CN112779788A - Antibacterial fabric and preparation method thereof - Google Patents

Antibacterial fabric and preparation method thereof Download PDF

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Publication number
CN112779788A
CN112779788A CN202110028673.8A CN202110028673A CN112779788A CN 112779788 A CN112779788 A CN 112779788A CN 202110028673 A CN202110028673 A CN 202110028673A CN 112779788 A CN112779788 A CN 112779788A
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parts
fabric
reaction
antibacterial
ammonium chloride
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靳云平
叶先明
潘新江
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Xinxiang Patron Saint Special Fabric Co Ltd
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Xinxiang Patron Saint Special Fabric Co Ltd
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    • 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
    • D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/12—Processes in which the treating agent is incorporated in microcapsules
    • 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
    • D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • 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
    • 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
    • D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
    • 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
    • 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
    • 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
    • D06M15/15—Proteins or derivatives thereof
    • 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
    • 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
    • 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

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

Abstract

The invention relates to an antibacterial fabric and a preparation method thereof, wherein the antibacterial fabric comprises a fabric base material and a composite microcapsule antibacterial agent added in the fabric base material, and the preparation method of the antibacterial fabric comprises five steps of preparation of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, emulsification reaction, complex coacervation reaction, crosslinking reaction and combination of the composite microcapsule antibacterial agent and the fabric base material. According to the invention, the antibacterial active ingredients of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, thujoram oil and anise oil are prepared into a microcapsule formulation, so that the fabric has a high-efficiency antibacterial effect, good slow release performance and good safety performance, is good in washing resistance, can still maintain good antibacterial performance after being used for a long time, and has a wide industrial application prospect.

Description

Antibacterial fabric and preparation method thereof
Technical Field
The invention belongs to the technical field of spinning, and particularly relates to an antibacterial fabric and a preparation method thereof.
Background
With the development of human science and technology and the improvement of living standard of people, people put more demands on the sanitation of fabrics while paying attention to the beauty and comfort of the fabrics, and the antibacterial fabrics gradually become an important new industrial field. The antibacterial fabric has wide application, and is generally used for manufacturing underwear, pajamas, sportswear, socks, shoe linings and diapers for infants; bed sheets, quilt covers, blankets, napkins, towels, sofa cloth, curtain cloth and carpets of hospitals, hotels and families; the medical garment, the food garment, the work garment in the service industry, the army garment, the bandage, the gauze and the like have great social benefits. The antibacterial fabric has the functions of preventing the fabric from being contaminated by microorganisms, preventing infectious diseases, ensuring the safety and health of human bodies and the comfort of wearing, reducing the cross infection rate of public environments and ensuring that the fabric simultaneously has the health and health care functions.
The preparation method of the antibacterial fabric generally comprises two methods: one is to directly weave antibacterial fabric by adopting antibacterial fiber; the other is to fix the antibacterial agent on the fiber by post-treatment processing. Currently, in the antibacterial processing of textiles, the methods of antibacterial finishing processing account for about 70%. Most of antibacterial finishing agents for antibacterial finishing of textiles are organic antibacterial agents. Organic antibacterial agents are classified into chemically synthesized antibacterial agents and natural antibacterial ingredients. The chemical synthesis antibacterial agent is the most widely used antibacterial agent at present, but has the problems of poor high temperature resistance and stability, certain risk caused by dissolution and the like. Although the natural antibacterial component has good safety performance, the washing resistance is poor, and the antibacterial effect is greatly reduced after long-time use.
Disclosure of Invention
The invention aims to provide an antibacterial fabric and a preparation method thereof, and aims to solve the technical problems that the existing antibacterial fabric is poor in high-temperature resistance stability, poor in safety, poor in washing resistance and incapable of maintaining antibacterial effect.
The invention provides an antibacterial fabric, which comprises a fabric base material, wherein a composite microcapsule antibacterial agent is added into the fabric base material; the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 5-10 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 2-5 parts of thujoram oil, 2-5 parts of anise oil, 25-40 parts of gelatin, 10-15 parts of N-nonane, 0.5-1 part of glutaraldehyde crosslinking agent, 5-8 parts of 10% sodium hydroxide aqueous solution, 2-4 parts of calcium chloride dihydrate, 0.5-1 part of emulsifier, 10-15 parts of adhesive resin and 80-100 parts of distilled water.
Preferably, the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 7-9 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 3-4 parts of thujoram oil, 3-4 parts of anise oil, 30-35 parts of gelatin, 12-14 parts of N-nonane, 0.7-0.9 part of glutaraldehyde crosslinking agent, 6-7 parts of 10% sodium hydroxide aqueous solution, 3-4 parts of calcium chloride dihydrate, 0.6-0.8 part of emulsifier, 12-14 parts of adhesive resin and 85-95 parts of distilled water.
Preferably, the emulsifier is any one of OP-10, PVA, TX-10 and SE-10.
Preferably, the textile substrate is a regenerated fiber, a synthetic fiber or a natural fiber.
The invention also provides a preparation method of the antibacterial fabric, which comprises the following steps:
step (1) preparation of N-2-hydroxypropyl trimethyl ammonium chloride chitosan: dissolving chitosan in dilute acetic acid solution, adding glycidol trimethyl ammonium chloride into a reaction system, regulating the molar ratio of chitosan to glycidol trimethyl ammonium chloride to be 1:5, then regulating the pH value of the solution to be 6.0-6.5 by using dilute hydrochloric acid, reacting for 14 hours at 85 ℃, after the reaction is finished, precipitating and filtering a product by using ethanol, finally washing the product by using 70% ethanol aqueous solution to obtain a crude product, dissolving the crude product by using water, filtering by using a sand core funnel, precipitating and separating filtrate by using acetone, and filtering again to obtain a solid final product, namely the N-2-hydroxypropyl trimethyl ammonium chloride chitosan.
And (2) emulsification reaction: weighing a certain weight of gelatin, thujoram oil, fennel oil, n-nonane and an emulsifier in sequence according to the weight part ratio, placing the mixture into a reaction bottle, adding distilled water into the reaction bottle, stirring and mixing the mixture uniformly, heating the mixture to 65 ℃ to dissolve reactants, and carrying out an emulsification reaction in a high-shear emulsifying machine at a rotating speed of 3000r/min after the reactants are dissolved.
And (3) complex coacervation reaction: and (2) placing the emulsified product obtained in the step (2) in a water bath at 40 ℃ for heat preservation, then adding a proper amount of distilled water into the N-2-hydroxypropyl trimethyl ammonium chloride chitosan obtained in the step (1) to dissolve the solution to obtain a solution A, slowly dropwise adding the solution A into the emulsified product obtained in the step (2) under the condition of continuous stirring, adding a 10% sodium hydroxide aqueous solution into a reaction system to adjust the pH value of the reaction solution to 6.0-6.4 after dropwise adding is finished, finally adding calcium chloride dihydrate, and placing the reaction system at 40 ℃ for continuous reaction for 30 min.
Step (4), crosslinking reaction: and (4) placing the reaction liquid obtained in the step (3) in an ice water bath, adding a glutaraldehyde crosslinking agent, reacting for 1-1.5 hours under the condition of continuous stirring, after the reaction is finished, and after the reaction system returns to the room temperature, performing suction filtration, washing and drying to obtain the composite microcapsule antibacterial agent.
Combining the composite microcapsule antibacterial agent with the fabric base material in the step (5): and (3) uniformly mixing the composite microcapsule antibacterial agent obtained in the step (4) with bonding resin, spraying the mixture on a fabric substrate for multiple times, carrying out two-dipping and two-rolling with a dipping rate of 80-90%, drying the fabric at 70 ℃ for 15min, and then baking the fabric at 110 ℃ for 10min to finally obtain the antibacterial fabric.
Preferably, the binder resin is any one of a modified acrylic resin, an amino resin, and a urethane resin.
The invention has the beneficial effects that: according to the invention, the antibacterial active ingredients of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, thujoram oil and anise oil are added into the fabric base material to prepare the antibacterial fabric, the modified chitosan and the natural antibacterial ingredients are compounded, so that the high-temperature-resistant stability and the safety performance are good, the antibacterial fabric is prepared into a microcapsule formulation, the slow-release performance and the washing resistance are good, the antibacterial performance can be kept well after long-time use, the high-efficiency antibacterial effect of the fabric can be kept for a long time, and the industrial application prospect is wide.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
The invention provides an antibacterial fabric, which comprises a fabric base material, wherein a composite microcapsule antibacterial agent is added into the fabric base material; the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 5-10 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 2-5 parts of thujoram oil, 2-5 parts of anise oil, 25-40 parts of gelatin, 10-15 parts of N-nonane, 0.5-1 part of glutaraldehyde crosslinking agent, 5-8 parts of 10% sodium hydroxide aqueous solution, 2-4 parts of calcium chloride dihydrate, 0.5-1 part of emulsifier, 10-15 parts of adhesive resin and 80-100 parts of distilled water.
The N-2-hydroxypropyl trimethyl ammonium chloride chitosan has good water solubility, and has good bactericidal effect on staphylococcus aureus, bacillus subtilis, staphylococcus epidermidis and candida albicans. The antibacterial mechanism of the N-2-hydroxypropyl trimethyl ammonium chloride chitosan is as follows: n-2-hydroxypropyl trimethyl ammonium chloride chitosan is a polycation electrolyte with high charge density, the antibacterial action site of the chitosan is the bacterial cell surface with negative charges, the chitosan interacts with acidic macromolecules generated on the bacterial cell surface to form a polymer film, and the bacteria are inhibited from carrying out substance and energy exchange with the outside, so that the growth of the bacteria is disturbed.
When the concentration of the antibacterial active ingredient juniperic acid in the thujoram oil is 25-200 mg/kg, the development of almost all bacteria and fungi can be prevented, and the safety to people and livestock is extremely high.
The anise oil has good inhibitory effect on staphylococcus aureus and fungi.
Preferably, the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 7-9 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 3-4 parts of thujoram oil, 3-4 parts of anise oil, 30-35 parts of gelatin, 12-14 parts of N-nonane, 0.7-0.9 part of glutaraldehyde crosslinking agent, 6-7 parts of 10% sodium hydroxide aqueous solution, 3-4 parts of calcium chloride dihydrate, 0.6-0.8 part of emulsifier, 12-14 parts of adhesive resin and 85-95 parts of distilled water.
Preferably, the emulsifier is any one of OP-10, PVA, TX-10 and SE-10.
OP-10 and TX-10 belong to alkylphenol polyoxyethylene ether emulsifiers, have high chemical stability, strong acid and alkali resistance, and have good wettability, permeability and emulsibility. SE-10 belongs to fatty acid polyoxyethylene ester emulsifier. PVA is polyvinyl alcohol, has unique smoothness and wear resistance, and has good adhesion and film forming property in aqueous solution.
Preferably, the textile substrate is a regenerated fiber, a synthetic fiber or a natural fiber.
The invention also provides a preparation method of the antibacterial fabric, which comprises the following steps:
step (1) preparation of N-2-hydroxypropyl trimethyl ammonium chloride chitosan: dissolving chitosan in dilute acetic acid solution, adding glycidol trimethyl ammonium chloride into a reaction system, regulating the molar ratio of chitosan to glycidol trimethyl ammonium chloride to be 1:5, then regulating the pH value of the solution to be 6.0-6.5 by using dilute hydrochloric acid, reacting for 14 hours at 85 ℃, after the reaction is finished, precipitating and filtering a product by using ethanol, finally washing the product by using 70% ethanol aqueous solution to obtain a crude product, dissolving the crude product by using water, filtering by using a sand core funnel, precipitating and separating filtrate by using acetone, and filtering again to obtain a solid final product, namely the N-2-hydroxypropyl trimethyl ammonium chloride chitosan.
And (2) emulsification reaction: weighing a certain weight of gelatin, thujoram oil, fennel oil, n-nonane and an emulsifier in sequence according to the weight part ratio, placing the mixture into a reaction bottle, adding distilled water into the reaction bottle, stirring and mixing the mixture uniformly, heating the mixture to 65 ℃ to dissolve reactants, and carrying out an emulsification reaction in a high-shear emulsifying machine at a rotating speed of 3000r/min after the reactants are dissolved.
And (3) complex coacervation reaction: and (2) placing the emulsified product obtained in the step (2) in a water bath at 40 ℃ for heat preservation, then adding a proper amount of distilled water into the N-2-hydroxypropyl trimethyl ammonium chloride chitosan obtained in the step (1) to dissolve the solution to obtain a solution A, slowly dropwise adding the solution A into the emulsified product obtained in the step (2) under the condition of continuous stirring, adding a 10% sodium hydroxide aqueous solution into a reaction system to adjust the pH value of the reaction solution to 6.0-6.4 after dropwise adding is finished, finally adding calcium chloride dihydrate, and placing the reaction system at 40 ℃ for continuous reaction for 30 min.
Step (4), crosslinking reaction: and (4) placing the reaction liquid obtained in the step (3) in an ice water bath, adding a glutaraldehyde crosslinking agent, reacting for 1-1.5 hours under the condition of continuous stirring, after the reaction is finished, and after the reaction system returns to the room temperature, performing suction filtration, washing and drying to obtain the composite microcapsule antibacterial agent. The particle size and the distribution of the microcapsules are important performance indexes of the microcapsules, and not only the slow release performance of the microcapsules is influenced, but also the isolation performance of the coated isolated microcapsules is influenced. The pH value of the complex coacervation reaction in the step (3), the time of the complex coacervation reaction, the time of the crosslinking reaction in the step (4) and the like have great influence on the particle size and distribution of the microcapsules. Through a large number of long-term experimental operations, the invention finally discovers that the outer surface of the prepared microcapsule is regular and smooth, the average particle size is several microns, and the particle size distribution is concentrated under the conditions that the pH value of the complex coacervation reaction is 6.0-6.4, the time of the complex coacervation reaction is 30min and the time of the crosslinking reaction is 1-1.5 hours.
Combining the composite microcapsule antibacterial agent with the fabric base material in the step (5): and (3) uniformly mixing the composite microcapsule antibacterial agent obtained in the step (4) with bonding resin, spraying the mixture on a fabric substrate for multiple times, carrying out two-dipping and two-rolling with a dipping rate of 80-90%, drying the fabric at 70 ℃ for 15min, and then baking the fabric at 110 ℃ for 10min to finally obtain the antibacterial fabric.
Preferably, the binder resin is any one of a modified acrylic resin, an amino resin, and a urethane resin.
Example 1
The invention provides an antibacterial fabric, which comprises a fabric base material, wherein the fabric base material is regenerated fibers, and a composite microcapsule antibacterial agent is added into the fabric base material; the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 5 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 2 parts of thujoram oil, 2 parts of anise oil, 25 parts of gelatin, 10 parts of N-nonane, 0.5 part of glutaraldehyde crosslinking agent, 5 parts of 10% sodium hydroxide aqueous solution, 2 parts of calcium chloride dihydrate, 100.5 parts of emulsifier OP-100.5 parts, 10 parts of modified acrylic resin and 80 parts of distilled water.
The invention also provides a preparation method of the antibacterial fabric, which comprises the following steps:
step (1) preparation of N-2-hydroxypropyl trimethyl ammonium chloride chitosan: dissolving chitosan in dilute acetic acid solution, adding glycidol trimethyl ammonium chloride into a reaction system, regulating the molar ratio of chitosan to glycidol trimethyl ammonium chloride to be 1:5, then regulating the pH value of the solution to be 6.0-6.5 by using dilute hydrochloric acid, reacting for 14 hours at 85 ℃, after the reaction is finished, precipitating and filtering a product by using ethanol, finally washing the product by using 70% ethanol aqueous solution to obtain a crude product, dissolving the crude product by using water, filtering by using a sand core funnel, precipitating and separating filtrate by using acetone, and filtering again to obtain a solid final product, namely the N-2-hydroxypropyl trimethyl ammonium chloride chitosan.
And (2) emulsification reaction: weighing a certain weight of gelatin, thujoram oil, fennel oil, n-nonane and an emulsifier in sequence according to the weight part ratio, placing the mixture into a reaction bottle, adding distilled water into the reaction bottle, stirring and mixing the mixture uniformly, heating the mixture to 65 ℃ to dissolve reactants, and carrying out an emulsification reaction in a high-shear emulsifying machine at a rotating speed of 3000r/min after the reactants are dissolved.
And (3) complex coacervation reaction: and (2) placing the emulsified product obtained in the step (2) in a water bath at 40 ℃ for heat preservation, then adding a proper amount of distilled water into the N-2-hydroxypropyl trimethyl ammonium chloride chitosan obtained in the step (1) to dissolve the solution to obtain a solution A, slowly dropwise adding the solution A into the emulsified product obtained in the step (2) under the condition of continuous stirring, adding a 10% sodium hydroxide aqueous solution into a reaction system to adjust the pH value of the reaction solution to 6.0-6.4 after dropwise adding is finished, finally adding calcium chloride dihydrate, and placing the reaction system at 40 ℃ for continuous reaction for 30 min.
Step (4), crosslinking reaction: and (4) placing the reaction liquid obtained in the step (3) in an ice water bath, adding a glutaraldehyde crosslinking agent, reacting for 1-1.5 hours under the condition of continuous stirring, after the reaction is finished, and after the reaction system returns to the room temperature, performing suction filtration, washing and drying to obtain the composite microcapsule antibacterial agent. The particle size and the distribution of the microcapsules are important performance indexes of the microcapsules, and not only the slow release performance of the microcapsules is influenced, but also the isolation performance of the coated isolated microcapsules is influenced. The pH value of the complex coacervation reaction in the step (3), the time of the complex coacervation reaction, the time of the crosslinking reaction in the step (4) and the like have great influence on the particle size and distribution of the microcapsules. Through a large number of long-term experimental operations, the invention finally discovers that the outer surface of the prepared microcapsule is regular and smooth, the average particle size is several microns, and the particle size distribution is concentrated under the conditions that the pH value of the complex coacervation reaction is 6.0-6.4, the time of the complex coacervation reaction is 30min and the time of the crosslinking reaction is 1-1.5 hours.
Combining the composite microcapsule antibacterial agent with the fabric base material in the step (5): and (3) uniformly mixing the composite microcapsule antibacterial agent obtained in the step (4) with bonding resin, spraying the mixture on a fabric substrate for multiple times, carrying out two-dipping and two-rolling with a dipping rate of 80-90%, drying the fabric at 70 ℃ for 15min, and then baking the fabric at 110 ℃ for 10min to finally obtain the antibacterial fabric.
Example 2
An antibacterial fabric comprises a fabric base material, wherein the fabric base material is synthetic fiber, and a composite microcapsule antibacterial agent is added into the fabric base material; the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 10 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 5 parts of thujoram oil, 5 parts of fennel oil, 40 parts of gelatin, 15 parts of N-nonane, 1 part of glutaraldehyde crosslinking agent, 8 parts of 10% sodium hydroxide aqueous solution, 4 parts of calcium chloride dihydrate, 1 part of emulsifier PVA, 15 parts of amino resin and 100 parts of distilled water. The preparation method of the antibacterial fabric is the same as that of example 1.
Example 3
An antibacterial fabric comprises a fabric base material, wherein the fabric base material is natural fiber, and a composite microcapsule antibacterial agent is added into the fabric base material; the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 7 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 3 parts of thujoram oil, 3 parts of anise oil, 30 parts of gelatin, 12 parts of N-nonane, 0.7 part of glutaraldehyde crosslinking agent, 6 parts of 10% sodium hydroxide aqueous solution, 3 parts of calcium chloride dihydrate, 100.6 parts of emulsifier TX-100, 12 parts of polyurethane resin and 85 parts of distilled water. The preparation method of the antibacterial fabric is the same as that of example 1.
Example 4
An antibacterial fabric comprises a fabric base material, wherein the fabric base material is regenerated fibers, and a composite microcapsule antibacterial agent is added into the fabric base material; the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 9 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 4 parts of thujoram oil, 4 parts of anise oil, 35 parts of gelatin, 14 parts of N-nonane, 0.9 part of glutaraldehyde crosslinking agent, 7 parts of 10% sodium hydroxide aqueous solution, 4 parts of calcium chloride dihydrate, 100.8 parts of emulsifier SE-14, 14 parts of modified acrylic resin and 95 parts of distilled water. The preparation method of the antibacterial fabric is the same as that of example 1.
Example 5
An antibacterial fabric comprises a fabric base material, wherein the fabric base material is natural fiber, and a composite microcapsule antibacterial agent is added into the fabric base material; the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 6 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 3 parts of thujoram oil, 4 parts of anise oil, 36 parts of gelatin, 13 parts of N-nonane, 0.8 part of glutaraldehyde crosslinking agent, 6 parts of 10% sodium hydroxide aqueous solution, 4 parts of calcium chloride dihydrate, 100.9 parts of emulsifier TX-11, 11 parts of modified acrylic resin and 90 parts of distilled water. The preparation method of the antibacterial fabric is the same as that of example 1.
The antibacterial fabrics prepared in examples 1 to 5 were subjected to antibacterial performance tests, and the test results are shown in table 1.
TABLE 1
Figure BDA0002891228710000071
Figure BDA0002891228710000081
In conclusion, the fabric prepared by adopting the raw material composition, the raw material proportion and the preparation process has high-efficiency antibacterial effect, good slow release performance, good safety performance, good washing resistance, and wide industrial application prospect, and can still keep good antibacterial performance after being used for a long time.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.

Claims (6)

1. An antibacterial fabric comprising a fabric substrate, characterized in that: the fabric base material is added with a composite microcapsule antibacterial agent; the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 5-10 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 2-5 parts of thujoram oil, 2-5 parts of anise oil, 25-40 parts of gelatin, 10-15 parts of N-nonane, 0.5-1 part of glutaraldehyde crosslinking agent, 5-8 parts of 10% sodium hydroxide aqueous solution, 2-4 parts of calcium chloride dihydrate, 0.5-1 part of emulsifier, 10-15 parts of adhesive resin and 80-100 parts of distilled water.
2. The antimicrobial fabric of claim 1, wherein: the composite microcapsule antibacterial agent comprises the following raw material components in parts by weight: 7-9 parts of N-2-hydroxypropyl trimethyl ammonium chloride chitosan, 3-4 parts of thujoram oil, 3-4 parts of anise oil, 30-35 parts of gelatin, 12-14 parts of N-nonane, 0.7-0.9 part of glutaraldehyde crosslinking agent, 6-7 parts of 10% sodium hydroxide aqueous solution, 3-4 parts of calcium chloride dihydrate, 0.6-0.8 part of emulsifier, 12-14 parts of adhesive resin and 85-95 parts of distilled water.
3. The antimicrobial fabric of claim 1, wherein: the emulsifier is any one of OP-10, PVA, TX-10 and SE-10.
4. The antimicrobial fabric of claim 1, wherein: the fabric substrate is a regenerated fiber, a synthetic fiber or a natural fiber.
5. The method of making an antimicrobial fabric of any of claims 1-4, wherein: the method comprises the following steps:
step (1) preparation of N-2-hydroxypropyl trimethyl ammonium chloride chitosan: dissolving chitosan in dilute acetic acid solution, adding glycidol trimethyl ammonium chloride into a reaction system, wherein the molar ratio of chitosan to glycidol trimethyl ammonium chloride is 1:5, then adjusting the pH value of the solution to 6.0-6.5 by using dilute hydrochloric acid, reacting for 14 hours at 85 ℃, after the reaction is finished, precipitating and filtering a product by using ethanol, finally washing the product by using 70% ethanol aqueous solution to obtain a crude product, dissolving the crude product by using water, filtering by using a sand core funnel, precipitating and separating out filtrate by using acetone, and filtering again to obtain a solid final product, namely N-2-hydroxypropyl trimethyl ammonium chloride chitosan;
and (2) emulsification reaction: sequentially weighing a certain weight of gelatin, thujoram oil, fennel oil, n-nonane and an emulsifier according to the weight part ratio, placing the gelatin, the thujoram oil, the fennel oil, the n-nonane and the emulsifier in a reaction bottle, adding distilled water into the reaction bottle, stirring and mixing uniformly, heating to 65 ℃ to dissolve reactants, and carrying out an emulsification reaction in a high-shear emulsifying machine at a rotating speed of 3000r/min after the reactants are dissolved;
and (3) complex coacervation reaction: putting the emulsified product obtained in the step (2) into a water bath at 40 ℃ for heat preservation, then adding a proper amount of distilled water into the N-2-hydroxypropyl trimethyl ammonium chloride chitosan obtained in the step (1) to dissolve the solution A to obtain a solution A, slowly dropwise adding the solution A into the emulsified product obtained in the step (2) under the condition of continuous stirring, adding a 10% sodium hydroxide aqueous solution into a reaction system after dropwise adding is finished to adjust the pH value of the reaction solution to 6.0-6.4, finally adding calcium chloride dihydrate, and putting the reaction system at 40 ℃ for continuous reaction for 30 min;
step (4), crosslinking reaction: placing the reaction liquid obtained in the step (3) in an ice water bath, adding a glutaraldehyde crosslinking agent, reacting for 1-1.5 hours under the condition of continuous stirring, after the reaction is finished, and after the reaction system returns to the room temperature, performing suction filtration, washing and drying to obtain a composite microcapsule antibacterial agent;
combining the composite microcapsule antibacterial agent with the fabric base material in the step (5): and (3) uniformly mixing the composite microcapsule antibacterial agent obtained in the step (4) with bonding resin, spraying the mixture on a fabric substrate for multiple times, carrying out two-dipping and two-rolling with a dipping rate of 80-90%, drying the fabric at 70 ℃ for 15min, and then baking the fabric at 110 ℃ for 10min to finally obtain the antibacterial fabric.
6. The method of making an antimicrobial fabric according to claim 5, wherein: the adhesive resin is any one of modified acrylic resin, amino resin and polyurethane resin.
CN202110028673.8A 2021-01-11 2021-01-11 Antibacterial fabric and preparation method thereof Pending CN112779788A (en)

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CN113957723A (en) * 2021-10-27 2022-01-21 温州远大服饰有限公司 Antibacterial upper garment and production process thereof
CN114481632A (en) * 2022-02-28 2022-05-13 江苏锐晟纺织科技有限公司 Long-acting biological antibacterial washable rayon crepe and preparation method thereof

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CN102061625A (en) * 2009-11-16 2011-05-18 香港理工大学 Mugwort leaf oil microcapsule antibacterial crease-resistant fabric and preparation method thereof
CN102251408A (en) * 2011-06-13 2011-11-23 泉州红瑞兴纺织有限公司 Microcapsule nano silver antibacterial fabric and preparation method thereof
CN104975513A (en) * 2015-05-29 2015-10-14 天津城建大学 Efficient antibacterial chitosan essential oil microcapsule preparation method

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CN101591859A (en) * 2009-06-22 2009-12-02 华南农业大学 A kind of Blumea oil microcapsule textile composite finishing agent and application thereof
CN102061625A (en) * 2009-11-16 2011-05-18 香港理工大学 Mugwort leaf oil microcapsule antibacterial crease-resistant fabric and preparation method thereof
CN102251408A (en) * 2011-06-13 2011-11-23 泉州红瑞兴纺织有限公司 Microcapsule nano silver antibacterial fabric and preparation method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113957723A (en) * 2021-10-27 2022-01-21 温州远大服饰有限公司 Antibacterial upper garment and production process thereof
CN114481632A (en) * 2022-02-28 2022-05-13 江苏锐晟纺织科技有限公司 Long-acting biological antibacterial washable rayon crepe and preparation method thereof
CN114481632B (en) * 2022-02-28 2023-11-28 江苏锐晟纺织科技有限公司 Long-acting biological antibacterial washable human cotton crepe and preparation method thereof

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Application publication date: 20210511