CN113981676A - Preparation process of antibacterial fabric, fabric with antibacterial property and graphene oxide-loaded silver composite material - Google Patents

Preparation process of antibacterial fabric, fabric with antibacterial property and graphene oxide-loaded silver composite material Download PDF

Info

Publication number
CN113981676A
CN113981676A CN202111373884.1A CN202111373884A CN113981676A CN 113981676 A CN113981676 A CN 113981676A CN 202111373884 A CN202111373884 A CN 202111373884A CN 113981676 A CN113981676 A CN 113981676A
Authority
CN
China
Prior art keywords
antibacterial
graphene oxide
fabric
aqueous solution
composite material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111373884.1A
Other languages
Chinese (zh)
Inventor
薛书兵
张志勇
俞小华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changshu Huarui Needle Textile Co ltd
Original Assignee
Changshu Huarui Needle Textile Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changshu Huarui Needle Textile Co ltd filed Critical Changshu Huarui Needle Textile Co ltd
Priority to CN202111373884.1A priority Critical patent/CN113981676A/en
Publication of CN113981676A publication Critical patent/CN113981676A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • D06M11/73—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
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/208—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads cellulose-based
    • D03D15/217—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads cellulose-based natural from plants, e.g. cotton
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/50—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
    • 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
    • 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
    • D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic

Abstract

The application relates to the field of antibacterial fabrics, in particular to a preparation process of an antibacterial fabric, an antibacterial fabric and a graphene oxide-loaded silver composite material. The preparation process of the antibacterial fabric comprises the following steps: the preparation method comprises the steps of preparing a graphene oxide-loaded silver composite material, preparing antibacterial fibers, preparing an antibacterial fabric and the like. The fabric with antibacterial property is prepared by adopting the preparation process of the antibacterial fabric. The graphene oxide-loaded silver composite material is prepared by the following steps: taking an alkaline aqueous solution of graphene oxide, and adding epichlorohydrin into the alkaline aqueous solution; after the reaction, adding silver ion-containing solution and ammonia water in turn for reaction; the solid material was separated and dried. According to the antibacterial fabric, the silver and the textile fibers are firmly connected together through the connection mediation effect of the graphene oxide and the ammonia, so that the fibers and the fabric formed by the fibers have good antibacterial property, the fibers and the fabric have good washing resistance, and the antibacterial property is more durable.

Description

Preparation process of antibacterial fabric, fabric with antibacterial property and graphene oxide-loaded silver composite material
Technical Field
The application relates to the field of antibacterial fabrics, in particular to a preparation process of an antibacterial fabric, an antibacterial fabric and a graphene oxide-loaded silver composite material.
Background
The textile fabric composed of the fibers is beneficial to the attachment, survival and propagation of microorganisms due to more gaps; especially, the protein component of the fabric made of natural fibers can provide nutrients for breeding of microorganisms such as bacteria and the like. Along with the development of society and the improvement of living standard of people, the health is concerned more and more, so the antibacterial performance of the textile is concerned more and more.
At present, silver is adopted as an antibacterial agent in the related art to improve the antibacterial property of the fabric; the silver has an adsorption effect on microorganisms such as bacteria and the like, and can destroy enzymes with the respiratory effect of the microorganisms to ensure that the microorganisms die quickly; and compared with other antibacterial agents, the antibacterial agent has less toxicity to human bodies caused by silver ions or nano silver particles.
However, the inventors found in their studies that: in the related art, the silver-containing antibacterial agent is prepared into an antibacterial solution, then the fabric is immersed in the antibacterial solution for a period of time, so that silver ions or nano silver particles are migrated into the tissue of the fiber, and finally the fabric is dried to obtain the antibacterial fabric. According to the antibacterial fabric obtained by the method, the silver and the fibers are usually physically combined, and the binding force is poor, so that the antibacterial property of the fabric is poor in washing resistance, and the use of the antibacterial fabric is greatly limited.
Disclosure of Invention
In order to improve the washing resistance of the antibacterial property of the fabric, the application provides a preparation process of the antibacterial fabric, the fabric with the antibacterial property and a graphene oxide-loaded silver composite material.
In a first aspect, a preparation process of an antibacterial fabric is provided, which adopts the following technical scheme:
the preparation process of the antibacterial fabric comprises the following steps:
preparing a graphene oxide-loaded silver composite material: taking an alkaline aqueous solution of graphene oxide, adding epoxy chloropropane into the alkaline aqueous solution, and reacting for 3-8h at 50-80 ℃; then sequentially adding a silver ion-containing solution and ammonia water into the graphite oxide aqueous solution, and reacting at 50-70 ℃ for 1.5-5.5 h; then separating out solid substances, and drying to obtain the graphene oxide-loaded silver composite material;
preparing antibacterial fibers: preparing a graphene oxide-loaded silver composite material into an aqueous solution, and finishing the aqueous solution on pre-oxidized textile fibers to obtain antibacterial fibers;
preparing an antibacterial fabric: and weaving the antibacterial fibers into a fabric to obtain the antibacterial fabric.
By adopting the technical scheme, the epoxy chloropropane can modify the graphene oxide, and the molecular chain of the graphene oxide is connected with the active group, so that the reaction activity of the graphene oxide is improved. The ammonia water can react with the silver nitrate to combine the ammonia and the silver in a complexing mode and the like to form amino; the amino group can be combined with the modified graphene oxide, so that silver (silver ions or reduced nano silver particles) is firmly connected with the graphene oxide, and the silver is firmly loaded in the graphene oxide. Meanwhile, the graphene oxide subjected to surface modification can form a covalent bond with textile fibers, so that the graphene oxide and the textile fibers can be stably connected together. Therefore, through the connection medium of ammonia and graphene oxide, silver is firmly connected with the fibers forming the fabric; therefore, the antibacterial property of the fiber and the fabric formed by the fiber is endowed, and the antibacterial property of the fiber and the fabric has good water washing resistance. In addition, the graphene oxide also has good antibacterial property, so that the graphene oxide and silver are matched with each other to enable the obtained fabric to have more ideal antibacterial property.
Optionally, in the preparation step of the graphene oxide-supported silver composite material: the mass ratio of the graphene oxide to the epichlorohydrin is 100: (1.5-3.5).
By adopting the technical scheme, the proportion of the graphene oxide and the epoxy chloropropane is optimized, and the graphene oxide with more ideal reaction activity can be obtained, so that the bonding fastness of silver and textile fiber can be improved, and the fabric with good antibacterial performance, good washing resistance and good antibacterial durability can be obtained.
Optionally, in the preparation step of the graphene oxide-supported silver composite material: the pH value of the alkaline aqueous solution of the graphene oxide is 9-13.
Optionally, in the preparation step of the graphene oxide-supported silver composite material: the silver ion-containing solution is a silver nitrate solution, and the mass ratio of the graphene oxide to the silver nitrate is 100: (50-150).
By adopting the technical scheme, the proportion of the graphene oxide and the silver nitrate is optimized, and the graphene oxide is favorably loaded with more silver, so that the antibacterial property of the obtained fabric is favorably improved.
Optionally, in the preparation step of the graphene oxide-supported silver composite material: the mass ratio of the silver nitrate to the ammonia water is 100: (50-75).
By adopting the technical scheme, the proportion of silver nitrate and ammonia water is optimized, and the connection intermediary effect of the ammonia water is favorably and better exerted, so that the fabric with better antibacterial property, antibacterial performance and washing resistance is obtained.
Optionally, in the preparation step of the antibacterial fiber: and finishing the graphene oxide-loaded silver composite material aqueous solution on the pre-oxidized textile fiber by adopting a one-dipping-one-rolling method.
Optionally, in the preparation step of the antibacterial fiber: the concentration of the graphene oxide-loaded silver composite material aqueous solution is 0.5-1g/L, and the temperature is 50-80 ℃; in the process of one-time soaking and one-time rolling, the soaking time is controlled to be 60-90min, and the rolling residual rate is 50-75%.
By adopting the technical scheme, the technological parameters for finishing the graphene oxide-loaded silver composite material on the textile fibers are optimized, and the antibacterial performance of the obtained fabric is favorable for having more ideal water washing resistance.
Optionally, in the preparation step of the antibacterial fiber: the method for pre-oxidizing the textile fiber comprises the following steps: soaking textile fiber in 50-80 deg.C sodium periodate water solution for 20-30min, and controlling bath ratio to 1: (2-5); the concentration of the sodium periodate aqueous solution is 3-5 g/L.
By adopting the technical scheme, the fiber is favorably connected with the modified graphene oxide through covalent bonds.
In a second aspect, a fabric with antibacterial performance is provided, and the following technical scheme is adopted:
the fabric with antibacterial property is prepared by adopting the preparation process of the antibacterial fabric.
By adopting the technical scheme, the obtained fabric has good antibacterial property, and the obtained antibacterial performance has good washing resistance.
In a third aspect, a graphene oxide-loaded silver composite material is provided, which adopts the following technical scheme:
the graphene oxide-loaded silver composite material is prepared by the following steps:
taking an alkaline aqueous solution of graphene oxide, adding epoxy chloropropane into the alkaline aqueous solution, and reacting for 3-8h at 50-80 ℃;
sequentially adding a silver ion-containing solution and ammonia water into the graphite oxide aqueous solution, and reacting at 50-70 ℃ for 1.5-5.5 h;
and separating out solid substances, and drying to obtain the graphene oxide-loaded silver composite material.
By adopting the technical scheme, the graphene oxide-loaded silver composite material has good antibacterial property and can form firm connection with textile fibers, so that the textile fibers and the fabric formed by the textile fibers have lasting antibacterial property.
In summary, the present application has at least one of the following beneficial technical effects:
1. according to the preparation method, the silver and the textile fibers are firmly connected together through the connection intermediary effect of the graphene oxide modified by the epichlorohydrin and the ammonia, so that the fibers and the fabric formed by the fibers have good antibacterial property, the fibers and the fabric have good washing resistance, and the antibacterial property is more durable.
2. The antibacterial fabric obtained by the application forms antibacterial rings under the microbial environment; wherein, the ring width of the staphylococcus aureus inhibiting ring exceeds 10mm, the ring width of the escherichia coli inhibiting ring exceeds 14.5mm, and the good antibacterial performance is shown. Meanwhile, after 30 times of washing, the reduction amplitude of the width of the antibacterial ring of the fabric obtained by the method is not more than 25%, and most of the width of the antibacterial ring is not more than 15%; compared with the conventional method, the antibacterial performance of the antibacterial agent shows better water washing resistance and better antibacterial durability.
3. The graphene oxide-loaded silver composite material has good antibacterial property, can be firmly connected with textile fibers, and is favorable for endowing the textile fibers and fabrics formed by the textile fibers with better antibacterial property and washing resistance.
Detailed Description
The present application will be described in further detail with reference to examples.
The starting materials used in the examples are all commercially available. Wherein: the diameter of a sheet layer of the graphene oxide is 0.2-10 mu m, the number of the sheet layers is 1-2, and the carbon content is less than 48% and the oxygen content is more than 45%. The amino silicone oil softener is purchased from Guanlong textile auxiliary Co., Ltd, Dongguan city.
Example 1
The embodiment discloses a preparation process of an antibacterial fabric, which specifically comprises the following steps:
s10, preparing the graphene oxide-loaded silver composite material:
and S11, adding the graphene oxide into deionized water to prepare a graphene oxide aqueous solution with the concentration of 5 g/L.
S12, dropwise adding a 25wt% sodium hydroxide solution into the graphene oxide aqueous solution obtained in the step S11, and adjusting the pH of the graphene oxide aqueous solution to 9.
S13, taking 20L of the graphene oxide aqueous solution obtained in the S12, adding 1.5g of epichlorohydrin into the graphene oxide aqueous solution, and then stirring and reacting at the temperature of 50 ℃ for 3 h.
S14, slowly adding 588.2g of silver nitrate solution with the concentration of 8.5wt% into the graphite oxide aqueous solution obtained in the step S13 while stirring, and controlling the adding time to be 6 min; then, slowly adding 100g of ammonia water with the concentration of 25wt% into the graphite oxide aqueous solution, stirring while adding, and controlling the adding time to be 4 min; the reaction was then stirred at a temperature of 50 ℃ for 1.5 h.
S15, carrying out suction filtration on the product obtained in the S14; then washing with ethanol for three times, and washing with distilled water for three times; and drying to obtain the graphene oxide-loaded silver composite material.
S20, preparation of antibacterial fibers:
s21, adding the graphene oxide-supported silver composite material into deionized water to prepare a graphene oxide-supported silver composite material aqueous solution with the concentration of 0.5 g/L.
S22, soaking cotton fibers in 3g/L sodium periodate aqueous solution for pre-oxidation treatment; the temperature of the sodium periodate aqueous solution is controlled at 80 ℃, the immersion time is 20min, and the bath ratio is 1: 5.
S23, taking 10L of the graphene oxide-loaded silver composite material aqueous solution obtained in the step S21 and 1kg of cotton fibers obtained in the step S22; heating the graphene oxide-loaded silver composite material aqueous solution to 50 ℃, and adding the cotton fiber into the aqueous solution to be soaked for 90 min; then taking out the cotton fiber, and enabling the cotton fiber to pass through a roller, wherein the percent rolling is controlled to be 60%; and then drying the cotton fiber to obtain the antibacterial fiber.
S30, preparing the antibacterial fabric:
and S31, twisting the antibacterial fiber obtained in the step S23, and weaving the antibacterial fabric by a plain weaving method. In this embodiment, the antimicrobial fiber has a twist of 60, and the resulting fabric has a total of 190 warp and weft yarns per 1 inch (i.e., 190T).
S32, soaking the antibacterial fabric obtained in the step S31 in an aqueous solution of an amino silicone oil softening agent for 10min, wherein the dosage of the amino silicone oil softening agent is controlled to be 5% of the weight of the antibacterial fabric, and the bath ratio is 1: 15; taking out and drying after dipping. The step is favorable for improving the hand feeling of the antibacterial fabric.
The embodiment also discloses a fabric with antibacterial property, which is prepared by adopting the preparation process of the antibacterial fabric. The fabric has good antibacterial performance, and the antibacterial performance is good in washing resistance and durability.
The embodiment also discloses a graphene oxide-loaded silver composite material which is prepared by the preparation process S10 of the antibacterial fabric. The graphene oxide-loaded silver composite material has good antibacterial performance through the synergistic effect of silver and graphene oxide, and can be firmly connected with textile fibers, so that the textile fibers and fabrics formed by the textile fibers have lasting antibacterial performance.
Examples 2 to 10
As shown in table 1, examples 2-10 are essentially the same as example 1, with the main differences: in the preparation process of the antibacterial fabric, the control parameters of S13 are different.
Table 1 control parameters of S13 for the process of making the antimicrobial fabrics of examples 1-10
Item dosage/L of graphene oxide aqueous solution Amount of epichlorohydrin/g Reaction temperature/. degree.C Reaction time/h
Example 1 20 1.5 50 3
Example 2 20 2.0 50 3
Example 3 20 2.5 50 3
Example 4 20 3.0 50 3
Example 5 20 3.5 50 3
Example 6 20 3.0 60 3
Example 7 20 3.0 70 3
Example 8 20 3.0 80 3
Example 9 20 3.0 70 5
Example 10 20 3.0 70 8
Examples 11 to 18
As shown in Table 2, examples 11-18 are essentially the same as example 9, with the main differences: in the preparation process of the antibacterial fabric, the control parameters of S14 are different.
Table 2 control parameters of S14 for the process of making the antibacterial fabrics of examples 9, 11-18
Item dosage/L of graphene oxide aqueous solution Silver nitrate solution dosage/g Amount of ammonia water per gram Reaction temperature/. degree.C Reaction time/h
Example 9 20 588.2 100 50 1.5
Example 11 20 1176.4 200 50 1.5
Example 12 20 1764.6 300 50 1.5
Example 13 20 1176.4 240 50 1.5
Example 14 20 1176.4 300 50 1.5
Example 15 20 1176.4 240 60 1.5
Example 16 20 1176.4 240 70 1.5
Example 17 20 1176.4 240 60 3.5
Example 18 20 1176.4 240 60 5.5
Example 19
This example is substantially the same as example 17, with the main differences: the control parameters of the steps in the preparation process of the antibacterial fabric are different.
The method specifically comprises the following steps:
s10, preparing the graphene oxide-loaded silver composite material:
s11, adding the graphene oxide into deionized water to prepare a graphene oxide aqueous solution with the concentration of 2.5 g/L.
S12, dropwise adding a 25wt% sodium hydroxide solution into the graphene oxide aqueous solution obtained in the step S11, and adjusting the pH of the graphene oxide aqueous solution to 11.
S13, taking 40L of the graphene oxide aqueous solution obtained in the S12, adding 3g of epoxy chloropropane, and then stirring and reacting for 5h at the temperature of 70 ℃.
S14, slowly adding 2941.2g of silver nitrate solution with the concentration of 3.4wt% into the graphite oxide aqueous solution obtained in the step S13 while stirring, and controlling the adding time to be 10 min; then, 240g of ammonia water with the concentration of 25wt% is slowly added into the graphite oxide water solution, stirring is carried out while adding, and the adding time is controlled to be 4 min; the reaction was then stirred at a temperature of 60 ℃ for 3.5 h.
S15, carrying out suction filtration on the product obtained in the S14; then washing with ethanol for three times, and washing with distilled water for three times; and drying to obtain the graphene oxide-loaded silver composite material.
S20, preparation of antibacterial fibers:
s21, adding the graphene oxide-supported silver composite material into deionized water to prepare a graphene oxide-supported silver composite material aqueous solution with the concentration of 0.8 g/L.
S22, soaking cotton fibers in a 4g/L sodium periodate aqueous solution for pre-oxidation treatment; the temperature of the sodium periodate aqueous solution is controlled to be 65 ℃, the immersion time is 25min, and the bath ratio is 1: 3.5.
S23, taking 3.75L of the graphene oxide-loaded silver composite water solution obtained in the step S21 and 1kg of cotton fiber obtained in the step S22; heating the graphene oxide-loaded silver composite material aqueous solution to 80 ℃, and adding the cotton fiber into the aqueous solution to be soaked for 80 min; then taking out the cotton fiber, and enabling the cotton fiber to pass through a roller, wherein the percent rolling is controlled to be 75%; and then drying the cotton fiber to obtain the antibacterial fiber.
S30, preparing the antibacterial fabric:
and S31, twisting the antibacterial fiber obtained in the step S23, and weaving the antibacterial fabric by a plain weaving method. In this embodiment, the antimicrobial fiber has a twist of 60, and the resulting fabric has a total of 190 warp and weft yarns per 1 inch (i.e., 190T).
S32, soaking the antibacterial fabric obtained in the step S31 in an aqueous solution of an amino silicone oil softening agent for 20min, wherein the dosage of the amino silicone oil softening agent is controlled to be 3% of the weight of the antibacterial fabric, and the bath ratio is 1: 12; taking out and drying after dipping.
Example 20
This example is substantially the same as example 17, with the main differences: the control parameters of the steps in the preparation process of the antibacterial fabric are different.
The method specifically comprises the following steps:
s10, preparing the graphene oxide-loaded silver composite material:
and S11, adding the graphene oxide into deionized water to prepare a graphene oxide aqueous solution with the concentration of 4 g/L.
S12, dropwise adding a 25wt% sodium hydroxide solution into the graphene oxide aqueous solution obtained in the step S11, and adjusting the pH of the graphene oxide aqueous solution to 13.
S13, taking 25L of the graphene oxide aqueous solution obtained in the S12, adding 3g of epoxy chloropropane, and then stirring and reacting for 5h at the temperature of 70 ℃.
S14, slowly adding 735.3g of silver nitrate solution with the concentration of 13.6wt% into the graphite oxide aqueous solution obtained in the step S13 while stirring, and controlling the adding time to be 8 min; then, 240g of ammonia water with the concentration of 25wt% is slowly added into the graphite oxide water solution, stirring is carried out while adding, and the adding time is controlled to be 4 min; the reaction was then stirred at a temperature of 60 ℃ for 3.5 h.
S15, carrying out suction filtration on the product obtained in the S14; then washing with ethanol for three times, and washing with distilled water for three times; and drying to obtain the graphene oxide-loaded silver composite material.
S20, preparation of antibacterial fibers:
s21, adding the graphene oxide-supported silver composite material into deionized water to prepare a graphene oxide-supported silver composite material aqueous solution with the concentration of 1 g/L.
S22, soaking cotton fibers in 5g/L sodium periodate aqueous solution for pre-oxidation treatment; the temperature of the sodium periodate aqueous solution is controlled at 50 ℃, the immersion time is 30min, and the bath ratio is 1: 2.
S23, taking 8L of the graphene oxide-loaded silver composite material aqueous solution obtained in the step S21 and 1kg of cotton fibers obtained in the step S22; heating the graphene oxide-loaded silver composite material aqueous solution to 70 ℃, and adding the cotton fiber into the aqueous solution to be soaked for 60 min; then taking out the cotton fiber, and enabling the cotton fiber to pass through a roller, wherein the percent rolling is controlled to be 50%; and then drying the cotton fiber to obtain the antibacterial fiber.
S30, preparing the antibacterial fabric:
and S31, twisting the antibacterial fiber obtained in the step S23, and weaving the antibacterial fabric by a plain weaving method. In this embodiment, the antimicrobial fiber has a twist of 60, and the resulting fabric has a total of 190 warp and weft yarns per 1 inch (i.e., 190T).
S32, soaking the antibacterial fabric obtained in the step S31 in an aqueous solution of an amino silicone oil softening agent for 30min, wherein the dosage of the amino silicone oil softening agent is controlled to be 2% of the weight of the antibacterial fabric, and the bath ratio is 1: 10; taking out and drying after dipping.
Comparative example 1
The comparative example discloses a preparation process of an antibacterial fabric, which specifically comprises the following steps:
p11, adding nano silver particles (with average particle size of 25 nm) into deionized water to prepare nano silver aqueous solution with concentration of 0.125 g/L.
P12, soaking cotton fiber in 3g/L sodium periodate water solution for pre-oxidation treatment; the temperature of the sodium periodate aqueous solution is controlled at 80 ℃, the immersion time is 20min, and the bath ratio is 1: 5.
P13, taking 10L of nano-silver aqueous solution obtained from P11 and 1kg of cotton fiber obtained from P12; heating the nano-silver aqueous solution to 50 ℃, and adding the cotton fiber into the nano-silver aqueous solution to be soaked for 90 min; then taking out the cotton fiber, and enabling the cotton fiber to pass through a roller, wherein the percent rolling is controlled to be 60%; and then drying the cotton fiber to obtain the antibacterial fiber.
P14, twisting the antibacterial fiber obtained from P13, and weaving the fabric by a plain weaving method to obtain the antibacterial fabric; wherein, the twist of the antibacterial fiber is 60, and the sum of the number of the warp and weft yarns in each 1 inch of the obtained fabric is 190 (namely 190T).
P15, soaking the antibacterial fabric obtained from P14 in an aqueous solution of an amino silicone oil softening agent for 10min, wherein the dosage of the amino silicone oil softening agent is controlled to be 5% of the weight of the antibacterial fabric, and the bath ratio is 1: 15; taking out and drying after dipping.
Comparative example 2
The comparative example discloses a preparation process of an antibacterial fabric, which specifically comprises the following steps:
p21, preparing a silver nitrate aqueous solution with a concentration of 0.2 g/L.
P22, soaking cotton fiber in 3g/L sodium periodate water solution for pre-oxidation treatment; the temperature of the sodium periodate aqueous solution is controlled at 80 ℃, the immersion time is 20min, and the bath ratio is 1: 5.
P23, taking 10L of silver nitrate water solution of P21 and 1kg of cotton fiber obtained by P22; heating silver nitrate water solution to 50 deg.C, adding cotton fiber, and soaking for 90 min; then taking out the cotton fiber, and enabling the cotton fiber to pass through a roller, wherein the percent rolling is controlled to be 60%; and then drying the cotton fiber to obtain the antibacterial fiber.
P24, twisting the antibacterial fiber obtained from P23, and weaving the fabric by a plain weaving method to obtain the antibacterial fabric; wherein, the twist of the antibacterial fiber is 60, and the sum of the number of the warp and weft yarns in each 1 inch of the obtained fabric is 190 (namely 190T).
P25, soaking the antibacterial fabric obtained from P24 in an aqueous solution of an amino silicone oil softening agent for 10min, wherein the dosage of the amino silicone oil softening agent is controlled to be 5% of the weight of the antibacterial fabric, and the bath ratio is 1: 15; taking out and drying after dipping.
Performance detection
Carrying out performance detection on the fabrics with antibacterial performance obtained in examples 1-20 and comparative examples 1-2; the results are shown in Table 3.
1. And (3) antibacterial testing:
(1) 1mL of the strain with the concentration of 1X 108CFU/mL-5×108And adding the CFU/mL bacterial solution into 100mL nutrient agar culture medium, and uniformly mixing. Wherein the strain is selected from Staphylococcus aureusStaphylococcus aureus(ATCC 6538) or Escherichia coliEscherichia coli（8099）。
(2) A90 mm dish was taken and 10mL of nutrient agar was added, after which 5mL of the product obtained in step (1) was poured into the dish and allowed to coagulate.
(3) The fabrics with antibacterial performance obtained in examples 1-20 and comparative examples 1-2 were cut into test discs with a diameter of 30mm, and the test discs were in one-to-one correspondence with the plates in step (2).
(4) Test discs were placed on agar medium corresponding to the center of the plate.
(4) The plate is placed in an environment with 37 +/-1 ℃ for culturing for 36 h.
(5) The loop width of the bacteriostatic loop formed around the test disc was measured.
2. Wash resistance test of antibacterial properties:
(1) the fabrics with antibacterial performance obtained in the examples 1-20 and the comparative examples 1-2 are taken, washed by hand with clear water at 35 ℃ for 2min, and wrung. The washing was repeated 30 times.
(2) The antibacterial property of the washed antibacterial fabric is tested by the antibacterial testing method.
Table 3 performance test of fabrics having antibacterial properties of examples 1 to 20 and comparative examples 1 to 2
Item Ring width/mm of staphyloccocus ring Ring width/mm of staphyloccocus ring after washing Ring width/mm of Escherichia coli inhibiting ring Ring width/mm of Escherichia coli-inhibiting ring after washing
Example 1 10.3 8.0 14.8 11.1
Example 2 10.5 8.3 15.0 11.4
Example 3 10.6 8.7 14.9 11.6
Example 4 10.8 9.2 15.2 12.3
Example 5 10.8 9.1 15.1 12.2
Example 6 11.2 9.6 15.8 13.0
Example 7 11.4 10.1 16.2 13.8
Example 8 11.5 10.2 16.1 13.7
Example 9 11.8 10.8 16.7 14.5
Example 10 11.6 10.6 16.8 14.6
Example 11 15.6 14.4 20.6 18.1
Example 12 16.2 14.9 21.9 19.3
Example 13 16.5 14.7 22.8 20.5
Example 14 16.7 14.6 23.1 20.8
Example 15 17.2 16.2 23.5 21.4
Example 16 17.7 16.6 23.8 21.9
Example 17 18.0 17.1 24.4 22.7
Example 18 18.3 17.4 24.7 22.9
Example 19 18.2 17.4 24.6 23.1
Example 20 17.5 16.6 24.0 22.3
Comparative example 1 20.3 10.0 26.1 11.7
Comparative example 2 19.0 4.6 25.6 5.1
Referring to Table 3, it can be found from the test results of examples 1 to 20 and comparative examples 1 to 2 that: the fabric with antibacterial performance (hereinafter referred to as fabric) obtained in the embodiments of the application forms antibacterial rings; wherein, the ring width of the staphylococcus aureus inhibiting ring exceeds 10mm, the ring width of the escherichia coli inhibiting ring exceeds 14.5mm, and the good antibacterial performance is shown. Meanwhile, after 30 times of washing, the reduction amplitude of the width of the antibacterial ring of the fabric obtained in each embodiment of the application is not more than 25%, and most of the width of the antibacterial ring of the fabric is not more than 15%; in comparison, the reduction range of the width of the antibacterial ring of the fabric obtained in the comparative examples 1-2 after washing exceeds 50%, and the reduction range of the width of the antibacterial ring of the fabric obtained in the comparative examples 2 only adopting the silver nitrate aqueous solution even exceeds 75%; the antibacterial fabric obtained in the embodiments of the application has better washing resistance and antibacterial durability.
The results of the tests of examples 1 to 5 were analyzed to find that: with the increase of the usage amount of the epichlorohydrin, the reduction range of the ring width of the bacteriostatic ring of the obtained fabric is in a descending trend, namely the antibacterial property of the fabric is better and better in washing resistance. The surface of the graphene oxide is modified by the epichlorohydrin, so that the reactivity of the graphene oxide is improved, the graphene oxide has good bonding property with fibers and silver, the graphene oxide can better play a role in connecting media, the silver is more firmly connected to the textile fibers, and the washing resistance of the antibacterial property of the fabric is improved.
The results of the tests of examples 4, 6 to 8 were analyzed to find that: with the increase of the reaction temperature, the graphene oxide can be better modified by epoxy chloropropane, so that the bonding fastness of the graphene oxide with fiber and silver can be improved, the reduction range of the antibacterial ring width of the obtained fabric is in a whole descending trend, and the washing resistance of the antibacterial performance of the fabric is better and better.
The results of the tests of examples 7, 9 to 10 were analyzed to find that: with the increase of the reaction time, the reduction range of the width of the antibacterial ring of the obtained fabric is in a descending trend as a whole; the improvement of the reaction time can enable the epichlorohydrin to react with the graphene oxide more fully, so that the washing resistance of the antibacterial property of the fabric is improved.
As a result of examination of comparative examples 9, 11 to 12, it was found that: the increase of the using amount of the silver nitrate solution is beneficial to increasing the amount of silver loaded in the graphene oxide, so that the ring width of a bacteriostatic ring formed by the fabric is obviously increased, namely the antibacterial property of the obtained fabric is improved.
As a result of the examination of comparative examples 11 and 13 to 14, it was found that: the increase of the ammonia water relative to the use amount of the silver nitrate solution can obviously improve the ring width of the antibacterial ring of the obtained fabric, and can also reduce the reduction range of the ring width of the antibacterial ring after washing, namely the antibacterial property and the washing resistance of the antibacterial property of the obtained fabric are improved; the reason for this may be: the ammonia water can react with the silver nitrate to combine the ammonia with the silver, and meanwhile, the amino group formed by the ammonia water can be combined with the graphene oxide modified by the epoxy chloropropane, so that the ammonia water plays a role of connecting an intermediary, the bonding fastness of the graphene oxide and the silver is favorably improved, the silver loading amount in the graphene oxide is improved, and the antibacterial property washing resistance of the obtained fabric are further improved.
As a result of examination of comparative examples 13, 15 to 16, it was found that: with the increase of the reaction temperature, the function of the ammonia water connecting medium is more remarkable, so that the combination fastness of the graphene oxide and the silver is higher, and the antibacterial property and the washing resistance of the antibacterial property of the obtained fabric are improved.
As a result of examination of comparative examples 15, 17 to 18, it was found that: the effect of the ammonia water connection medium can be more fully exerted by prolonging the reaction time, so that the combination between the graphene oxide and the silver is more stable, the loading amount of the silver in the graphene oxide is higher, the antibacterial property and the washing resistance of the antibacterial property of the obtained fabric are improved, and the antibacterial durability is improved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (10)

1. The preparation process of the antibacterial fabric is characterized by comprising the following steps: the method comprises the following steps:
preparing a graphene oxide-loaded silver composite material: taking an alkaline aqueous solution of graphene oxide, adding epoxy chloropropane into the alkaline aqueous solution, and reacting for 3-8h at 50-80 ℃; then sequentially adding a silver ion-containing solution and ammonia water into the graphite oxide aqueous solution, and reacting at 50-70 ℃ for 1.5-5.5 h; then separating out solid substances, and drying to obtain the graphene oxide-loaded silver composite material;
preparing antibacterial fibers: preparing a graphene oxide-loaded silver composite material into an aqueous solution, and finishing the aqueous solution on pre-oxidized textile fibers to obtain antibacterial fibers;
preparing an antibacterial fabric: and weaving the antibacterial fibers into a fabric to obtain the antibacterial fabric.
2. The preparation process of the antibacterial fabric according to claim 1, characterized by comprising the following steps: in the preparation step of the graphene oxide-supported silver composite material: the mass ratio of the graphene oxide to the epichlorohydrin is 100: (1.5-3.5).
3. The preparation process of the antibacterial fabric according to claim 2, characterized by comprising the following steps: in the preparation step of the graphene oxide-supported silver composite material: the pH value of the alkaline aqueous solution of the graphene oxide is 9-13.
4. The preparation process of the antibacterial fabric according to claim 1, characterized by comprising the following steps: in the preparation step of the graphene oxide-supported silver composite material: the silver ion-containing solution is a silver nitrate solution, and the mass ratio of the graphene oxide to the silver nitrate is 100: (50-150).
5. The preparation process of the antibacterial fabric according to claim 4, characterized by comprising the following steps: in the preparation step of the graphene oxide-supported silver composite material: the mass ratio of the silver nitrate to the ammonia water is 100: (50-75).
6. The preparation process of the antibacterial fabric according to claim 1, characterized by comprising the following steps: in the preparation step of the antibacterial fiber: and finishing the graphene oxide-loaded silver composite material aqueous solution on the pre-oxidized textile fiber by adopting a one-dipping-one-rolling method.
7. The preparation process of the antibacterial fabric according to claim 6, characterized by comprising the following steps: in the preparation step of the antibacterial fiber: the concentration of the graphene oxide-loaded silver composite material aqueous solution is 0.5-1g/L, and the temperature is 50-80 ℃; in the process of one-time soaking and one-time rolling, the soaking time is controlled to be 60-90min, and the rolling residual rate is 50-75%.
8. The preparation process of the antibacterial fabric according to claim 6, characterized by comprising the following steps: in the preparation step of the antibacterial fiber: the method for pre-oxidizing the textile fiber comprises the following steps: soaking textile fiber in 50-80 deg.C sodium periodate water solution for 20-30min, and controlling bath ratio to 1: (2-5); the concentration of the sodium periodate aqueous solution is 3-5 g/L.
9. The fabric with antibacterial property is characterized in that: the antibacterial fabric is prepared by adopting the preparation process of the antibacterial fabric of any one of claims 1 to 8.
10. The graphene oxide-loaded silver composite material is characterized in that: the preparation method comprises the following steps:
taking an alkaline aqueous solution of graphene oxide, adding epoxy chloropropane into the alkaline aqueous solution, and reacting for 3-8h at 50-80 ℃;
sequentially adding a silver ion-containing solution and ammonia water into the graphite oxide aqueous solution, and reacting at 50-70 ℃ for 1.5-5.5 h;
and separating out solid substances, and drying to obtain the graphene oxide-loaded silver composite material.
CN202111373884.1A 2021-11-19 2021-11-19 Preparation process of antibacterial fabric, fabric with antibacterial property and graphene oxide-loaded silver composite material Pending CN113981676A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111373884.1A CN113981676A (en) 2021-11-19 2021-11-19 Preparation process of antibacterial fabric, fabric with antibacterial property and graphene oxide-loaded silver composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111373884.1A CN113981676A (en) 2021-11-19 2021-11-19 Preparation process of antibacterial fabric, fabric with antibacterial property and graphene oxide-loaded silver composite material

Publications (1)

Publication Number Publication Date
CN113981676A true CN113981676A (en) 2022-01-28

Family

ID=79749490

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111373884.1A Pending CN113981676A (en) 2021-11-19 2021-11-19 Preparation process of antibacterial fabric, fabric with antibacterial property and graphene oxide-loaded silver composite material

Country Status (1)

Country Link
CN (1) CN113981676A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115287895A (en) * 2022-10-09 2022-11-04 南通缘棉家纺有限公司 Bacteriostatic mite-killing fabric based on plant fibers and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03145410A (en) * 1989-10-31 1991-06-20 Agency Of Ind Science & Technol Antimicrobial silver zeolite and antimicrobial polymer composition free from change of color
WO2016145985A1 (en) * 2015-03-18 2016-09-22 上海和伍复合材料有限公司 Graphene/silver composite material and preparation method thereof
CN108624409A (en) * 2018-06-20 2018-10-09 曾宣 A kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent
CN112064341A (en) * 2020-09-28 2020-12-11 王磊 Graphene-based composite antibacterial material and preparation method thereof
CN112806389A (en) * 2021-02-01 2021-05-18 苏州大学 Preparation method, material, application and product of graphene oxide/silver nano composite hybrid antibacterial material
CN112832019A (en) * 2021-02-01 2021-05-25 苏州大学 Method for finishing fibers/fabrics by nano-silver graphene oxide composite nano-material and fibers/fabrics

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03145410A (en) * 1989-10-31 1991-06-20 Agency Of Ind Science & Technol Antimicrobial silver zeolite and antimicrobial polymer composition free from change of color
WO2016145985A1 (en) * 2015-03-18 2016-09-22 上海和伍复合材料有限公司 Graphene/silver composite material and preparation method thereof
CN108624409A (en) * 2018-06-20 2018-10-09 曾宣 A kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent
CN112064341A (en) * 2020-09-28 2020-12-11 王磊 Graphene-based composite antibacterial material and preparation method thereof
CN112806389A (en) * 2021-02-01 2021-05-18 苏州大学 Preparation method, material, application and product of graphene oxide/silver nano composite hybrid antibacterial material
CN112832019A (en) * 2021-02-01 2021-05-25 苏州大学 Method for finishing fibers/fabrics by nano-silver graphene oxide composite nano-material and fibers/fabrics

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115287895A (en) * 2022-10-09 2022-11-04 南通缘棉家纺有限公司 Bacteriostatic mite-killing fabric based on plant fibers and preparation method thereof

Similar Documents

Publication Publication Date Title
CN109287658A (en) A kind of carrying silver antimicrobials and preparation method thereof
JP2003531315A (en) Methods and fabrics to combat nosocomial infections
EP3543396B1 (en) Organic antimicrobial textile
JP7066628B2 (en) Antimicrobial fabric assembly
CN113981676A (en) Preparation process of antibacterial fabric, fabric with antibacterial property and graphene oxide-loaded silver composite material
Qin et al. Structure and properties of Cu (II) complex bamboo pulp fabrics
CN112647294B (en) Antibacterial cotton fabric with excellent washing fastness and preparation process thereof
Marcato et al. Biogenic silver nanoparticles: antibacterial and cytotoxicity applied to textile fabrics
US20060278534A1 (en) Method for producing nanosilver on a large scale, method for manufacturing nanosilver-adsorbed fiber, and antibacterial fiber thereby
KR20120046714A (en) Method for preparing an antimicrobial cotton of cellulose matrix having chemically and/or physically bonded silver and antimicrobial cotton prepared therefrom
Ibrahim et al. Enhancing the antibacterial properties of cotton fabric
CN112455022A (en) Antibacterial home furnishing cloth material and production process and application thereof
CN107100016B (en) Sandwich processing method of antibacterial non-natural leather
US20030159200A1 (en) Antimicrobial fabrics through surface modification
CN111534650A (en) Durable antibacterial soft leather for leather bags and preparation method thereof
Pedrosa et al. Comparison of the antibacterial activity of modified‐cotton with magainin I and LL‐37 with potential as wound‐dressings
CN112779767B (en) Antibacterial finishing agent for fiber yarns and cloth and preparation method thereof
KR20040000623A (en) Antibacterial textile by treated with nano-silver colloidal solution and their manufacturing methods
CN114351444B (en) Antibacterial non-woven fabric and preparation method thereof
CN113737344B (en) Antibacterial and deodorant spandex-covered yarn
EP1594555B1 (en) Disposable feminine hygiene products
JP3548917B2 (en) Antibacterial and UV-blocking textiles and method for producing the same
KR200392113Y1 (en) Nanosilver particles impregnated anti-bacterial textile and anti-bacterial socks, anti-bacterial cushiony products or inner wear using thereof
EP2993252A1 (en) Impregnatable matrix of plant, animal or synthetic origin or mixtures of same, containing a uniformly distributed antimicrobial compound, method for impregnating said matrix with a compound, and use thereof in the production of antimicrobial elements
CN108677272B (en) Micron-sized inorganic antibacterial fiber and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination