Grafted long-acting and washable antibacterial fabric and preparation method thereof

By forming covalent bonds with cellulose-based fabrics, the problem of easy loss of antibacterial agents in traditional antibacterial fabrics is solved, and the preparation of grafted long-acting antibacterial fabrics is realized, which significantly improves the washing resistance and long-lasting antibacterial fabrics. Effect.

CN119308140APending Publication Date: 2025-01-14ROCKET FORCE UNIV OF ENG
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Patent Information

Application Number
CN202411737925.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-29
Publication Date
2025-01-14

AI Technical Summary

Technical Problem

The antibacterial agents of traditional antibacterial fabrics are easily lost, and their antibacterial properties are greatly reduced, resulting in poor antibacterial protection in humid environments.

Method used

By chemically modifying the polyhexamethyleneguanidine hydrochloride, a PHMG-based antibacterial agent is prepared and covalent bonds are formed with the cellulose-based fabric to prepare a grafted long-acting and water-resistant antibacterial fabric.

Benefits of technology

The firm combination between the antibacterial agent and the fabric is achieved, which significantly improves the washing resistance and long-lasting antibacterial effect of the antibacterial fabric, ensuring that it still has excellent antibacterial properties after multiple washes.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a grafted long-acting and washable antibacterial fabric and a preparation method thereof, and the preparation method comprises the following steps: carrying out chemical modification on polyhexamethylene guanidine hydrochloride through epoxide to prepare a PHMG-based antibacterial agent; the fabric is soaked in an N, N-dimethylformamide solution containing the PHMG-based antibacterial agent, the PHMG-based antibacterial agent reacts with the fabric, and the grafted long-acting and washable antibacterial fabric is obtained. The PHMG-based antibacterial agent is combined to the surface of the fabric through a chemical grafting method, so that the PHMG-based antibacterial agent and the fabric have stable binding force, and the long-acting antibacterial function and washing resistance are achieved at the same time.
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Description

Technical Field

[0001] The invention belongs to the technical field of polymer materials and relates to a grafted long-lasting and washable antibacterial fabric and a preparation method thereof. Background Art

[0002] Conventional fabrics are prone to adsorbing and breeding bacteria due to their strong moisture absorption properties. This not only causes the fabric fibers to fade and the mechanical strength to decrease, but may also produce odors, increase the risk of infection and disease transmission, and even endanger the life and health of the user in severe cases. Therefore, it is particularly important to give fabrics antibacterial properties to effectively reduce the harm of bacteria to the human body.

[0003] At present, antibacterial textiles have a weak adhesion to the antibacterial agent, which is easily reduced in antibacterial effect due to friction during washing or use. In order to enhance the binding force between the antibacterial agent and the fiber and improve the durability and antibacterial persistence of the antibacterial fabric, a new method for preparing antibacterial fabrics needs to be developed.

[0004] The present invention aims to meet the demand for antibacterial protective textiles in humid environments, break through the synthesis of highly efficient, durable, low-toxic and comfortable antibacterial agents, and the green and environmentally friendly reactive processing technology of fabrics, and solve the technical bottleneck of easy loss of antibacterial agents in traditional antibacterial fabrics and significantly reduced antibacterial properties. Summary of the invention

[0005] In order to solve the technical bottleneck that the antibacterial agent of traditional antibacterial fabrics is easy to lose and the antibacterial performance is greatly reduced, the purpose of the present invention is to provide a grafted long-lasting and washable antibacterial fabric and a preparation method thereof. The antibacterial agent in the antibacterial fabric prepared by this method forms a strong covalent bond with the fabric, is not easy to lose, has a long-lasting antibacterial function and washing resistance.

[0006] To achieve the above purpose, the technical solution adopted by the present invention is as follows: A method for preparing a grafted long-lasting and washable antibacterial fabric comprises the following steps: Polyhexamethyleneguanidine hydrochloride was chemically modified by epoxide to prepare PHMG-based antimicrobial agent; The fabric is immersed in an N,N-dimethylformamide solution containing a PHMG-based antibacterial agent, and the PHMG-based antibacterial agent reacts with the fabric to obtain a grafted, long-lasting, washable antibacterial fabric.

[0007] Further, polyhexamethyleneguanidine hydrochloride is chemically modified by epoxide to prepare a PHMG-based antibacterial agent, comprising the following steps: adding epoxide to an ethanol solution of polyhexamethyleneguanidine hydrochloride, and then o C, add a catalyst to obtain a mixture, and heat the mixture at 30-60 oC for 12-24 hours to obtain a PHMG-based antibacterial agent solution.

[0008] Furthermore, the mass concentration of the N,N-dimethylformamide solution of the PHMG-based antibacterial agent is 0.5-2.5%.

[0009] Furthermore, the epoxide is any one of epichlorohydrin, propylene oxide and diglycidyl ether. Furthermore, the catalyst is one of triethylamine and potassium hydroxide.

[0010] Further, in the mixture, the concentration of PHMG is 5-10 wt %, the concentration of epoxide is 0.5-1 mol / L, and the concentration of catalyst is 0.1-0.3 mol / L.

[0011] Furthermore, the temperature at which the HMG-based antimicrobial agent reacts with the fabric is 60-100 o C, time is 2-3 h.

[0012] Furthermore, the fabric is a cellulose-based fabric or a fabric in which the mass ratio of the cellulose-based fabric in the fabric is greater than 20%.

[0013] Furthermore, the cellulose-based fabric raw material is any one of cotton, viscose fiber, modal, tencel, cupro fiber and acetate fiber.

[0014] A grafted, long-lasting, washable antibacterial fabric.

[0015] Compared with the prior art, the present invention has the following beneficial effects: The present invention prepares a PHMG-based antibacterial agent by modifying polyhexamethyleneguanidine hydrochloride with epoxide. The reaction mechanism is that the epoxy group opens the ring to form new hydroxyl groups and ether bonds, which react with the amino group (-NH2) or guanidine group (-C(NH)-NH2) of PHMG by nucleophilic reaction and covalent bonding to form a stable modified polymer chain. The antibacterial agent is impregnated into the surface of the fabric to prepare the antibacterial fabric. Compared with the prior art, the present invention solves the problem of high molecular weight polymer antibacterial agent dissolving on the material surface, and well combines the antibacterial functional components with the fabric to achieve a lasting antibacterial effect, so as to achieve washing resistance.

[0016] Further, polyhexamethyleneguanidine hydrochloride and epoxide are reacted at 30-60 o C for 12-24h to avoid all epoxy groups from reacting with the amine groups of PHMG.

[0017] Furthermore, the PHMG-based antimicrobial agent reacts with the fabric at a temperature of 60-100 o C, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 is the chemical reaction formula for synthesizing PHMG of the present invention; Figure 2 is the chemical reaction formula of propylene oxide modified PHMG; Figure 3 is the chemical reaction formula of epichlorohydrin modified PHMG; Figure 4 It is the chemical reaction formula of diglycidyl ether modified PHMG. Specific embodiments In order to facilitate the understanding of the present invention, the present invention will be described more fully below with reference to the relevant drawings. The preferred embodiments of the present invention are given in the drawings. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thoroughly and comprehensively understood.

[0020] The method for preparing a grafted long-lasting and washable antibacterial fabric of the present invention comprises the following steps: 1) Add guanidine hydrochloride, hexamethyleneamine and DMF into the reactor, stir to make guanidine hydrochloride and hexamethyleneamine fully mixed and completely dissolved in N,N-dimethylformamide (DMF), and then heat to 80-150 o C, polyethylene glycol is added during the heating process, and the reaction is continued for 2-3 hours until no NH3 is released in the reactor, and the reaction is completed to obtain polyhexamethyleneguanidine hydrochloride (PHMG), i.e., a polymer antibacterial agent precursor. PHMG contains a large number of amine and guanidine structures.

[0021] The mass ratio of guanidine hydrochloride to hexamethyleneamine is 1:1, and the total mass fraction of guanidine hydrochloride and hexamethyleneamine is 15-30wt%.

[0022] Polyethylene glycol is used as a catalyst, and the usage amount of polyethylene glycol is 0.5-1% of the total mass of guanidine hydrochloride and hexamethylenediamine.

[0023] The degree of polymerization of polyhexamethyleneguanidine hydrochloride is greater than 1500.

[0024] 2) The polymer antibacterial agent precursor obtained in step 1) is chemically modified by epoxide to prepare a high molecular weight polymer PHMG-based antibacterial agent. Specifically, the PHMG in step 1) is uniformly dissolved in anhydrous ethanol, epoxide is slowly added dropwise, and heated (30-60 °C) under slow stirring. oC), then add the catalyst, and then react for 12-24 hours. After the reaction, use one of saturated sodium chloride and dilute hydrochloric acid (4 mol / L) for neutralization to precipitate the by-products. After washing the product, dissolve it in DMF to obtain a PHMG-based antibacterial agent solution. The concentration of PHMG in anhydrous ethanol is 5-10wt%, the concentration of epoxide is 0.5-1mol / L, and the concentration of the catalyst is 0.1-0.3 mol / L.

[0025] Wherein, the epoxide is any one of epichlorohydrin, propylene oxide and diglycidyl ether. The catalyst is one of triethylamine and potassium hydroxide.

[0026] The reaction mechanism in step 2) is that the epoxy group opens the ring to form new hydroxyl and ether bonds, which react with the amino group (-NH2) or guanidine group (-C(NH)-NH2) of PHMG to form a stable modified polymer chain.

[0027] The key to the reaction process in step 2) is to control the reaction conditions to avoid all epoxy groups from reacting with the amine groups of PHMG.

[0028] 3) Immerse a certain amount of fabric in the PHMG-based antimicrobial agent solution prepared in step 2) (the mass concentration of the PHMG-based antimicrobial agent solution is 0.5-2.5%; the solvent is DMF), and the reaction temperature is 60-100 o C, time 2-3 h, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric.

[0029] Wherein, the fabric is any one of cotton fabric, cellulose-based fabric and synthetic fiber-based fabric.

[0030] Preferably, the cellulose-based fabric is any one of viscose fiber, cuprammonium fiber and acetate fiber, and the synthetic fiber-based fabric is any one of polyester fiber, nylon and polypropylene fiber.

[0031] The reaction process in step 3) occurs between the hydroxyl groups on the fabric polymer chain and the epoxy groups. Through the ring-opening reaction, the PHMG-based antimicrobial agent is covalently bonded to the hydroxyl groups on the fabric polymer chain.

[0032] According to the grafted long-lasting and washable antibacterial fabric prepared by the method as described above, the grafting rate of the antibacterial agent on the textile is 4-20.5%.

[0033] The following are specific embodiments.

[0034] Example 1 1) See Figure 1, add guanidine hydrochloride, hexamethyleneamine and DMF into the reaction kettle, stir to make guanidine hydrochloride and hexamethyleneamine fully mixed and completely dissolved in N,N-dimethylformamide (DMF), and then heat to 80 o C, polyethylene glycol was added during the heating process, and the reaction was continued for 3 hours until no NH3 was released from the reactor, and the reaction was completed to obtain polyhexamethyleneguanidine hydrochloride (PHMG). The mass ratio of guanidine hydrochloride to hexamethyleneamine is 1:1, and the total mass fraction of guanidine hydrochloride and hexamethyleneamine is 15 wt %.

[0035] Polyethylene glycol is used as a catalyst, and the usage amount of polyethylene glycol is 0.5% of the total weight of guanidine hydrochloride and hexamethylenediamine.

[0036] 2) See Figure 2 , dissolve the PHMG in step 1) uniformly in anhydrous ethanol, slowly add propylene oxide dropwise, and heat to 30 o C, add catalyst triethylamine, and keep warm for 6 hours. After the reaction is completed, add appropriate amount of hydrochloric acid (4 mol / L) for neutralization. After washing, the product is dissolved in DMF to obtain a PHMG-based antibacterial agent solution (mass concentration is 0.5%). The concentration of PHMG in anhydrous ethanol is 5wt%, the concentration of propylene oxide is 0.5 mol / L, and the concentration of the catalyst is 0.1 mol / L.

[0037] 3) Immerse a certain amount of fabric in the PHMG-based antimicrobial agent solution obtained in step 2) at a reaction temperature of 60 o C, time 2 h, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric.

[0038] Example 2 1) Add guanidine hydrochloride, hexamethyleneamine and DMF into the reactor, stir to make guanidine hydrochloride and hexamethyleneamine fully mixed and completely dissolved in N,N-dimethylformamide (DMF), and then heat to 150 o C, polyethylene glycol was added during the heating process, and the reaction was continued for 2 hours until no NH3 was released from the reactor, and the reaction was completed to obtain polyhexamethyleneguanidine hydrochloride (PHMG). The mass ratio of guanidine hydrochloride to hexamethyleneamine is 1:1, and the total mass fraction of guanidine hydrochloride and hexamethyleneamine is 20 wt %.

[0039] Polyethylene glycol is used as a catalyst, and the usage amount of polyethylene glycol is 1% of the total mass of guanidine hydrochloride and hexamethylenediamine.

[0040] 2) See Figure 3, dissolve the PHMG in step 1) uniformly in anhydrous ethanol, slowly add epichlorohydrin dropwise, and heat to 40 o C, add potassium hydroxide as catalyst, and keep warm for 3 hours. After the reaction is completed, add an appropriate amount of hydrochloric acid (4 mol / L) for neutralization. After washing, the product is dissolved in DMF to obtain a PHMG-based antibacterial agent solution (mass concentration is 1.2%). The concentration of PHMG in anhydrous ethanol is 10wt%, the concentration of propylene oxide is 0.5 mol / L, and the concentration of the catalyst is 0.3 mol / L.

[0041] 3) Immerse a certain amount of fabric in the PHMG-based antimicrobial agent solution obtained in step 2) at a reaction temperature of 60 o C, time 2 h, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric.

[0042] Example 3 1) Add guanidine hydrochloride, hexamethyleneamine and DMF into the reactor, stir to make guanidine hydrochloride and hexamethyleneamine fully mixed and completely dissolved in N,N-dimethylformamide (DMF), and then heat to 100 o C, polyethylene glycol was added during the heating process, and the reaction was continued for 2.5 hours until no NH3 was released from the reactor, and the reaction was completed to obtain polyhexamethyleneguanidine hydrochloride (PHMG). The mass ratio of guanidine hydrochloride to hexamethyleneamine is 1:1, and the total mass fraction of guanidine hydrochloride and hexamethyleneamine is 30 wt %.

[0043] Polyethylene glycol is used as a catalyst, and the usage amount of polyethylene glycol is 0.6% of the total weight of guanidine hydrochloride and hexamethylenediamine.

[0044] 2) See Figure 4 , dissolve the PHMG in step 1) uniformly in anhydrous ethanol, slowly add diglycidyl ether dropwise, and heat to 40 o C, add catalyst triethylamine, and keep warm for 10 hours. After the reaction is completed, add appropriate amount of hydrochloric acid (4 mol / L) for neutralization. After washing, the product is dissolved in DMF to obtain a PHMG-based antibacterial agent solution (mass concentration is 0.8%). The concentration of PHMG in anhydrous ethanol is 7wt%, the concentration of diglycidyl ether is 0.5 mol / L, and the concentration of the catalyst is 0.1 mol / L.

[0045] 3) Immerse a certain amount of fabric in the PHMG-based antimicrobial agent solution obtained in step 2) at a reaction temperature of 60 o C, time 2 h, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric.

[0046] Example 4 1) Add guanidine hydrochloride, hexamethyleneamine and DMF into the reactor, stir to make guanidine hydrochloride and hexamethyleneamine fully mixed and completely dissolved in N,N-dimethylformamide (DMF), and then heat to 120 o C, polyethylene glycol was added during the heating process, and the reaction was continued for 2.5 hours until no NH3 was released from the reactor, and the reaction was completed to obtain polyhexamethyleneguanidine hydrochloride (PHMG). The mass ratio of guanidine hydrochloride to hexamethyleneamine is 1:1, and the total mass fraction of guanidine hydrochloride and hexamethyleneamine is 25 wt %.

[0047] Polyethylene glycol is used as a catalyst, and the usage amount of polyethylene glycol is 0.8% of the total weight of guanidine hydrochloride and hexamethylenediamine.

[0048] The degree of polymerization of polyhexamethyleneguanidine hydrochloride is greater than 1500.

[0049] 2) Dissolve the PHMG in step 1) evenly in anhydrous ethanol, slowly add propylene oxide dropwise, and heat to 33°C while stirring slowly. o C, add catalyst triethylamine, and keep warm for 5 hours. After the reaction is completed, add appropriate amount of hydrochloric acid (4 mol / L) for neutralization. After washing, the product is dissolved in DMF to obtain a PHMG-based antibacterial agent solution (mass concentration is 0.5%). The concentration of PHMG in anhydrous ethanol is 8wt%, the concentration of propylene oxide is 0.5 mol / L, and the concentration of the catalyst is 0.1 mol / L.

[0050] 3) Immerse a certain amount of fabric in the PHMG-based antimicrobial agent solution obtained in step 2) at a reaction temperature of 60 o C, time 2 h, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric.

[0051] In this embodiment 4, propylene oxide in embodiment 1 is selected to modify the antibacterial precursor, and the optimal concentration is selected by adjusting the concentration of the antibacterial agent.

[0052] Example 5 1) Add guanidine hydrochloride, hexamethyleneamine and DMF into the reactor, stir to make guanidine hydrochloride and hexamethyleneamine fully mixed and completely dissolved in N,N-dimethylformamide (DMF), and then heat to 140 o C, polyethylene glycol was added during the heating process, and the reaction was continued for 2 hours until no NH3 was released from the reactor, and the reaction was completed to obtain polyhexamethyleneguanidine hydrochloride (PHMG). The mass ratio of guanidine hydrochloride to hexamethyleneamine is 1:1, and the total mass fraction of guanidine hydrochloride and hexamethyleneamine is 18 wt %.

[0053] Polyethylene glycol is used as a catalyst, and the usage amount of polyethylene glycol is 0.7% of the total weight of guanidine hydrochloride and hexamethylenediamine.

[0054] The degree of polymerization of polyhexamethyleneguanidine hydrochloride is greater than 1500.

[0055] 2) Dissolve the PHMG in step 1) evenly in anhydrous ethanol, slowly add propylene oxide dropwise, and heat to 38 o C, add catalyst triethylamine, and keep warm for 3 hours. After the reaction is completed, add appropriate amount of hydrochloric acid (4 mol / L) for neutralization. After washing, the product is dissolved in DMF to obtain a PHMG-based antibacterial agent solution (mass concentration is 1.0%). The concentration of PHMG in anhydrous ethanol is 6wt%, the concentration of propylene oxide is 0.6 mol / L, and the concentration of the catalyst is 0.1 mol / L.

[0056] 3) Immerse a certain amount of fabric in the PHMG-based antimicrobial agent solution obtained in step 2) at a reaction temperature of 60 o C, time 2 h, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric.

[0057] Example 6 1) Add guanidine hydrochloride, hexamethyleneamine and DMF into the reactor, stir to make guanidine hydrochloride and hexamethyleneamine fully mixed and completely dissolved in N,N-dimethylformamide (DMF), and then heat to 90 o C, polyethylene glycol was added during the heating process, and the reaction was continued for 3 hours until no NH3 was released from the reactor, and the reaction was completed to obtain polyhexamethyleneguanidine hydrochloride (PHMG). The mass ratio of guanidine hydrochloride to hexamethyleneamine is 1:1, and the total mass fraction of guanidine hydrochloride and hexamethyleneamine is 22 wt %.

[0058] Polyethylene glycol is used as a catalyst, and the usage amount of polyethylene glycol is 0.9% of the total weight of guanidine hydrochloride and hexamethylenediamine.

[0059] The degree of polymerization of polyhexamethyleneguanidine hydrochloride is greater than 1500.

[0060] 2) Dissolve the PHMG in step 1) evenly in anhydrous ethanol, slowly add propylene oxide dropwise, and heat to 40°C while stirring slowly. oC, add catalyst triethylamine, and keep warm for 3 hours. After the reaction is completed, add appropriate amount of hydrochloric acid (4 mol / L) for neutralization. After washing, the product is dissolved in DMF to obtain a PHMG-based antibacterial agent solution (mass concentration is 1.5%). The concentration of PHMG in anhydrous ethanol is 9wt%, the concentration of propylene oxide is 0.8 mol / L, and the concentration of the catalyst is 0.3 mol / L.

[0061] 3) Immerse a certain amount of fabric in the PHMG-based antimicrobial agent solution obtained in step 2) at a reaction temperature of 60 o C, time 2 h, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric.

[0062] Example 7 1) Add guanidine hydrochloride, hexamethyleneamine and DMF into the reactor, stir to make guanidine hydrochloride and hexamethyleneamine fully mixed and completely dissolved in N,N-dimethylformamide (DMF), and then heat to 110 o C, polyethylene glycol was added during the heating process, and the reaction was continued for 2.5 hours until no NH3 was released from the reactor, and the reaction was completed to obtain polyhexamethyleneguanidine hydrochloride (PHMG). The mass ratio of guanidine hydrochloride to hexamethyleneamine is 1:1, and the total mass fraction of guanidine hydrochloride and hexamethyleneamine is 26 wt %.

[0063] Polyethylene glycol is used as a catalyst, and the usage amount of polyethylene glycol is 0.5% of the total weight of guanidine hydrochloride and hexamethylenediamine.

[0064] The degree of polymerization of polyhexamethyleneguanidine hydrochloride is greater than 1500.

[0065] 2) Dissolve the PHMG in step 1) evenly in anhydrous ethanol, slowly add propylene oxide dropwise, and heat to 40°C while stirring slowly. o C, add the catalyst triethylamine, and keep warm for 3-6 hours. After the reaction is completed, add an appropriate amount of hydrochloric acid (4 mol / L) for neutralization. After washing, the product is dissolved in DMF to obtain a PHMG-based antibacterial agent solution (mass concentration is 2.0%). The concentration of PHMG in anhydrous ethanol is 55wt%, the concentration of propylene oxide is 0.7 mol / L, and the concentration of the catalyst is 0.1 mol / L.

[0066] 3) Immerse a certain amount of fabric in the PHMG-based antimicrobial agent solution obtained in step 2) at a reaction temperature of 60 o C, time 2 h, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric.

[0067] Example 8 1) Add guanidine hydrochloride, hexamethyleneamine and DMF into the reactor, stir to make guanidine hydrochloride and hexamethyleneamine fully mixed and completely dissolved in N,N-dimethylformamide (DMF), and then heat to 150 o C, polyethylene glycol was added during the heating process, and the reaction was continued for 2 hours until no NH3 was released from the reactor, and the reaction was completed to obtain polyhexamethyleneguanidine hydrochloride (PHMG). The mass ratio of guanidine hydrochloride to hexamethyleneamine is 1:1, and the total mass fraction of guanidine hydrochloride and hexamethyleneamine is 15 wt %.

[0068] Polyethylene glycol is used as a catalyst, and the usage amount of polyethylene glycol is 1% of the total mass of guanidine hydrochloride and hexamethylenediamine.

[0069] The degree of polymerization of polyhexamethyleneguanidine hydrochloride is greater than 1500.

[0070] 2) Dissolve the PHMG in step 1) evenly in anhydrous ethanol, slowly add propylene oxide dropwise, and heat to 30°C while stirring slowly. o C, add catalyst triethylamine, and keep warm for 5.5 hours. After the reaction is completed, add appropriate amount of hydrochloric acid (4 mol / L) for neutralization. After washing, the product is dissolved in DMF to obtain a PHMG-based antibacterial agent solution (mass concentration is 2.5%). The concentration of PHMG in anhydrous ethanol is 10wt%, the concentration of propylene oxide is 1 mol / L, and the concentration of the catalyst is 0.2 mol / L.

[0071] The product obtained in step 2) was analyzed by FTIR spectrum, and the epoxy group was found to have a characteristic absorption peak at about 910 cm - ¹.

[0072] 3) Immerse a certain amount of fabric in the PHMG-based antimicrobial agent solution obtained in step 2) at a reaction temperature of 60 o C, time 2 h, so that the antibacterial agent and the fabric fully react to form a strong covalent bond, and prepare a grafted long-lasting and washable antibacterial fabric.

[0073] The present invention conducted antibacterial tests on the antibacterial fabrics described in the above Examples 4-8 and the pure cotton fabric without grafting, that is, the inhibitory and killing effects of the antibacterial fabrics on Staphylococcus aureus, Escherichia coli, and Candida albicans, as well as the antifungal activity on Trichophyton rubrum were tested, and the results are shown in Table 1 (wherein the antibacterial fabrics of Examples 4-8 are numbered 1, 2, 3, 4, and 5 respectively; the cotton fabric is numbered 6).

[0074] Table 1 Antibacterial test results

[0075] From the test results in Table 1, it can be seen that the inhibitory and killing effects of the original fabric obtained by No. 6 on pathogens are basically 0, indicating that the original fabric generally has no antibacterial effect. Therefore, it is necessary to treat the original fabric, adsorb, bond or bond the inorganic antibacterial agent or the organic antibacterial agent to the fabric, and the fabric will have an antibacterial effect. It is a very popular method to bond the organic antibacterial agent to the textile by bonding, and the bonding method makes the antibacterial agent and the textile more firmly bonded. The present invention provides a method of grafting the antibacterial agent on the fabric, so that the textile has a lasting and significant broad-spectrum antibacterial and bactericidal effect, and in the antibacterial textile prepared by the present invention, the antibacterial functional group molecules are firmly fixed on the surface of the textile by chemical bonds, and the antibacterial textile provided by the present invention still has an excellent antibacterial effect after multiple washings with water.

[0076] The above description is only for the best embodiment of the present invention, but it should not be understood as limiting the claims. The present invention is not limited to the above embodiments, and its specific structure is allowed to be changed. However, all changes made within the protection scope of the independent claims of the present invention are within the protection scope of the present invention.

[0077] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more related listed items.

Claims

1. A method for preparing a grafted long-lasting and washable antibacterial fabric, characterized in that: The steps include: Polyhexamethyleneguanidine hydrochloride was chemically modified by epoxide to prepare PHMG-based antimicrobial agent; The fabric is immersed in an N,N-dimethylformamide solution containing a PHMG-based antibacterial agent, and the PHMG-based antibacterial agent reacts with the fabric to obtain a grafted, long-lasting, washable antibacterial fabric.

2. The grafted long-lasting and washable antibacterial fabric and its preparation method according to claim 1, characterized in that: The PHMG-based antimicrobial agent is prepared by chemically modifying polyhexamethyleneguanidine hydrochloride with epoxide, comprising the following steps: adding epoxide to an ethanol solution of polyhexamethyleneguanidine hydrochloride, and then o C, add a catalyst to obtain a mixture, and heat the mixture at 30-60 o C for 12-24 hours to obtain a PHMG-based antibacterial agent solution.

3. The method for preparing the grafted long-lasting and washable antibacterial fabric according to claim 2, characterized in that: The mass concentration of the N,N-dimethylformamide solution of the PHMG-based antibacterial agent is 0.5-2.5%.

4. The method for preparing the grafted long-lasting and washable antibacterial fabric according to claim 2, characterized in that: The epoxide is any one of epichlorohydrin, propylene oxide and diglycidyl ether.

5. The method for preparing the grafted long-lasting and washable antibacterial fabric according to claim 2, characterized in that: The catalyst is one of triethylamine and potassium hydroxide.

6. The method for preparing the grafted long-lasting and washable antibacterial fabric according to claim 2, characterized in that: In the mixture, the concentration of PHMG is 5-10wt%, the concentration of epoxide is 0.5-1 mol / L, and the concentration of catalyst is 0.1-0.3 mol / L.

7. The method for preparing the grafted long-lasting and washable antibacterial fabric according to claim 1, characterized in that: The temperature at which HMG-based antimicrobial agents react with fabrics is 60-100 o C, time is 2-3 h.

8. The method for preparing the grafted long-lasting and washable antibacterial fabric according to claim 1, characterized in that: The fabric is a cellulose-based fabric or a fabric in which the mass ratio of the cellulose-based fabric in the fabric is greater than 20%.

9. The method for preparing the grafted long-lasting and washable antibacterial fabric according to claim 8, characterized in that: The cellulose-based fabric raw material is any one of cotton, viscose fiber, modal, tencel, cupro fiber and acetate fiber.

10. A grafted long-lasting and washable antibacterial fabric prepared according to the method according to any one of claims 1 to 9.

Citation Information

Patent Citations

  • Washable and antibacterial fabric and preparation method thereof

    CN113756092A