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CN109653005A - A kind of antibacterial fabric preparation method based on graphene - Google Patents

A kind of antibacterial fabric preparation method based on graphene Download PDF

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Publication number
CN109653005A
CN109653005A CN201811602932.8A CN201811602932A CN109653005A CN 109653005 A CN109653005 A CN 109653005A CN 201811602932 A CN201811602932 A CN 201811602932A CN 109653005 A CN109653005 A CN 109653005A
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fabric
graphene
temperature
antibacterial
preparation
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CN201811602932.8A
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CN109653005B (en
Inventor
易汉平
韩建坊
刘宏伟
高古辉
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Tianjin North Graphene Industrial Research Institute
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Tianjin North Graphene Industrial Research Institute
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651Compounds without nitrogen
    • D06P1/65106Oxygen-containing compounds
    • D06P1/65125Compounds containing ester groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/73Treating 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
    • D06M11/74Treating 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/0032Determining dye recipes and dyeing parameters; Colour matching or monitoring
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/445Use of auxiliary substances before, during or after dyeing or printing
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/60General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
    • D06P1/613Polyethers without nitrogen
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/673Inorganic compounds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/673Inorganic compounds
    • D06P1/67333Salts or hydroxides
    • D06P1/6735Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/34Material containing ester groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The antibacterial fabric preparation method based on graphene that the present invention provides a kind of, comprising the following steps: (1) fabric pre-treatment: fabric is impregnated using the treatment fluid containing lye and bleeding agent, then fabric is washed till neutrality with water;(2) prepared by dye liquor: graphene oxide slurry is diluted with water, buffer solution and BB lotion is then added, mixes to obtain dye liquor;BB lotion is the mixed emulsion of Ergol and castor oil polyoxyethylene ether;(3) with certain bath raio, using the method for temperature programming, high-temperature dyeing high-temperature dyeing: is carried out to fabric;(4) drying bake: the temperature condition prior to 110-150 DEG C dries the fabric after high-temperature dyeing, later by the fabric after drying in 180-200 DEG C baking 1-5 minutes, as based on the antibacterial fabric of graphene.Antibacterial fabric preparation method of the present invention based on graphene, simple process is easily operated, and the textile fabric of preparation has excellent antibacterial, anti-ultraviolet function and Contact cool feeling performance.

Description

A kind of antibacterial fabric preparation method based on graphene
Technical field
The invention belongs to technical field of textile manufacture, are related to a kind of textile fabric processing technology with safeguard function, Especially a kind of antibacterial fabric preparation method based on graphene.
Background technique
As people require increasingly to improve to environmental sanitation, the application of anti-biotic material is by more extensive concern.Bacterium Breeding can be mushroomed out in suitable environmental conditions, and by spreading the disease with human contact, the body for influencing people is strong. The textile fabric consisted of fibers, since the chemical structure of its porous type body form and high molecular polymer is conducive to micro- life Object attachment, becomes the good parasitic body of the microbe survivals such as bacterium, fungi, breeding.The textile that people contact in daily life It is the ground of the good existence of these microorganisms and the important propagating source of various diseases, so exploitation has the weaving of antibacterial row Product have extremely important meaning.
Currently, most of the textile with antibacterial functions is to carry out final finishing to textile with antibacterial finishing agent agent, with Obtain the textile with anti-microbial property.Reason agent is divided into inorganic antibacterial finishing agent, organic anti-bacterial finishing agent after common antibacterial is whole With natural biological antibacterial finishing agent three categories.Inorganic antiseptic is with inorganic metal class antibacterial agent, photocatalysis antibacterial agent and nanoparticle Based on sub- antibacterial agent;Organic antibacterial agent is then a kind of the molecule with antibacterial activity to be bonded in one with carrier by covalent bond It rises, mainly includes quaternary ammonium salt antibacterial agent, quaternary phosphonium salt antibacterial agent, alcohols antibacterial agent, phenolic antiseptic etc.;Natural biological is anti- Microbial inoculum is the antibacterial agent of the polymer composition with antibacterial functions extracted in natural biological, and there are commonly shells Glycan, allicin etc..
Graphene oxide (GO) is an important derivative in graphene family, essentially identical with the structure of graphene, Only there is the oxygen containing functional group such as a large amount of hydroxyl, carboxyl, epoxy group on its surface, these functional groups impart graphite oxide The many unique properties of alkene, such as good wettability and surface-active, can be with the compatibility of some polymer etc., this can To assign material more chemical reactivities, adjacent layer can also be made to form network structure raising monolithic interlayer by being crosslinked Interaction force, so as to improve the physical property of material.With the development of GO functional method, the oxygen-containing collection of different function Group assigns GO more potential advantage, also starts to increase in the application of antibiosis.
Currently based on graphene antibacterial dacron fabric preparation method there are mainly two types of, one is preparing polyester slice Stage adds graphene, prepares graphene dacron thread, and one is be organized in by padding method combining graphene on fabric. It is easy to cause the reunion of graphene in dicing phase addition graphene, and complex process, graphene dispersion uniformity cannot get Guarantee.It is arranged in the final finishing stage by padding method, the graphene amount for needing to add organic crosslinking agent, and being combined on fabric Less, binding force is weaker;High-temperature and high pressure dyeing process, in the case where being baked without high temperature, the binding force of graphene and fabric Weaker, fastness to washing does not reach requirement.
Summary of the invention
In view of this, the present invention is directed to propose a kind of antibacterial fabric preparation method based on graphene, to overcome existing skill The defect of art, simple process is easily operated, is suitable for factory mass production, and the textile fabric of preparation has excellent resist Bacterium, anti-ultraviolet function and Contact cool feeling performance, can be applied to underwear, bedding, hygienic material, footgear, decoration material The fields such as material, non-woven fabrics.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of antibacterial fabric preparation method based on graphene, comprising the following steps:
(1) fabric pre-treatment: impregnating fabric using the treatment fluid containing lye and bleeding agent, then with water by face Material is washed till neutrality;
(2) prepared by dye liquor: graphene oxide slurry is diluted with water, buffer solution and BB lotion is then added, mixes to obtain dye Liquid;BB lotion is the mixed emulsion of Ergol and castor oil polyoxyethylene ether;
(3) with certain bath raio, using the method for temperature programming, high-temperature dyeing high-temperature dyeing: is carried out to fabric;Wherein, The process of temperature programming are as follows: -85 DEG C of room temperature, 2 DEG C of heating rate is per minute;85 DEG C -110 DEG C, 1 DEG C of heating rate per minute, is protected It is 6-14 minutes warm;110 DEG C -130 DEG C, 0.5 DEG C of heating rate per minute, keeps the temperature 25-35 minutes;130 DEG C -50 DEG C, rate of temperature fall 3 DEG C per minute;
(4) drying bakes: the temperature condition prior to 110-150 DEG C dries the fabric after high-temperature dyeing, later will Fabric after drying in 180-200 DEG C baking 1-5 minutes, as based on the antibacterial fabric of graphene.
Preferably, in step (1), the treatment fluid includes each component of following mass fraction: the hydrogen-oxygen of 1-5wt% Change sodium, the bleeding agent of 0.1-3wt%, surplus is water.The addition of bleeding agent can be significantly reduced the use of sodium hydroxide.
Preferably, in step (1), after the method for fabric pre-treatment is the following steps are included: be first heated to 35 DEG C for treatment fluid It is put into fabric;85 DEG C are then warming up to, keeps the temperature 1 hour;It is impregnated 10 minutes with 60 DEG C of water again;It is primary with 50 DEG C of washings again;Finally Web surface is washed to 30 DEG C to be in neutrality.
Preferably, in step (1), the bath raio of fabric and treatment fluid is 1:20.
Preferably, in step (1), one or more of bleeding agent JFC, JFC-1, JFC-2, JFC-E's is mixed Close object;In step (2), in resulting dye liquor, graphene oxide content is 0.05-0.5g/L, buffer content 0.10- 0.50g/L, BB emulsion content are 0.1-1.0g/L.
Preferably, in step (2), the graphene oxide solid content in the graphene oxide slurry is 1.0- 3.4wt%, and the oxygen content of surface of graphene oxide is 40-50wt%.
Preferably, in step (2), the buffer is acetic acid salt system buffer, and dye liquor pH value is controlled in 3-5.
Preferably, in the BB lotion, the mass ratio of Ergol and castor oil polyoxyethylene ether is 1:4-4: 1。
Preferably, in step (3), 85 DEG C -110 DEG C, 1 DEG C of heating rate per minute, keeps the temperature 10 minutes;110℃-130 DEG C, 0.5 DEG C of heating rate per minute, keeps the temperature 30 minutes;Bath raio is 1:5-1:30.
Preferably, the fabric is polyester fabric;In step (4), after temperature condition prior to 130 DEG C is to high-temperature dyeing Fabric dried, later by the fabric after drying in 180-200 DEG C baking 1-5 minutes, as based on the antibacterial of graphene Fabric.
It should be noted that existing directly heating solution dyeing is uneven, dyeing quality be cannot be guaranteed, the present invention Middle progress gradient increased temperature can make graphene oxide is more uniform to be distributed on polyester fabric.In addition, polyester fabric (namely Polyester fabric) at 180-200 DEG C, the lattice movement of polyester fiber can be reinforced, and graphene oxide molecule is made to enter terylene fibre In dimension, it is equivalent to and snaps into polyester fiber, so that graphene and polyester fabric are firmly combined, if being baked without high temperature, Graphene oxide cannot be introduced into inside polyester fiber, when there is external force, be easy for being washed off.There are also be exactly the present invention In, graphene oxide in the dyeing course of high temperature and pressure can part carry out restore (hydrothermal reduction), do not need to fabric On graphene oxide carry out it is special reduction i.e. can reach antibacterial, antiultraviolet and Contact cool feeling performance, work can be saved Skill and energy consumption.
Compared with the existing technology, a kind of antibacterial fabric preparation method based on graphene of the present invention has following Advantage:
(1) simple process, it is easily operated, and yield is high, at low cost, fastness to washing is good.
(2) the graphene oxide antibacterial fabric prepared, according to standard GB/T 20944.3-2008 " GBT 20944.3- The evaluation third portion of 2008 antibacterial textile performances: succusion " test, to staphylococcus aureus, Escherichia coli and white Candida albicans has excellent antibacterial effect;According to GB/T18830-2009 " evaluation of ultraviolet resistance of fabric " standard into Row test, the UV protection factor of fabric are up to 2000 or more;According to GB/T 35263-2017, " textile Contact is cool The detection and evaluation of perceptual energy ", the Contact cool feeling coefficient of fabric is 0.15 or more.
(3) amount of this method fabric combination graphene is more, and combination fastness is stronger, and special-less process requirement, complete It can use dye-works's existing equipment entirely to be produced, be suitable for large-scale promotion.
(4) the graphene oxide antibacterial fabric prepared, can be applied to various underwears, bedding, hygienic material, shoes Socks, ornament materials, non-woven fabrics etc..
Detailed description of the invention
Fig. 1 is that the examining report of graphene oxide antibacterial fabric anti-microbial property prepared by embodiment 4 (aoxidizes when preparation Graphene concentration 0.25g/L);
Fig. 2 is the examining report of graphene oxide antibacterial fabric ultraviolet resistance prepared by embodiment 4 (when preparation Graphene oxide concentration 0.25g/L);
Fig. 3 is graphene oxide antibacterial fabric ultraviolet resistance and Contact cool feeling performance prepared by embodiment 1 Examining report (graphene oxide concentration 0.05g/L when preparation);
Fig. 4 is the examining report (system of graphene oxide antibacterial fabric Contact cool feeling performance prepared by embodiment 4 Graphene oxide concentration 0.25g/L when standby).
Specific embodiment
In addition to being defined, technical term used in following embodiment has general with those skilled in the art of the invention All over the identical meanings understood.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent;Institute Experimental method is stated, is conventional method unless otherwise specified.
Below with reference to examples and drawings, the present invention will be described in detail.
One, raw material sources and explanation
Graphene oxide employed in embodiment 1-5 and comparative example is the graphite oxide of the hexa-atomic element production in Changzhou Alkene, model 3522.
Polyester fabric employed in embodiment 1-5 and comparative example is 75D, 100%DTY of the knitting mill Cixi Xu Dong production Terylene, grammes per square metre 110.The molecular structural formula of terylene are as follows:
In treatment fluid employed in embodiment 1-5 other than sodium hydroxide and JFC, surplus is water.
Two, embodiment 1-5
Embodiment 1
A kind of antibacterial fabric preparation method based on graphene, including set gradually fabric pre-treatment, dye liquor preparation, High-temperature dyeing, drying bake four programs.Detailed process are as follows:
Fabric pre-treatment: contain the sodium hydroxide of 1wt%, the JFC of 0.1wt%, at bath raio 1:20 in treatment fluid Reason, processing routine are that polyester fabric is added in 35 DEG C for the treatment of fluid, are warming up to 85 DEG C, keep the temperature 1 hour, are impregnated with 60 DEG C of water It is 10 minutes, primary with 50 DEG C of washings, web surface, which is washed to, with 30 DEG C is in neutrality.
Dye liquor preparation: with water by graphene oxide pulp dilution, Acetate-acetate buffer solution and BB lotion (its are added In, the mass ratio of Ergol and castor oil polyoxyethylene ether is 1:4), it is sufficiently stirred and mixes to obtain graphene oxide content The dye liquor for being 0.30g/L for 0.05g/L, buffer content 0.20g/L, BB emulsion content, dye liquor pH are 3.8.
High-temperature dyeing: with the bath raio of 1:30, using the method for temperature programming, high-temperature dyeing is carried out to polyester fabric.Heating Program is -85 DEG C of room temperature, and 2 DEG C of heating rate is per minute;85 DEG C -110 DEG C, 1 DEG C of heating rate per minute, keeps the temperature 10 minutes; 110 DEG C -130 DEG C, 0.5 DEG C of heating rate per minute, keeps the temperature 30 minutes;130 DEG C -50 DEG C, 3 DEG C of rate of temperature fall is per minute.
Drying bakes: the temperature condition prior to 130 DEG C dries the polyester fabric after high-temperature dyeing, will dry later Polyester fabric after dry bakes 4 minutes in 189-191 DEG C, as based on the antibacterial fabric of graphene described in the present embodiment.
Embodiment 2
A kind of antibacterial fabric preparation method based on graphene, including set gradually fabric pre-treatment, dye liquor preparation, High-temperature dyeing, drying bake four programs.Detailed process are as follows:
Fabric pre-treatment: contain the sodium hydroxide of 2wt%, the JFC of 0.5wt%, at bath raio 1:20 in treatment fluid Reason, processing routine are that polyester fabric is added in 35 DEG C for the treatment of fluid, are warming up to 85 DEG C, keep the temperature 1 hour, are impregnated with 60 DEG C of water It is 10 minutes, primary with 50 DEG C of washings, web surface, which is washed to, with 30 DEG C is in neutrality.
Dye liquor preparation: addition Acetate-acetate buffer solution and BB lotion (wherein, Ergol and castor oil polyoxy second The mass ratio of alkene ether be 2:3), be sufficiently stirred mix graphene oxide content be 0.10g/L, buffer content is 0.30g/L, BB emulsion content are the dye liquor of 0.40g/L, and dye liquor pH is 4.2.
High-temperature dyeing: with the bath raio of 1:30, using the method for temperature programming, high-temperature dyeing is carried out to polyester fabric.Heating Program is -85 DEG C of room temperature, and 2 DEG C of heating rate is per minute;85 DEG C -110 DEG C, 1 DEG C of heating rate per minute, keeps the temperature 10 minutes; 110 DEG C -130 DEG C, 0.5 DEG C of heating rate per minute, keeps the temperature 30 minutes;130 DEG C -50 DEG C, 3 DEG C of rate of temperature fall is per minute.
Drying bakes: the temperature condition prior to 115 DEG C dries the polyester fabric after high-temperature dyeing, will dry later Polyester fabric after dry bakes 5 minutes in 185-187 DEG C, as based on the antibacterial fabric of graphene described in the present embodiment.
Embodiment 3
A kind of antibacterial fabric preparation method based on graphene, including set gradually fabric pre-treatment, dye liquor preparation, High-temperature dyeing, drying bake four programs.Detailed process are as follows:
Fabric pre-treatment: contain the sodium hydroxide of 1wt%, the JFC of 3wt%, at bath raio 1:20 in treatment fluid Reason, processing routine are that polyester fabric is added in 35 DEG C for the treatment of fluid, are warming up to 85 DEG C, keep the temperature 1 hour, are impregnated with 60 DEG C of water It is 10 minutes, primary with 50 DEG C of washings, web surface, which is washed to, with 30 DEG C is in neutrality.
Dye liquor preparation: with water by graphene oxide pulp dilution, Acetate-acetate buffer solution and BB lotion (its are added In, the mass ratio of Ergol and castor oil polyoxyethylene ether is 4:1), it is sufficiently stirred and mixes to obtain graphene oxide content The dye liquor for being 0.50g/L for 0.15g/L, buffer content 0.40g/L, BB emulsion content, dye liquor pH are 4.7.
High-temperature dyeing: with the bath raio of 1:20, using the method for temperature programming, high-temperature dyeing is carried out to polyester fabric.Heating Program is -85 DEG C of room temperature, and 2 DEG C of heating rate is per minute;85 DEG C -110 DEG C, 1 DEG C of heating rate per minute, keeps the temperature 10 minutes; 110 DEG C -130 DEG C, 0.5 DEG C of heating rate per minute, keeps the temperature 30 minutes;130 DEG C -50 DEG C, 3 DEG C of rate of temperature fall is per minute.
Drying bakes: the temperature condition prior to 130 DEG C dries the polyester fabric after high-temperature dyeing, will dry later Polyester fabric after dry bakes 4 minutes in 189-191 DEG C, as based on the antibacterial fabric of graphene described in the present embodiment.
Embodiment 4
A kind of antibacterial fabric preparation method based on graphene, including set gradually fabric pre-treatment, dye liquor preparation, High-temperature dyeing, drying bake four programs.Detailed process are as follows:
Fabric pre-treatment: contain the sodium hydroxide of 5wt%, the JFC of 0.1wt%, at bath raio 1:20 in treatment fluid Reason, processing routine are that polyester fabric is added in 35 DEG C for the treatment of fluid, are warming up to 85 DEG C, keep the temperature 1 hour, are impregnated with 60 DEG C of water It is 10 minutes, primary with 50 DEG C of washings, web surface, which is washed to, with 30 DEG C is in neutrality.
Dye liquor preparation: with water by graphene oxide pulp dilution, Acetate-acetate buffer solution and BB lotion (its are added In, the mass ratio of Ergol and castor oil polyoxyethylene ether is 1:1), it is sufficiently stirred and mixes to obtain graphene oxide content The dye liquor pH for being 0.30g/L for 0.25g/L, buffer content 0.20g/L, BB emulsion content is 4.0.
High-temperature dyeing: with the bath raio of 1:20, using the method for temperature programming, high-temperature dyeing is carried out to polyester fabric.Heating Program is -85 DEG C of room temperature, and 2 DEG C of heating rate is per minute;85 DEG C -110 DEG C, 1 DEG C of heating rate per minute, keeps the temperature 10 minutes; 110 DEG C -130 DEG C, 0.5 DEG C of heating rate per minute, keeps the temperature 30 minutes;130 DEG C -50 DEG C, 3 DEG C of rate of temperature fall is per minute.
Drying bakes: the temperature condition prior to 130 DEG C dries the polyester fabric after high-temperature dyeing, will dry later Polyester fabric after dry bakes 4 minutes in 194-195 DEG C, as based on the antibacterial fabric of graphene described in the present embodiment.
Embodiment 5
A kind of antibacterial fabric preparation method based on graphene, including set gradually fabric pre-treatment, dye liquor preparation, High-temperature dyeing, drying bake four programs.Detailed process are as follows:
Fabric pre-treatment: contain the sodium hydroxide of 3wt%, the JFC of 1wt%, at bath raio 1:20 in treatment fluid Reason, processing routine are that polyester fabric is added in 35 DEG C for the treatment of fluid, are warming up to 85 DEG C, keep the temperature 1 hour, are impregnated with 60 DEG C of water It is 10 minutes, primary with 50 DEG C of washings, web surface, which is washed to, with 30 DEG C is in neutrality.
Dye liquor preparation: with water by graphene oxide pulp dilution, Acetate-acetate buffer solution and BB lotion (its are added In, the mass ratio of Ergol and castor oil polyoxyethylene ether is 3:2), it is sufficiently stirred and mixes to obtain graphene oxide content The dye liquor for being 0.20g/L for 0.50g/L, buffer content 0.50g/L, BB emulsion content, dye liquor pH are 4.5.
High-temperature dyeing: with the bath raio of 1:10, using the method for temperature programming, high-temperature dyeing is carried out to polyester fabric.Heating Program is -85 DEG C of room temperature, and 2 DEG C of heating rate is per minute;85 DEG C -110 DEG C, 1 DEG C of heating rate per minute, keeps the temperature 8 minutes;110 DEG C -130 DEG C, 0.5 DEG C of heating rate per minute, keeps the temperature 32 minutes;130 DEG C -50 DEG C, 3 DEG C of rate of temperature fall is per minute.
Drying bakes: the temperature condition prior to 140 DEG C dries the polyester fabric after high-temperature dyeing, will dry later Polyester fabric after dry bakes 3 minutes in 189-191 DEG C, as based on the antibacterial fabric of graphene described in the present embodiment.
Comparative example
A kind of preparation method of Graphene antibiosis fabric, it is substantially same as Example 2, the difference is that: it is dried in drying After roasting step, also need to carry out antibacterial fabric special reduction treatment, reduction treatment is with sodium hydrosulfite 5g/L, hydrogen specifically Polyester fabric after the solution of sodium oxide molybdena 1.2g/L bakes drying restores under conditions of 85 DEG C of temperature, the recovery time 30 minutes.
Three, the performance test of embodiment 1-5 and comparative example
1, antibacterial effect
Graphene antibiosis fabric prepared by embodiment 1-5 is according to GB/T 20944.3-2008 " GBT 20944.3-2008 The evaluation third portion of antibacterial textile performance: succusion " standard testing, to staphylococcus aureus, Escherichia coli and white Candida albicans has excellent antibacterial effect;Bacteriostasis rate is stepped up with the raising of GO content in dye liquor, is up to greater than 99%;The anti-microbial property examining report (the outer detection of committee) of embodiment 4 is shown in Fig. 1.The antibiotic rate of embodiment 1,2,4 and comparative example is real It tests room detection data and is shown in Table 1.
The polyester fabric bacteriostasis rate of 1 laboratory test various concentration graphene oxide bath foam of table preparation
Sample ID 3# (embodiment 4) 8# (embodiment 2) 11# (embodiment 1) B# (comparative example)
Bacteriostasis rate 95.5% 88.8% 52.0% 86.6%
Remarks: it is 0.25g/L that graphene oxide dispersion concentration is used when in table prepared by sample 3#;
The graphene oxide dispersion concentration that sample 8# is used when preparing is 0.1g/L;
The graphene oxide dispersion concentration that sample 11# is used when preparing is 0.05g/L;
It is 0.10g/L that graphene oxide dispersion concentration is used when prepared by sample B#, by the functional surfaces of reduction after preparation Material.
As it can be seen from table 1 with the increase for preparing GO concentration in Graphene antibiosis fabric dye liquor, the antibiotic property of fabric It can be promoted, and can be seen that whether reduction treatment is carried out to fabric after drying bakes from embodiment 2 and comparative example, to fabric Anti-microbial property influence less, and for embodiment 2 and comparative example, embodiment 2 without reduction treatment fabric it is anti- Bacterium rate will also rate be higher than comparative example.
2, ultraviolet resistance
Graphene antibiosis fabric prepared by embodiment 1-5 is according to GB/T18830-2009 " ultraviolet resistance of fabric Evaluation " standard carries out ultraviolet resistance test, the UV protection factor of fabric is greater than 2000.The UV resistance of embodiment 1 Performance detection report is shown in that Fig. 3, the uv resistance energy examining report of embodiment 4 are shown in Fig. 2.Can be seen that according to fig. 2 with Fig. 3 with The increase of GO concentration in Graphene antibiosis fabric dye liquor is prepared, the ultraviolet resistance of fabric is promoted.
3, moment cool feeling performance
" textile Contact is cool according to GB/T 35263-2017 for Graphene antibiosis fabric prepared by embodiment 1 and 4 It is perceptual can detection and evaluation " standard carries out the detection (examining report of embodiment 1 and embodiment 4 of Contact cool feeling performance Fig. 3 and Fig. 4 are seen respectively), the Contact cool feeling coefficient of fabric is respectively 0.18 and 0.17, is above technical requirements.As it can be seen that There is cool feeling by the polyester fabric that the antibacterial fabric preparation method of the present invention based on graphene arranges, the summer can be improved Season comforts of use.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of antibacterial fabric preparation method based on graphene, it is characterised in that: the following steps are included:
(1) fabric pre-treatment: fabric is impregnated using the treatment fluid containing lye and bleeding agent, then is washed till fabric with water It is neutral;
(2) prepared by dye liquor: graphene oxide slurry is diluted with water, buffer solution and BB lotion is then added, mixes to obtain dye liquor;BB Lotion is the mixed emulsion of Ergol and castor oil polyoxyethylene ether;
(3) with certain bath raio, using the method for temperature programming, high-temperature dyeing high-temperature dyeing: is carried out to fabric;Wherein, program The process of heating are as follows: -85 DEG C of room temperature, 2 DEG C of heating rate is per minute;85 DEG C -110 DEG C, 1 DEG C of heating rate per minute, keeps the temperature 6- 14 minutes;110 DEG C -130 DEG C, 0.5 DEG C of heating rate per minute, keeps the temperature 25-35 minutes;130 DEG C -50 DEG C, 3 DEG C of rate of temperature fall every Minute;
(4) drying bakes: the temperature condition prior to 110-150 DEG C dries the fabric after high-temperature dyeing, later will drying Fabric afterwards in 180-200 DEG C baking 1-5 minutes, as based on the antibacterial fabric of graphene.
2. the antibacterial fabric preparation method according to claim 1 based on graphene, it is characterised in that: in step (1), institute The treatment fluid stated includes each component of following mass fraction: the sodium hydroxide of 1-5wt%, the bleeding agent of 0.1-3wt%, surplus are Water.
3. the antibacterial fabric preparation method according to claim 1 or 2 based on graphene, it is characterised in that: step (1) In, the method for fabric pre-treatment the following steps are included: treatment fluid is first heated to 35 DEG C after be put into fabric;Then it is warming up to 85 DEG C, keep the temperature 1 hour;It is impregnated 10 minutes with 60 DEG C of water again;It is primary with 50 DEG C of washings again;Finally being washed to web surface with 30 DEG C is in It is neutral.
4. the antibacterial fabric preparation method according to claim 3 based on graphene, it is characterised in that: in step (1), face The bath raio of material and treatment fluid is 1:20.
5. the antibacterial fabric preparation method according to claim 1 or 2 based on graphene, it is characterised in that: step (1) In, the mixture of one or more of bleeding agent JFC, JFC-1, JFC-2, JFC-E;In step (2), resulting dye In liquid, graphene oxide content is 0.05-0.5g/L, and buffer content 0.10-0.50g/L, BB emulsion content is 0.1- 1.0g/L。
6. the antibacterial fabric preparation method according to claim 1 based on graphene, it is characterised in that: in step (2), institute The graphene oxide solid content in graphene oxide slurry stated is 1.0-3.4wt%, and the oxygen content of surface of graphene oxide For 40-50wt%.
7. the antibacterial fabric preparation method according to claim 1 based on graphene, it is characterised in that: in step (2), institute The buffer stated is acetic acid salt system buffer, and dye liquor pH value is controlled in 3-5.
8. the antibacterial fabric preparation method according to claim 1 based on graphene, it is characterised in that: the BB lotion In, the mass ratio of Ergol and castor oil polyoxyethylene ether is 1:4-4:1.
9. the antibacterial fabric preparation method according to claim 1 based on graphene, it is characterised in that: in step (3), 85 DEG C -110 DEG C, 1 DEG C of heating rate per minute, keeps the temperature 10 minutes;110 DEG C -130 DEG C, 0.5 DEG C of heating rate per minute, keeps the temperature 30 Minute;Bath raio is 1:5-1:30.
10. the antibacterial fabric preparation method according to claim 1 based on graphene, it is characterised in that: the fabric is Polyester fabric;In step (4), the temperature condition prior to 130 DEG C dries the fabric after high-temperature dyeing, after drying later Fabric in 180-200 DEG C baking 1-5 minutes, as based on the antibacterial fabric of graphene.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111206418A (en) * 2020-03-21 2020-05-29 深圳市寒暑科技新能源有限公司 Antibacterial yarn and preparation method thereof
CN112796100A (en) * 2021-02-03 2021-05-14 青岛烯泰科技有限公司 Finished garment fabric graphene adding preparation method

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CN106811967A (en) * 2016-04-01 2017-06-09 青岛大学 A kind of preparation method of graphene oxide antimicrobial coating fabric
CN107724132A (en) * 2017-11-16 2018-02-23 河南工程学院 A kind of dacron is antistatic and a step processing method is bathed in dyeing one
CN108589346A (en) * 2018-07-30 2018-09-28 嘉兴学院 A kind of method that graphene is used for the arrangement of terylene product

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CN106811967A (en) * 2016-04-01 2017-06-09 青岛大学 A kind of preparation method of graphene oxide antimicrobial coating fabric
CN107724132A (en) * 2017-11-16 2018-02-23 河南工程学院 A kind of dacron is antistatic and a step processing method is bathed in dyeing one
CN108589346A (en) * 2018-07-30 2018-09-28 嘉兴学院 A kind of method that graphene is used for the arrangement of terylene product

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111206418A (en) * 2020-03-21 2020-05-29 深圳市寒暑科技新能源有限公司 Antibacterial yarn and preparation method thereof
CN112796100A (en) * 2021-02-03 2021-05-14 青岛烯泰科技有限公司 Finished garment fabric graphene adding preparation method

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