CN113388917A - Modified silk moisture-conducting antibacterial fabric and preparation method thereof - Google Patents

Modified silk moisture-conducting antibacterial fabric and preparation method thereof Download PDF

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CN113388917A
CN113388917A CN202110574897.9A CN202110574897A CN113388917A CN 113388917 A CN113388917 A CN 113388917A CN 202110574897 A CN202110574897 A CN 202110574897A CN 113388917 A CN113388917 A CN 113388917A
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modified
silk
essential oil
tea tree
raw material
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沈建海
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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
    • 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
    • D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin 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
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • 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
    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/52—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with selenium, tellurium, polonium or their compounds; with sulfur, dithionites or compounds containing sulfur and halogens, with or without oxygen; by sulfohalogenation with chlorosulfonic acid; by sulfohalogenation with a mixture of sulfur dioxide and free halogens
    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/005—Compositions containing perfumes; Compositions containing deodorants
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
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    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • 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
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/10—Animal fibres
    • 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
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a modified silk moisture-conducting antibacterial fabric and a preparation method thereof, and relates to the field of fabrics, wherein the silk and essential oil extracts are combined more tightly by carrying out microwave activation treatment and crosslinking fixation treatment, and then the silk and the essential oil extracts are fixed by a crosslinking agent, so that the antibacterial effect can be played for a longer time, the silk is modified by polymer emulsion, the polymer emulsion can form a net-shaped high-strength and toughness layer structure on the surface of the silk under the condition of negative pressure, the essential oil extracts can be further cured on the one hand, and the toughness and the strength of the silk can be greatly enhanced on the other hand, the modified fibers adopted by the embodiment of the invention are modified fibers subjected to surface micropore modification treatment, and the moisture absorption and the moisture discharge of the fibers can be fully improved by carrying out the surface micropore modification treatment on the fibers, the fabric has excellent comfort and air permeability.

Description

Modified silk moisture-conducting antibacterial fabric and preparation method thereof
Technical Field
The invention relates to the technical field of fabrics, in particular to a modified silk moisture-conducting antibacterial fabric and a preparation method thereof.
Background
The silk fabric is excellent in skin-friendly performance, comfortable to wear after being used for manufacturing the fabric, and the existing fabric part has an antibacterial effect, but the antibacterial active components are easy to dissipate, the antibacterial effect is poor, and the antibacterial aging is short, so that the modified silk moisture-conducting antibacterial fabric and the preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide a modified silk moisture-conducting antibacterial fabric and a preparation method thereof, and aims to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
the modified silk moisture-conducting antibacterial fabric comprises the following raw materials in parts by weight: 10-100 parts of modified silk, 10-100 parts of modified fiber, 10-30 parts of essential oil extract, 5-20 parts of cross-linking agent, 5-30 parts of polymer emulsion, 20-50 parts of polyethylene aminoethyl ester, 20-60 parts of polyethylene resin and 10-30 parts of ethyl acetate; the preparation method of the modified silk comprises the following steps: uniformly mixing silk and essential oil extract, and performing microwave activation for 1-5 min; placing the mixture of silk and essential oil extracts subjected to microwave activation treatment into a cross-linking agent solution, and performing cross-linking fixation under the condition of stirring; and (2) performing solid-liquid separation on the mixture after the crosslinking fixation, placing the solid part in a sealed container, vacuumizing by using a vacuum pump until the negative pressure is 0.1-0.3MPa, then injecting polymer emulsion with the solid content of 30-40% into the container, standing for 1-2h under the condition of keeping stable negative pressure, and fishing out the solid of the mixture after standing for 2 days under the conditions that the relative humidity is 50% and the temperature is 24 ℃ to obtain the modified silk.
As a further scheme of the invention: the cross-linking agent is a 3% chitin solution, and the temperature in the cross-linking process is 50 ℃; the polymer emulsion is polyvinyl alcohol emulsion.
As a still further scheme of the invention: the preparation method of the essential oil extract comprises the following steps: crushing tea tree wood by adopting a low-temperature gas explosion method to obtain tea tree powder; putting the tea tree powder into a filter bag, placing the filter bag into an extraction tank, and introducing a liquid solvent into the extraction tank from a solvent tank for extraction to obtain crude tea tree oil; distilling the crude tea tree oil under reduced pressure to obtain tea tree essential oil; dispersing the tea tree essential oil in a compound solution of sodium alginate and sodium caseinate which is 10 times of the volume of the tea tree essential oil, homogenizing for 15min under the condition of 1000r/min to obtain tea tree essential oil microparticles, adding the tea tree essential oil microparticles into a calcium lactate solution with the concentration of 1%, and stirring for 30min to obtain a solidified essential oil extract in a microparticle form.
As a still further scheme of the invention: the compound solution of sodium alginate and sodium caseinate is a sodium alginate solution with the mass concentration of 2% and a sodium caseinate solution with the mass concentration of 1% according to the volume ratio of 5: 1 to form a compound solution.
As a still further scheme of the invention: the preparation method of the modified fiber comprises the following steps: taking polyester as a raw material, slicing, drying and melting to obtain a molten liquid; mixing sodium dihydrogen phosphate into the molten liquid, performing blended spinning and post-processing to obtain modified fibers with modified surface micropores; the temperature of the blended spinning is controlled at 300 ℃ and the pressure is 10 MPa.
As a still further scheme of the invention: the modified silk and modified fiber raw materials are subjected to sterilization treatment before modification treatment, and the sterilization treatment specifically comprises the following steps: humidifying the modified silk raw material and the modified fiber raw material to enable the water content of the modified silk raw material and the water content of the modified fiber raw material to be 20-30%; uniformly laying the humidified modified silk raw material and modified fiber raw material for electron beam radiation treatment, wherein the electron beam radiation dose is controlled to be 2-5kGy, and the radiation time is 5-10 s; placing the modified silk raw material and the modified fiber raw material subjected to electron beam radiation treatment in an alkaline bactericide with the mass fraction of 5-10%, uniformly stirring, placing in an autoclave for inactivation for 50min at 120 ℃, then performing ultrasonic treatment for 1-2h, finally performing solid-liquid separation, and washing solid content to obtain the modified silk raw material and the modified fiber raw material subjected to sterilization treatment.
As a still further scheme of the invention: the alkaline bactericide is lime sulfur or Bordeaux mixture.
As a still further scheme of the invention: the preparation method of the modified silk moisture-conducting antibacterial fabric comprises the following steps: mixing polyethylene aminoethyl ester, polyethylene resin and ethyl acetate, heating to melt, adding modified silk and modified fiber, stirring uniformly, and putting into a spinneret plate to extrude to form single fibers; and then weaving the fibers into the fabric.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, microwave activation treatment is firstly carried out to carry out crosslinking and fixing treatment so that the silk and the essential oil extract are combined more tightly, then the silk and the essential oil extract are fixed through a crosslinking agent, so that the bacteriostatic action can be played for a longer time, the silk is modified through the polymer emulsion, the polymer emulsion can form a reticular high-strength and high-toughness layer structure on the surface of the silk under the condition of negative pressure, the essential oil extract can be further solidified on the one hand, the toughness and the strength of the silk can be greatly enhanced on the other hand, the tea tree essential oil has good bacteriostatic activity, the bacteriostatic effect of the silk can be greatly improved by adding the polymer emulsion into the silk, so that the antibacterial capability of the fabric is improved, and in the invention, purified tea tree microparticles are solidified, and then are better attached to the surface of the silk, and meanwhile, the tea tree essential oil extract after the microparticle solidification is more stable and is not easy to dissipate, and has longer action time and antibacterial effect.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a modified silk moisture-conducting antibacterial fabric which comprises the following raw materials in parts by weight: 10-100 parts of modified silk, 10-100 parts of modified fiber, 10-30 parts of essential oil extract, 5-20 parts of cross-linking agent, 5-30 parts of polymer emulsion, 20-50 parts of polyethylene aminoethyl ester, 20-60 parts of polyethylene resin and 10-30 parts of ethyl acetate; the preparation method of the modified silk comprises the following steps: uniformly mixing silk and essential oil extract, and performing microwave activation for 1-5 min; placing the mixture of silk and essential oil extracts subjected to microwave activation treatment into a cross-linking agent solution, and performing cross-linking fixation under the condition of stirring; and (2) performing solid-liquid separation on the mixture after the crosslinking fixation, placing the solid part in a sealed container, vacuumizing by using a vacuum pump until the negative pressure is 0.1-0.3MPa, then injecting polymer emulsion with the solid content of 30-40% into the container, standing for 1-2h under the condition of keeping stable negative pressure, and fishing out the solid of the mixture after standing for 2 days under the conditions that the relative humidity is 50% and the temperature is 24 ℃ to obtain the modified silk.
In the embodiment of the invention, the silk and the essential oil extract are combined more tightly by carrying out microwave activation treatment and crosslinking fixation treatment, then the silk and the essential oil extract are fixed by a crosslinking agent, so that the bacteriostatic action can be carried out for a longer time, the silk is modified by the polymer emulsion, the polymer emulsion can form a reticular high-strength toughness layer structure on the surface of the silk under the condition of negative pressure, the essential oil extract can be further cured on one hand, and the toughness and the strength of the silk can be greatly enhanced on the other hand.
In the embodiment of the invention, the cross-linking agent is a 3% chitin solution, and the temperature in the cross-linking process is 50 ℃. The polymer emulsion is polyvinyl alcohol emulsion.
In the embodiment of the invention, the preparation method of the essential oil extract comprises the following steps: crushing tea tree wood by adopting a low-temperature gas explosion method to obtain tea tree powder; putting the tea tree powder into a filter bag, placing the filter bag into an extraction tank, and introducing a liquid solvent into the extraction tank from a solvent tank for extraction to obtain crude tea tree oil; distilling the crude tea tree oil under reduced pressure to obtain tea tree essential oil; dispersing the tea tree essential oil in a compound solution of sodium alginate and sodium caseinate which is 10 times of the volume of the tea tree essential oil, homogenizing for 15min at the speed of 1000r/min to obtain tea tree essential oil microparticles, adding the tea tree essential oil microparticles into a calcium lactate solution with the concentration of 1%, and stirring for 30min to obtain a solidified essential oil extract in a microparticle form; the compound solution of sodium alginate and sodium caseinate is a sodium alginate solution with the mass concentration of 2% and a sodium caseinate solution with the mass concentration of 1% according to the volume ratio of 5: 1 to form a compound solution.
In the embodiment of the invention, the tea tree essential oil has good bacteriostatic activity, the bacteriostatic effect of silk can be greatly improved by adding the tea tree essential oil into the silk for use, so that the antibacterial capability of the fabric is improved, the purified tea tree essential oil microparticles are solidified and then are better attached to the surface of the silk, and meanwhile, the tea tree essential oil extract solidified by the microparticles is more stable and is not easy to dissipate, and has longer action time and bacteriostatic effect.
In the embodiment of the invention, the preparation method of the modified fiber comprises the following steps: taking polyester as a raw material, slicing, drying and melting to obtain a molten liquid; mixing sodium dihydrogen phosphate into the molten liquid, performing blended spinning and post-processing to obtain modified fibers with modified surface micropores; the temperature of the blended spinning is controlled at 300 ℃ and the pressure is 10 MPa.
In the embodiment of the invention, the moisture absorption and moisture removal performance of the fiber can be fully improved by carrying out surface micropore modification treatment on the modified fiber, so that the fabric has excellent comfort and air permeability, and the chemical structure, the microstructure and the surface morphological structure of the fiber are the key for determining the moisture absorption capacity. The more hydrophilic groups on the fiber, the more polar the groups, and the better the moisture absorption capacity of the fiber. Most synthetic fibers are made of nonpolar high polymer materials, and the hygroscopicity is poor; because the internal molecules are arranged closely and hydrophilic structures are lacked among the molecules, the moisture regain is low, the moisture absorption performance is poor, and the clothes are stuffy and hot to wear, airtight and poor in comfort. The modified fiber adopted by the embodiment of the invention is the modified fiber subjected to surface micropore modification treatment, and the moisture absorption and moisture removal performance of the fiber can be fully improved by performing the surface micropore modification treatment on the fiber, so that the fabric has excellent comfort and air permeability.
In the embodiment of the invention, the raw materials of the modified silk and the modified fiber are sterilized before modification, and the sterilization treatment specifically comprises the following steps: humidifying the modified silk raw material and the modified fiber raw material to enable the water content of the modified silk raw material and the water content of the modified fiber raw material to be 20-30%; uniformly laying the humidified modified silk raw material and modified fiber raw material for electron beam radiation treatment, wherein the electron beam radiation dose is controlled to be 2-5kGy, and the radiation time is 5-10 s; placing the modified silk raw material and the modified fiber raw material subjected to electron beam radiation treatment in an alkaline bactericide with the mass fraction of 5-10%, uniformly stirring, placing in an autoclave for inactivation for 50min at 120 ℃, then performing ultrasonic treatment for 1-2h, finally performing solid-liquid separation, and washing solid content to obtain the modified silk raw material and the modified fiber raw material subjected to sterilization treatment.
In the embodiment of the invention, the raw materials of modified silk and modified fiber are subjected to electron beam radiation treatment firstly, so that the bacterial activity can be effectively reduced, humidification treatment is carried out before treatment to enhance the radiation treatment effect, meanwhile, certain protection treatment is carried out on the raw materials to prevent the radiation treatment from damaging the structure of the raw materials, and then the raw materials are subjected to bactericide, high temperature and ultrasonic inactivation to achieve more thorough sterilization.
In the embodiment of the invention, the alkaline bactericide is lime sulphur or Bordeaux mixture.
In the embodiment of the invention, the preparation method of the modified silk moisture-conducting antibacterial fabric comprises the following steps: mixing polyethylene aminoethyl ester, polyethylene resin and ethyl acetate, heating to melt, adding modified silk and modified fiber, stirring uniformly, and putting into a spinneret plate to extrude to form single fibers; and then weaving the fibers into the fabric.
Examples of certain embodiments of the invention are given below, which are not intended to limit the scope of the invention.
In addition, it should be noted that the numerical values given in the following examples are as precise as possible, but those skilled in the art will understand that each numerical value should be understood as a divisor rather than an absolutely exact numerical value due to measurement errors and experimental operational problems that cannot be avoided. For example, with respect to the weight values of the respective raw materials in the high toughness modified plastics of the respective examples, it should be understood that they may have an error of. + -. 2% or. + -. 1% due to an error of a weighing instrument.
Example 1
In this embodiment, the modified silk moisture-conducting and antibacterial fabric comprises the following raw materials by weight: 100 parts of modified silk, 10 parts of modified fiber, 10 parts of essential oil extract, 5 parts of cross-linking agent, 5 parts of polyvinyl alcohol emulsion, 20 parts of polyethylene aminoethyl ester, 20 parts of polyethylene resin and 10 parts of ethyl acetate;
sterilizing the raw materials, and humidifying the modified silk raw materials and the modified fiber raw materials to ensure that the water content of the modified silk raw materials and the modified fiber raw materials is 20%; uniformly laying the humidified modified silk raw material and modified fiber raw material for electron beam radiation treatment, wherein the electron beam radiation dose is controlled to be 2kGy, and the radiation time is 5 s; placing the modified silk raw material and the modified fiber raw material subjected to electron beam radiation treatment into a lime sulfur mixture with the mass fraction of 10%, uniformly stirring, placing into an autoclave for inactivation for 50min at 120 ℃, then performing ultrasonic treatment for 2h, finally performing solid-liquid separation, and washing solid content with water to obtain the modified silk raw material and the modified fiber raw material subjected to sterilization treatment for later use.
Preparing an essential oil extract: crushing tea tree wood by adopting a low-temperature gas explosion method to obtain tea tree powder; putting the tea tree powder into a filter bag, placing the filter bag into an extraction tank, and introducing a liquid solvent into the extraction tank from a solvent tank for extraction to obtain crude tea tree oil; distilling the crude tea tree oil under reduced pressure to obtain tea tree essential oil; dispersing the tea tree essential oil into a compound solution of sodium alginate and sodium caseinate, wherein the volume of the compound solution is 10 times that of the tea tree essential oil, and the compound solution of sodium alginate and sodium caseinate is a sodium alginate solution with the mass concentration of 2% and a sodium caseinate solution with the mass concentration of 1% according to the volume ratio of 5: 1, homogenizing for 15min at 1000r/min to obtain tea tree essential oil microparticles, adding the tea tree essential oil microparticles into 1% calcium lactate solution, and stirring for 30min to obtain solidified essential oil extract in microparticle form.
Preparing modified silk: uniformly mixing silk and essential oil extract, and performing microwave activation treatment for 3 min; placing the mixture of silk and essential oil extract subjected to microwave activation treatment in a 3% chitin solution, and performing crosslinking fixation under stirring at 50 deg.C; and (2) performing solid-liquid separation on the mixture after the crosslinking fixation, placing the solid part in a sealed container, vacuumizing by using a vacuum pump until the negative pressure is 0.3MPa, then injecting polyvinyl alcohol emulsion with the solid content of 40% into the container, standing for 2 hours under the condition of keeping stable negative pressure, taking out the solid of the mixture after standing, and maintaining for 2 days under the conditions that the relative humidity is 50% and the temperature is 24 ℃ to obtain the modified silk for later use.
Preparing modified fibers: taking polyester as a raw material, slicing, drying and melting to obtain a molten liquid; mixing sodium dihydrogen phosphate into the molten liquid, performing blended spinning and post-processing to obtain modified fibers with modified surface micropores; the temperature of the blended spinning is controlled at 300 ℃ and the pressure is 10 MPa.
Mixing polyethylene aminoethyl ester, polyethylene resin and ethyl acetate, heating to melt, adding modified silk and modified fiber, stirring uniformly, and putting into a spinneret plate to extrude to form single fibers; and then weaving the fibers into the fabric.
Example 2
In this embodiment, the modified silk moisture-conducting and antibacterial fabric comprises the following raw materials by weight: 50 parts of modified silk, 50 parts of modified fiber, 20 parts of essential oil extract, 10 parts of cross-linking agent, 15 parts of polyvinyl alcohol emulsion, 30 parts of polyvinyl aminoethyl ester, 30 parts of polyethylene resin and 20 parts of ethyl acetate;
sterilizing the raw materials, and humidifying the modified silk raw materials and the modified fiber raw materials to ensure that the water content of the modified silk raw materials and the modified fiber raw materials is 20%; uniformly paving the humidified modified silk raw material and modified fiber raw material for electron beam radiation treatment, wherein the electron beam radiation dose is controlled to be 3kGy, and the radiation time is 8 s; placing the modified silk raw material and the modified fiber raw material subjected to electron beam radiation treatment into 10 mass percent Bordeaux mixture, uniformly stirring, placing into an autoclave for inactivation for 50min at 120 ℃, then performing ultrasonic treatment for 2h, finally performing solid-liquid separation, and washing solid content with water to obtain the modified silk raw material and the modified fiber raw material subjected to sterilization treatment for later use.
Preparing an essential oil extract: crushing tea tree wood by adopting a low-temperature gas explosion method to obtain tea tree powder; putting the tea tree powder into a filter bag, placing the filter bag into an extraction tank, and introducing a liquid solvent into the extraction tank from a solvent tank for extraction to obtain crude tea tree oil; distilling the crude tea tree oil under reduced pressure to obtain tea tree essential oil; dispersing the tea tree essential oil into a compound solution of sodium alginate and sodium caseinate, wherein the volume of the compound solution is 10 times that of the tea tree essential oil, and the compound solution of sodium alginate and sodium caseinate is a sodium alginate solution with the mass concentration of 2% and a sodium caseinate solution with the mass concentration of 1% according to the volume ratio of 5: 1, homogenizing for 15min at 1000r/min to obtain tea tree essential oil microparticles, adding the tea tree essential oil microparticles into 1% calcium lactate solution, and stirring for 30min to obtain solidified essential oil extract in microparticle form.
Preparing modified silk: uniformly mixing silk and essential oil extract, and performing microwave activation treatment for 3 min; placing the mixture of silk and essential oil extract subjected to microwave activation treatment in a 3% chitin solution, and performing crosslinking fixation under stirring at 50 deg.C; and (2) performing solid-liquid separation on the mixture after the crosslinking fixation, placing the solid part in a sealed container, vacuumizing by using a vacuum pump until the negative pressure is 0.3MPa, then injecting polyvinyl alcohol emulsion with the solid content of 40% into the container, standing for 2 hours under the condition of keeping stable negative pressure, taking out the solid of the mixture after standing, and maintaining for 2 days under the conditions that the relative humidity is 50% and the temperature is 24 ℃ to obtain the modified silk for later use.
Preparing modified fibers: taking polyester as a raw material, slicing, drying and melting to obtain a molten liquid; mixing sodium dihydrogen phosphate into the molten liquid, performing blended spinning and post-processing to obtain modified fibers with modified surface micropores; the temperature of the blended spinning is controlled at 300 ℃ and the pressure is 10 MPa.
Mixing polyethylene aminoethyl ester, polyethylene resin and ethyl acetate, heating to melt, adding modified silk and modified fiber, stirring uniformly, and putting into a spinneret plate to extrude to form single fibers; and then weaving the fibers into the fabric.
Example 3
In this embodiment, the modified silk moisture-conducting and antibacterial fabric comprises the following raw materials by weight: 10 parts of modified silk, 100 parts of modified fiber, 30 parts of essential oil extract, 20 parts of cross-linking agent, 30 parts of polyvinyl alcohol emulsion, 50 parts of polyethylene aminoethyl ester, 60 parts of polyethylene resin and 30 parts of ethyl acetate;
sterilizing the raw materials, and humidifying the modified silk raw materials and the modified fiber raw materials to ensure that the water content of the modified silk raw materials and the modified fiber raw materials is 20%; uniformly laying the humidified modified silk raw material and modified fiber raw material for electron beam radiation treatment, wherein the electron beam radiation dose is controlled to be 5kGy, and the radiation time is 10 s; placing the modified silk raw material and the modified fiber raw material subjected to electron beam radiation treatment into 10 mass percent Bordeaux mixture, uniformly stirring, placing into an autoclave for inactivation for 50min at 120 ℃, then performing ultrasonic treatment for 2h, finally performing solid-liquid separation, and washing solid content with water to obtain the modified silk raw material and the modified fiber raw material subjected to sterilization treatment for later use.
Preparing an essential oil extract: crushing tea tree wood by adopting a low-temperature gas explosion method to obtain tea tree powder; putting the tea tree powder into a filter bag, placing the filter bag into an extraction tank, and introducing a liquid solvent into the extraction tank from a solvent tank for extraction to obtain crude tea tree oil; distilling the crude tea tree oil under reduced pressure to obtain tea tree essential oil; dispersing the tea tree essential oil into a compound solution of sodium alginate and sodium caseinate, wherein the volume of the compound solution is 10 times that of the tea tree essential oil, and the compound solution of sodium alginate and sodium caseinate is a sodium alginate solution with the mass concentration of 2% and a sodium caseinate solution with the mass concentration of 1% according to the volume ratio of 5: 1, homogenizing for 15min at 1000r/min to obtain tea tree essential oil microparticles, adding the tea tree essential oil microparticles into 1% calcium lactate solution, and stirring for 30min to obtain solidified essential oil extract in microparticle form.
Preparing modified silk: uniformly mixing silk and essential oil extract, and performing microwave activation treatment for 3 min; placing the mixture of silk and essential oil extract subjected to microwave activation treatment in a 3% chitin solution, and performing crosslinking fixation under stirring at 50 deg.C; and (2) performing solid-liquid separation on the mixture after the crosslinking fixation, placing the solid part in a sealed container, vacuumizing by using a vacuum pump until the negative pressure is 0.3MPa, then injecting polyvinyl alcohol emulsion with the solid content of 40% into the container, standing for 2 hours under the condition of keeping stable negative pressure, taking out the solid of the mixture after standing, and maintaining for 2 days under the conditions that the relative humidity is 50% and the temperature is 24 ℃ to obtain the modified silk for later use.
Preparing modified fibers: taking polyester as a raw material, slicing, drying and melting to obtain a molten liquid; mixing sodium dihydrogen phosphate into the molten liquid, performing blended spinning and post-processing to obtain modified fibers with modified surface micropores; the temperature of the blended spinning is controlled at 300 ℃ and the pressure is 10 MPa.
Mixing polyethylene aminoethyl ester, polyethylene resin and ethyl acetate, heating to melt, adding modified silk and modified fiber, stirring uniformly, and putting into a spinneret plate to extrude to form single fibers; and then weaving the fibers into the fabric.
Design of experiments
Air permeability test
The modified silk moisture-wicking antibacterial fabrics prepared in examples 1 to 3 and commercially available fabrics were subjected to air permeability test using a KES-F8-AP1 air permeameter. The test method comprises the following steps: after the fabric is placed in an environment with the temperature of 20 ℃ and the relative humidity of 65% for balancing for 20 hours, setting the speed to be 2cm/sec and the sensitivity to be a middle grade on an instrument panel, taking different positions on the same sample for testing 10 times, and taking an average value to obtain the gas resistance value (unit: KPa s/m 2) of each group of fabrics, wherein the recorded data are as follows:
Figure DEST_PATH_IMAGE002
as can be seen from the above table, the air resistance value of the modified silk moisture-conducting antibacterial fabric provided in the embodiment of the invention is obviously smaller than that of the fabric sold in the market; therefore, compared with the existing fabric, the modified silk moisture-conducting antibacterial fabric has good air permeability.
Verification of antibacterial effect
The experimental method comprises the following steps: culturing with conventional Staphylococcus aureus culture medium, continuously inoculating twice Staphylococcus aureus cultures, respectively taking small amount of fresh bacteria from the culture medium with inoculating loop, adding into sterile physiological saline, and counting under microscope to obtain a solution containing bacteria with concentration of 1X105CFU/ml experimental bacterial liquid for later use; the antibacterial rate was measured by thin film coating method, and the fabric prepared in examples 1-3 was sterilized at 1cm X1 cm, and placed in the center of a petri dish, and 20uL of Staphylococcus aureus liquid for experiment ((1X 10)5CFU/ml) is dripped on the surface of the fabric, a polyethylene film is clamped by a pair of sterilization forceps to cover a test piece, the test piece is paved, the bacteria liquid is uniformly contacted with the test piece, and aerobic culture is carried out for 24 hours under the conditions of 35 ℃ and the relative humidity of more than 90 percent. Then the fabric is taken out and put into a test tube, 2ml of sterile physiological saline is added to be violently shaken on an oscillator, after the fabric is fully shaken up, l0uL is respectively inoculated on a Sapaul agar plate and an MH agar plate, after aerobic culture is carried out for 24 hours at 35 ℃, bacterial colony counting is carried out, and the experiment is repeated for 3 times to take an average value. The control group is prepared by replacing the modified silk with the common silk on the basis of example 3.
Figure DEST_PATH_IMAGE004
As can be seen from the table above, the number of colonies contained in the fabric provided by the embodiment of the invention is obviously less than that of the control group, and therefore, the bacteriostatic effect of the modified silk is obviously better than that of the common silk.
Verification of continuous aging
The test method is the same as the above, the experimental subject provides more products for example 3, the control group is replaced by equal amount of silk and conventional essential oil extract without modification treatment, the test is respectively carried out after ten days and three months of product processing, and the colony number data is recorded as follows:
grouping Experimental group Control group
Colony count of product ten days later 30.2 43.5
Bacterial colony count of product after March 30.5 82.3
As can be seen from the table above, the product provided by the embodiment of the invention has a bacteriostatic effect obviously superior to that of the control group, and the bacteriostatic effect of the control group is obviously reduced after a period of time, and the bacteriostatic effective period is insufficient.
It should be particularly noted that, although the present specification describes embodiments, each embodiment does not include only an independent technical solution, and such description of the specification is only for clarity, and those skilled in the art should take the specification as a whole, and technical solutions in various embodiments may be appropriately combined to form other embodiments that can be understood by those skilled in the art, and the above-mentioned embodiments only express the preferred embodiments of the technical solutions, and the description thereof is more specific and detailed, but should not be construed as limiting the scope of the claims of the technical solutions. It should be noted that, for those skilled in the art, various modifications, improvements and substitutions can be made without departing from the spirit of the invention, and all of them belong to the protection scope of the technical solution.

Claims (9)

1. The modified silk moisture-conducting antibacterial fabric is characterized by comprising the following raw materials in parts by weight: 10-100 parts of modified silk, 10-100 parts of modified fiber, 10-30 parts of essential oil extract, 5-20 parts of cross-linking agent, 5-30 parts of polymer emulsion, 20-50 parts of polyethylene aminoethyl ester, 20-60 parts of polyethylene resin and 10-30 parts of ethyl acetate;
the preparation method of the modified silk comprises the following steps: uniformly mixing silk and essential oil extract, and performing microwave activation for 1-5 min; placing the mixture of silk and essential oil extracts subjected to microwave activation treatment into a cross-linking agent solution, and performing cross-linking fixation under the condition of stirring; and (2) performing solid-liquid separation on the mixture after the crosslinking fixation, placing the solid part in a sealed container, vacuumizing by using a vacuum pump until the negative pressure is 0.1-0.3MPa, then injecting polymer emulsion with the solid content of 30-40% into the container, standing for 1-2h under the condition of keeping stable negative pressure, and fishing out the solid of the mixture after standing for 2 days under the conditions that the relative humidity is 50% and the temperature is 24 ℃ to obtain the modified silk.
2. The modified silk moisture-conducting antibacterial fabric according to claim 1, wherein the cross-linking agent is a 3% chitin solution, and the temperature during the cross-linking process is 50 ℃.
3. The modified silk moisture-conducting and antibacterial fabric according to claim 2, wherein the polymer emulsion is polyvinyl alcohol emulsion.
4. The modified silk moisture-conducting and antibacterial fabric according to claim 3, wherein the preparation method of the essential oil extract comprises the following steps: crushing tea tree wood by adopting a low-temperature gas explosion method to obtain tea tree powder; putting the tea tree powder into a filter bag, placing the filter bag into an extraction tank, and introducing a liquid solvent into the extraction tank from a solvent tank for extraction to obtain crude tea tree oil; distilling the crude tea tree oil under reduced pressure to obtain tea tree essential oil; dispersing the tea tree essential oil in a compound solution of sodium alginate and sodium caseinate which is 10 times of the volume of the tea tree essential oil, homogenizing for 15min under the condition of 1000r/min to obtain tea tree essential oil microparticles, adding the tea tree essential oil microparticles into a calcium lactate solution with the concentration of 1%, and stirring for 30min to obtain a solidified essential oil extract in a microparticle form.
5. The modified silk moisture-conducting antibacterial fabric according to claim 4, wherein the compound solution of sodium alginate and sodium caseinate is a sodium alginate solution with a mass concentration of 2% and a sodium caseinate solution with a mass concentration of 1% in a volume ratio of 5: 1 to form a compound solution.
6. The modified silk moisture-conducting and antibacterial fabric according to claim 5, wherein the preparation method of the modified fibers comprises the following steps: taking polyester as a raw material, slicing, drying and melting to obtain a molten liquid; mixing sodium dihydrogen phosphate into the molten liquid, performing blended spinning and post-processing to obtain modified fibers with modified surface micropores; the temperature of the blended spinning is controlled at 300 ℃ and the pressure is 10 MPa.
7. The modified silk moisture-conducting antibacterial fabric according to claim 6, wherein the raw materials of the modified silk and the modified fiber are subjected to sterilization treatment before the modification treatment, and the sterilization treatment specifically comprises the following steps: humidifying the modified silk raw material and the modified fiber raw material to enable the water content of the modified silk raw material and the water content of the modified fiber raw material to be 20-30%; uniformly laying the humidified modified silk raw material and modified fiber raw material for electron beam radiation treatment, wherein the electron beam radiation dose is controlled to be 2-5kGy, and the radiation time is 5-10 s; placing the modified silk raw material and the modified fiber raw material subjected to electron beam radiation treatment in an alkaline bactericide with the mass fraction of 5-10%, uniformly stirring, placing in an autoclave for inactivation for 50min at 120 ℃, then performing ultrasonic treatment for 1-2h, finally performing solid-liquid separation, and washing solid content to obtain the modified silk raw material and the modified fiber raw material subjected to sterilization treatment.
8. The modified silk moisture-conducting and antibacterial fabric according to claim 7, wherein the alkaline bactericide is lime sulfur or Bordeaux mixture.
9. The preparation method of the modified silk moisture-conducting and antibacterial fabric according to any one of claims 1 to 8, characterized by comprising the following steps: mixing polyethylene aminoethyl ester, polyethylene resin and ethyl acetate, heating to melt, adding modified silk and modified fiber, stirring uniformly, and putting into a spinneret plate to extrude to form single fibers; and then weaving the fibers into the fabric.
CN202110574897.9A 2021-05-26 2021-05-26 Modified silk moisture-conducting antibacterial fabric and preparation method thereof Withdrawn CN113388917A (en)

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Application publication date: 20210914