolute value of the Zeta potential of the spinning solution is 20mV-30 mV.

7. The method for producing an antibacterial fiber according to claim 1, characterized in that: in the step of electrostatic spinning, the voltage is 1.25 to 1.35 times of the mass fraction of PVA in the PVA aqueous solution.

8. The method for producing an antibacterial fiber according to claim 7, characterized in that: in the step of electrostatic spinning, the advancing speed is 0.3mL/h-0.8mL/h, the receiving distance is 12cm-18cm, and the voltage is 10KV-20 KV.

9. An antibacterial fiber produced by the production method according to any one of claims 1 to 8.

10. An antimicrobial product made from the antimicrobial fiber of claim 9.

Technical Field

The invention relates to the technical field of antibacterial materials, in particular to an antibacterial fiber, a preparation method thereof and an antibacterial product.

Background

TiO with nano-grade dispersion degree₂The photo-generated electrons generated by photocatalysis and photo-generated holes and water or hydroxyl adsorbed on the surface of the catalyst form active hydroxyl or superoxide ions with strong oxidizing property, and the active hydroxyl or superoxide ions and bacterial cells or components in the bacteria are subjected to biochemical reaction to thoroughly kill the bacteria, and meanwhile, toxic compounds released by the bacteria are degraded to prevent endotoxin from causing secondary pollution. Using nano TiO₂The prepared antibacterial fiber can be widely used for weaving daily sanitary textiles such as clothes, bed sheets, curtains and the like, and in recent years, the antibacterial fiber is also widely used for weaving filter materials, packaging materials, medical and health materials and the like.

However, nano TiO is currently used₂In the prepared antibacterial fiber, nano TiO₂The particle size is not uniform, the loading on the fiber is not uniform enough, and simultaneously, the nano TiO₂The particles are not loaded firmly enough and have poor washing fastness.

Disclosure of Invention

In order to solve the problems in the prior art, the preparation method of the antibacterial fiber provided by the invention is simple in process, the obtained antibacterial fiber has excellent antibacterial and bacteriostatic effects, and the nano TiO in the antibacterial fiber₂The antibacterial fiber has the advantages of firm particle loading, good washing fastness and durable antibacterial performance, and further, an antibacterial product with excellent and durable antibacterial performance can be prepared by using the antibacterial fiber.

In order to achieve the purpose, the invention is realized by the following technical scheme:

a preparation method of antibacterial fiber comprises the following steps:

providing a PVA aqueous solution, wherein the mass fraction of PVA in the PVA aqueous solution is 8-15%;

adding nano titanium dioxide particles and a dispersing agent into the PVA aqueous solution, and performing ultrasonic dispersion to obtain a spinning solution, wherein the mass ratio of the PVA aqueous solution to the nano titanium dioxide particles is 100:1-100:15, and the absolute value of the Zeta potential of the spinning solution is 10mV-40 mV; and

and (3) carrying out electrostatic spinning on the spinning solution to obtain the antibacterial fiber.

Optionally, the dispersant is selected from stearic acid.

Optionally, the mass of the dispersing agent is 0.1-1% of the mass of the nano titanium dioxide particles.

Optionally, the particle size of the nano titanium dioxide particles is 3nm-50 nm.

Optionally, the particle size of the nano titanium dioxide particles is 5nm-20nm, and the mass ratio of the PVA aqueous solution to the nano titanium dioxide particles is 100:5-100: 10.

Optionally, the absolute value of the Zeta potential of the spinning solution is 20mV to 30 mV.

Optionally, in the step of electrospinning, the voltage is 1.25 times to 1.35 times of the mass fraction of PVA in the aqueous PVA solution.

Optionally, in the step of electrostatic spinning, the advancing speed is 0.3mL/h-0.8mL/h, the receiving distance is 12cm-18cm, and the voltage is 10KV-20 KV.

An antibacterial fiber prepared by the preparation method.

An antibacterial product made of the antibacterial fiber.

Compared with the prior art, the invention has the following beneficial effects:

in the preparation method of the antibacterial fiber, PVA aqueous solution and nano TiO are adopted₂The particles are prepared into spinning solution, and nano TiO in the spinning solution₂Van der Waals force and electrostatic repulsion force exist between particles, so the invention adds nano TiO into PVA water solution₂Dispersing the particles by an ultrasonic method, assisting by using a dispersing agent, and controlling the Zeta potential of the spinning solution to be 10mV-40mV so as to ensure that the nano TiO₂The particles are uniformly dispersed in the spinning solution. Further, the spinning solution is subjected to electrostatic spinningThe antibacterial fiber can be obtained by silk, the preparation process is simple, and in the obtained antibacterial fiber, the nano TiO₂The particles are uniformly loaded on the PVA carrier, so that the antibacterial rate of the antibacterial fiber on escherichia coli and yellow glucose bacteria reaches over 90 percent, the antibacterial rate on candida albicans reaches over 80 percent, and meanwhile, the nano TiO is₂The combination fastness of the particles and the PVA carrier is strong, the particles are not easy to fall off, and the bacteriostasis rate is not reduced by more than 5 percent after the particles are circularly washed for 50 times, which are all far higher than the antibacterial standard.

Therefore, the antibacterial products such as spinning products, filtering materials, packaging materials, medical and health materials and the like prepared by the antibacterial fiber have excellent antibacterial and bacteriostatic properties and have lasting effect.

Drawings

FIG. 1 is a scanning electron microscope image of the antibacterial fiber prepared in example 1 of the present invention.

Detailed Description

The following description will further explain the antibacterial fiber provided by the present invention, its preparation method and antibacterial product with reference to the attached figure 1 of the specification.

The preparation method of the antibacterial fiber provided by the invention comprises the following steps:

s1, providing a PVA aqueous solution, wherein the mass fraction of PVA in the PVA aqueous solution is 8% -15%;

s2, adding nano titanium dioxide particles and a dispersing agent into the PVA aqueous solution, and performing ultrasonic dispersion to obtain a spinning solution, wherein the mass ratio of the PVA aqueous solution to the nano titanium dioxide particles is 100:1-100:15, and the absolute value of the Zeta potential of the spinning solution is 10mV-40 mV;

and S3, performing electrostatic spinning on the spinning solution to obtain the antibacterial fiber.

In step S1, the mass fraction of PVA in the PVA aqueous solution (polyvinyl alcohol aqueous solution) is more preferably 10% to 12%.

In step S2, PVA water solution and nano TiO are adopted₂When the particles are prepared into spinning solution, the nano TiO in the spinning solution₂Van der Waals force and electrostatic repulsion force exist between the particles, and the nano TiO can be influenced₂The dispersing effect of the particles. Therefore, the present inventionAdding nano TiO into PVA water solution₂Dispersing by an ultrasonic method during particle preparation, and using a dispersing agent for assistance to control the Zeta potential of the spinning solution to be 10mV-40mV so as to enable the nano TiO₂The particles are uniformly dispersed in the spinning solution.

Optionally, when the dispersion is performed by using an ultrasonic method, the frequency of the ultrasonic disperser is preferably 28KHz to 40 KHz.

Optionally, the dispersant is selected from stearic acid, and the mass of the dispersant is 0.1% -1%, preferably 0.5% -0.8% of the mass of the nano titanium dioxide particles.

Optionally, the absolute value of the Zeta potential of the spinning solution can be further optimized to be 20mV-30mV through controlling the ultrasonic dispersion and the dispersing agent, so that the nano TiO can be obtained₂The spinning solution with better particle dispersion effect can be used for obtaining the antibacterial fiber with better performance through electrostatic spinning.

Optionally, the particle size of the nano titanium dioxide particles is 3nm-50nm, more preferably 5nm-20nm, and the mass ratio of the PVA aqueous solution to the nano titanium dioxide particles in the spinning solution is more preferably 100:5-100: 10.

In step S3, in the step of electrospinning the spinning solution, the voltage is 1.25 to 1.35 times the mass fraction of PVA in the PVA aqueous solution, for example, when the mass fraction of PVA in the PVA aqueous solution is 10%, the voltage is 12.5 to 13.5KV, and in this matching relationship, the antibacterial fiber can be stably obtained.

Optionally, in the step of electrostatic spinning, the advancing speed is 0.3mL/h-0.8mL/h, the receiving distance is 12cm-18cm, the voltage is 10KV-20KV, the spinning needle is connected with the anode, the receiving end is connected with the cathode, and the superfine denier polyester fiber fabric is used as the receiving substrate.

Optionally, after electrostatic spinning is finished, the fiber is naturally dried at normal temperature to obtain the antibacterial fiber.

In the antibacterial fiber, nano TiO₂The particles are uniformly loaded on the PVA carrier, so that the antibacterial rate of the antibacterial fiber on escherichia coli and yellow glucose bacteria reaches over 90 percent, and the antibacterial rate on candida albicans reachesMore than 80 percent of nano TiO₂The particles and the PVA carrier have strong binding fastness and are not easy to fall off, the bacteriostasis rate is not reduced by more than 5 percent after the particles and the PVA carrier are circularly washed for 50 times, the bacteriostasis rate is far higher than the antibacterial standard, and the particles have excellent antibacterial and bacteriostatic properties and lasting effect.

In addition, the invention adopts the electrostatic spinning method to obtain the antibacterial fiber with excellent performance, has simple preparation process and is suitable for industrial production.

Based on the preparation method, the invention also provides the antibacterial fiber. It can be understood that the antibacterial fiber of the present invention comprises a PVA carrier and nano TiO supported on the PVA carrier₂Particle, nano TiO₂The particle size of the particles is 3nm-50nm, more preferably 5nm-20nm, and the antibacterial fiber has excellent antibacterial and bacteriostatic properties and lasting effect.

The invention also provides an antibacterial product prepared from the antibacterial fiber. It can be understood that the antibacterial product comprises daily hygiene textiles such as clothes, bed sheets and curtains, and also comprises filtering materials, packaging materials, medical and health materials and the like, and has excellent antibacterial and bacteriostatic properties and a lasting effect.

Hereinafter, the antibacterial fiber, the preparation method thereof, and the antibacterial product will be further described by the following specific examples.

Example 1:

100 parts by weight of PVA aqueous solution with the mass fraction of 8% is prepared, 5 parts by weight of nano titanium dioxide particles with the particle size of 20nm and 0.005 part by weight of stearic acid are added, and ultrasonic dispersion is carried out at the frequency of 30KHz, so as to obtain spinning solution with the Zeta potential absolute value of 15 mV.

And (3) carrying out electrostatic spinning on the spinning solution, wherein in the electrostatic spinning, the advancing speed is 0.3mL/h, the receiving distance is 12cm, the voltage is 10KV and is 1.25 times of the mass fraction, the spinning needle is connected with the anode, the receiving end is connected with the cathode, the superfine denier polyester fiber fabric is used as a receiving substrate, and after the electrostatic spinning is finished, the spinning solution is naturally dried at normal temperature to obtain the antibacterial fiber.

Example 2:

100 parts by weight of PVA aqueous solution with the mass fraction of 10% is prepared, 10 parts by weight of nano titanium dioxide particles with the particle size of 15nm and 0.04 part by weight of stearic acid are added, and ultrasonic dispersion is carried out at the frequency of 30KHz to obtain the spinning solution with the Zeta potential absolute value of 20 mV.

And (3) carrying out electrostatic spinning on the spinning solution, wherein in the electrostatic spinning, the propelling speed is 0.5mL/h, the receiving distance is 13cm, the voltage is 13KV and is 1.3 times of the mass fraction, the spinning needle is connected with the anode, the receiving end is connected with the cathode, the superfine denier polyester fiber fabric is used as a receiving substrate, and after the electrostatic spinning is finished, the spinning solution is naturally dried at normal temperature to obtain the antibacterial fiber.

Example 3:

100 parts by weight of PVA aqueous solution with the mass fraction of 12% is prepared, 10 parts by weight of nano titanium dioxide particles with the particle size of 10nm and 0.06 part by weight of stearic acid are added, and ultrasonic dispersion is carried out at the frequency of 35KHz to obtain spinning solution with the Zeta potential absolute value of 25 mV.

And (3) carrying out electrostatic spinning on the spinning solution, wherein in the electrostatic spinning, the advancing speed is 0.6mL/h, the receiving distance is 15cm, the voltage is 15KV and is 1.25 times of the mass fraction, a spinning needle is connected with a positive electrode, a receiving end is connected with a negative electrode, the superfine denier polyester fiber fabric is used as a receiving substrate, and after the electrostatic spinning is finished, the superfine denier polyester fiber fabric is naturally dried at normal temperature to obtain the antibacterial fiber.

Example 4:

100 parts by weight of PVA aqueous solution with the mass fraction of 13% is prepared, 12 parts by weight of nano titanium dioxide particles with the particle size of 20nm and 0.08 part by weight of stearic acid are added, and ultrasonic dispersion is carried out at the frequency of 35KHz to obtain spinning solution with the Zeta potential absolute value of 30 mV.

And (3) carrying out electrostatic spinning on the spinning solution, wherein in the electrostatic spinning, the advancing speed is 0.6mL/h, the receiving distance is 16cm, the voltage is 17KV, the spinning needle is connected with the anode, the receiving end is connected with the cathode, the superfine denier polyester fiber fabric is used as a receiving substrate, and after the electrostatic spinning is finished, the spinning solution is naturally dried at normal temperature to obtain the antibacterial fiber.

Example 5:

preparing 100 parts by weight of PVA aqueous solution with the mass fraction of 15%, adding 15 parts by weight of nano titanium dioxide particles with the particle size of 40nm and 0.15 part by weight of stearic acid, and performing ultrasonic dispersion at the frequency of 40KHz to obtain spinning solution with the Zeta potential absolute value of 40 mV.

And (3) carrying out electrostatic spinning on the spinning solution, wherein in the electrostatic spinning, the advancing speed is 0.8mL/h, the receiving distance is 18cm, the voltage is 20KV, the spinning needle is connected with the anode, the receiving end is connected with the cathode, the superfine denier polyester fiber fabric is used as a receiving substrate, and after the electrostatic spinning is finished, the spinning solution is naturally dried at normal temperature to obtain the antibacterial fiber.

Example 6:

preparing 100 parts by weight of PVA aqueous solution with the mass fraction of 10%, adding 3 parts by weight of nano titanium dioxide particles with the particle size of 5nm and 0.03 part by weight of stearic acid, and performing ultrasonic dispersion at the frequency of 35KHz to obtain spinning solution with the Zeta potential absolute value of 10 mV.

And (3) carrying out electrostatic spinning on the spinning solution, wherein in the electrostatic spinning, the advancing speed is 0.5mL/h, the receiving distance is 16cm, the voltage is 13.5KV, the spinning needle is connected with the anode, the receiving end is connected with the cathode, the superfine denier polyester fiber fabric is used as a receiving substrate, and after the electrostatic spinning is finished, the spinning solution is naturally dried at normal temperature to obtain the antibacterial fiber.

The antibacterial fibers obtained in examples 1 to 6 were produced into cloth of the same specification under the same conditions, and subjected to antibacterial tests, with the results shown in tables 1 to 3.

TABLE 1

TABLE 2

TABLE 3

The cloth thus produced was washed 50 times and then subjected to an antibacterial test, and the results are shown in tables 4 to 6.

TABLE 4

TABLE 5

TABLE 6

Finally, it should be noted that the present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.