A quaternary ammonium salt / borneol / photo-killing antibacterial coating
Through the penetration of ammonium salt/linoleum/light killing antibacterial coating on PET fiber, the existing textiles lack effective antibacterial function, and realized the risk of effective killing and cross -infection diseases.
Patent Information
- Application Number
- CN202310555533.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-17
- Publication Date
- 2025-01-28
- Estimated Expiration
- 2043-05-17
AI Technical Summary
Existing textiles lack effective antibacterial functions, resulting in an increased risk of bacterial growth and cross-infection diseases.
Using daily ammonium salt/采/light killing antibacterial coating, the coating is used to introduce the citizen ammonium salt into a chunolitheramine to form the citizen -molicized seasonal ammonium salt and collaborate with the Levota Dragon brain collaborative The function is significantly improved, and it has branched it on PET fiber.
The excellent antibacterial performance of PET fibers can effectively kill bacteria and reduce the risk of cross -infection diseases without damage to human flora.
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Abstract
Description
Technical Field
[0001] The invention relates to the field of antibacterial materials, in particular to a quaternary ammonium salt / borneol / photo-killing antibacterial coating. Background Art
[0002] Infections caused by microorganisms such as bacteria, viruses and fungi pose a huge threat to human health. Textile materials are ideal media for the growth of microorganisms and may cause a variety of cross-infection diseases. Since general textiles do not have antibacterial functions, ordinary fabrics will instead lead to the proliferation of a large number of various bacteria. In order to reduce the cross-infection of diseases caused by pathogenic microorganisms, antibacterial finishing of textiles and antibacterial materials has been widely studied. Among the many antibacterial agents, quaternary ammonium compounds and silver or silver-based compounds have received widespread attention as effective antibacterial agents in different fields.
[0003] Since quaternary ammonium salts have strong antibacterial ability, spectrum antibacterial, and are easy to obtain, antibacterial materials prepared with quaternary ammonium salts have good antibacterial properties and are widely used in many aspects such as medical treatment, water treatment, and food. The effective bactericidal part of quaternary ammonium salts is the cationic group formed by the combination of organic roots and single particles. Quaternary ammonium salts adsorb bacteria, and then use the nearby long carbon chain to destroy the bacterial cell membrane, causing the substances in the cell to leak out and kill the cell.
[0004] The stereochemical antimicrobial strategy is a new antimicrobial concept based on the control of microbial behavior. Based on the recognition and perception of microorganisms on the surface of materials, microorganisms can automatically leave the surface materials when they recognize stereochemical signals, protecting us from harmful organisms while not harming the inherent flora of humans, and achieving harmonious coexistence between humans and microorganisms. Facing the microbial society, this harmonious antimicrobial concept achieves "defeating the enemy without fighting"; the stereochemical antimicrobial strategy advocates that under the premise of not attacking microorganisms, by changing the stereochemical properties of the material itself, microorganisms "retreat when they see difficulty". L-borneol has good antimicrobial adhesion.
[0005] The reactive oxygen species produced by photosensitizers under light have extremely high oxidative properties, causing nonspecific cell damage and broad-spectrum bactericidal ability. At the same time, they do not produce drug resistance after repeated use and have good antibacterial properties against drug-resistant bacteria. This photodynamic antibacterial chemotherapy is an effective and low-cost antibacterial strategy.
[0006] The invention provides a quaternary ammonium salt / borneol / photo-killing antibacterial coating. The synthesized quaternary ammonium salt / borneol / photo-killing antibacterial coating is prepared by introducing a quaternary ammonium salt into a branched polyethyleneimine to form a branched quaternary ammonium salt coated with a photosensitizer. At the same time, the introduction of L-borneol produces a synergistic effect with a high-density quaternary ammonium salt in the system to make its antibacterial effect remarkable. The polymer is prepared by first using a branched polyethyleneimine to methylate the primary amine and the tertiary amine on the branched polyethyleneimine through an Eschweiler-Clarke methylation reaction. Then, L-borneol chloroacetate is introduced to react with a tertiary amine to form a quaternary ammonium salt branched polymer, which is then coated with a photosensitizer and grafted onto a PET fiber to prepare a PET fiber with excellent antibacterial properties. Summary of the invention
[0007] The purpose of the present invention is to provide a quaternary ammonium salt / borneol / photo-killing antibacterial coating in view of the deficiencies of the prior art.
[0008] The objective of the present invention is achieved through the following technical scheme: a quaternary ammonium salt / borneol / photo-killing antibacterial coating, wherein the quaternary ammonium salt / borneol / photo-killing antibacterial coating is prepared by the following steps:
[0009] (1) 1-3 g of L-borneol, 0.5-1 g of pyridine, 0.5-2 g of chloroacetyl chloride and 15-50 mL of a first solvent are mixed and stirred at -10-20° C. for 10-60 min, and then stirred at room temperature for 12-48 h; the clear liquid is filtered and removed, and a colorless oil is obtained by rotary evaporation; anhydrous ether is added, and the mixture is washed with a hydrochloric acid solution, then with a saturated sodium carbonate solution, and then with a sodium chloride solution; then dried with a desiccant, and then dried by rotary evaporation to obtain L-borneol chloroacetate;
[0010] (2) mixing 0.7-2 g of methylated branched polyethyleneimine, 1-3 g of L-borneol chloroacetate prepared in step (1) and 5-15 mL of a second solvent at 50-120° C. for 1-48 h; then centrifuging the precipitate to obtain borneol-modified methylated branched polyethyleneimine;
[0011] (3) 80-100 mL of ethanol and 10-20 mL of deionized water are mixed, the pH is adjusted to 3.0-6.0 with acetic acid, and then 1%-5% of a volume fraction of a compatibilizer crosslinker is added, and the mixture is stirred at 50-120° C. for 0.5-2 h; then 0.3-1 g of plasma-treated PET fiber is added and stirred for 24-48 h to obtain a PET fiber with a surface grafted with a compatibilizer crosslinker;
[0012] (4) dissolving the borneol-modified methylated branched polyethyleneimine prepared in step (2) in chloroform to obtain a chloroform solution of 0.005-0.015 g / mL borneol-modified methylated branched polyethyleneimine; and obtaining a photosensitizer aqueous solution of 0.001-0.003 g / mL; then taking 50-100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 50-100 mL of the photosensitizer aqueous solution, mixing them, separating the lower layer of the solution, and drying it by rotary evaporation to obtain the borneol-modified methylated branched polyethyleneimine coated with the photosensitizer;
[0013] (5) 0.5-1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) is dissolved in 1-5 mL of chloroform, 0.3-1 g of an epoxy crosslinking agent is added, and the mixture is evenly coated on a PET fiber with a surface grafted with a compatibilizing crosslinking agent and placed on a polytetrafluoroethylene substrate, and cured at 50-90° C. for 1 h to 7 d to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0014] Furthermore, the desiccant is anhydrous magnesium sulfate or anhydrous sodium sulfate.
[0015] Furthermore, the compatibilizing crosslinking agent is γ-glycidyloxypropyltrimethoxysilane, 3-glycidyloxypropyltrimethoxysilane, 3-glycidyloxypropyltriethoxysilane, 3-glycidyloxypropylmethyldiethoxysilane or 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane.
[0016] Furthermore, the photosensitizer aqueous solution is a Bengal rose red aqueous solution, a toluidine blue aqueous solution, an indocyanine green aqueous solution or a methylene blue aqueous solution.
[0017] Furthermore, the epoxy crosslinking agent is epoxy resin E51, trimethylolpropane glycidyl ether or epoxy resin E44.
[0018] Furthermore, the first solvent is anhydrous ether, tetrahydrofuran, chloroform or acetone.
[0019] Furthermore, the second solvent is toluene, xylene, N,N-dimethylformamide or N,N-dimethylacetamide.
[0020] The beneficial effects of the present invention are as follows: the branched quaternary ammonium salt coated with a photosensitizer is introduced into a PET fiber system, and the epoxy groups contained in the compatibilizing crosslinking agent and the epoxy crosslinking agent in the system can react with the remaining amino groups on the branched quaternary ammonium salt, thereby improving the crosslinking degree of the system, and the high-density quaternary ammonium salt structure can ensure excellent antibacterial ability, and the branched quaternary ammonium salt contains a stereochemical structure and has excellent antibacterial adhesion ability. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 The infrared spectra of pure PET fiber and the quaternary ammonium salt / borneol / photo-killing antibacterial coating prepared in Example 3;
[0022] Figure 2 is the antibacterial diagram against Staphylococcus aureus, where Figure 2 (a) is the antibacterial graph of pure PET fiber against Staphylococcus aureus. Figure 2 (b) is the antibacterial graph of the quaternary ammonium salt / borneol / photokilling antibacterial coating prepared in Example 3 against Staphylococcus aureus;
[0023] Figure 3 This is the nuclear magnetic hydrogen spectrum of the quaternary ammonium salt / borneol / photo-killing antibacterial coating prepared in Example 3;
[0024] Figure 4 This is a physical picture of the quaternary ammonium salt / borneol / photokilling antibacterial coating prepared in Example 3. DETAILED DESCRIPTION
[0025] In order to make the purpose, technical scheme and advantages of the present invention more clear, the present invention is further described in detail in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.
[0026] The experimental methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials described are commercially available unless otherwise specified.
[0027] The principle of the invention is to utilize Menschutkin reaction to react long-chain halogenated hydrocarbon with branched polyethyleneimine to generate quaternary ammonium salt polymer, then coat photosensitizer, and then mix and solidify with polysiloxane and epoxy crosslinking agent to obtain antibacterial PET fiber.
[0028] The methylated branched polyethyleneimine used in this experiment was synthesized in the laboratory.
[0029] Embodiment 1:
[0030] (1) 1 g of L-borneol, 0.5 g of pyridine, 0.5 g of chloroacetyl chloride and 15 mL of tetrahydrofuran were mixed and stirred at -10°C for 10 min, and then stirred at room temperature for 12 h; the supernatant was filtered and removed, and the supernatant was subjected to rotary evaporation at 45°C to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25°C to obtain L-borneol chloroacetate.
[0031] The tetrahydrofuran is the first solvent; in the present invention, the first solvent is anhydrous ether, tetrahydrofuran, chloroform or acetone.
[0032] The anhydrous magnesium sulfate is a desiccant; in the present invention, the desiccant is anhydrous magnesium sulfate or anhydrous sodium sulfate.
[0033] (2) 0.7 g of methylated branched polyethyleneimine, 1 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylformamide were mixed and stirred at 50° C. for 1 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylformamide to obtain borneol-modified methylated branched polyethyleneimine.
[0034] The N,N-dimethylformamide is the second solvent; in the present invention, the second solvent is toluene, xylene, N,N-dimethylformamide or N,N-dimethylacetamide.
[0035] (3) 80 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 6.0 with acetic acid, and then 5% by volume of γ-glycidyloxypropyltrimethoxysilane was added, and stirred at 50° C. for 2 h; then 0.3 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0036] The γ-glycidyloxypropyl trimethoxysilane is a compatibilizing crosslinking agent; in the present invention, the compatibilizing crosslinking agent is γ-glycidyloxypropyl trimethoxysilane, 3-glycidyloxypropyl trimethoxysilane, 3-glycidyloxypropyl triethoxysilane, 3-glycidyloxypropyl methyldiethoxysilane or 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane.
[0037] (4) dissolving 1.5 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.015 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtaining a 0.001 g / mL Bengal rose red aqueous solution; subsequently, mixing 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the Bengal rose red aqueous solution, the mixture was separated using a separating funnel, and the lower layer of the solution was taken and dried by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0038] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 1 mL of chloroform, 1 g of trimethylolpropane glycidyl ether was added, and the mixture was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene substrate, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0039] The trimethylolpropane glycidyl ether is an epoxy crosslinking agent; in the present invention, the epoxy crosslinking agent is epoxy resin E51, trimethylolpropane glycidyl ether or epoxy resin E44.
[0040] Embodiment 2:
[0041] (1) 3 g of L-borneol, 1 g of pyridine, 2 g of chloroacetyl chloride and 50 mL of tetrahydrofuran were mixed and stirred at 20° C. for 60 min, and then stirred at room temperature for 48 h; the supernatant was filtered out, and the supernatant was subjected to rotary evaporation at 45° C. to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25° C. to obtain L-borneol chloroacetate.
[0042] (2) 2 g of methylated branched polyethyleneimine, 3 g of L-borneol chloroacetate prepared in step (1) and 15 mL of N,N-dimethylformamide were mixed and stirred at 120° C. for 48 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylformamide to obtain borneol-modified methylated branched polyethyleneimine.
[0043] (3) Mix 100 mL of ethanol and 10 mL of deionized water, adjust the pH to 3.0 with acetic acid, add 1% by volume of γ-glycidyloxypropyltrimethoxysilane, and stir at 120° C. for 0.5 h; then add 1 g of plasma-treated PET fiber and stir for 24 h, then take out the PET fiber to obtain a PET fiber with a surface grafted compatibilizer crosslinking agent.
[0044] (4) Dissolve 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 200 mL of chloroform to obtain a 0.005 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtain a 0.003 g / mL Bengal rose red aqueous solution; subsequently, 50 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 50 mL of the Bengal rose red aqueous solution were mixed and stirred, and then separated using a separating funnel, and the lower layer solution was taken and dried by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0045] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 5 mL of chloroform, and after adding 0.3 g of trimethylolpropane glycidyl ether, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene board, and cured at 90° C. for 1 h to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0046] Embodiment 3:
[0047] (1) 1 g of L-borneol, 0.77 g of pyridine, 0.73 g of chloroacetyl chloride and 20 mL of tetrahydrofuran were mixed and stirred at 0° C. for 30 min, and then stirred at room temperature for 24 h; the supernatant was filtered out, and the supernatant was evaporated at 45° C. to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25° C. to obtain L-borneol chloroacetate.
[0048] (2) 1 g of methylated branched polyethyleneimine, 1.214 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylformamide were mixed and stirred at 70° C. for 48 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylformamide to obtain borneol-modified methylated branched polyethyleneimine.
[0049] (3) Mix 90 mL of ethanol and 10 mL of deionized water, adjust the pH to 4.0 with acetic acid, add 2% by volume of γ-glycidyloxypropyltrimethoxysilane, and stir at 70°C for 0.5 h; then add 0.5 g of plasma-treated PET fiber and stir for 48 h, then take out the PET fiber to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0050] (4) dissolving 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtaining a 0.002 g / mL Bengal rose red aqueous solution; subsequently, mixing 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the Bengal rose red aqueous solution, separating the solutions using a separating funnel, taking the lower layer and drying it by rotary evaporation at 40° C., to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0051] (5) 0.5 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 1.5 mL of chloroform, and after adding 0.5 g of trimethylolpropane glycidyl ether, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene substrate, and cured at 70° C. for 1 day to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0052] Figure 1 It is the infrared spectra of pure PET fiber and the quaternary ammonium salt / borneol / photo-killing antibacterial coating prepared in Example 3. Figure 3 This is the H NMR spectrum of the quaternary ammonium salt / borneol / photo-killing antibacterial coating prepared in Example 3. Figure 1 As shown, "PET" is pure PET fiber without adding quaternary ammonium salt material, and "PDT-30" is the quaternary ammonium salt / borneol / photo-killing antibacterial coating prepared in Example 3. Figure 1 It can be seen that the infrared spectrum of the quaternary ammonium salt / borneol / photon-killing antibacterial coating prepared in Example 3 has an absorption peak at 907.08 cm-1, indicating that the quaternary ammonium salt / borneol / photon-killing antibacterial coating prepared in Example 3 is grafted with quaternary ammonium salt. Figure 3 It can be seen that the nuclear magnetic hydrogen spectrum of the quaternary ammonium salt / borneol / photo-killing antibacterial coating prepared in Example 3 has a displacement peak at 3.63 belonging to the hydrogen on the quaternary ammonium salt, which also confirms the synthesis of the polyethyleneimine long carbon chain quaternary ammonium salt.
[0053] Figure 2 is the antibacterial diagram against Staphylococcus aureus, where Figure 2 (a) is the antibacterial graph of pure PET fiber against Staphylococcus aureus. Figure 2(b) is an antibacterial graph of the quaternary ammonium salt / borneol / light-killing antibacterial coating prepared in Example 3 against Staphylococcus aureus. The antibacterial rate of the quaternary ammonium salt / borneol / light-killing antibacterial coating prepared in Example 3 against Staphylococcus aureus is 98.9%. The quaternary ammonium salt / borneol / light-killing antibacterial coating prepared in Example 3 is a PET fiber to which a certain amount of borneol-modified methylated branched polyethyleneimine coated with a photosensitizer is added, and has excellent antibacterial properties.
[0054] Figure 4 This is a physical picture of the quaternary ammonium salt / borneol / photokilling antibacterial coating prepared in Example 3.
[0055] Embodiment 4:
[0056] (1) 1 g of L-borneol, 0.5 g of pyridine, 0.5 g of chloroacetyl chloride and 5 mL of chloroform were mixed and stirred at 10° C. for 20 min, and then stirred at room temperature for 12 h; the supernatant was filtered out, and the supernatant was evaporated at 45° C. to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25° C. to obtain L-borneol chloroacetate.
[0057] (2) 1 g of methylated branched polyethyleneimine, 1 g of L-borneol chloroacetate prepared in step (1) and 5 mL of toluene were mixed and stirred at 50° C. for 24 h; after the reaction was completed, the precipitate was centrifuged to remove the toluene to obtain borneol-modified methylated branched polyethyleneimine.
[0058] (3) 80 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 6 with acetic acid, and then 5% by volume of 2-(3,4-epoxycyclohexyl)ethyltriethoxysilane was added, and stirred at 50° C. for 2 h; then 1 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0059] (4) Dissolve 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtain a 0.002 g / mL aqueous solution of toluidine blue; subsequently, mix and stir 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the aqueous solution of toluidine blue, separate the solutions using a separating funnel, take the lower layer of the solution and dry it by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0060] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 3 mL of chloroform, and after adding 0.5 g of epoxy resin E51, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene board, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0061] Embodiment 5:
[0062] (1) 1 g of L-borneol, 1 g of pyridine, 2 g of chloroacetyl chloride and 5 mL of acetone were mixed and stirred at 5° C. for 10 min, and then stirred at room temperature for 12 h; the supernatant was filtered and removed, and the supernatant was evaporated at 45° C. to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25° C. to obtain L-borneol chloroacetate.
[0063] (2) 1.5 g of methylated branched polyethyleneimine, 2 g of borneol chloroacetate prepared in step (1) and 10 mL of xylene were mixed and stirred at 70° C. for 48 h; after the reaction was completed, the precipitate was centrifuged to remove the xylene to obtain borneol-modified methylated branched polyethyleneimine.
[0064] (3) 80 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 6 with acetic acid, and then 5% by volume of γ-glycidyloxypropyltrimethoxysilane was added, and stirred at 50° C. for 2 h; then 0.5 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0065] (4) Dissolve 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtain a 0.002 g / mL aqueous solution of indocyanine green; subsequently, mix and stir 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the aqueous solution of indocyanine green, separate the solutions using a separating funnel, take the lower layer of the solution and dry it by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0066] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 2 mL of chloroform, and after adding 0.5 g of epoxy resin E44, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene substrate, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0067] Embodiment 6:
[0068] (1) 1 g of L-borneol, 0.5 g of pyridine, 0.5 g of chloroacetyl chloride and 5 mL of chloroform were mixed and stirred at 0° C. for 10 min, and then stirred at room temperature for 12 h; the supernatant was filtered out, and the supernatant was evaporated at 45° C. to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous sodium sulfate, and then dried by rotary evaporation at 25° C. to obtain L-borneol chloroacetate.
[0069] (2) 0.7 g of methylated branched polyethyleneimine, 1 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylacetamide were mixed and stirred at 50° C. for 24 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylacetamide to obtain borneol-modified methylated branched polyethyleneimine.
[0070] (3) 80 mL of ethanol and 10 mL of deionized water were mixed, the pH was adjusted to 4.5 with acetic acid, and then 5% by volume of 3-glycidyloxypropyltrimethoxysilane was added, and stirred at 50° C. for 2 h; then 0.3 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0071] (4) Dissolve 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtain a 0.002 g / mL aqueous solution of methylene blue; subsequently, 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the aqueous solution of methylene blue were mixed and stirred, and then separated using a separating funnel, and the lower layer of the solution was taken and dried by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0072] (5) 0.5 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 5 mL of chloroform, and after adding 0.5 g of trimethylolpropane glycidyl ether, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene board, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0073] Embodiment 7:
[0074] (1) 1 g of L-borneol, 0.65 g of pyridine, 0.77 g of chloroacetyl chloride and 5 mL of tetrahydrofuran were mixed and stirred at 0° C. for 30 min, and then stirred at room temperature for 12 h; the supernatant was filtered out, and the supernatant was evaporated at 45° C. to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous sodium sulfate, and then dried by rotary evaporation at 25° C. to obtain L-borneol chloroacetate.
[0075] (2) 1 g of methylated branched polyethyleneimine, 2.3 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylformamide were mixed and stirred at 70° C. for 24 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylformamide to obtain borneol-modified methylated branched polyethyleneimine.
[0076] (3) 90 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 5 with acetic acid, and then 4% by volume of 3-glycidyloxypropyltriethoxysilane was added, and stirred at 50° C. for 2 h; then 0.3 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0077] (4) dissolving 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtaining a 0.002 g / mL Bengal rose red aqueous solution; subsequently, mixing 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the Bengal rose red aqueous solution, the mixture was separated using a separating funnel, and the lower layer of the solution was taken and dried by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0078] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 5 mL of chloroform, and after adding 0.5 g of epoxy resin E51, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene substrate, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0079] Embodiment 8:
[0080] (1) 1 g of L-borneol, 1 g of pyridine, 1 g of chloroacetyl chloride and 20 mL of tetrahydrofuran were mixed and stirred at -10°C for 10 min, and then stirred at room temperature for 12 h; the supernatant was filtered out, and the supernatant was evaporated at 45°C to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25°C to obtain L-borneol chloroacetate.
[0081] (2) 0.7 g of methylated branched polyethyleneimine, 1 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylformamide were mixed and stirred at 50° C. for 24 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylformamide to obtain borneol-modified methylated branched polyethyleneimine.
[0082] (3) 80 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 6 with acetic acid, and then 5% by volume of 3-glycidyloxypropylmethyldiethoxysilane was added, and stirred at 80° C. for 2 h; then 0.3 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0083] (4) Dissolve 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtain a 0.002 g / mL aqueous solution of toluidine blue; subsequently, mix and stir 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the aqueous solution of toluidine blue, separate the solutions using a separating funnel, take the lower layer of the solution and dry it by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0084] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 2 mL of chloroform, and after adding 0.5 g of trimethylolpropane glycidyl ether, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene board, and cured at 70° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0085] Embodiment 9:
[0086] (1) 1 g of L-borneol, 0.5 g of pyridine, 0.5 g of chloroacetyl chloride and 5 mL of tetrahydrofuran were mixed and stirred at -10°C for 10 min, and then stirred at room temperature for 12 h; the supernatant was filtered and removed, and the supernatant was subjected to rotary evaporation at 45°C to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25°C to obtain L-borneol chloroacetate.
[0087] (2) 0.7 g of methylated branched polyethyleneimine, 1 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylacetamide were mixed and stirred at 50° C. for 24 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylacetamide to obtain borneol-modified methylated branched polyethyleneimine.
[0088] (3) 80 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 6 with acetic acid, and then 3% by volume of γ-glycidyloxypropyltrimethoxysilane was added, and stirred at 50° C. for 2 h; then 0.3 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0089] (4) dissolving 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtaining a 0.002 g / mL Bengal rose red aqueous solution; subsequently, mixing 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the Bengal rose red aqueous solution, the mixture was separated using a separating funnel, and the lower layer of the solution was taken and dried by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0090] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 5 mL of chloroform, and after adding 0.5 g of epoxy resin E44, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene board, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0091] Embodiment 10:
[0092] (1) 1 g of L-borneol, 0.5 g of pyridine, 0.5 g of chloroacetyl chloride and 5 mL of tetrahydrofuran were mixed and stirred at -10°C for 10 min, and then stirred at room temperature for 12 h; the supernatant was filtered and removed, and the supernatant was subjected to rotary evaporation at 45°C to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25°C to obtain L-borneol chloroacetate.
[0093] (2) 1 g of methylated branched polyethyleneimine, 1 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylformamide were mixed and stirred at 50° C. for 24 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylformamide to obtain borneol-modified methylated branched polyethyleneimine.
[0094] (3) 80 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 6 with acetic acid, and then 5% by volume of γ-glycidyloxypropyltrimethoxysilane was added, and stirred at 50° C. for 2 h; then 0.3 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0095] (4) dissolving 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtaining a 0.002 g / mL Bengal rose red aqueous solution; subsequently, mixing 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the Bengal rose red aqueous solution, the mixture was separated using a separating funnel, and the lower layer of the solution was taken and dried by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0096] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 5 mL of chloroform, and after adding 0.5 g of epoxy resin E44, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene board, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0097] Embodiment 11:
[0098] (1) 1 g of L-borneol, 0.5 g of pyridine, 0.5 g of chloroacetyl chloride and 5 mL of tetrahydrofuran were mixed and stirred at -10°C for 10 min, and then stirred at room temperature for 12 h; the supernatant was filtered and removed, and the supernatant was subjected to rotary evaporation at 45°C to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25°C to obtain L-borneol chloroacetate.
[0099] (2) 0.7 g of methylated branched polyethyleneimine, 1 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylformamide were mixed and stirred at 50° C. for 24 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylformamide to obtain borneol-modified methylated branched polyethyleneimine.
[0100] (3) 80 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 6 with acetic acid, and then 5% by volume of γ-glycidyloxypropyltrimethoxysilane was added, and stirred at 50° C. for 2 h; then 0.3 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0101] (4) dissolving 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtaining a 0.002 g / mL Bengal rose red aqueous solution; subsequently, mixing 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the Bengal rose red aqueous solution, the mixture was separated using a separating funnel, and the lower layer of the solution was taken and dried by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0102] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 5 mL of chloroform, and after adding 1 g of epoxy resin E44, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene substrate, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0103] Embodiment 12:
[0104] (1) 1 g of L-borneol, 0.5 g of pyridine, 0.5 g of chloroacetyl chloride and 5 mL of acetone were mixed and stirred at -10°C for 10 min, and then stirred at room temperature for 12 h; the supernatant was filtered and removed, and the supernatant was evaporated at 45°C to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25°C to obtain L-borneol chloroacetate.
[0105] (2) 0.7 g of methylated branched polyethyleneimine, 1 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylformamide were mixed and stirred at 50° C. for 24 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylformamide to obtain borneol-modified methylated branched polyethyleneimine.
[0106] (3) 80 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 6 with acetic acid, and then 5% by volume of γ-glycidyloxypropyltrimethoxysilane was added, and stirred at 50° C. for 2 h; then 0.3 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0107] (4) dissolving 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtaining a 0.002 g / mL Bengal rose red aqueous solution; subsequently, mixing 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the Bengal rose red aqueous solution, the mixture was separated using a separating funnel, and the lower layer of the solution was taken and dried by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0108] (5) 1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 5 mL of chloroform, and after adding 1 g of epoxy resin E55, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene board, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0109] Embodiment 13:
[0110] (1) 3 g of L-borneol, 1 g of pyridine, 1 g of chloroacetyl chloride and 15 mL of anhydrous ether were mixed and stirred at 5° C. for 10 min, and then stirred at room temperature for 12 h; the supernatant was filtered out, and the supernatant was evaporated at 45° C. to obtain a colorless oil; 20 mL of anhydrous ether was added to the obtained colorless oil, and the oil was washed with 20 mL of 1 mol / L hydrochloric acid solution, then washed with 20 mL of saturated sodium carbonate solution, and then washed with 20 mL of sodium chloride solution; then dried with anhydrous magnesium sulfate, and then dried by rotary evaporation at 25° C. to obtain L-borneol chloroacetate.
[0111] (2) 0.7 g of methylated branched polyethyleneimine, 1 g of L-borneol chloroacetate prepared in step (1) and 5 mL of N,N-dimethylformamide were mixed and stirred at 50° C. for 24 h; after the reaction was completed, the precipitate was centrifuged to remove N,N-dimethylformamide to obtain borneol-modified methylated branched polyethyleneimine.
[0112] (3) 80 mL of ethanol and 20 mL of deionized water were mixed, the pH was adjusted to 6 with acetic acid, and then 5% by volume of γ-glycidyloxypropyltrimethoxysilane was added, and stirred at 50° C. for 2 h; then 0.3 g of plasma-treated PET fiber was added and stirred for 48 h, and the PET fiber was taken out to obtain PET fiber with a surface grafted compatibilizer crosslinking agent.
[0113] (4) Dissolve 1 g of the borneol-modified methylated branched polyethyleneimine obtained in step (2) in 100 mL of chloroform to obtain a 0.01 g / mL chloroform solution of the borneol-modified methylated branched polyethyleneimine, and simultaneously obtain a 0.002 g / mL aqueous solution of indocyanine green; subsequently, mix and stir 100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 100 mL of the aqueous solution of indocyanine green, separate the solutions using a separating funnel, take the lower layer of the solution and dry it by rotary evaporation at 40° C. to obtain the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer.
[0114] (5) 0.5 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) was dissolved in 3 mL of chloroform, and after adding 0.1 g of trimethylolpropane glycidyl ether, it was evenly coated on the PET fiber with a surface grafted compatibilizer crosslinking agent prepared in step (3) and placed on a polytetrafluoroethylene substrate, and cured at 50° C. for 7 days to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
[0115] The above description is only a preferred embodiment of the present invention and is not intended to limit 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 quaternary ammonium salt / borneol / photo-killing antibacterial coating, characterized in that: The quaternary ammonium salt / borneol / photo-killing antibacterial coating is prepared by the following steps: (1) 1-3 g of L-borneol, 0.5-1 g of pyridine, 0.5-2 g of chloroacetyl chloride and 15-50 mL of the first solvent were mixed and stirred at -10-20° C. for 10-60 min, and then stirred at room temperature for 12-48 h; the clear liquid was removed by filtration, and a colorless oil was obtained by rotary evaporation; Add anhydrous ether, wash with hydrochloric acid solution, then wash with saturated sodium carbonate solution, and then wash with sodium chloride solution; then dry with a desiccant, and then dry by rotary evaporation to obtain L-borneol chloroacetate; (2) mixing 0.7-2 g of methylated branched polyethyleneimine, 1-3 g of L-borneol chloroacetate prepared in step (1) and 5-15 mL of a second solvent at 50-120° C. for 1-48 h; then centrifuging the precipitate to obtain borneol-modified methylated branched polyethyleneimine; (3) 80-100 mL of ethanol and 10-20 mL of deionized water are mixed, the pH is adjusted to 3.0-6.0 with acetic acid, and then 1%-5% of a volume fraction of a compatibilizer crosslinker is added, and the mixture is stirred at 50-120° C. for 0.5-2 h; then 0.3-1 g of plasma-treated PET fiber is added and stirred for 24-48 h to obtain a PET fiber with a surface grafted with a compatibilizer crosslinker; The compatibilizing crosslinking agent is γ-glycidyloxypropyl trimethoxysilane, 3-glycidyloxypropyl trimethoxysilane, 3-glycidyloxypropyl triethoxysilane, 3-glycidyloxypropyl methyl diethoxysilane or 2-(3,4-epoxycyclohexyl)ethyl triethoxysilane; (4) dissolving the borneol-modified methylated branched polyethyleneimine prepared in step (2) in chloroform to obtain a chloroform solution of 0.005-0.015 g / mL borneol-modified methylated branched polyethyleneimine; and obtaining a photosensitizer aqueous solution of 0.001-0.003 g / mL; then taking 50-100 mL of the chloroform solution of the borneol-modified methylated branched polyethyleneimine and 50-100 mL of the photosensitizer aqueous solution, mixing them, separating the lower layer of the solution, and drying it by rotary evaporation to obtain the borneol-modified methylated branched polyethyleneimine coated with the photosensitizer; (5) 0.5-1 g of the borneol-modified methylated branched polyethyleneimine coated with a photosensitizer prepared in step (4) is dissolved in 1-5 mL of chloroform, 0.3-1 g of an epoxy crosslinking agent is added, and the mixture is evenly coated on a PET fiber with a surface grafted with a compatibilizing crosslinking agent and placed on a polytetrafluoroethylene substrate, and cured at 50-90° C. for 1 h to 7 d to obtain a quaternary ammonium salt / borneol / photokilling antibacterial coating.
2. A quaternary ammonium salt / borneol / photo-killing antibacterial coating according to claim 1, characterized in that: The desiccant is anhydrous magnesium sulfate or anhydrous sodium sulfate.
3. A quaternary ammonium salt / borneol / photo-killing antibacterial coating according to claim 1, characterized in that: The photosensitizer aqueous solution is a Bengal rose red aqueous solution, a toluidine blue aqueous solution, an indocyanine green aqueous solution or a methylene blue aqueous solution.
4. A quaternary ammonium salt / borneol / photo-killing antibacterial coating according to claim 1, characterized in that: The epoxy crosslinking agent is epoxy resin E51, trimethylolpropane glycidyl ether or epoxy resin E44.
5. A quaternary ammonium salt / borneol / photo-killing antibacterial coating according to claim 1, characterized in that: The first solvent is anhydrous ether, tetrahydrofuran, chloroform or acetone.
6. A quaternary ammonium salt / borneol / photo-killing antibacterial coating according to claim 1, characterized in that: The second solvent is toluene, xylene, N,N-dimethylformamide or N,N-dimethylacetamide.
Citation Information
Patent Citations
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