CN111254512A - Antibacterial composite polyvinyl alcohol fiber and preparation method and application thereof - Google Patents
Antibacterial composite polyvinyl alcohol fiber and preparation method and application thereof Download PDFInfo
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- CN111254512A CN111254512A CN202010200387.0A CN202010200387A CN111254512A CN 111254512 A CN111254512 A CN 111254512A CN 202010200387 A CN202010200387 A CN 202010200387A CN 111254512 A CN111254512 A CN 111254512A
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 121
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 121
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 95
- 239000000835 fiber Substances 0.000 title claims abstract description 80
- 239000002131 composite material Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 186
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 102
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 88
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 51
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 51
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 51
- 241001122767 Theaceae Species 0.000 claims abstract description 49
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 49
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 49
- 238000009987 spinning Methods 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 230000001678 irradiating effect Effects 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 16
- 230000001681 protective effect Effects 0.000 claims description 6
- 239000000243 solution Substances 0.000 abstract description 26
- 238000002156 mixing Methods 0.000 abstract description 20
- 230000000052 comparative effect Effects 0.000 description 14
- 229920000742 Cotton Polymers 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229920001817 Agar Polymers 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 238000009960 carding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001332 colony forming effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/001—Treatment with visible light, infrared or ultraviolet, X-rays
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/24—Polymers or copolymers of alkenylalcohols or esters thereof; Polymers or copolymers of alkenylethers, acetals or ketones
Abstract
The invention provides a preparation method of an antibacterial composite polyvinyl alcohol fiber, which comprises the following steps: (1) mixing tea polyphenol with silver nitrate solution to obtain mixed solution A, wherein the mass concentration of silver nitrate is 0.5-3%, and the mass concentration of tea polyphenol is 2.5-4.0%; (2) dissolving polyvinyl alcohol in the mixed solution A, and stirring for 3-5 hours at 80-100 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 5-15: 100; (3) adding graphene, dispersing uniformly, and standing; (4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating under ultraviolet light to obtain the antibacterial composite polyvinyl alcohol fiber. According to the method, the mixed solution of polyvinyl alcohol, tea polyphenol, silver nitrate and lithium chloride is stirred for 3-5 hours at 80-100 ℃, graphene is added for standing and spinning, the antibacterial performance of the antibacterial composite polyvinyl alcohol fiber is improved by irradiation of ultraviolet light, and the non-woven fabric prepared from the antibacterial composite polyvinyl alcohol fiber has better antibacterial performance.
Description
Technical Field
The invention relates to the field of antibacterial fiber materials, in particular to an antibacterial composite polyvinyl alcohol fiber and a preparation method and application thereof.
Background
The non-woven fabric used for the sanitary products is produced by polypropylene fibers, terylene and the like, has strict requirements on temperature during production, high operation difficulty and high overall hardness, and the non-woven fabric produced by ES fibers has the characteristics of fluffiness, softness, high strength, oil absorption, water absorption and the like, can be used for disposable sanitary products such as masks, paper diapers, sanitary towels and the like, but has limited performance and no antibacterial property.
The invention application with the application number of 201911020794.7 discloses a preparation method of high-performance non-woven fabric, which comprises the following steps: step 1, mixing a polymer, a natural antibacterial agent and silver nitrate according to a mass ratio of 3: 1:1, stirring and reacting the obtained mixed system for 2-24 hours at the temperature of 0-15 ℃, and then preparing an antibacterial polymer layer by electrostatic spinning under the conditions of electrostatic voltage of 20-25 kV and distance between a spinneret orifice and a receiving plate of 30-50 cm; step 2, carding and grinding cotton fibers, and flatly placing a cotton fiber layer on the surface of the ES fiber non-woven fabric layer through a carding machine; step 3, performing single-sided or double-sided spunlace process, and solidifying the cotton fibers of the soft cotton layer on the upper surface of the ES fiber non-woven fabric layer; and 4, adhering the antibacterial polymer layer to the ES fiber non-woven fabric layer. However, the application only forms the non-woven fabric after the polymer, the natural antibacterial agent and the silver nitrate are simply mixed to form the spinning solution to prepare the fiber, and the antibacterial performance is poor.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides an antibacterial composite polyvinyl alcohol fiber and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of an antibacterial composite polyvinyl alcohol fiber comprises the following steps:
(1) preparing tea polyphenol, silver nitrate and lithium chloride to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 0.5-3%, the mass concentration of the tea polyphenol is 2.5-4.0%, and the mass concentration of the lithium chloride in the mixed solution A is 0.1-0.5%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3-5 hours at 80-100 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 5-15: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and then standing;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating under ultraviolet light to obtain the antibacterial composite polyvinyl alcohol fiber.
According to the method, the mixed solution of the polyvinyl alcohol, the tea polyphenol, the silver nitrate and the lithium chloride is stirred for 3-5 hours at 80-100 ℃, the graphene is added, standing and spinning are carried out, the antibacterial performance of the antibacterial composite polyvinyl alcohol fiber is improved through irradiation under ultraviolet light, and the antibacterial performance of the non-woven fabric prepared from the antibacterial composite polyvinyl alcohol fiber is better.
Preferably, in the step (3), the standing time is 6-12 hours, in the step (4), the wavelength of the ultraviolet light is 180-250 nm, and the irradiation time of the ultraviolet light is 0.5-1.5 hours.
The inventor finds that the antibacterial composite polyvinyl alcohol fiber prepared under the conditions has better antibacterial effect.
Preferably, in the step (3), the graphene is used in an amount of: the weight ratio of the graphene to the mixed solution A is (0.05-0.2): 100.
The inventor finds that when the weight ratio of the graphene to the mixed solution A is (0.05-0.2): 100, the prepared antibacterial composite polyvinyl alcohol fiber has a better antibacterial effect.
Preferably, in the step (3), the graphene is used in an amount of: the weight ratio of the graphene to the mixed solution A is (0.1-0.15): 100.
The inventor finds that when the weight ratio of the graphene to the mixed solution A is (0.1-0.15): 100, the prepared antibacterial composite polyvinyl alcohol fiber has better antibacterial effect.
Preferably, in the step (1), the mass concentration of the silver nitrate in the mixed solution a is 1% to 2%.
The inventor finds that when the mass concentration of the silver nitrate in the mixed solution A is 1-2%, the prepared antibacterial composite polyvinyl alcohol fiber has a better antibacterial effect.
Preferably, in the step (1), the mass concentration of the silver nitrate in the mixed solution a is 1.5%.
Preferably, in the step (1), the mass concentration of lithium chloride in the mixed solution a is 0.3% to 0.4%.
The inventor finds that when the mass concentration of lithium chloride in the mixed solution A is 0.3-0.4%, the prepared antibacterial composite polyvinyl alcohol fiber has better antibacterial effect.
Preferably, in the step (1), the mass concentration of the tea polyphenol in the mixed solution a is 3.0-3.5%.
The inventor discovers that when the mass concentration of the tea polyphenol in the mixed solution A is 3.0-3.5%, the prepared antibacterial composite polyvinyl alcohol fiber has better antibacterial effect.
Preferably, in the step (2), the weight ratio of the polyvinyl alcohol to the mixed solution A is 8-12: 100.
The inventor finds that when the weight ratio of polyvinyl alcohol to the mixed solution A is 8-12: 100, the prepared antibacterial composite polyvinyl alcohol fiber has a better antibacterial effect.
The invention also provides the antibacterial composite polyvinyl alcohol fiber prepared by any one of the methods.
The invention also provides a non-woven fabric prepared from the antibacterial composite polyvinyl alcohol fiber.
The invention also provides application of the non-woven fabric in medical protective products, wherein the medical protective products comprise a mask, protective clothing and a protective cap.
The invention has the beneficial effects that: the invention provides an antibacterial composite polyvinyl alcohol fiber and a preparation method and application thereof.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 2
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 0.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 3
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 4
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 2%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 5
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 2.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 6
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 2.5%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 7
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 3.5%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 8
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 4.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 9
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.05: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 10
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.15: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 11
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.2: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 12
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 8: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Example 13
The preparation method of the antibacterial composite polyvinyl alcohol fiber provided by the embodiment of the invention comprises the following steps:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Comparative example 1
A method for preparing an antibacterial composite polyvinyl alcohol fiber as a comparative example of the present invention, the method comprising the steps of:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3) to obtain the antibacterial composite polyvinyl alcohol fiber.
Comparative example 2
A method for preparing an antibacterial composite polyvinyl alcohol fiber as a comparative example of the present invention, the method comprising the steps of:
(1) mixing silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, and the mass concentration of the lithium chloride in the mixed solution A is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the silver nitrate solution is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Comparative example 3
A method for preparing an antibacterial composite polyvinyl alcohol fiber as a comparative example of the present invention, the method comprising the steps of:
(1) mixing tea polyphenol with a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the tea polyphenol in the mixed solution A is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in a tea polyphenol solution to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the tea polyphenol solution is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Comparative example 4
A method for preparing an antibacterial composite polyvinyl alcohol fiber as a comparative example of the present invention, the method comprising the steps of:
(1) mixing tea polyphenol, silver nitrate and a lithium chloride solution to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 1.5%, the mass concentration of the tea polyphenol is 3.0%, and the mass concentration of the lithium chloride is 0.3%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) standing the mixed solution B for 8 hours;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Comparative example 5
A method for preparing an antibacterial composite polyvinyl alcohol fiber as a comparative example of the present invention, the method comprising the steps of:
(1) mixing tea polyphenol and a silver nitrate solution to obtain a mixed solution A, wherein the mass concentration of silver nitrate in the mixed solution A is 1.5%, and the mass concentration of tea polyphenol is 3.0%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3 hours at 90 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 12: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and standing for 8 hours; the weight ratio of the graphene to the mixed solution A is 0.1: 100;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating for 40 minutes under the ultraviolet light of 180-250 nm to obtain the antibacterial composite polyvinyl alcohol fiber.
Effect example 1
The antibacterial composite polyvinyl alcohol fibers of examples 1 to 13 and comparative examples 1 to 5 were prepared as nonwoven fabric samples, respectively, and two bacterial strains were evaluated by the agar diffusion method according to the national standard GB/T20944.1-2007: coli and s.
The nonwoven fabric sample was cut into a circle with a diameter of 20mm and sterilized in a clean bench with ultraviolet light for 30 min. Will contain 1X 105Luria Broth (LB) agar plates of individual colony forming units (CFU/mL) bacteria were used for the culture. After incubation for 24h at 37 ℃, the diameter of the inhibition zone was evaluated, and the inhibition rate was calculated, with the results shown in table 1;
TABLE 1 bacteriostasis rates of nonwoven fabric samples
As can be seen from Table 1, comparative example 1 and comparative example 1 show that irradiation for 40 minutes under ultraviolet light of 180-250 nm after spinning has an important effect on improving the antibacterial performance of the antibacterial composite polyvinyl alcohol fiber; by comparing the example 1 and the comparative examples 2 to 5, it is shown that silver nitrate, tea polyphenol, graphene and lithium chloride are indispensable in improving the antibacterial performance of the antibacterial composite polyvinyl alcohol fiber, and a synergistic effect is achieved; through comparison between the embodiment 1 and the embodiment 5, the antibacterial effect of the prepared antibacterial composite polyvinyl alcohol fiber is better when the mass concentration of silver nitrate in the mixed solution A is 1.0-2%; by comparing the example 1 with the examples 6 to 8, the antibacterial effect of the prepared antibacterial composite polyvinyl alcohol fiber is better when the mass concentration of the tea polyphenol in the mixed solution A is 3.0 to 3.5 percent; by comparing example 1 and examples 9 to 11, it is demonstrated that the antibacterial effect of the prepared antibacterial composite polyvinyl alcohol fiber is better when the weight ratio of graphene to the mixed solution A is (0.1-0.15): 100.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation method of the antibacterial composite polyvinyl alcohol fiber is characterized by comprising the following steps of:
(1) preparing tea polyphenol, silver nitrate and lithium chloride to obtain a mixed solution A, wherein the mass concentration of the silver nitrate in the mixed solution A is 0.5-3%, the mass concentration of the tea polyphenol in the mixed solution A is 2.5-4.0%, and the mass concentration of the lithium chloride in the mixed solution A is 0.1-0.5%;
(2) dissolving polyvinyl alcohol in the mixed solution A to obtain a mixed solution B, and stirring for 3-5 hours at 80-100 ℃, wherein the weight ratio of the polyvinyl alcohol to the mixed solution A is 5-15: 100;
(3) adding graphene into the mixed solution B, uniformly dispersing, and then standing;
(4) and (4) spinning the mixed solution obtained in the step (3), and then irradiating under ultraviolet light to obtain the antibacterial composite polyvinyl alcohol fiber.
2. The preparation method of the antibacterial composite polyvinyl alcohol fiber according to claim 1, wherein in the step (3), the standing time is 6-12 hours, in the step (4), the wavelength of the ultraviolet light is 180-250 nm, and the irradiation time of the ultraviolet light is 0.5-1.5 hours.
3. The method for preparing antibacterial composite polyvinyl alcohol fiber according to claim 1, wherein in the step (3), the graphene is used in an amount of: the weight ratio of the graphene to the mixed solution A is (0.05-0.2): 100.
4. The method for preparing antibacterial composite polyvinyl alcohol fiber according to claim 1, wherein in the step (3), the graphene is used in an amount of: the weight ratio of the graphene to the mixed solution A is (0.1-0.15): 100.
5. The method for preparing antibacterial composite polyvinyl alcohol fibers according to claim 1, wherein in the step (1), the mass concentration of silver nitrate in the mixed solution A is 1-2%.
6. The method for preparing antibacterial composite polyvinyl alcohol fibers according to claim 1, wherein in the step (1), the mass concentration of lithium chloride in the mixed solution A is 0.3-0.4%.
7. The method for preparing antibacterial composite polyvinyl alcohol fiber according to claim 1, wherein in the step (1), the mass concentration of tea polyphenol in the mixed solution A is 3.0-3.5%; in the step (2), the weight ratio of the polyvinyl alcohol to the mixed solution A is 8-12: 100.
8. An antibacterial composite polyvinyl alcohol fibre prepared by the method of any one of claims 1 to 7.
9. A nonwoven fabric produced from the antibacterial conjugate polyvinyl alcohol fiber according to claim 8.
10. Use of the nonwoven fabric of claim 9 in medical shields including masks, protective clothing and protective headgear.
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