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CN117107514A - Surface treatment method of high-strength fabric for children tent - Google Patents

Surface treatment method of high-strength fabric for children tent Download PDF

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Publication number
CN117107514A
CN117107514A CN202311285317.XA CN202311285317A CN117107514A CN 117107514 A CN117107514 A CN 117107514A CN 202311285317 A CN202311285317 A CN 202311285317A CN 117107514 A CN117107514 A CN 117107514A
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weight
parts
solution
surface treatment
treatment method
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赵光路
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Wuyi Luoke Leisure Products Co ltd
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Wuyi Luoke Leisure Products Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/02Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/47Oxides or hydroxides of elements of Groups 5 or 15 of the Periodic Table; Vanadates; Niobates; Tantalates; Arsenates; Antimonates; Bismuthates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188Monocarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50Treating 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
    • D06M13/51Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/327Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/333Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
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  • Plasma & Fusion (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention relates to a surface treatment method of a high-strength fabric for a children tent, and belongs to the technical field of surface treatment of fabrics. The surface treatment method of the invention utilizes bismuth vanadate to dope titanium dioxide sol, so that the doped sol is directly prepared on polyester fiber fabric, the antibacterial performance is better, and meanwhile, after the treatment of the modified silane coupling agent, the modified silane coupling agent is not easy to peel off, the strength of the fiber fabric is not affected, and after the water washing and friction test, the higher antibacterial activity is still maintained.

Description

Surface treatment method of high-strength fabric for children tent
Technical Field
The invention belongs to the technical field of fabric surface treatment, and particularly relates to a surface treatment method of a high-strength fabric for a children tent.
Background
The fabric for manufacturing the tent in the market mainly comprises silk woven by polyester (polyester fiber) yarns, and for children, because the outdoor environment is complex, a plurality of bacteria and microorganisms are arranged, and the body is easy to be injured, nano titanium dioxide is often added to ensure that the tent has antibacterial property when the tent suitable for the children is manufactured.
In the prior art, the antibacterial property of the polyester fiber is mainly realized by a mode of blending spinning and coating. The blended yarn is prepared by directly adding nano titanium dioxide into fiber slices in the form of an additive for melt spinning, and the fiber obtained by the method has good antibacterial property, but the additive has poor miscibility with polyester, so that the strength of the fiber fabric is often influenced. The coating mode is simple to operate and high in production efficiency, but the method can enable the combination of the nano titanium dioxide and the polyester fiber to be unstable and easy to peel, meanwhile, in daily life, the tent needs to be cleaned frequently, the tent needs to be folded every time when being used, and a large amount of friction exists, so that the antibacterial performance of the tent is not durable. In addition, when the nano titanium dioxide is used as a photocatalyst, the available solar energy is only about 4 percent, the particle size of the nano titanium dioxide is small, the nano titanium dioxide has a tendency of spontaneous agglomeration, the nano titanium dioxide is easy to agglomerate, and the inherent properties limit the antibacterial capability of the nano titanium dioxide to a great extent.
Therefore, there are still many places where the production of children tents with antibacterial activity using nano titanium dioxide and polyester fiber is needed to be improved, and it is urgent to provide a new surface treatment method.
Patent CN106223025a discloses an antibacterial ultraviolet-proof polyester fiber fabric and a preparation method thereof, comprising the following steps: (1) Dissolving glycerol monostearate, acrylamide, potassium thiocyanate and tetradecyl trimethyl ammonium chloride in deionized water to form an aqueous solution; (2) Adding nano titanium dioxide into the aqueous solution to obtain finishing liquid; (3) Putting the antibacterial fabric matrix into finishing liquid, soaking for two times, and carrying out liquid carrying rate of 60% -75%; (4) Pre-baking the antibacterial fabric matrix at 60-80deg.C for 15min, baking at 130-150deg.C for 1min, and shaping to obtain antibacterial fabric; (5) And uniformly coating the fluoroquaternary amine silane coupling agent on the antibacterial fabric to obtain the antibacterial and ultraviolet-proof polyester fiber fabric. The invention discloses a method for directly coating by utilizing a fluorine quaternary amine silane coupling agent, which has the problems of the defects.
Patent CN101701370a discloses an antibacterial polyester fiber, the preparation process comprises the following steps: firstly adding nano-scale titanium dioxide (TiO in the synthesis of polyester 2 ) And copper oxide (CuO) to obtain nano modified polyester, and directly passing the polyester through melt spinning processObtaining the nano modified poly (1, 2-propylene glycol terephthalate) fiber. The invention utilizes modified nano titanium dioxide to prepare polyester fiber, but belongs to the blended yarn technology, and has the problems.
Patent CN113463220a discloses an antibacterial ultraviolet-proof polyester fiber fabric and a preparation method thereof, wherein the polyester fiber fabric specifically comprises the following raw materials in parts by weight: 70-90 parts of core polyester and 17-25 parts of skin PET resin. The core polyester is mainly prepared by esterification and polycondensation of dihydric alcohol, vanillic acid and succinic anhydride, and is prepared by adding chitosan and an ultraviolet absorbent during the esterification and polycondensation; the cortex PET resin is treated by sodium carbonate and sodium dodecyl benzene sulfonate to form porous resin, and chitosan is loaded in pore canal of the porous structure. The invention discloses a melt blending spinning technology.
Patent CN108978179a discloses an antibacterial hydrophilic finishing process of plasma-chitosan-based silver-loaded nano titanium oxide of polyester fabric, which comprises the following steps: (1) alkali deweighting treatment of polyester fabric; (2) a plasma treatment method; (3) antibacterial hydrophilic finishing of the polyester fabric; (4) And (3) carrying out nano titanium oxide after-finishing on the polyester fabric by a high-temperature high-pressure-bath method. The invention discloses a finishing process of an antibacterial hydrophilic coating, namely surface treatment of the coating, which has the problems.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide the surface treatment method of the high-strength fabric for the children tent, and the surface treatment method of the invention utilizes bismuth vanadate to dope titanium dioxide sol, so that the doped sol is directly prepared on the polyester fiber fabric, the antibacterial performance is better, the peeling is not easy, the strength of the fiber fabric is not influenced, and the high antibacterial activity is still maintained after the washing and friction test.
The aim of the invention can be achieved by the following technical scheme:
the surface treatment method of the high-strength fabric for the children tent comprises the following steps of:
(1) 4-8 parts by weight of tetrabutyl titanate and 25-30 parts by weight of absolute ethyl alcohol are stirred for 20-30min and mixed to obtain a solution A;
(2) Mixing 80-100 parts by weight of deionized water, 1-1.5 parts by weight of bismuth nitrate pentahydrate and 3-4 parts by weight of concentrated nitric acid under stirring, adding 7-10 parts by weight of polyvinylpyrrolidone, and ultrasonically stirring for 30-45min to obtain a solution B;
(3) Dropwise adding a mixture consisting of 0.5-1 parts by weight of ammonium metavanadate, 80-100 parts by weight of deionized water and 0.5-0.8 part by weight of citric acid into the solution B under stirring, and reacting for 5-10 hours at 80-120 ℃ to obtain sol;
(4) Adding 80-100 parts by weight of deionized water into the sol for dilution, then adding 5-10 parts by weight of hydrochloric acid and stirring for 5-10min to obtain a solution C;
(5) Completely soaking the polyester fiber fabric in the solution C;
(6) After the soaking is finished, dropwise adding the solution A into the solution C, controlling the dropwise adding time to be 45-60min, simultaneously maintaining the temperature to be 80-100 ℃ all the time, stirring and reacting for 2-3h, taking out the polyester fiber fabric after the reaction is finished, and performing ultrasonic treatment for 15-20min;
(7) And (3) immersing the polyester fiber fabric subjected to ultrasonic treatment in a surface treatment agent for 1-2 hours, and then sequentially carrying out drying shaping, water washing and drying again to finish the treatment.
As a preferable technical scheme of the invention, the concentration of the concentrated nitric acid in the step (2) is 8-9mol/L.
As a preferable technical scheme of the invention, the power of the ultrasonic wave in the step (2) is 200-300W.
As a preferable technical scheme of the invention, the dripping speed in the step (3) is 5-10 drops/s.
As a preferable technical scheme of the invention, the concentration of the hydrochloric acid in the step (4) is 4-6mol/L.
As a preferable technical scheme of the invention, the soaking time in the step (5) is 30-60min.
As a preferable technical scheme of the invention, the power of the ultrasonic treatment in the step (6) is 600-700W.
As a preferable technical scheme of the invention, the surface treating agent in the step (7) is formed by mixing 15-25 parts by weight of modified silane coupling agent, 10-15 parts by weight of polyvinyl alcohol and 5-7 parts by weight of calcium stearate.
Further, the modified silane coupling agent is prepared by the steps of:
step a: mixing 5-7 parts by weight of KH550 silane coupling agent and 10-15 parts by weight of absolute ethyl alcohol at 25-30 ℃ for 10-15min to obtain a solution a;
step b: mixing 1-3 parts by weight of phthalic anhydride, 5-6 parts by weight of tert-butyl hydroperoxide and 20-30 parts by weight of absolute ethyl alcohol at 30-40 ℃ for 20-30min to obtain a solution b;
step c: mixing the solution a and the solution b, stirring and reacting for 8-12 hours at 30-40 ℃ under the microwave of 500-600W, distilling for 20-30min at 90-100 ℃ after the reaction is finished, and removing volatile matters to obtain the modified silane coupling agent.
As a preferable technical scheme of the invention, the temperature of the drying and shaping in the step (7) is 120-150 ℃, the time of the drying and shaping is 2-3h, the temperature of the re-drying is 70-80 ℃, and the time of the re-drying is 45-60min.
The invention has the beneficial effects that:
(1) Compared with the prior art that nano titanium dioxide particles or dispersion liquid thereof are directly used for surface treatment, the technology has better antibacterial performance, is more firmly combined with the polyester fiber fabric, can adhere a large amount of sol on the surface of the fiber fabric to form an antibacterial layer, and can be deeply infiltrated into the fiber fabric.
(2) The KH550 silane coupling agent is creatively modified and added into the surface treatment agent, so that the adhesive force between polyester fiber fabric and titanium dioxide/bismuth vanadate can be enhanced when the adhesive is acted on the doped sol of the polyester fiber fabric and the titanium dioxide/bismuth vanadate, and the adhesive force is not easy to peel, thereby improving the antibacterial durability. Meanwhile, the modified silane coupling agent can better coat the doped sol, and the compatibility of the modified silane coupling agent with polyester fiber fabric is improved.
(3) The antibacterial property of the polyester fiber fabric subjected to surface treatment is greatly improved, the strength is not reduced, and the polyester fiber fabric still maintains high antibacterial activity and lasting antibacterial property after being subjected to water washing or friction test.
(4) The surface treating agent used in the invention also adds polyvinyl alcohol to disperse the doped sol, thus preventing the doped sol from coagulating and agglomerating gel and better playing the antibacterial activity.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention for achieving the intended purpose, the following detailed description is given below with reference to the embodiments, structures, features and effects according to the present invention.
Example 1
The surface treatment method of the high-strength fabric for the children tent comprises the following steps of:
(1) 4 parts by weight of tetrabutyl titanate and 25 parts by weight of absolute ethyl alcohol are stirred and mixed for 20min to obtain a solution A;
(2) Mixing 80 parts by weight of deionized water, 1 part by weight of bismuth nitrate pentahydrate and 3 parts by weight of concentrated nitric acid with the concentration of 8mol/L, and then adding 7 parts by weight of polyvinylpyrrolidone, and stirring for 30min under 200W ultrasonic power to obtain a solution B;
(3) Dropwise adding a mixture consisting of 0.5 weight part of ammonium metavanadate, 80 weight parts of deionized water and 0.5 weight part of citric acid into the solution B under stirring, controlling the dropwise adding speed to be 5 drops/s, and reacting for 5 hours at 80 ℃ to obtain sol;
(4) Adding 80 parts by weight of deionized water into the sol for dilution, and then adding 5 parts by weight of hydrochloric acid with the concentration of 4mol/L for stirring for 5min to obtain a solution C;
(5) Completely soaking the polyester fiber fabric in the solution C for 30min;
(6) After the soaking is finished, dropwise adding the solution A into the solution C, controlling the dropwise adding time to be 45min, simultaneously maintaining the temperature at 80 ℃ all the time, stirring and reacting for 2h, taking out the polyester fiber fabric after the reaction is finished, and performing ultrasonic treatment for 15min, wherein the ultrasonic power is 600W;
(7) And (3) immersing the polyester fiber fabric subjected to ultrasonic treatment in a surface treatment agent for 1h, and then sequentially drying and shaping, washing and re-drying, wherein the temperature of the drying and shaping is 120 ℃, the time of the drying and shaping is 2h, the temperature of the re-drying is 70 ℃, and the time of the re-drying is 45min, so that the treatment is completed.
Wherein the surface treating agent is formed by mixing 15 parts by weight of modified silane coupling agent, 10 parts by weight of polyvinyl alcohol and 5 parts by weight of calcium stearate.
The modified silane coupling agent is prepared by the following steps:
step a: mixing 5 parts by weight of KH550 silane coupling agent and 10 parts by weight of absolute ethyl alcohol at 25 ℃ for 10min to obtain a solution a;
step b: mixing 1 part by weight of phthalic anhydride, 5 parts by weight of tert-butyl hydroperoxide and 20 parts by weight of absolute ethyl alcohol at 30 ℃ for 20 minutes to obtain a solution b;
step c: mixing the solution a and the solution b, stirring at 30 ℃ under 500W microwave for reaction for 8 hours, distilling at 90 ℃ for 20 minutes after the reaction is completed, and removing volatile matters to obtain the modified silane coupling agent.
Example 2
The surface treatment method of the high-strength fabric for the children tent comprises the following steps of:
(1) Stirring 8 parts by weight of tetrabutyl titanate and 30 parts by weight of absolute ethyl alcohol for 30min to mix to obtain a solution A;
(2) 100 parts by weight of deionized water, 1.5 parts by weight of bismuth nitrate pentahydrate and 4 parts by weight of concentrated nitric acid with the concentration of 9mol/L are stirred and mixed, 10 parts by weight of polyvinylpyrrolidone is then added, and stirring is carried out for 45min under the ultrasonic power of 300W, so as to obtain a solution B;
(3) Dropwise adding a mixture consisting of 1 part by weight of ammonium metavanadate, 100 parts by weight of deionized water and 0.8 part by weight of citric acid into the solution B under stirring, controlling the dropwise adding speed to be 10 drops/s, and reacting for 10 hours at 120 ℃ to obtain sol;
(4) Adding 100 parts by weight of deionized water into the sol for dilution, and then adding 10 parts by weight of hydrochloric acid with the concentration of 6mol/L for stirring for 10min to obtain a solution C;
(5) Completely soaking the polyester fiber fabric in the solution C for 60min;
(6) After the soaking is finished, dropwise adding the solution A into the solution C, wherein the dropwise adding time is controlled to be 60min, and simultaneously, the temperature is always kept at 100 ℃ for stirring reaction for 3h, after the reaction is finished, taking out the polyester fiber fabric, and performing ultrasonic treatment for 20min, wherein the ultrasonic power is 700W;
(7) And (3) immersing the polyester fiber fabric subjected to ultrasonic treatment in a surface treatment agent for 2 hours, and then sequentially drying and shaping, washing and re-drying, wherein the temperature of the drying and shaping is 150 ℃, the time of the drying and shaping is 3 hours, the temperature of the re-drying is 80 ℃, and the time of the re-drying is 60 minutes, so that the treatment is completed.
Wherein the surface treating agent is formed by mixing 25 parts by weight of modified silane coupling agent, 15 parts by weight of polyvinyl alcohol and 7 parts by weight of calcium stearate.
The modified silane coupling agent is prepared by the following steps:
step a: 7 parts by weight of KH550 silane coupling agent and 15 parts by weight of absolute ethyl alcohol are stirred for 15min and mixed at 30 ℃ to obtain a solution a;
step b: 3 parts by weight of phthalic anhydride, 6 parts by weight of tert-butyl hydroperoxide and 30 parts by weight of absolute ethyl alcohol are stirred for 30min and mixed at 40 ℃ to obtain a solution b;
step c: mixing the solution a and the solution b, stirring at 40 ℃ under 600W microwave for reaction for 12 hours, distilling at 100 ℃ for 30 minutes after the reaction is completed, and removing volatile matters to obtain the modified silane coupling agent.
Example 3
The surface treatment method of the high-strength fabric for the children tent comprises the following steps of:
(1) 7 parts by weight of tetrabutyl titanate and 27 parts by weight of absolute ethyl alcohol are stirred and mixed for 25min to obtain a solution A;
(2) 90 parts by weight of deionized water, 1.2 parts by weight of bismuth nitrate pentahydrate and 3.5 parts by weight of concentrated nitric acid with the concentration of 8.5mol/L are stirred and mixed, then 8.5 parts by weight of polyvinylpyrrolidone is added, and stirring is carried out for 40min under the ultrasonic power of 250W, so as to obtain a solution B;
(3) Dropwise adding a mixture consisting of 0.7 part by weight of ammonium metavanadate, 90 parts by weight of deionized water and 0.7 part by weight of citric acid into the solution B while stirring, controlling the dropwise adding speed to be 8 drops/s, and reacting for 7 hours at 100 ℃ to obtain sol;
(4) Adding 90 parts by weight of deionized water into the sol for dilution, and then adding 7 parts by weight of hydrochloric acid with the concentration of 5mol/L for stirring for 8min to obtain a solution C;
(5) Completely soaking the polyester fiber fabric in the solution C for 45min;
(6) After the soaking is finished, dropwise adding the solution A into the solution C, wherein the dropwise adding time is controlled to be 50min, and simultaneously, the temperature is kept at 90 ℃ all the time, stirring is carried out for 2.5h, after the reaction is finished, taking out the polyester fiber fabric, and carrying out ultrasonic treatment for 18min, wherein the ultrasonic power is 650W;
(7) And (3) immersing the polyester fiber fabric subjected to ultrasonic treatment in a surface treatment agent for 1.5 hours, and then sequentially carrying out drying and shaping, washing and re-drying, wherein the temperature of the drying and shaping is 140 ℃, the time of the drying and shaping is 2.5 hours, the temperature of the re-drying is 75 ℃, and the time of the re-drying is 50 minutes, so that the treatment is finished.
Wherein the surface treating agent is formed by mixing 20 parts by weight of modified silane coupling agent, 13 parts by weight of polyvinyl alcohol and 6 parts by weight of calcium stearate.
The modified silane coupling agent is prepared by the following steps:
step a: 6 parts by weight of KH550 silane coupling agent and 12 parts by weight of absolute ethyl alcohol are stirred at 27 ℃ for 13min and mixed to obtain a solution a;
step b: 2 parts by weight of phthalic anhydride, 5.5 parts by weight of tert-butyl hydroperoxide and 25 parts by weight of absolute ethanol are stirred at 35 ℃ for 25min and mixed to obtain a solution b;
step c: mixing the solution a and the solution b, stirring and reacting for 10 hours at 35 ℃ under 550W microwave, distilling for 25 minutes at 95 ℃ after the reaction is finished, and removing volatile matters to obtain the modified silane coupling agent.
Comparative example 1
The surface treatment method of the high-strength fabric for the children tent comprises the following steps of:
(1) 4 parts by weight of tetrabutyl titanate and 25 parts by weight of absolute ethyl alcohol are stirred and mixed for 20min to obtain a solution A;
(2) Adding 5 parts by weight of hydrochloric acid with the concentration of 4mol/L into 80 parts by weight of deionized water, and stirring for 5min to obtain a solution B;
(3) Completely soaking the polyester fiber fabric in the solution B for 30min;
(4) After the soaking is finished, dropwise adding the solution A into the solution B, wherein the dropwise adding time is controlled to be 45min, and meanwhile, the temperature is always maintained at 80 ℃ for stirring reaction for 2h, after the reaction is finished, taking out the polyester fiber fabric, and performing ultrasonic treatment for 15min, wherein the ultrasonic power is 600W;
(5) And (3) immersing the polyester fiber fabric subjected to ultrasonic treatment in a surface treatment agent for 1h, and then sequentially drying and shaping, washing and re-drying, wherein the temperature of the drying and shaping is 120 ℃, the time of the drying and shaping is 2h, the temperature of the re-drying is 70 ℃, and the time of the re-drying is 45min, so that the treatment is completed.
Wherein the surface treating agent is formed by mixing 15 parts by weight of modified silane coupling agent, 10 parts by weight of polyvinyl alcohol and 5 parts by weight of calcium stearate.
The modified silane coupling agent is prepared by the following steps:
step a: mixing 5 parts by weight of KH550 silane coupling agent and 10 parts by weight of absolute ethyl alcohol at 25 ℃ for 10min to obtain a solution a;
step b: mixing 1 part by weight of phthalic anhydride, 5 parts by weight of tert-butyl hydroperoxide and 20 parts by weight of absolute ethyl alcohol at 30 ℃ for 20 minutes to obtain a solution b;
step c: mixing the solution a and the solution b, stirring at 30 ℃ under 500W microwave for reaction for 8 hours, distilling at 90 ℃ for 20 minutes after the reaction is completed, and removing volatile matters to obtain the modified silane coupling agent.
Comparative example 2
The surface treatment method of the high-strength fabric for the children tent comprises the following steps of:
(1) 4 parts by weight of tetrabutyl titanate and 25 parts by weight of absolute ethyl alcohol are stirred and mixed for 20min to obtain a solution A;
(2) Mixing 80 parts by weight of deionized water, 1 part by weight of bismuth nitrate pentahydrate and 3 parts by weight of concentrated nitric acid with the concentration of 8mol/L, and then adding 7 parts by weight of polyvinylpyrrolidone, and stirring for 30min under 200W ultrasonic power to obtain a solution B;
(3) Dropwise adding a mixture consisting of 0.5 weight part of ammonium metavanadate, 80 weight parts of deionized water and 0.5 weight part of citric acid into the solution B under stirring, controlling the dropwise adding speed to be 5 drops/s, and reacting for 5 hours at 80 ℃ to obtain sol;
(4) Adding 80 parts by weight of deionized water into the sol for dilution, and then adding 5 parts by weight of hydrochloric acid with the concentration of 4mol/L for stirring for 5min to obtain a solution C;
(5) Completely soaking the polyester fiber fabric in the solution C for 30min;
(6) After the soaking is finished, dropwise adding the solution A into the solution C, controlling the dropwise adding time to be 45min, simultaneously maintaining the temperature at 80 ℃ all the time, stirring and reacting for 2h, taking out the polyester fiber fabric after the reaction is finished, and performing ultrasonic treatment for 15min, wherein the ultrasonic power is 600W;
(7) And (3) immersing the polyester fiber fabric subjected to ultrasonic treatment in a surface treatment agent for 1h, and then sequentially drying and shaping, washing and re-drying, wherein the temperature of the drying and shaping is 120 ℃, the time of the drying and shaping is 2h, the temperature of the re-drying is 70 ℃, and the time of the re-drying is 45min, so that the treatment is completed.
Wherein the surface treating agent is formed by mixing 15 parts by weight of KH550 silane coupling agent, 10 parts by weight of polyvinyl alcohol and 5 parts by weight of calcium stearate.
Comparative example 3
The surface treatment method of the high-strength fabric for the children tent comprises the following steps of:
(1) 4 parts by weight of tetrabutyl titanate and 25 parts by weight of absolute ethyl alcohol are stirred and mixed for 20min to obtain a solution A;
(2) Mixing 80 parts by weight of deionized water, 1 part by weight of bismuth nitrate pentahydrate and 3 parts by weight of concentrated nitric acid with the concentration of 8mol/L, and then adding 7 parts by weight of polyvinylpyrrolidone, and stirring for 30min under 200W ultrasonic power to obtain a solution B;
(3) Dropwise adding a mixture consisting of 0.5 weight part of ammonium metavanadate, 80 weight parts of deionized water and 0.5 weight part of citric acid into the solution B under stirring, controlling the dropwise adding speed to be 5 drops/s, and reacting for 5 hours at 80 ℃ to obtain sol;
(4) Adding 80 parts by weight of deionized water into the sol for dilution, and then adding 5 parts by weight of hydrochloric acid with the concentration of 4mol/L for stirring for 5min to obtain a solution C;
(5) Completely soaking the polyester fiber fabric in the solution C for 30min;
(6) After the soaking is finished, dropwise adding the solution A into the solution C, controlling the dropwise adding time to be 45min, simultaneously maintaining the temperature at 80 ℃ all the time, stirring and reacting for 2h, taking out the polyester fiber fabric after the reaction is finished, and performing ultrasonic treatment for 15min, wherein the ultrasonic power is 600W;
(7) And (3) immersing the polyester fiber fabric subjected to ultrasonic treatment in a surface treatment agent for 1h, and then sequentially drying and shaping, washing and re-drying, wherein the temperature of the drying and shaping is 120 ℃, the time of the drying and shaping is 2h, the temperature of the re-drying is 70 ℃, and the time of the re-drying is 45min, so that the treatment is completed.
Wherein the surface treating agent is formed by mixing 15 parts by weight of modified silane coupling agent and 5 parts by weight of calcium stearate.
The modified silane coupling agent is prepared by the following steps:
step a: mixing 5 parts by weight of KH550 silane coupling agent and 10 parts by weight of absolute ethyl alcohol at 25 ℃ for 10min to obtain a solution a;
step b: mixing 1 part by weight of phthalic anhydride, 5 parts by weight of tert-butyl hydroperoxide and 20 parts by weight of absolute ethyl alcohol at 30 ℃ for 20 minutes to obtain a solution b;
step c: mixing the solution a and the solution b, stirring at 30 ℃ under 500W microwave for reaction for 8 hours, distilling at 90 ℃ for 20 minutes after the reaction is completed, and removing volatile matters to obtain the modified silane coupling agent.
Test example 1
Antibacterial test:
antibacterial properties were tested using E.coli (ATCC 8099) and Staphylococcus aureus (ATCC 6538P) as representative.
(1) Coli (ATCC 8099) and Staphylococcus aureus (ATCC 6538P) were inoculated onto the NA medium, respectively, and then activated in a constant temperature incubator at 37℃for 12 hours.
(2) Placing the two activated strains into physiological saline respectively, and adjusting the concentration to 10 6 CFU/mL。
(3) Cutting the polyester fiber fabrics with the surface treated in the embodiment 1 and the comparative examples 1-3 (the sizes are 1 multiplied by 1 cm), respectively adding 10mL of PBS buffer solution, and then respectively dripping 0.2mL of PBS buffer solution with the concentration of 10 in the step (2) 6 CFU/mL bacterial liquid.
(4) A400W metal halogen lamp is used for simulating a solar light source, a photocatalysis antibacterial experiment is carried out at the normal temperature of 25 ℃, and the irradiation time is 24 hours.
(5) After the irradiation, 0.1mL of the solution was taken out from the above, diluted with 5mL of PBS buffer, uniformly spread on NA plates, incubated at 37℃for 24 hours, and finally the number of colonies was observed to obtain the sterilization rate.
TABLE 1 antibacterial Property test results of example 1 and comparative examples 1-3
E.coli sterilization rate/% Staphylococcus aureus bactericidal rate/%
Example 1 78.5 68.9
Comparative example 1 49.2 40.1
Comparative example 2 70.1 62.8
Comparative example 3 72.8 63.3
Test example 2
Intensity test:
according to the requirements of the standard GB/T14344-2008 chemical fiber filament tensile property test method, an InSTRON3367 tensile tester is adopted to test the strength of the polyester fiber fabric subjected to surface treatment in the examples 1-3, and the strength of the polyester fiber fabric is compared with that of the polyester fiber fabric which is not subjected to any treatment. The strength of the polyester fiber is between 44 and 71 cN/dtex.
TABLE 2 Strength test results for examples 1-3
Test example 3
Washing test:
the polyester fiber fabrics (cut into 5×5 cm) with the surface treated in example 1 and comparative examples 1 to 3 were washed with water and dried, respectively, and after repeating 10 times, antibacterial test was performed according to the procedure of test example 1 (except that the polyester fiber fabric in step (3) was replaced).
TABLE 3 antibacterial Property test results after 10 water washes of example 1 and comparative examples 1-3
E.coli sterilization rate/% Staphylococcus aureus bactericidal rate/%
Example 1 72.5 62.1
Comparative example 1 46.7 37.2
Comparative example 2 48.5 38.0
Comparative example 3 65.7 56.4
Test example 4
Friction test:
the polyester fiber fabrics (cut into 5X 5 cm) with the surface treated in example 1 and comparative examples 1-3 were respectively dragged back and forth for 20cm on 800 mesh sand paper under a pressure of 100g weight, and after 10 times of dragging (two times in one round), antibacterial test was performed according to the procedure in test example 1 (except that the polyester fiber fabrics in the step (3) were replaced).
TABLE 4 antibacterial property test results after 10 rubs of example 1 and comparative examples 1-3
As can be seen from the comparison results of examples 1-3, comparative examples 1-3 and test examples 1-4 above:
as is clear from comparison between example 1 and comparative example 1, the photocatalytic activity of the titanium dioxide doped with bismuth vanadate is greatly improved, i.e., the antibacterial performance is enhanced.
As is evident from a comparison of examples 1-3 and test example 2, the surface treatment method of the present invention has no effect on the strength of the polyester fiber, and still retains the inherent characteristics of high strength.
As is clear from the comparison of example 1, comparative examples 1 to 3 and test example 1, the titanium dioxide was not doped, the modified silane coupling agent was not used and the polyvinyl alcohol dispersing agent was not used, and the antibacterial performance thereof was reduced.
As is clear from the comparison of example 1, comparative examples 1 to 3 and test example 3, the antibacterial properties of the polyester fiber fabric were reduced by the water washing, but the antibacterial properties of comparative example 2, which did not use the modified silane coupling agent, were significantly reduced more rapidly.
Similarly, comparison of example 1, comparative examples 1 to 3 and test example 4 shows that after rubbing, the antibacterial property of comparative example 2 without using the modified silane coupling agent also significantly decreased more rapidly.
In conclusion, the surface treatment method disclosed by the invention has the advantages that bismuth vanadate is used for doping titanium dioxide sol, so that the doped sol is directly prepared on the polyester fiber fabric, the antibacterial performance is better, meanwhile, after the modified silane coupling agent is treated, the modified polyester fiber fabric is not easy to peel off, the strength of the fiber fabric is not influenced, and the higher antibacterial activity is still maintained after the water washing and friction test.
The present invention is not limited to the above embodiments, but is capable of modification and variation in detail, and other modifications and variations can be made by those skilled in the art without departing from the scope of the present invention.

Claims (10)

1. A surface treatment method of a high-strength fabric for a children tent is characterized by comprising the following steps: the surface treatment method comprises the following steps:
(1) 4-8 parts by weight of tetrabutyl titanate and 25-30 parts by weight of absolute ethyl alcohol are stirred for 20-30min and mixed to obtain a solution A;
(2) Mixing 80-100 parts by weight of deionized water, 1-1.5 parts by weight of bismuth nitrate pentahydrate and 3-4 parts by weight of concentrated nitric acid under stirring, adding 7-10 parts by weight of polyvinylpyrrolidone, and ultrasonically stirring for 30-45min to obtain a solution B;
(3) Dropwise adding a mixture consisting of 0.5-1 parts by weight of ammonium metavanadate, 80-100 parts by weight of deionized water and 0.5-0.8 part by weight of citric acid into the solution B under stirring, and reacting for 5-10 hours at 80-120 ℃ to obtain sol;
(4) Adding 80-100 parts by weight of deionized water into the sol for dilution, then adding 5-10 parts by weight of hydrochloric acid and stirring for 5-10min to obtain a solution C;
(5) Completely soaking the polyester fiber fabric in the solution C;
(6) After the soaking is finished, dropwise adding the solution A into the solution C, controlling the dropwise adding time to be 45-60min, simultaneously maintaining the temperature to be 80-100 ℃ all the time, stirring and reacting for 2-3h, taking out the polyester fiber fabric after the reaction is finished, and performing ultrasonic treatment for 15-20min;
(7) And (3) immersing the polyester fiber fabric subjected to ultrasonic treatment in a surface treatment agent for 1-2 hours, and then sequentially carrying out drying shaping, water washing and drying again to finish the treatment.
2. The surface treatment method of the high-strength fabric for the children tent according to claim 1, which is characterized in that: the concentration of the concentrated nitric acid in the step (2) is 8-9mol/L.
3. The surface treatment method of the high-strength fabric for the children tent according to claim 1, which is characterized in that: and (3) the power of the ultrasonic wave in the step (2) is 200-300W.
4. The surface treatment method of the high-strength fabric for the children tent according to claim 1, which is characterized in that: the dropping speed in the step (3) is 5-10 drops/s.
5. The surface treatment method of the high-strength fabric for the children tent according to claim 1, which is characterized in that: the concentration of the hydrochloric acid in the step (4) is 4-6mol/L.
6. The surface treatment method of the high-strength fabric for the children tent according to claim 1, which is characterized in that: the soaking time in the step (5) is 30-60min.
7. The surface treatment method of the high-strength fabric for the children tent according to claim 1, which is characterized in that: the power of the ultrasonic treatment in the step (6) is 600-700W.
8. The surface treatment method of the high-strength fabric for the children tent according to claim 1, which is characterized in that: the surface treating agent in the step (7) is formed by mixing 15-25 parts by weight of modified silane coupling agent, 10-15 parts by weight of polyvinyl alcohol and 5-7 parts by weight of calcium stearate.
9. The surface treatment method of the high-strength fabric for the children tent according to claim 8, wherein the surface treatment method is characterized by comprising the following steps: the modified silane coupling agent is prepared by the following steps:
step a: mixing 5-7 parts by weight of KH550 silane coupling agent and 10-15 parts by weight of absolute ethyl alcohol at 25-30 ℃ for 10-15min to obtain a solution a;
step b: mixing 1-3 parts by weight of phthalic anhydride, 5-6 parts by weight of tert-butyl hydroperoxide and 20-30 parts by weight of absolute ethyl alcohol at 30-40 ℃ for 20-30min to obtain a solution b;
step c: mixing the solution a and the solution b, stirring and reacting for 8-12 hours at 30-40 ℃ under the microwave of 500-600W, distilling for 20-30min at 90-100 ℃ after the reaction is finished, and removing volatile matters to obtain the modified silane coupling agent.
10. The surface treatment method of the high-strength fabric for the children tent according to claim 1, which is characterized in that: the temperature of the drying and shaping in the step (7) is 120-150 ℃, the time of the drying and shaping is 2-3h, the temperature of the re-drying is 70-80 ℃, and the time of the re-drying is 45-60min.
CN202311285317.XA 2023-10-07 2023-10-07 Surface treatment method of high-strength fabric for children tent Pending CN117107514A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118308884A (en) * 2024-04-19 2024-07-09 湖北鱼鹤制衣有限公司 Preparation method of antibacterial tent fabric

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN118308884A (en) * 2024-04-19 2024-07-09 湖北鱼鹤制衣有限公司 Preparation method of antibacterial tent fabric

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