A zinc oxide grafted modified antibacterial biomimetic blood-like polyester / polyamide chopped short fiber, its preparation method and application

CN122980201APending Publication Date: 2026-10-27DONGHUA UNIV +1
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Patent Information

Application Number
CN202611082771.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-07-21
Publication Date
2026-10-27

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Benefits of technology

本申请通过弱碱温和刻蚀时间的精准把控、氧化锌低浓度单层均匀负载的实现,以及梯度控温分段干燥固化的协同作用,成功解决了传统抗菌改性工艺造成的血丝发白、褪色及纹理遮蔽问题,使得仿生血丝纤维的天然红色层次与透光性能得以完整保留。

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Abstract

This application relates to the field of biomedical biomimetic fiber technology, and discloses a zinc oxide grafted modified antibacterial biomimetic blood-like polyester / polyamide chopped fiber, its preparation method, and its application. The preparation method includes the following steps: pretreating the biomimetic blood-like polyester / polyamide chopped fiber, followed by alkaline etching and hydroxylation activation to obtain activated fiber; pre-modifying the surface of the activated fiber with a silane coupling agent to obtain a precursor; immersing the precursor in a grafting solution and performing graft deposition on its surface using room-temperature ultrasonic impregnation to obtain an intermediate; and subjecting the intermediate to gradient-heat drying to obtain the zinc oxide grafted modified antibacterial biomimetic blood-like polyester / polyamide chopped fiber. The zinc oxide grafted modified antibacterial biomimetic blood-like polyester / polyamide chopped fiber prepared in this application retains the original appearance and color of biomimetic blood-like fibers, meeting the aesthetic requirements of dental prostheses, while maintaining its original toughening and reinforcing properties, exhibiting highly effective antibacterial effects, and demonstrating good stability.
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Description

Technical Field

[0001] This application relates to the field of biomedical biomimetic fiber technology, and in particular to a zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide short-cut fiber, its preparation method and application. Background Technology

[0002] Conventional removable dentures and partial dentures mostly use PMMA pink resin as the base material. Its color is monotonous and lacks the natural capillary texture of the gums, resulting in insufficient realism and aesthetics. Existing improvement methods include hand-painting blood vessels on the surface, pre-embedding red cotton thread, and filling with commercially stained short fibers. However, hand-painted blood vessels have poor wear resistance and low mass production consistency; red cotton thread has weak bonding with the resin interface, making it prone to falling off and fading over time in the oral environment, and the fiber morphology and color are far inferior to natural blood vessels.

[0003] To address the aforementioned pain points, the applicant independently developed biomimetic blood-like polyester / polyamide chopped fibers (patent CN122279785 A). Utilizing a masterbatch blending melt spinning process, the red pigment is evenly distributed within the fiber, resulting in a color depth closely resembling natural gingival blood streaks. When filled into denture resin, it forms a natural, translucent blood-like texture, while significantly improving the flexural strength and modulus of the PMMA base, balancing aesthetics and mechanical properties. However, this biomimetic blood-like polyester / polyamide chopped fiber itself lacks antibacterial capabilities. Prolonged exposure to the moist oral environment allows Staphylococcus aureus and Candida albicans to easily adhere and colonize the base surface and fiber gaps, leading to complications such as denture stomatitis, gingival redness and swelling, and bad breath. Therefore, antibacterial modification is urgently needed.

[0004] However, conventional antibacterial modification methods are insufficient to meet the aesthetic requirements of this fiber. Conventional silver coatings or high-concentration inorganic antibacterial powder impregnation easily lead to whitening, yellowing, and loss of opacity in the fiber, destroying its natural layered red color. Incorporation into resin can also cause color differences in the denture base and reduced translucency, significantly diminishing the biomimetic effect. Furthermore, traditional processes rely heavily on physical adsorption to load antibacterial components, resulting in weak binding forces. These components quickly detach under saliva immersion and chewing friction, leading to a rapid decline in antibacterial efficacy and potential irritation of the oral mucosa by the detached powder, posing a safety risk. In addition, the lack of gentle activation pretreatment results in a scarcity of active sites on the fiber surface, leading to uneven antibacterial powder loading and poor stability. Currently, there is no complete process that can achieve long-term stable antibacterial effects while fully preserving the original color and morphology, failing to simultaneously meet the triple requirements of biomimetic aesthetics, mechanical reinforcement, and long-term oral antibacterial action for denture bases. Summary of the Invention

[0005] This application provides a zinc oxide graft-modified antibacterial biomimetic blood-fiber polyester / polyamide short-cut fiber, its preparation method and application, aiming to solve the technical problems of existing antibacterial modification processes that easily damage the appearance and color of the fiber blood fibers, have weak adhesion of antibacterial powder, and have poor antibacterial durability.

[0006] To achieve the above objectives, the present application adopts the following technical solution.

[0007] The first aspect of this application provides a method for preparing zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide chopped short fibers, comprising the following steps: S1, pre-treat biomimetic blood-fiber polyester / polyamide short-cut fibers, and then perform alkaline etching and hydroxylation activation to obtain activated fibers; S2, the activated fibers are pre-modified with silane using a silane coupling agent to obtain a precursor; S3, the precursor is immersed in the grafting solution and grafted onto its surface by ultrasonic impregnation at room temperature to obtain the intermediate; S4. The intermediate is subjected to gradient temperature drying to obtain zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide chopped fibers.

[0008] Preferably, the preprocessing specifically includes: The biomimetic blood-like polyester / polyamide short-cut fibers were ultrasonically cleaned in sequence with acetone, anhydrous ethanol and deionized water, and then dried at 80~110℃ to constant weight. The alkaline etching hydroxylation activation specifically involves: The pretreated biomimetic blood-like polyester / polyamide chopped fibers were immersed in an alkaline solution and etched at 60°C for 1-3 hours. They were then washed until neutral and dried at 80-110°C to constant weight to obtain activated fibers.

[0009] More preferably, the alkaline solution is a NaOH solution with a concentration of 0.1~10wt%.

[0010] Further preferably, the mass-to-volume ratio of the pretreated biomimetic blood-like polyester / polyamide short-cut fibers to the alkaline solution is 1g:30~60mL. Preferably, the silane coupling agent modified solution is prepared by the following method: Add KH-550 coupling agent to a mixed solvent of anhydrous ethanol and deionized water, and stir to allow it to fully hydrolyze, thus obtaining a silane coupling agent modified solution; wherein the volume fraction of KH-550 coupling agent is 0.5-10%; The surface silane pre-modification specifically involves: The activated fibers are immersed in a silane coupling agent modified solution, ultrasonically treated at room temperature for 90-120 minutes, then rinsed with anhydrous ethanol and dried.

[0011] Preferably, the grafting solution is prepared by the following method: ZnO is added to a mixed solvent of anhydrous ethanol and deionized water, and dispersed by stirring and ultrasonication to obtain a ZnO suspension dispersion, i.e., graft solution. The solid content of ZnO in the grafting solution is 0.2~1.5 g / L; The volume ratio of anhydrous ethanol to deionized water is 9:1.

[0012] Preferably, the mass-to-volume ratio of the precursor to the grafting solution is 1g:30~65mL.

[0013] The preferred gradient heating method is as follows: The intermediate is first pre-dried at 50~80℃ for 60 min, and then heated to 80~120℃ for constant temperature curing for 2 h.

[0014] A second aspect of this application provides zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide chopped fibers prepared by the above preparation method.

[0015] A third aspect of this application provides the application of zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide chopped fibers prepared by the above preparation method in denture base materials.

[0016] Compared with the prior art, the beneficial effects of this application are as follows: This application successfully solves the problems of whitening, fading and texture obscuring caused by traditional antibacterial modification processes by precisely controlling the etching time with weak alkali and mild etching, achieving uniform loading of a single layer with low concentration of zinc oxide, and the synergistic effect of gradient temperature-controlled segmented drying and curing. This allows the natural red layers and light transmission properties of the biomimetic blood fiber to be completely preserved.

[0017] 1) It fully preserves the original appearance and color of the biomimetic blood streaks, adapting to the aesthetic requirements of dental prostheses, while maintaining its original toughening and reinforcing properties.

[0018] 2) Highly effective antibacterial, adapted to the moist environment of oral saliva, with an antibacterial rate of 99.04% against Staphylococcus aureus and 95.61% against Candida albicans.

[0019] 3) Silane coupling agents act as molecular bridges to achieve chemical bonding and fixation of zinc oxide, resulting in uniform powder dispersion, resistance to saliva rinsing and easy shedding, and good stability.

[0020] 4) The process is safe and simple, with no harmful residues and high medical biosafety. Attached Figure Description

[0021] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments recorded in this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1Fourier transform infrared spectra of ungrafted biomimetic blood-like polyester short fibers from Examples 1-3 and Comparative Example 2. Figure 2 Physical images of the chopped fibers prepared in Examples 1-7 and Comparative Examples 1-2; Figure 3 The image shows a physical photograph of the denture base composite material prepared by filling PMMA with chopped fibers using Comparative Example 1 and Example 2. Detailed Implementation

[0023] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.

[0024] In the following description of this embodiment, the terms "including", "comprising", "having", and "containing" are all open-ended terms, meaning that they include but are not limited to.

[0025] In the following description of this embodiment, the term "and / or" is used to describe the association relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, B existing alone, and A and B existing simultaneously. A and B can be singular or plural. The character " / " generally indicates that the preceding and following related objects have an "or" relationship.

[0026] In the following description of this embodiment, the term "at least one" means one or more, and "more than one" means two or more. "At least one of the following" or similar expressions refer to any combination of these items, including any combination of single or multiple items. For example, "at least one of a, b, or c", or "at least one of a, b, and c", can both mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple.

[0027] The terminology used in the embodiments of this application is for the purpose of describing particular embodiments only and is not intended to be limiting of this application. The singular forms "a" and "the" as used in the embodiments of this application and the appended claims are also intended to include the plural forms, unless the context clearly indicates otherwise.

[0028] Those skilled in the art should understand that, in the following description of the embodiments of this application, the sequence of numbers does not imply the order of execution. Some or all steps may be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this application.

[0029] Those skilled in the art will understand that the numerical ranges in the embodiments of this application should be understood as each intermediate value between the upper and lower limits of the specifically disclosed range. Each smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this application. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0030] Unless otherwise stated, the technical / scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains. While this application describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this application. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0031] This application describes the preparation of antibacterial biomimetic filament polyester / polyamide chopped fibers through a process involving pretreatment to remove impurities, surface hydroxyl activation, silane coupling agent pretreatment modification, ultrasonic-assisted in-situ grafting of zinc oxide dispersion, and gradient temperature curing and anchoring. The method for preparing the filament polyester / polyamide chopped fibers is described in another invention patent of the applicant, CN 122279785 A.

[0032] The preparation method specifically includes the following steps: S1, pre-treat biomimetic blood-fiber polyester / polyamide short-cut fibers, and then perform alkaline etching and hydroxylation activation to obtain activated fibers; In this application, the biomimetic blood-fiber polyester / polyamide chopped fibers are pretreated to remove impurities. Specifically, the biomimetic blood-fiber polyester / polyamide chopped fibers are ultrasonically cleaned sequentially with acetone, anhydrous ethanol, and deionized water to remove surface dust, spinning oil residue, and molding processing aids; then they are dried at 80~110℃ to constant weight for later use.

[0033] In this application, pretreated biomimetic blood-like polyester / polyamide chopped fibers are immersed in an alkaline solution and subjected to a gentle etching reaction at a constant temperature of 60°C in a water bath for 1-3 hours. The alkaline solution is preferably a NaOH aqueous solution with a concentration of 0.1-10 wt%. The preferred mass-to-volume ratio of the pretreated biomimetic blood-like polyester / polyamide chopped fibers to the alkaline solution is 1 g: 30-60 mL. This application utilizes a low-concentration alkaline solution to lightly etch the fiber surface, increasing the number of surface active hydroxyl groups without eroding the red masterbatch pigment inside the fiber or altering the original color and filamentous morphology of the blood vessels. After alkaline etching, the fiber is washed until the pH is neutral to completely remove residual alkaline solution and hydrolysis byproducts; then it is dried at 80-110℃ to constant weight to obtain activated fibers with a surface rich in active hydroxyl functional groups.

[0034] S2, the activated fibers are pre-modified with silane using a silane coupling agent to obtain a precursor; Specifically, KH-550 coupling agent is added to a mixed solvent of anhydrous ethanol and deionized water, and stirred to ensure complete hydrolysis, thus obtaining a silane coupling agent modified solution. The activated fiber is immersed in the hydrolyzed silane coupling agent modified solution and ultrasonically treated at room temperature for 90-120 minutes. Then, it is rinsed with anhydrous ethanol to remove unreacted free coupling agent from the surface, and finally dried at 80°C. The coupling agent undergoes dehydration condensation with the hydroxyl groups on the fiber surface, completing the functionalization modification of the fiber surface.

[0035] The volume ratio of anhydrous ethanol to deionized water is preferably 9:1; the volume fraction of KH-550 coupling agent in the silane coupling agent modified solution is 0.5-10%, preferably 2%.

[0036] S3, the precursor is immersed in the grafting solution and grafted onto its surface by ultrasonic impregnation at room temperature to obtain the intermediate; In this application, the grafting solution is prepared by the following method: ZnO was added to a mixed solvent of anhydrous ethanol and deionized water, and dispersed by stirring and ultrasonication to obtain a ZnO suspension, i.e., the grafting solution. The volume ratio of anhydrous ethanol to deionized water was 9:1.

[0037] Specifically, ZnO is added to a mixed solvent of anhydrous ethanol and deionized water, and the powder is first magnetically stirred at room temperature for 10 min to break up any agglomerates. Then, it is ultrasonically dispersed for 20–30 min to obtain a uniform, stable suspension without precipitate.

[0038] In this application, the solid content of ZnO in the grafting solution is 0.2~1.5 g / L. Using a low concentration of zinc oxide avoids excessive powder accumulation that could obscure the red streaks of the fiber, preventing the fiber from whitening, losing its opacity, or discoloring.

[0039] The mass-to-volume ratio of the precursor to the grafting solution is 1g:30~65mL. The precursor is completely immersed in the ZnO suspension dispersion to ensure complete fiber wetting without floating or stacking. Ultrasonic impregnation is performed at room temperature for 40-60 minutes. The ultrasonic action promotes the uniform dispersion and adsorption of trace ZnO particles on the fiber surface, and they coordinate and bond with the active groups of the silane coupling agent, achieving uniform thin-layer in-situ grafting deposition of zinc oxide. The trace monolayer of zinc oxide does not obscure the red streaks inside the fiber. After impregnation, the fiber is slowly removed and excess dispersion is allowed to drain naturally to avoid localized accumulation of ZnO particles and localized whitening of the fiber caused by violent shaking.

[0040] S4. The intermediate is subjected to gradient temperature drying to obtain zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide chopped fibers.

[0041] The gradient temperature drying process involves pre-drying the intermediate at 50-80℃ for 60 minutes, followed by constant-temperature curing at 80-120℃ for 2 hours. The preferred pre-drying temperature is 60℃, and the preferred constant-temperature curing temperature is 105℃.

[0042] In this application, the intermediate is placed in a drying oven and dried at 50~80℃ for 60 min to slowly evaporate the residual solvent and prevent the powder from rapidly drying and locally agglomerating to form white spots, which would damage the appearance of the blood streaks. Then, the temperature is raised to 80~120℃ and kept constant for 2 h for curing. The heat treatment promotes the full cross-linking of the silane coupling agent and constructs a three-dimensional chemical bonding interface of biomimetic blood streaks polyester / polyamide fiber-silane coupling agent-zinc oxide, converting physically adsorbed ZnO into a chemically bonded grafted structure. The heat treatment temperature is mild throughout the process and will not cause fiber oxidation or decomposition and fading of the red pigment. Finally, the fiber is taken out and naturally cooled to room temperature to obtain zinc oxide chemically grafted antibacterial biomimetic blood streaks short chopped fiber with no change in appearance or original blood streak color.

[0043] This application successfully solves the problems of whitening, fading, and texture obscuring caused by traditional antibacterial modification processes by precisely controlling the etching time with a weak alkali and gentle temperature, achieving uniform loading of a single layer of low-concentration zinc oxide, and the synergistic effect of gradient-controlled segmented drying and curing. This allows the natural red hue and light transmittance of the biomimetic blood-like fibers to be fully preserved. The preparation method of this application is safe and simple, leaves no harmful residues, and has high medical biosafety.

[0044] The zinc oxide-grafted modified antibacterial biomimetic blood-like polyester / polyamide chopped fibers prepared in this application retain the original appearance and color of the biomimetic blood-like fibers, meeting the aesthetic requirements of dental prostheses, while maintaining their original toughening and reinforcing properties and exhibiting excellent toughening effects with PMMA resin. Simultaneously, they possess highly effective antibacterial properties, adapting to the moist environment of oral saliva, with an antibacterial rate of 99.04% against Staphylococcus aureus and 95.61% against Candida albicans. Furthermore, in the zinc oxide-grafted modified antibacterial biomimetic blood-like polyester / polyamide chopped fibers of this application, a silane coupling agent acts as a molecular bridge to achieve chemical bonding and fixation of zinc oxide, resulting in uniform powder dispersion, resistance to saliva erosion and non-detachment, and good stability.

[0045] The zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide chopped fibers prepared in this application can be used as denture base materials, and can also be applied to plush toys, automotive interiors, furniture soft furnishings, cosmetics and other fields.

[0046] The present application will be further described below through specific embodiments.

[0047] Example 1 This embodiment provides a zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester short-cut fiber, the preparation method of which includes: S1. Take short-cut PET fibers with imitation blood-like texture and clean them sequentially with acetone, anhydrous ethanol, and deionized water for 20 minutes each to remove surface dust, oil, and residual textile processing agents. Finally, dry them in an oven at 60°C to constant weight to ensure the fiber surface is clean.

[0048] Prepare a 1wt% NaOH solution, completely immerse the dried fiber, react in a 60℃ water bath for 1 hour, rinse with plenty of deionized water until neutral, and dry at 80℃ to obtain activated fiber.

[0049] S2, using anhydrous ethanol and deionized water (volume ratio 9:1) as dispersion solvent, added KH-550 coupling agent to a volume fraction of 2%, and magnetically stirred at room temperature for 30 min to ensure complete hydrolysis; the activated fiber was immersed in the silane coupling agent modified solution, ultrasonically treated at room temperature for 90 min, removed, washed with ethanol, and dried at 80 ℃ to complete the functionalization modification and obtain the precursor.

[0050] S3. Using an ethanol / water (9:1) mixed solution as the medium, weigh ZnO powder to prepare a dispersion with a concentration of 1.5 g / L. First, stir magnetically for 10 min, then ultrasonically disperse for 30 min to break up agglomerates and obtain a uniform and stable ZnO suspension dispersion. 1g of the precursor was completely immersed in 45mL of ZnO suspension and ultrasonicated at room temperature for 60min to obtain the intermediate.

[0051] S4. Pre-dry the intermediate at 60℃ for 60 minutes; then heat to 105℃ and cure at a constant temperature for 2 hours. After natural cooling, the antibacterial modified finished fiber is obtained, namely zinc oxide grafted modified antibacterial biomimetic blood fiber polyester short chopped fiber.

[0052] Examples 2-7 and Comparative Examples 1-2 were prepared using the above-described method, and the specific process parameters are shown in Tables 1 and 2.

[0053] Table 1. Process parameters for Examples 1-5 Table 1. Process parameters for Examples 6-7 and Comparative Examples 1-2 Figure 1 Fourier transform infrared spectra of the biomimetic blood-like polyester chopped fibers of Examples 1-3 after alkali treatment without grafting modification and the biomimetic blood-like polyester chopped fibers of Comparative Example 2 without alkali treatment and grafting modification. Figure 1 It can be seen that when the alkali treatment time is 2 h, the spectrum is in the range of 3200~3500 cm⁻¹. -1 The intensity of the characteristic peak of hydroxyl stretching vibration within the range reaches its maximum value, indicating that the hydroxylation reaction on the fiber surface is most complete under this process condition, and the content of active hydroxyl groups generated is the highest, which can provide sufficient reaction sites for the subsequent chemical bonding and grafting of zinc oxide particles.

[0054] Figure 2 Physical images of the chopped fibers prepared in Examples 1-7 and Comparative Examples 1-2. From Figure 2 It can be seen that the color of the fiber does not change significantly after alkaline etching and grafting treatment, indicating that the preparation method of this application will not affect the appearance of the biomimetic blood-like polyester / polyamide chopped fiber.

[0055] The antibacterial properties of the fibers prepared in Examples 1-7 and Comparative Examples 1-2 were tested using the following method: GB / T20944.3 Evaluation of antibacterial properties of textiles - Part 3: Oscillation method. The test data are shown in Table 3.

[0056] Table 3. Antimicrobial performance data of fibers in the examples and comparative examples. As can be seen from the data in Table 3, the fibers prepared in Examples 1-7 all showed good antibacterial properties against Staphylococcus aureus and Candida albicans. Among them, Example 2 had the best antibacterial properties, indicating that alkali etching for 2 hours was most conducive to grafting zinc oxide onto the fibers, and the zinc oxide concentration in the prepared fibers was the highest.

[0057] The fibers prepared in Example 2 and Comparative Example 1 were used to prepare denture base materials, respectively, and the specific methods are as follows: 0.02g of fiber was dispersed in 10g of denture powder containing BPO. After thorough mixing, an appropriate amount of denture water was added and stirred until a viscous slurry was formed. The mixture was then poured into a mold and cured under high temperature and pressure to form a denture base sample.

[0058] Figure 3 The images show physical specimens of the denture base composite materials prepared using chopped fibers filled with PMMA in Comparative Example 1 and Example 2, respectively. Visual comparison reveals no significant differences in the overall color, biomimetic blood vessel texture, and light transmittance between the two groups of samples, proving that the zinc oxide grafting modification process in this application does not alter the aesthetic characteristics of the final denture base composite material. This conclusion is consistent with… Figure 2 The results of the appearance observation of the medium fiber body are consistent.

[0059] Although this application has been described in detail in this specification with general descriptions and specific embodiments, some modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, such modifications or improvements made without departing from the spirit of this application are all within the scope of protection claimed in this application.

Claims

1. A method for preparing zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide chopped strand fibers, characterized in that, Includes the following steps: S1, pre-treat biomimetic blood-fiber polyester / polyamide short-cut fibers, and then perform alkaline etching and hydroxylation activation to obtain activated fibers; S2, the activated fibers are pre-modified with silane using a silane coupling agent to obtain a precursor; S3, the precursor is immersed in the grafting solution and grafted onto its surface by ultrasonic impregnation at room temperature to obtain the intermediate; S4. The intermediate is subjected to gradient temperature drying to obtain zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide chopped fibers.

2. The preparation method according to claim 1, characterized in that, The preprocessing specifically includes: The biomimetic blood-like polyester / polyamide short-cut fibers were ultrasonically cleaned in sequence with acetone, anhydrous ethanol and deionized water, and then dried at 80~110℃ to constant weight. The alkaline etching hydroxylation activation specifically involves: The pretreated biomimetic blood-like polyester / polyamide chopped fibers were immersed in an alkaline solution and etched at 60°C for 1-3 hours. They were then washed until neutral and dried at 80-110°C to constant weight to obtain activated fibers.

3. The preparation method according to claim 2, characterized in that, The alkaline solution is a NaOH solution with a concentration of 0.1~10wt%.

4. The preparation method according to claim 2, characterized in that, The mass-to-volume ratio of the pretreated biomimetic blood-like polyester / polyamide short-cut fibers to the alkaline solution was 1g:30~60mL.

5. The preparation method according to claim 1, characterized in that, The silane coupling agent modified solution is prepared by the following method: Add KH-550 coupling agent to a mixed solvent of anhydrous ethanol and deionized water, and stir to allow it to fully hydrolyze, thus obtaining a silane coupling agent modified solution; wherein the volume fraction of KH-550 coupling agent is 0.5-10%; The surface silane pre-modification specifically involves: The activated fibers are immersed in a silane coupling agent modified solution, ultrasonically treated at room temperature for 90-120 minutes, then rinsed with anhydrous ethanol and dried.

6. The preparation method according to claim 1, characterized in that, The grafting solution is prepared by the following method: ZnO is added to a mixed solvent of anhydrous ethanol and deionized water, and dispersed by stirring and ultrasonication to obtain a ZnO suspension dispersion, i.e., graft solution. The solid content of ZnO in the grafting solution is 0.2~1.5 g / L; The volume ratio of anhydrous ethanol to deionized water is 9:

1.

7. The preparation method according to claim 1, characterized in that, The mass-to-volume ratio of the precursor to the grafting solution is 1 g: 30~65 mL.

8. The preparation method according to claim 1, characterized in that, The gradient heating specifically refers to: The intermediate is first pre-dried at 50~80℃ for 60 min, and then heated to 80~120℃ for constant temperature curing for 2 h.

9. Zinc oxide grafted modified antibacterial biomimetic blood-fiber polyester / polyamide short-cut fibers prepared by the preparation method according to any one of claims 1-8.

10. The application of zinc oxide grafted modified antibacterial biomimetic blood-like polyester / polyamide chopped fibers prepared by the preparation method according to any one of claims 1-8 in denture base materials.

Citation Information

Patent Citations

  • Polyester / polyamide chopped fiber with bionic blood streak form as well as preparation method and application of polyester / polyamide chopped fiber

    CN122279785A