CN109653005B - Preparation method of antibacterial fabric based on graphene - Google Patents

Preparation method of antibacterial fabric based on graphene Download PDF

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CN109653005B
CN109653005B CN201811602932.8A CN201811602932A CN109653005B CN 109653005 B CN109653005 B CN 109653005B CN 201811602932 A CN201811602932 A CN 201811602932A CN 109653005 B CN109653005 B CN 109653005B
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fabric
temperature
graphene
antibacterial
emulsion
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CN109653005A (en
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易汉平
韩建坊
刘宏伟
高古辉
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Tianjin North Graphene Industry Research Institute
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Tianjin North Graphene Industry 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
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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

Abstract

The invention provides a preparation method of an antibacterial fabric based on graphene, which comprises the following steps: (1) pretreatment of the fabric: soaking the fabric by using a treatment solution containing an alkali solution and a penetrating agent, and washing the fabric to be neutral by using water; (2) preparing a dye solution: diluting the graphene oxide slurry with water, then adding a buffer solution and a BB emulsion, and uniformly mixing to obtain a dye solution; the BB emulsion is a mixed emulsion of benzyl benzoate and castor oil polyoxyethylene ether; (3) high-temperature dyeing: dyeing the fabric at high temperature by adopting a programmed heating method according to a certain bath ratio; (4) drying and baking: drying the fabric dyed at the high temperature under the temperature conditions of 110-. The preparation method of the graphene-based antibacterial fabric is simple in process and easy to operate, and the prepared textile fabric has excellent antibacterial and ultraviolet-proof functions and instant cool feeling performance in contact.

Description

Preparation method of antibacterial fabric based on graphene
Technical Field
The invention belongs to the technical field of textile manufacturing, relates to a textile fabric processing technology with a protection function, and particularly relates to a preparation method of an antibacterial fabric based on graphene.
Background
With the increasing demand of people on environmental sanitation, the application of antibacterial materials is concerned more widely. Bacteria can rapidly grow and reproduce under proper environmental conditions, and diseases are transmitted through contact with human bodies, so that the health of people is influenced. The textile fabric composed of the fibers is favorable for the attachment of microorganisms due to the porous object shape and the chemical structure of the high molecular polymer, and becomes a good parasite for the survival and propagation of the microorganisms such as bacteria, fungi and the like. Textiles that come into contact with people in daily life are the place where these microorganisms live well and are also important sources of transmission of various diseases, so the development of textiles with antibacterial properties is of great importance.
At present, most of textiles with antibacterial function are subjected to after-treatment by using an antibacterial finishing agent to obtain the textiles with antibacterial property. Common antibacterial finishing agents are classified into three major classes, namely inorganic antibacterial finishing agents, organic antibacterial finishing agents and natural biological antibacterial finishing agents. The inorganic antibacterial agent mainly comprises an inorganic metal antibacterial agent, a photocatalytic antibacterial agent and a nano-particle antibacterial agent; the organic antibacterial agent is a compound which bonds molecules with antibacterial activity with a carrier through covalent bonds, and mainly comprises a quaternary ammonium salt antibacterial agent, a quaternary phosphonium salt antibacterial agent, an alcohol antibacterial agent, a phenol antibacterial agent and the like; the natural biological antibacterial agent is an antibacterial agent composed of organic high molecular substances extracted from natural organisms and having antibacterial function, and commonly used chitosan, garlicin and the like.
Graphene Oxide (GO) is an important derivative in graphene family, has basically the same structure as graphene, and only has a large number of oxygen-containing functional groups such as hydroxyl, carboxyl, epoxy and the like on the surface, and the functional groups endow the graphene oxide with a plurality of unique properties such as good wetting property and surface activity, compatibility with some polymers and the like, so that the graphene oxide can endow materials with more chemical reaction performance, and can also form a network structure by crosslinking to improve the interaction force between single sheets, thereby improving the physical properties of the materials. With the development of GO functionalization methods, oxygen-containing groups with different functions offer more potential advantages to GO, and the application of GO in the aspect of antibiosis is also increased.
At present, two preparation methods of the graphene-based antibacterial polyester fabric are mainly used, one is to add graphene in the stage of preparing polyester chips to prepare graphene polyester yarns, and the other is to combine graphene on the fabric by finishing through a padding method. The addition of graphene at the slicing stage easily causes the agglomeration of graphene, the process is complex, and the dispersion uniformity of the graphene cannot be guaranteed. In the post-finishing stage, finishing is performed through a padding method, an organic cross-linking agent needs to be added, the amount of graphene combined on the fabric is small, and the binding force is weak; according to the high-temperature high-pressure dyeing method, under the condition that high-temperature baking is not carried out, the binding force between graphene and the fabric is weak, and the washing fastness cannot meet the requirement.
Disclosure of Invention
In view of the above, the invention aims to provide a preparation method of an antibacterial fabric based on graphene, so as to overcome the defects of the prior art, the preparation method is simple in process, easy to operate and suitable for mass production in factories, and the prepared textile fabric has excellent antibacterial and ultraviolet-proof functions and contact instant cool feeling performance and can be applied to the fields of underwear, bedding, sanitary materials, shoes and socks, decorative materials, non-woven fabrics and the like.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of an antibacterial fabric based on graphene comprises the following steps:
(1) pretreatment of the fabric: soaking the fabric by using a treatment solution containing an alkali solution and a penetrating agent, and washing the fabric to be neutral by using water;
(2) preparing a dye solution: diluting the graphene oxide slurry with water, then adding a buffer solution and a BB emulsion, and uniformly mixing to obtain a dye solution; the BB emulsion is a mixed emulsion of benzyl benzoate and castor oil polyoxyethylene ether;
(3) high-temperature dyeing: dyeing the fabric at high temperature by adopting a programmed heating method according to a certain bath ratio; wherein, the procedure of temperature programming is as follows: normal temperature-85 deg.c, heating rate of 2 deg.c per minute; the temperature is 85-110 ℃, the heating rate is 1 ℃ per minute, and the temperature is kept for 6-14 minutes; 110-130 ℃, the heating rate is 0.5 ℃ per minute, and the temperature is kept for 25-35 minutes; at a temperature of between 130 and 50 ℃ and a cooling rate of 3 ℃ per minute;
(4) drying and baking: drying the fabric dyed at the high temperature under the temperature conditions of 110-.
Preferably, in the step (1), the treatment liquid comprises the following components in percentage by mass: 1-5 wt% of sodium hydroxide, 0.1-3 wt% of penetrating agent and the balance of water. The use of sodium hydroxide can be greatly reduced by adding the penetrant.
Preferably, in the step (1), the method for pre-treating the fabric comprises the following steps: firstly, heating the treating fluid to 35 ℃ and then putting the treating fluid into the fabric; then heating to 85 ℃, and preserving heat for 1 hour; soaking in 60 deg.C water for 10 min; washing with 50 deg.C water; finally, washing the fabric with water at 30 ℃ until the surface of the fabric is neutral.
Preferably, in the step (1), the bath ratio of the fabric to the treatment liquid is 1: 20.
Preferably, in the step (1), the penetrating agent is one or a mixture of more than two of JFC, JFC-1, JFC-2 and JFC-E; in the step (2), the content of graphene oxide in the obtained dye solution is 0.05-0.5g/L, the content of the buffer solution is 0.10-0.50g/L, and the content of BB emulsion is 0.1-1.0 g/L.
Preferably, in the step (2), the solid content of graphene oxide in the graphene oxide slurry is 1.0-3.4 wt%, and the oxygen content on the surface of graphene oxide is 40-50 wt%.
Preferably, in the step (2), the buffer solution is an acetate system buffer solution, and the pH value of the dye solution is controlled to be 3-5.
Preferably, in the BB emulsion, the mass ratio of the benzyl benzoate to the castor oil polyoxyethylene ether is 1:4-4: 1.
Preferably, in the step (3), the temperature is 85-110 ℃, the heating rate is 1 ℃ per minute, and the temperature is kept for 10 minutes; 110-130 ℃, the heating rate is 0.5 ℃ per minute, and the temperature is kept for 30 minutes; the bath ratio is 1: 5-1: 30.
preferably, the fabric is a polyester fabric; in the step (4), the fabric dyed at the high temperature is dried at the temperature of 130 ℃, and then the dried fabric is baked at the temperature of 180 ℃ and 200 ℃ for 1-5 minutes, so that the graphene-based antibacterial fabric is obtained.
The method comprises the steps of heating the polyester fabric, heating the polyester fabric by using a heating device, and heating the solution by using a heating device. In addition, dacron surface fabric (also be the polyester surface fabric) when 180 supplyes 200 ℃, the lattice motion of dacron fiber can strengthen, makes the graphene oxide molecule enter into dacron fiber, in being equivalent to the card to dacron fiber, makes graphite alkene and dacron surface fabric firmly combine like this, if do not carry out high temperature and bake, inside the graphene oxide can't enter into the dacron fiber, when the exogenic action, just easily washed away. In addition, in the invention, the graphene oxide can be partially reduced (hydrothermal reduction) in the dyeing process at high temperature and high pressure, and the performances of antibiosis, ultraviolet resistance and instant cool feeling in contact can be achieved without special reduction of the graphene oxide on the fabric, so that the process and the energy consumption can be saved.
Compared with the prior art, the preparation method of the graphene-based antibacterial fabric has the following advantages:
(1) simple process, easy operation, high yield, low cost and good washing fastness.
(2) The prepared graphene oxide antibacterial fabric is evaluated according to the part 3 of the standard GB/T20944.3-2008 GBT20944.3-2008 textile antibacterial performance: the oscillation method tests that the antibacterial agent has excellent antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans; the fabric is tested according to the GB/T18830-2009 evaluation on ultraviolet resistance of textiles, and the ultraviolet protection coefficient of the fabric is up to more than 2000; according to GB/T35263 and 2017 detection and evaluation of the cool feeling performance of the textile at the moment of contact, the cool feeling coefficient of the textile at the moment of contact is more than 0.15.
(3) The method has the advantages of more amount of the combined graphene, stronger combination firmness, no special process requirement, capability of completely utilizing the existing equipment of a dye factory for production, and suitability for large-scale popularization.
(4) The prepared graphene oxide antibacterial fabric can be applied to various aspects such as underwear, bedding, sanitary materials, shoes and socks, decorative materials, non-woven fabrics and the like.
Drawings
Fig. 1 is a detection report of the antibacterial performance of the graphene oxide antibacterial fabric prepared in example 4 (the concentration of graphene oxide is 0.25g/L during preparation);
fig. 2 is a detection report of ultraviolet resistance performance of the graphene oxide antibacterial fabric prepared in example 4 (graphene oxide concentration is 0.25g/L during preparation);
FIG. 3 is a detection report of ultraviolet protection performance and instantaneous contact cooling performance of the graphene oxide antibacterial fabric prepared in example 1 (the concentration of graphene oxide is 0.05g/L during preparation);
fig. 4 is a report of detection of cooling performance of the graphene oxide antibacterial fabric prepared in example 4 at the moment of contact (graphene oxide concentration is 0.25g/L during preparation).
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to the following examples and accompanying drawings.
Raw material sources and descriptions
The graphene oxides used in examples 1-5 and the comparative example were all graphene oxide produced by Hexagon, model 3522.
The polyester fabrics used in examples 1-5 and comparative examples were 75D, 100% DTY polyester produced by Cixi Xudong knitting plant with a grammage of 110. The molecular structural formula of terylene is:
Figure GDA0001969551420000061
the treatment solutions used in examples 1 to 5 were water except for sodium hydroxide and JFC.
Second, examples 1 to 5
Example 1
A preparation method of an antibacterial fabric based on graphene comprises four procedures of fabric pretreatment, dye liquor preparation, high-temperature dyeing and drying and baking which are sequentially arranged. The specific process is as follows:
pretreatment of the fabric: the treating solution contains 1wt% of sodium hydroxide and 0.1wt% of JFC, and is treated in a bath ratio of 1:20, wherein the treating procedure comprises the steps of adding polyester fabric into the treating solution at 35 ℃, heating to 85 ℃, keeping the temperature for 1 hour, soaking in water at 60 ℃ for 10 minutes, washing once at 50 ℃, and washing with water at 30 ℃ until the surface of the fabric is neutral.
Preparing a dye solution: diluting the graphene oxide slurry with water, adding a sodium acetate-acetic acid buffer solution and a BB emulsion (wherein the mass ratio of benzyl benzoate to castor oil polyoxyethylene ether is 1:4), fully stirring and uniformly mixing to obtain a dye liquor with the graphene oxide content of 0.05g/L and the buffer solution content of 0.20g/L, BB and the emulsion content of 0.30g/L, wherein the pH value of the dye liquor is 3.8.
High-temperature dyeing: and (3) dyeing the polyester fabric at high temperature by adopting a temperature programming method according to a bath ratio of 1: 30. The temperature rise program is normal temperature-85 ℃, and the temperature rise rate is 2 ℃ per minute; the temperature is 85-110 ℃, the heating rate is 1 ℃ per minute, and the temperature is kept for 10 minutes; 110-130 ℃, the heating rate is 0.5 ℃ per minute, and the temperature is kept for 30 minutes; 130-50 ℃ and the cooling rate is 3 ℃ per minute.
Drying and baking: firstly, drying the polyester fabric dyed at the high temperature at the temperature of 130 ℃, and then, baking the dried polyester fabric at 189-.
Example 2
A preparation method of an antibacterial fabric based on graphene comprises four procedures of fabric pretreatment, dye liquor preparation, high-temperature dyeing and drying and baking which are sequentially arranged. The specific process is as follows:
pretreatment of the fabric: the treatment solution contains 2 wt% of sodium hydroxide and 0.5 wt% of JFC, and is treated by a bath ratio of 1:20, wherein the treatment procedure comprises the steps of adding polyester fabric into the treatment solution at 35 ℃, heating to 85 ℃, keeping the temperature for 1 hour, soaking in water at 60 ℃ for 10 minutes, washing once at 50 ℃, and washing with water at 30 ℃ until the surface of the fabric is neutral.
Preparing a dye solution: adding sodium acetate-acetic acid buffer solution and BB emulsion (wherein the mass ratio of the benzyl benzoate to the castor oil polyoxyethylene ether is 2:3), fully stirring and uniformly mixing to obtain dye liquor with the graphene oxide content of 0.10g/L and the buffer solution content of 0.30g/L, BB and the emulsion content of 0.40g/L, wherein the pH value of the dye liquor is 4.2.
High-temperature dyeing: and (3) dyeing the polyester fabric at high temperature by adopting a temperature programming method according to a bath ratio of 1: 30. The temperature rise program is normal temperature-85 ℃, and the temperature rise rate is 2 ℃ per minute; the temperature is 85-110 ℃, the heating rate is 1 ℃ per minute, and the temperature is kept for 10 minutes; 110-130 ℃, the heating rate is 0.5 ℃ per minute, and the temperature is kept for 30 minutes; 130-50 ℃ and the cooling rate is 3 ℃ per minute.
Drying and baking: the polyester fabric dyed at the high temperature is dried at a temperature of 115 ℃, and then the dried polyester fabric is baked at 185-187 ℃ for 5 minutes, so that the graphene-based antibacterial fabric is obtained in the embodiment.
Example 3
A preparation method of an antibacterial fabric based on graphene comprises four procedures of fabric pretreatment, dye liquor preparation, high-temperature dyeing and drying and baking which are sequentially arranged. The specific process is as follows:
pretreatment of the fabric: the treatment solution contains 1wt% of sodium hydroxide and 3 wt% of JFC, and is treated according to a bath ratio of 1:20, the treatment procedure is that polyester fabric is added into the treatment solution at 35 ℃, the temperature is raised to 85 ℃, the heat preservation is carried out for 1 hour, the polyester fabric is soaked in water at 60 ℃ for 10 minutes, the polyester fabric is washed once at 50 ℃, and the polyester fabric is washed with water at 30 ℃ until the surface of the polyester fabric is neutral.
Preparing a dye solution: diluting the graphene oxide slurry with water, adding a sodium acetate-acetic acid buffer solution and BB emulsion (wherein the mass ratio of benzyl benzoate to castor oil polyoxyethylene ether is 4:1), fully stirring and uniformly mixing to obtain a dye liquor with the graphene oxide content of 0.15g/L and the buffer solution content of 0.40g/L, BB and the emulsion content of 0.50g/L, wherein the pH value of the dye liquor is 4.7.
High-temperature dyeing: and (3) dyeing the polyester fabric at high temperature by adopting a programmed heating method at a bath ratio of 1: 20. The temperature rise program is normal temperature-85 ℃, and the temperature rise rate is 2 ℃ per minute; the temperature is 85-110 ℃, the heating rate is 1 ℃ per minute, and the temperature is kept for 10 minutes; 110-130 ℃, the heating rate is 0.5 ℃ per minute, and the temperature is kept for 30 minutes; 130-50 ℃ and the cooling rate is 3 ℃ per minute.
Drying and baking: firstly, drying the polyester fabric dyed at the high temperature at the temperature of 130 ℃, and then, baking the dried polyester fabric at 189-.
Example 4
A preparation method of an antibacterial fabric based on graphene comprises four procedures of fabric pretreatment, dye liquor preparation, high-temperature dyeing and drying and baking which are sequentially arranged. The specific process is as follows:
pretreatment of the fabric: the treatment solution contains 5wt% of sodium hydroxide and 0.1wt% of JFC, and is treated by a bath ratio of 1:20, wherein the treatment procedure comprises the steps of adding polyester fabric into the treatment solution at 35 ℃, heating to 85 ℃, keeping the temperature for 1 hour, soaking in water at 60 ℃ for 10 minutes, washing once at 50 ℃, and washing with water at 30 ℃ until the surface of the fabric is neutral.
Preparing a dye solution: diluting the graphene oxide slurry with water, adding a sodium acetate-acetic acid buffer solution and a BB emulsion (wherein the mass ratio of benzyl benzoate to castor oil polyoxyethylene ether is 1:1), and fully and uniformly stirring to obtain a dye solution with the graphene oxide content of 0.25g/L and the buffer solution content of 0.20g/L, BB and the emulsion content of 0.30g/L, wherein the pH value of the dye solution is 4.0.
High-temperature dyeing: and (3) dyeing the polyester fabric at high temperature by adopting a programmed heating method at a bath ratio of 1: 20. The temperature rise program is normal temperature-85 ℃, and the temperature rise rate is 2 ℃ per minute; the temperature is 85-110 ℃, the heating rate is 1 ℃ per minute, and the temperature is kept for 10 minutes; 110-130 ℃, the heating rate is 0.5 ℃ per minute, and the temperature is kept for 30 minutes; 130-50 ℃ and the cooling rate is 3 ℃ per minute.
Drying and baking: firstly, drying the polyester fabric dyed at the high temperature at the temperature of 130 ℃, and then, baking the dried polyester fabric at 194-195 ℃ for 4 minutes, thereby obtaining the graphene-based antibacterial fabric of the embodiment.
Example 5
A preparation method of an antibacterial fabric based on graphene comprises four procedures of fabric pretreatment, dye liquor preparation, high-temperature dyeing and drying and baking which are sequentially arranged. The specific process is as follows:
pretreatment of the fabric: the treatment solution contains 3 wt% of sodium hydroxide and 1wt% of JFC, and is treated according to a bath ratio of 1:20, the treatment procedure is that polyester fabric is added into the treatment solution at 35 ℃, the temperature is raised to 85 ℃, the heat preservation is carried out for 1 hour, the polyester fabric is soaked in water at 60 ℃ for 10 minutes, the polyester fabric is washed once at 50 ℃, and the polyester fabric is washed with water at 30 ℃ until the surface of the polyester fabric is neutral.
Preparing a dye solution: diluting the graphene oxide slurry with water, adding a sodium acetate-acetic acid buffer solution and BB emulsion (wherein the mass ratio of benzyl benzoate to castor oil polyoxyethylene ether is 3:2), fully stirring and uniformly mixing to obtain a dye liquor with the graphene oxide content of 0.50g/L and the buffer solution content of 0.50g/L, BB and the emulsion content of 0.20g/L, wherein the pH value of the dye liquor is 4.5.
High-temperature dyeing: and (3) dyeing the polyester fabric at high temperature by adopting a temperature programming method according to a bath ratio of 1: 10. The temperature rise program is normal temperature-85 ℃, and the temperature rise rate is 2 ℃ per minute; the temperature is 85-110 ℃, the heating rate is 1 ℃ per minute, and the temperature is kept for 8 minutes; 110-130 ℃, the heating rate is 0.5 ℃ per minute, and the temperature is kept for 32 minutes; 130-50 ℃ and the cooling rate is 3 ℃ per minute.
Drying and baking: the polyester fabric dyed at a high temperature is dried at a temperature of 140 ℃, and then the dried polyester fabric is baked at 189-.
Comparative example
A preparation method of a graphene antibacterial fabric, which is basically the same as that in example 2, except that: after the drying and baking step, special reduction treatment needs to be carried out on the antibacterial fabric, specifically, the polyester fabric after drying and baking is reduced by using a solution of 5g/L sodium hydrosulfite and 1.2g/L sodium hydroxide at the temperature of 85 ℃ for 30 minutes.
Performance test of three, examples 1-5 and comparative example
1. Antibacterial effect
The graphene antibacterial fabric prepared in examples 1 to 5 is evaluated according to the evaluation part 3 of GB/T20944.3-2008 GBT20944.3-2008 textile antibacterial performance: the standard test of the oscillatory method shows that the antibacterial agent has excellent antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans; the bacteriostasis rate gradually increases along with the increase of the GO content in the dye liquor, and the highest bacteriostasis rate is more than 99 percent; the antimicrobial performance test report (ex-commission test) of example 4 is shown in fig. 1. The laboratory test data for the antibacterial ratio of examples 1, 2, 4 and comparative example are shown in table 1.
Table 1 laboratory test of bacteriostasis rate of polyester fabric prepared from graphene oxide bath solution with different concentrations
Sample name 3# (embodiment 4) 8# (embodiment 2) 11# (embodiment 1) B # (comparative example)
Rate of inhibition of bacteria 95.5% 88.8% 52.0% 86.6%
Remarking: in the table, the concentration of the graphene oxide dispersion used in the preparation of sample No. 3 is 0.25 g/L;
the concentration of the graphene oxide dispersion used in the preparation of sample No. 8 was 0.1 g/L;
the concentration of the graphene oxide dispersion used in the preparation of sample No. 11 was 0.05 g/L;
the graphene oxide dispersion solution with the concentration of 0.10g/L is used for preparing the sample B #, and the prepared functional fabric is reduced.
From table 1, it can be seen that the antibacterial performance of the fabric is improved with the increase of GO concentration in the dye liquor for preparing the graphene antibacterial fabric, and from example 2 and the comparative example, it can be seen that whether the fabric is subjected to reduction treatment after drying and baking has little influence on the antibacterial performance of the fabric, and in terms of example 2 and the comparative example, the antibacterial rate of the fabric which is not subjected to reduction treatment in example 2 is higher than that of the comparative example.
2. Ultraviolet ray resistance
The graphene antibacterial fabric prepared in the embodiments 1-5 is subjected to ultraviolet resistance performance test according to the GB/T18830-2009 evaluation on ultraviolet resistance performance of textiles, and the ultraviolet protection coefficient of the fabric is larger than 2000. The report of the test of the ultraviolet resistance of the example 1 is shown in fig. 3, and the report of the test of the ultraviolet resistance of the example 4 is shown in fig. 2. According to the graph 2 and the graph 3, the ultraviolet resistance of the fabric is improved along with the increase of the GO concentration in the dye liquor for preparing the graphene antibacterial fabric.
3. Instant cool feeling performance
The graphene antibacterial fabrics prepared in the embodiments 1 and 4 are subjected to detection of the contact instant cooling performance according to the standard of GB/T35263 plus 2017 detection and evaluation of textile contact instant cooling performance (the detection reports of the embodiments 1 and 4 are respectively shown in FIGS. 3 and 4), and the contact instant cooling coefficients of the fabrics are respectively 0.18 and 0.17, which are higher than the technical requirements. Therefore, the polyester fabric finished by the preparation method of the graphene-based antibacterial fabric has cool feeling, and the comfort level in summer can be improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (1)

1. A preparation method of an antibacterial fabric based on graphene is characterized by comprising the following steps: the method comprises the following steps:
pretreatment of the fabric: treating with a bath ratio of 1:20, wherein the treatment process comprises the steps of adding a polyester fabric into a treatment solution at 35 ℃, heating to 85 ℃, keeping the temperature for 1 hour, soaking in water at 60 ℃ for 10 minutes, washing with water at 50 ℃ once, and washing with water at 30 ℃ until the surface of the fabric is neutral; wherein the treatment liquid is an aqueous solution containing 5wt% of sodium hydroxide and 0.1wt% of JFC;
preparing a dye solution: diluting the graphene oxide slurry with water, adding a sodium acetate-acetic acid buffer solution and a BB emulsion, wherein the BB emulsion is a mixture of benzyl benzoate and castor oil polyoxyethylene ether in a mass ratio of 1:1, fully stirring and uniformly mixing to obtain a dye solution with the graphene oxide content of 0.25g/L and the buffer solution content of 0.20g/L, BB and the emulsion content of 0.30g/L, and the pH value of the dye solution is 4.0;
high-temperature dyeing: carrying out high-temperature dyeing on the polyester fabric by adopting a programmed heating method at a bath ratio of 1: 20; the temperature rise program is normal temperature-85 ℃, and the temperature rise rate is 2 ℃ per minute; the temperature is 85-110 ℃, the heating rate is 1 ℃ per minute, and the temperature is kept for 10 minutes; 110-130 ℃, the heating rate is 0.5 ℃ per minute, and the temperature is kept for 30 minutes; at a temperature of between 130 and 50 ℃ and a cooling rate of 3 ℃ per minute;
drying and baking: firstly drying the polyester fabric dyed at the high temperature at the temperature of 130 ℃, and then baking the dried polyester fabric at 194-195 ℃ for 4 minutes to obtain the graphene-based antibacterial fabric.
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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

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