Antibacterial cotton fiber blended yarn and method for manufacturing the same

By blending polyester, cotton, and wool fibers and treating them with acrylic emulsion, the problems of easy hydrolysis and poor hydrophilicity of polyester fibers in acidic environments were solved, and a blended yarn with excellent antibacterial and hydrophilic properties was prepared.

CN118147799BActive Publication Date: 2025-12-26YINGJIANG DAJINGWEI TEXTILE CO LTD
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Patent Information

Application Number
CN202410236745.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-03-01
Publication Date
2025-12-26
Estimated Expiration
2044-03-01

AI Technical Summary

Technical Problem

The polyester fibers in existing blended yarns are prone to hydrolysis in acidic environments and have poor hydrophilicity, which cannot meet consumer demand.

Method used

The blended yarn is made by spinning polyester, cotton, and wool fibers in parallel. An acrylic emulsion is formed by copolymerizing acrylic monomers, allyl catechol, and antibacterial agents. This emulsion is then used to impregnate the blended yarn, thereby improving its antibacterial properties and hydrophilicity.

Benefits of technology

The prepared antibacterial cotton fiber blended yarn retains excellent antibacterial and hydrophilic properties after multiple washes, and its acid corrosion resistance is improved, making it highly practical.

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Abstract

The application relates to the technical field of blended yarn, in particular to an antibacterial cotton fiber blended yarn and a preparation method thereof. The scheme is that polyester fibers, cotton fibers and wool fibers are blended to form blended yarn, acrylic ester monomers, allyl-containing o-diphenol and antibacterial agents are used as reaction monomers to copolymerize to form an acrylic ester emulsion, the blended yarn is immersed in the acrylic ester emulsion, and the yarn with the surface immersed with the acrylic ester emulsion is formed after drying. The yarn has excellent hydrophilic performance, good antibacterial performance, long-term durability and excellent antibacterial performance after multiple washes.
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Description

TECHNICAL FIELD

[0001] The application relates to the technical field of blended yarns, in particular to an antibacterial cotton fiber blended yarn and a preparation method thereof. BACKGROUND

[0002] The blended yarn refers to yarn spun by two or more than two different fibers according to a certain proportion, such as polyester-cotton blended yarn, polyester-viscose blended yarn and the like; when the blended yarn is prepared, polyester fibers and cotton fibers are generally used for blending, but the polyester fibers have poor acid corrosion resistance because the polyester fibers will hydrolyze in an acidic environment, and the polyester fibers have poor hydrophilicity, so that the polyester fibers cannot meet the needs of consumers in actual application.

[0003] Therefore, based on the situation, the application discloses an antibacterial cotton fiber blended yarn and a preparation method thereof, the surface hydrophilic finishing of the polyester fibers is performed, and the antibacterial performance of the blended yarn is improved, which is a technical problem to be solved by the application. SUMMARY

[0004] The application aims to provide an antibacterial cotton fiber blended yarn and a preparation method thereof to solve the problems in the background.

[0005] In order to solve the above technical problems, the application provides the following technical scheme:

[0006] A preparation method of an antibacterial cotton fiber blended yarn, comprising the following steps:

[0007] (1) mixing an emulsifier and deionized water, stirring uniformly to obtain an emulsifier solution; mixing an initiator and deionized water, stirring uniformly to obtain an initiator solution;

[0008] mixing an acrylic ester monomer and an allyl-containing catechol, adding 1 / 2 mass fraction of the emulsifier solution, stirring and dispersing for 15-20 min, adding an antibacterial agent and the remaining 1 / 2 mass fraction of the emulsifier solution, continuing to stir and disperse for 15-20 min, heating to 75-80 DEG C under a nitrogen environment, adding the initiator solution, and keeping warm for 5-6 h, and cooling to room temperature to obtain an acrylic ester emulsion;

[0009] (2) blending and spinning the polyester fibers, the cotton fibers and the wool fibers to form a blended yarn, immersing the blended yarn in the acrylic ester emulsion for 20-30 min, pre-drying at 100-110 DEG C for 3-5 min, and drying at 140-150 DEG C to obtain a finished product.

[0010] In the preferred scheme, in the step (2), the mass ratio of the polyester fibers, the cotton fibers and the wool fibers is (6-7) :(1-2) :1.

[0011] In the step (1), the emulsifier is a mixture of cetyltrimethylammonium bromide and fatty alcohol polyoxyethylene ether, and the mass ratio is 2:3; the concentration of the emulsifier solution is 30-40 g / L; the amount of the emulsifier is 5-6 wt% of the total amount of the acrylate monomers; the concentration of the initiator solution is 8-10 g / L; the amount of the initiator is 1.5-2 wt% of the total amount of the acrylate monomers; and the initiator is potassium persulfate.

[0012] In the step (1), the acrylate monomers are a mixture of methyl methacrylate, butyl acrylate, hydroxyethyl methacrylate and acrylic acid, and the mass ratio is 6:8:5:1; the amount of the catechol containing allyl group is 4-5 wt% of the total amount of the acrylate monomers; the antibacterial agent is a mixture of eugenol and eugenol containing epoxy group, and the mass ratio is 1:2; and the amount of the antibacterial agent is 4-6 wt% of the total amount of the acrylate monomers.

[0013] In the step (1), the acrylate monomers are a mixture of methyl methacrylate, butyl acrylate, hydroxyethyl methacrylate and acrylic acid, and the mass ratio is 6:8:5:1; the amount of the catechol containing allyl group is 4-5 wt% of the total amount of the acrylate monomers; the antibacterial agent is a mixture of eugenol and eugenol containing epoxy group, and the mass ratio is 1:2; and the amount of the antibacterial agent is 4-6 wt% of the total amount of the acrylate monomers.

[0014] In the step (1), the acrylate monomers are a mixture of methyl methacrylate, butyl acrylate, hydroxyethyl methacrylate and acrylic acid, and the mass ratio is 6:8:5:1; the amount of the catechol containing allyl group is 4-5 wt% of the total amount of the acrylate monomers; the antibacterial agent is a mixture of eugenol and eugenol containing epoxy group, and the mass ratio is 1:2; and the amount of the antibacterial agent is 4-6 wt% of the total amount of the acrylate monomers.

[0015] In the step (1), the acrylate monomers are a mixture of methyl methacrylate, butyl acrylate, hydroxyethyl methacrylate and acrylic acid, and the mass ratio is 6:8:5:1; the amount of the catechol containing allyl group is 4-5 wt% of the total amount of the acrylate monomers; the antibacterial agent is a mixture of eugenol and eugenol containing epoxy group, and the mass ratio is 1:2; and the amount of the antibacterial agent is 4-6 wt% of the total amount of the acrylate monomers.

[0016] In the step (1), the acrylate monomers are a mixture of methyl methacrylate, butyl acrylate, hydroxyethyl methacrylate and acrylic acid, and the mass ratio is 6:8:5:1; the amount of the catechol containing allyl group is 4-5 wt% of the total amount of the acrylate monomers; the antibacterial agent is a mixture of eugenol and eugenol containing epoxy group, and the mass ratio is 1:2; and the amount of the antibacterial agent is 4-6 wt% of the total amount of the acrylate monomers.

[0017] In the step (1), the acrylate monomers are a mixture of methyl methacrylate, butyl acrylate, hydroxyethyl methacrylate and acrylic acid, and the mass ratio is 6:8:5:1; the amount of the catechol containing allyl group is 4-5 wt% of the total amount of the acrylate monomers; the antibacterial agent is a mixture of eugenol and eugenol containing epoxy group, and the mass ratio is 1:2; and the amount of the antibacterial agent is 4-6 wt% of the total amount of the acrylate monomers.

[0018] In the step (1), the acrylate monomers are a mixture of methyl methacrylate, butyl acrylate, hydroxyethyl methacrylate and acrylic acid, and the mass ratio is 6:8:5:1; the amount of the catechol containing allyl group is 4-5 wt% of the total amount of the acrylate monomers; the antibacterial agent is a mixture of eugenol and eugenol containing epoxy group, and the mass ratio is 1:2; and the amount of the antibacterial agent is 4-6 wt% of the total amount of the acrylate monomers.

[0019] The blended yarn is prepared by the preparation method of the antibacterial blended yarn according to any one of the preceding solutions.

[0020] Compared with the prior art, the present application has the following beneficial effects:

[0021] The application discloses a preparation method of an antibacterial blended yarn of cotton fibers, which comprises the following steps: blending polyester fibers, cotton fibers and wool fibers to form a blended yarn; introducing 2-(oxo-methyl allyl) phenol, potassium carbonate and methyl chloroacrylate as reaction components to prepare 2-(oxo-methyl allyl) phenol; performing a Claisen rearrangement at high temperature to obtain 3-methyl allyl-1,2-benzene diol and 4-methyl allyl-1,2-benzene diol; introducing the 2-(oxo-methyl allyl) phenol as a reaction monomer into an acrylic ester emulsion polymerization; and introducing an antibacterial agent to realize antibacterial modification of the blended yarn.

[0022] The 2-(oxo-methyl allyl) phenol is prepared by the reaction of the components of 2-(oxo-methyl allyl) phenol, potassium carbonate and methyl chloroacrylate, and then the Claisen rearrangement is performed at high temperature to obtain the 3-methyl allyl-1,2-benzene diol and 4-methyl allyl-1,2-benzene diol mixture. The 2-(oxo-methyl allyl) phenol is introduced as a reaction monomer into the acrylic ester emulsion polymerization, and has the following technical effects: the 2-(oxo-methyl allyl) phenol group is introduced into the system, the acrylic ester emulsion can be effectively attached to the surface of the blended yarn, so that the blended yarn still has excellent antibacterial performance and hydrophilic performance after multiple washes.

[0023] Meanwhile, the antibacterial agent is introduced, the eugenol, benzyl triethyl ammonium chloride and epichlorohydrin are used as reaction components to graft the epoxy group on the eugenol to obtain the eugenol containing the epoxy group, and the eugenol containing the epoxy group is compounded with the eugenol as the antibacterial agent. The antibacterial agent participates in the acrylic ester polymerization, so that the antibacterial modification of the blended yarn is realized. The existence of the eugenol containing the epoxy group can improve the crosslinking density of the reaction system, so that the acid corrosion resistance of the blended yarn is improved, so as to solve the problem that the polyester fibers are hydrolyzed under the acidic condition. On the other hand, the antibacterial performance of the eugenol containing the epoxy group is slightly worse than that of the eugenol, so that the eugenol is added and compounded with the eugenol as the antibacterial agent, so that the antibacterial performance of the product can be guaranteed to the maximum extent, and a large amount of antibacterial agent does not need to be added, so that the cost is reduced.

[0024] The application discloses a preparation method of an antibacterial blended yarn of cotton fibers, which comprises the following steps: blending polyester fibers, cotton fibers and wool fibers to form a blended yarn; introducing 2-(oxo-methyl allyl) phenol, potassium carbonate and methyl chloroacrylate as reaction components to prepare 2-(oxo-methyl allyl) phenol; performing a Claisen rearrangement at high temperature to obtain 3-methyl allyl-1,2-benzene diol and 4-methyl allyl-1,2-benzene diol; introducing the 2-(oxo-methyl allyl) phenol as a reaction monomer into an acrylic ester emulsion polymerization; and introducing an antibacterial agent to realize antibacterial modification of the blended yarn. DETAILED DESCRIPTION

[0025] The technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the present application.

[0026] In the embodiment, the fatty alcohol polyoxyethylene ether is AEO-9, which is provided by Shanghai Maikelin; the polyester fiber has a length of 38 mm and a fineness of 1.65 dtex, which is provided by Jiangsu Jiangyin Huahong Chemical Fiber Co., Ltd.; the cotton fiber has a length of 38 mm, a micronaire value of 3.2, and a single fiber strength of 4.3 cN, which is Xinjiang long-staple cotton of grade 1. The wool fiber has a fineness of 4.6 dtex and a length of 50 mm.

[0027] Embodiment 1: A preparation method of an antibacterial cotton fiber blended yarn, comprising the following steps:

[0028] (1) 1.5 g of emulsifier and deionized water are mixed and stirred uniformly to obtain an emulsifier solution; the emulsifier is a compound of 0.6 g of cetyltrimethylammonium bromide and 0.9 g of fatty alcohol polyoxyethylene ether. The concentration of the emulsifier solution is 40 g / L. The amount of the emulsifier is 5 wt% of the total amount of the acrylate monomers.

[0029] 0.6 g of initiator and deionized water are mixed and stirred uniformly to obtain an initiator solution; the initiator is potassium persulfate; the concentration of the initiator solution is 10 g / L. The amount of the initiator is 2 wt% of the total amount of the acrylate monomers.

[0030] 30 g of acrylate monomers, 1.5 g of o-benzene-diol containing allyl groups, 1 / 2 mass fraction of the emulsifier solution, 1.8 g of antibacterial agent, and the remaining 1 / 2 mass fraction of the emulsifier solution are mixed and stirred and dispersed for 15 min, then the temperature is raised to 75 DEG C under a nitrogen environment, the initiator solution is added, and the reaction is carried out for 6 h, and then the temperature is cooled to room temperature to obtain an acrylate emulsion.

[0031] The acrylate monomers are a compound of 9 g of methyl methacrylate, 12 g of butyl acrylate, 7.5 g of hydroxyethyl methacrylate, and 1.5 g of acrylic acid. The amount of the o-benzene-diol containing allyl groups is 5 wt% of the total amount of the acrylate monomers; the antibacterial agent is a compound of 0.6 g of eugenol and 1.2 g of eugenol containing epoxy groups. The amount of the antibacterial agent is 6 wt% of the total amount of the acrylate monomers.

[0032] (2) Spinning polyester fibers, cotton fibers, and wool fibers into a blended yarn, with a mass ratio of 7:2:1; immersing the blended yarn in an acrylate emulsion for 20 minutes, pre-drying at 100°C for 5 minutes, and drying at 140°C to obtain the finished product. The immersion bath ratio is 1:5.

[0033] The preparation steps of the allyl-containing catechol are as follows:

[0034] Step A: Mix 10 g of catechol, 50 g of N,N-dimethylformamide, and 7 g of potassium carbonate, stir until uniform, add 12 g of methyl chloroallyl, and react at 70°C for 15 h. After the reaction is complete, separate the organic phase, purify, and obtain 2-(oxo-methylallyl) phenol.

[0035] Step B: Mix 2-(oxo-methylallyl) phenol with N,N-diethyl aniline, heat to 190°C, and perform a Claisen rearrangement for 3 h. After the reaction is complete, extract and separate, and remove impurities by rotary evaporation to obtain the allyl-containing catechol.

[0036] The preparation steps of the epoxy-containing eugenol are as follows: Mix 0.5 mol of eugenol, benzyl triethyl ammonium chloride, and 0.6 mol of epichlorohydrin, stir until uniform, and stand at 20°C for 14 days. Remove the epichlorohydrin by rotary evaporation at 40°C, add toluene and sodium hydroxide, stir for 5 h, purify, and dry to obtain the epoxy-containing eugenol. The amount of benzyl triethyl ammonium chloride is 12 wt% of the eugenol; the mass ratio of sodium hydroxide to eugenol is 2.1:1.

[0037] Example 2: A method for preparing an antibacterial cotton fiber blended yarn, comprising the following steps:

[0038] (1) Mix 1.5 g of emulsifier and deionized water, stir until uniform, and obtain an emulsifier solution; the emulsifier is a compound of 0.6 g of hexadecyl trimethyl ammonium bromide and 0.9 g of fatty alcohol polyoxyethylene ether. The concentration of the emulsifier solution is 40 g / L. The amount of emulsifier is 5 wt% of the total amount of acrylate monomers.

[0039] Mix 0.6 g of initiator and deionized water, stir until uniform, and obtain an initiator solution; the initiator is potassium persulfate; the concentration of the initiator solution is 10 g / L. The amount of initiator is 2 wt% of the total amount of acrylate monomers.

[0040] 30 g of acrylate monomers, 1.5 g of allyl-containing catechol, 1 / 2 mass fraction of emulsifier solution, stirring and dispersing for 20 min, 1.8 g of antibacterial agent and the remaining 1 / 2 mass fraction of emulsifier solution, continue stirring and dispersing for 20 min, heat to 80℃ under nitrogen environment, add initiator solution, incubate for 5.5 h, cool to room temperature, and obtain an acrylate emulsion.

[0041] The allyl-containing catechol is prepared by the following steps: 10 g of catechol, 50 g of N,N-dimethylformamide, 7 g of potassium carbonate are mixed and stirred uniformly, 12 g of methyl chloroacrylate is added, and the mixture is reacted at 80℃ for 12 h. After the reaction is completed, the organic phase is separated, purified, and 2-(oxo-methylallyl) phenol is obtained.

[0042] (2) Spinning the polyester fiber, cotton fiber and wool fiber in a mass ratio of 7:2:1 to form a blended yarn, immersing the blended yarn in the acrylate emulsion for 25 min, pre-drying at 105℃ for 4 min, and drying at 145℃ to obtain a finished product. The immersion bath ratio is 1:5.

[0043] The allyl-containing catechol is prepared by the following steps:

[0044] Step A: 10 g of catechol, 50 g of N,N-dimethylformamide, 7 g of potassium carbonate are mixed and stirred uniformly, 12 g of methyl chloroacrylate is added, and the mixture is reacted at 80℃ for 12 h. After the reaction is completed, the organic phase is separated, purified, and 2-(oxo-methylallyl) phenol is obtained.

[0045] Step B: 2-(oxo-methylallyl) phenol is mixed with N,N-diethyl aniline, heated to 195℃, and subjected to Claisen rearrangement for 2.5 h. After the reaction is completed, the product is extracted and separated by rotary evaporation to remove impurities, and the allyl-containing catechol is obtained.

[0046] The allyl-containing catechol is prepared by the following steps: 10 g of catechol, 50 g of N,N-dimethylformamide, 7 g of potassium carbonate are mixed and stirred uniformly, 12 g of methyl chloroacrylate is added, and the mixture is reacted at 80℃ for 12 h. After the reaction is completed, the organic phase is separated, purified, and 2-(oxo-methylallyl) phenol is obtained.

[0047] Example 3: A method for preparing an antibacterial cotton fiber blended yarn, comprising the following steps:

[0048] (1) 1.5 g emulsifier and deionized water were mixed and stirred uniformly to obtain an emulsifier solution; the emulsifier was 0.6 g cetyltrimethylammonium bromide and 0.9 g fatty alcohol polyoxyethylene ether compound. The concentration of the emulsifier solution was 40 g / L. The amount of the emulsifier was 5 wt% of the acrylate monomer.

[0049] 0.6 g initiator and deionized water were mixed and stirred uniformly to obtain an initiator solution; the initiator was potassium persulfate; the concentration of the initiator solution was 10 g / L. The amount of the initiator was 2 wt% of the total amount of the acrylate monomer.

[0050] 30 g acrylate monomer, 1.5 g allyl-containing catechol, 1 / 2 mass fraction of the emulsifier solution, stirring and dispersing for 20 min, 1.8 g antibacterial agent and the remaining 1 / 2 mass fraction of the emulsifier solution, continuing to stir and disperse for 20 min, heating to 80℃ under nitrogen, adding the initiator solution, incubating for 5 h, cooling to room temperature, to obtain an acrylate emulsion.

[0051] The acrylate monomer was 9 g methyl methacrylate, 12 g butyl acrylate, 7.5 g hydroxyethyl methacrylate, and 1.5 g acrylic acid compound. The amount of allyl-containing catechol was 5 wt% of the total amount of the acrylate monomer; the antibacterial agent was 0.6 g eugenol and 1.2 g eugenol containing epoxy compound. The amount of the antibacterial agent was 6 wt% of the total amount of the acrylate monomer.

[0052] (2) The polyester fiber, cotton fiber and wool fiber were blended to form a blended yarn, and the mass ratio of the polyester fiber, cotton fiber and wool fiber was 7:2:1; the blended yarn was immersed in the acrylate emulsion for 30 min, pre-dried at 110℃ for 5 min, and dried at 150℃ to obtain a finished product. The immersion bath ratio was 1:5.

[0053] The preparation steps of the allyl-containing catechol were as follows:

[0054] Step A: 10 g catechol, 50 g N,N-dimethylformamide, 7 g potassium carbonate were mixed and stirred uniformly, 12 g methyl chloroacrylate was added, and the reaction was carried out at 90℃ for 10 h. After the reaction was completed, the organic phase was separated and purified to obtain 2-(oxy-methylallyl) phenol.

[0055] Step B: 2-(oxy-methylallyl) phenol and N,N-diethyl aniline were mixed and heated to 200℃ to perform Claisen rearrangement, the rearrangement time was 2 h. After the reaction was completed, extraction separation was performed, and impurities were removed by rotary evaporation to obtain the allyl-containing catechol.

[0056] The preparation steps of the eugenol containing epoxy group are as follows: 0.5 mol of eugenol, benzyl triethyl ammonium chloride and 0.6 mol of epichlorohydrin are mixed, stirred uniformly, and then left to stand at 20°C for 14 days; epichlorohydrin is removed by rotary evaporation at 45°C; toluene and sodium hydroxide are added, stirred for 4 h, purified, dried, and the eugenol containing epoxy group is obtained. The amount of benzyl triethyl ammonium chloride is 12 wt% of eugenol; the mass ratio of sodium hydroxide to eugenol is 2.1:1.

[0057] Comparative Example 1: In Comparative Example 1, eugenol is not added, only eugenol containing epoxy group is used as antibacterial agent, and the rest of the steps and process parameters are the same as those in Example 3.

[0058] A preparation method of an antibacterial cotton fiber blended yarn, comprising the following steps:

[0059] (1) 1.5 g of emulsifier and deionized water are mixed and stirred uniformly to obtain an emulsifier solution; the emulsifier is a compound of 0.6 g of hexadecyl trimethyl ammonium bromide and 0.9 g of fatty alcohol polyoxyethylene ether. The concentration of the emulsifier solution is 40 g / L. The amount of emulsifier is 5 wt% of the total amount of acrylate monomers.

[0060] 0.6 g of initiator and deionized water are mixed and stirred uniformly to obtain an initiator solution; the initiator is potassium persulfate; the concentration of the initiator solution is 10 g / L. The amount of initiator is 2 wt% of the total amount of acrylate monomers.

[0061] 30 g of acrylate monomers, 1.5 g of catechol containing allyl group, 1 / 2 mass fraction of emulsifier solution, 1.8 g of antibacterial agent and the remaining 1 / 2 mass fraction of emulsifier solution are mixed and stirred for 20 min, heated to 80°C under nitrogen environment, 1 / 2 mass fraction of initiator solution is added, and the reaction is carried out for 5 h, and then cooled to room temperature to obtain an acrylate emulsion.

[0062] The acrylate monomers are a compound of 9 g of methyl methacrylate, 12 g of butyl acrylate, 7.5 g of hydroxyethyl methacrylate and 1.5 g of acrylic acid. The amount of catechol containing allyl group is 5 wt% of the total amount of acrylate monomers; the antibacterial agent is eugenol containing epoxy group. The amount of antibacterial agent is 6 wt% of the total amount of acrylate monomers.

[0063] (2) The polyester fiber, cotton fiber and wool fiber are blended and mixed to form a blended yarn, and the mass ratio of the polyester fiber, cotton fiber and wool fiber is 7:2:1; the blended yarn is immersed in the acrylate emulsion for 30 min, pre-dried at 110°C for 5 min, and dried at 150°C to obtain a finished product. The immersion bath ratio is 1:5.

[0064] The preparation steps of the allyl-containing catechol are as follows:

[0065] Step A: 10 g of catechol, 50 g of N,N-dimethylformamide, and 7 g of potassium carbonate are mixed and stirred uniformly, 12 g of methyl chloroallyl is added, and the mixture is reacted at 90°C for 10 h. After the reaction is completed, the organic phase is separated, and purified to obtain 2-(oxo-methylallyl) phenol.

[0066] Step B: 2-(oxo-methylallyl) phenol is mixed with N,N-diethyl aniline, and the mixture is heated to 200°C to perform Claisen rearrangement. The rearrangement time is 2 h. After the reaction is completed, the mixture is extracted and separated, and impurities are removed by rotary evaporation to obtain the allyl-containing catechol.

[0067] The preparation steps of the epoxy-containing eugenol are as follows: 0.5 mol of eugenol, benzyltriethylammonium chloride, and 0.6 mol of epichlorohydrin are mixed, stirred uniformly, and then left to stand at 20°C for 14 days. Epichlorohydrin is removed by rotary evaporation at 45°C. Toluene and sodium hydroxide are added, and the mixture is stirred for 4 h. After purification and drying, the epoxy-containing eugenol is obtained. The amount of the benzyltriethylammonium chloride is 12 wt% of the eugenol. The mass ratio of the sodium hydroxide to the eugenol is 2.1:1.

[0068] Comparative Example 2: The allyl-containing catechol is not added in the comparative example 2, and the remaining steps and process parameters are unchanged.

[0069] (1) 1.5 g of emulsifier and deionized water are mixed and stirred uniformly to obtain an emulsifier solution. The emulsifier is a mixture of 0.6 g of hexadecyltrimethylammonium bromide and 0.9 g of fatty alcohol polyoxyethylene ether. The concentration of the emulsifier solution is 40 g / L. The amount of the emulsifier is 5 wt% of the total amount of the acrylate monomers.

[0070] 0.6 g of initiator and deionized water are mixed and stirred uniformly to obtain an initiator solution. The initiator is potassium persulfate. The concentration of the initiator solution is 10 g / L. The amount of the initiator is 2 wt% of the total amount of the acrylate monomers.

[0071] 30 g of acrylate monomers and 1 / 2 mass fraction of the emulsifier solution are mixed and stirred for 20 min. 1.8 g of the antibacterial agent and the remaining 1 / 2 mass fraction of the emulsifier solution are added, and the mixture is continuously stirred for 20 min. The mixture is heated to 80°C under a nitrogen atmosphere, and the initiator solution is added. The mixture is reacted for 5 h, and then cooled to room temperature to obtain an acrylate emulsion.

[0072] The acrylic ester monomer is 9 g of methyl methacrylate, 12 g of butyl acrylate, 7.5 g of hydroxyethyl methacrylate, and 1.5 g of acrylic acid. The antibacterial agent is 0.6 g of eugenol and 1.2 g of eugenol containing epoxy groups. The amount of the antibacterial agent is 6 wt% of the total amount of the acrylic ester monomers.

[0073] (2) Spinning the blended yarn by blending polyester fibers, cotton fibers, and wool fibers in a mass ratio of 7:2:1; immersing the blended yarn in the acrylic ester emulsion for 30 min, pre-drying at 110°C for 5 min, and drying at 150°C to obtain the finished product. The immersion bath ratio is 1:5.

[0074] The preparation steps of the eugenol containing epoxy groups are as follows: mixing 0.5 mol of eugenol, benzyltriethylammonium chloride, and 0.6 mol of epichlorohydrin, stirring uniformly, standing at 20°C for 14 days, removing epichlorohydrin by rotary evaporation at 45°C, adding toluene and sodium hydroxide, stirring for 4 h, purifying, and drying to obtain eugenol containing epoxy groups. The amount of benzyltriethylammonium chloride is 12 wt% of the eugenol; the mass ratio of sodium hydroxide to eugenol is 2.1:1.

[0075] Comparative Example 3: Using Example 3 as a control group, only eugenol is added in Comparative Example 2, and the remaining steps and process parameters remain unchanged.

[0076] A method for preparing an antibacterial cotton fiber blended yarn, comprising the following steps:

[0077] (1) Mixing 1.5 g of emulsifier and deionized water, stirring uniformly to obtain an emulsifier solution; the emulsifier is 0.6 g of cetyltrimethylammonium bromide and 0.9 g of fatty alcohol polyoxyethylene ether; the concentration of the emulsifier solution is 40 g / L; the amount of the emulsifier is 5 wt% of the acrylic ester monomers.

[0078] Mixing 0.6 g of initiator and deionized water, stirring uniformly to obtain an initiator solution; the initiator is potassium persulfate; the concentration of the initiator solution is 10 g / L; the amount of the initiator is 2 wt% of the total amount of the acrylic ester monomers.

[0079] Mixing 30 g of acrylic ester monomers and 1.5 g of o-benzene diol containing allyl groups, adding 1 / 2 mass fraction of the emulsifier solution, stirring and dispersing for 20 min, adding 1.4 g of antibacterial agent and the remaining 1 / 2 mass fraction of the emulsifier solution, continuing to stir and disperse for 20 min, heating to 80°C under nitrogen environment, adding the initiator solution, and incubating for 5 h to obtain an acrylic ester emulsion.

[0080] The acrylic ester monomer is 9 g of methyl methacrylate, 12 g of butyl acrylate, 7.5 g of hydroxyethyl methacrylate, and 1.5 g of acrylic acid. The allyl-containing catechol is used in an amount of 5 wt% of the total amount of the acrylic ester monomer; and the antibacterial agent is eugenol.

[0081] (2) Spinning the polyester fiber, cotton fiber, and wool fiber in a mass ratio of 7:2:1 to form a blended yarn, immersing the blended yarn in an acrylic ester emulsion for 30 min, pre-drying at 110°C for 5 min, and drying at 150°C to obtain a finished product. The immersion bath ratio is 1:5.

[0082] The preparation steps of the allyl-containing catechol are as follows:

[0083] Step A: Mixing 10 g of catechol, 50 g of N,N-dimethylformamide, and 7 g of potassium carbonate, stirring uniformly, adding 12 g of methyl chloroacrylate, and reacting at 90°C for 10 h. After the reaction is completed, the organic phase is separated, purified, and 2-(oxo-methylallyl) phenol is obtained.

[0084] Step B: Mixing 2-(oxo-methylallyl) phenol with N,N-diethyl aniline, heating to 200°C, and performing Claisen rearrangement for 2 h. After the reaction is completed, the product is extracted and separated by rotary evaporation to remove impurities, and the allyl-containing catechol is obtained.

[0085] Detection experiment:

[0086] The blended yarns prepared in Examples 1-3 and Comparative Examples 1-3 are knitted into fabrics, and the fabric weight is 200 g / cm 2 ; and the following performance tests are performed:

[0087] 1. Antibacterial property: The antibacterial property of the fabric is tested according to the method disclosed in GB / T20944.3-2008 “Evaluation of antibacterial property of textiles Part 3: oscillation method”, and the test bacteria is Escherichia coli.

[0088] A standard washing procedure is performed on a 10 cm x 10 cm fabric: washing in 150 mL of water at 40°C for 60 min, and then rinsing with 100 mL of deionized water. The washing procedure is repeated 15 times, and the antibacterial property of the fabric is retested.

[0089] 2. A 5 cm x 5 cm fabric is immersed in a 1.28 specific gravity sulfuric acid solution at 70°C for 168 h, washed to neutral after being taken out, and vacuum dried at 100°C. The weight of the fabric before and after immersion is recorded, and the weight loss rate is calculated.

[0090] 3. Place 5cm x 5cm fabric in deionized water, soak for 24h at 25℃, take out and wipe off surface moisture, record the weight of the fabric before and after soaking, and record the water absorption rate.

[0091] Item Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Antibacterial rate % 99.1% 99.2% 99.2% 97.6% 99.1% 99.4% Antibacterial rate % after 15 washes 94.2% 94.4% 94.5% 92.7% 88.4% 91.3% Weight loss rate % 0.47% 0.45% 0.44% 0.46% 0.52% 0.68% Water absorption rate % 34.4% 35.2% 35.6% / / /

[0092] Conclusion: The application discloses a preparation method of antibacterial cotton fiber blended yarn, which adjusts the yarn ratio of the blended yarn, and impregnates the surface of the blended yarn with an acrylate solution, so that the prepared blended yarn has excellent antibacterial performance, improved acid corrosion resistance, long-term durability, and high practicality.

[0093] Finally, it should be noted that: the above only for the preferred embodiments of the application, and not for limiting the application, although the application is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still can be modified to the technical scheme recorded in the foregoing embodiments, or equivalent replacement of some technical features. Any modification, equivalent replacement, improvement, etc. within the spirit and principles of the application shall be included in the protection scope of the application.

Claims

1. A method for preparing an antibacterial blended yarn of cotton fiber, characterized by: The method comprises the following steps: (1) mixing emulsifier and deionized water, stirring uniformly to obtain an emulsifier solution; mixing initiator and deionized water, stirring uniformly to obtain an initiator solution; The acrylic ester monomer and the allyl-containing catechol are mixed, 1 / 2 mass fraction of the emulsifier solution is added, stirring and dispersing for 15-20 min, the antibacterial agent and the remaining 1 / 2 mass fraction of the emulsifier solution are added, and stirring and dispersing is continued for 15-20 min, the temperature is raised to 75-80℃ under nitrogen atmosphere, the initiator solution is added, and reaction is carried out for 5-6 h, and the temperature is cooled to room temperature, to obtain an acrylic ester emulsion; (2) blending and spinning the polyester fiber, the cotton fiber and the wool fiber to form blended yarn, immersing the blended yarn in the acrylic ester emulsion for 20-30 min, pre-drying at 100-110℃ for 3-5 min, and drying at 140-150℃ to obtain a finished product; In step (1), the acrylic ester monomer is a mixture of methyl methacrylate, butyl acrylate, hydroxyethyl methacrylate and acrylic acid, and the mass ratio is 6:8:5:1; the allyl-containing catechol is used in an amount of 4-5 wt% of the total amount of the acrylic ester monomer; the antibacterial agent is a mixture of eugenol and eugenol containing epoxy groups, and the mass ratio is 1:2; and the antibacterial agent is used in an amount of 4-6 wt% of the total amount of the acrylic ester monomer. The preparation steps of the eugenol containing epoxy groups are as follows: mixing eugenol, benzyltriethylammonium chloride and epichlorohydrin, stirring uniformly, standing at 15-20℃ for 12-14 days, removing epichlorohydrin by rotary evaporation at 40-45℃, adding toluene and sodium hydroxide, stirring for 4-5 h, purifying, and drying to obtain the eugenol containing epoxy groups.

2. A method of producing an antibacterial blended yarn of cotton fiber according to claim 1, characterized in that: In step (2), the mass ratio of the polyester fiber, the cotton fiber and the wool fiber is (6-7):(1-2):

1.

3. A method of producing an antibacterial blended yarn of cotton fiber according to claim 1, characterized in that: In step (1), the emulsifier is a mixture of cetyltrimethylammonium bromide and fatty alcohol polyoxyethylene ether, and the mass ratio is 2:3; the emulsifier is used in an amount of 5-6 wt% of the acrylic ester monomer; and the initiator is potassium persulfate, and the initiator is used in an amount of 1.5-2 wt% of the total amount of the acrylic ester monomer.

4. A method of producing an antibacterial blended yarn of cotton fiber according to claim 1, characterized in that: The preparation steps of the allyl-containing catechol are as follows: Step A: mixing catechol, N,N-dimethylformamide and potassium carbonate, stirring uniformly, adding methyl chloroacrylate, and reacting at 70-90℃ for 10-15 h; after the reaction is completed, the organic phase is separated, and purified to obtain 2-(oxo-methylallyl)phenol; Step B: mixing 2-(oxo-methylallyl)phenol and N,N-diethylphenylamine, heating to 190-200℃, performing Claisen rearrangement for 2-3 h, after the reaction is completed, extracting and separating, and removing impurities by rotary evaporation to obtain the allyl-containing catechol.

5. The method for preparing an antibacterial cotton fiber blended yarn according to claim 4, characterized in that: In step A, the mass ratio of the catechol, potassium carbonate, methyl chloroacrylate and N,N-dimethylformamide is 1:(0.7-0.8):(1-1.2):(5-5.2).

6. A method of producing an antibacterial blended yarn of cotton fiber according to claim 1, characterized in that: The molar ratio of the eugenol and epichlorohydrin is 1:(1-1.2); and the amount of the benzyltriethylammonium chloride is 10-15 wt% of the eugenol.

7. A blended yarn prepared according to the method of any one of claims 1 to 6.

Citation Information

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