Preparation process of antibacterial fiber and textile fabric thereof

Abstract

The present invention relates to the field of fiber technology and discloses a preparation process for antibacterial fiber and textile fabric thereof. The method comprises chelating carboxybenzoate-treated tea polyphenol with silver acetate to obtain a tea polyphenol-silver complex; the resulting product is then spun with polyethylene terephthalate in a melt spinning machine to obtain the antibacterial fiber. The carboxybenzoate-treated tea polyphenol contains a relatively large amount of benzoate structures, which makes the tea polyphenol-silver complex highly compatible with PET and has minimal effect on the mechanical properties of the PET fiber, resulting in excellent breaking strength of the fiber. The carboxybenzoate-treated tea polyphenol contains carboxyl and phenolic hydroxyl hydrophilic groups, which help improve the hydrophilicity and moisture regain of the fiber. Furthermore, the tea polyphenol-silver complex contains tea polyphenol antibacterial structures and silver ion antibacterial agents, significantly enhancing the antibacterial and bactericidal capabilities of the fiber. The fiber can be used to produce a polyester textile fabric with excellent antibacterial and hygroscopic properties.

Description

Technical Field

[0001] The present invention relates to the field of fiber technology, in particular to a preparation process of an antibacterial fiber and a textile fabric thereof. Background Art

[0002] Polyester fiber is a synthetic fiber with good heat resistance and excellent wrinkle resistance. It is widely used in textile fabrics, clothing and home textiles. Traditional polyester fibers have a low moisture regain and poor hydrophilicity, which will affect the hygroscopicity and wearing comfort of the fabric. Therefore, it is necessary to improve the hydrophilicity of polyester fibers. Adding antimicrobial agents to the fibers can improve the antimicrobial and bactericidal properties of textile fabrics, so that the fabrics remain clean, hygienic and safe. Common antimicrobial agents include natural antimicrobial agents such as tea polyphenols, and inorganic antimicrobial agents such as silver ions. Patent application with publication number CN119685957A discloses a method for preparing antimicrobial modified fibers for textile fabrics. Copper-tea polyphenol-based hyperbranched polyamide is spun with nylon to improve the tensile properties and antimicrobial properties of nylon fibers. However, the fibers do not show good hydrophilicity and moisture regain, which is not conducive to the application of the fibers in hydrophilic hygroscopic textile fabrics. Summary of the Invention

[0003] (1) The technical problem solved by the present invention is to solve the problem of poor antibacterial and hygroscopic properties of polyester fibers.

[0004] (II) Technical solution: A preparation process for antibacterial fiber:

[0005] Step S1, add ethyl acetate, 420-590 parts by weight of tea polyphenols, 100 parts by weight of pyromellitic anhydride, and 76-102 parts by weight of pyridine into a flask, stir to react, filter, rotary evaporate the filtrate, wash with petroleum ether, dissolve the product in ethyl acetate, heat to volatilize, cool and crystallize to obtain carboxybenzoic acid esterified tea polyphenols, and the preparation reaction formula is:

[0006] .

[0007] Step S2: add deionized water and 100 parts by weight of carboxybenzoic acid-esterified tea polyphenols into a flask, stir, dropwise add acetic acid solution, then dropwise add an aqueous solution containing 5-8 parts by weight of silver acetate, stir to react in the dark, filter, wash with water and ethanol, and dry to obtain a tea polyphenol silver complex.

[0008] Step S3: 100 parts by weight of polyethylene terephthalate and 8-20 parts by weight of tea polyphenol silver complex are mixed, spun in a melt spinning machine, and then drawn to obtain antibacterial fibers.

[0009] Furthermore, the reaction temperature in step S1 is 50-70° C., and the reaction time is 12-24 h.

[0010] Furthermore, in step S2, acetic acid solution is added dropwise to adjust the pH to 3-3.5.

[0011] Furthermore, the reaction temperature in S2 is 20-35° C., and the reaction time is 1-3 h.

[0012] Furthermore, the spinning temperature of the melt spinning machine in S3 is 260-280° C. in zones 1-5, and the spinning speed is 800-1500 m / min.

[0013] Furthermore, the antibacterial fiber is used to make antibacterial and moisture-absorbing polyester textile fabrics.

[0014] (III) Beneficial Technical Effects: The present invention reacts pyromellitic anhydride with an excess of tea polyphenols to produce carboxybenzoate-esterified tea polyphenols. The carboxyl and hydroxyl groups are then used to chelate silver ions, resulting in a tea polyphenol-silver complex with a high silver ion loading. This complex is then melt-spun with polyethylene terephthalate to produce antibacterial fibers. Carboxybenzoate-esterified tea polyphenols contain a relatively high number of benzoate structures, similar to the benzoate structural units of PET (polyethylene terephthalate). This results in excellent compatibility between the tea polyphenol-silver complex and PET, allowing it to be evenly dispersed in the fiber matrix, with minimal effect on the mechanical properties of the PET fiber, resulting in excellent fiber breaking strength.

[0015] The carboxybenzoate-esterified tea polyphenols of the present invention contain carboxyl and phenolic hydroxyl hydrophilic groups, which are beneficial to improving the hydrophilicity and moisture regain of the fiber. In addition, the tea polyphenol-silver complex contains a tea polyphenol antibacterial structure and a silver ion antibacterial agent. The tea polyphenol-silver complex is uniformly dispersed in the fiber matrix, has more bactericidal sites, and significantly improves the antibacterial and bactericidal ability of the fiber. The fiber can be used to make polyester textile fabrics with excellent antibacterial and hygroscopic properties. DETAILED DESCRIPTION

[0016] The following is a detailed description of the specific embodiments of the present invention. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention and are not intended to limit the present invention.

[0017] Example 1 (1) 800 mL of ethyl acetate, 50 g of tea polyphenols, 10 g of pyromellitic anhydride, and 8.8 g of pyridine were added to a flask, and the mixture was stirred at 65°C for 18 h. After filtering, the filtrate was rotary evaporated and washed with petroleum ether. The product was dissolved in ethyl acetate, heated for volatilization, and cooled for crystallization to obtain carboxybenzoic acid esterified tea polyphenols.

[0018] (2) Add 1.5 L of deionized water and 80 g of carboxybenzoate-esterified tea polyphenols into a flask, stir, add acetic acid solution dropwise to adjust the pH to 3, then add 450 mL of an aqueous solution containing 4 g of silver acetate dropwise, and react at 25 ° C for 1 h in the dark. After filtering, wash with water and ethanol, and dry to obtain a tea polyphenol silver complex.

[0019] (3) 2 kg of polyethylene terephthalate and 160 g of tea polyphenol silver complex were mixed and spun in a melt spinning machine. The temperatures in zones 1-5 were 260°C, 275°C, 280°C, 280°C, and 275°C, and the spinning speed was 800-1500 m / min. The fiber was then drawn at a draw ratio of 4 to obtain an antibacterial fiber.

[0020] Example 2 (1) 900 mL of ethyl acetate, 59 g of tea polyphenols, 10 g of pyromellitic anhydride, and 10.2 g of pyridine were added to a flask, and the mixture was stirred at 50°C for 24 h. After filtering, the filtrate was rotary evaporated and washed with petroleum ether. The product was dissolved in ethyl acetate, heated for volatilization, and cooled for crystallization to obtain carboxybenzoic acid esterified tea polyphenols.

[0021] (2) Add 2 L of deionized water and 80 g of carboxybenzoate-esterified tea polyphenols into a flask, stir, add acetic acid solution dropwise to adjust the pH to 3.5, then add 550 mL of an aqueous solution containing 5 g of silver acetate dropwise, and react at 20 ° C for 3 h in the dark. After filtering, wash with water and ethanol, and dry to obtain a tea polyphenol silver complex.

[0022] (3) 2 kg of polyethylene terephthalate and 300 g of tea polyphenol silver complex were mixed and spun in a melt spinning machine. The temperatures in zones 1-5 were 260°C, 275°C, 280°C, 280°C, and 275°C, and the spinning speed was 800-1500 m / min. The fiber was then drawn at a draw ratio of 4 to obtain an antibacterial fiber.

[0023] Example 3 (1) 800-900 mL of ethyl acetate, 42 g of tea polyphenols, 10 g of pyromellitic anhydride, and 7.6 g of pyridine were added to a flask, and the mixture was stirred at 70°C for 12 h. After filtering, the filtrate was rotary evaporated and washed with petroleum ether. The product was dissolved in ethyl acetate, heated for volatilization, and cooled for crystallization to obtain carboxybenzoic acid esterified tea polyphenols.

[0024] (2) Add 2 L of deionized water and 80 g of carboxybenzoate-esterified tea polyphenols into a flask, stir, and then add dropwise acetic acid solution to adjust the pH to 3. Then add dropwise 700 mL of an aqueous solution containing 4 g of silver acetate. The mixture is reacted at 35 °C for 2 h in the dark. After filtering, the mixture is washed with water and ethanol and dried to obtain a tea polyphenol silver complex.

[0025] (3) 2 kg of polyethylene terephthalate and 400 g of tea polyphenol silver complex were mixed and spun in a melt spinning machine. The temperatures in zones 1-5 were 260°C, 275°C, 280°C, 280°C, and 275°C, and the spinning speed was 800-1500 m / min. The fiber was then drawn at a draw ratio of 4 to obtain an antibacterial fiber.

[0026] Comparative Example 1

[0027] (1) 2 kg of polyethylene terephthalate was spun in a melt spinning machine at temperatures of 260°C, 275°C, 280°C, 280°C, and 275°C in zones 1-5 at a spinning speed of 800-1500 m / min, and then drawn at a draw ratio of 4 to obtain fibers.

[0028] Comparative Example 2

[0029] (1) 2 kg of polyethylene terephthalate and 160 g of tea polyphenols were mixed and spun in a melt spinning machine. The temperatures in zones 1-5 were 260°C, 275°C, 280°C, 280°C, and 275°C, and the spinning speed was 800-1500 m / min. The mixture was then drawn at a draw ratio of 4 to obtain fibers.

[0030] Comparative Example 3

[0031] (1) 2 kg of polyethylene terephthalate and 160 g of carboxybenzoate-esterified tea polyphenol (prepared in Example 1) were spun in a melt spinning machine at temperatures of 260°C, 275°C, 280°C, 280°C, and 275°C in zones 1-5 at a spinning speed of 800-1500 m / min, and then drawn at a draw ratio of 4 to obtain fibers.

[0032] Comparative Example 4

[0033] (1) Add 1.5 L of deionized water and 80 g of tea polyphenols into a flask, stir, add acetic acid solution dropwise to adjust the pH to 3, then add 450 mL of an aqueous solution containing 4 g of silver acetate dropwise, and react at 25 ° C for 1 h in the dark. After filtering, wash with water and ethanol, and dry to obtain a tea polyphenol silver complex.

[0034] (2) 2 kg of polyethylene terephthalate and 160 g of tea polyphenol silver complex were mixed and spun in a melt spinning machine. The temperatures in zones 1-5 were 260°C, 275°C, 280°C, 280°C, and 275°C, and the spinning speed was 800-1500 m / min. The fiber was then drawn at a draw ratio of 4 to obtain an antibacterial fiber.

[0035] The antibacterial properties of the fiber are tested according to GB / T 20944.3-2008. The moisture regain is tested according to GB / T 6503-2017. The tensile properties are tested according to GB / T 14344-2022.

[0036] Table 1 Antibacterial properties of fibers

[0037]

[0038] As shown in Table 1, the antibacterial rates of the polyester fibers of Examples 1 to 3 against Escherichia coli and Staphylococcus aureus are as high as 99.9%, with excellent antibacterial properties, and the moisture regain reaches 0.942-2.275%, with excellent hygroscopic properties, while maintaining good breaking strength and mechanical properties. This is mainly due to the addition of tea polyphenol silver complex, in which carboxybenzoate tea polyphenol contains more benzoate structure, which is similar to the benzoate structural unit of PET polyethylene terephthalate, making the tea polyphenol silver complex The compatibility of the compound with PET is good, and the effect on the mechanical properties of PET fiber is very small, so that the fiber has good breaking strength. At the same time, carboxyl benzoate-esterified tea polyphenols contain carboxyl and phenolic hydroxyl hydrophilic groups, which significantly improve the hydrophilicity and moisture regain of the fiber. The tea polyphenol silver complex contains the antibacterial structure of tea polyphenols, and the carboxyl groups it contains have a higher chelating ability for silver ions, which can increase the loading amount of tea polyphenols on silver ion antibacterial agents. The tea polyphenol silver complex is evenly dispersed in the fiber matrix, which significantly improves the antibacterial and bactericidal ability of the fiber.

[0039] In Comparative Example 2, only tea polyphenols were added, which had poor compatibility with PET polyethylene terephthalate, affecting the mechanical properties of the fiber and resulting in lower breaking strength. In addition, tea polyphenols did not contain carboxyl hydrophilic groups, resulting in a lower moisture regain of the fiber than that of the other embodiments. At the same time, tea polyphenols did not complex silver ions, resulting in a low antibacterial rate of the fiber and poor antibacterial and bactericidal ability.

[0040] Comparative Example 3 added carboxybenzoate-esterified tea polyphenols, which did not complex silver ions, had a low antibacterial rate and poor antibacterial and sterilization capabilities.

[0041] Comparative Example 4 uses tea polyphenols to complex silver ions. Tea polyphenols do not contain carboxyl groups, have low chelating ability for silver ions, and have a small silver ion loading capacity, which affects the antibacterial rate. In addition, tea polyphenols do not contain ester groups, have low compatibility with PET, and have poor dispersibility in fibers, resulting in an antibacterial rate lower than that of the various embodiments, and the fiber has a low breaking strength.

[0042] The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, various simple variations of the technical solution of the present invention may be made, including combining the various technical features in any other appropriate manner. These simple variations and combinations should also be regarded as disclosed in the present invention and fall within the scope of protection of the present invention.

Claims

1. A process for preparing antibacterial fiber, characterized in that: The preparation process comprises: Step S1, adding ethyl acetate, tea polyphenols, pyromellitic anhydride, and pyridine into a flask, stirring to react, filtering, rotary evaporating the filtrate, washing, dissolving the product in ethyl acetate, heating for volatilization, cooling for crystallization, and obtaining carboxybenzoic acid esterified tea polyphenols; Step S2, adding deionized water and carboxybenzoic acid esterified tea polyphenols into a flask, stirring, adding dropwise acetic acid solution, and then adding dropwise silver acetate aqueous solution, stirring to react under light protection, filtering, washing, and drying to obtain a tea polyphenol silver complex; Step S3: mixing polyethylene terephthalate and tea polyphenol silver complex, spinning in a melt spinning machine, and then drawing to obtain antibacterial fiber.

2. The preparation process of the antibacterial fiber according to claim 1, characterized in that: In step S1, the amount of tea polyphenols used is 420-590 parts by weight, the amount of pyromellitic anhydride is 100 parts by weight, and the amount of pyridine is 76-102 parts by weight.

3. The preparation process of the antibacterial fiber according to claim 1, characterized in that: The reaction temperature in step S1 is 50-70° C., and the reaction time is 12-24 hours.

4. The preparation process of the antibacterial fiber according to claim 1, characterized in that: In step S2, acetic acid solution is added dropwise to adjust the pH to 3-3.

5.

5. The preparation process of the antibacterial fiber according to claim 1, characterized in that: In step S2, the amount of carboxybenzoate-esterified tea polyphenols used is 100 parts by weight, and the amount of silver acetate used is 5-8 parts by weight.

6. The process for preparing the antibacterial fiber according to claim 1, characterized in that: The reaction temperature in S2 is 20-35° C., and the reaction time is 1-3 h.

7. The process for preparing the antibacterial fiber according to claim 1, characterized in that: The amount of polyethylene terephthalate in S3 is 100 parts by weight, and the amount of tea polyphenol silver complex is 8-20 parts by weight.

8. The process for preparing the antibacterial fiber according to claim 1, characterized in that: The spinning temperature of the melt spinning machine in S3 is 260-280° C. in zones 1-5, and the spinning speed is 800-1500 m / min.

9. An antibacterial fiber obtained by the preparation process according to any one of claims 1 to 8.

10. A polyester textile fabric made of the antibacterial fiber according to claim 9.

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