Antibacterial composite fabric and preparation process thereof
By fixing the curcumin@UiO-66-NH2 complex on cotton fabric, the problem of poor antibacterial effect caused by the poor solubility of curcumin was solved, and high-efficiency and long-lasting antibacterial performance was achieved without damaging the fabric.
Patent Information
- Application Number
- CN202511101961.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-07
- Publication Date
- 2025-09-16
AI Technical Summary
The existing curcumin finishing method has poor solubility, resulting in poor antibacterial effect and difficulty in maintaining it for a long time. Cotton fabrics are prone to breeding bacteria in humid environments.
After the cotton fabric was treated with NaOH aqueous solution, it was immersed in a curcumin@UiO-66-NH2 complex solution, combined with Tris-HCl buffer solution and n-dodecanethiol, and curcumin was fixed on the cotton fabric through a low-temperature finishing process to form an antibacterial composite fabric.
Within the range of 20–80 g/L active ingredients, the antibacterial rates of cotton fabric against Escherichia coli and Staphylococcus aureus reached ≥96% and ≥98%, respectively. The antibacterial rate remained ≥80% after 50 industrial washings, and the process was gentle and did not damage the fibers.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of textile fabrics, and in particular to an antibacterial composite fabric and a preparation process thereof. Background Art
[0002] Cotton fabrics are highly hygroscopic and easily form a humid microenvironment when worn against the skin, becoming a breeding ground for bacteria.
[0003] Curcumin, the primary yellow polyphenol found in turmeric rhizomes, possesses a symmetrical β-diketone-phenolic hydroxyl structure. Upon contact with bacteria, it not only disrupts membrane structures and inhibits key enzyme activity, achieving broad-spectrum antimicrobial activity, but also exerts anti-inflammatory and free radical-scavenging antioxidant effects by blocking the NF-κB pathway. Experiments have demonstrated multiple biological activities, including anti-tumor, antiviral, and wound-healing activities. However, its extremely low water solubility and stability limit its direct application. Due to curcumin's poor solubility and low bioavailability, existing finishing methods offer limited antimicrobial efficacy and suffer from the problem of long-term antimicrobial performance. Summary of the Invention
[0004] In order to solve the problems existing in the prior art, the present invention provides an antibacterial composite fabric and a preparation process thereof.
[0005] The present invention is achieved through the following technical solutions:
[0006] A method for preparing an antibacterial composite fabric comprises the following steps:
[0007] Step S1: treating the fabric with a NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washing with deionized water, and drying at 80°C; then soaking the fabric in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washing with deionized water, and drying at 80°C;
[0008] Step S2: 50 g of the fabric obtained in step S1 was soaked in 150 mL of a curcumin@UiO-66-NH2 complex aqueous solution at 30° C. for 24 h; and then dried to obtain an antibacterial composite fabric.
[0009] Furthermore, the finishing agent in step S1 is a Tris-HCl buffer solution with a pH of 7, wherein the concentration of dopamine hydrochloride is 5 g / L and the concentration of n-dodecyl mercaptan is 3 mL / L.
[0010] Furthermore, the concentration of the NaOH aqueous solution in step S1 is 4 g / L.
[0011] Furthermore, the drying step in step S2 is pre-baking at 100° C. for 5 minutes and then baking at 180° C. for 5 minutes.
[0012] Furthermore, the concentration of the flavin@UiO-66-NH2 complex aqueous solution in step S2 is 20 g / L to 80 g / L.
[0013] Furthermore, the preparation method of the curcumin@UiO-66-NH2 complex is:
[0014] 2.5 mg of curcumin was dissolved in 10 mL of chloroform, and then 10 mg of UiO-66-NH2 was added and stirred at 30°C for 10 to 50 h. The precipitate was obtained by centrifugation, washed with chloroform three times, and then dried at room temperature to obtain the curcumin@UiO-66-NH2 complex.
[0015] Furthermore, the preparation method of the UiO-66-NH2 is:
[0016] ZrCl4 and 2-aminoterephthalic acid were dissolved in a mixed solvent consisting of DMF and ethanol, and ultrasonicated after being fully dissolved; the mixture was then reacted at 100°C for 8 hours; after the reaction, the precipitate was collected by centrifugation, fully washed with ethanol, and then dried to obtain UiO-66-NH2.
[0017] Furthermore, the present invention provides an antibacterial composite fabric prepared by the above-mentioned method for preparing the antibacterial composite fabric.
[0018] Compared with the prior art, the present invention has the following advantages and beneficial effects:
[0019] The present invention uses "natural curcumin-UiO-66-NH2-MOF" low-temperature finishing to enable cotton fabrics to achieve an antibacterial rate of ≥96% for Escherichia coli and ≥98% for Staphylococcus aureus within the range of 20-80g / L active components. The antibacterial retention rate remains ≥80% after 50 industrial washings. The process is gentle and does not damage cotton fibers. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] The drawings described herein are used to provide a further understanding of the embodiments of the present invention, constitute a part of this application, and do not constitute a limitation of the embodiments of the present invention.
[0021] Figure 1 This is the SEM image of the curcumin@UiO-66-NH2 complex in the present invention. DETAILED DESCRIPTION
[0022] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with examples and drawings. The exemplary embodiments of the present invention and their descriptions are only used to explain the present invention and are not intended to limit the present invention.
[0023] The fabric of the present invention is a pure cotton plain fabric woven from Xinjiang long-staple cotton, wherein the warp yarn and the weft yarn are both JC 7.4tex yarns, the warp density is 787 yarns / 10cm, the weft density is 710 yarns / 10cm, and the thickness is 0.18mm.
[0024] The synthesis method of Fe-MOF in the present invention is:
[0025] Mix 1 g of FeCl2 and 1 g of 2-aminoterephthalic acid in 10 mL of DMF at room temperature to obtain a slurry mixture. Seal the slurry and place it in a 110°C oven to react for 24 hours. After the reaction is completed, filter the mixture and wash the resulting solid with DMF to remove unreacted organic ligands and then with methanol to remove residual DMF. Finally, dry the solid in an 80°C oven for 4 hours and store it in a vacuum oven for later use.
[0026] The synthesis method of UiO-66-NH2 in the present invention is:
[0027] 242 mg of ZrCl4 and 543 mg of 2-aminoterephthalic acid were dissolved in a mixed solvent consisting of 40 mL of DMF and 40 mL of ethanol. After complete dissolution, the mixture was ultrasonicated for 20 min. The mixture was then transferred to a polytetrafluoroethylene-lined stainless steel reactor and reacted at 100°C for 8 h. After the reaction, the precipitate was collected by centrifugation, washed thoroughly with ethanol, and then dried in an oven at 80°C for 4 h. The obtained UiO-66-NH2 solid was vacuum-stored for later use.
[0028] Example 1
[0029] A preparation process of an antibacterial composite fabric comprises the following steps:
[0030] Step S1:
[0031] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0032] Step S2:
[0033] 50 g of the fabric obtained in step S1 was soaked in 150 mL of a 20 g / L curcumin@UiO-66-NH2 complex aqueous solution at 30°C for 24 h; then pre-baked at 100°C for 5 min and then baked at 180°C for 5 min to obtain an antibacterial composite fabric.
[0034] The preparation method of curcumin@UiO-66-NH2 complex is as follows:
[0035] 2.5 mg of curcumin was dissolved in 10 mL of chloroform, and then 10 mg of UiO-66-NH2 was added and stirred at 30°C for 20 h. The precipitate was obtained by centrifugation, washed with chloroform three times, and then dried at room temperature to obtain the curcumin@UiO-66-NH2 complex. Figure 1 This is the SEM image of the curcumin@UiO-66-NH2 complex in the present invention.
[0036] Example 2
[0037] A preparation process of an antibacterial composite fabric comprises the following steps:
[0038] Step S1:
[0039] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0040] Step S2:
[0041] 50 g of the fabric obtained in step S1 was soaked in 150 mL of 40 g / L curcumin@UiO-66-NH2 aqueous solution at 30 °C.
[0042] Then, the antibacterial composite fabric was obtained by pre-baking at 100°C for 5 minutes and then baking at 180°C for 5 minutes.
[0043] The preparation method of the curcumin@UiO-66-NH2 complex is the same as that in Example 1.
[0044] Example 3
[0045] A preparation process of an antibacterial composite fabric comprises the following steps:
[0046] Step S1:
[0047] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0048] Step S2:
[0049] 50 g of the fabric obtained in step S1 was soaked in 150 mL of 60 g / L curcumin@UiO-66-NH2 aqueous solution at 30 °C.
[0050] Then, the antibacterial composite fabric was obtained by pre-baking at 100°C for 5 minutes and then baking at 180°C for 5 minutes.
[0051] The preparation method of the curcumin@UiO-66-NH2 complex is the same as that in Example 1.
[0052] Example 4
[0053] A preparation process of an antibacterial composite fabric comprises the following steps:
[0054] Step S1:
[0055] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0056] Step S2:
[0057] 50 g of the fabric obtained in step S1 was soaked in 150 mL of 80 g / L curcumin@UiO-66-NH2 aqueous solution at 30 °C.
[0058] Then, the antibacterial composite fabric was obtained by pre-baking at 100°C for 5 minutes and then baking at 180°C for 5 minutes.
[0059] The preparation method of the curcumin@UiO-66-NH2 complex is the same as that in Example 1.
[0060] Example 5
[0061] A preparation process of an antibacterial composite fabric comprises the following steps:
[0062] Step S1:
[0063] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0064] Step S2:
[0065] 50 g of the fabric obtained in step S1 was soaked in 150 mL of a 40 g / L curcumin@UiO-66-NH2 complex aqueous solution at 30°C for 24 h; then pre-baked at 100°C for 5 min and then baked at 180°C for 5 min to obtain an antibacterial composite fabric.
[0066] The preparation method of curcumin@UiO-66-NH2 complex is as follows:
[0067] 2.5 mg of curcumin was dissolved in 10 mL of chloroform, and then 10 mg of UiO-66-NH2 was added and stirred at 30°C for 10 h. The precipitate was obtained by centrifugation, washed with chloroform three times, and then dried at room temperature to obtain the curcumin@UiO-66-NH2 complex.
[0068] Example 6
[0069] A preparation process of an antibacterial composite fabric comprises the following steps:
[0070] Step S1:
[0071] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0072] Step S2:
[0073] 50 g of the fabric obtained in step S1 was soaked in 150 mL of a 40 g / L curcumin@UiO-66-NH2 complex aqueous solution at 30°C for 24 h; then pre-baked at 100°C for 5 min and then baked at 180°C for 5 min to obtain an antibacterial composite fabric.
[0074] The preparation method of curcumin@UiO-66-NH2 complex is as follows:
[0075] 2.5 mg of curcumin was dissolved in 10 mL of chloroform, and then 10 mg of UiO-66-NH2 was added and stirred at 30°C for 30 h. The precipitate was obtained by centrifugation, washed with chloroform three times, and then dried at room temperature to obtain the curcumin@UiO-66-NH2 complex.
[0076] Example 7
[0077] A preparation process of an antibacterial composite fabric comprises the following steps:
[0078] Step S1:
[0079] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0080] Step S2:
[0081] 50 g of the fabric obtained in step S1 was soaked in 150 mL of a 40 g / L curcumin@UiO-66-NH2 complex aqueous solution at 30°C for 24 h; then pre-baked at 100°C for 5 min and then baked at 180°C for 5 min to obtain an antibacterial composite fabric.
[0082] The preparation method of curcumin@UiO-66-NH2 complex is as follows:
[0083] 2.5 mg of curcumin was dissolved in 10 mL of chloroform, and then 10 mg of UiO-66-NH2 was added and stirred at 30°C for 40 h. The precipitate was obtained by centrifugation, washed with chloroform three times, and then dried at room temperature to obtain the curcumin@UiO-66-NH2 complex.
[0084] Example 8
[0085] A preparation process of an antibacterial composite fabric comprises the following steps:
[0086] Step S1:
[0087] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0088] Step S2:
[0089] 50 g of the fabric obtained in step S1 was soaked in 150 mL of a 40 g / L curcumin@UiO-66-NH2 complex aqueous solution at 30°C for 24 h; then pre-baked at 100°C for 5 min and then baked at 180°C for 5 min to obtain an antibacterial composite fabric.
[0090] The preparation method of curcumin@UiO-66-NH2 complex is as follows:
[0091] 2.5 mg of curcumin was dissolved in 10 mL of chloroform, and then 10 mg of UiO-66-NH2 was added and stirred at 30°C for 50 h. The precipitate was obtained by centrifugation, washed with chloroform three times, and then dried at room temperature to obtain the curcumin@UiO-66-NH2 complex.
[0092] Comparative Example 1
[0093] A preparation process of an antibacterial composite fabric comprises the following steps:
[0094] Step S1:
[0095] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0096] Step S2:
[0097] 50 g of the fabric obtained in step S1 was soaked in 150 mL of a 40 g / L curcumin@Fe-MOF complex aqueous solution at 30° C. for 24 h; then pre-baked at 100° C. for 5 min and then baked at 180° C. for 5 min to obtain an antibacterial composite fabric.
[0098] The preparation method of curcumin@Fe-MOF complex is as follows:
[0099] 2.5 mg of curcumin was dissolved in 10 mL of chloroform, and then 10 mg of Fe-MOF was added and stirred at 30°C for 20 h. The precipitate was obtained by centrifugation, washed with chloroform three times, and then dried at room temperature to obtain the curcumin@Fe-MOF complex.
[0100] Comparative Example 2
[0101] A preparation process of an antibacterial composite fabric comprises the following steps:
[0102] Step S1:
[0103] The fabric was treated with a 4g / L NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washed with deionized water, and dried at 80°C. The fabric was then immersed in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washed with deionized water, and dried at 80°C. The finishing agent was a Tris-HCl buffer solution with a pH of 7, containing 5g / L dopamine hydrochloride and 3mL / L n-dodecyl mercaptan.
[0104] Step S2:
[0105] 50 g of the fabric obtained in step S1 was soaked in 150 mL of an 80 g / L curcumin@Fe-MOF complex aqueous solution at 30° C. for 24 h; then pre-baked at 100° C. for 5 min and then baked at 180° C. for 5 min to obtain an antibacterial composite fabric.
[0106] The preparation method of the curcumin@Fe-MOF complex is the same as that of Comparative Example 1.
[0107] Test Example 1
[0108] The antibacterial rate test and evaluation method refers to T / GDBX 024-2020 "Functional Technical Specifications for Household Textiles", and the test bacteria are Escherichia coli and Staphylococcus aureus.
[0109] Table 1 Performance test
[0110]
[0111] As can be seen from Table 1, the examples and comparative examples show that the curcumin@UiO-66-NH2 complex shows better inhibition of Escherichia coli and Staphylococcus aureus than the curcumin@Fe-MOF complex. Furthermore, the curcumin@UiO-66-NH2 complex maintains a good inhibition rate even after multiple washes.
[0112] As can be seen from Example 2, during the preparation of the curcumin@UiO-66-NH2 complex, when the reaction time was 20 hours, the inhibition rate against Escherichia coli was 96%, and the inhibition rate against Staphylococcus aureus was 98%. In Examples 4 to 8, the preparation times of the curcumin@UiO-66-NH2 complex were 10 hours, 30 hours, 40 hours, and 50 hours, respectively. When the reaction time was greater than or equal to 20 hours, the inhibition rate no longer increased significantly, indicating that during the preparation of the curcumin@UiO-66-NH2 complex, at least 20 hours were required to achieve ideal adsorption of curcumin on UiO-66-NH2.
[0113] The specific implementation methods described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific implementation method of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A method for preparing an antibacterial composite fabric, characterized in that: The following steps are involved: Step S1: treating the fabric with a NaOH aqueous solution at a bath ratio of 1:50 at 100°C for 30 minutes, washing with deionized water, and drying at 80°C; then soaking the fabric in a finishing agent at a bath ratio of 1:40 at 40°C for 24 hours, then washing with deionized water, and drying at 80°C; Step S2: 50 g of the fabric obtained in step S1 was soaked in 150 mL of a curcumin@UiO-66-NH2 complex aqueous solution at 30° C. for 24 h; and then dried to obtain an antibacterial composite fabric.
2. The method for preparing an antibacterial composite fabric according to claim 1, characterized in that: The finishing agent in step S1 is a Tris-HCl buffer solution with a pH of 7, wherein the concentration of dopamine hydrochloride is 5 g / L and the concentration of n-dodecanethiol is 3 mL / L.
3. The method for preparing an antibacterial composite fabric according to claim 1, characterized in that: The concentration of the NaOH aqueous solution in step S1 is 4 g / L.
4. The method for preparing an antibacterial composite fabric according to claim 1, characterized in that: The drying step in step S2 is pre-baking at 100° C. for 5 minutes and then baking at 180° C. for 5 minutes.
5. The method for preparing an antibacterial composite fabric according to claim 1, characterized in that: The concentration of the flavin@UiO-66-NH2 complex aqueous solution in step S2 is 20 g / L to 80 g / L.
6. The method for preparing an antibacterial composite fabric according to claim 1, characterized in that: The preparation method of the curcumin@UiO-66-NH2 complex is as follows: 2.5 mg of curcumin was dissolved in 10 mL of chloroform, and then 10 mg of UiO-66-NH2 was added and stirred at 30°C for 10 to 50 h. The precipitate was obtained by centrifugation, washed with chloroform three times, and then dried at room temperature to obtain the curcumin@UiO-66-NH2 complex.
7. The method for preparing an antibacterial composite fabric according to claim 6, characterized in that: The preparation method of the UiO-66-NH2 is: ZrCl4 and 2-aminoterephthalic acid were dissolved in a mixed solvent consisting of DMF and ethanol, and ultrasonicated after being fully dissolved; the mixture was then reacted at 100°C for 8 hours; after the reaction, the precipitate was collected by centrifugation, washed thoroughly with ethanol, and then dried to obtain UiO-66-NH2.
8. An antibacterial composite fabric prepared by the method for preparing an antibacterial composite fabric according to any one of claims 1 to 7.
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