阅读说明：本技术 一种抗菌聚丙烯腈纤维的制备方法 (Preparation method of antibacterial polyacrylonitrile fiber ) 是由 谢建江 于 2019-05-24 设计创作，主要内容包括：本发明公开了一种抗菌聚丙烯腈纤维的制备方法,包括如下步骤；(1)天然纤维素纤维溶解；(2)聚丙烯腈纤维溶解；(3)配置纺丝原液；(4)静电纺丝处理；(5)抗菌后处理。本发明一种抗菌聚丙烯腈纤维的制备方法,通过将具有抗菌性能的天然纤维素纤维与聚丙烯腈纤维和天然抗菌植物提取物制备成纺丝原液,经静电纺丝制备出具有本质抗菌性能的抗菌纤维,再利用天然纤维素纤维与铜离子之间的螯合作用在纤维表面稳固连接一层铜离子,从而使纤维表面构成稳定的抗菌层,所得抗菌聚丙烯腈纤维从表面到内部具有稳定的抗菌性能。(The invention discloses a preparation method of antibacterial polyacrylonitrile fiber, which comprises the following steps; (1) dissolving natural cellulose fibers; (2) dissolving polyacrylonitrile fibers; (3) preparing a spinning solution; (4) carrying out electrostatic spinning treatment; (5) and (5) performing antibacterial post-treatment. The invention relates to a preparation method of antibacterial polyacrylonitrile fiber, which comprises the steps of preparing a spinning solution from natural cellulose fiber with antibacterial property, polyacrylonitrile fiber and natural antibacterial plant extracts, preparing antibacterial fiber with intrinsic antibacterial property through electrostatic spinning, and firmly connecting a layer of copper ions on the surface of the fiber by utilizing the chelation between the natural cellulose fiber and the copper ions, so that the surface of the fiber forms a stable antibacterial layer, and the obtained antibacterial polyacrylonitrile fiber has stable antibacterial property from the surface to the inside.)

1. The preparation method of the antibacterial polyacrylonitrile fiber is characterized by comprising the following steps:

(1) dissolving natural cellulose fibers: under the protection of nitrogen, adding 15-20 parts of chitin fiber and 20-25 parts of bamboo fiber into a flask filled with a first cellulose dissolving solution, and performing activation treatment, stirring dissolving treatment and ultrasonic defoaming treatment to obtain a uniform and stable natural cellulose spinning solution;

(2) dissolving polyacrylonitrile fibers: under the protection of nitrogen, adding 25-35 parts of polyacrylonitrile fibers into the second cellulose dissolving solution, and stirring and dissolving to obtain a polyacrylonitrile spinning solution;

(3) preparing a spinning solution: mixing the natural cellulose spinning solution obtained in the step (1), the polyacrylonitrile spinning solution obtained in the step (2), 10-15 parts of acrylonitrile, 8-12 parts of mint extract, 3-5 parts of radix euphorbiae lantu flower extract, 10-20 parts of sarcandra glabra extract and 5-10 parts of linseed oil to obtain a mixed solution, adding a certain amount of sodium thiocyanate aqueous solution, and mixing to obtain a spinning stock solution;

(4) electrostatic spinning treatment: spinning the spinning stock solution obtained in the step (3) by using an electrostatic spinning machine, and drying by using a vacuum oven to obtain primary antibacterial polyacrylonitrile fibers;

(5) and (3) antibacterial post-treatment: and (4) immersing the nascent antibacterial polyacrylonitrile fiber obtained in the step (4) into a cuprammonium solution for reaction, and drying in vacuum to obtain the antibacterial polyacrylonitrile fiber.

2. The method for preparing the antibacterial polyacrylonitrile fiber according to claim 1, wherein in the step (1), the first cellulose dissolving solution is a mixture of dimethylacetamide and lithium chloride, wherein the weight ratio of the dimethylacetamide to the lithium chloride is 2-3: 1 in a mass ratio; the activation temperature is 100-120 ℃, and the activation time is 1.5-2 h; the conditions of the stirring and dissolving treatment are as follows: firstly stirring for 2-3 hours at the speed of 500-800 r/min under the condition of 80-90 ℃, then stirring and cooling to room temperature at the speed of 300-500 r/min, and then continuously stirring for 1-2 hours at the speed of 200-300 r/min.

3. The preparation method of the antibacterial polyacrylonitrile fiber according to claim 1, wherein in the step (1), the mass of the first cellulose dissolving solution is 5-10 times of the total mass of the chitin fiber and the bamboo fiber.

4. The preparation method of the antibacterial polyacrylonitrile fiber according to claim 1, wherein in the step (2), the first cellulose dissolving solution is dimethylacetamide, and the adding mass of the dimethylacetamide is 5-10 times of the mass of the polyacrylonitrile fiber.

5. The preparation method of the antibacterial polyacrylonitrile fiber according to claim 1, wherein in the step (3), the mass concentration of the sodium thiocyanate aqueous solution is 40-45%, and the adding volume of the sodium thiocyanate aqueous solution is 0.5-1.5 times of the volume of the mixed solution.

6. The method of claim 1, wherein the step of preparing the polyacrylonitrile fiber comprisesIn the step (4), the process conditions of the electrostatic spinning are as follows: the humidity is 45-48%, the temperature is 40-42 ℃, the voltage is 20 kV, the spinning advancing speed is 10-15 multiplied by 10^-4mm/s, and the rotating speed of the receiver is 35-38 r/min.

7. The preparation method of the antibacterial polyacrylonitrile fiber according to the claim 1, wherein in the step (5), the reaction temperature is 35-45 ℃, the reaction time is 30-50 min, and the reaction is manually stirred at the speed of 5-10 r/min; the vacuum drying conditions are as follows: the temperature is 40-50 ℃, the vacuum degree is 0.01-0.03 MPa, and the drying time is 5-10 h.

Technical Field

The invention relates to the field of polyacrylonitrile fibers, in particular to a preparation method of antibacterial polyacrylonitrile fibers.

Background

The polyacrylonitrile has fluffy appearance, soft feeling, good light resistance, weather resistance, elasticity and heat retention, and is called artificial wool. The polyacrylonitrile is the most dominant raw material in wool spinning and artificial fur in China. The excellent performance of the polypropylene wax can be widely applied to the fields of clothes, clothes and industrial fields. The polyacrylonitrile fiber can be spun or blended with natural fiber, or woven into blanket, carpet, etc. according to the requirements of different applications, and can also be blended with cotton, artificial fiber and other synthetic fiber to be woven into various clothes and indoor articles.

The conventional preparation methods of the prior antibacterial polyacrylonitrile fiber comprise antibacterial post-treatment, antibacterial agent surface adhesion, antibacterial agent blending spinning and the like, and the polyacrylonitrile fiber prepared by the methods has excellent antibacterial performance, but has the defects that the antibacterial performance of the two is not durable and the two are easy to elute after washing; the fiber prepared by the third method has few antibacterial components on the surface and limited antibacterial performance.

The research at home and abroad finds that the natural cellulose fiber has good electrostatic spinning performance and can be complexed with copper ions, and the complexing mechanism is as follows: 0H to Cu on cellulose²⁺Providing empty orbitals to bind the two, complexed Cu²⁺The fiber surface stability is good, and the fiber is not easy to migrate.

Disclosure of Invention

The invention mainly solves the technical problem of providing a preparation method of antibacterial polyacrylonitrile fiber, which can solve the problems of the existing antibacterial modified acrylonitrile fiber.

In order to solve the technical problems, the invention adopts a technical scheme that: the preparation method of the antibacterial polyacrylonitrile fiber is characterized by comprising the following steps:

(1) dissolving natural cellulose fibers: under the protection of nitrogen, adding 15-20 parts of chitin fiber and 20-25 parts of bamboo fiber into a flask filled with a first cellulose dissolving solution, and performing activation treatment, stirring dissolving treatment and ultrasonic defoaming treatment to obtain a uniform and stable natural cellulose spinning solution;

(2) dissolving polyacrylonitrile fibers: under the protection of nitrogen, adding 25-35 parts of polyacrylonitrile fibers into the second cellulose dissolving solution, and stirring and dissolving to obtain a polyacrylonitrile spinning solution;

(3) preparing a spinning solution: mixing the natural cellulose spinning solution obtained in the step (1), the polyacrylonitrile spinning solution obtained in the step (2), 10-15 parts of acrylonitrile, 8-12 parts of mint extract, 3-5 parts of radix euphorbiae lantu flower extract, 10-20 parts of sarcandra glabra extract and 5-10 parts of linseed oil to obtain a mixed solution, adding a certain amount of sodium thiocyanate aqueous solution, and mixing to obtain a spinning stock solution;

(4) electrostatic spinning treatment: spinning the spinning stock solution obtained in the step (3) by using an electrostatic spinning machine, and drying by using a vacuum oven to obtain primary antibacterial polyacrylonitrile fibers;

(5) and (3) antibacterial post-treatment: and (4) immersing the nascent antibacterial polyacrylonitrile fiber obtained in the step (4) into a cuprammonium solution for reaction, and drying in vacuum to obtain the antibacterial polyacrylonitrile fiber.

In a preferred embodiment of the present invention, in the step (1), the first cellulose dissolving solution is a mixture of dimethylacetamide and lithium chloride in a weight ratio of 2-3: 1 in a mass ratio; the activation temperature is 100-120 ℃, and the activation time is 1.5-2 h; the conditions of the stirring and dissolving treatment are as follows: firstly stirring for 2-3 hours at the speed of 500-800 r/min under the condition of 80-90 ℃, then stirring and cooling to room temperature at the speed of 300-500 r/min, and then continuously stirring for 1-2 hours at the speed of 200-300 r/min.

In a preferred embodiment of the present invention, in the step (1), the mass of the first cellulose dissolving solution is 5 to 10 times of the total mass of the chitin fibers and the bamboo fibers.

In a preferred embodiment of the present invention, in the step (2), the first cellulose dissolving solution is dimethylacetamide, and an addition mass of the dimethylacetamide is 5 to 10 times of a mass of the polyacrylonitrile fiber.

In a preferred embodiment of the present invention, in the step (3), the mass concentration of the sodium thiocyanate aqueous solution is 40 to 45%, and the adding volume of the sodium thiocyanate aqueous solution is 0.5 to 1.5 times of the volume of the mixed solution.

In a preferred embodiment of the present invention, in the step (4), the process conditions of the electrostatic spinning are as follows: the humidity is 45-48%, the temperature is 40-42 ℃, the voltage is 20 kV, the spinning advancing speed is 10-15 multiplied by 10^-4mm/s, and the rotating speed of the receiver is 35-38 r/min.

In a preferred embodiment of the present invention, in the step (5), the temperature of the reaction is 35 to 45 ℃, the time is 30 to 50min, and the stirring is performed manually at a speed of 5 to 10 r/min; the vacuum drying conditions are as follows: the temperature is 40-50 ℃, the vacuum degree is 0.01-0.03 MPa, and the drying time is 5-10 h.

The invention has the beneficial effects that: the invention relates to a preparation method of antibacterial polyacrylonitrile fiber, which comprises the steps of preparing a spinning solution from natural cellulose fiber with antibacterial property, polyacrylonitrile fiber and natural antibacterial plant extracts, preparing antibacterial fiber with intrinsic antibacterial property through electrostatic spinning, and firmly connecting a layer of copper ions on the surface of the fiber by utilizing the chelation between the natural cellulose fiber and the copper ions, so that the surface of the fiber forms a stable antibacterial layer, and the obtained antibacterial polyacrylonitrile fiber has stable antibacterial property from the surface to the inside.

Detailed Description

The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.

The embodiment of the invention comprises the following steps: