CN112900089A - Waterproof fiber knitted fabric and preparation method thereof - Google Patents

Waterproof fiber knitted fabric and preparation method thereof Download PDF

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Publication number
CN112900089A
CN112900089A CN202110103318.2A CN202110103318A CN112900089A CN 112900089 A CN112900089 A CN 112900089A CN 202110103318 A CN202110103318 A CN 202110103318A CN 112900089 A CN112900089 A CN 112900089A
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China
Prior art keywords
fiber
fibers
solution
ptt
knitted fabric
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Granted
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CN202110103318.2A
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Chinese (zh)
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CN112900089B (en
Inventor
崔永珍
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Guangzhou Chuanqi Garment Co ltd
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Guangzhou Shenduo Clothing Co ltd
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Priority to CN202110103318.2A priority Critical patent/CN112900089B/en
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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
    • 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
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04B—KNITTING
    • D04B1/00—Weft knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
    • D04B1/14—Other fabrics or articles characterised primarily by the use of particular thread materials
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04B—KNITTING
    • D04B1/00—Weft knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
    • D04B1/14—Other fabrics or articles characterised primarily by the use of particular thread materials
    • D04B1/16—Other fabrics or articles characterised primarily by the use of particular thread materials synthetic threads
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04B—KNITTING
    • D04B21/00—Warp knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
    • 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
    • D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
    • D—TEXTILES; PAPER
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    • 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
    • D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/30—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with oxides of halogens, oxyacids of halogens or their salts, e.g. with perchlorates
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    • 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
    • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
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    • 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
    • D06M11/50—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 hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
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    • 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
    • D06M11/74—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 or graphite; with carbides; with graphitic acids or their salts
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    • 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
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
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    • 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
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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
    • 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
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0061—Organic fillers or organic fibrous fillers, e.g. ground leather waste, wood bark, cork powder, vegetable flour; Other organic compounding ingredients; Post-treatment with organic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
    • D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
    • D06N3/146—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes characterised by the macromolecular diols used
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • 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
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
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    • 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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    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/50—Modified hand or grip properties; Softening compositions
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    • D06N2203/00—Macromolecular materials of the coating layers
    • D06N2203/06—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • D06N2209/00—Properties of the materials
    • D06N2209/04—Properties of the materials having electrical or magnetic properties
    • D06N2209/046—Anti-static
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    • D06N2209/00—Properties of the materials
    • D06N2209/10—Properties of the materials having mechanical properties
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    • D06N2209/00—Properties of the materials
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    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/01—Natural vegetable fibres
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    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/02—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
    • D10B2331/021—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides aromatic polyamides, e.g. aramides
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    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]

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  • Chemical & Material Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • Biochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Inorganic Chemistry (AREA)
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  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a waterproof fiber knitted fabric and a preparation method thereof, and the preparation method comprises the following steps: the method comprises the following steps of firstly, manufacturing grey cloth, wherein modified PTT fibers, aramid fibers, modified cotton fibers and bamboo fibers are adopted according to the mass ratio of 1: 1: 1: 1, blending and interweaving the materials into grey cloth, wherein the surface layer adopts modified PTT fiber and aramid fiber, and the inner layer adopts modified cotton fiber and bamboo fiber; secondly, preshrinking, dyeing and shaping, preshrinking and dyeing the gray cloth obtained in the first step, and finally coating a coating agent on the surface layer for curing and shaping to obtain the waterproof fiber knitted fabric; due to the existence of the modified cotton fiber, the modified PTT fiber and the waterborne polyurethane coating agent, the waterproof fiber knitted fabric prepared by the invention has good skin-friendly, smooth and antibacterial properties, and also has the properties of flame retardance, water resistance, static resistance and the like.

Description

Waterproof fiber knitted fabric and preparation method thereof
Technical Field
The invention belongs to the technical field of knitted fabric preparation, and particularly relates to a waterproof fiber knitted fabric and a preparation method thereof.
Background
With the development of modern society, the living standard of people is continuously improved, and various comfort performance, appearance performance and special performance of textiles are more and more emphasized. Among them, the knitted fabric is popular, the knitting is a fabric formed by bending yarns into loops by using a knitting needle and mutually interlooping, and the knitted fabric is different from the carboxyknitted fabric in that the form of the yarns in the fabric is different. At present, knitted fabrics are widely applied to products such as garment fabrics, linings and home textiles, but the knitted fabrics have a common problem that knitted fabrics have various qualities, such as various knitted fabrics, sweaters, woollen sweaters, bedding and the like, and the knitted fabrics are easy to be nodular due to continuous large or small friction in the actual wearing and washing processes, have poor waterproof and air permeability, are easy to breed mold bacteria, are easy to generate electrostatic action, have poor flame retardant performance, and seriously restrict the application of the knitted fabrics in places such as garments, bedding, buildings and the like, so that the technical problem needing to be solved at present is to provide the knitted fabrics with the characteristics of waterproofness, antistatic property, flame retardance, antibiosis and wear resistance.
Disclosure of Invention
The invention aims to provide a waterproof fiber knitted fabric and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
in the prior art, fiber fabrics are easy to be nodulated due to continuous large or small friction in the actual wearing and washing processes, and have poor waterproof and air permeability, easy growth of mould and bacteria, easy generation of electrostatic action and poor flame retardant property.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of waterproof fiber knitted fabric comprises the following steps:
the method comprises the following steps of firstly, manufacturing grey cloth, wherein modified PTT fibers, aramid fibers, modified cotton fibers and bamboo fibers are adopted according to the mass ratio of 1: 1: 1: 1, blending and interweaving the materials into grey cloth, wherein the surface layer adopts modified PTT fiber and aramid fiber, and the inner layer adopts modified cotton fiber and bamboo fiber;
and secondly, preshrinking, dyeing and shaping, preshrinking and dyeing the gray cloth obtained in the first step, and finally coating a coating agent on the surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
Further, the preparation method of the coating agent comprises the following steps:
step S11, adding 1-butyl-3-methylimidazole chloride and ethylene glycol into a reaction kettle, stirring at a rotating speed of 80r/min for 10min, adding copper chloride dihydrate into the reaction kettle, continuously stirring at a constant rotating speed for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 20-40min, washing precipitates for 3-5 times by using an ethanol solution with a mass fraction of 40%, and finally drying in an oven at 60 ℃ for 8-10h to obtain nano copper sulfide;
step S12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant-temperature vacuum oven at 80 ℃ for 2h, adding the dried 1, 4-butanediol and polytetrahydrofuran ether glycol into a three-neck flask under the protection of nitrogen, then adding isophorone diisocyanate, bis (hydroxymethyl) propionic acid, N-dimethylacetamide and dibutyltin dilaurate, reacting for 2h in a constant-temperature oil bath environment at 75 ℃, cooling to 55 ℃, adding hydroxyethyl methacrylate and pentaerythritol triacrylate into the three-neck flask, stirring at the rotation speed of 100-, adding deionized water, reacting for 40min at constant rotation speed, and distilling under reduced pressure to remove acetone to obtain the coating agent.
Further, the amount ratio of the 1-butyl-3-methylimidazole chloride, the ethylene glycol, the copper chloride dihydrate and the thioacetamide in step S11 is 1 g: 20-40 mL: 3 g: 3g, wherein the mass ratio of the 1, 4-butanediol, the polytetrahydrofuran ether glycol, the isophorone diisocyanate, the bis (hydroxymethyl) propionic acid, the N, N-dimethylacetamide and the dibutyltin dilaurate in the step S12 is 3: 5: 8-10: 3: 10: 0.1-0.3; the mass ratio of 1, 4-butanediol, hydroxyethyl methacrylate, pentaerythritol triacrylate, (3-bornyl) triethoxysilane, nano copper sulfide, nano silicon dioxide, acetone, triethylamine and deionized water is 3: 1: 1: 0.1: 0.5: 0.5: 5: 0.2: 8-15.
The method comprises the steps of using a mixed solution of ethylene glycol and water as a solvent, using thioacetamide and copper chloride dihydrate as a sulfur source and a nitrogen source, synthesizing nano copper sulfide by a hydrothermal method, adding the prepared nano copper sulfide and nano silicon dioxide into the prepared aqueous polyurethane solution to obtain a coating agent, wherein due to the addition of hydroxyethyl methacrylate and pentaerythritol triacrylate as acrylic components, the water resistance and heat resistance of an aqueous polyurethane adhesive film can be effectively improved, and due to the presence of (3-hydrophobic propyl) triethoxysilane as an end capping agent and hydrophobic silicon, the hydrophobic silicon is enriched in the interior and on the surface of the adhesive film, so that the water shielding effect of the adhesive film is improved, water molecules are difficult to enter, the hydrophobic property of the polyurethane solution is improved, and the-OC (3-hydrophobic propyl) triethoxysilane is used as an-OC (OC) component2H5The groups react with-OH on the nano silicon dioxide and the nano copper sulfide to obtain the coating agent by taking the nano silicon dioxide and the nano copper sulfide as crosslinking points, wherein the addition of the nano silicon dioxide forms a Si-O-Si crosslinking network to block intermolecular movement and increase the stability and the wear resistance of the coating, the nano copper sulfide belongs to a semiconductor material, the antistatic property of the knitted fabric can be effectively improved by adding the nano copper sulfide into the coating agent, and the nano copper sulfide has stronger ultraviolet absorption capacity and is beneficial to ultraviolet rays due to uneven surfaceSo that the fabric finished by the nano copper sulfide has good ultraviolet resistance effect.
Further, the modified cotton fiber is prepared by the following steps:
step S21, placing cotton in a sodium periodate solution with the concentration of 10g/L, soaking for 2h at the temperature of 30 ℃ in the dark, taking out, washing for 3-5 times by deionized water, transferring to a glycerol solution with the concentration of 0.1mol/L, soaking for 30-60min, washing for 3-5 times by deionized water, dehydrating and airing to obtain oxidized cotton fibers;
step S22, mixing a sodium hypochlorite solution with a molar concentration of 0.025mol/L and a hydrogen peroxide solution with a molar concentration of 0.1mol/L according to a volume ratio of 1: 1, adding the mixture into a beaker, sealing and reacting for 5min by using a preservative film to obtain an oxidation solution a, soaking the oxidized cotton fibers in the oxidation solution a for 1-3h, taking out, cleaning, dehydrating and drying, then placing the oxidized cotton fibers in a silk fibroin solution with the mass fraction of 1-5%, treating for 2h at the temperature of 37 ℃, taking out, washing for 4-6 times by using deionized water, and drying in an oven at the temperature of 50-55 ℃ to constant weight to obtain grafted cotton fibers;
step S23, mixing trihydroxymethyl aminomethane and deionized water according to the weight ratio of 0.5-1 g: adding 50mL of the chitosan into a beaker, stirring at the rotation speed of 50-80r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding a gallic acid monohydrate solution with the concentration of 0.5g/L into the beaker, adding chitosan into a hydrochloric acid solution with the concentration of 0.1mol/L to obtain a chitosan dispersion solution, adding the chitosan dispersion solution into the beaker, and stirring at the rotation speed of 100 plus materials for 200r/min for 30-60min to obtain an antibacterial solution;
the reaction process is as follows:
Figure BDA0002916830480000041
and S24, soaking the grafted cotton fiber obtained in the S22 in the antibacterial liquid obtained in the S23 for 3-5 hours, taking out, washing with 75% volume fraction ethanol solution and deionized water for three times respectively, and finally drying in a 65 ℃ vacuum drying oven for 12 hours to obtain the modified cotton fiber.
Further, the dosage ratio of the tris, the gallic acid monohydrate solution, the chitosan, and the hydrochloric acid solution in step S23 is 0.5-1 g: 100mL of: 1 g: 20-30 mL.
The method comprises the steps of carrying out primary oxidation on cotton by sodium periodate, further oxidizing the cotton by sodium chlorite and hydrogen peroxide to ensure that hydroxyl on the cotton is firstly oxidized into aldehyde groups and then oxidized into carboxyl groups, soaking the cotton in silk fibroin solution, carrying out amide reaction on the carboxyl groups of the cotton and amino groups of the silk fibroin to ensure that the silk fibroin is grafted on the cotton, improving the heat-resistant water washing dissolution loss retention rate of the cotton fibers to obtain grafted cotton fibers, soaking the grafted cotton fibers in antibacterial solution, and carrying out Michael addition or Schiff base reaction on 3,4, 5-trihydroxybenzoic acid which is oxidized into quinone and primary amine groups in chitosan molecules under alkaline Tris buffer solution to ensure that the grafted cotton fibers and the grafted cotton fibers are co-deposited on the surfaces of the grafted cotton fibers, so that the physical properties of the fibers are not damaged and the antibacterial performance of the cotton fibers is endowed.
Further, the modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fibers in acetone for 4 hours, washing the PTT fibers for 3 times by deionized water, placing the PTT fibers in a drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, obtaining washed fibers, soaking the washed fibers in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fibers, washing the washed fibers for 3 times by deionized water, placing the washed fibers in the drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, transferring the PTT fibers to a KH-550 ethanol solution with the mass fraction of 5%, and performing ultrasonic dispersion for 30min at the frequency of 30-40kHz to obtain treated PTT fibers;
step S32, tetrabutyl titanate, triphenyl phosphite and treated PTT fiber are mixed according to the dosage ratio of 3-5 g: 700 mL: 100g of the PTT fiber is uniformly mixed, stirred for 3 hours at the rotating speed of 100-; mixing carbon microspheres, sodium hydroxide and 45% of ethanol solution by mass percent according to the weight ratio of 2-4 g: 1 g: adding 10-20mL of the PTT fiber into a beaker, performing ultrasonic dispersion at the frequency of 20kHz for 20min, adding magnesium chloride into the beaker, stirring and reacting for 15-30min, adding a polyethylene glycol solution with the volume fraction of 1% into the beaker, performing constant-temperature reaction at 40-60 ℃ for 18-24 min to obtain a flame retardant solution, soaking the PTT fiber subjected to moisture draining treatment into the flame retardant solution, performing three-dipping and three-rolling treatment for 3 times with the soaking time of 12h, 3h and 1h respectively and the roller pressure of 0.1MPa for 3 times, and finally drying the dipped and rolled fiber at 90 ℃ for 72h to obtain the modified PTT fiber.
Further, in the step S32, the dosage ratio of the carbon microspheres, the magnesium chloride and the polyethylene glycol solution is 1 g: 1 g: 80-120 mL.
Because the polyester fiber has high degree of orientation of surface molecular chain arrangement, compact crystal lattice, high crystallinity and few active groups, the surface of the fiber presents larger chemical inertness, the surface of the fiber is smooth, no physical engagement point exists between the fiber surface and the groups, and the compounding of the polyester fiber and other materials such as resin, fiber and the like is influenced, the invention uses lithium chloride to etch the surface of the polyester fiber, so that the surface of the polyester fiber presents a rough structure, then uses tetrabutyl titanate and triphenyl phosphite to carry out activation treatment on the polyester fiber, so as to improve the surface activity and the adhesiveness of the fiber surface, further prepares the magnesium oxide wrapped carbon microsphere flame retardant through a hydrothermal synthesis method, further pads the fiber surface to stably load the flame retardant, avoids the pollution of the halogen-containing flame retardant, utilizes the excellent flame retardant, smoke suppression performance and the synergistic flame retardant effect of triphenyl phosphite of the magnesium oxide including the carbon microsphere flame retardant, and forms a compact carbon layer capable of effectively playing the isolation and, thereby blocking heat transfer and release of combustible material.
Further, the preparation method of the waterproof fiber knitted fabric specifically comprises the following steps:
the method comprises the following steps of firstly, manufacturing grey cloth, wherein modified PTT fibers, aramid fibers, modified cotton fibers and bamboo fibers are adopted according to the mass ratio of 1: 1: 1: 1, blending and interweaving the materials into grey cloth, wherein the surface layer adopts modified PTT fiber and aramid fiber, and the inner layer adopts modified cotton fiber and bamboo fiber;
and secondly, preshrinking, dyeing and shaping, preshrinking and dyeing the gray cloth obtained in the first step, and finally coating a coating agent on the surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
The invention has the beneficial effects that:
the grey cloth surface layer is made of modified PTT fiber and aramid fiber, and the inner layer is made of modified cotton fiber and bamboo fiberThe waterproof fiber knitted fabric is prepared by preshrinking, dyeing and sizing, wherein the coating agent is a composite aqueous polyurethane solution, the composite aqueous polyurethane solution has the inner layer of skin-friendly antibacterial, the outer layer of flame-retardant smoke-suppressing and integral waterproof moisture-permeable performances, the waterproofness is that a polyurethane material contains certain hydrophilic groups, the groups firstly capture water vapor molecules emitted by a human body in a hydrogen bond mode, instant gaps are formed among molecular chains due to the thermal motion of the molecular chains of the polyurethane, and the water vapor molecules are transmitted to the other side from one side with high vapor pressure along the dense molecular chain gaps by the push of the water vapor pressure difference between the inner side and the outer side of the film, namely the side contacting with the skin is transmitted to the surrounding environment to achieve the moisture-permeable purpose, and the-OC (3-hydrophobic propyl) triethoxysilane is used for-OC (OC) of2H5The groups react with-OH on nano silicon dioxide and nano copper sulfide, the nano silicon dioxide and the nano copper sulfide are taken as crosslinking points to obtain a coating agent, wherein the addition of the nano silicon dioxide forms a Si-O-Si crosslinking network to block intermolecular movement and increase the stability and the wear resistance of a coating, the nano copper sulfide belongs to a semiconductor material, the antistatic property of a knitted fabric can be effectively improved by adding the nano copper sulfide into the coating agent, the nano copper sulfide has stronger ultraviolet absorption capacity, and the nano copper sulfide is beneficial to reflection and scattering of ultraviolet due to uneven surface and has good ultraviolet resistance effect, wherein protein is grafted on cotton, the hot water washing loss retention rate of the cotton fiber is improved, the grafted cotton fiber is obtained, the grafted cotton fiber is soaked in antibacterial solution, and under the alkaline Tris buffer solution, oxidizing 3,4, 5-trihydroxy benzoic acid into quinone, carrying out Michael addition or Schiff base reaction with a primary amine group in a chitosan molecule, co-depositing the two on the surface of the grafted cotton fiber, endowing the cotton fiber with antibacterial performance while not damaging the physical performance of the fiber, and cooperatively playing the antibacterial performance with the bamboo fibril; the surface of the polyester fiber is etched by using lithium chloride to form a rough structure on the surface, and then is activated by using tetrabutyl titanate and triphenyl phosphite to improve the surface activity and the adhesiveness of the surface of the fiber, and then the magnesium oxide coated carbon microsphere flame retardant is prepared by a hydrothermal synthesis methodAnd then padding to enable the fiber surface to stably load a flame retardant, so that pollution of a halogen-containing flame retardant is avoided, and a compact carbon layer can be effectively formed during combustion by utilizing excellent flame retardant and smoke suppression performance of magnesium oxide including a carbon microsphere flame retardant and the synergistic flame retardant effect of triphenyl phosphite, so that heat transfer and release of combustible substances are blocked.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of waterproof fiber knitted fabric comprises the following steps:
the method comprises the following steps of firstly, manufacturing grey cloth, wherein modified PTT fibers, aramid fibers, modified cotton fibers and bamboo fibers are adopted according to the mass ratio of 1: 1: 1: 1, blending and interweaving the materials into grey cloth, wherein the surface layer adopts modified PTT fiber and aramid fiber, and the inner layer adopts modified cotton fiber and bamboo fiber;
and secondly, preshrinking, dyeing and shaping, preshrinking and dyeing the gray cloth obtained in the first step, and finally coating a coating agent on the surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
The preparation method of the coating agent comprises the following steps:
step S11, adding 1-butyl-3-methylimidazole chloride and ethylene glycol into a reaction kettle, stirring at a rotating speed of 80r/min for 10min, adding copper chloride dihydrate into the reaction kettle, continuously stirring at a constant rotating speed for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 20min, washing precipitates for 3 times by using an ethanol solution with a mass fraction of 40%, and finally drying in an oven at 60 ℃ for 8h to obtain nano copper sulfide;
step S12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant-temperature vacuum oven at 80 ℃ for 2h, adding the dried 1, 4-butanediol and polytetrahydrofuran ether glycol into a three-neck flask under the protection of nitrogen, then adding isophorone diisocyanate, bis (hydroxymethyl) propionic acid, N-dimethylacetamide and dibutyltin dilaurate, reacting for 2h in a constant-temperature oil bath environment at 75 ℃, cooling to 55 ℃, adding hydroxyethyl methacrylate and pentaerythritol triacrylate into the three-neck flask, stirring at the rotating speed of 100r/min for 1h, cooling to 35 ℃, adding (3-hydrophobic propyl) triethoxysilane, nano copper sulfide, nano silicon dioxide and acetone into the three-neck flask, stirring at a constant rotating speed for 3h, adding triethylamine into the three-neck flask, increasing the rotating speed to 300r/min, stirring for 30min, adding deionized water, reacting for 40min at constant rotation speed, and distilling under reduced pressure to remove acetone to obtain the coating agent.
The dosage ratio of the 1-butyl-3-methylimidazole chloride, the glycol, the copper chloride dihydrate and the thioacetamide in the step S11 is 1 g: 20mL of: 3 g: 3g, wherein the mass ratio of the 1, 4-butanediol, the polytetrahydrofuran ether glycol, the isophorone diisocyanate, the bis (hydroxymethyl) propionic acid, the N, N-dimethylacetamide and the dibutyltin dilaurate in the step S12 is 3: 5: 8: 3: 10: 0.1; the mass ratio of 1, 4-butanediol, hydroxyethyl methacrylate, pentaerythritol triacrylate, (3-bornyl) triethoxysilane, nano copper sulfide, nano silicon dioxide, acetone, triethylamine and deionized water is 3: 1: 1: 0.1: 0.5: 0.5: 5: 0.2: 8.
the modified cotton fiber is prepared by the following steps:
step S21, placing cotton in a sodium periodate solution with the concentration of 10g/L, soaking for 2h at the temperature of 30 ℃ in the dark, taking out, washing for 3 times by using deionized water, transferring to a glycerol solution with the concentration of 0.1mol/L, soaking for 30min, washing for 3 times by using the deionized water, dehydrating and airing to obtain oxidized cotton fibers;
step S22, mixing a sodium hypochlorite solution with a molar concentration of 0.025mol/L and a hydrogen peroxide solution with a molar concentration of 0.1mol/L according to a volume ratio of 1: 1, adding the mixture into a beaker, sealing and reacting for 5min by using a preservative film to obtain an oxidation solution a, soaking the oxidized cotton fibers in the oxidation solution a for 1h, taking out, cleaning, dehydrating and drying, then placing the oxidized cotton fibers in a silk fibroin solution with the mass fraction of 1%, treating the oxidized cotton fibers at 37 ℃ for 2h, taking out, washing the oxidized cotton fibers for 4 times by using deionized water, and drying the oxidized cotton fibers in a 50 ℃ oven to constant weight to obtain grafted cotton fibers;
step S23, mixing tris and deionized water according to a ratio of 0.5 g: adding 50mL of the chitosan into a beaker, stirring at the rotating speed of 50r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding a gallic acid monohydrate solution with the concentration of 0.5g/L into the beaker, adding chitosan into a hydrochloric acid solution with the concentration of 0.1mol/L to obtain a chitosan dispersion solution, adding the chitosan dispersion solution into the beaker, and stirring at the rotating speed of 100r/min for 30min to obtain an antibacterial solution;
and S24, soaking the grafted cotton fiber obtained in the S22 in the antibacterial liquid obtained in the S23 for 3 hours, taking out, washing with ethanol solution with volume fraction of 75% and deionized water for three times respectively, and finally drying in a 65 ℃ vacuum drying oven for 12 hours to obtain the modified cotton fiber.
The dosage ratio of the tris (hydroxymethyl) aminomethane, the gallic acid monohydrate solution, the chitosan and the hydrochloric acid solution in step S23 is 0.5 g: 100mL of: 1 g: 20 mL.
The modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fibers in acetone for 4 hours, washing the PTT fibers for 3 times by deionized water, placing the PTT fibers in a drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, obtaining washed fibers, soaking the washed fibers in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fibers, washing the washed fibers for 3 times by deionized water, placing the washed fibers in the drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, transferring the PTT fibers to a KH-550 ethanol solution with the mass fraction of 5%, and performing ultrasonic dispersion for 30 minutes at the frequency of 30kHz to obtain treated PTT fibers;
step S32, mixing tetrabutyl titanate, triphenyl phosphite and treated PTT fiber according to the dosage ratio of 3 g: 700 mL: uniformly mixing 100g of the PTT fiber, stirring for 3 hours at the rotating speed of 100r/min, standing for 3 hours, taking out the PTT fiber, and draining for later use; mixing carbon microspheres, sodium hydroxide and 45% of ethanol solution by mass percent according to the following ratio of 2 g: 1 g: adding 10mL of the PTT fiber into a beaker, performing ultrasonic dispersion at the frequency of 20kHz for 20min, adding magnesium chloride into the beaker, stirring and reacting for 15min, adding a polyethylene glycol solution with the volume fraction of 1% into the beaker, reacting at the constant temperature of 40 ℃ for 18h to obtain a flame retardant solution, soaking the PTT fiber subjected to moisture draining treatment into the flame retardant solution, performing three-soaking and three-rolling treatment by adopting three times of soaking for 12h, 3h and 1h respectively, and the roller pressure for 3 times of 0.1MPa, and finally drying the soaked and rolled fiber at the temperature of 90 ℃ for 72h to obtain the modified PTT fiber.
In the step S32, the dosage ratio of the carbon microspheres to the magnesium chloride to the polyethylene glycol solution is 1 g: 1 g: 80 mL.
Example 2
A preparation method of waterproof fiber knitted fabric comprises the following steps:
the method comprises the following steps of firstly, manufacturing grey cloth, wherein modified PTT fibers, aramid fibers, modified cotton fibers and bamboo fibers are adopted according to the mass ratio of 1: 1: 1: 1, blending and interweaving the materials into grey cloth, wherein the surface layer adopts modified PTT fiber and aramid fiber, and the inner layer adopts modified cotton fiber and bamboo fiber;
and secondly, preshrinking, dyeing and shaping, preshrinking and dyeing the gray cloth obtained in the first step, and finally coating a coating agent on the surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
The preparation method of the coating agent comprises the following steps:
step S11, adding 1-butyl-3-methylimidazole chloride and ethylene glycol into a reaction kettle, stirring at a rotating speed of 80r/min for 10min, adding copper chloride dihydrate into the reaction kettle, continuously stirring at a constant rotating speed for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 30min, washing precipitates for 4 times by using an ethanol solution with a mass fraction of 40%, and finally drying in an oven at 60 ℃ for 9h to obtain nano copper sulfide;
step S12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant-temperature vacuum oven at 80 ℃ for 2h, adding the dried 1, 4-butanediol and polytetrahydrofuran ether glycol into a three-neck flask under the protection of nitrogen, then adding isophorone diisocyanate, bis (hydroxymethyl) propionic acid, N-dimethylacetamide and dibutyltin dilaurate, reacting for 2h in a constant-temperature oil bath environment at 75 ℃, cooling to 55 ℃, adding hydroxyethyl methacrylate and pentaerythritol triacrylate into the three-neck flask, stirring for 1h at the rotation speed of 150r/min, cooling to 35 ℃, adding (3-hydrophobic propyl) triethoxysilane, nano copper sulfide, nano silicon dioxide and acetone into the three-neck flask, stirring for 3h at a constant rotation speed, adding triethylamine into the three-neck flask, increasing the rotation speed to 400r/min, stirring for 30min, adding deionized water, reacting for 40min at constant rotation speed, and distilling under reduced pressure to remove acetone to obtain the coating agent.
The dosage ratio of the 1-butyl-3-methylimidazole chloride, the glycol, the copper chloride dihydrate and the thioacetamide in the step S11 is 1 g: 30mL of: 3 g: 3g, wherein the mass ratio of the 1, 4-butanediol, the polytetrahydrofuran ether glycol, the isophorone diisocyanate, the bis (hydroxymethyl) propionic acid, the N, N-dimethylacetamide and the dibutyltin dilaurate in the step S12 is 3: 5: 9: 3: 10: 0.2; the mass ratio of 1, 4-butanediol, hydroxyethyl methacrylate, pentaerythritol triacrylate, (3-bornyl) triethoxysilane, nano copper sulfide, nano silicon dioxide, acetone, triethylamine and deionized water is 3: 1: 1: 0.1: 0.5: 0.5: 5: 0.2: 11.
the modified cotton fiber is prepared by the following steps:
step S21, placing cotton in sodium periodate solution with the concentration of 10g/L, soaking for 2h at the temperature of 30 ℃ in the dark, taking out, washing for 4 times by using deionized water, transferring to glycerol solution with the concentration of 0.1mol/L, soaking for 45min, washing for 3-5 times by using the deionized water, dehydrating and airing to obtain oxidized cotton fibers;
step S22, mixing a sodium hypochlorite solution with a molar concentration of 0.025mol/L and a hydrogen peroxide solution with a molar concentration of 0.1mol/L according to a volume ratio of 1: 1, adding the mixture into a beaker, sealing and reacting for 5min by using a preservative film to obtain an oxidation solution a, soaking the oxidized cotton fibers in the oxidation solution a for 2h, taking out, cleaning, dehydrating and drying, then placing the oxidized cotton fibers in a silk fibroin solution with the mass fraction of 2%, treating the oxidized cotton fibers for 2h at the temperature of 37 ℃, taking out, washing the oxidized cotton fibers for 5 times by using deionized water, and drying the oxidized cotton fibers in a drying oven at the temperature of 52 ℃ to constant weight to obtain grafted cotton fibers;
step S23, mixing tris and deionized water according to a ratio of 0.8 g: adding 50mL of the chitosan into a beaker, stirring at the rotating speed of 60r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding a gallic acid monohydrate solution with the concentration of 0.5g/L into the beaker, adding chitosan into a hydrochloric acid solution with the concentration of 0.1mol/L to obtain a chitosan dispersion solution, adding the chitosan dispersion solution into the beaker, and stirring at the rotating speed of 150r/min for 40min to obtain an antibacterial solution;
and S24, soaking the grafted cotton fiber obtained in the S22 in the antibacterial liquid obtained in the S23 for 4 hours, taking out, washing with ethanol solution with volume fraction of 75% and deionized water for three times respectively, and finally drying in a 65 ℃ vacuum drying oven for 12 hours to obtain the modified cotton fiber.
The dosage ratio of the tris (hydroxymethyl) aminomethane, the gallic acid monohydrate solution, the chitosan and the hydrochloric acid solution in step S23 is 0.8 g: 100mL of: 1 g: 25 mL.
The modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fibers in acetone for 4 hours, washing the PTT fibers for 3 times by deionized water, placing the PTT fibers in a drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, obtaining washed fibers, soaking the washed fibers in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fibers, washing the washed fibers for 3 times by deionized water, placing the washed fibers in the drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, transferring the PTT fibers to a KH-550 ethanol solution with the mass fraction of 5%, and performing ultrasonic dispersion for 30min at the frequency of 35kHz to obtain treated PTT fibers;
step S32, tetrabutyl titanate, triphenyl phosphite and treated PTT fiber are mixed according to the dosage ratio of 4 g: 700 mL: uniformly mixing 100g of the PTT fiber, stirring for 3 hours at the rotating speed of 120r/min, standing for 3 hours, taking out the PTT fiber, and draining for later use; mixing carbon microspheres, sodium hydroxide and 45% of ethanol solution by mass percent according to the weight ratio of 3 g: 1 g: adding 15mL of the PTT fiber into a beaker, performing ultrasonic dispersion at the frequency of 20kHz for 20min, adding magnesium chloride into the beaker, stirring and reacting for 25min, adding a polyethylene glycol solution with the volume fraction of 1% into the beaker, performing constant-temperature reaction at 50 ℃ for 20h to obtain a flame retardant solution, soaking the PTT fiber subjected to moisture draining treatment in the flame retardant solution, performing three-soaking and three-rolling treatment by adopting three times of soaking for 12h, 3h and 1h respectively, and performing rolling pressure at 0.1MPa for 3 times, and finally drying the soaked and rolled fiber at 90 ℃ for 72h to obtain the modified PTT fiber.
In the step S32, the dosage ratio of the carbon microspheres to the magnesium chloride to the polyethylene glycol solution is 1 g: 1 g: 100 mL.
Example 3
A preparation method of waterproof fiber knitted fabric comprises the following steps:
the method comprises the following steps of firstly, manufacturing grey cloth, wherein modified PTT fibers, aramid fibers, modified cotton fibers and bamboo fibers are adopted according to the mass ratio of 1: 1: 1: 1, blending and interweaving the materials into grey cloth, wherein the surface layer adopts modified PTT fiber and aramid fiber, and the inner layer adopts modified cotton fiber and bamboo fiber;
and secondly, preshrinking, dyeing and shaping, preshrinking and dyeing the gray cloth obtained in the first step, and finally coating a coating agent on the surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
The preparation method of the coating agent comprises the following steps:
step S11, adding 1-butyl-3-methylimidazole chloride and ethylene glycol into a reaction kettle, stirring at a rotating speed of 80r/min for 10min, adding copper chloride dihydrate into the reaction kettle, continuously stirring at a constant rotating speed for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 40min, washing precipitates for 5 times by using an ethanol solution with a mass fraction of 40%, and finally drying in an oven at 60 ℃ for 8-10h to obtain nano copper sulfide;
step S12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant-temperature vacuum oven at 80 ℃ for 2h, adding the dried 1, 4-butanediol and polytetrahydrofuran ether glycol into a three-neck flask under the protection of nitrogen, then adding isophorone diisocyanate, bis (hydroxymethyl) propionic acid, N-dimethylacetamide and dibutyltin dilaurate, reacting for 2h in a constant-temperature oil bath environment at 75 ℃, cooling to 55 ℃, adding hydroxyethyl methacrylate and pentaerythritol triacrylate into the three-neck flask, stirring at the rotation speed of 200r/min for 1h, cooling to 35 ℃, adding (3-hydrophobic propyl) triethoxysilane, nano copper sulfide, nano silicon dioxide and acetone into the three-neck flask, stirring at the constant rotation speed for 3h, adding triethylamine into the three-neck flask, increasing the rotation speed to 500r/min, stirring for 30min, adding deionized water, reacting for 40min at constant rotation speed, and distilling under reduced pressure to remove acetone to obtain the coating agent.
The dosage ratio of the 1-butyl-3-methylimidazole chloride, the glycol, the copper chloride dihydrate and the thioacetamide in the step S11 is 1 g: 40mL of: 3 g: 3g, wherein the mass ratio of the 1, 4-butanediol, the polytetrahydrofuran ether glycol, the isophorone diisocyanate, the bis (hydroxymethyl) propionic acid, the N, N-dimethylacetamide and the dibutyltin dilaurate in the step S12 is 3: 5: 10: 3: 10: 0.3; the mass ratio of 1, 4-butanediol, hydroxyethyl methacrylate, pentaerythritol triacrylate, (3-bornyl) triethoxysilane, nano copper sulfide, nano silicon dioxide, acetone, triethylamine and deionized water is 3: 1: 1: 0.1: 0.5: 0.5: 5: 0.2: 15.
the modified cotton fiber is prepared by the following steps:
step S21, placing cotton in a sodium periodate solution with the concentration of 10g/L, soaking for 2h at the temperature of 30 ℃ in the dark, taking out, washing for 5 times by using deionized water, transferring to a glycerol solution with the concentration of 0.1mol/L, soaking for 60min, washing for 5 times by using the deionized water, dehydrating and airing to obtain oxidized cotton fibers;
step S22, mixing a sodium hypochlorite solution with a molar concentration of 0.025mol/L and a hydrogen peroxide solution with a molar concentration of 0.1mol/L according to a volume ratio of 1: 1, adding the mixture into a beaker, sealing and reacting for 5min by using a preservative film to obtain an oxidation solution a, soaking the oxidized cotton fibers in the oxidation solution a for 3h, taking out, cleaning, dehydrating and drying, then placing the oxidized cotton fibers in a silk fibroin solution with the mass fraction of 5%, treating the oxidized cotton fibers for 2h at the temperature of 37 ℃, taking out, washing the oxidized cotton fibers for 6 times by using deionized water, and drying the dehydrated cotton fibers in a 55 ℃ oven to constant weight to obtain grafted cotton fibers;
step S23, mixing trihydroxymethyl aminomethane and deionized water according to the proportion of 1 g: adding 50mL of the chitosan into a beaker, stirring at the rotating speed of 80r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding a gallic acid monohydrate solution with the concentration of 0.5g/L into the beaker, adding chitosan into a hydrochloric acid solution with the concentration of 0.1mol/L to obtain a chitosan dispersion solution, adding the chitosan dispersion solution into the beaker, and stirring at the rotating speed of 200r/min for 60min to obtain an antibacterial solution;
and S24, soaking the grafted cotton fiber obtained in the S22 in the antibacterial liquid obtained in the S23 for 5 hours, taking out, washing with ethanol solution with volume fraction of 75% and deionized water for three times respectively, and finally drying in a vacuum drying oven at 65 ℃ for 12 hours to obtain the modified cotton fiber.
The dosage ratio of the tris (hydroxymethyl) aminomethane, the gallic acid monohydrate solution, the chitosan and the hydrochloric acid solution in step S23 is 1 g: 100mL of: 1 g: 30 mL.
The modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fibers in acetone for 4 hours, washing the PTT fibers for 3 times by deionized water, placing the PTT fibers in a drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, obtaining washed fibers, soaking the washed fibers in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fibers, washing the washed fibers for 3 times by deionized water, placing the washed fibers in the drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, transferring the PTT fibers to a KH-550 ethanol solution with the mass fraction of 5%, and performing ultrasonic dispersion for 30min at the frequency of 40kHz to obtain treated PTT fibers;
step S32, mixing tetrabutyl titanate, triphenyl phosphite and treated PTT fiber according to the dosage ratio of 5 g: 700 mL: uniformly mixing 100g of the PTT fiber, stirring for 3 hours at the rotating speed of 150r/min, standing for 3 hours, taking out the PTT fiber, and draining for later use; mixing carbon microspheres, sodium hydroxide and 45% of ethanol solution by mass percent according to a ratio of 4 g: 1 g: adding 20mL of the PTT fiber into a beaker, performing ultrasonic dispersion at the frequency of 20kHz for 20min, adding magnesium chloride into the beaker, stirring and reacting for 30min, adding a polyethylene glycol solution with the volume fraction of 1% into the beaker, performing constant-temperature reaction at 60 ℃ for 24 min to obtain a flame retardant solution, soaking the PTT fiber subjected to moisture draining treatment in the flame retardant solution, performing three-dipping and three-rolling treatment for 3 times, wherein the dipping time is 12h, 3h and 1h respectively, the rolling pressure is 0.1MPa for 3 times, and finally drying the dipped and rolled fiber at 90 ℃ for 72h to obtain the modified PTT fiber.
In the step S32, the dosage ratio of the carbon microspheres to the magnesium chloride to the polyethylene glycol solution is 1 g: 1 g: 120 mL.
Comparative example
The comparative example is a fiber knitted fabric commonly seen on the market.
Examples 1-3 and comparative examples were tested for performance, with the following test criteria:
limiting oxygen index: according to the standard/LOI in FZT 50017 + 2011;
antibacterial property: according to the GB/T20944.3-2008 standard, determining the bacteriostatic rate of the fiber fabric on staphylococcus aureus;
antistatic performance: the volume resistivity/omega cm is measured and is required to be lower than 1014Ω·cm；
Skin-friendly Properties: cutting the fabric into the same size, distributing the fabric to 10 testees, evaluating the soft feeling of the fabric by 0 to 5 parts, and taking an average value to record;
air permeability: measuring air permeability (mm/s) by using a YG (B) model 461D digital fabric air permeameter according to the detection method described in GB/T5453-1997;
moisture permeability: the moisture permeability (g/m) was measured by the detection method described in GB/T12704-91 using a DH-400 moisture permeability test apparatus2·24h)。
The test structure is shown in the following table:
Figure BDA0002916830480000171
as can be seen from the above table, the performances of examples 1-3 in the processes of limiting oxygen index, bacteriostasis rate, volume resistivity, soft feeling, air permeability and moisture permeability test are superior to those of comparative examples, which shows that the waterproof fiber fabric prepared by the invention has flame retardant, antibacterial, antistatic, moisture permeable and breathable properties and skin-friendly and soft performances.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.

Claims (8)

1. The waterproof fiber knitted fabric is characterized by being prepared by the following steps:
the method comprises the following steps of firstly, manufacturing grey cloth, wherein modified PTT fibers, aramid fibers, modified cotton fibers and bamboo fibers are adopted according to the mass ratio of 1: 1: 1: 1, blending and interweaving the materials into grey cloth, wherein the surface layer adopts modified PTT fiber and aramid fiber, and the inner layer adopts modified cotton fiber and bamboo fiber;
and secondly, preshrinking, dyeing and shaping, preshrinking and dyeing the gray cloth obtained in the first step, and finally coating a coating agent on the surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
2. The waterproof fiber knitted fabric according to claim 1, wherein the preparation method of the coating agent comprises the following steps:
step S11, adding 1-butyl-3-methylimidazole chloride and ethylene glycol into a reaction kettle, stirring at a rotating speed of 80r/min for 10min, adding copper chloride dihydrate into the reaction kettle, continuously stirring at a constant rotating speed for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 20-40min, washing precipitates for 3-5 times by using an ethanol solution with a mass fraction of 40%, and finally drying in an oven at 60 ℃ for 8-10h to obtain nano copper sulfide;
step S12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant-temperature vacuum oven at 80 ℃ for 2h, adding the dried 1, 4-butanediol and polytetrahydrofuran ether glycol into a three-neck flask under the protection of nitrogen, then adding isophorone diisocyanate, bis (hydroxymethyl) propionic acid, N-dimethylacetamide and dibutyltin dilaurate, reacting for 2h in a constant-temperature oil bath environment at 75 ℃, cooling to 55 ℃, adding hydroxyethyl methacrylate and pentaerythritol triacrylate into the three-neck flask, stirring at the rotation speed of 100-, adding deionized water, reacting for 40min at constant rotation speed, and distilling under reduced pressure to remove acetone to obtain the coating agent.
3. The waterproof fiber knitted fabric according to claim 2, wherein the amount ratio of 1-butyl-3-methylimidazole chloride, ethylene glycol, copper chloride dihydrate and thioacetamide used in step S11 is 1 g: 20-40 mL: 3 g: 3g, wherein the mass ratio of the 1, 4-butanediol, the polytetrahydrofuran ether glycol, the isophorone diisocyanate, the bis (hydroxymethyl) propionic acid, the N, N-dimethylacetamide and the dibutyltin dilaurate in the step S12 is 3: 5: 8-10: 3: 10: 0.1-0.3; the mass ratio of 1, 4-butanediol, hydroxyethyl methacrylate, pentaerythritol triacrylate, (3-bornyl) triethoxysilane, nano copper sulfide, nano silicon dioxide, acetone, triethylamine and deionized water is 3: 1: 1: 0.1: 0.5: 0.5: 5: 0.2: 8-15.
4. The waterproof fiber knitted fabric according to claim 1, wherein the modified cotton fiber is prepared by the following steps:
step S21, placing cotton in a sodium periodate solution with the concentration of 10g/L, soaking for 2h at the temperature of 30 ℃ in the dark, taking out, washing for 3-5 times by deionized water, transferring to a glycerol solution with the concentration of 0.1mol/L, soaking for 30-60min, washing for 3-5 times by deionized water, dehydrating and airing to obtain oxidized cotton fibers;
step S22, mixing a sodium hypochlorite solution with a molar concentration of 0.025mol/L and a hydrogen peroxide solution with a molar concentration of 0.1mol/L according to a volume ratio of 1: 1, adding the mixture into a beaker, sealing and reacting for 5min by using a preservative film to obtain an oxidation solution a, soaking the oxidized cotton fibers in the oxidation solution a for 1-3h, taking out, cleaning, dehydrating and drying, then placing the oxidized cotton fibers in a silk fibroin solution with the mass fraction of 1-5%, treating for 2h at the temperature of 37 ℃, taking out, washing for 4-6 times by using deionized water, and drying in an oven at the temperature of 50-55 ℃ to constant weight to obtain grafted cotton fibers;
step S23, mixing trihydroxymethyl aminomethane and deionized water according to the weight ratio of 0.5-1 g: adding 50mL of the chitosan into a beaker, stirring at the rotation speed of 50-80r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding a gallic acid monohydrate solution with the concentration of 0.5g/L into the beaker, adding chitosan into a hydrochloric acid solution with the concentration of 0.1mol/L to obtain a chitosan dispersion solution, adding the chitosan dispersion solution into the beaker, and stirring at the rotation speed of 100 plus materials for 200r/min for 30-60min to obtain an antibacterial solution;
and S24, soaking the grafted cotton fiber obtained in the S22 in the antibacterial liquid obtained in the S23 for 3-5 hours, taking out, washing with 75% volume fraction ethanol solution and deionized water for three times respectively, and finally drying in a 65 ℃ vacuum drying oven for 12 hours to obtain the modified cotton fiber.
5. The waterproof fiber knitted fabric according to claim 4, wherein the dosage ratio of the tris, the gallic acid monohydrate solution, the chitosan, and the hydrochloric acid solution in step S23 is 0.5-1 g: 100mL of: 1 g: 20-30 mL.
6. The waterproof fiber knitted fabric according to claim 1, wherein the modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fibers in acetone for 4 hours, washing the PTT fibers for 3 times by deionized water, placing the PTT fibers in a drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, obtaining washed fibers, soaking the washed fibers in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fibers, washing the washed fibers for 3 times by deionized water, placing the washed fibers in the drying oven at 60 ℃ for drying until the weight of the PTT fibers is constant, transferring the PTT fibers to a KH-550 ethanol solution with the mass fraction of 5%, and performing ultrasonic dispersion for 30min at the frequency of 30-40kHz to obtain treated PTT fibers;
step S32, tetrabutyl titanate, triphenyl phosphite and treated PTT fiber are mixed according to the dosage ratio of 3-5 g: 700 mL: 100g of the PTT fiber is uniformly mixed, stirred for 3 hours at the rotating speed of 100-; mixing carbon microspheres, sodium hydroxide and 45% of ethanol solution by mass percent according to the weight ratio of 2-4 g: 1 g: adding 10-20mL of the PTT fiber into a beaker, performing ultrasonic dispersion at the frequency of 20kHz for 20min, adding magnesium chloride into the beaker, stirring and reacting for 15-30min, adding a polyethylene glycol solution with the volume fraction of 1% into the beaker, performing constant-temperature reaction at 40-60 ℃ for 18-24 min to obtain a flame retardant solution, soaking the PTT fiber subjected to moisture draining treatment into the flame retardant solution, performing three-dipping and three-rolling treatment for 3 times with the soaking time of 12h, 3h and 1h respectively and the roller pressure of 0.1MPa for 3 times, and finally drying the dipped and rolled fiber at 90 ℃ for 72h to obtain the modified PTT fiber.
7. The waterproof fiber knitted fabric according to claim 6, wherein the amount ratio of the carbon microspheres to the magnesium chloride to the polyethylene glycol solution in step S32 is 1 g: 1 g: 80-120 mL.
8. The preparation method of the waterproof fiber knitted fabric according to claim 1, which is characterized by comprising the following steps:
the method comprises the following steps of firstly, manufacturing grey cloth, wherein modified PTT fibers, aramid fibers, modified cotton fibers and bamboo fibers are adopted according to the mass ratio of 1: 1: 1: 1, blending and interweaving the materials into grey cloth, wherein the surface layer adopts modified PTT fiber and aramid fiber, and the inner layer adopts modified cotton fiber and bamboo fiber;
and secondly, preshrinking, dyeing and shaping, preshrinking and dyeing the gray cloth obtained in the first step, and finally coating a coating agent on the surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
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