CN112900089B - 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
CN112900089B
CN112900089B CN202110103318.2A CN202110103318A CN112900089B CN 112900089 B CN112900089 B CN 112900089B CN 202110103318 A CN202110103318 A CN 202110103318A CN 112900089 B CN112900089 B CN 112900089B
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fiber
solution
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deionized water
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CN112900089A (en
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崔永珍
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Guangzhou Chuanqi Garment Co ltd
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Guangzhou Chuanqi Garment 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
    • 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
    • D—TEXTILES; PAPER
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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
    • 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
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    • 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
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    • 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
    • D06N2203/068—Polyurethanes
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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
    • D06N2209/105—Resistant to abrasion, scratch
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    • D06N2209/00—Properties of the materials
    • D06N2209/16—Properties of the materials having other properties
    • D06N2209/1678—Resistive to light or to UV
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    • 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
    • D10B2201/02—Cotton
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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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  • Engineering & Computer Science (AREA)
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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Biochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Inorganic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a waterproof fiber knitted fabric and a preparation method thereof, comprising the following steps: firstly, manufacturing grey cloth, wherein modified PTT fiber, aramid fiber, modified cotton fiber and bamboo fiber are adopted according to the mass ratio of 1:1:1:1 blending and interweaving the mixture 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, namely preshrinking and dyeing the embryo cloth obtained in the first step, and finally coating a coating agent on a 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 aqueous polyurethane coating agent, the waterproof fiber knitted fabric prepared by the invention not only has good skin-friendly, soft and antibacterial performance, but also has the performances 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 increasingly valued. The knitted fabric is popular, namely, the knitted fabric is formed by bending yarns into loops by using knitting needles and mutually stringing the yarns, and the knitted fabric is different from the carboxywoven fabric in the form of the yarns in the fabric. At present, knitted fabrics are widely applied to products such as clothing fabrics, lining fabrics, home textiles and the like, but the knitted fabrics have a common problem, for example, various knitted fabrics, knitted sweaters, woolen sweaters, bedding articles and the like, and the knitted fabrics are easy to form balls, are poor in waterproof and air permeability, are easy to grow mold bacteria and are easy to generate electrostatic effect due to continuous or small friction in actual wearing and washing processes, and the flame retardant property of the fabrics is poor, so that the knitted fabrics are seriously restricted from being applied to places such as clothing, bedding and buildings, and therefore, the knitted fabrics with waterproof, antistatic, flame retardant, antibacterial and wear-resistant functions are the technical problem to be solved at present.
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, the fiber fabric is easy to ball due to continuous friction with larger or smaller friction in the actual wearing and washing process, has poor waterproof and air permeability, is easy to breed mould bacteria, is easy to generate static electricity, and has poor flame retardant property.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of waterproof fiber knitted fabric comprises the following steps:
firstly, manufacturing grey cloth, wherein modified PTT fiber, aramid fiber, modified cotton fiber and bamboo fiber are adopted according to the mass ratio of 1:1:1:1 blending and interweaving the mixture 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, namely preshrinking and dyeing the embryo cloth obtained in the step one, and finally coating a coating agent on a 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:
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 rotating speed of unchanged for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 20-40min, washing the precipitate with 40% ethanol solution for 3-5 times, and finally drying in a 60 ℃ oven for 8-10h to obtain nano copper sulfide;
s12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant temperature vacuum oven at 80 ℃ for 2 hours, 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 2 hours in an oil bath environment at 75 ℃ constant temperature, cooling to 55 ℃, adding hydroxyethyl methacrylate and pentaerythritol triacrylate into the three-neck flask, stirring for 1 hour at the rotating speed of 100-200r/min, cooling to 35 ℃, adding (3-mercaptopropyl) triethoxysilane, nano copper sulfide, nano silicon dioxide and acetone into the three-neck flask, stirring for 3 hours at the constant rotating speed, adding triethylamine into the three-neck flask, stirring for 30 minutes at the rotating speed of 300-500r/min, adding deionized water, continuously reacting for 40 minutes at the constant rotating speed, and distilling under reduced pressure to remove the acetone, thereby obtaining the coating agent.
Further, the dosage ratio of 1-butyl-3-methylimidazole chloride, ethylene glycol, copper chloride dihydrate and thioacetamide in step S11 is 1g:20-40mL:3g:3g, wherein the mass ratio of the 1, 4-butanediol, polytetrahydrofuran ether glycol, isophorone diisocyanate, dimethylolpropionic acid, N-dimethylacetamide and 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-lyophobyl) 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.
With mixtures of ethylene glycol and waterThe preparation method comprises the steps of using thioacetamide and copper chloride dihydrate as sulfur sources and nitrogen sources, synthesizing nano copper sulfide by a hydrothermal method, adding the prepared nano copper sulfide and nano silicon dioxide into a prepared aqueous polyurethane solution to obtain a coating agent, effectively improving the water resistance and heat resistance of the aqueous polyurethane adhesive film by adding hydroxyethyl methacrylate and pentaerythritol triacrylate as acrylic components, and enriching the hydrophobic silicon in the adhesive film and on the surface by using (3-hydrophobic) triethoxysilane as a blocking agent, so that the shielding effect of the adhesive film on water is improved, water molecules are difficult to enter, the hydrophobic property of the polyurethane solution is improved, and the hydrophobic property of the polyurethane solution is improved by using (3-hydrophobic) triethoxysilane-OC 2 H 5 The group reacts with-OH on nano silicon dioxide and nano copper sulfide, the nano silicon dioxide and the nano copper sulfide are used as crosslinking points to obtain a coating agent, wherein the nano silicon dioxide is added to form a Si-O-Si crosslinking network to block movement among molecules, so that the stability and wear resistance of the coating are improved, the nano copper sulfide belongs to a semiconductor material, and the nano copper sulfide is added into the coating agent, so that the antistatic performance of a knitted fabric can be effectively improved, and the nano copper sulfide has stronger ultraviolet absorption capability, and is favorable for reflecting and scattering ultraviolet due to uneven surface, so that the fabric finished by the nano copper sulfide has good ultraviolet resistance.
Further, the modified cotton fiber is prepared by the following steps:
s21, placing cotton in a sodium periodate solution with the concentration of 10g/L, soaking for 2 hours at the temperature of 30 ℃ in a dark condition, taking out, washing with deionized water for 3-5 times, transferring to a glycerol solution with the concentration of 0.1mol/L, soaking for 30-60min, washing with deionized water for 3-5 times, dehydrating, and airing to obtain oxidized cotton fibers;
step S22, 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 are mixed according to a volume ratio of 1:1, adding into a beaker, sealing with a preservative film for reaction for 5min to obtain an oxidation solution a, soaking oxidized cotton fibers in the oxidation solution a for 1-3h, taking out, washing, dehydrating, airing, putting into a silk fibroin solution with the mass fraction of 1-5%, treating for 2h at the temperature of 37 ℃, taking out, washing with deionized water for 4-6 times, and drying in a baking oven at the temperature of 50-55 ℃ to constant weight to obtain grafted cotton fibers;
step S23, mixing the tris (hydroxymethyl) aminomethane and deionized water according to 0.5-1g: adding 50mL into a beaker, stirring at a rotating speed of 50-80r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding gallic acid monohydrate solution with a concentration of 0.5g/L into the beaker, adding chitosan into hydrochloric acid solution with a concentration of 0.1mol/L to obtain chitosan dispersion liquid, adding the chitosan dispersion liquid into the beaker, and stirring at a rotating speed of 100-200r/min for 30-60min to obtain antibacterial liquid;
the reaction process is as follows:
Figure BDA0002916830480000041
and S24, soaking the grafted cotton fibers obtained in the step S22 in the antibacterial liquid obtained in the step S23 for 3-5 hours, taking out, washing three times with ethanol solution with the volume fraction of 75% and deionized water respectively, and finally drying in a vacuum drying oven at 65 ℃ for 12 hours to obtain the modified cotton fibers.
Further, the dosage ratio of the tris (hydroxymethyl) aminomethane, the gallic acid monohydrate solution, the chitosan and the hydrochloric acid solution in the step S23 is 0.5-1g:100mL:1g:20-30mL.
The cotton is subjected to preliminary oxidation by sodium periodate, and is further oxidized by sodium chlorite and hydrogen peroxide, so that hydroxyl groups on the cotton are oxidized into aldehyde groups and then carboxyl groups, and then the aldehyde groups are soaked in a silk fibroin solution, the carboxyl groups of the cotton and amino groups of the silk fibroin are subjected to amide reaction, so that silk fibroin is grafted on the cotton, the heat-resistant water washing dissolution retention rate of cotton fibers is improved, the grafted cotton fibers are obtained, the grafted cotton fibers are soaked in an antibacterial solution, and 3,4, 5-trihydroxybenzoic acid is oxidized into quinone under an alkaline Tris buffer solution and subjected to Michael addition or Schiff base reaction with primary amine groups in chitosan molecules, so that the hydroxyl groups and the carboxyl groups are co-deposited on the surfaces of the grafted cotton fibers, and the antibacterial properties of the cotton fibers are endowed without damaging the physical properties of the fibers.
Further, the modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fiber in acetone for 4 hours, washing with deionized water for 3 times, drying in an oven at 60 ℃ until the weight is constant to obtain washed fiber, soaking the washed fiber in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fiber, washing with deionized water for 3 times, drying in the oven at 60 ℃ until the weight is constant, transferring the washed fiber into a KH-550 ethanol solution with the mass fraction of 5%, and performing ultrasonic dispersion for 30 minutes at the frequency of 30-40kHz to obtain treated PTT fiber;
step S32, tetrabutyl titanate, triphenyl phosphite and treated PTT fiber are mixed according to the dosage ratio of 3-5g:700mL:100g of the PTT fiber is uniformly mixed, stirred for 3 hours at the rotating speed of 100-150r/min, then kept stand for 3 hours, taken out for processing the PTT fiber, and drained for standby; mixing carbon microspheres, sodium hydroxide and 45% ethanol solution according to the mass fraction of 2-4g:1g: adding 10-20mL into a beaker, performing ultrasonic dispersion for 20min at the frequency of 20kHz, adding magnesium chloride into the beaker, stirring for reaction for 15-30min, adding polyethylene glycol solution with the volume fraction of 1% into the beaker, performing constant-temperature reaction at the temperature of 40-60 ℃ for 18-24 min to obtain flame retardant liquid, soaking PTT fibers subjected to water draining treatment into the flame retardant liquid, performing three-soaking and three-rolling treatment for 3 times, wherein the soaking time is 12h, 3h and 1h respectively, the roller pressure is 0.1MPa for 3 times, and finally drying the padded fibers at the temperature of 90 ℃ for 72h to obtain the modified PTT fibers.
Further, the dosage ratio of the carbon microsphere, magnesium chloride and polyethylene glycol solution in the step S32 is 1g:1g:80-120mL.
The invention uses lithium chloride to etch the surface of the polyester fiber to make the surface of the polyester fiber have a rough structure, then uses tetrabutyl titanate and triphenyl phosphite to activate the surface, improves the surface activity and adhesiveness of the fiber surface, and further prepares magnesium oxide to wrap the carbon microsphere flame retardant through a hydrothermal synthesis method, and then padding to make the fiber surface stably load the flame retardant, thereby avoiding pollution of halogen-containing flame retardant.
Further, the preparation method of the waterproof fiber knitted fabric specifically comprises the following steps:
firstly, manufacturing grey cloth, wherein modified PTT fiber, aramid fiber, modified cotton fiber and bamboo fiber are adopted according to the mass ratio of 1:1:1:1 blending and interweaving the mixture 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, namely preshrinking and dyeing the embryo cloth obtained in the step one, and finally coating a coating agent on a surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
The invention has the beneficial effects that:
the grey fabric surface layer is made of modified PTT fiber and aramid fiber, the inner layer is made of modified cotton fiber and bamboo fiber, and then the waterproof fiber knitted fabric is obtained through preshrinking, dyeing and shaping, wherein the coating agent is a composite aqueous polyurethane solution, has the functions of inner layer skin-friendly antibacterial, outer layer flame retardance and smoke suppression, and integral waterproof moisture permeability, wherein the waterproof property is that the polyurethane material contains certain hydrophilic groups, the groups firstly capture water vapor molecules emitted by a human body in a hydrogen bond form, instant gaps are formed between molecular chains due to the thermal motion of polyurethane molecular chains, the water vapor molecules are transferred from one side with high vapor pressure to the other side along the dense molecular chain gaps by pushing the difference of water vapor pressure at the inner side and the outer side of the film, namely one side contacted with skin is transferred to the surrounding environment, and the moisture permeability is achieved by the-OC of (3-hydrophobic) triethoxysilane 2 H 5 The radical reacts with-OH on nano silicon dioxide and nano copper sulfide, and the nano silicon dioxide and nano copper sulfide are used as crosslinking points to obtain the coating agent, wherein nano IIThe silicon oxide is added to form a Si-O-Si cross-linked network to block movement among molecules and increase stability and wear resistance of a coating, nano copper sulfide belongs to a semiconductor material, and is added to a coating agent to effectively improve antistatic performance of a knitted fabric, and the nano copper sulfide has stronger ultraviolet absorption capacity, so that the fabric finished by the nano copper sulfide has good ultraviolet resistance effect due to uneven surface, is favorable for reflection and scattering of ultraviolet rays, wherein silk fibroin is grafted on cotton to improve the heat-resistant water washing loss retention rate of cotton fibers, the grafted cotton fibers are obtained, the grafted cotton fibers are soaked in an antibacterial solution, and 3,4, 5-trihydroxybenzoic acid is oxidized into quinone under an alkaline Tris buffer solution to perform Michael addition or Schiff base reaction with primary amine groups in chitosan molecules, so that the nano copper sulfide is co-deposited on the surface of the grafted cotton fibers, and the nano copper sulfide can give antibacterial performance to the cotton fibers and the bamboo fibers to play antibacterial performance synergistically; the surface of the polyester fiber is etched by using lithium chloride to form a rough structure, tetrabutyl titanate and triphenyl phosphite are used for activating the polyester fiber, so that the surface activity and adhesiveness of the fiber surface are improved, magnesium oxide is prepared to wrap a carbon microsphere flame retardant through a hydrothermal synthesis method, the fiber surface is further padded to stably load the flame retardant, pollution of the halogen-containing flame retardant is avoided, the magnesium oxide comprises the synergistic flame retardant effect of the carbon microsphere flame retardant and the triphenyl phosphite, and a compact carbon layer can effectively play isolation and protection effects when combustion is carried out, and heat transfer and release of combustible substances are blocked.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of waterproof fiber knitted fabric comprises the following steps:
firstly, manufacturing grey cloth, wherein modified PTT fiber, aramid fiber, modified cotton fiber and bamboo fiber are adopted according to the mass ratio of 1:1:1:1 blending and interweaving the mixture 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, namely preshrinking and dyeing the embryo cloth obtained in the step one, and finally coating a coating agent on a surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
The preparation method of the coating agent comprises the following steps:
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 rotating speed of unchanged for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 20min, washing the precipitate with 40% ethanol solution for 3 times, and finally drying in a baking oven at 60 ℃ for 8h to obtain nano copper sulfide;
s12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant temperature vacuum oven at 80 ℃ for 2 hours, 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 2 hours 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 1 hour at the rotating speed of 100r/min, cooling to 35 ℃, adding (3-lyophobic) triethoxysilane, nano copper sulfide, nano silicon dioxide and acetone into the three-neck flask, stirring for 3 hours at the rotating speed of unchanged, adding triethylamine into the three-neck flask, stirring for 30 minutes after the rotating speed is increased to 300r/min, adding deionized water, continuously reacting for 40 minutes at the rotating speed, and distilling under reduced pressure to remove the acetone, thereby obtaining the coating agent.
The dosage ratio of the 1-butyl-3-methylimidazole chloride, the ethylene glycol, the copper chloride dihydrate and the thioacetamide in the step S11 is 1g:20mL:3g:3g, wherein the mass ratio of the 1, 4-butanediol, polytetrahydrofuran ether glycol, isophorone diisocyanate, dimethylolpropionic acid, N-dimethylacetamide and 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-lyophobyl) 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:
s21, placing cotton in a sodium periodate solution with the concentration of 10g/L, soaking for 2 hours at the temperature of 30 ℃ in a dark condition, taking out, washing with deionized water for 3 times, transferring to a glycerol solution with the concentration of 0.1mol/L, soaking for 30 minutes, washing with deionized water for 3 times, dehydrating and airing to obtain oxidized cotton fibers;
step S22, 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 are mixed according to a volume ratio of 1:1 adding into a beaker, sealing with a preservative film for reaction for 5min to obtain an oxidation solution a, soaking oxidized cotton fibers in the oxidation solution a for 1h, taking out, washing, dehydrating, airing, putting into a silk fibroin solution with the mass fraction of 1%, treating for 2h at 37 ℃, taking out, washing with deionized water for 4 times, and drying in a 50 ℃ oven to constant weight to obtain grafted cotton fibers;
step S23, mixing tris (hydroxymethyl) aminomethane and deionized water according to 0.5g: adding 50mL into a beaker, stirring at a rotating speed of 50r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding gallic acid monohydrate solution with a concentration of 0.5g/L into the beaker, adding chitosan into hydrochloric acid solution with a concentration of 0.1mol/L to obtain chitosan dispersion liquid, adding the chitosan dispersion liquid into the beaker, and stirring for 30min at a rotating speed of 100r/min to obtain antibacterial liquid;
and S24, soaking the grafted cotton fibers obtained in the step S22 in the antibacterial liquid obtained in the step S23 for 3 hours, taking out, washing three times with ethanol solution with the volume fraction of 75% and deionized water respectively, and finally drying in a vacuum drying oven at 65 ℃ for 12 hours to obtain the modified cotton fibers.
The dosage ratio of the trimethylol aminomethane, the gallic acid monohydrate solution, the chitosan and the hydrochloric acid solution in the step S23 is 0.5g:100mL:1g:20mL.
The modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fiber in acetone for 4 hours, washing with deionized water for 3 times, drying in an oven at 60 ℃ until the weight is constant to obtain washed fiber, soaking the washed fiber in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fiber, washing with deionized water for 3 times, drying in the oven at 60 ℃ until the weight is constant, transferring the washed fiber into 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 fiber;
step S32, tetrabutyl titanate, triphenyl phosphite and treated PTT fiber are mixed according to the dosage ratio of 3g:700mL:100g of the PTT fiber is uniformly mixed, stirred for 3 hours at the rotating speed of 100r/min, then kept still for 3 hours, taken out for processing the PTT fiber, and drained for standby; the carbon microspheres, sodium hydroxide and 45% ethanol solution by mass percent are mixed according to the following weight percentage of 2g:1g: adding 10mL into a beaker, performing ultrasonic dispersion for 20min at the frequency of 20kHz, adding magnesium chloride into the beaker, stirring and reacting for 15min, adding polyethylene glycol solution with the volume fraction of 1% into the beaker, performing constant-temperature reaction for 18h at the temperature of 40 ℃ to obtain flame retardant liquid, soaking the PTT fiber subjected to water draining treatment into the flame retardant liquid, performing three-soaking and three-rolling treatment for 3 times respectively for 12h, 3h and 1h, and performing roller pressure for 3 times for 0.1MPa, and finally drying the padded fiber at the temperature of 90 ℃ for 72h to obtain the modified PTT fiber.
The dosage ratio of the carbon microsphere, the magnesium chloride and the polyethylene glycol solution in the step S32 is 1g:1g:80mL.
Example 2
A preparation method of waterproof fiber knitted fabric comprises the following steps:
firstly, manufacturing grey cloth, wherein modified PTT fiber, aramid fiber, modified cotton fiber and bamboo fiber are adopted according to the mass ratio of 1:1:1:1 blending and interweaving the mixture 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, namely preshrinking and dyeing the embryo cloth obtained in the step one, and finally coating a coating agent on a surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
The preparation method of the coating agent comprises the following steps:
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 rotating speed of unchanged for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 30min, washing the precipitate with 40% ethanol solution for 4 times, and finally drying in a 60 ℃ oven for 9h to obtain nano copper sulfide;
s12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant temperature vacuum oven at 80 ℃ for 2 hours, 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 2 hours 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 1 hour at the rotating speed of 150r/min, cooling to 35 ℃, adding (3-lyophobic) triethoxysilane, nano copper sulfide, nano silicon dioxide and acetone into the three-neck flask, stirring for 3 hours at the rotating speed of unchanged, adding triethylamine into the three-neck flask, stirring for 30 minutes at the rotating speed of 400r/min, adding deionized water, continuously reacting for 40 minutes at the rotating speed of unchanged, and distilling under reduced pressure to remove the acetone, thereby obtaining the coating agent.
The dosage ratio of the 1-butyl-3-methylimidazole chloride, the ethylene glycol, the copper chloride dihydrate and the thioacetamide in the step S11 is 1g:30mL:3g:3g, wherein the mass ratio of the 1, 4-butanediol, polytetrahydrofuran ether glycol, isophorone diisocyanate, dimethylolpropionic acid, N-dimethylacetamide and 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-lyophobyl) 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:
s21, placing cotton in a sodium periodate solution with the concentration of 10g/L, soaking for 2 hours at the temperature of 30 ℃ in a dark condition, taking out, washing for 4 times by using deionized water, transferring to a glycerol solution with the concentration of 0.1mol/L, soaking for 45 minutes, washing for 3-5 times by using deionized water, dehydrating and airing to obtain oxidized cotton fibers;
step S22, 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 are mixed according to a volume ratio of 1:1, adding into a beaker, sealing with a preservative film for reaction for 5min to obtain an oxidation solution a, soaking oxidized cotton fibers in the oxidation solution a for 2h, taking out, washing, dehydrating, airing, putting into a silk fibroin solution with the mass fraction of 2%, treating for 2h at the temperature of 37 ℃, taking out, washing with deionized water for 5 times, and drying in a 52 ℃ oven to constant weight to obtain grafted cotton fibers;
step S23, mixing tris (hydroxymethyl) aminomethane and deionized water according to 0.8g: adding 50mL into a beaker, stirring at a rotating speed of 60r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding gallic acid monohydrate solution with a concentration of 0.5g/L into the beaker, adding chitosan into hydrochloric acid solution with a concentration of 0.1mol/L to obtain chitosan dispersion liquid, adding the chitosan dispersion liquid into the beaker, and stirring for 40min at a rotating speed of 150r/min to obtain antibacterial liquid;
and S24, soaking the grafted cotton fibers obtained in the step S22 in the antibacterial liquid obtained in the step S23 for 4 hours, taking out, washing three times with ethanol solution with the volume fraction of 75% and deionized water respectively, and finally drying in a vacuum drying oven at 65 ℃ for 12 hours to obtain the modified cotton fibers.
The dosage ratio of the trimethylol aminomethane, the gallic acid monohydrate solution, the chitosan and the hydrochloric acid solution in the step S23 is 0.8g:100mL:1g:25mL.
The modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fiber in acetone for 4 hours, washing with deionized water for 3 times, drying in an oven at 60 ℃ until the weight is constant to obtain washed fiber, soaking the washed fiber in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fiber, washing with deionized water for 3 times, drying in the oven at 60 ℃ until the weight is constant, transferring the washed fiber into a KH-550 ethanol solution with the mass fraction of 5%, and performing ultrasonic dispersion for 30 minutes at the frequency of 35kHz to obtain treated PTT fiber;
step S32, tetrabutyl titanate, triphenyl phosphite and treated PTT fiber are mixed according to the dosage ratio of 4g:700mL:100g of the PTT fiber is uniformly mixed, stirred for 3 hours at the rotating speed of 120r/min, then kept still for 3 hours, taken out for processing the PTT fiber, and drained for standby; the method comprises the steps of mixing carbon microspheres, sodium hydroxide and 45% ethanol solution according to the mass fraction of 3g:1g:15mL is added into a beaker, after ultrasonic dispersion is carried out for 20min at the frequency of 20kHz, magnesium chloride is added into the beaker, stirring reaction is carried out for 25min, polyethylene glycol solution with the volume fraction of 1% is added into the beaker, constant temperature reaction is carried out for 20h at 50 ℃ to obtain flame retardant liquid, the PTT fiber subjected to water draining treatment is soaked in the flame retardant liquid, three soaking and three rolling treatments are adopted, the soaking time is respectively 12h, 3h and 1h, the roller pressure is 0.1MPa for 3 times, and finally the soaked fiber is dried for 72h at 90 ℃ to obtain the modified PTT fiber.
The dosage ratio of the carbon microsphere, the magnesium chloride and the polyethylene glycol solution in the step S32 is 1g:1g:100mL.
Example 3
A preparation method of waterproof fiber knitted fabric comprises the following steps:
firstly, manufacturing grey cloth, wherein modified PTT fiber, aramid fiber, modified cotton fiber and bamboo fiber are adopted according to the mass ratio of 1:1:1:1 blending and interweaving the mixture 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, namely preshrinking and dyeing the embryo cloth obtained in the step one, and finally coating a coating agent on a surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
The preparation method of the coating agent comprises the following steps:
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 rotating speed of unchanged for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 40min, washing the precipitate with 40% ethanol solution for 5 times, and finally drying in a 60 ℃ oven for 8-10h to obtain nano copper sulfide;
s12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant temperature vacuum oven at 80 ℃ for 2 hours, 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 2 hours 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 1 hour at the rotating speed of 200r/min, cooling to 35 ℃, adding (3-lyophobic) triethoxysilane, nano copper sulfide, nano silicon dioxide and acetone into the three-neck flask, stirring for 3 hours at the rotating speed of unchanged, adding triethylamine into the three-neck flask, stirring for 30 minutes after the rotating speed is increased to 500r/min, adding deionized water, continuously reacting for 40 minutes at the rotating speed, and distilling under reduced pressure to remove the acetone, thereby obtaining the coating agent.
The dosage ratio of the 1-butyl-3-methylimidazole chloride, the ethylene glycol, the copper chloride dihydrate and the thioacetamide in the step S11 is 1g:40mL:3g:3g, wherein the mass ratio of the 1, 4-butanediol, polytetrahydrofuran ether glycol, isophorone diisocyanate, dimethylolpropionic acid, N-dimethylacetamide and 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-lyophobyl) 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:
s21, placing cotton in a sodium periodate solution with the concentration of 10g/L, soaking for 2 hours at the temperature of 30 ℃ in a dark condition, taking out, washing with deionized water for 5 times, transferring to a glycerol solution with the concentration of 0.1mol/L, soaking for 60 minutes, washing with deionized water for 5 times, dehydrating and airing to obtain oxidized cotton fibers;
step S22, 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 are mixed according to a volume ratio of 1:1, adding into a beaker, sealing with a preservative film for reaction for 5min to obtain an oxidation solution a, soaking oxidized cotton fibers in the oxidation solution a for 3h, taking out, washing, dehydrating, airing, putting into a silk fibroin solution with the mass fraction of 5%, treating for 2h at the temperature of 37 ℃, taking out, washing with deionized water for 6 times, and drying in a baking oven at the temperature of 55 ℃ to constant weight to obtain grafted cotton fibers;
step S23, mixing tris (hydroxymethyl) aminomethane and deionized water according to the weight ratio of 1g: adding 50mL into a beaker, stirring at a rotating speed of 80r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding gallic acid monohydrate solution with a concentration of 0.5g/L into the beaker, adding chitosan into hydrochloric acid solution with a concentration of 0.1mol/L to obtain chitosan dispersion liquid, adding the chitosan dispersion liquid into the beaker, and stirring for 60min at a rotating speed of 200r/min to obtain antibacterial liquid;
and S24, soaking the grafted cotton fibers obtained in the step S22 in the antibacterial liquid obtained in the step S23 for 5 hours, taking out, washing three times with ethanol solution with the volume fraction of 75% and deionized water respectively, and finally drying in a vacuum drying oven at 65 ℃ for 12 hours to obtain the modified cotton fibers.
The dosage ratio of the trimethylol aminomethane, the gallic acid monohydrate solution, the chitosan and the hydrochloric acid solution in the step S23 is 1g:100mL:1g:30mL.
The modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fiber in acetone for 4 hours, washing with deionized water for 3 times, drying in an oven at 60 ℃ until the weight is constant to obtain washed fiber, soaking the washed fiber in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fiber, washing with deionized water for 3 times, drying in the oven at 60 ℃ until the weight is constant, transferring the washed fiber into a KH-550 ethanol solution with the mass fraction of 5%, and performing ultrasonic dispersion for 30 minutes at the frequency of 40kHz to obtain treated PTT fiber;
step S32, tetrabutyl titanate, triphenyl phosphite and treated PTT fiber are mixed according to the dosage ratio of 5g:700mL:100g of the PTT fiber is uniformly mixed, stirred for 3 hours at the rotating speed of 150r/min, then kept still for 3 hours, taken out for processing the PTT fiber, and drained for standby; mixing carbon microspheres, sodium hydroxide and 45% ethanol solution according to the mass fraction of 4g:1g: adding 20mL into a beaker, performing ultrasonic dispersion for 20min at the frequency of 20kHz, adding magnesium chloride into the beaker, stirring and reacting for 30min, adding polyethylene glycol solution with the volume fraction of 1% into the beaker, performing constant-temperature reaction at the temperature of 60 ℃ for 24 hours to obtain flame retardant liquid, soaking the PTT fiber subjected to water draining treatment into the flame retardant liquid, performing three-soaking and three-rolling treatment for 3 times, wherein the soaking time is 12h, 3h and 1h respectively, the roller pressure is 0.1MPa for 3 times, and finally drying the padded fiber at the temperature of 90 ℃ for 72h to obtain the modified PTT fiber.
The dosage ratio of the carbon microsphere, the magnesium chloride and the polyethylene glycol solution in the step S32 is 1g:1g:120mL.
Comparative example
The comparative example is a fiber knitted fabric commonly found in the market.
The performance test was performed on examples 1-3 and comparative examples, with the following criteria:
limiting oxygen index: standard/LOI according to FZT 50017-2011;
antibacterial performance: according to GB/T20944.3-2008 standard, determining the antibacterial rate of the fiber fabric to staphylococcus aureus;
antistatic properties: the volume resistivity/Ω & cm is measured and is required to be less than 10 14 Ω·cm；
Skin-friendly properties: the fabric was cut into the same size shape and distributed to 10 subjects who evaluated the soft feel in 0 to 5 parts, and recorded on average;
air permeability: according to the detection method described in GB/T5453-1997, the air permeability (mm/s) was measured by using YG (B) 461D type digital fabric air permeability meter;
moisture permeability: according to the detection method described in GB/T12704-91, the moisture permeability (g/m) was measured using a DH-400 type moisture permeability test apparatus 2 ·24h)。
The test structures are shown in the following table:
Figure BDA0002916830480000171
as can be seen from the table, the performances of the examples 1-3 are better than those of the comparative examples in the test process of limiting oxygen index, antibacterial rate, volume resistivity, soft feel, air permeability and moisture permeability, and the waterproof fiber fabric prepared by the invention has the performances of flame retardance, antibacterial property, static resistance, moisture permeability and air permeability and skin-friendly and flexible properties.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.

Claims (5)

1. The waterproof fiber knitted fabric is characterized by being prepared by the following steps:
firstly, manufacturing grey cloth, wherein modified PTT fiber, aramid fiber, modified cotton fiber and bamboo fiber are adopted according to the mass ratio of 1:1:1:1 blending and interweaving the mixture 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, namely preshrinking and dyeing the embryo cloth obtained in the first step, and finally coating a coating agent on a surface layer for curing and shaping to obtain the waterproof fiber knitted fabric;
the preparation method of the coating agent comprises the following steps:
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 rotating speed of unchanged for 10min, adding thioacetamide, continuously stirring for 5min, adding deionized water, centrifuging at a rotating speed of 12000r/min for 20-40min, washing the precipitate with 40% ethanol solution for 3-5 times, and finally drying in a 60 ℃ oven for 8-10h to obtain nano copper sulfide;
s12, drying 1, 4-butanediol and polytetrahydrofuran ether glycol in a constant temperature vacuum oven at 80 ℃ for 2 hours, 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 2 hours in an oil bath environment at 75 ℃ constant temperature, cooling to 55 ℃, adding hydroxyethyl methacrylate and pentaerythritol triacrylate into the three-neck flask, stirring for 1 hour at the rotating speed of 100-200r/min, cooling to 35 ℃, adding (3-mercaptopropyl) triethoxysilane, nano copper sulfide, nano silicon dioxide and acetone into the three-neck flask, stirring for 3 hours at the constant rotating speed, adding triethylamine into the three-neck flask, stirring for 30 minutes at the rotating speed of 300-500r/min, adding deionized water, continuously reacting for 40 minutes at the constant rotating speed, and distilling under reduced pressure to remove the acetone to obtain the coating agent;
the modified cotton fiber is prepared by the following steps:
s21, placing cotton in a sodium periodate solution with the concentration of 10g/L, soaking for 2 hours at the temperature of 30 ℃ in a dark condition, taking out, washing with deionized water for 3-5 times, transferring to a glycerol solution with the concentration of 0.1mol/L, soaking for 30-60min, washing with deionized water for 3-5 times, dehydrating, and airing to obtain oxidized cotton fibers;
step S22, 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 are mixed according to a volume ratio of 1:1, adding into a beaker, sealing with a preservative film for reaction for 5min to obtain an oxidation solution a, soaking oxidized cotton fibers in the oxidation solution a for 1-3h, taking out, washing, dehydrating, airing, putting into a silk fibroin solution with the mass fraction of 1-5%, treating for 2h at the temperature of 37 ℃, taking out, washing with deionized water for 4-6 times, and drying in a baking oven at the temperature of 50-55 ℃ to constant weight to obtain grafted cotton fibers;
step S23, mixing the tris (hydroxymethyl) aminomethane and deionized water according to 0.5-1g: adding 50mL into a beaker, stirring at a rotating speed of 50-80r/min for 10min, adding hydrochloric acid into the beaker to adjust the pH value to 8.5, then adding gallic acid monohydrate solution with a concentration of 0.5g/L into the beaker, adding chitosan into hydrochloric acid solution with a concentration of 0.1mol/L to obtain chitosan dispersion liquid, adding the chitosan dispersion liquid into the beaker, and stirring at a rotating speed of 100-200r/min for 30-60min to obtain antibacterial liquid;
step S24, soaking the grafted cotton fibers obtained in the step S22 in the antibacterial liquid obtained in the step S23 for 3-5 hours, taking out, washing three times with ethanol solution with the volume fraction of 75% and deionized water respectively, and finally drying in a vacuum drying oven at 65 ℃ for 12 hours to obtain modified cotton fibers;
the modified PTT fiber is prepared by the following steps:
step S31, soaking PTT fiber in acetone for 4 hours, washing with deionized water for 3 times, drying in an oven at 60 ℃ until the weight is constant to obtain washed fiber, soaking the washed fiber in a lithium chloride ethanol solution with the mass fraction of 6.5% for 3 hours, taking out the washed fiber, washing with deionized water for 3 times, drying in the oven at 60 ℃ until the weight is constant, transferring the washed fiber into a KH-550 ethanol solution with the mass fraction of 5%, and performing ultrasonic dispersion for 30 minutes at the frequency of 30-40kHz to obtain treated PTT fiber;
step S32, tetrabutyl titanate, triphenyl phosphite and treated PTT fiber are mixed according to the dosage ratio of 3-5g:700mL:100g of the PTT fiber is uniformly mixed, stirred for 3 hours at the rotating speed of 100-150r/min, then kept stand for 3 hours, taken out for processing the PTT fiber, and drained for standby; mixing carbon microspheres, sodium hydroxide and 45% ethanol solution according to the mass fraction of 2-4g:1g: adding 10-20mL into a beaker, performing ultrasonic dispersion for 20min at the frequency of 20kHz, adding magnesium chloride into the beaker, stirring for reaction for 15-30min, adding polyethylene glycol solution with the volume fraction of 1% into the beaker, performing constant-temperature reaction at the temperature of 40-60 ℃ for 18-24 min to obtain flame retardant liquid, soaking PTT fibers subjected to water draining treatment into the flame retardant liquid, performing three-soaking and three-rolling treatment for 3 times, wherein the soaking time is 12h, 3h and 1h respectively, the roller pressure is 0.1MPa for 3 times, and finally drying the padded fibers at the temperature of 90 ℃ for 72h to obtain the modified PTT fibers.
2. The waterproof fiber knitted fabric according to claim 1, wherein the dosage ratio of 1-butyl-3-methylimidazole chloride, ethylene glycol, copper chloride dihydrate and thioacetamide in step S11 is 1g:20-40mL:3g:3g, wherein the mass ratio of the 1, 4-butanediol, polytetrahydrofuran ether glycol, isophorone diisocyanate, dimethylolpropionic acid, N-dimethylacetamide and 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-lyophobyl) 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.
3. The waterproof fiber knitted fabric according to claim 1, wherein the dosage ratio of the tris (hydroxymethyl) aminomethane, the gallic acid monohydrate solution, the chitosan and the hydrochloric acid solution in the step S23 is 0.5-1g:100mL:1g:20-30mL.
4. The waterproof fiber knitted fabric according to claim 1, wherein the dosage ratio of the carbon microsphere, magnesium chloride and polyethylene glycol solution in the step S32 is 1g:1g:80-120mL.
5. The method for preparing the waterproof fiber knitted fabric according to claim 1, which is characterized by comprising the following steps:
firstly, manufacturing grey cloth, wherein modified PTT fiber, aramid fiber, modified cotton fiber and bamboo fiber are adopted according to the mass ratio of 1:1:1:1 blending and interweaving the mixture 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, namely preshrinking and dyeing the embryo cloth obtained in the step one, and finally coating a coating agent on a surface layer for curing and shaping to obtain the waterproof fiber knitted fabric.
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