Surface treatment method for high-strength fabric used in children's tents
By doping the polyester fiber fabric with bismuth vanadate titanium dioxide sol and treating it with a modified silane coupling agent, the problem of insufficiency of nanotitanium dioxide and polyester fiber is solved, achieving efficient and long-lasting antibacterial properties and photocatalytic effects.
Patent Information
- Application Number
- CN202311285317.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-07
- Publication Date
- 2025-07-25
- Estimated Expiration
- 2043-10-07
AI Technical Summary
In the prior art, the combination of nanotitanium dioxide and polyester fibers is not strong, easy to peel, has a short antibacterial performance, and is low in photocatalytic efficiency, making it difficult to meet the antibacterial needs of children's tents.
The titanium dioxide sol is doped with bismuth vanadate and treated with a modified silane coupling agent to form a doped sol, which enhances the binding force and antibacterial properties with polyester fibers, and adds polyvinyl alcohol for dispersion to prevent gel formation.
The durability and photocatalytic efficiency of antibacterial properties are improved, and the fiber fabrics still maintain high antibacterial activity after washing and friction without affecting the fiber strength.
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Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of fabric surface treatment, and particularly relates to a surface treatment method for high-strength fabrics for children's tents. Background Art
[0002] The fabrics used to make tents on the market are mainly spun silk woven from polyester (polyester fiber). For children, due to the complex outdoor environment with many bacteria and microorganisms that can easily cause harm to the body, when making tents suitable for children, nano-titanium dioxide is often added to make them antibacterial.
[0003] In current technologies, the antibacterial property of polyester fibers is mainly achieved through blending spinning and coating. Blending spinning is to directly add nano-titanium dioxide into fiber chips in the form of an additive for melt spinning. Although the fibers obtained by this method have good antibacterial properties, the compatibility between the additive and polyester is poor, which often affects the strength of the fiber fabric. The coating method, although simple in operation and high in production efficiency, makes the combination of nano-titanium dioxide and polyester fibers not firm, easy to peel off. At the same time, in daily life, the tent needs to be cleaned frequently and folded every time it is used, with a lot of friction, resulting in non-persistent antibacterial properties. In addition, when nano-titanium dioxide itself is used as a photocatalyst, only about 4% of solar energy can be utilized, and its particle size is small, with a tendency of spontaneous aggregation and easy to agglomerate into clusters. These inherent properties have greatly limited its antibacterial ability.
[0004] Therefore, there are still many areas that need to be improved in the current production of children's tents with antibacterial activity using nano-titanium dioxide and polyester fibers. It has become an urgent task to provide a new surface treatment method.
[0005] Patent CN106223025A discloses an antibacterial and anti-ultraviolet polyester fiber fabric and its preparation method, including the following steps: (1) Dissolve glycerol monostearate, acrylamide, potassium thiocyanate, and tetradecyltrimethylammonium chloride in deionized water to form an aqueous solution; (2) Add nano-titanium dioxide to the aqueous solution to obtain a finishing solution; (3) Put the antibacterial fabric substrate into the finishing solution, dip and pad twice, with a liquor ratio of 60%-75%; (4) Pre-dry the antibacterial fabric substrate at 60-80°C for 15 minutes, and then dry it at 130-150°C for 1 minute for shaping to obtain an antibacterial fabric; (5) Uniformly coat the fluorinated quaternary ammonium silane coupling agent on the antibacterial fabric to obtain an antibacterial and anti-ultraviolet polyester fiber fabric. What this invention discloses is directly coating with a fluorinated quaternary ammonium silane coupling agent, having the above-mentioned defect problems.
[0006] Patent CN101701370A discloses an antibacterial polyester fiber, and its preparation process includes the following steps: First, add nanoscale titanium dioxide (TiO2) and copper oxide (CuO) during the synthesis of polyester to obtain nanomodified polyester, and the polyester is directly made into nanomodified poly(1,2-propanediol terephthalate) fiber through the melt spinning process. Although this invention uses modified nanoscale titanium dioxide to prepare polyester fiber, it belongs to the blending spinning technology and has the above-mentioned defect problems.
[0007] Patent CN113463220A discloses an antibacterial and ultraviolet-proof polyester fiber fabric and its preparation method. The polyester fiber fabric specifically includes the following raw materials in parts by weight: 70-90 parts of core-layer polyester and 17-25 parts of cortical PET resin. The core-layer polyester is mainly prepared by the esterification and polycondensation reactions of diol, vanillic acid, and succinic anhydride, and chitosan and an ultraviolet absorber are added during the process; the cortical PET resin is treated with sodium carbonate and sodium dodecylbenzenesulfonate to form a porous structure resin, and chitosan is loaded in the pores of the porous structure. What this invention discloses is still the technology of melt blending spinning.
[0008] Patent CN108978179A discloses an antibacterial and hydrophilic finishing process of plasma-chitosan-based silver-loaded-nano titanium dioxide for polyester fabrics, including the following steps: (1) alkali weight reduction treatment of polyester fabrics; (2) plasma treatment method; (3) antibacterial and hydrophilic finishing of polyester fabrics; (4) post-finishing of nano titanium dioxide for polyester fabrics by high temperature and high pressure-bath method. What this invention discloses is the finishing process of an antibacterial and hydrophilic coating, that is, surface treatment by coating, and it has the above-mentioned defect problems. Summary of the Invention
[0009] Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a surface treatment method for a high-strength fabric for children's tents. The surface treatment method of the present invention uses bismuth vanadate to dope titanium dioxide sol, so as to directly prepare doped sol on the polyester fiber fabric, which has better antibacterial performance, is not easy to peel off, does not affect the strength of the fiber fabric, and still maintains a high antibacterial activity after washing and friction tests.
[0010] The purpose of the present invention can be achieved through the following technical solutions:
[0011] A surface treatment method for a high-strength fabric for children's tents, the surface treatment method includes the following steps:
[0012] (1) Stir and mix 4-8 parts by weight of tetrabutyl titanate and 25-30 parts by weight of absolute ethanol for 20-30 minutes to obtain solution A;
[0013] (2) Stir and mix 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, then add 7 - 10 parts by weight of polyvinylpyrrolidone, and stir ultrasonically for 30 - 45 min to obtain Solution B;
[0014] (3) While stirring, dropwise add a mixture composed of 0.5 - 1 part by weight of ammonium metavanadate, 80 - 100 parts by weight of deionized water, and 0.5 - 0.8 part by weight of citric acid to Solution B, and react at 80 - 120 °C for 5 - 10 h to obtain a sol;
[0015] (4) Dilute the sol by adding 80 - 100 parts by weight of deionized water, then add 5 - 10 parts by weight of hydrochloric acid and stir for 5 - 10 min to obtain Solution C;
[0016] (5) Completely immerse the polyester fiber fabric in Solution C;
[0017] (6) After the immersion is completed, dropwise add Solution A to Solution C, control the dropping time within 45 - 60 min, and simultaneously keep stirring and reacting at a temperature of 80 - 100 °C for 2 - 3 h. After the reaction is completed, take out the polyester fiber fabric and perform ultrasonic treatment for 15 - 20 min;
[0018] (7) Immerse the ultrasonically treated polyester fiber fabric in the surface treatment agent for 1 - 2 h, then perform drying and shaping, water washing, and then drying in sequence to complete the treatment.
[0019] As a preferred technical solution of the present invention, the concentration of the concentrated nitric acid in step (2) is 8 - 9 mol / L.
[0020] As a preferred technical solution of the present invention, the power of the ultrasonic wave in step (2) is 200 - 300 W.
[0021] As a preferred technical solution of the present invention, the dropping speed in step (3) is 5 - 10 drops / s.
[0022] As a preferred technical solution of the present invention, the concentration of the hydrochloric acid in step (4) is 4 - 6 mol / L.
[0023] As a preferred technical solution of the present invention, the immersion time in step (5) is 30 - 60 min.
[0024] As a preferred technical solution of the present invention, the power of the ultrasonic treatment in step (6) is 600 - 700 W.
[0025] As a preferred technical solution of the present invention, the surface treatment agent described in step (7) is composed of 15-25 parts by weight of a modified silane coupling agent, 10-15 parts by weight of polyvinyl alcohol, and 5-7 parts by weight of calcium stearate.
[0026] Further, the modified silane coupling agent is prepared by the following steps:
[0027] Step a: Mix 5-7 parts by weight of KH550 silane coupling agent and 10-15 parts by weight of absolute ethanol at 25-30 °C with stirring for 10-15 min to obtain solution a;
[0028] Step b: Mix 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 ethanol at 30-40 °C with stirring for 20-30 min to obtain solution b;
[0029] Step c: Mix solution a and solution b, then under microwave of 500-600 W, stir and react at 30-40 °C for 8-12 h. After the reaction is completed, distill at 90-100 °C for 20-30 min to remove volatiles, and thus obtain the modified silane coupling agent.
[0030] As a preferred technical solution of the present invention, the temperature of the drying and shaping in step (7) is 120-150 °C, the time of the drying and shaping is 2-3 h, the temperature of the re-drying is 70-80 °C, and the time of the re-drying is 45-60 min.
[0031] Advantages of the present invention:
[0032] (1) The present invention creatively uses bismuth vanadate to dope titanium dioxide sol, so as to directly prepare doped sol on the polyester fiber fabric. Compared with the prior art that directly uses nano-titanium dioxide particles or their dispersion liquid for surface treatment, the antibacterial performance of the technology of the present invention is better, and at the same time, the combination with the polyester fiber fabric is firmer. Not only can a large amount of sol adhere to the surface of the fiber fabric to form an antibacterial layer, but also it can penetrate deeper into the fiber fabric.
[0033] (2) The present invention creatively modifies the KH550 silane coupling agent and adds it to the surface treatment agent. When it acts on the polyester fiber fabric and the doped sol of titanium dioxide / bismuth vanadate, it can enhance the adhesion between them and is not easy to peel off, thereby improving the antibacterial persistence. At the same time, the modified silane coupling agent can better coat the doped sol and improve its compatibility with the polyester fiber fabric.
[0034] (3) After the polyester fiber fabric is surface-treated by the present invention, its antibacterial property is greatly improved, and at the same time, the strength does not decrease. After being washed or subjected to friction testing, it still maintains a high antibacterial activity, and the antibacterial performance is persistent.
[0035] (4) The surface treatment agent used in the present invention also adds polyvinyl alcohol to disperse the doped sol, preventing it from coagulating and forming gel masses, and better exerting the antibacterial activity. Detailed implementation manners
[0036] To further elaborate on the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the following combines examples to describe in detail the specific implementation manners, structures, features and their effects according to the present invention.
[0037] Example 1
[0038] A surface treatment method for a high-strength fabric for children's tents, the surface treatment method comprising the following steps:
[0039] (1) Stir 4 parts by weight of tetrabutyl titanate and 25 parts by weight of absolute ethanol for 20 min to obtain solution A;
[0040] (2) Stir and mix 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 a concentration of 8 mol / L, then add 7 parts by weight of polyvinylpyrrolidone, and stir for 30 min under an ultrasonic power of 200 W to obtain solution B;
[0041] (3) Dropwise add the mixture composed of 0.5 part by weight of ammonium metavanadate, 80 parts by weight of deionized water and 0.5 part by weight of citric acid into solution B while stirring, control the dropping speed at 5 drops / s, and react at 80 °C for 5 h to obtain a sol;
[0042] (4) Dilute the sol by adding 80 parts by weight of deionized water, then add 5 parts by weight of hydrochloric acid with a concentration of 4 mol / L and stir for 5 min to obtain solution C;
[0043] (5) Completely immerse the polyester fiber fabric in solution C for 30 min;
[0044] (6) After the immersion is completed, dropwise add solution A into solution C, control the dropping time at 45 min, and at the same time keep stirring and reacting at a temperature of 80 °C for 2 h. After the reaction is completed, take out the polyester fiber fabric and then perform ultrasonic treatment for 15 min with an ultrasonic power of 600 W;
[0045] (7) Immerse the ultrasonically treated polyester fiber fabric in the surface treatment agent for 1 h, then perform drying and shaping, water washing, and then drying in sequence. The temperature for drying and shaping is 120 °C, the time for drying and shaping is 2 h, the temperature for the subsequent drying is 70 °C, and the time for the subsequent drying is 45 min, thus completing the treatment.
[0046] Among them, the surface treatment agent is composed of a mixture of 15 parts by weight of a modified silane coupling agent, 10 parts by weight of polyvinyl alcohol, and 5 parts by weight of calcium stearate.
[0047] The modified silane coupling agent is prepared through the following steps:
[0048] Step a: Stir and mix 5 parts by weight of KH550 silane coupling agent and 10 parts by weight of absolute ethanol at 25 °C for 10 min to obtain solution a;
[0049] Step b: Stir and mix 1 part by weight of phthalic anhydride, 5 parts by weight of tert-butyl hydroperoxide, and 20 parts by weight of absolute ethanol at 30 °C for 20 min to obtain solution b;
[0050] Step c: Mix solution a and solution b, then under 500 W of microwave, stir and react at 30 °C for 8 h. After the reaction is completed, distill at 90 °C for 20 min to remove the volatiles, thus obtaining the modified silane coupling agent.
[0051] Example 2
[0052] A surface treatment method for a high-strength fabric for children's tents, the surface treatment method comprising the following steps:
[0053] (1) Stir and mix 8 parts by weight of tetrabutyl titanate and 30 parts by weight of absolute ethanol for 30 min to obtain solution A;
[0054] (2) Stir and mix 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 a concentration of 9 mol / L, then add 10 parts by weight of polyvinylpyrrolidone and stir at an ultrasonic power of 300 W for 45 min to obtain solution B;
[0055] (3) While stirring, dropwise add the mixture composed of 1 part by weight of ammonium metavanadate, 100 parts by weight of deionized water, and 0.8 part by weight of citric acid to solution B, control the dropping speed at 10 drops / s, and react at 120 °C for 10 h to obtain a sol;
[0056] (4) Add 100 parts by weight of deionized water to the sol for dilution, then add 10 parts by weight of hydrochloric acid with a concentration of 6 mol / L and stir for 10 min to obtain solution C;
[0057] (5) Immerse the polyester fiber fabric completely in Solution C for 60 min;
[0058] (6) After the immersion is completed, add Solution A dropwise to Solution C. The dropping time is controlled within 60 min, and at the same time, keep stirring and reacting at a temperature of 100 °C for 3 h. After the reaction is completed, take out the polyester fiber fabric and then perform ultrasonic treatment for 20 min with an ultrasonic power of 700 W;
[0059] (7) Immerse the polyester fiber fabric after ultrasonic treatment in the surface treatment agent for 2 h, and then perform drying and shaping, water washing, and then drying in sequence. The temperature for drying and shaping is 150 °C, the time for drying and shaping is 3 h, the temperature for re-drying is 80 °C, and the time for re-drying is 60 min, thus completing the treatment.
[0060] Among them, the surface treatment agent is composed of 25 parts by weight of modified silane coupling agent, 15 parts by weight of polyvinyl alcohol, and 7 parts by weight of calcium stearate mixed.
[0061] The modified silane coupling agent is prepared through the following steps:
[0062] Step a: Stir and mix 7 parts by weight of KH550 silane coupling agent and 15 parts by weight of absolute ethanol at 30 °C for 15 min to obtain Solution a;
[0063] Step b: Stir and mix 3 parts by weight of phthalic anhydride, 6 parts by weight of tert-butyl hydroperoxide, and 30 parts by weight of absolute ethanol at 40 °C for 30 min to obtain Solution b;
[0064] Step c: Mix Solution a and Solution b, and then stir and react at 40 °C under 600 W of microwave for 12 h. After the reaction is completed, distill at 100 °C for 30 min to remove the volatiles, thus obtaining the modified silane coupling agent.
[0065] Example 3
[0066] A surface treatment method for a high-strength fabric for children's tents, the surface treatment method comprising the following steps:
[0067] (1) Stir and mix 7 parts by weight of tetrabutyl titanate and 27 parts by weight of absolute ethanol for 25 min to obtain Solution A;
[0068] (2) Stir and mix 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 a concentration of 8.5 mol / L, and then add 8.5 parts by weight of polyvinylpyrrolidone and stir for 40 min under an ultrasonic power of 250 W to obtain Solution B;
[0069] (3) While stirring, a mixture composed of 0.7 parts by weight of ammonium metavanadate, 90 parts by weight of deionized water, and 0.7 parts by weight of citric acid was added dropwise to Solution B. The dropping rate was controlled at 8 drops / s, and the reaction was carried out at 100 °C for 7 h to obtain a sol;
[0070] (4) 90 parts by weight of deionized water was added to the sol for dilution, and then 7 parts by weight of hydrochloric acid with a concentration of 5 mol / L was added and stirred for 8 min to obtain Solution C;
[0071] (5) The polyester fiber fabric was completely immersed in Solution C for 45 min;
[0072] (6) After the immersion was completed, Solution A was added dropwise to Solution C. The dropping time was controlled at 50 min, and at the same time, the mixture was continuously stirred and reacted at a temperature of 90 °C for 2.5 h. After the reaction was completed, the polyester fiber fabric was taken out and then subjected to ultrasonic treatment for 18 min with an ultrasonic power of 650 W;
[0073] (7) The polyester fiber fabric after ultrasonic treatment was immersed in the surface treatment agent for 1.5 h, and then dried and shaped, washed with water, and dried again in sequence. The temperature for drying and shaping was 140 °C, the time for drying and shaping was 2.5 h, the temperature for re-drying was 75 °C, and the time for re-drying was 50 min, thus completing the treatment.
[0074] Among them, the surface treatment agent was composed of a mixture of 20 parts by weight of a modified silane coupling agent, 13 parts by weight of polyvinyl alcohol, and 6 parts by weight of calcium stearate.
[0075] The modified silane coupling agent was prepared through the following steps:
[0076] Step a: 6 parts by weight of KH550 silane coupling agent and 12 parts by weight of absolute ethanol were stirred and mixed at 27 °C for 13 min to obtain Solution a;
[0077] 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 were stirred and mixed at 35 °C for 25 min to obtain Solution b;
[0078] Step c: Solution a and Solution b were mixed, and then stirred and reacted under microwave at 550 W and 35 °C for 10 h. After the reaction was completed, distillation was carried out at 95 °C for 25 min to remove volatiles, thus obtaining the modified silane coupling agent.
[0079] Comparative Example 1
[0080] A surface treatment method for a high-strength fabric for children's tents, the surface treatment method comprising the following steps:
[0081] (1) Stir 4 parts by weight of tetrabutyl titanate and 25 parts by weight of absolute ethanol for 20 min to mix them, obtaining solution A;
[0082] (2) Add 5 parts by weight of hydrochloric acid with a concentration of 4 mol / L to 80 parts by weight of deionized water and stir for 5 min, obtaining solution B;
[0083] (3) Immerse the polyester fiber fabric completely in solution B for 30 min;
[0084] (4) After the immersion is completed, add solution A dropwise to solution B, control the dropping time within 45 min, and at the same time keep stirring and reacting at a temperature of 80 °C for 2 h. After the reaction is completed, take out the polyester fiber fabric and then perform ultrasonic treatment for 15 min with an ultrasonic power of 600 W;
[0085] (5) Immerse the ultrasonically treated polyester fiber fabric in the surface treatment agent for 1 h, and then perform drying and shaping, water washing, and then drying in sequence. The temperature for drying and shaping is 120 °C, the time for drying and shaping is 2 h, the temperature for the second drying is 70 °C, and the time for the second drying is 45 min, thus completing the treatment.
[0086] Among them, the surface treatment agent is composed of 15 parts by weight of modified silane coupling agent, 10 parts by weight of polyvinyl alcohol, and 5 parts by weight of calcium stearate mixed together.
[0087] The modified silane coupling agent is prepared through the following steps:
[0088] Step a: Stir 5 parts by weight of KH550 silane coupling agent and 10 parts by weight of absolute ethanol at 25 °C for 10 min to mix them, obtaining solution a;
[0089] Step b: Stir 1 part by weight of phthalic anhydride, 5 parts by weight of tert-butyl hydroperoxide, and 20 parts by weight of absolute ethanol at 30 °C for 20 min to mix them, obtaining solution b;
[0090] Step c: Mix solution a and solution b, and then under 500 W of microwave, stir and react at 30 °C for 8 h. After the reaction is completed, distill at 90 °C for 20 min to remove the volatiles, thus obtaining the modified silane coupling agent.
[0091] Comparative Example 2
[0092] A surface treatment method for a high-strength fabric for children's tents, the surface treatment method comprising the following steps:
[0093] (1) Stir 4 parts by weight of tetrabutyl titanate and 25 parts by weight of absolute ethanol for 20 min to mix them, obtaining solution A;
[0094] (2) Stir and mix 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 a concentration of 8 mol / L. Then add 7 parts by weight of polyvinylpyrrolidone and stir for 30 min under an ultrasonic power of 200 W to obtain Solution B;
[0095] (3) While stirring, slowly add a mixture composed of 0.5 part by weight of ammonium metavanadate, 80 parts by weight of deionized water, and 0.5 part by weight of citric acid to Solution B. The dropping rate is controlled at 5 drops / s, and the reaction is carried out at 80 °C for 5 h to obtain a sol;
[0096] (4) Dilute the sol by adding 80 parts by weight of deionized water, then add 5 parts by weight of hydrochloric acid with a concentration of 4 mol / L and stir for 5 min to obtain Solution C;
[0097] (5) Immerse the polyester fiber fabric completely in Solution C for 30 min;
[0098] (6) After the immersion is completed, slowly add Solution A drop by drop to Solution C. The dropping time is controlled at 45 min, and at the same time, keep stirring and reacting at a temperature of 80 °C for 2 h. After the reaction is completed, take out the polyester fiber fabric and then perform ultrasonic treatment for 15 min with an ultrasonic power of 600 W;
[0099] (7) Immerse the ultrasonically treated polyester fiber fabric in the surface treatment agent for 1 h, and then perform drying and shaping, washing with water, and then drying in sequence. The temperature for drying and shaping is 120 °C, the time for drying and shaping is 2 h, the temperature for re-drying is 70 °C, and the time for re-drying is 45 min, and the treatment is completed.
[0100] Among them, the surface treatment agent is composed of a mixture of 15 parts by weight of KH550 silane coupling agent, 10 parts by weight of polyvinyl alcohol, and 5 parts by weight of calcium stearate.
[0101] Comparative Example 3
[0102] A surface treatment method for a high-strength fabric for children's tents, the surface treatment method comprising the following steps:
[0103] (1) Stir and mix 4 parts by weight of tetrabutyl titanate and 25 parts by weight of absolute ethanol for 20 min to obtain Solution A;
[0104] (2) Stir and mix 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 a concentration of 8 mol / L. Then add 7 parts by weight of polyvinylpyrrolidone and stir for 30 min under an ultrasonic power of 200 W to obtain Solution B;
[0105] (3) While stirring solution B, a mixture composed of 0.5 parts by weight of ammonium metavanadate, 80 parts by weight of deionized water, and 0.5 parts by weight of citric acid is added dropwise. The dropping rate is controlled at 5 drops / s, and the reaction is carried out at 80 °C for 5 h to obtain a sol.
[0106] (4) 80 parts by weight of deionized water is added to the sol for dilution, and then 5 parts by weight of hydrochloric acid with a concentration of 4 mol / L is added and stirred for 5 min to obtain solution C.
[0107] (5) The polyester fiber fabric is completely immersed in solution C for 30 min.
[0108] (6) After the immersion is completed, solution A is added dropwise to solution C. The dropping time is controlled at 45 min, and at the same time, stirring and reaction are maintained at 80 °C for 2 h. After the reaction is completed, the polyester fiber fabric is taken out and then ultrasonically treated for 15 min with an ultrasonic power of 600 W.
[0109] (7) The ultrasonically treated polyester fiber fabric is immersed in the surface treatment agent for 1 h, and then dried and shaped, washed with water, and dried again in sequence. The temperature for drying and shaping is 120 °C, the time for drying and shaping is 2 h, the temperature for re-drying is 70 °C, and the time for re-drying is 45 min, and the treatment is completed.
[0110] Among them, the surface treatment agent is composed of a mixture of 15 parts by weight of a modified silane coupling agent and 5 parts by weight of calcium stearate.
[0111] The modified silane coupling agent is prepared through the following steps:
[0112] Step a: 5 parts by weight of KH550 silane coupling agent and 10 parts by weight of absolute ethanol are stirred and mixed at 25 °C for 10 min to obtain solution a.
[0113] Step b: 1 part by weight of phthalic anhydride, 5 parts by weight of tert-butyl hydroperoxide, and 20 parts by weight of absolute ethanol are stirred and mixed at 30 °C for 20 min to obtain solution b.
[0114] Step c: Solution a and solution b are mixed, and then stirred and reacted under 500 W of microwave at 30 °C for 8 h. After the reaction is completed, distillation is carried out at 90 °C for 20 min to remove volatiles, and the modified silane coupling agent is obtained.
[0115] Test Example 1
[0116] Antibacterial test:
[0117] Using Escherichia coli (ATCC8099) and Staphylococcus aureus (ATCC6538P) as typical representatives, the antibacterial performance is tested.
[0118] (1) Inoculate Escherichia coli (ATCC8099) and Staphylococcus aureus (ATCC6538P) onto NA medium respectively, and then activate them in a constant temperature incubator at 37°C for 12 h.
[0119] (2) Place the two activated strains into physiological saline respectively, and adjust the concentration to 10 6 CFU / mL.
[0120] (3) Cut the surface-treated polyester fiber fabrics of Example 1 and Comparative Examples 1-3 (with a size of 1×1 cm), add 10 mL of PBS buffer respectively, and then drop 0.2 mL of the bacterial solution with a concentration of 10 6 CFU / mL in step (2).
[0121] (4) Use a 400W metal halide lamp to simulate the sun light source, and conduct a photocatalytic antibacterial experiment at room temperature of 25°C, with an irradiation time of 24 h for all.
[0122] (5) After the irradiation, take out 0.1 mL of the solution from each and dilute it in 5 mL of PBS buffer, then evenly coat it on the NA plate and culture it at a constant temperature of 37°C for 24 h. Finally, observe the number of colonies to obtain the sterilization rate.
[0123] Table 1. Test results of antibacterial properties of Example 1 and Comparative Examples 1-3
[0124] Escherichia coli bactericidal 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
[0125] Test Example 2
[0126] Strength test:
[0127] In accordance with the requirements of the standard "GB / T 14344-2008 Test method for tensile properties of chemical fiber filaments", use the INSTRON3367 type tensile testing machine of Instron Company to conduct strength tests on the surface-treated polyester fiber fabrics of Examples 1-3, and compare with the strength of the polyester fiber without any treatment. The strength of the polyester fiber is between 44-71 cN / dtex.
[0128] Table 2. Test results of strength of Examples 1-3
[0129]
[0130]
[0131] Test Example 3
[0132] Washing test:
[0133] The surface-treated polyester fiber fabrics of Example 1 and Comparative Examples 1-3 (cut into sizes of 5×5 cm each) were successively washed and dried, and after repeating 10 times, antibacterial tests were carried out according to the steps in Test Example 1 (only replacing the polyester fiber fabric in step (3)).
[0134] Table 3. Antibacterial performance test results of Example 1 and Comparative Examples 1-3 after 10 washes
[0135] Escherichia coli bactericidal 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
[0136] Test Example 4
[0137] Friction test:
[0138] The surface-treated polyester fiber fabrics of Example 1 and Comparative Examples 1-3 (cut into sizes of 5×5 cm each) were respectively dragged back and forth 20 cm on 800-mesh sandpaper under the pressure of a 100-g weight, and after dragging 10 times in total (one round trip counts as two times), antibacterial tests were carried out according to the steps in Test Example 1 (only replacing the polyester fiber fabric in step (3)).
[0139] Table 4. Antibacterial performance test results of Example 1 and Comparative Examples 1-3 after 10 frictions
[0140]
[0141]
[0142] From the comparison results of the above Examples 1-3, Comparative Examples 1-3 and Test Examples 1-4, it can be seen that:
[0143] By comparing Example 1 and Comparative Example 1, it can be known that the photocatalytic activity of titanium dioxide doped with bismuth vanadate has been greatly improved, that is, the antibacterial performance has been enhanced.
[0144] By comparing Examples 1-3 and Test Example 2, it can be known that the surface treatment method of the present invention has no influence on the strength of polyester fiber and still maintains its inherent high-strength characteristics.
[0145] By comparing Example 1, Comparative Examples 1-3 and Test Example 1, it can be known that not doping titanium dioxide, not using a modified silane coupling agent and not using a polyvinyl alcohol dispersant will all reduce its antibacterial performance.
[0146] By comparing Example 1, Comparative Examples 1-3 and Test Example 3, it can be known that although the antibacterial performance of polyester fiber fabrics treated with different surface treatment methods has decreased after washing, for Comparative Example 2 without using a modified silane coupling agent, its antibacterial performance has decreased significantly faster.
[0147] Similarly, by comparing Example 1, Comparative Examples 1-3 and Test Example 4, it can be seen that after friction, the antibacterial performance of Comparative Example 2 without using the modified silane coupling agent also decreases significantly faster.
[0148] In summary, the surface treatment method of the present invention uses bismuth vanadate to dope titanium dioxide sol, so as to directly prepare doped sol on the polyester fiber fabric, with better antibacterial performance. At the same time, after being treated with the modified silane coupling agent, it is not easy to peel off, does not affect the strength of the fiber fabric, and still maintains high antibacterial activity after washing and friction tests.
[0149] The above are only the preferred embodiments of the present invention, and do not impose any form of limitation on the present invention. Although the present invention has been disclosed above with preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some changes or modifications to equivalent embodiments by using the disclosed technical content within the scope of the technical solution of the present invention. However, as long as it does not depart from the technical solution content of the present invention, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.
Claims
1. A surface treatment method for a high-strength fabric used in a children's tent, characterized in that: The surface treatment method includes the following steps: (1) Stir 4 - 8 parts by weight of tetrabutyl titanate and 25 - 30 parts by weight of absolute ethanol for 20 - 30 min to mix, obtaining solution A; (2) Stir and mix 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, then add 7 - 10 parts by weight of polyvinylpyrrolidone, and ultrasonically stir for 30 - 45 min to obtain solution B; (3) Dropwise add the mixture composed of 0.5 - 1 part 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 solution B while stirring, and react at 80 - 120 °C for 5 - 10 h to obtain a sol; (4) Add 80 - 100 parts by weight of deionized water to dilute the sol, then add 5 - 10 parts by weight of hydrochloric acid and stir for 5 - 10 min to obtain solution C; (5) Completely immerse the polyester fiber fabric in solution C; (6) After immersion, dropwise add solution A into solution C, control the dropping time within 45 - 60 min, and simultaneously keep stirring and reacting at a temperature of 80 - 100 °C for 2 - 3 h. After the reaction is completed, take out the polyester fiber fabric and then perform ultrasonic treatment for 15 - 20 min; (7) Immerse the ultrasonically treated polyester fiber fabric in the surface treatment agent for 1 - 2 h, then successively perform drying and shaping, water washing, and then drying, and the treatment is completed; The surface treatment agent described in step (7) is composed of 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 mixed; The modified silane coupling agent is prepared through the following steps: Step a: Stir 5 - 7 parts by weight of KH550 silane coupling agent and 10 - 15 parts by weight of absolute ethanol at 25 - 30 °C for 10 - 15 min to mix, obtaining solution a; Step b: Stir 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 ethanol at 30 - 40 °C for 20 - 30 min to mix, obtaining solution b; Step c: Mix solution a and solution b, then under microwave of 500 - 600 W, stir and react at 30 - 40 °C for 8 - 12 h. After the reaction is completed, distill at 90 - 100 °C for 20 - 30 min to remove volatiles, and the modified silane coupling agent is obtained.
2. The surface treatment method of a high-strength fabric for a children's tent according to claim 1, characterized in that: The concentration of the concentrated nitric acid described in step (2) is 8 - 9 mol / L.
3. The surface treatment method of a high-strength fabric for a children's tent according to claim 1, characterized in that: The power of the ultrasonic treatment described in step (2) is 200 - 300 W.
4. The surface treatment method of a high-strength fabric for a children's tent according to claim 1, characterized in that: The dropping speed described in step (3) is 5 - 10 drops / s.
5. The surface treatment method of a high-strength fabric for a children's tent according to claim 1, characterized in that: The concentration of the hydrochloric acid described in step (4) is 4 - 6 mol / L.
6. The surface treatment method of a high-strength fabric for a children's tent according to claim 1, characterized in that: The immersion time described in step (5) is 30 - 60 min.
7. The surface treatment method of a high-strength fabric for a children's tent according to claim 1, characterized in that: The power of the ultrasonic treatment described in step (6) is 600 - 700 W.
8. The surface treatment method of a high-strength fabric for a children's tent according to claim 1, characterized in that: The temperature of the drying and shaping described in step (7) is 120 - 150 °C, the time of the drying and shaping is 2 - 3 h, the temperature of the re - drying is 70 - 80 °C, and the time of the re - drying is 45 - 60 min.
Citation Information
Patent Citations
Antibacterial polyester fibre
CN101701370A
Antibacterial ultraviolet-proof polyester fiber fabric and preparation method thereof
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CN108978179A
Preparation method of visible photocatalytic functional fabric in interface nanometer mixed crystal structure
CN103205889A
Silane coupling agent, waterborne acrylate laminating adhesive emulsion and waterborne acrylate laminating adhesive
CN113321678A