CN110592713B - Preparation method of antibacterial polyacrylonitrile fiber - Google Patents
Preparation method of antibacterial polyacrylonitrile fiber Download PDFInfo
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- CN110592713B CN110592713B CN201910441334.5A CN201910441334A CN110592713B CN 110592713 B CN110592713 B CN 110592713B CN 201910441334 A CN201910441334 A CN 201910441334A CN 110592713 B CN110592713 B CN 110592713B
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- polyacrylonitrile
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/06—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/08—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Artificial Filaments (AREA)
Abstract
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.
Description
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:
example 1
The invention discloses a preparation method of antibacterial polyacrylonitrile fibers, which comprises the following steps:
(1) dissolving natural cellulose fibers: under the protection of nitrogen, adding 15 parts of chitin fiber and 20 parts of bamboo fiber into a dimethylacetamide solution, heating to 100 ℃ under the condition of reflux condensation, and activating for 2 hours; then stopping heating, cooling to 80 ℃, quickly adding a certain amount of anhydrous LiCl powder, stirring for 3 hours at the speed of 500r/min, then stirring and cooling to room temperature at the speed of 300r/min, and continuing stirring for 2 hours at the speed of 200 r/min; finally, ultrasonic defoaming is carried out to prepare uniform and stable cellulose spinning solution;
wherein the mass ratio of the dimethylacetamide to the lithium chloride is 2: 1; the mass (the total mass of dimethylacetamide and lithium chloride) of the first cellulose dissolving solution is 5 times of the total mass of the chitin fibers and the bamboo fibers;
(2) dissolving polyacrylonitrile fibers: under the protection of nitrogen, adding 25 parts of polyacrylonitrile fiber into dimethyl acetamide which is a second cellulose dissolving solution, and stirring and dissolving to obtain a polyacrylonitrile spinning solution;
wherein the adding mass of the dimethylacetamide is 5 times of the mass of the polyacrylonitrile fiber;
(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 parts of acrylonitrile, 8 parts of mint extract, 3 parts of radix euphorbiae lantu flower extract, 10 parts of sarcandra glabra extract and 5 parts of linseed oil to obtain a mixed solution, adding a sodium thiocyanate aqueous solution with the mass concentration of 40% which is 1.5 times of the volume of the mixed 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; the electrostatic spinning process conditions are as follows: humidity of 45-48%, and temperature40-42 ℃, 20 kV voltage and 10-15 multiplied by 10 spinning advancing speed-4mm/s, and the rotating speed of the receiver is 35-38 r/min;
(5) and (3) antibacterial post-treatment: and (3) immersing the primary antibacterial polyacrylonitrile fiber obtained in the step (4) into a copper ammonia solution, reacting for 50min by manually and gently stirring at the speed of 5r/min under the condition that the temperature is 35 ℃, and then drying for 10h under the low-temperature vacuum degree of 40 ℃ and the vacuum degree of 0.01MPa to obtain the antibacterial polyacrylonitrile fiber.
Example 2
The invention discloses a preparation method of antibacterial polyacrylonitrile fibers, which comprises the following steps:
(1) dissolving natural cellulose fibers: under the protection of nitrogen, adding 20 parts of chitin fiber and 25 parts of bamboo fiber into a dimethylacetamide solution, heating to 120 ℃ under the condition of reflux condensation, and activating for 1.5 hours; then stopping heating, cooling to 90 ℃, quickly adding a certain amount of anhydrous LiCl powder, stirring at the speed of 800r/min for 2h, then stirring at the speed of 500r/min, cooling to room temperature, and continuing stirring at the speed of 300r/min for 1 h; finally, ultrasonic defoaming is carried out to prepare uniform and stable cellulose spinning solution;
wherein the mass ratio of the dimethylacetamide to the lithium chloride is 3: 1; the mass (the total mass of dimethylacetamide and lithium chloride) of the first cellulose dissolving solution is 10 times of the total mass of the chitin fibers and the bamboo fibers;
(2) dissolving polyacrylonitrile fibers: under the protection of nitrogen, adding 35 parts of polyacrylonitrile fibers into dimethyl acetamide which is a second cellulose dissolving solution, and stirring and dissolving to obtain a polyacrylonitrile spinning solution;
wherein the adding mass of the dimethylacetamide is 10 times of the mass of the polyacrylonitrile fiber;
(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), 15 parts of acrylonitrile, 12 parts of mint extract, 5 parts of radix euphorbiae lantu flower extract, 20 parts of sarcandra glabra extract and 10 parts of linseed oil to obtain a mixed solution, adding a 45 mass percent sodium thiocyanate aqueous solution which is 0.5 time of the volume of the mixed 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; the electrostatic spinning process conditions 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;
(5) and (3) antibacterial post-treatment: and (3) immersing the primary antibacterial polyacrylonitrile fiber obtained in the step (4) into a copper ammonia solution, carrying out manual gentle stirring reaction at the speed of 10r/min for 30min at the temperature of 45 ℃, and then drying for 5h at the low temperature of 50 ℃ and the vacuum degree of 0.03MPa to obtain the antibacterial polyacrylonitrile fiber.
Tests show that the antibacterial polyacrylonitrile fiber obtained by the method has broad-spectrum antibacterial property, the antibacterial rate to staphylococcus aureus is more than 90%, the antibacterial rate to escherichia coli is more than 85%, the breaking strength is higher than 4.0cN/dtex, the performance change after washing for 50 times is less than 2%, and the antibacterial polyacrylonitrile fiber has excellent antibacterial stability.
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.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (1)
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; the first cellulose dissolving solution is prepared by mixing dimethyl acetamide and lithium chloride in a 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 at the temperature 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; the mass of the first cellulose dissolving solution is 5-10 times of the total mass of the chitin fibers and the bamboo fibers;
(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; the second cellulose dissolving solution is dimethylacetamide, and the adding mass of the dimethylacetamide is 5-10 times of the mass of the polyacrylonitrile fiber;
(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; 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;
(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; the electrostatic spinning process conditions 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 35-38r/min；
(5) And (3) antibacterial post-treatment: immersing the primary antibacterial polyacrylonitrile fiber obtained in the step (4) into a copper ammonia solution for reaction, and performing vacuum drying to obtain the antibacterial polyacrylonitrile fiber; 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.
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| CN112813524B (en) * | 2021-01-09 | 2022-07-12 | 青岛邦特生态纺织科技有限公司 | Acrylic fiber containing plant source extract and collagen micro powder and preparation method thereof |
| CN115182064B (en) * | 2021-04-01 | 2023-12-22 | 中国石油天然气股份有限公司 | Plant antibacterial acrylic fiber and production method thereof |
| CN115747996B (en) * | 2022-11-04 | 2024-03-05 | 苏州大学 | Modified acrylic fiber based on polyelectrolyte compound and preparation method thereof |
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| CN1467314A (en) * | 2003-06-12 | 2004-01-14 | 东南大学 | Antibiotic nanometer fibrous material and method for preparing the same |
| CN1807712A (en) * | 2006-02-09 | 2006-07-26 | 东华大学 | Process for preparing antibacterial polyacrylonitrile fiber |
| CN101240468A (en) * | 2008-03-14 | 2008-08-13 | 东华大学 | Polyacrylonitrile-chitin composite fiber and its production process |
| CN104294479B (en) * | 2014-09-05 | 2018-03-30 | 上海工程技术大学 | A kind of native cellulose/polyacrylonitrile nano anti-bacterial fibre film and preparation method thereof |
| CN105332076B (en) * | 2015-12-02 | 2016-10-26 | 山传雷 | A kind of Folium Menthae extract menthol cool feeling material composite modified additive and application thereof |
| CN106995943B (en) * | 2017-03-24 | 2018-08-07 | 青岛邦特生态纺织科技有限公司 | A kind of Chloranthus glaber efficient antibacterial antiviral cellulose fibre and preparation method thereof |
| CN108301060A (en) * | 2018-03-05 | 2018-07-20 | 厦门安踏体育用品有限公司 | Mint extract microcapsules, acrylic fiber, fabric and relevant preparation method |
| CN108691024A (en) * | 2018-06-29 | 2018-10-23 | 百事基材料（青岛）股份有限公司 | Modified acrylic fibres and preparation method thereof containing plant extracts |
| CN108642714A (en) * | 2018-07-13 | 2018-10-12 | 合肥洁诺医疗用品有限公司 | A kind of disposable medical sheet non-woven fabrics |
| CN109371499A (en) * | 2018-10-30 | 2019-02-22 | 中科纺织研究院（青岛）有限公司 | A kind of plant modified dacron fabric and preparation method thereof |
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