Moisture-absorbing, antibacterial titanium fiber fabric and preparation method thereof

Abstract

The application relates to the technical field of fabrics, and discloses a moisture-absorbing, sweat-releasing and antibacterial titanium fiber fabric and a preparation method thereof. The 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methyl acrylamide]-1,3,5-homotriazine is used to graft modify the polyamide fiber fabric, the hydrophilic amide bond, imino and a large number of hydroxyl groups are grafted to the fabric surface, the hydrophilicity and the moisture regain of the fabric are significantly improved, and the moisture-absorbing and sweat-releasing performance of the fabric is improved. Meanwhile, the limiting oxygen index and the flame-retardant performance are improved. A large number of hydroxyl groups on the surface of the polyamide fabric can interact with the hydroxyl groups on the surface of the titanium dioxide precursor generated by hydrolysis of tetrabutyl titanate, the generated nanometer titanium dioxide can be uniformly loaded on the fabric surface, more photocatalytic antibacterial sites are exposed, and the antibacterial performance of the fabric is significantly improved.

Description

Technical Field

[0001] This invention relates to the field of fabric technology, specifically to a moisture-wicking, perspiration-absorbing, and antibacterial titanium fiber fabric and its preparation method. Background Technology

[0002] Nylon fiber fabrics are tough, abrasion-resistant, and highly elastic, making them widely used. However, traditional nylon fabrics have a low moisture regain rate, affecting their moisture absorption and wicking properties. Furthermore, nylon fabrics have poor antibacterial and flame-retardant properties, hindering their practical application in high-end clothing. Currently, methods to improve the moisture absorption and antibacterial properties of nylon fabrics mainly include finishing agents and chemical grafting modification. Common chemical grafting monomers include acrylic acid, hydroxyethyl acrylate, and acrylamide.

[0003] Nano titanium dioxide is non-toxic and pollution-free, has a simple preparation method, and strong antibacterial properties. It is widely used in materials such as fabrics, plastics, and rubber. Loading nano titanium dioxide onto the surface of fabrics can give them excellent antibacterial properties. However, nano titanium dioxide is prone to agglomeration and has poor dispersion on the fabric surface, which will affect its antibacterial properties. Summary of the Invention

[0004] (I) Technical problem to be solved: In view of the shortcomings of the existing technology, the present invention provides a moisture-wicking and antibacterial titanium fiber fabric and its preparation method, which solves the problem of poor moisture-wicking, antibacterial and flame-retardant properties of nylon fiber fabric.

[0005] (II) Technical Solution: A method for preparing a moisture-wicking, perspiration-absorbing, and antibacterial titanium fiber fabric:

[0006] (1) Add N-(3-aminopropyl)methacrylamide hydrochloride and 2,4-bis(N,N-dihydroxyethylamino)-6-chloro-1,3,5-triazine to 1,4-dioxane, add sodium carbonate aqueous solution dropwise, cool after reaction, filter, evaporate the filtrate by rotary evaporation, and recrystallize the crude product in ethanol to obtain 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine.

[0007] (2) The cleaned nylon fiber fabric is added to an aqueous solution of potassium persulfate for pre-reaction. Then the fabric is added to an aqueous solution containing 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine. The bath ratio A is adjusted to carry out the grafting reaction. Finally, the fabric is added to deionized water, boiled, washed with water, and dried to obtain a moisture-wicking nylon fiber fabric.

[0008] (3) Add tetrabutyl titanate to ethanol to prepare a tetrabutyl titanate solution, add moisture-wicking nylon fiber fabric, adjust the bath ratio B, and perform a two-dip and two-nip treatment. Then add the fabric to deionized water, adjust the bath ratio C, take out the fabric after the reaction, wash it with ethanol and water, and dry it to obtain a moisture-wicking and antibacterial titanium fiber fabric.

[0009] Furthermore, in (1), the molar ratio of N-(3-aminopropyl)methacrylamide hydrochloride and 2,4-bis(N,N-dihydroxyethylamino)-6-chloro-1,3,5-triazine is (1-1.2):1.

[0010] Furthermore, in (1), the reaction temperature is 75-85℃ and the reaction time is 6-10h.

[0011] Furthermore, in (2), the concentration of the potassium persulfate aqueous solution is (0.01-0.025) mol / L.

[0012] Furthermore, in (2), the bath ratio A is 1:(35-50).

[0013] Furthermore, in (2), the pre-reaction temperature is 70-80℃ and the reaction time is 20-40min.

[0014] Furthermore, in (2), the concentration of the aqueous solution of 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine is (0.5-1.5) mol / L.

[0015] Furthermore, in (2), the grafting reaction temperature is 65-80℃ and the reaction time is 2-3h.

[0016] Furthermore, (2) the mass fraction of the tetrabutyl titanate solution is 20-30%.

[0017] Furthermore, the liquor ratio B is 1:(30-40), and the liquor ratio C is 1:(30-50).

[0018] Furthermore, in (3), the reaction temperature is 90-95℃ and the reaction time is 6-8h.

[0019] (III) Beneficial technical effects: This invention utilizes 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine containing alkenyl groups to graft and modify nylon fiber fabrics, grafting hydrophilic amide bonds, imino groups, and a large number of hydroxyl groups onto the fabric surface, significantly improving the fabric's hydrophilicity and moisture regain, which is beneficial for improving the fabric's moisture absorption and perspiration wicking performance.

[0020] This invention grafts triazine groups onto the surface of nylon fabric. During combustion, the triazine groups thermally decompose to release gases such as nitrogen, which can dilute the oxygen concentration, inhibit combustion, and improve the limiting oxygen index and flame retardant properties.

[0021] This invention introduces a large number of hydroxyl groups onto the surface of nylon fabric. These hydroxyl groups can interact with the hydroxyl groups on the surface of the titanium dioxide precursor generated by the hydrolysis of tetrabutyl titanate, thereby uniformly loading the titanium dioxide precursor onto the fabric surface. Furthermore, through a high-temperature hydrothermal method, the generated nano-titanium dioxide can be uniformly loaded onto the fabric surface, exposing more photocatalytic antibacterial sites and significantly improving the antibacterial rate and antibacterial performance of Escherichia coli. Detailed Implementation

[0022] To make the objectives, technical solutions, and advantages of the present invention clearer, the technical solutions of the present disclosure will be clearly and completely described below in conjunction with the embodiments of the present disclosure. Obviously, the described embodiments are only some embodiments of the present disclosure, and not all embodiments.

[0023] The preparation method of 2,4-bis(N,N-dihydroxyethylamino)-6-chloro-1,3,5-homogeneous triazine is as follows: 18.4 g (0.1 mol) of cyanuric chloride was added to 50 mL of ethanol, and after stirring, 50 mL of an ethanol solution containing 22.05 g (0.21 mol) of triethanolamine and 22 g of triethylamine was added dropwise. The mixture was stirred for 0.5 h, heated to 50 °C, and reacted for 5 h. After cooling to room temperature, the mixture was filtered, and the filtrate was evaporated by rotary evaporation. The product was recrystallized in dichloromethane to obtain 2,4-bis(N,N-dihydroxyethylamino)-6-chloro-1,3,5-homogeneous triazine, with the structural formula [insert structural formula here]. .

[0024] Example 1

[0025] (1) Add 80 mmol of N-(3-aminopropyl)methacrylamide hydrochloride and 80 mmol of 2,4-bis(N,N-dihydroxyethylamino)-6-chloro-1,3,5-triazine to 300 mL of 1,4-dioxane, add dropwise 100 mL of an aqueous solution containing 192 mmol of sodium carbonate, heat to 85 °C, react for 6 h, cool, filter, evaporate the filtrate by rotary evaporation, and recrystallize the crude product in ethanol to obtain 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine. The preparation reaction formula is:

[0026] .

[0027] (2) The cleaned nylon fiber fabric is added to a 0.01 mol / L potassium persulfate aqueous solution, heated to 75°C, and reacted for 20 min. Then the fabric is added to a 0.5 mol / L aqueous solution of 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine with a bath ratio of 1:40. The solution is heated to 70°C and reacted for 3 h. Finally, the fabric is added to deionized water, boiled for 10 min, washed with water, and dried to obtain a moisture-wicking nylon fiber fabric.

[0028] (3) Add tetrabutyl titanate to ethanol to prepare a 20% tetrabutyl titanate solution. Add moisture-wicking nylon fiber fabric with a bath ratio of 1:40. After two dips and two nips, the nips are 85%. Then add the fabric to deionized water with a bath ratio of 1:30. Heat to 95°C and react for 6 hours. Take out the fabric, wash with ethanol and water, and dry to obtain moisture-wicking and antibacterial titanium fiber fabric.

[0029] Example 2

[0030] (1) Add 96 mmol of N-(3-aminopropyl)methacrylamide hydrochloride and 80 mmol of 2,4-bis(N,N-dihydroxyethylamino)-6-chloro-1,3,5-triazine to 400 mL of 1,4-dioxane, add 120 mL of aqueous solution containing 216 mmol of sodium carbonate, heat to 80 °C, react for 10 h, cool, filter, evaporate the filtrate by rotary evaporation, recrystallize the crude product in ethanol to obtain 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine.

[0031] (2) The cleaned nylon fiber fabric is added to a 0.018 mol / L potassium persulfate aqueous solution, heated to 70°C, and reacted for 40 min. Then the fabric is added to a 1 mol / L aqueous solution of 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine with a bath ratio of 1:50. The solution is heated to 65°C and reacted for 3 h. Finally, the fabric is added to deionized water, boiled for 20 min, washed with water, and dried to obtain a moisture-wicking nylon fiber fabric.

[0032] (3) Add tetrabutyl titanate to ethanol to prepare a 30% tetrabutyl titanate solution. Add moisture-wicking nylon fiber fabric with a bath ratio of 1:30. Perform a two-dip and two-nip treatment with a nip rate of 90%. Then add the fabric to deionized water with a bath ratio of 1:50. Heat to 90°C and react for 8 hours. Remove the fabric, wash with ethanol and water, and dry to obtain a moisture-wicking and antibacterial titanium fiber fabric.

[0033] Example 3

[0034] (1) Add 88 mmol of N-(3-aminopropyl)methacrylamide hydrochloride and 80 mmol of 2,4-bis(N,N-dihydroxyethylamino)-6-chloro-1,3,5-triazine to 350 mL of 1,4-dioxane, add 120 mL of aqueous solution containing 224 mmol of sodium carbonate, heat to 75 °C, react for 10 h, cool, filter, evaporate the filtrate by rotary evaporation, recrystallize the crude product in ethanol to obtain 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine.

[0035] (2) The cleaned nylon fiber fabric is added to a 0.025 mol / L potassium persulfate aqueous solution, heated to 80°C, and reacted for 20 min. Then the fabric is added to a 1.5 mol / L aqueous solution of 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine with a bath ratio of 1:35. The solution is heated to 80°C and reacted for 2 h. Finally, the fabric is added to deionized water, boiled for 20 min, washed with water, and dried to obtain a moisture-wicking nylon fiber fabric.

[0036] (3) Add tetrabutyl titanate to ethanol to prepare a tetrabutyl titanate solution with a mass fraction of 25%. Add moisture-wicking nylon fiber fabric with a bath ratio of 1:40. After two dips and two nips, the nips are 85%. Then add the fabric to deionized water with a bath ratio of 1:40. Heat to 95°C and react for 7 hours. Take out the fabric, wash with ethanol and water, and dry to obtain moisture-wicking and antibacterial titanium fiber fabric.

[0037] Comparative Example 1 is a nylon fiber fabric.

[0038] Comparative Example 2

[0039] (1) Add tetrabutyl titanate to ethanol to prepare a tetrabutyl titanate solution with a mass fraction of 30%. Add nylon fiber fabric with a bath ratio of 1:30. Perform two dips and two nips, with a nips ratio of 90%. Then add the fabric to deionized water with a bath ratio of 1:50. Heat to 80°C and react for 4 hours. Take out the fabric, wash with ethanol and water, and dry to obtain titanium fiber fabric.

[0040] Comparative Example 3

[0041] (1) The cleaned nylon fiber fabric is added to a 0.01 mol / L potassium persulfate aqueous solution, heated to 75°C, and reacted for 20 min. Then the fabric is added to a 0.5 mol / L hydroxyethyl acrylate aqueous solution with a bath ratio of 1:40, heated to 70°C, and reacted for 3 h. Finally, the fabric is added to deionized water, boiled for 10 min, washed with water, and dried to obtain the grafted nylon fiber fabric.

[0042] (2) Add tetrabutyl titanate to ethanol to prepare a tetrabutyl titanate solution with a mass fraction of 20%. Add grafted nylon fiber fabric with a bath ratio of 1:40. Perform two dips and two nips, with a nips ratio of 85%. Then add the fabric to deionized water with a bath ratio of 1:30. Heat to 95°C and react for 6 hours. Take out the fabric, wash with ethanol and water, and dry to obtain titanium fiber fabric.

[0043] Comparative Example 4

[0044] (1) Add 80 mmol of N-(3-aminopropyl)methacrylamide hydrochloride and 80 mmol of 2,4-di-(N,N'-diethylamino)-6-chlorotriazine (CAS Registry No. 580-48-3, structural formula: ) to 300 mL of 1,4-dioxane. ), 100 mL of an aqueous solution containing 192 mmol of sodium carbonate was added dropwise, heated to 85 °C, and reacted for 6 h. After cooling, the mixture was filtered, and the filtrate was evaporated by rotary evaporation. The crude product was recrystallized in ethanol to give 2,4-bis-(N,N'-diethylamino)-6-[N-(3-aminopropyl)methacrylamide]triazine, with the structural formula […]. .

[0045] (2) The cleaned nylon fiber fabric was added to a 0.01 mol / L potassium persulfate aqueous solution, heated to 75°C, and reacted for 20 min. Then the fabric was added to a 0.5 mol / L aqueous solution of 2,4-di-(N,N'-diethylamino)-6-[N-(3-aminopropyl)methacrylamide]triazine with a bath ratio of 1:40. The solution was heated to 70°C and reacted for 3 h. Finally, the fabric was added to deionized water, boiled for 10 min, washed with water, and dried to obtain the grafted nylon fiber fabric.

[0046] (3) Add tetrabutyl titanate to ethanol to prepare a tetrabutyl titanate solution with a mass fraction of 20%. Add grafted nylon fiber fabric with a bath ratio of 1:40. Perform two dips and two nips, with a nips ratio of 85%. Then add the fabric to deionized water with a bath ratio of 1:30. Heat to 95°C and react for 6 hours. Take out the fabric, wash with ethanol and water, and dry to obtain titanium fiber fabric.

[0047] The moisture regain of the fabric was tested according to GB / T 9994-2018 standard.

[0048] The antibacterial properties were tested according to GB / T 23763-2009 standard. The antibacterial rate = (C0-C1) / C0×100%, where C0 is the viable bacteria count (cfu) of the control sample (nylon fiber fabric of Comparative Example 1) after incubation under light conditions. C1 is the viable bacteria count (cfu) of the photocatalyst sample after incubation.

[0049] Flame retardant properties were tested according to GB / T 5454-1997.

[0050] Table 1 Performance Tests of Nylon Fiber Fabrics

[0051]

[0052] After testing, the nylon fiber fabric of Comparative Example 1 showed low moisture regain and limiting oxygen index, poor moisture absorption and flame retardancy, and poor antibacterial properties. The nylon fiber fabrics of Examples 1-3 showed high moisture regain, antibacterial rate, and limiting oxygen index, exhibiting better moisture absorption, antibacterial properties, and flame retardancy. This was mainly due to the grafting modification of the nylon fiber fabric with alkenyl-containing 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine, which grafted hydrophilic amide bonds, imino groups, and a large number of hydroxyl groups onto the fabric surface, significantly improving the fabric's hydrophilicity and moisture regain properties. Furthermore, the triazine group contains a large amount of nitrogen, which releases nitrogen and other gases during combustion through thermal decomposition. This can dilute the oxygen concentration, inhibit combustion, and improve the limiting oxygen index and flame retardant performance. In addition, the large number of hydroxyl groups can interact with the hydroxyl groups on the surface of the titanium dioxide precursor generated by the hydrolysis of tetrabutyl titanate, thereby uniformly loading the titanium dioxide precursor onto the fabric surface. After further processing through a high-temperature hydrothermal method, the generated nano-titanium dioxide can be uniformly loaded onto the fabric surface, exposing more photocatalytic antibacterial sites and significantly improving the antibacterial rate and antibacterial performance of Escherichia coli.

[0053] Comparative Example 2 did not utilize 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine to graft and modify the nylon fiber fabric. As a result, amide bonds, imino groups, a large number of hydroxyl groups, and triazine groups were not grafted onto the fabric surface, leading to lower moisture regain and limiting oxygen index of the fabric. Furthermore, the nano-titanium dioxide had poor dispersion on the fabric surface and fewer photocatalytic antibacterial sites, resulting in a lower antibacterial rate against Escherichia coli.

[0054] Comparative Example 3 uses hydroxyethyl acrylate to graft and modify nylon fiber fabric. It has a low hydroxyl content and does not contain amide bonds, imino groups, or triazine groups, resulting in a lower moisture regain and limiting oxygen index than in Example 1. Furthermore, the nano-titanium dioxide has poor dispersion on the fabric surface and fewer photocatalytic antibacterial sites, leading to a lower antibacterial rate against Escherichia coli.

[0055] Comparative Example 4 uses 2,4-di-(N,N'-diethylamino)-6-[N-(3-aminopropyl)methacrylamide]triazine to graft-modify nylon fiber fabric. Since it does not contain a large number of hydroxyl groups, the fabric has a low moisture regain rate. Furthermore, the nano-titanium dioxide has poor dispersion on the fabric surface and fewer photocatalytic antibacterial sites, resulting in a low antibacterial rate against Escherichia coli.

[0056] The above embodiments are only used to illustrate the technical solutions of this disclosure, and are not intended to limit it. Although this disclosure has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this disclosure.

Claims

1. A method for preparing a moisture-wicking, perspiration-absorbing, and antibacterial titanium fiber fabric, characterized in that, The preparation method includes: (1) The cleaned nylon fiber fabric is added to an aqueous solution of potassium persulfate for pre-reaction. Then the fabric is added to an aqueous solution containing 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine. The bath ratio A is adjusted to carry out the grafting reaction. Finally, the fabric is added to deionized water, boiled, washed with water, and dried to obtain a moisture-wicking nylon fiber fabric. The structural formula of the 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine is as follows: ; (2) Add tetrabutyl titanate to ethanol to prepare a tetrabutyl titanate solution, add moisture-wicking nylon fiber fabric, adjust the bath ratio B, and perform a two-dip and two-nip treatment. Then add the fabric to deionized water, adjust the bath ratio C, take out the fabric after the reaction, wash it with ethanol and water, and dry it to obtain a moisture-wicking and antibacterial titanium fiber fabric. The concentration of the potassium persulfate aqueous solution in (1) is (0.01-0.025) mol / L; The concentration of the aqueous solution of 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine in (1) is (0.5-1.5) mol / L; The mass fraction of the tetrabutyl titanate solution in (2) is 20-30%; the bath ratio B is 1:(30-40), and the bath ratio C is 1:(30-50).

2. The method for preparing the moisture-wicking, perspiration-absorbing, and antibacterial titanium fiber fabric according to claim 1, characterized in that, In (1), the bath ratio A is 1:(35-50).

3. The method for preparing the moisture-wicking, perspiration-absorbing, and antibacterial titanium fiber fabric according to claim 1, characterized in that, The pre-reaction temperature in (1) is 70-80℃ and the reaction time is 20-40min.

4. The method for preparing the moisture-wicking, perspiration-absorbing, and antibacterial titanium fiber fabric according to claim 1, characterized in that, The grafting reaction in (1) is carried out at a temperature of 65-80℃ and for a reaction time of 2-3h.

5. The method for preparing the moisture-wicking, perspiration-absorbing, and antibacterial titanium fiber fabric according to claim 1, characterized in that, The reaction temperature in (2) is 90-95℃ and the reaction time is 6-8h.

6. The method for preparing the moisture-wicking, perspiration-absorbing, and antibacterial titanium fiber fabric according to claim 1, characterized in that, The preparation method of 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine is as follows: N-(3-aminopropyl)methacrylamide hydrochloride and 2,4-bis(N,N-dihydroxyethylamino)-6-chloro-1,3,5-triazine are added to 1,4-dioxane in a molar ratio of (1-1.2):1, sodium carbonate aqueous solution is added dropwise, the mixture is heated to 75-85℃, reacted for 6-10 h, cooled and filtered, the filtrate is evaporated by rotary evaporation, and the crude product is recrystallized in ethanol to obtain 2,4-bis(N,N-dihydroxyethylamino)-6-[N-(3-aminopropyl)methacrylamide]-1,3,5-triazine.

7. A moisture-wicking, antibacterial titanium fiber fabric obtained by the preparation method according to any one of claims 1-6.

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