CN111793975A - Antibacterial fabric and preparation method thereof - Google Patents
Antibacterial fabric and preparation method thereof Download PDFInfo
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- CN111793975A CN111793975A CN202010723700.9A CN202010723700A CN111793975A CN 111793975 A CN111793975 A CN 111793975A CN 202010723700 A CN202010723700 A CN 202010723700A CN 111793975 A CN111793975 A CN 111793975A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M11/77—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 silicon or compounds thereof
- D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M13/10—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 oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M13/322—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 nitrogen
- D06M13/46—Compounds containing quaternary nitrogen atoms
- D06M13/47—Compounds containing quaternary nitrogen atoms derived from heterocyclic compounds
- D06M13/477—Compounds containing quaternary nitrogen atoms derived from heterocyclic compounds having six-membered heterocyclic rings
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/05—Cellulose or derivatives thereof
- D06M15/09—Cellulose ethers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- 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
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
Abstract
The invention discloses an antibacterial fabric and a preparation method thereof, wherein the preparation method of the antibacterial fabric comprises the following steps: soaking the fabric in a finishing agent, soaking and rolling the fabric, washing the fabric with water, and baking the fabric; the finishing agent is an antibacterial finishing agent or a moisture absorption antibacterial composite finishing agent. The antibacterial fabric has good antibacterial performance and moisture permeability, and meanwhile, the antibacterial active ingredient and the fabric are high in binding fastness and resistant to washing.
Description
Technical Field
The invention relates to the technical field of textiles, in particular to an antibacterial fabric and a preparation method thereof.
Background
Textile fabrics generally include weft-knitted textile fabrics and warp-knitted textile fabrics. Weft-knitted textile fabrics are usually made from low-stretch polyester yarns or special-shaped polyester yarns, nylon yarns, cotton yarns, wool yarns and the like as raw materials by knitting flat stitch, variable flat stitch, rib flat stitch, double rib flat stitch, jacquard weave, terry weave and the like on various weft knitting machines. Textile fabric has porous ventilative structure, can provide the comfort for the human body when processing for the clothing is worn, but this kind of structure also absorbs human secreted grease, sweat easily, then the dust in the adhesion environment, impurity etc. build good living place for the microorganism, lead to breeding such as bacterium, dust mite. The fabric is yellowed and discolored, unpleasant smell is caused, and human body infection diseases and harm to body health can be caused in severe cases.
To inhibit the growth of bacteria, dust mites, etc., it is common practice to modify the fabric to be antibacterial. However, currently commonly used antibacterial agents are not resistant to washing with water, resulting in a non-lasting antibacterial activity; in addition, after the fabric is modified by using the antibacterial agents, the wearability of the fabric is often affected, for example, the moisture permeability and air permeability are poor, and the mechanical performance is poor. Therefore, it is very important to develop an antibacterial fabric and simultaneously improve the antibacterial performance, the water washing resistance and the wearability of the fabric.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an antibacterial fabric and a preparation method thereof.
The preparation method of the antibacterial fabric comprises the following steps: and (3) soaking the fabric in the finishing agent, soaking for two times and rolling for two times, baking, washing and drying to obtain the antibacterial fabric.
Preferably, the preparation method of the antibacterial fabric comprises the following steps: soaking the fabric in a moisture-absorbing and antibacterial composite finishing agent at 40-60 ℃ for 50-100min, wherein the mass ratio of the finishing agent to the fabric is (10-60) to 1; two-dipping and two-rolling, wherein the rolling residual rate is 70-100%; pre-baking at 40-60 deg.C for 1-5min, baking at 80-120 deg.C for 20-50min, washing with water, and drying to obtain antibacterial fabric.
Preferably, the fabric is any one of a pure cotton fabric, a polyester fabric, a polypropylene fabric, a bamboo fiber fabric, a viscose fiber fabric, a cotton-polyester fabric, a wool fabric and a polyamide fabric.
Preferably, the finishing agent is an antibacterial finishing agent or a moisture absorption antibacterial composite finishing agent.
Preferably, the antibacterial finishing agent is prepared by the following method: adding sodium lignosulfonate, a modified quaternary ammonium salt antibacterial agent and sodium citrate into water, and stirring at 60-80 ℃ for 10-60min, wherein the mass ratio of the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent, the sodium citrate and the water is (0.1-1): 0.5-5): 0.1-1): 50-100, so as to obtain the antibacterial finishing agent.
Preferably, the modified quaternary ammonium salt antibacterial agent is prepared by the following method: adding cyanuric chloride and triethylamine into tetrahydrofuran, wherein the mass ratio of the cyanuric chloride to the triethylamine to the tetrahydrofuran is (1-5) to (30-50), and stirring at the room temperature for 10-30min at the stirring speed of 100-500 rpm; then adding a tetrahydrofuran solution of quaternary ammonium salt at the speed of 5-15 mL/h, continuing to react for 0.5-2h at room temperature after the addition, wherein the stirring speed is 100-500rpm, and the mass ratio of the tetrahydrofuran solution of quaternary ammonium salt to cyanuric chloride is (10-30) to (1-5); after the reaction was completed, the solvent was removed under reduced pressure in vacuo.
Preferably, the tetrahydrofuran solution of the quaternary ammonium salt is a mixture of the quaternary ammonium salt and tetrahydrofuran according to a mass ratio of (1-5) to (15-20).
Preferably, the quaternary ammonium salt is any one of chlorinated-2-hydroxy-3- (trimethylamino) propyl polyethylene oxide cellulose ether, dodecyl methyl dihydroxyethyl ammonium bromide and (3-hydroxyphenyl) trimethyl ammonium chloride; further preferably, the quaternary ammonium salt is dodecyl methyl dihydroxyethyl ammonium bromide.
The modified quaternary ammonium salt antibacterial agent provided by the invention can be chemically bonded with-OH and-NH on the surface of the textile fabric in a covalent grafting manner and the like2And the active groups are subjected to chemical reaction, so that the antibacterial property of the fabric is improved, and the washing resistance is also improved. However, the inventor finds that although the modified quaternary ammonium salt antibacterial agent improves the antibacterial performance of the fabric, the modified quaternary ammonium salt antibacterial agent also causes a new problem that the moisture permeability of the fabric is poor. Therefore, in order to enable the moisture permeability of the fabric not to be affected, the inventor takes the modified quaternary ammonium salt antibacterial agent as a raw material to prepare the moisture-absorbing antibacterial composite finishing agent.
The moisture-absorbing antibacterial composite finishing agent comprises the following raw materials: modified nano silicon dioxide, sodium lignosulfonate, a modified quaternary ammonium salt antibacterial agent, sodium citrate and water; the sodium lignosulfonate is used as a dispersing agent, so that active ingredients in a finishing agent system can be better dispersed, and the effect of each active ingredient can be optimal; the sodium citrate is used as a stabilizer, so that all active ingredients in the whole system can be more stable, and a better effect can be exerted; the modified nano-silica serves as a provider of moisture absorption performance, the moisture absorption performance of a finishing agent system can be better, the nano-silica is modified by a modifier 2- (4-chlorosulfonated phenyl) ethyltrimethoxysilane or 6-azidosulfonyl hexyltriethoxysilane, a large number of sulfonic acid groups are introduced to the surface of nanoparticles, and the hydrophilicity of the nano-silica is improved. Furthermore, the modifier 2- (4-chlorosulfonyl phenyl) ethyltrimethoxysilane and 6-azido sulfonyl hexyl triethoxysilane are compounded to realize synergistic interaction, so that the moisture absorption performance of the moisture absorption antibacterial composite finishing agent is further improved; the reason is probably that two modifiers with different structures are grafted to the surface of the nano silicon dioxide in a covalent bonding mode respectively, branched chain structures can complement each other, so that steric hindrance is reduced, the surface of the modified nano silicon dioxide has more sulfonic groups, and meanwhile, the modified nano silicon dioxide has better dispersibility and compatibility, so that the moisture absorption performance of the moisture absorption antibacterial composite finishing agent is further improved.
Preferably, the finishing agent is a moisture absorption antibacterial composite finishing agent; the moisture-absorbing antibacterial composite finishing agent is prepared by the following method:
(1) adding nano silicon dioxide into tetrahydrofuran, and performing ultrasonic treatment for 20-60min, wherein the ultrasonic power is 500-1500W, the ultrasonic frequency is 20-50kHz, and the mass ratio of the nano silicon dioxide to the tetrahydrofuran is (1-30): 150; adding a tetrahydrofuran solution of a modifier at the speed of 5-35mL \ h, refluxing and stirring at 60-80 ℃ for 20-30h, wherein the mass ratio of the tetrahydrofuran solution of the modifier to the nano silicon dioxide is (10-30) to 1, cooling to room temperature, filtering, washing with tetrahydrofuran, and drying to obtain modified nano silicon dioxide; the tetrahydrofuran solution of the modifier is a mixture of the modifier and tetrahydrofuran according to a mass ratio of 1 (10-30);
(2) adding modified nano-silica, sodium lignosulfonate, a modified quaternary ammonium salt antibacterial agent and sodium citrate into water, stirring at the temperature of 60-80 ℃ for 10-60min at the stirring speed of 300-600rpm, wherein the mass ratio of the modified nano-silica, the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent, the sodium citrate and the water is (1-10), (0.1-1), (0.5-5), (0.1-1), (50-100), and obtaining the moisture-absorbing antibacterial composite finishing agent.
Preferably, the modifier is at least one of N-perfluorooctanesulfonyltriethoxysilane, 2- (4-chlorosulfonylphenyl) ethyltrimethoxysilane, 6-azidosulfonylhexyltriethoxysilane and (N-perfluorooctylsulfonyl) -aminopropyltrimethoxysilane;
further preferably, the modifier is a mixture of 2- (4-chlorosulfonylphenyl) ethyltrimethoxysilane and 6-azidosulfonylhexyltriethoxysilane according to the mass ratio of 3 (1-3).
The invention also provides an antibacterial fabric prepared by the method.
The invention has the beneficial effects that: the antibacterial fabric prepared by the invention has good antibacterial performance and washing resistance, and does not have negative influence on the mechanical property, moisture permeability, air permeability, color and other wearability of the fabric. The modified quaternary ammonium salt antibacterial agent provided by the invention can be chemically bonded with-OH and-NH on the surface of the textile fabric in a covalent grafting manner and the like2And the active groups are subjected to chemical reaction, so that the antibacterial property of the fabric is improved, and the washing resistance is also improved.
The moisture-absorbing antibacterial composite finishing agent is prepared by taking modified nano-silica, sodium lignosulfonate, a modified quaternary ammonium salt antibacterial agent and sodium citrate as raw materials, wherein the sodium lignosulfonate is taken as a dispersing agent, so that active ingredients in a finishing agent system can be better dispersed, and the effect of each active ingredient can be optimal; the modified quaternary ammonium salt antibacterial agent is used as a high-efficiency antibacterial agent, and the excellent antibacterial activity and antibacterial water-washing resistance of a finishing agent system are improved; the sodium citrate is used as a stabilizer, so that all active ingredients in the whole system can be more stable, and a better effect can be exerted; the modified nano-silica serves as a provider of moisture absorption performance, the moisture absorption performance of a finishing agent system can be better, the nano-silica is modified by a modifier 2- (4-chlorosulfonated phenyl) ethyltrimethoxysilane or 6-azidosulfonyl hexyltriethoxysilane, a large number of sulfonic acid groups are introduced to the surface of nanoparticles, and the hydrophilicity of the nano-silica is improved.
Detailed Description
The above summary of the present invention is described in further detail below with reference to specific embodiments, but it should not be understood that the scope of the above subject matter of the present invention is limited to the following examples.
Introduction of some raw materials in this application:
cotton-polyester fabric, gram weight: 160g/m2The components and contents are as follows: 82% cotton, 18% polyester, available from Wujiang Keren and Shunyang textile Co., Ltd.
Chlorinated-2-hydroxy-3- (trimethylamino) propyl polyethylene oxide cellulose ether, CAS No.: 68610-92-4, purity: 99% from Shanghai Baomann Biotech, Inc.
Dodecyl methyl dihydroxy ethyl ammonium bromide, CAS No.: 57122-49-3, purity: 98% from Shanghai Bigdi pharmaceutical technology, Inc.
Cyanuric chloride, CAS No.: 108-77-0, purity: 99% from the Nezel Biotech limited.
Triethylamine, CAS number: 121-44-8, purity: 99.9% from Jinan Renyuan chemical Co.
2- (4-chlorosulfonylphenyl) ethyltrimethoxysilane, CAS No.: 126519-89-9, purity: 97% of the total weight of the product obtained from Shanghai Chuqing New Material science and technology Co.
Nanosilica, No. M600, aqueous, particle size: 10-20nm, purity: 99.8% from Guangzhou Macrowu materials science and technology, Inc.
Sodium lignosulfonate, CAS No.: 8061-51-6, purity: 99% of the total weight of the composition, purchased from Wuhanxin Confucian chemical Co.
Sodium citrate, CAS No.: 68-04-2, purity: 99% from Wuhanyitai science and technology Limited.
6-azidosulfonylhexyltriethoxysilane, CAS No.: 96550-26-4, purity: 98 percent of the total saponin is purchased from Shanghai Tuoqing chemical Co.
In the application, the same raw material is the same source of raw material.
Comparative example 1
The preparation method of the antibacterial fabric comprises the following steps: soaking the fabric in an antibacterial finishing agent at 50 ℃ for 60min, wherein the mass ratio of the antibacterial finishing agent to the fabric is 25: 1; two-dipping and two-rolling, wherein the rolling residual rate is 95 percent; pre-baking at 55 ℃ for 2min, continuously baking at 87 ℃ for 28min, washing with deionized water for 2 times, and naturally drying to obtain the antibacterial fabric. The fabric is a cotton-polyester fabric.
The antibacterial finishing agent is prepared by the following method:
adding sodium lignin sulfonate, dodecyl methyl dihydroxy ethyl ammonium bromide and sodium citrate into deionized water, stirring for 50min at 72 ℃ and the stirring speed of 500rpm, wherein the mass ratio of the sodium lignin sulfonate, the dodecyl methyl dihydroxy ethyl ammonium bromide, the sodium citrate to the deionized water is 0.5:1:0.5:98, and thus obtaining the antibacterial finishing agent.
An antibacterial fabric is prepared by the method.
Example 1
The preparation method of the antibacterial fabric comprises the following steps: soaking the fabric in an antibacterial finishing agent at 50 ℃ for 60min, wherein the mass ratio of the antibacterial finishing agent to the fabric is 25: 1; two-dipping and two-rolling, wherein the rolling residual rate is 95 percent; pre-baking at 55 ℃ for 2min, continuously baking at 87 ℃ for 28min, washing with deionized water for 2 times, and naturally drying to obtain the antibacterial fabric. The fabric is a cotton-polyester fabric.
The antibacterial finishing agent is prepared by the following method:
adding sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent and sodium citrate into deionized water, stirring at 72 ℃ for 50min at a stirring speed of 500rpm, wherein the mass ratio of the sodium lignosulfonate to the modified quaternary ammonium salt antibacterial agent to the sodium citrate to the deionized water is 0.5:1:0.5:98, and thus obtaining the antibacterial finishing agent.
The modified quaternary ammonium salt antibacterial agent is prepared by the following method: adding cyanuric chloride and triethylamine into tetrahydrofuran, wherein the mass ratio of the cyanuric chloride to the triethylamine to the tetrahydrofuran is 2:2:36, and stirring at the room temperature for 20min at the stirring speed of 300 rpm; adding a tetrahydrofuran solution of quaternary ammonium salt at the speed of 12mL \ h, continuing to react for 1h at room temperature after the addition, wherein the stirring speed is 300rpm, and the mass ratio of the tetrahydrofuran solution of quaternary ammonium salt to cyanuric chloride is 22: 2; the reaction was monitored by TLC and after completion of the reaction, the solvent was removed under reduced pressure in vacuo to give the product. The tetrahydrofuran solution of the quaternary ammonium salt is a mixture of the quaternary ammonium salt and tetrahydrofuran according to the mass ratio of 3.5: 18.5; the quaternary ammonium salt is chlorinated-2-hydroxy-3- (trimethylamino) propyl polyethylene oxide cellulose ether.
An antibacterial fabric is prepared by the method.
Example 2
The preparation method of the antibacterial fabric comprises the following steps: soaking the fabric in an antibacterial finishing agent at 50 ℃ for 60min, wherein the mass ratio of the antibacterial finishing agent to the fabric is 25: 1; two-dipping and two-rolling, wherein the rolling residual rate is 95 percent; pre-baking at 55 ℃ for 2min, continuously baking at 87 ℃ for 28min, washing with deionized water for 2 times, and naturally drying to obtain the antibacterial fabric. The fabric is a cotton-polyester fabric.
The antibacterial finishing agent is prepared by the following method:
adding sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent and sodium citrate into deionized water, stirring at 72 ℃ for 50min at a stirring speed of 500rpm, wherein the mass ratio of the sodium lignosulfonate to the modified quaternary ammonium salt antibacterial agent to the sodium citrate to the deionized water is 0.5:1:0.5:98, and thus obtaining the antibacterial finishing agent.
The modified quaternary ammonium salt antibacterial agent is prepared by the following method: adding cyanuric chloride and triethylamine into tetrahydrofuran, wherein the mass ratio of the cyanuric chloride to the triethylamine to the tetrahydrofuran is 2:2:36, and stirring at the room temperature for 20min at the stirring speed of 300 rpm; adding a tetrahydrofuran solution of quaternary ammonium salt at the speed of 12mL \ h, continuing to react for 1h at room temperature after the addition, wherein the stirring speed is 300rpm, and the mass ratio of the tetrahydrofuran solution of quaternary ammonium salt to cyanuric chloride is 22: 2; the reaction was monitored by TLC and after completion of the reaction, the solvent was removed under reduced pressure in vacuo to give the product. The tetrahydrofuran solution of the quaternary ammonium salt is a mixture of the quaternary ammonium salt and tetrahydrofuran according to the mass ratio of 3.5: 18.5; the quaternary ammonium salt is dodecyl methyl dihydroxyethyl ammonium bromide.
An antibacterial fabric is prepared by the method.
Example 3
The preparation method of the antibacterial fabric comprises the following steps: soaking the fabric in a moisture-absorbing antibacterial composite finishing agent at 50 ℃ for 60min, wherein the mass ratio of the moisture-absorbing antibacterial composite finishing agent to the fabric is 25: 1; two-dipping and two-rolling, wherein the rolling residual rate is 95 percent; pre-baking at 55 ℃ for 2min, continuously baking at 87 ℃ for 28min, washing with deionized water for 2 times, and naturally drying to obtain the antibacterial fabric. The fabric is a cotton-polyester fabric.
The moisture-absorbing antibacterial composite finishing agent is prepared by the following method:
adding nano silicon dioxide, sodium lignosulfonate, a modified quaternary ammonium salt antibacterial agent and sodium citrate into deionized water, stirring for 50min at 72 ℃ and at the stirring speed of 500rpm, wherein the mass ratio of the nano silicon dioxide, the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent, the sodium citrate to the deionized water is 8:0.5:1:0.5:90, and thus obtaining the moisture-absorbing antibacterial composite finishing agent.
The modified quaternary ammonium salt antibacterial agent is prepared by the following method: adding cyanuric chloride and triethylamine into tetrahydrofuran, wherein the mass ratio of the cyanuric chloride to the triethylamine to the tetrahydrofuran is 2:2:36, and stirring at the room temperature for 20min at the stirring speed of 300 rpm; adding a tetrahydrofuran solution of quaternary ammonium salt at the speed of 12mL \ h, continuing to react for 1h at room temperature after the addition, wherein the stirring speed is 300rpm, and the mass ratio of the tetrahydrofuran solution of quaternary ammonium salt to cyanuric chloride is 22: 2; the reaction was monitored by TLC and after completion of the reaction, the solvent was removed under reduced pressure in vacuo to give the product. The tetrahydrofuran solution of the quaternary ammonium salt is a mixture of the quaternary ammonium salt and tetrahydrofuran according to the mass ratio of 3.5: 18.5; the quaternary ammonium salt is dodecyl methyl dihydroxyethyl ammonium bromide.
An antibacterial fabric is prepared by the method.
Example 4
The preparation method of the antibacterial fabric comprises the following steps: soaking the fabric in a moisture-absorbing antibacterial composite finishing agent at 50 ℃ for 60min, wherein the mass ratio of the moisture-absorbing antibacterial composite finishing agent to the fabric is 25: 1; two-dipping and two-rolling, wherein the rolling residual rate is 95 percent; pre-baking at 55 ℃ for 2min, continuously baking at 87 ℃ for 28min, washing with deionized water for 2 times, and naturally drying to obtain the antibacterial fabric. The fabric is a cotton-polyester fabric.
The moisture-absorbing antibacterial composite finishing agent is prepared by the following method:
(1) adding nano silicon dioxide into tetrahydrofuran, and carrying out ultrasonic treatment for 30min, wherein the ultrasonic power is 1000W, the ultrasonic frequency is 30kHz, and the mass ratio of the nano silicon dioxide to the tetrahydrofuran is 1: 150; adding a tetrahydrofuran solution of a modifier at the rate of 20mL \ h, refluxing and stirring at 65 ℃ for 25h, wherein the mass ratio of the tetrahydrofuran solution of the modifier to the nano-silica is 15:1, cooling to room temperature, filtering, washing with tetrahydrofuran for 2 times, and drying to obtain modified nano-silica; the tetrahydrofuran solution of the modifier is a mixture of the modifier and tetrahydrofuran in a mass ratio of 1: 14; the modifier is 2- (4-chlorosulfonic acid phenyl) ethyl trimethoxy silane;
(2) adding the modified nano-silica, the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent and the sodium citrate into deionized water, stirring for 50min at 72 ℃ and at a stirring speed of 500rpm, wherein the mass ratio of the modified nano-silica, the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent, the sodium citrate to the deionized water is 8:0.5:1:0.5:90, and thus obtaining the moisture-absorbing antibacterial composite finishing agent.
The modified quaternary ammonium salt antibacterial agent is prepared by the following method: adding cyanuric chloride and triethylamine into tetrahydrofuran, wherein the mass ratio of the cyanuric chloride to the triethylamine to the tetrahydrofuran is 2:2:36, and stirring at the room temperature for 20min at the stirring speed of 300 rpm; adding a tetrahydrofuran solution of quaternary ammonium salt at the speed of 12mL \ h, continuing to react for 1h at room temperature after the addition, wherein the stirring speed is 300rpm, and the mass ratio of the tetrahydrofuran solution of quaternary ammonium salt to cyanuric chloride is 22: 2; the reaction was monitored by TLC and after completion of the reaction, the solvent was removed under reduced pressure in vacuo to give the product. The tetrahydrofuran solution of the quaternary ammonium salt is a mixture of the quaternary ammonium salt and tetrahydrofuran according to the mass ratio of 3.5: 18.5; the quaternary ammonium salt is dodecyl methyl dihydroxyethyl ammonium bromide.
An antibacterial fabric is prepared by the method.
Example 5
The preparation method of the antibacterial fabric comprises the following steps: soaking the fabric in a moisture-absorbing antibacterial composite finishing agent at 50 ℃ for 60min, wherein the mass ratio of the moisture-absorbing antibacterial composite finishing agent to the fabric is 25: 1; two-dipping and two-rolling, wherein the rolling residual rate is 95 percent; pre-baking at 55 ℃ for 2min, continuously baking at 87 ℃ for 28min, washing with deionized water for 2 times, and naturally drying to obtain the antibacterial fabric. The fabric is a cotton-polyester fabric.
The moisture-absorbing antibacterial composite finishing agent is prepared by the following method:
(1) adding nano silicon dioxide into tetrahydrofuran, and carrying out ultrasonic treatment for 30min, wherein the ultrasonic power is 1000W, the ultrasonic frequency is 30kHz, and the mass ratio of the nano silicon dioxide to the tetrahydrofuran is 1: 150; adding a tetrahydrofuran solution of a modifier at the rate of 20mL \ h, refluxing and stirring at 65 ℃ for 25h, wherein the mass ratio of the tetrahydrofuran solution of the modifier to the nano-silica is 15:1, cooling to room temperature, filtering, washing with tetrahydrofuran for 2 times, and drying to obtain modified nano-silica; the tetrahydrofuran solution of the modifier is a mixture of the modifier and tetrahydrofuran in a mass ratio of 1: 14; the modifier is 6-azido sulfonyl hexyl triethoxysilane;
(2) adding the modified nano-silica, the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent and the sodium citrate into deionized water, stirring for 50min at 72 ℃ and at a stirring speed of 500rpm, wherein the mass ratio of the modified nano-silica, the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent, the sodium citrate to the deionized water is 8:0.5:1:0.5:90, and thus obtaining the moisture-absorbing antibacterial composite finishing agent.
The modified quaternary ammonium salt antibacterial agent is prepared by the following method: adding cyanuric chloride and triethylamine into tetrahydrofuran, wherein the mass ratio of the cyanuric chloride to the triethylamine to the tetrahydrofuran is 2:2:36, and stirring at the room temperature for 20min at the stirring speed of 300 rpm; adding a tetrahydrofuran solution of quaternary ammonium salt at the speed of 12mL \ h, continuing to react for 1h at room temperature after the addition, wherein the stirring speed is 300rpm, and the mass ratio of the tetrahydrofuran solution of quaternary ammonium salt to cyanuric chloride is 22: 2; the reaction was monitored by TLC and after completion of the reaction, the solvent was removed under reduced pressure in vacuo to give the product. The tetrahydrofuran solution of the quaternary ammonium salt is a mixture of the quaternary ammonium salt and tetrahydrofuran according to the mass ratio of 3.5: 18.5; the quaternary ammonium salt is dodecyl methyl dihydroxyethyl ammonium bromide.
An antibacterial fabric is prepared by the method.
Example 6
The preparation method of the antibacterial fabric comprises the following steps: soaking the fabric in a moisture-absorbing antibacterial composite finishing agent at 50 ℃ for 60min, wherein the mass ratio of the moisture-absorbing antibacterial composite finishing agent to the fabric is 25: 1; two-dipping and two-rolling, wherein the rolling residual rate is 95 percent; pre-baking at 55 ℃ for 2min, continuously baking at 87 ℃ for 28min, washing with deionized water for 2 times, and naturally drying to obtain the antibacterial fabric. The fabric is a cotton-polyester fabric.
The moisture-absorbing antibacterial composite finishing agent is prepared by the following method:
(1) adding nano silicon dioxide into tetrahydrofuran, and carrying out ultrasonic treatment for 30min, wherein the ultrasonic power is 1000W, the ultrasonic frequency is 30kHz, and the mass ratio of the nano silicon dioxide to the tetrahydrofuran is 1: 150; adding a tetrahydrofuran solution of a modifier at the rate of 20mL \ h, refluxing and stirring at 65 ℃ for 25h, wherein the mass ratio of the tetrahydrofuran solution of the modifier to the nano-silica is 15:1, cooling to room temperature, filtering, washing with tetrahydrofuran for 2 times, and drying to obtain modified nano-silica; the tetrahydrofuran solution of the modifier is a mixture of the modifier and tetrahydrofuran in a mass ratio of 1: 14; the modifier is a mixture of 2- (4-chlorosulfonyl phenyl) ethyltrimethoxysilane and 6-azido sulfonyl hexyl triethoxysilane according to the mass ratio of 3: 2;
(2) adding the modified nano-silica, the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent and the sodium citrate into deionized water, stirring for 50min at 72 ℃ and at a stirring speed of 500rpm, wherein the mass ratio of the modified nano-silica, the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent, the sodium citrate to the deionized water is 8:0.5:1:0.5:90, and thus obtaining the moisture-absorbing antibacterial composite finishing agent.
The modified quaternary ammonium salt antibacterial agent is prepared by the following method: adding cyanuric chloride and triethylamine into tetrahydrofuran, wherein the mass ratio of the cyanuric chloride to the triethylamine to the tetrahydrofuran is 2:2:36, and stirring at the room temperature for 20min at the stirring speed of 300 rpm; adding a tetrahydrofuran solution of quaternary ammonium salt at the speed of 12mL \ h, continuing to react for 1h at room temperature after the addition, wherein the stirring speed is 300rpm, and the mass ratio of the tetrahydrofuran solution of quaternary ammonium salt to cyanuric chloride is 22: 2; the reaction was monitored by TLC and after completion of the reaction, the solvent was removed under reduced pressure in vacuo to give the product. The tetrahydrofuran solution of the quaternary ammonium salt is a mixture of the quaternary ammonium salt and tetrahydrofuran according to the mass ratio of 3.5: 18.5; the quaternary ammonium salt is dodecyl methyl dihydroxyethyl ammonium bromide.
An antibacterial fabric is prepared by the method.
Test example 1
And (3) testing antibacterial performance: according to the national standard GB/T20944.3-2008, evaluation part 3 of antibacterial performance of textiles: vibration method the antibacterial fabrics of the examples and comparative examples were tested. The tested bacteria are: staphylococcus aureus (ATCC6538), escherichia coli (ATC C11229); the antibacterial rate was measured after washing times 0 and 50 times, respectively, and 5 groups were paralleled and averaged.
TABLE 1 antibacterial Property test Table
From the example 2 and the comparative example 1, the modified quaternary ammonium salt antibacterial agent has obviously improved antibacterial performance, and particularly has obviously improved antibacterial performance of water washing resistance. The modified quaternary ammonium salt antibacterial agent provided by the invention can be chemically bonded with-OH and-NH on the surface of the textile fabric in a covalent grafting manner and the like2And the active groups are subjected to chemical reaction, so that the antibacterial property of the fabric is improved, and the washing resistance is also improved.
Test example 2
Moisture permeability test: according to the national standard GB/T12704.1-2009 part 1 of textile fabric moisture permeability test method: wet absorption method the antibacterial fabrics of the examples and comparative examples were tested. Setting test conditions of the test box: temperature (38 ℃), relative humidity (90%), air flow speed (0.3-0.5 m/s); parallel to 5 groups, average. The control group refers to cotton-polyester fabric that was not treated with a finish.
TABLE 2 moisture permeability test chart
| Moisture permeability (g/(m)2·24h)) | |
| Control group | 6208.25 |
| Example 2 | 5875.16 |
| Example 3 | 6016.51 |
| Example 4 | 6120.03 |
| Example 5 | 6167.50 |
| Example 6 | 6239.98 |
As can be seen from table 2, the moisture-absorbing antibacterial composite finishing agent of the present invention can improve the antibacterial property of the fabric and ensure that the moisture permeability of the fabric is not negatively affected. The moisture-absorbing antibacterial composite finishing agent comprises the following raw materials: modified nano silicon dioxide, sodium lignosulfonate, a modified quaternary ammonium salt antibacterial agent, sodium citrate and deionized water; the sodium lignosulfonate is used as a dispersing agent, so that active ingredients in a finishing agent system can be better dispersed, and the effect of each active ingredient can be optimal; the sodium citrate is used as a stabilizer, so that all active ingredients in the whole system can be more stable, and a better effect can be exerted; the modified nano-silica serves as a provider of moisture absorption performance, the moisture absorption performance of a finishing agent system can be better, the nano-silica is modified by a modifier 2- (4-chlorosulfonated phenyl) ethyltrimethoxysilane or 6-azidosulfonyl hexyltriethoxysilane, a large number of sulfonic acid groups are introduced to the surface of nanoparticles, and the hydrophilicity of the nano-silica is improved. Further comparing examples 4-6, it can be seen that the moisture absorption performance of the moisture absorption antibacterial composite finishing agent is further improved by using the modifier 2- (4-chlorosulfonato phenyl) ethyltrimethoxysilane and 6-azidosulfonyl hexyltriethoxysilane for compounding to realize synergistic interaction; the reason is probably that two modifiers with different structures are grafted to the surface of the nano silicon dioxide in a covalent bonding mode respectively, branched chain structures can complement each other, so that steric hindrance is reduced, the surface of the modified nano silicon dioxide has more sulfonic groups, and meanwhile, the modified nano silicon dioxide has better dispersibility and compatibility, so that the moisture absorption performance of the moisture absorption antibacterial composite finishing agent is further improved.
Test example 3
And (3) testing the air permeability: the antibacterial fabrics of the examples and comparative examples were tested according to the national standard GB/T5453-1997 determination of air permeability of textile fabrics. Test area 20cm2The pressure drop is 100 Pa; parallel 10 groups, take the average. The control group refers to cotton-polyester fabric that was not treated with a finish.
TABLE 3 air permeability test chart
| Air permeability (mm/s) | |
| Control group | 213.3 |
| Example 2 | 205.0 |
| Example 3 | 207.5 |
| Example 4 | 209.6 |
| Example 5 | 210.3 |
| Example 6 | 212.9 |
The foregoing is considered as illustrative and not restrictive in character, and that all equivalent and simple variations on the principles taught herein are included within the scope of the present invention; various modifications, additions and substitutions for the specific embodiments described may be made by those skilled in the art without departing from the scope of the invention as defined in the accompanying claims.
Claims (10)
1. The preparation method of the antibacterial fabric is characterized by comprising the following steps: and (3) soaking the fabric in the finishing agent, soaking for two times and rolling for two times, baking, washing and drying.
2. The method for preparing the antibacterial fabric according to claim 1, characterized by comprising the following steps: soaking the fabric in a moisture-absorbing and antibacterial composite finishing agent at 40-60 ℃ for 50-100min, wherein the mass ratio of the finishing agent to the fabric is (10-60) to 1; two-dipping and two-rolling, wherein the rolling residual rate is 70-100%; pre-baking at 40-60 deg.C for 1-5min, baking at 80-120 deg.C for 20-50min, washing with water, and drying.
3. The method for preparing an antibacterial fabric according to claim 2, wherein the finishing agent is an antibacterial finishing agent or a moisture-absorbing antibacterial composite finishing agent.
4. The method for preparing the antibacterial fabric according to claim 3, wherein the antibacterial finishing agent is prepared by the following method: adding sodium lignosulfonate, a modified quaternary ammonium salt antibacterial agent and sodium citrate into water, and stirring at 60-80 ℃ for 10-60min, wherein the mass ratio of the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent, the sodium citrate and the water is (0.1-1): 0.5-5): 0.1-1): 50-100, so as to obtain the antibacterial finishing agent.
5. The method for preparing the antibacterial fabric according to claim 3, wherein the moisture-absorbing antibacterial composite finishing agent is prepared by the following method:
(1) adding nano silicon dioxide into tetrahydrofuran, and performing ultrasonic treatment for 20-60min, wherein the ultrasonic power is 500-1500W, the ultrasonic frequency is 20-50kHz, and the mass ratio of the nano silicon dioxide to the tetrahydrofuran is (1-30): 150; adding a tetrahydrofuran solution of a modifier at the speed of 5-35mL \ h, refluxing and stirring at 60-80 ℃ for 20-30h, wherein the mass ratio of the tetrahydrofuran solution of the modifier to the nano silicon dioxide is (10-30) to 1, cooling to room temperature, filtering, washing with tetrahydrofuran, and drying to obtain modified nano silicon dioxide; the tetrahydrofuran solution of the modifier is a mixture of the modifier and tetrahydrofuran according to a mass ratio of 1 (10-30);
(2) adding modified nano-silica, sodium lignosulfonate, a modified quaternary ammonium salt antibacterial agent and sodium citrate into water, stirring at the temperature of 60-80 ℃ for 10-60min at the stirring speed of 300-600rpm, wherein the mass ratio of the modified nano-silica, the sodium lignosulfonate, the modified quaternary ammonium salt antibacterial agent, the sodium citrate and the water is (1-10), (0.1-1), (0.5-5), (0.1-1), (50-100), and obtaining the moisture-absorbing antibacterial composite finishing agent.
6. The method for preparing an antibacterial fabric according to claim 5, wherein the modifier is at least one of N-perfluorooctanesulfonyltriethoxysilane, 2- (4-chlorosulfonylphenyl) ethyltrimethoxysilane, 6-azidosulfonylhexyltriethoxysilane, and (N-perfluorooctylsulfonyl) -aminopropyltrimethoxysilane.
7. The method for preparing the antibacterial fabric according to claim 4 or 5, wherein the modified quaternary ammonium salt antibacterial agent is prepared by the following method: adding cyanuric chloride and triethylamine into tetrahydrofuran, wherein the mass ratio of the cyanuric chloride to the triethylamine to the tetrahydrofuran is (1-5) to (30-50), and stirring at the room temperature for 10-30min at the stirring speed of 100-500 rpm; then adding a tetrahydrofuran solution of quaternary ammonium salt at the speed of 5-15 mL/h, continuing to react for 0.5-2h at room temperature after the addition, wherein the stirring speed is 100-500rpm, and the mass ratio of the tetrahydrofuran solution of quaternary ammonium salt to cyanuric chloride is (10-30) to (1-5); after the reaction is finished, removing the solvent under vacuum reduced pressure; the tetrahydrofuran solution of the quaternary ammonium salt is a mixture of the quaternary ammonium salt and tetrahydrofuran according to the mass ratio of (1-5) to (15-20).
8. The method for preparing an antibacterial fabric according to claim 7, wherein the quaternary ammonium salt is any one of chlorinated-2-hydroxy-3- (trimethylamino) propyl polyethylene oxide cellulose ether, dodecyl methyl dihydroxyethyl ammonium bromide and (3-hydroxyphenyl) trimethyl ammonium chloride.
9. The method for preparing the antibacterial fabric according to claim 2, wherein the fabric is any one of a pure cotton fabric, a polyester fabric, a polypropylene fabric, a bamboo fiber fabric, a viscose fiber fabric, a cotton-polyester fabric, a wool fabric and a nylon fabric.
10. An antibacterial fabric, characterized by being prepared by the method of any one of claims 1 to 9.
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| CN112144278A (en) * | 2020-10-22 | 2020-12-29 | 上海婉静纺织科技有限公司 | Antibacterial fabric |
| CN112981956A (en) * | 2021-02-19 | 2021-06-18 | 张霞 | Moisture-absorbing breathable jean fabric |
| CN113152086A (en) * | 2021-02-19 | 2021-07-23 | 刘利红 | Antibacterial moisture-absorption breathable fabric |
| CN113605093A (en) * | 2021-08-03 | 2021-11-05 | 常州崇高纳米材料有限公司 | Novel mixed textile fabric and preparation method thereof |
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| US4406892A (en) * | 1979-11-06 | 1983-09-27 | International Paper Company | Organosilicon quaternary ammonium antimicrobial compounds |
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| CN112144278A (en) * | 2020-10-22 | 2020-12-29 | 上海婉静纺织科技有限公司 | Antibacterial fabric |
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