CN111809385B - Preparation method of polyamide fabric with lasting antibacterial effect - Google Patents
Preparation method of polyamide fabric with lasting antibacterial effect Download PDFInfo
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- CN111809385B CN111809385B CN202010654281.8A CN202010654281A CN111809385B CN 111809385 B CN111809385 B CN 111809385B CN 202010654281 A CN202010654281 A CN 202010654281A CN 111809385 B CN111809385 B CN 111809385B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic System
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—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 nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—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 nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—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
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
- D06M13/262—Sulfated compounds thiosulfates
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a preparation method of a lasting antibacterial polyamide fabric, which comprises the following steps: placing the polyamide fabric in an inorganic acid solution for acid treatment, discharging liquid, neutralizing with a sodium hydroxide solution, washing with water to be neutral, and drying to obtain a modified polyamide fabric; adding sodium dodecyl benzene sulfonate into a hydrochloric acid aqueous solution, stirring to fully dissolve the sodium dodecyl benzene sulfonate, adding an antibacterial agent, stirring to uniformly disperse the antibacterial agent, gradually adding a precursor, continuing stirring after the precursor is added, and then heating to react under the stirring condition to obtain a composite antibacterial agent; adding sodium hypophosphite into the composite antibacterial agent, adjusting the pH value by using an alkaline agent, modifying the modified polyamide fabric by adopting a two-dipping and two-rolling method, rolling, baking, washing and drying to prepare the durable antibacterial polyamide fabric. The invention has simple process and easily controlled conditions, and the prepared polyamide fabric has broad-spectrum, high-efficiency and lasting antibacterial property.
Description
Technical Field
The invention belongs to the field of textiles, and particularly relates to a processing technology of a durable antibacterial polyamide fabric.
Background
The textile has a loose and porous structure, so that excrement secreted by metabolism of a human body can be easily absorbed, a favorable place and required nutrients are provided for attachment and propagation of microorganisms, and a large amount of germs are propagated. The presence of microorganisms on textiles not only affects their performance (e.g., mildew, catalysis, deterioration, etc.), but also poses serious health risks to the wearer (e.g., causing skin disorders, entering the body to induce disease, etc.). Therefore, the antibacterial finishing is carried out on the textile to hinder and inhibit the metabolism and reproduction of microorganisms in the using and storing processes of the textile, and the antibacterial finishing has important significance for protecting human health. In recent years, antibacterial textiles have become a focus of research in the field of functional textiles. New coronavirus has been abused in 2019, and by the time that countries and regions affected by epidemic situations are more than 200, infected persons are over 1100 and over ten thousand, and death persons are over 50 and over ten thousand. The rapid propagation of new coronavirus makes the research and development of antibacterial and antiviral textile fabric become the research focus at home and abroad.
The antibacterial textile is usually realized by adding an antibacterial agent into the textile, and the preparation method mainly comprises a fibril method and a post-finishing method, and also can realize the antibacterial function by a blending or interweaving method. The fibril method is that antibacterial agent is added into spinning solution to prepare antibacterial fiber through a spinning process, and the fabric prepared by the method has obvious and lasting antibacterial property, but has the defects of high technical difficulty, high cost and the like. The blending or interweaving method is to compound the fiber with antibacterial property and the common fiber to prepare the antibacterial fabric, and the antibacterial effect of the fabric is mainly determined by the content of the antibacterial fiber. The post-finishing method is to apply an antibacterial agent to the surface of the fiber by coating or padding to endow the fabric with an antibacterial effect, and is the most studied antibacterial fabric preparation method at present due to simple operation, but the antibacterial durability of the fabric prepared by the method is to be further improved.
The antibacterial finishing agent is one of important factors influencing the antibacterial effect of the fabric. The antibacterial finishing agent can be divided into inorganic antibacterial agent, organic antibacterial agent and natural antibacterial agent according to factors such as the source, action mechanism, composition structure and the like of the antibacterial finishing agent. The inorganic antibacterial agent mainly comprises silver and copper, wherein silver is high in price and is easily oxidized to generate dark silver oxide or black simple substance silver, copper is low in price and has a certain antiviral effect, and the color of the copper can change the color of the fabric. The organic antibacterial agent mainly comprises quaternary ammonium salts, guanidines, halogenated phenols and halogen amines, and the antibacterial agent generally has high toxicity and is easy to cause bacteria to generate drug resistance. The natural antibacterial agent has the advantages of good biocompatibility, natural degradation, no drug resistance of bacteria and the like, and is an antibacterial agent with great development potential. In order to meet the increasing demands of people on health, comfort and safety, an ideal antibacterial finishing agent should have the characteristics of safety, broad spectrum, durability and the like, and simultaneously have no obvious influence on the original excellent characteristics and appearance of textiles.
Therefore, a further solution is necessary to overcome the defects of the existing antibacterial protective fabric.
Disclosure of Invention
The invention aims to provide a preparation method of a lasting antibacterial polyamide fabric, and the preparation method is used for solving the problems.
The technical scheme of the invention is as follows:
a preparation method of a lasting antibacterial polyamide fabric comprises the following steps:
(1) fiber surface modification treatment: placing polyamide fabric in an inorganic acid solution, carrying out acid treatment for 10-30min at the temperature of 25-35 ℃, discharging liquid, neutralizing with a sodium hydroxide solution, washing to be neutral, and drying for 30-60min at the temperature of 80-100 ℃ to obtain modified polyamide fabric;
(2) preparing a composite antibacterial agent: adding sodium dodecyl benzene sulfonate into a hydrochloric acid aqueous solution, stirring for 30-60min at the temperature of 25 ℃ to fully dissolve the sodium dodecyl benzene sulfonate, adding an antibacterial agent, continuously stirring for 30-60min to uniformly disperse the antibacterial agent, gradually adding a precursor within 20-30min, continuously stirring for 20-30min after the precursor is added, heating to 50-60 ℃ at the heating rate of 1-2 ℃/min, and reacting for 3-4h under the stirring condition to obtain a composite antibacterial agent, wherein the stirring rotation speed is 150-;
(3) modified fabric antibacterial finishing: adding sodium hypophosphite into the composite antibacterial agent, adjusting the pH value to 6-7 by using an alkaline agent, modifying the modified polyamide fabric by adopting a two-dipping two-rolling method at room temperature, wherein the rolling residue is 80-100%, baking for 5-15min at the temperature of 80-90 ℃, baking for 1-5min at the temperature of 130-150 ℃, washing with water, and finally drying at the temperature of 80-100 ℃ to prepare the durable antibacterial polyamide fabric.
Further, the polyamide fabric in the step (1) is selected from any one of a polyamide filament fabric, a polyamide staple fiber and polyamide filament interwoven fabric, a polyamide staple fiber and polyamide filament core spun yarn fabric, and a fabric made of a polyamide staple fiber and polyamide filament drawn and twisted yarn.
Further, in the step (1), the mass percentage concentration of the inorganic acid solution is 3-8%, the inorganic acid in the inorganic acid solution is selected from any one of hydrochloric acid, sulfuric acid and nitric acid, and the mass percentage concentration of the sodium hydroxide solution is 1-3%.
Further, in the step (1), in the acid treatment process, the mass ratio of the polyamide fabric to the inorganic acid solution is 1-150, and in the water washing to neutrality process, the mass ratio of the polyamide fabric to the sodium hydroxide solution is 1-150.
Further, in the step (2), the antibacterial agent is selected from any one or a mixture of several of a metal antibacterial agent, an organic antibacterial agent and a natural antibacterial agent, wherein the metal antibacterial agent is selected from any one of silver-based, copper-based and zinc-based antibacterial agents, the organic antibacterial agent is selected from any one of quaternary ammonium salts or quaternary phosphonium salts containing siloxane groups, and the natural antibacterial agent is selected from chitosan with deacetylation degree of 80-90%.
Further, the precursor in the step (2) is selected from any one or more of methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane and ethyltriethoxysilane.
Further, in the step (2), the precursor is 20-40g/L, the sodium dodecyl benzene sulfonate is 0.5-1g/L, the hydrochloric acid is 3-5g/L, and the antibacterial agent is 5-10 g/L.
Further, in the step (2), the composite antibacterial agent takes polysiloxane sol as a carrier, the antibacterial agent is fixed in the grid, and the particle size of the polysiloxane sol is 50-100 nm.
Further, the alkaline agent in the step (3) is sodium hydroxide solution with the mass concentration of 5-10 g/L.
Further, the sodium hypophosphite in the step (3) is 5-10 g/L.
The invention provides a preparation method of a lasting antibacterial polyamide fabric, which adopts polysiloxane sol as a carrier, fixes a plurality of antibacterial agents in grids to prepare a composite antibacterial agent, and then uses the composite antibacterial agent for antibacterial finishing of textiles, and has the following advantages:
1. the process is simple, and the process parameters are stable and easy to control;
2. the fabric has broad-spectrum antibacterial property;
3. the fabric has lasting antibacterial ability and good washability.
Detailed Description
The invention discloses a preparation method of a lasting antibacterial polyamide fabric, which comprises the following specific process steps:
firstly, fiber surface modification treatment
The method comprises the following specific steps: placing the polyamide fabric in an inorganic acid solution with the mass percentage concentration of 3-8%, wherein the polyamide fabric is selected from one of polyamide filament fabric, polyamide staple fiber fabric, interwoven fabric of polyamide staple fibers and polyamide filaments, fabric of polyamide staple fibers and polyamide filament covering yarns, and fabric made by drawing and twisting polyamide staple fibers and polyamide filaments, the inorganic acid is any one of hydrochloric acid, sulfuric acid and nitric acid, performing acid treatment for 10-30min at the temperature of 25-35 ℃, discharging liquid, neutralizing with a sodium hydroxide solution with the mass percentage concentration of 1-3%, washing with water to be neutral, and drying for 30-60min at the temperature of 80-100 ℃. The mass ratio of the fiber to the treatment liquid in the processes of acid treatment, water washing and neutralization is 1: 5-10.
The principle of the step is as follows: amide bonds in the molecular structure of the polyamide fiber are easy to hydrolyze under an acidic condition to generate two reactive groups of amino and carboxyl, the reactivity of the fiber surface and a chemical auxiliary agent can be improved through acid hydrolysis, and common acid agents comprise hydrochloric acid, nitric acid and sulfuric acid. In addition, the acid hydrolysis process is a surface-to-interior process, and can be controlled by conditions, and the acid hydrolysis is utilized to generate a rough structure on the surface of the fiber, so that the specific surface area of the fiber is increased, and the loading capacity of the fiber for the antibacterial agent is further improved.
Preparation of composite antibacterial agent
Adding 0.5-1g/L sodium dodecyl benzene sulfonate into 3-5g/L hydrochloric acid aqueous solution, stirring at 25 deg.C for 30-60min to fully dissolve the sodium dodecyl benzene sulfonate, adding 5-10g/L antibacterial agent selected from one or more of metal antibacterial agent, organic antibacterial agent and natural antibacterial agent, wherein the metal antibacterial agent is preferably silver-based, copper-based or zinc-based antibacterial agent, the organic antibacterial agent is preferably quaternary ammonium salt or quaternary phosphonium salt containing siloxane group, and the natural antibacterial agent is preferably chitosan with deacetylation degree of 80-90%. Stirring for 30-60min to disperse the antibacterial agent uniformly, and gradually adding 20-40g/L precursor selected from one or more of methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane and ethyltriethoxysilane within 20-30 min. After the precursor is added, the mixture is continuously stirred for 20-30min, then the temperature is raised to 50-60 ℃ at the speed of 1-2 ℃/min, the mixture reacts for 3-4h under the stirring condition, and the composite antibacterial agent with the particle size of 50-100nm is obtained, wherein the stirring speed in the step is 150-.
The principle of the step is as follows: the invention selects polysiloxane hydrosol as a carrier to prepare the composite antibacterial agent, and the composite antibacterial agent is based on the following points: the polysiloxane hydrosol has good film-forming property, and silicon hydroxyl (-Si-OH) which is not subjected to self-crosslinking can be chemically formed with carboxyl (-COOH) formed by hydrolysis on the surface of fiber to form a film, and a plurality of antibacterial agents are fixed in a sol grid by fiber, alkoxy in siloxane groups is hydrolyzed to generate silicon hydroxyl (Si-OH) to perform chemical reaction, so that firm valence bond combination is formed, and the load fastness of the antibacterial agents on the surface of the fiber is improved; the mesh formed by dehydrating the silicon hydroxyl groups can lock the antibacterial agent and improve the washability of the fabric finished by the antibacterial agent.
Third, modified fabric antibacterial finishing
Adding 5-10g/L sodium hypophosphite into the composite antibacterial agent, adjusting the pH value to 6-7 by using an alkaline agent, wherein the alkaline agent is a sodium hydroxide solution with the mass concentration of 5-10g/L, modifying the fabric by adopting a two-dipping two-rolling method at room temperature, baking the fabric for 5-15min at the temperature of 80-90 ℃ and baking the fabric for 1-5min at the temperature of 130-150 ℃, washing the fabric with water, and baking the fabric at the temperature of 80-100 ℃.
The principle of the step is as follows: the effective hydrolysis of the precursor of the polysiloxane hydrosol is the basis for preparing the silica sol, and the acidity adjustment is beneficial to the hydrolysis of the precursor. However, polyamide fibers are susceptible to hydrolysis under acidic conditions, which in turn affects the performance properties of the fabric. The pH value of the silica sol is adjusted to 6-7, which can not cause the rapid condensation of the sol particles and can not cause obvious influence on the fiber strength.
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanying the present invention are further described below. The invention is not limited to the embodiments listed but also comprises any other known variations within the scope of the invention as claimed.
Reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Comparative example
Modifying the polyamide fabric by adopting a two-dipping two-rolling method at room temperature, wherein the dosage of the polysiloxane quaternary ammonium salt antibacterial agent is 10g/L, the rolling residual rate is 90%, baking is carried out for 4min at 90 ℃, baking is carried out for 1min at 130 ℃, washing is carried out, and drying is carried out at 80 ℃.
Example 1
The embodiment shows a preparation method of a lasting antibacterial polyamide fabric according to the following steps:
1. fiber surface modification treatment: placing the interwoven fabric of the polyamide short fibers and the polyamide filaments in a hydrochloric acid solution with the mass percentage concentration of 3%, carrying out acid treatment for 10min at the temperature of 25 ℃, discharging liquid, neutralizing by using a sodium hydroxide solution with the mass percentage concentration of 1%, washing to be neutral, and drying for 30min at the temperature of 80 ℃. The mass ratio of the fiber to the treatment liquid in the processes of acid treatment, water washing and neutralization is 1: 5.
2. Preparing a composite antibacterial agent: adding 0.5g/L sodium dodecyl benzene sulfonate into 3g/L hydrochloric acid water solution, stirring at 25 deg.C for 30min to fully dissolve the sodium dodecyl benzene sulfonate, adding 5g/L metal antibacterial agent, preferably silver, copper and zinc antibacterial agents, stirring for 30min to uniformly disperse the metal antibacterial agent, and gradually adding 20g/L methyltrimethoxysilane within 20 min. After the methyltrimethoxysilane is added, stirring for 20min, heating to 50 ℃ at the speed of 1 ℃/min, and reacting for 3h under the stirring condition to obtain the composite antibacterial agent with the particle size of 50nm, wherein the stirring speed is 150 r/min.
3. Modified fabric antibacterial finishing: adding 5g/L sodium hypophosphite into the composite antibacterial agent, adjusting the pH value to 6 by using an alkaline agent, wherein the alkaline agent is a sodium hydroxide solution with the mass concentration of 5g/L, modifying the fabric by adopting a two-dipping two-rolling method at room temperature, controlling the rolling residual rate to be 80%, baking for 5min at 80 ℃, baking for 1min at 130 ℃, washing and drying at 80 ℃.
Example 2
The embodiment shows a preparation method of the lasting antibacterial polyamide fabric according to the following steps:
1. fiber surface modification treatment: placing polyamide short fiber and polyamide filament core-spun yarn fabric in a sulfuric acid solution with the mass percentage concentration of 4%, carrying out acid treatment for 15min at the temperature of 28 ℃, discharging liquid, neutralizing with a sodium hydroxide solution with the mass percentage concentration of 2%, washing with water to be neutral, and drying for 40min at the temperature of 90 ℃. The mass ratio of the fiber to the treatment liquid in the processes of acid treatment, water washing and neutralization is 1: 7.
2. Preparing a composite antibacterial agent: adding 0.6g/L sodium dodecyl benzene sulfonate into 3.5g/L hydrochloric acid water solution, stirring at 25 deg.C for 50min to fully dissolve the sodium dodecyl benzene sulfonate, adding 6g/L organic antibacterial agent, preferably quaternary ammonium salt or quaternary phosphonium salt containing siloxane group. Stirring for 40min to disperse the antibacterial agent uniformly, and gradually adding 25g/L methyl triethoxysilane within 22 min. After the methyl triethoxysilane is added, the mixture is continuously stirred for 22min, then the temperature is raised to 52 ℃ at the speed of 1.2 ℃/min, and the mixture reacts for 3.3h under the stirring condition, so that the composite antibacterial agent with the particle size of 60nm is obtained, and the stirring speed is 200 r/min.
3. Modified fabric antibacterial finishing: adding 7g/L sodium hypophosphite into the composite antibacterial agent, adjusting the pH value to 6 by using an alkaline agent, wherein the alkaline agent is a sodium hydroxide solution with the mass concentration of 6g/L, modifying the fabric by adopting a two-dipping two-rolling method at room temperature, baking the fabric for 8min at 82 ℃ with the rolling residue rate of 85%, baking for 2min at 135 ℃, washing and drying at 85 ℃.
Example 3
The embodiment shows a preparation method of a lasting antibacterial polyamide fabric according to the following steps:
1. fiber surface modification treatment: putting a fabric made of polyamide short fibers and polyamide filament yarns through drawing and twisting in a hydrochloric acid solution with the mass percentage concentration of 7%, performing acid treatment for 25min at the temperature of 30 ℃, discharging liquid, neutralizing with a sodium hydroxide solution with the mass percentage concentration of 2%, washing with water to be neutral, and drying for 35min at the temperature of 95 ℃. The mass ratio of the fiber to the treatment liquid in the processes of acid treatment, water washing and neutralization is 1: 8.
2. Preparing a composite antibacterial agent: adding 0.8g/L sodium dodecyl benzene sulfonate into 4g/L hydrochloric acid water solution, stirring at 25 deg.C for 45min to fully dissolve the sodium dodecyl benzene sulfonate, and adding 8g/L chitosan with deacetylation degree of 80%. Stirring for 50min to disperse the antibacterial agent, and gradually adding 35g/L ethyl trimethoxy silane within 28 min. After the ethyl trimethoxy silane is added, stirring is continued for 27min, then the temperature is raised to 58 ℃ at the speed of 1 ℃/min, and the reaction is carried out for 3.7h under the stirring condition, so as to obtain the composite antibacterial agent with the particle size of 90nm, wherein the stirring speed is 250 r/min.
3. Modified fabric antibacterial finishing: adding 8g/L sodium hypophosphite into the composite antibacterial agent, adjusting the pH value to 7 by using an alkaline agent, wherein the alkaline agent is a sodium hydroxide solution with the mass concentration of 8g/L, modifying the fabric by adopting a two-dipping and two-rolling method at room temperature, controlling the rolling residual rate to be 90%, baking at 88 ℃ for 12min, baking at 145 ℃ for 4min, washing with water, and drying at 90 ℃.
Example 4
The embodiment shows a preparation method of a lasting antibacterial polyamide fabric according to the following steps:
1. fiber surface modification treatment: placing the polyamide filament fabric in a nitric acid solution with the mass percentage concentration of 8%, carrying out acid treatment for 30min at the temperature of 35 ℃, discharging liquid, neutralizing with a sodium hydroxide solution with the mass percentage concentration of 3%, washing to be neutral, and drying for 60min at the temperature of 100 ℃. The mass ratio of the fiber to the treatment liquid in the processes of acid treatment, water washing and neutralization treatment is 1: 10.
2. Preparing a composite antibacterial agent: adding 1g/L sodium dodecyl benzene sulfonate into 5g/L hydrochloric acid water solution, stirring at 25 deg.C for 60min to fully dissolve sodium dodecyl benzene sulfonate, adding 10g/L natural antibacterial agent, preferably chitosan with deacetylation degree of 90%. And continuously stirring for 60min to uniformly disperse the antibacterial agent, gradually adding 40g/L of ethyl triethoxysilane within 30min, continuously stirring for 30min after the ethyl triethoxysilane is added, heating to 60 ℃ at the speed of 2 ℃/min, and reacting for 4h under the stirring condition to obtain the composite antibacterial agent with the particle size of 100nm, wherein the stirring speed is 300 revolutions per minute.
3. Modified fabric antibacterial finishing: adding 10g/L sodium hypophosphite into the composite antibacterial agent, adjusting the pH value to 7 by using an alkaline agent, wherein the alkaline agent is a sodium hydroxide solution with the mass concentration of 10g/L, modifying the fabric by adopting a two-dipping two-rolling method at room temperature, controlling the rolling residual rate to be 100%, baking for 15min at 90 ℃, baking for 5min at 150 ℃, washing and drying at 100 ℃.
TABLE 1
In summary, compared with the prior art, the invention has the beneficial effects that: according to the preparation method of the lasting antibacterial polyamide fabric, the sol-gel method is adopted to prepare the high-efficiency, lasting, safe, harmless or low-harm composite antibacterial finishing agent on the basis of systematic screening of the antibacterial agent, and the finishing agent is further applied to polyamide fibers with excellent performance to prepare the high-performance antibacterial protective polyamide fabric and series products thereof. The invention has simple process and easily controlled conditions, and the prepared polyamide fabric has broad-spectrum, high-efficiency and lasting antibacterial property.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (3)
1. A preparation method of a lasting antibacterial polyamide fabric is characterized by comprising the following steps:
(1) fiber surface modification treatment: placing a polyamide fabric in an inorganic acid solution, carrying out acid treatment for 10-30min at the temperature of 25-35 ℃, discharging liquid, neutralizing with a sodium hydroxide solution, washing to be neutral, and drying for 30-60min at the temperature of 80-100 ℃ to obtain a modified polyamide fabric, wherein the mass percentage concentration of the inorganic acid solution is 3-8%, the inorganic acid in the inorganic acid solution is selected from any one of hydrochloric acid, sulfuric acid and nitric acid, the mass percentage concentration of the sodium hydroxide solution is 1-3%, the mass ratio of the polyamide fabric to the inorganic acid solution is 1: 5-10 in the acid treatment process, and the mass ratio of the polyamide fabric to the sodium hydroxide solution is 1: 5-10 in the washing to be neutral process;
(2) preparing a composite antibacterial agent: adding 0.5-1g/L sodium dodecyl benzene sulfonate into 3-5g/L hydrochloric acid aqueous solution, stirring for 30-60min at the temperature of 25 ℃ to fully dissolve the sodium dodecyl benzene sulfonate, adding 5-10g/L antibacterial agent, continuously stirring for 30-60min to uniformly disperse the antibacterial agent, gradually adding 20-40g/L precursor within 20-30min, continuously stirring for 20-30min after the precursor is added, heating to 50-60 ℃ at the heating rate of 1-2 ℃/min, reacting for 3-4h under the stirring condition to obtain the composite antibacterial agent with the particle size of 50-100nm, wherein the stirring rotation speed is 150-300 r/min, and the precursor is selected from methyltrimethoxysilane, and the like, Any one or more of methyl triethoxysilane, ethyl trimethoxysilane and ethyl triethoxysilane;
(3) modified fabric antibacterial finishing: adding 5-10g/L sodium hypophosphite into the composite antibacterial agent, adjusting the pH value to 6-7 by using an alkaline agent, modifying the modified polyamide fabric by adopting a two-dipping and two-rolling method at room temperature, wherein the rolling residual rate is 80-100%, baking for 5-15min at the temperature of 80-90 ℃, baking for 1-5min at the temperature of 130-150 ℃, washing with water, and finally baking at the temperature of 80-100 ℃ to prepare the durable antibacterial polyamide fabric, wherein the alkaline agent is a sodium hydroxide solution with the mass concentration of 5-10 g/L.
2. The preparation method of the lasting antibacterial polyamide fabric according to claim 1, characterized in that: the polyamide fabric in the step (1) is any one of a polyamide filament fabric, a polyamide short fiber and polyamide filament interwoven fabric, a polyamide short fiber and polyamide filament core-spun yarn fabric and a fabric made by doubling and twisting polyamide short fibers and polyamide filaments.
3. The preparation method of the lasting antibacterial polyamide fabric according to claim 1, characterized in that: in the step (2), the antibacterial agent is selected from any one or a mixture of several of a metal antibacterial agent, an organic antibacterial agent and a natural antibacterial agent, wherein the metal antibacterial agent is selected from any one of a silver-series antibacterial agent, a copper-series antibacterial agent and a zinc-series antibacterial agent, the organic antibacterial agent is selected from any one of quaternary ammonium salt or quaternary phosphonium salt containing siloxane groups, and the natural antibacterial agent is selected from chitosan with deacetylation degree of 80-90%.
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