Multi-mechanism synergistic photodynamic high-efficiency antibacterial medical textile and one-step dyeing and finishing process for realizing color matching and antibacterial production

CN118007449BActive Publication Date: 2026-10-30JIANGNAN UNIV +2
View PDF 1 Cites 0 Cited by

Patent Information

Application Number
CN202410213994.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-02-27
Publication Date
2026-10-30
Estimated Expiration
2044-02-27

AI Technical Summary

Benefits of technology

[0030](1)制得的纺织品在光动力抗菌效果方面实现了协同增效:

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN118007449B_ABST
    Figure CN118007449B_ABST
Patent Text Reader

Abstract

The present application belongs to the field of antibacterial functional materials, and particularly relates to a multi-mechanism synergistic photodynamic high-efficiency antibacterial medical textile and a production process for realizing color matching antibacterial effect by one-step dyeing and finishing, comprising the following steps: desizing, grey cloth preshrinking, dissolving curcumin, methylene blue and bambusin in a cosolvent solution at the same time, stirring overnight, adjusting pH to 4-5, adding a dispersing agent to obtain a photosensitizer pigment dyeing solution; dyeing the grey cloth by using the photosensitizer pigment dyeing solution, wherein, the dyeing is carried out at room temperature, the total amount of curcumin, methylene blue and bambusin is 2% owf; heating to 80 DEG C, then heating to 125-130 DEG C, keeping for 30-60 min, cooling, to obtain a dyed textile; reducing cleaning, then drying in a dark hot air environment, to obtain a high-efficiency antibacterial colored textile. The present application can simultaneously realize better high-efficiency and spectral antibacterial effect, improve the color fastness to rubbing of the textile, and can simply and conveniently adjust the color of the textile.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention belongs to the field of antibacterial functional materials technology, and specifically relates to a multi-mechanism synergistic photodynamic high-efficiency antibacterial medical textile and its one-step dyeing and finishing process for achieving color matching and antibacterial properties. Background Technology

[0002] Hospital-acquired infections (HAIs) are one of the leading causes of morbidity and mortality in hospitals, with an incidence rate of approximately 5-15%, primarily caused by opportunistic pathogens and common drug-resistant bacteria. To address the problem of HAIs caused by pathogens, especially drug-resistant bacteria, while effectively reducing the negative environmental impact of antimicrobial materials, seeking new antimicrobial materials specifically targeting bacterial infections is currently the main approach. Utilizing bio-based antimicrobial agents with a multi-effect synergistic mechanism for broad-spectrum and highly effective antimicrobial action, constructing an antimicrobial interface with high adsorption and in-situ killing effects on the fiber surface, forms a protective layer against infectious pathogens, thereby reducing the incidence of hospital-acquired infections. Therefore, as an effective means of reducing the prevalence of hospital-acquired infections, the research and development of key technologies and the industrialization of medical textiles that actively protect against pathogens are urgently needed. Summary of the Invention

[0003] [Technical Issues]

[0004] This invention provides a high-efficiency antibacterial colored textile production process to simultaneously achieve superior high-efficiency and broad-spectrum antibacterial effects, improve the color fastness of textiles to rubbing, and easily adjust the color of textiles. The resulting textiles can meet the performance requirements of Chinese pharmaceutical industry standards for medical textiles.

[0005] [Technical Concept]

[0006] This invention involves mixing three photosensitizers (PSs) with different properties: curcumin, methylene blue, and bamboo red pigment. During mixing, these three substances form a supramolecular complex through electrostatic interactions. This supramolecular complex is then used as a dye to prepare a photosensitizer-based dye solution. This solution is then applied to a one-step dyeing and finishing process for producing highly efficient antibacterial colored textiles. This research demonstrates that the supramolecular complex formed by curcumin, methylene blue, and bamboo red pigment can control or prevent molecular aggregation, improve the generation of reactive oxygen species (ROS), increase photobleaching stability, and interfere with degradation mechanisms, thereby enhancing the photosensitizing and antibacterial activity of textiles. This enhanced photosensitivity helps improve biodistribution and cellular uptake, thus improving the safety and efficacy of photodynamic therapy (PDT). Curcumin, methylene blue, and bamboo red pigment exert their highly efficient photodynamic antibacterial effects through a multi-mechanism synergistic effect. The supramolecular complex used in this invention can effectively absorb the energy of photons after being excited by light and transfer it to surrounding molecules. It generates a large amount of reactive oxygen species (ROS) with bactericidal effects through photodynamic inactivation (aPDI). At the same time, the production process of this invention allows the supramolecular complex to be effectively loaded onto textiles, providing the textiles with photodynamic antibacterial properties.

[0007] in:

[0008] Curcumin can interfere with the quorum sensing system of bacteria (a way for bacteria to communicate with each other, which is essential for maintaining bacterial virulence factors, thereby reducing the production of bacterial virulence factors, and also preventing the formation of bacterial biofilms (a protective layer formed by bacteria in the host, which can enhance the bacteria's ability to resist drug treatment); curcumin can also prevent bacteria from adhering to host receptors, thereby inhibiting bacterial infection.

[0009] The cationic charge of methylene blue enhances its electrostatic adsorption with bacteria, enabling it to contact bacteria more effectively and thus inhibit the activity of lipopolysaccharides (LPS), a key component of bacterial cell walls. In this way, methylene blue disrupts bacterial cell walls, blocking the growth and reproduction of bacteria.

[0010] Bamboo red mycin exhibits high photoactivity and low dark toxicity. Under light conditions, it functions efficiently, while its toxicity to the host is relatively low under dark conditions. Bamboo red mycin also demonstrates good photobleaching stability, becoming even more stable and less prone to decomposition during light exposure. Its antibacterial mechanism also includes interfering with bacterial degradation processes, thereby effectively inhibiting bacterial growth.

[0011] The process based on this application allows for the controllability of textile colors by adjusting the proportions of curcumin, methylene blue, and bamboo red fungicide.

[0012] [Technical Solution]

[0013] On the one hand, a highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method is provided, which includes the following steps:

[0014] S1. Desizing: Textiles are desized and repeatedly washed to remove surface oils and impurities to obtain greige fabric;

[0015] S2. Fabric pre-shrinking: Soak the fabric in clean water and then dry it.

[0016] S3. Preparation of photosensitizer dye solution: Dissolve curcumin, methylene blue and bamboo red pigment simultaneously in an aqueous solution containing a solubilizer, stir overnight to allow the solubilizer to evaporate, adjust the pH to 4-5, and add a dispersant with a final concentration of 2-3 g / L to obtain the photosensitizer dye solution; wherein, the ratio of curcumin, methylene blue and bamboo red pigment is set according to the target color of the highly effective antibacterial colored textile.

[0017] S4. Dyeing: The photosensitizer dye solution prepared in step S3 is used to dye the greige fabric obtained in step S2. Dyeing is carried out at room temperature, and the sum of curcumin, methylene blue and bamboo red fungicide is 2% owf. The bath ratio of textile to photosensitizer dye solution is 1:(25-35) g / L. Then, the temperature is raised to 80℃ at the first heating rate, and then raised to 125-130℃ at the second heating rate. The temperature is then maintained at 125-130℃ for 30-60 min, and then cooled to obtain the dyed textile. The first heating rate is greater than the second heating rate.

[0018] S5. Reduction Cleaning: The dyed textiles obtained in S4 are reduced and cleaned in a reducing bath at 75-80℃ for 15-20 minutes, followed by washing in water at 55-60℃, and then dried in a dark hot air environment at 55-65℃ to obtain highly effective antibacterial colored textiles; wherein, the reducing bath is an aqueous solution containing 1.5-2 g / L sodium dithionite and 1.5-2 g / L sodium hydroxide; the bath ratio of textiles to reducing bath is 1:(20-35) g / L.

[0019] In some embodiments, in step S4, the amount of curcumin is 0.1-0.9% owf, the amount of methylene blue is 0.5-1.8% owf, and the amount of bamboo red fungin is 0.1-1.1% owf, and the sum of the amounts of curcumin, methylene blue and bamboo red fungin is 2% owf.

[0020] In some embodiments, in step S4, the amount of curcumin is 0.4% owf, the amount of methylene blue is 0.5% owf, and the amount of baicalein is 1.1% owf.

[0021] In some embodiments, the alkaline boiling solution used in step S1 for desizing is a mixed aqueous solution containing 1-2 g / L anhydrous sodium carbonate, 2-3 g / L sodium dodecylbenzenesulfonate and 1-2 g / L soap powder.

[0022] In some embodiments, the desizing in step S1 involves boiling and washing at 80°C for 30 minutes.

[0023] In some embodiments, the co-solvent in step S3 is at least one of acetone and ethanol.

[0024] In some embodiments, the dispersant in step S3 is at least one of sodium lignosulfonate, sodium dodecylbenzenesulfonate, and sodium dodecyl sulfonate.

[0025] In some embodiments, the first heating rate and the second heating rate in step S4 are in the range of 1-2 °C / min.

[0026] On the other hand, the aforementioned production process yields highly effective antibacterial colored textiles.

[0027] On the other hand, the aforementioned highly effective antibacterial colored textiles are used in the preparation of medical textiles.

[0028] [Beneficial Effects]

[0029] This application selects natural dyes curcumin, methylene blue, and bamboo red pigment, which have specific colors and photosensitive properties, and combines them in specific proportions. Combined with the specific production process (desizing → pre-shrinking → dyeing → reduction cleaning) and specific process parameters of this application, the production process of this application has the following advantages compared to existing technologies:

[0030] (1) The prepared textiles achieved synergistic effects in photodynamic antibacterial activity:

[0031] a. Significantly improved singlet oxygen yield and stability: Under the same total amount of photosensitizer pigment, the singlet oxygen yield and stability of colored textiles produced by using a photosensitizer pigment solution composed of curcumin, methylene blue, and bamboo red pigment are higher than those produced by using any two or one of curcumin, methylene blue, and bamboo red pigment. This confirms that curcumin, methylene blue, and bamboo red pigment mutually support each other in improving singlet oxygen yield, and the combined singlet oxygen yield is superior to that of any two or one of curcumin, methylene blue, and bamboo red pigment.

[0032] b. The resulting textiles exhibit highly efficient and broad-spectrum antibacterial effects: By mixing three photosensitizers (PSs) with different properties—curcumin, methylene blue, and baicalein—they can form a supramolecular complex through electrostatic interactions during the mixing process. Upon photoexcitation, this supramolecular complex generates a large amount of reactive oxygen species (ROS) through photodynamic inactivation (aPDI). ROS destroys the proteins, lipids, and nucleic acids of bacteria, thus achieving non-specific photodynamic antibacterial inactivation, effective against Gram-positive bacteria (such as *Gastrodia elata*). The bactericidal effect against Staphylococcus aureus and Gram-negative bacteria (such as Escherichia coli) reached 99.999% and 98%, respectively, demonstrating potential for killing multidrug-resistant bacteria and viruses. It was confirmed that, under the same total amount of photosensitizer pigment, colored textiles produced using a photosensitizer pigment solution containing a compound of curcumin, methylene blue, and bamboo red pigment showed significantly better antibacterial effects against Staphylococcus aureus and Escherichia coli under the same photodynamic conditions than those using any two or one of these compounds. This confirms that curcumin, methylene blue, and bamboo red pigment mutually support each other in enhancing antibacterial effects, and the combined antibacterial effect is superior to that of any two or one of these compounds.

[0033] Furthermore, the aforementioned effects have not been reported prior to this application, and have produced unexpected technical effects for those skilled in the art;

[0034] c. In this application, the supramolecular complex, upon photoexcitation, generates a large amount of reactive oxygen species (ROS) through photodynamic inactivation (aPDI), causing oxidative damage to nearby bacteria, leading to growth inhibition and cell death, while causing almost no damage to surrounding normal cells. Compared with antibiotic antibacterial solutions, the solution in this application has no risk of drug resistance, is reusable, and has good biocompatibility;

[0035] (2) The textiles obtained achieve synergistic effects in terms of rubbing fastness performance: while maintaining the color brightness, the risk of fading caused by friction during the use of highly effective antibacterial colored textiles is reduced, which helps to improve the overall quality and durability of highly effective antibacterial colored textiles. It is also confirmed that curcumin, methylene blue and bamboo red fungicide support each other in improving rubbing fastness performance. The combined rubbing fastness performance is superior to that of any two or any one of curcumin, methylene blue and bamboo red fungicide. This effect has not been reported before this application and has produced unexpected technical effects for those skilled in the art.

[0036] (3) By mixing three photosensitizers (i.e., curcumin, methylene blue, and baicalein) in different proportions, a pagoda-like diagram similar to the three primary colors can be created (e.g., Figure 5(As shown). Based on the production process of this application, by simply adjusting the ratio of curcumin, methylene blue, and bamboo red pigment, the different color requirements for high-efficiency antibacterial colored textiles in mass production can be met, realizing the controllability of textile color; it solves the technical defects of existing antibacterial textiles, such as the difficulty in color control or the complexity of producing antibacterial textiles of different colors; the production process based on this application can use traditional textile finishing equipment, and compared with existing antibacterial finishing processes, this application can realize the integration of dyeing and antibacterial finishing, solve the equipment problems in the process of large-scale production, shorten the production process of antibacterial textiles, thereby improving the production efficiency of antibacterial colored textiles and reducing the production cost of antibacterial colored textiles; at the same time, the high-efficiency antibacterial colored textiles obtained by this application have excellent dyeing effects (high dyeing rate and even dyeing rate)

[0037] (4) The production process of this application is simple to operate and environmentally friendly;

[0038] (5) The textiles produced can meet the requirements of Chinese pharmaceutical industry standards for the antibacterial properties, color variety, color fastness and mechanical properties of medical textiles. Attached Figure Description

[0039] Figure 1 The results of singlet oxygen tests are shown for the textiles prepared in each embodiment and comparative example.

[0040] Figure 2 The results of the antibacterial effect of textiles prepared in each embodiment and comparative example on Staphylococcus aureus are presented.

[0041] Figure 3 The results of the antibacterial effect of textiles prepared in each embodiment and comparative example on Escherichia coli are presented.

[0042] Figure 4 The results of K / S value measurements for textiles prepared in each embodiment and comparative example;

[0043] Figure 5 The pagoda diagram shows different colors that can be mixed using the colors of curcumin, methylene blue, and bamboo red pigment of this invention as the three primary colors. Detailed Implementation

[0044] Example 1

[0045] A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method includes the following steps:

[0046] S1. Desizing: The polyester textile is boiled and washed at 80°C for 30 minutes in a mixed aqueous solution containing 2g / L anhydrous sodium carbonate, 3g / L sodium dodecylbenzenesulfonate and 2g / L soap powder. The washing is repeated to remove surface impurities and obtain the greige fabric.

[0047] S2. Fabric pre-shrinking: Soak the fabric in clean water and then dry it.

[0048] S3. Preparation of photosensitizer pigment dyeing solution: Dissolve curcumin, methylene blue and bamboo red pigment in acetone aqueous solution, stir overnight to allow acetone to evaporate, adjust pH to 4.5, add sodium dodecyl sulfate (as dispersant) to a final concentration of 2 g / L to obtain photosensitizer pigment dyeing solution; wherein, the volume ratio of water to acetone in acetone aqueous solution is 7:3, and the weight ratio of curcumin, methylene blue and bamboo red pigment is 1:18:1;

[0049] S4. Dyeing: The photosensitizer dye solution prepared in step S3 is used to dye the greige fabric obtained in step S2. Dyeing is carried out at room temperature. The amount of curcumin is 0.1% owf, the amount of methylene blue is 1.8% owf, and the amount of bamboo red fungin is 0.1% owf. The bath ratio of textile to photosensitizer dye solution is 1:30 g / L. Then, the temperature is increased to 80℃ at a heating rate of 2℃ / min, and then increased to 125-130℃ at a heating rate of 1℃ / min. Then, the temperature is maintained at 125-130℃ for 30 min, and then cooled to obtain the dyed textile.

[0050] S5. Reduction Cleaning: The dyed textiles obtained in S4 are reduced and cleaned at 80°C for 20 minutes using a reduction bath solution, followed by cleaning in deionized water at 60°C, and then dried in a dark hot air environment at 65°C to obtain highly effective antibacterial colored textiles; wherein, the reduction bath solution is an aqueous solution containing 1.5-2 g / L sodium dithionite (as a strong reducing agent) and 1.5-2 g / L sodium hydroxide; the bath ratio of textiles to reduction bath solution is 1:(20-35) g / L.

[0051] Example 2

[0052] A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method is described. Referring to Example 1, the only difference is that, while maintaining the total amount of photosensitizer pigment at 2% owf, the relative amounts of curcumin, methylene blue, and bamboo red fungicide in the photosensitizer pigment dye solution are adjusted. In Example 2, the amount of curcumin is 0.9% owf, the amount of methylene blue is 0.9% owf, and the amount of bamboo red fungicide is 0.2% owf, while other parameters remain unchanged.

[0053] Example 3

[0054] A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method is described. Referring to Example 1, the only difference is that, while maintaining the total amount of photosensitizer pigment at 2% owf, the relative amounts of curcumin, methylene blue, and bamboo red fungicide in the photosensitizer pigment dye solution are adjusted. In Example 3, the amount of curcumin is 0.4% owf, the amount of methylene blue is 0.5% owf, and the amount of bamboo red fungicide is 1.1% owf, while other parameters remain unchanged.

[0055] Comparative Example 1

[0056] A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method is described. Referring to Example 1, the only difference is that, while maintaining the total amount of photosensitizer pigment at 2% owf, the relative amounts of curcumin, methylene blue, and bamboo red fungicide in the photosensitizer pigment dye solution are adjusted. In Comparative Example 1, the amount of curcumin is 1.6% owf, the amount of methylene blue is 0.4% owf, and the amount of bamboo red fungicide is 0% owf, while other parameters remain unchanged.

[0057] Comparative Example 2

[0058] A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method is described. Referring to Example 1, the only difference is that, while maintaining the total amount of photosensitizer pigment at 2% owf, the relative amounts of curcumin, methylene blue, and bamboo red fungicide in the photosensitizer pigment dye solution are adjusted. In Comparative Example 2, the amount of curcumin is 0% owf, the amount of methylene blue is 1.9% owf, and the amount of bamboo red fungicide is 0.1% owf, while other parameters remain unchanged.

[0059] Comparative Example 3

[0060] A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method is described. Referring to Example 1, the only difference is that, while maintaining the total amount of photosensitizer pigment at 2% owf, the relative amounts of curcumin, methylene blue, and bamboo red fungicide in the photosensitizer pigment dye solution are adjusted. In Comparative Example 3, the amount of curcumin is 1.8% owf, the amount of methylene blue is 0% owf, and the amount of bamboo red fungicide is 0.2% owf, while other parameters remain unchanged.

[0061] Comparative Example 4

[0062] A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method is described. Referring to Example 1, the only difference is that, while maintaining the total amount of photosensitizer pigment at 2% owf, the relative amounts of curcumin, methylene blue, and bamboo red fungicide in the photosensitizer pigment dye solution are adjusted. In Comparative Example 4, the amount of curcumin is 2.0% owf, the amount of methylene blue is 0% owf, and the amount of bamboo red fungicide is 0% owf, while other parameters remain unchanged.

[0063] Comparative Example 5

[0064] A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method is described. Referring to Example 1, the only difference is that, while maintaining the total amount of photosensitizer pigment at 2% owf, the relative amounts of curcumin, methylene blue, and bamboo red fungicide in the photosensitizer pigment dye solution are adjusted. In Comparative Example 5, the amount of curcumin is 0% owf, the amount of methylene blue is 2.0% owf, and the amount of bamboo red fungicide is 0% owf, while other parameters remain unchanged.

[0065] Comparative Example 6

[0066] A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method is described. Referring to Example 1, the only difference is that, while maintaining the total amount of photosensitizer pigment at 2% owf, the relative amounts of curcumin, methylene blue, and bamboo red fungicide in the photosensitizer pigment dye solution are adjusted. In Comparative Example 6, the amount of curcumin is 0% owf, the amount of methylene blue is 0% owf, and the amount of bamboo red fungicide is 2.0% owf, while other parameters remain unchanged.

[0067] Performance testing

[0068] 1. Singlet oxygen test

[0069] A circular piece of textile sample with a diameter of 1.5 cm was immersed in 5 mL of a 74 μM solution of 1,3-diphenylisobenzofuran (DPBF) saturated with methanol and oxygen. A laser pointer (wavelength 532 nm, 85 ± 1 mW / cm²) was then used. 2 The circular textile sample was irradiated with an HTPOW Laser Limited instrument. During the irradiation process, the absorption spectrum of the oxidized DPBF solution and the absorbance at the characteristic wavelength of DPBF (410 nm) were recorded every 5 minutes using a UV spectrophotometer. The results are as follows: Figure 1 As shown.

[0070] The singlet oxygen test data showed that the absorbance of Examples 1 to 3 at the characteristic wavelength of 410 nm at 20 min was higher than that of Comparative Examples 1 to 6. Although the absorbance of Comparative Example 3 at the characteristic wavelength of 410 nm was slightly higher than that of Example 1 in the first 15 min, the rate of change of absorbance with time increased significantly after 15 min, indicating that its singlet oxygen yield decreased rapidly after 15 min. In contrast, the absorbance of Examples 1 to 3 at the characteristic wavelength of 410 nm changed steadily from 0 to 20 min. This confirmed that, under the same total amount of photosensitizer pigment, the singlet oxygen yield and stability of the colored textiles produced by using a photosensitizer pigment solution composed of curcumin, methylene blue and bamboo red pigment were higher than those produced by using a photosensitizer pigment solution composed of any two or any one of curcumin, methylene blue and bamboo red pigment. It has been confirmed that curcumin, methylene blue and baicalein support each other in improving singlet oxygen yield. The combined singlet oxygen yield is superior to that of any two or any one of curcumin, methylene blue and baicalein. This effect has not been reported before this application and has produced unexpected technical effects for those skilled in the art.

[0071] 2. Antibacterial test

[0072] The antibacterial properties of the textiles prepared in each embodiment and comparative example were analyzed using an improved method according to AATCC-100, "Anti-bacterial Assessment or Bacterial Resistance Test on Textile Material". The photodynamic (simulated sunlight) conditions were as follows:

[0073] Light source: XQ500W adjustable xenon lamp; actual wavelength range (after filter processing): 420-780nm; height of light source from sample: 15cm; each experimental group used 3 parallel samples for testing.

[0074] The experimental results of the antibacterial effect of the textiles prepared in each embodiment and comparative example against Staphylococcus aureus are as follows: Figure 2 As shown, Figure 2 Staphylococcus aureus (S. aureus), a Gram-positive bacterium. The experimental results of the antibacterial effects against Escherichia coli in the textiles prepared in each example and comparative example are as follows: Figure 3 As shown, Figure 3 Escherichia coli (E. coli) is a Gram-negative bacterium. Figure 2 and Figure 3 In the context of , hv represents a dark environment, and +hv represents a bright environment.

[0075] N% = N i / N0×100 (1)

[0076] The bacterial survival rate (N, %) was calculated using formula (1), and the bacterial inhibition rate was calculated using formula (2) to evaluate the antibacterial effect of textiles. Where N... i N is the colony count of the sample after antibacterial treatment, corresponding to the original bacterial solution at the same gradient. N0 is the maximum colony count of the original bacterial solution.

[0077] N'% = 1 - N% (2)

[0078] Depend on Figure 2 and Figure 3 It is evident that the bacterial survival rates of Staphylococcus aureus and Escherichia coli under light irradiation in Examples 1 to 3 were significantly lower than those in Comparative Examples 1 to 6. Calculations showed that Examples 1 to 3 (using a combination of curcumin, methylene blue, and baicalein) achieved a 99.999% inhibition rate against Staphylococcus aureus; under the same testing conditions, Comparative Examples 1 to 3 (using two of curcumin, methylene blue, and baicalein) achieved a 99.000% inhibition rate against Staphylococcus aureus; and under the same testing conditions, Comparative Examples 4 to 6 (using any one of curcumin, methylene blue, and baicalein) only achieved a 90.000% inhibition rate against Staphylococcus aureus. Examples 1 to 3 (using a combination of curcumin, methylene blue, and bamboo red fungicide) showed an inhibition rate of 98% against Escherichia coli. Under the same test conditions, Comparative Examples 1 to 3 (using a combination of two of curcumin, methylene blue, and bamboo red fungicide) showed an inhibition rate of only 93% against Escherichia coli. Under the same test conditions, Comparative Examples 4 to 6 (using any one of curcumin, methylene blue, and bamboo red fungicide) showed an inhibition rate of only 84% against Escherichia coli.

[0079] This demonstrates that, under the same total amount of photosensitizer pigment, colored textiles produced using a photosensitizer pigment solution containing a mixture of curcumin, methylene blue, and bamboo red pigment exhibit significantly better antibacterial effects against Staphylococcus aureus and Escherichia coli under the same photodynamic conditions compared to solutions using any two or one of these pigments. This confirms that curcumin, methylene blue, and bamboo red pigment mutually support each other in enhancing antibacterial effects, and the combined antibacterial effect is superior to that of any two or one of these pigments combined. This effect was not previously reported and has produced unexpected technical benefits for those skilled in the art.

[0080] 3. Test of the ratio of pigment absorption coefficient K to pigment dispersion coefficient S

[0081] The ratio (K / S value) of the pigment absorption coefficient K to the pigment dispersion coefficient S of the textiles prepared in each embodiment and comparative example was measured, and the results are as follows: Figure 4As shown.

[0082] Test results show that the K / S values ​​of all embodiments and comparative examples are high in the visible light band, confirming that the method of the present invention can achieve good dyeing effect. Among them, Example 3 has the highest K / S value, indicating that the dye has the best dyeing performance under this formulation.

[0083] 4. Color fastness to rubbing test

[0084] Color fastness to rubbing was tested according to ISO 105-X12 standard: Two identical textile samples (200X50mm) and a standard cotton lining (50X50mm) were prepared for dry and wet rubbing, respectively. For the dry rubbing test, the textile was placed on the test plate and secured at both ends with clips. The dry standard cotton lining was then fixed to the rubbing head, with the rubbing head moving in the same direction as the warp of the cotton lining. The rubbing head moved back and forth 10 times (10s, vertical pressure 9N) along a 10cm linear trajectory. For the wet rubbing color fastness test, the standard cotton lining was first soaked in deionized water, then squeezed with a rubbing roller to achieve a moisture content of 95-100%. After rubbing, the wet cotton lining was dried overnight, and finally, the staining grade of the rubbing cotton lining was assessed using a gray scale. The results are shown in Table 1.

[0085] Table 1 Results of Colorfastness to Abrasion Test

[0086] Example 3 Level 5 Level 4-5 Comparative Example 3 Level 4-5 Level 4-5 Comparative Example 4 Level 4-5 Level 4 Comparative Example 6 Level 4 Level 4

[0087] According to the staining grade assessment results in Table 1, the rubbing fastness of Example 3 is superior to that of Comparative Examples 3, 4, and 6. This confirms that, under the same total amount of photosensitizer pigment, the rubbing fastness of the colored textiles produced using a photosensitizer pigment solution composed of curcumin, methylene blue, and bamboo red pigment (Example 3) is superior to that of a photosensitizer pigment solution composed of any two (Comparative Example 3) or any one (Comparative Examples 4 and 6). This demonstrates that curcumin, methylene blue, and bamboo red pigment mutually support each other in improving rubbing fastness, and the combined rubbing fastness is superior to that of any two or any one of these pigments. This effect has not been reported before this application and produces unexpected technical benefits for those skilled in the art.

[0088] The excellent color fastness to rubbing in Example 3 is due to the new dyeing formula and improved dyeing process, which can reduce the risk of fading caused by friction during use of highly effective antibacterial colored textiles while maintaining color vibrancy, thus helping to improve the overall quality and durability of highly effective antibacterial colored textiles.

[0089] 5. Primary Color Scheme

[0090] By mixing three photosensitizers (curcumin, methylene blue, and baicalein) in different proportions, a pagoda-like diagram resembling the three primary colors can be created (e.g., Figure 5 (As shown). Based on the method of Example 1, by simply adjusting the ratio of curcumin, methylene blue, and bamboo red pigment, the different color requirements for highly effective antibacterial colored textiles in mass production can be met. That is, the process based on this application can achieve the controllability of textile color by adjusting the ratio of curcumin, methylene blue, and bamboo red pigment.

[0091] For example, the highly effective antibacterial textile prepared based on the method of Example 1 (using 0.1% owf of curcumin, 1.8% owf of methylene blue, and 0.1% owf of baicalein) has a color of 1 (e.g., Figure 5 (as shown);

[0092] For example, the highly effective antibacterial textile prepared based on the method of Example 2 (using 0.9% owf of curcumin, 0.9% owf of methylene blue, and 0.2% owf of bamboo red fungin) has a color of 2 (e.g. Figure 5 (as shown);

[0093] For example, the highly effective antibacterial textile prepared based on the method of Example 3 (using 0.4% owf of curcumin, 0.5% owf of methylene blue, and 1.1% owf of bamboo red fungicide) has a color of 3 (e.g., Figure 5 (as shown);

[0094] For example, the highly effective antibacterial textile prepared based on the method of Comparative Example 1 (using 1.6% owf of curcumin and 0.4% owf of methylene blue) has a color of 4 (e.g., Figure 5 (as shown);

[0095] For example, the highly effective antibacterial textile prepared based on the method of Comparative Example 2 (methylene blue dosage of 1.9% owf and bamboo red fungicide dosage of 0.1% owf) has a color of 5 (e.g. Figure 5 (as shown);

[0096] For example, the highly effective antibacterial textile prepared based on the method of Comparative Example 3 (using 1.8% owf of curcumin and 0.2% owf of bamboo red fungicide) has a color of 6 (e.g., Figure 5 (as shown);

[0097] For example, the color of the highly effective antibacterial textile prepared based on the method of Comparative Example 4 (using 2.0% owf of curcumin) is 7 (e.g., Figure 5 (as shown);

[0098] For example, the highly effective antibacterial textile prepared based on the method of Comparative Example 5 (using 2.0% owf of methylene blue) has a color of 8 (e.g., Figure 5 (as shown);

[0099] For example, the color of the highly effective antibacterial textile prepared based on the method of Comparative Example 6 (using 2.0% owf of bamboo red fungicide) is 9 (e.g. Figure 5 (As shown).

[0100] In summary, this application, by selecting natural dyes curcumin, methylene blue, and bamboo red pigments with specific colors and photosensitive properties, combined with its specific production process (desizing → pre-shrinking → dyeing → reduction washing), can simultaneously achieve effective dyeing and high-efficiency antibacterial effects on textiles. Compared to existing processes that require dyeing with traditional dyes before antibacterial finishing, this application's process, by selecting natural dyes curcumin, methylene blue, and bamboo red pigments with specific colors and photosensitive properties, simultaneously imparts antibacterial properties to textiles, thereby simplifying the dyeing and antibacterial finishing process, improving the production efficiency of antibacterial colored textiles, and reducing their production costs. Furthermore, the high-efficiency antibacterial colored textiles produced by this application exhibit excellent dyeing effects (high dye uptake and evenness), and their photodynamic antibacterial performance is among the best in similar antibacterial colored textiles. This application's one-step dyeing and finishing process for high-efficiency antibacterial colored textiles provides the textile industry with a new, economical, and effective solution for producing high-efficiency antibacterial colored textiles. The process based on this application allows for the controllability of textile colors by adjusting the proportions of curcumin, methylene blue, and bamboo red fungicide.

[0101] The innovation of this invention lies in combining rich and adjustable colors with highly efficient photodynamic antibacterial function through a one-step dyeing and antibacterial finishing process. Based on this invention, photosensitizers can be effectively loaded onto textiles, utilizing the reactive oxygen species generated by the photosensitizers under light conditions to kill bacteria, thereby providing antibacterial properties to the textiles; simultaneously, it can also impart specific colors to the textiles. This invention's production process not only expands the application range of textiles but also simplifies the production process and reduces costs. The method of this invention has significant application potential, especially in textile production that requires rapid response to different market demands.

[0102] The embodiments provided above are not intended to limit the scope of the invention, nor are the described steps intended to limit the order of execution. Any obvious modifications made to the invention by those skilled in the art based on existing common knowledge also fall within the scope of protection defined by the claims.

Claims

1. A highly efficient antibacterial colored textile production process based on a one-step dyeing and finishing method, characterized in that, Includes the following steps: S1. Desizing: Textiles are desized and repeatedly washed to remove surface oils and impurities to obtain greige fabric; S2. Fabric pre-shrinking: Soak the fabric in clean water and then dry it. S3. Preparation of photosensitizer dye solution: Dissolve curcumin, methylene blue and bamboo red pigment simultaneously in an aqueous solution containing a solubilizer, stir overnight to allow the solubilizer to evaporate, adjust the pH to 4-5, and add a dispersant with a final concentration of 2-3 g / L to obtain the photosensitizer dye solution; wherein, the ratio of curcumin, methylene blue and bamboo red pigment is set according to the target color of the highly effective antibacterial colored textile. S4. Dyeing: The photosensitizer dye solution prepared in step S3 is used to dye the greige fabric obtained in step S2. Dyeing is carried out at room temperature, and the sum of the amounts of curcumin, methylene blue, and bamboo red fungicide is 2% owf. The bath ratio of textile to photosensitizer dye solution is 1:(25-35) g / L. Then, the temperature is raised to 80 ℃ at a first heating rate, and then raised to 125-130 ℃ at a second heating rate. The temperature is then maintained at 125-130 ℃ for 30-60 min, and then cooled to obtain the dyed textile. The first heating rate is greater than the second heating rate. S5. Reduction Cleaning: The dyed textiles obtained in S4 are subjected to reduction cleaning at 75-80 ℃ for 15-20 min using a reduction bath solution, followed by washing in water at 55-60 ℃, and then dried in a dark hot air environment at 55-65 ℃ to obtain highly effective antibacterial colored textiles; wherein, the reduction bath solution is an aqueous solution containing 1.5-2 g / L sodium dithionite and 1.5-2 g / L sodium hydroxide; the bath ratio of textiles to reduction bath solution is 1:(20-35) g / L; In step S4, the amount of curcumin is 0.1~0.9% owf, the amount of methylene blue is 0.5~1.8% owf, and the amount of bamboo red fungin is 0.1~1.1% owf.

2. The production process according to claim 1, characterized in that, In step S4, the sum of the amounts of curcumin, methylene blue, and bamboo red fungicide is 2% owf.

3. The production process according to claim 2, characterized in that, In step S4, the amount of curcumin used is 0.4% owf, the amount of methylene blue used is 0.5% owf, and the amount of bamboo red fungin used is 1.1% owf.

4. The production process according to claim 1, characterized in that, The alkaline boiling solution used in step S1 for desizing is a mixed aqueous solution containing 1-2 g / L anhydrous sodium carbonate, 2-3 g / L sodium dodecylbenzenesulfonate and 1-2 g / L soap powder.

5. The production process according to claim 1 or 4, characterized in that, In step S1, desizing involves boiling and washing at 80 ℃ for 30 min.

6. The production process according to claim 1, characterized in that, The co-solvent in step S3 is at least one of acetone and ethanol.

7. The production process according to claim 1 or 6, characterized in that, In step S3, the dispersant is at least one of sodium lignosulfonate, sodium dodecylbenzenesulfonate, and sodium dodecyl sulfonate.

8. The production process according to claim 1, characterized in that, In step S4, the first heating rate and the second heating rate are in the range of 1-2℃ / min.

9. Highly effective antibacterial colored textiles produced by the manufacturing process of any one of claims 1 to 8.

10. The application of the highly efficient antibacterial colored textile according to claim 9 in the preparation of medical textiles.

Citation Information

Patent Citations

  • Preparation method of bio-based photosensitive dye synergistic antibacterial wool fabric

    CN122304205A