An antibacterial and deodorizing oil specifically for polyester FDY and its preparation method

Abstract

This application relates to the field of textile auxiliaries technology, and provides an antibacterial and deodorizing polyester FDY special oiling agent and its preparation method. The antibacterial and deodorizing polyester FDY special oiling agent includes an emulsifier; an antistatic agent; a bundler; an antibacterial composite system; a compatibility stabilizer; and the balance being a smoothing base oil. The antibacterial composite system includes a first antibacterial component and a second antibacterial component. The first antibacterial component includes at least one of benzisothiazolinone and iodopropynyl butylcarbamate; the second antibacterial component includes a quaternized aminosiloxane. This application combines the first and second antibacterial components, and uses a compatibility stabilizer to stably disperse and regulate the compatibility of the antibacterial composite system, enabling the antibacterial component to be stably introduced into the FDY oiling agent system. While ensuring the emulsification stability, oiling uniformity, antistatic properties, and bundler properties of the oiling agent, it imparts good antibacterial properties to the fiber and inhibits the generation of odors caused by microbial growth.

Description

Technical Field

[0001] This invention relates to the technical field of textile auxiliaries, and more specifically, to an antibacterial and deodorizing special oil for polyester FDY and its preparation method. Background Technology

[0002] Polyester FDY (Fully Drawn Yarn) typically requires the application of specialized oils during spinning and winding to impart good smoothness, antistatic properties, and cohesiveness to the filament bundle. This reduces friction between the fiber and equipment, minimizes static electricity buildup, improves the bundle's cohesion, and ensures stable operation of subsequent high-speed spinning, drawing, and winding processes. Therefore, FDY-specific oils are usually formulated from smoothing base oils, emulsifiers, antistatic agents, cohesive agents, and other functional additives to meet the performance requirements of the base oil while also considering emulsification stability, storage stability, and processing adaptability.

[0003] With the development of functional textiles, the market has placed higher demands on the antibacterial properties and odor control capabilities of polyester FDY fibers. In existing technologies, one approach is to impart antibacterial properties to the fibers through padding or coating during the finishing stage. However, this method suffers from increased process steps, higher processing costs, and limited durability. Another approach involves directly introducing antibacterial components into the FDY-specific oiling agent, enabling the fibers to acquire a certain antibacterial effect during the oiling process, while simultaneously inhibiting the generation of odors caused by microbial growth. This method offers advantages such as a shorter process path and ease of integration with existing spinning and oiling processes.

[0004] However, FDY-specific oils are multi-component composite systems, and the components within these systems often differ in polarity, interfacial activity, and solubility and dispersion characteristics. If antibacterial components are further introduced into this system, it is necessary to consider not only the activity of the antibacterial components themselves but also their compatibility and dispersion stability with the base components such as smoothing oil, emulsifiers, antistatic agents, and flocculating agents. In particular, the direct addition of different types of antibacterial components can easily lead to problems such as turbidity, precipitation, stratification, and filtration difficulties due to excessively high local concentrations, interfacial instability, or insufficient compounding. This, in turn, affects the uniformity of the oil's appearance, storage stability, oiling uniformity, and spinning processing stability.

[0005] Therefore, while adding conventional antibacterial agents to FDY-specific oil formulations can impart antibacterial effects to the oil to some extent, the stability of the system is often difficult to maintain during actual compounding, static storage, and subsequent filtration. This problem is not only related to the amount of antibacterial component added, but also closely related to the compatibility, dispersion state, and compounding method between antibacterial components and between antibacterial components and the base components of the oil.

[0006] In view of this, how to achieve the stable introduction of antibacterial components into FDY-specific oil systems without significantly affecting the emulsification stability, oiling uniformity, and spinning processability of FDY oils has become a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0007] This invention aims to provide an antibacterial and deodorizing polyester FDY special oiling agent and its preparation method. By compounding a first antibacterial component with a second antibacterial component and combining a compatibility stabilizer to stabilize and regulate the antibacterial composite system, the antibacterial component can be stably introduced into the FDY oiling agent system. While ensuring the emulsification stability, oiling uniformity, antistatic properties and binding properties of the oiling agent, it imparts good antibacterial properties to the fiber and inhibits the generation of odors caused by microbial growth.

[0008] To address the aforementioned problems, this invention provides an antibacterial and deodorizing polyester FDY special oiling agent, comprising, by weight percentage: 2-20% emulsifier; 0.5-10% antistatic agent; 0.1-8% bridging agent; 0.05-8% antibacterial complex system; 0.1-5% compatibility stabilizer; and the balance being a smoothing base oil; wherein the antibacterial complex system comprises a first antibacterial component and a second antibacterial component; the first antibacterial component comprises at least one of benzisothiazolinone and iodopropynyl butylcarbamate; and the second antibacterial component comprises quaternized aminosiloxane.

[0009] In the above technical solution, the emulsifier includes at least one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, and phosphate salt; and / or the antistatic agent includes at least one of fatty alcohol polyether phosphate salt and alkyl sulfosuccinate salt; and / or the bridging agent includes at least one of isotridecyl alcohol polyoxyethylene ether and polyethylene glycol fatty acid ester; and / or the compatibility stabilizer includes at least one of polyether modified siloxane and EO / PO block polyether; and / or the smoothing base oil includes at least one of fatty acid ester, diester, polyol ester, polyether, polyether ester, and siloxane modified ester.

[0010] In the above technical solution, the mass ratio of the first antibacterial component to the second antibacterial component is 1:(0.3~4).

[0011] In the above technical solution, the polyester FDY special oil also includes 0.01~2% of additives by weight percentage, including at least one of defoamer, antioxidant, and corrosion inhibitor.

[0012] This invention also provides a method for preparing an antibacterial and deodorizing polyester FDY special oil, the method being used to prepare any of the above-mentioned polyester FDY special oils, comprising the following steps: S100. Add the smoothing base oil to the reactor for dehydration treatment to obtain dehydrated base oil; S200: Add emulsifier, antistatic agent, clustering agent and 40-80% compatibility stabilizer to dehydrated base oil, and mix to obtain base oil phase; S300: The first antibacterial component, the second antibacterial component and the remaining compatibility stabilizer are compounded to obtain the antibacterial mother liquor; S400: Add the antibacterial mother liquor to the base oil phase and mix evenly. After degassing and filtration, a special oil agent for polyester FDY is obtained.

[0013] In the above technical solution, in S100, the dehydration treatment temperature is 50~95℃, the vacuum degree is -0.06~-0.095MPa, and the time is 20~120min.

[0014] In the above technical solution, in S200, the mixing temperature is 40~80℃ and the time is 20~90min.

[0015] In the above technical solution, in S300, the temperature of the compounding treatment is 25~70℃ and the time is 10~60min.

[0016] In the above technical solution, in S400, the antibacterial mother liquor accounts for 1~12% of the total mass of the base oil phase; and / or the filtration treatment is staged filtration, using 5~10μm filtration and 1~3μm filtration in sequence.

[0017] In the above technical solution, after the antibacterial mother liquor is added to S400, it is aged at 40~70℃ for 20~90 minutes.

[0018] Beneficial effects This invention provides an antibacterial and deodorizing oiling agent specifically for polyester FDY and its preparation method. By constructing an antibacterial composite system consisting of a first antibacterial component and a second antibacterial component, and combining it with a compatibility stabilizer and its preparation method, the antibacterial component can be stably introduced into the FDY oiling agent system. Compared with the prior art, this invention is beneficial to improving the overall performance of the oiling agent system after the stable introduction of the antibacterial component, and exhibits better antibacterial and deodorizing effects on the yarn sample after oiling. Detailed Implementation

[0019] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, a detailed description of specific embodiments of the present invention will be provided below.

[0020] Unless otherwise specified, all reagents and raw materials used in this invention are commercially available. Experimental methods in the following examples that do not specify particular conditions should be performed according to conventional methods and conditions, or as selected in the product instructions.

[0021] In existing polyester FDY oiling agents, adding conventional preservatives and antibacterial agents alone often only inhibits microbial contamination during storage, failing to establish a sustained and effective antibacterial effect on the fiber surface. Conversely, adding antibacterial components with surface adhesion capabilities can easily lead to compatibility conflicts with emulsifiers, antistatic agents, and bridging agents in the oiling agent, affecting system stability, transparency, and oiling uniformity. Therefore, the challenge lies in achieving a synergistic effect of both oiling agent-based antibacterial activity and sustained antibacterial and deodorizing properties on the fiber surface, while ensuring both system stability and spinning suitability.

[0022] This invention provides an antibacterial and deodorizing polyester FDY oil and its preparation method, which solves the problems in existing technologies such as the difficulty in stably introducing antibacterial components into the FDY oil system, the easy occurrence of precipitation and stratification, decreased filtration permeability, and fluctuations in spinning processing performance, enabling the oiled FDY fibers to achieve better antibacterial and deodorizing effects. The polyester FDY oil of this invention, by weight percentage, comprises: emulsifier, antistatic agent, bridging agent, antibacterial composite system, compatibility stabilizer, and the balance being a smoothing base oil.

[0023] Specifically, the emulsifier, antistatic agent, bundler, compatibility stabilizer, and smoothing base oil of this invention take into account the base oiling performance, system compatibility stability, and spinning processing stability. The emulsifier improves the interfacial wettability and dispersion stability of the oiling system; the antistatic agent reduces static electricity buildup during fiber processing; the bundler regulates the fiber bundle cohesion and improves operational stability; the compatibility stabilizer mitigates interfacial differences between different functional components and improves system homogeneity, storage stability, and filtration permeability; and the smoothing base oil serves as a base carrier, providing lubricity, film-forming properties, and thermal stability. These components are not isolated but work synergistically in the special high-temperature, high-shear, low-addition, continuous oiling system of FDY oiling to balance antibacterial properties, system compatibility stability, and spinning processability.

[0024] Furthermore, controlling the emulsifier content at 2-20% helps ensure the interfacial wetting and dispersion stability of the base oil phase and functional components. When the emulsifier content is too low, the system's emulsification and dispersion capabilities are insufficient, easily leading to poor oil uniformity, uneven distribution of antibacterial components, and fluctuations in oiling. When the emulsifier content is too high, it may cause excessive surface activity in the system, affecting the stability of the oil film structure. Controlling the antistatic agent content at 0.5-10% helps reduce static electricity accumulation during fiber processing and maintain stable fiber bundle operation. When its content is too low, the antistatic effect is insufficient, making it difficult to meet the static control requirements during high-speed spinning. When its content is too high, it may interfere with the system's interfacial state and oil film continuity, thereby affecting the uniformity of oiling and the fiber bundle cohesion. The concentration of the bundle binder is controlled at 0.1-8%, which helps regulate the cohesion of the filament bundles and improve operational stability. If its content is too low, the bundle binder will be insufficient, leading to filament separation, fuzzing, or unstable operation. If its content is too high, it may cause the filament bundles to become too sticky, have excessive cohesion, or exhibit abnormal friction, thus affecting winding and subsequent processing. The concentration of the compatibility stabilizer is controlled at 0.1-5%, which helps mitigate the interfacial differences between the antibacterial composite system and the base oil phase and improves system homogeneity, storage stability, and filtration permeability. If its content is too low, the compatibility adjustment effect is insufficient, making it difficult to effectively inhibit local aggregation and microphase separation. If its content is too high, it may cause excessive changes in system viscosity, interfacial state, or oil film characteristics, which is detrimental to maintaining the overall processing performance of the FDY oil. The balance is set as a smoothing base oil, which helps to provide the necessary lubricity, film-forming properties, and thermal stability to the oil system while satisfying the synergistic effects of the above functional components, thereby ensuring the performance of the base oil during FDY spinning.

[0025] It is worth noting that FDY high-speed spinning oiling systems are typically used under conditions of high temperature, high shear, low addition, and continuous oiling. The introduction of antibacterial components requires consideration not only of the antibacterial activity itself, but also of thermal stability, volatility migration tendency, oil film stability, compatibility and dispersion, filtration permeability, and tow friction and bundle properties. When small molecule antibacterial agents are used alone, although they have a relatively fast immediate antibacterial ability, they are prone to problems such as volatility migration, decreased thermal stability, or deterioration of oil film stability. When quaternized aminosiloxanes are used alone, although they have good surface adhesion and a certain degree of persistence, they are still insufficient in terms of immediate antibacterial speed, broad-spectrum coverage, and inhibition of odor sources. When the two are directly mixed, problems such as insufficient compatibility, precipitation, decreased filtration permeability, poor oiling uniformity, tow bundle aggregation, and fluctuations in friction properties may occur due to differences in structure and interfacial behavior.

[0026] In view of this, the antibacterial composite system of the present invention includes a first antibacterial component and a second antibacterial component, which takes into account immediate antibacterial effect, surface adhesion and long-lasting effect, system compatibility and stability and spinning processability, thereby achieving a comprehensive balance of antibacterial properties, compatibility and processability in the special application scenarios of FDY oil.

[0027] Preferably, the first antibacterial component includes at least one of benzisothiazolinone and iodopropynyl butylcarbamate. This type of component provides strong immediate antibacterial activity even at low addition levels and can rapidly inhibit microorganisms such as bacteria and molds that cause oil contamination and odor, thus facilitating the establishment of a basic antibacterial barrier in the early stages of oiling the fiber. Specifically, benzisothiazolinone has good broad-spectrum antibacterial properties and can inhibit microbial contamination that may be introduced during oil storage and use; iodopropynyl butylcarbamate has good inhibitory ability against molds and other microorganisms, helping to reduce the risk of odor and system instability caused by microbial growth. Therefore, using it as the first antibacterial component is beneficial for providing a rapid-acting antibacterial effect at low addition levels.

[0028] Preferably, the second antibacterial component includes quaternized aminosiloxane. This type of component possesses both the surface antibacterial ability of quaternary ammonium groups and the interfacial spreading, flexible film-forming, and adhesion-retention capabilities of siloxane segments. It can easily spread onto the fiber surface with the oiling agent and form a functional layer with a certain degree of adhesion, thereby enhancing the retention and persistence of the antibacterial component on the fiber surface. Specifically, the quaternary ammonium groups can interact with the surface of microbial cells through positively charged active centers, inhibiting microorganisms; the siloxane segments endow this type of component with low surface tension and good surface spreading ability, making it easier to distribute onto the fiber surface with the oil film and reducing interfacial disturbances caused by the introduction of purely polar bactericidal components. Therefore, using quaternized aminosiloxane as the second antibacterial component helps improve the adhesion and persistence of the antibacterial system on the fiber surface, and to a certain extent, balances oil film smoothness and fiber surface condition regulation.

[0029] Furthermore, the first antimicrobial component focuses on providing a faster antimicrobial response at a lower addition level, reducing the level of microbial growth on the oil and fiber surfaces; the second antimicrobial component focuses on enhancing the adhesion and sustained effect of the antimicrobial function on the fiber surface; and the compatibility stabilizer is used to mitigate the interfacial differences between the above two types of antimicrobial components and the base oil phase, reducing the local aggregation, precipitation, filtration difficulties and oiling fluctuations that may occur when used directly.

[0030] Furthermore, the mass ratio of the first antibacterial component to the second antibacterial component is 1:(0.3~4). Within this range, the rapid antibacterial response provided by the first antibacterial component and the fiber surface adhesion retention provided by the second antibacterial component can form a good synergy, which is beneficial for achieving the effects of antibacterial activity in the oil itself, sustained antibacterial activity on the fiber surface, and inhibition of odor caused by microorganisms. At the same time, this ratio range is also beneficial for controlling the interfacial distribution and compatibility dispersion of the two types of antibacterial components in the oil system, reducing the risk of interfacial disturbance, precipitation stratification, decreased filtration permeability, and fluctuations in oiling uniformity caused by an excessively high proportion of the second antibacterial component. It can also avoid the problem of insufficient adhesion retention on the fiber surface when the proportion of the second antibacterial component is too low. Specifically, when the proportion of the second antibacterial component is too low, its spreading, adhesion and retention on the fiber surface are insufficient, making it difficult to fully exert the synergistic effect of antibacterial persistence on the fiber surface and odor source inhibition; when the proportion of the second antibacterial component is too high, it is easy to enhance its influence on the interface state and oil film structure of the oil system, thereby increasing the possibility of compatibility imbalance with emulsifiers, antistatic agents, bundlers and base oil phases, resulting in decreased system transparency, poor dispersion stability, decreased filtration permeability, and even fluctuations in oiling uniformity, fiber bundle aggregation and friction performance.

[0031] As will be known to those skilled in the art, the polyester FDY special oiling agent of the present invention may also contain 0.01 to 2% of additives as needed. The additives include at least one of defoamers, antioxidants, and corrosion inhibitors, and are not specifically limited herein.

[0032] In specific operation, the preparation method of the polyester FDY special oil agent of the present invention includes the following steps: S100. Add the smoothing base oil to the reactor for dehydration treatment to obtain dehydrated base oil; S200: Add the emulsifier, the antistatic agent, the clustering agent and 40-80% of the compatibility stabilizer to the dehydrated base oil, and mix to obtain the base oil phase; S300: The first antibacterial component, the second antibacterial component and the remaining compatibility stabilizer are compounded to obtain the antibacterial mother liquor; S400: Add the antibacterial mother liquor to the base oil phase and mix evenly. After degassing and filtration, a special oil agent for polyester FDY is obtained.

[0033] In S100, the smoothing base oil is dehydrated to reduce the residual water in the base oil phase, thereby reducing the interference of water on the subsequent compounding process of emulsifiers, antistatic agents, clustering agents, compatibility stabilizers and antibacterial complexes, thus improving the homogeneity of the base oil phase and the compatibility and dispersion stability of the subsequent antibacterial complexes.

[0034] Preferably, the water content of the dehydrated base oil is not higher than 0.3 wt%. When the water content is too high, it is easy to change the local polarity and interface state of the system, increasing the risk of local aggregation, turbidity, precipitation and stratification, decreased filtration permeability and fluctuations in oiling uniformity. Controlling it within the above range is beneficial to balance system stability and process economy.

[0035] Furthermore, controlling the dehydration treatment temperature at 50~95℃, the vacuum degree at -0.06~-0.095MPa, and the time at 20~120min helps to ensure dehydration efficiency while avoiding performance fluctuations in the base oil phase due to excessive heat load or harsh operating conditions, thus balancing dehydration effect, base oil stability, and industrial operability.

[0036] In S200, emulsifiers, antistatic agents, clustering agents, and 40-80% compatibility stabilizers are added to the dehydrated base oil for mixing. This is to first construct a base oil phase with a relatively homogeneous composition and a relatively stable interfacial state, providing a suitable dispersion medium and interfacial environment for the subsequent introduction of the antibacterial mother liquor. By pre-adding emulsifiers, antistatic agents, clustering agents, and some compatibility stabilizers, a synergistic system of lubrication, emulsification, antistatic, and clustering that meets the performance requirements of the base oil in FDY oil formulations can be formed. Furthermore, the interfacial relationship between each component and the smoothing base oil is pre-adjusted with the help of compatibility stabilizers, thereby reducing the risk of local aggregation, precipitation, stratification, decreased filtration permeability, and oiling fluctuations when the antibacterial mother liquor is added subsequently.

[0037] Preferably, 40-80% of the total amount of compatibility stabilizer is added to S200 first. If this proportion is too low, the interfacial conditioning effect on the base oil phase will be insufficient, which is not conducive to the stable introduction of the subsequent antibacterial mother liquor; if this proportion is too high, it will result in insufficient compatibility stabilizer in S300 for the pre-combination of the first and second antibacterial components, which is not conducive to the dispersion and stability of the antibacterial mother liquor itself. Therefore, the above proportion setting is beneficial to balance the pre-stabilization of the base oil phase and the pre-dispersion of the antibacterial mother liquor.

[0038] Furthermore, the mixing temperature of S200 is preferably 40~80℃. This temperature range is beneficial for reducing the viscosity of the system, promoting the diffusion and uniform dispersion of each component, while avoiding excessive heat load on the surface active components and functional additives due to excessive temperature. The mixing time is preferably 20~90min. This time range is beneficial for the components to be fully mixed and form a relatively stable base oil phase, while taking into account both process economy and system stability.

[0039] Those skilled in the art will understand that, in specific implementations, steps S200 and S300 can be performed sequentially or in parallel, depending on the production organization requirements. Preferably, step S200 is used to prepare the base oil phase, and step S300 is used to prepare the antibacterial mother liquor. These steps can be performed separately in different containers, and after each reaches a predetermined homogeneous and stable state, the antibacterial mother liquor is added to the base oil phase in step S400 for mixing. Using a parallel implementation method is beneficial for shortening the production cycle and improving preparation efficiency; however, regardless of whether sequential or parallel implementation is used, it is preferable to first complete the construction of the base oil phase and the antibacterial mother liquor separately before subsequent merging, to ensure the stable introduction of the antibacterial composite system into the base oil phase.

[0040] In S300, the first antibacterial component, the second antibacterial component, and the remaining compatibility stabilizer are compounded to obtain an antibacterial mother liquor. This is mainly to pre-disperse, pre-compatibly compatible, and buffer the interface of the antibacterial composite system, thereby reducing the risk of excessively high local concentrations, uneven dispersion, and interfacial instability when it is directly added to the base oil phase. Because the first and second antibacterial components differ in molecular structure, polarity, and interfacial behavior, if they are directly added to the base oil phase, local high-concentration areas can easily form at the moment of addition, leading to problems such as local aggregation, turbidity, precipitation, decreased filtration permeability, and fluctuations in oil loading uniformity. By first compounding them with the remaining compatibility stabilizer to form an antibacterial mother liquor, the two types of antibacterial components are in a relatively stable and uniform pre-dispersed state before entering the base oil phase, thereby improving their compatibility and dispersion stability when subsequently added to the base oil phase.

[0041] Preferably, the compounding temperature of S300 is 25~70℃. This temperature range is beneficial to improving the diffusion efficiency and compounding uniformity of each component, while avoiding the adverse effects of excessively high temperature on the stability of the antibacterial component. The compounding time is 10~60min. This time range is beneficial to allow each component to fully contact and form a relatively stable antibacterial mother liquor, while taking into account both process efficiency and system stability.

[0042] Furthermore, the mother liquor method introduces the antibacterial composite system into the polyester FDY-specific oiling agent through a process of first ensuring compatibility and then incorporating it, thereby reducing the interfacial impact on the entire FDY oiling agent system caused by direct feeding. Compared with direct feeding, this method helps reduce the risk of interfacial impact and compatibility imbalance caused by localized high-concentration feeding, reduces local aggregation, turbidity, precipitation, stratification, and decreased filtration permeability, and also helps improve the storage stability and oiling uniformity of the finished oiling agent.

[0043] In S400, the antibacterial mother liquor is added to the base oil phase and mixed evenly. After aging, degassing and filtration, the antibacterial complex system is smoothly integrated into the base oil phase. This further facilitates the diffusion, distribution and interface reorganization of each functional component in the entire oil system, thereby improving the uniformity, storage stability, filtration permeability and oiling stability of the finished oil.

[0044] Preferably, the antibacterial mother liquor accounts for 1-12% of the total mass of the base oil phase. Within this range, it is beneficial to ensure the effective introduction of the first and second antibacterial components into the finished oil agent, and also to control the local concentration changes and interfacial disturbances when the antibacterial mother liquor merges into the base oil phase, thus balancing the antibacterial effect, system compatibility stability, and spinning processing stability. Furthermore, by using dropwise, slow, or metered addition methods over a period of 10-60 minutes, and maintaining the system temperature at 25-60°C during the addition process, it is beneficial to control the instantaneous concentration changes and interfacial impacts when the antibacterial mother liquor enters the base oil phase, avoiding localized high-concentration areas caused by rapid one-time addition. This reduces the risk of local aggregation, turbidity, precipitation, stratification, and uneven dispersion, thereby improving merging efficiency and component stability.

[0045] Furthermore, after the antibacterial mother liquor is added, it is aged at 40-70℃ for 20-90 minutes. This aging process facilitates further diffusion and interfacial equilibrium of the components, reduces the tendency for residual local aggregation and interfacial instability, thereby improving the system's homogeneity, compatibility stability, and filtration stability.

[0046] Furthermore, performing vacuum degassing or inert gas treatment before or during filtration helps remove entrained bubbles and some dissolved gases from the system, reducing the interference of gases on appearance uniformity, filtration stability and oiling continuity, and minimizing the adverse effects of oxygen on the stability of functional components.

[0047] In an optional embodiment, the filtration process employs staged filtration, sequentially performing 5-10 μm filtration and 1-3 μm filtration. The first stage of filtration is mainly used to remove larger particles and local aggregates, while the second stage is mainly used to further remove fine particles and tiny insoluble matter. Compared with single-stage fine filtration, the above-mentioned staged filtration method helps reduce the risk of clogging of the fine filtration media, improves the overall filtration throughput and the cleanliness of the finished oil, and reduces the risk of clogging in the subsequent oiling system and fluctuations in the spinning process. Example 1

[0048] This embodiment provides an antibacterial and deodorizing polyester FDY special oil and its preparation method. By weight percentage, it comprises: 9724g of pentaerythritol tetra(2-ethylhexanoic acid) ester as a smoothing base oil, 200g of fatty alcohol polyoxyethylene ether as an emulsifier, 50g of fatty alcohol polyether phosphate salt as an antistatic agent, 10g of isotretinoin polyoxyethylene ether as a bridging agent, 3.85g of benzisothiazolinone as a first antibacterial component, 1.15g of quaternized aminosiloxane as a second antibacterial component, 10g of polyether-modified siloxane as a compatibility stabilizer, and 1g of defoamer. The preparation method includes the following steps: S100. Add smooth base oil to the reactor and dehydrate it for 20 minutes at 50°C and a vacuum of -0.06MPa to obtain dehydrated base oil with a water content of no more than 0.3wt%. S200, add emulsifier, antistatic agent, clustering agent, defoamer and 4g compatibility stabilizer to dehydrated base oil, control the temperature inside the reactor to 40℃, stir for 20min to obtain base oil phase; S300. Add the first antibacterial component, the second antibacterial component and the remaining 6g of compatibility stabilizer to another container, stir and mix at 25°C for 10 minutes to obtain the antibacterial mother liquor. S400. The antibacterial mother liquor is added to the base oil phase by dropwise over a period of 10 minutes, while maintaining the system temperature at 25°C during the addition process. After the addition is complete, the mixture is aged at 40°C for 20 minutes. Subsequently, vacuum degassing is performed, followed by 5μm filtration and 1μm filtration to obtain the antibacterial and deodorizing polyester FDY special oil agent. Example 2

[0049] This embodiment provides an antibacterial and deodorizing polyester FDY special oil and its preparation method. By weight percentage, it comprises: 8350g of smoothing base oil (di(2-ethylhexyl) sebate), 500g of fatty alcohol polyoxyethylene ether and 300g of fatty acid polyoxyethylene ester as emulsifiers, 300g of fatty alcohol polyether phosphate salt as antistatic agent, 150g of polyethylene glycol fatty acid ester as a bridging agent, 60g of benzisothiazolinone and 40g of iodopropynyl butylcarbamate as a first antibacterial component, 100g of quaternized aminosiloxane as a second antibacterial component, 80g of polyether-modified siloxane and 70g of EO / PO block polyether as compatibility stabilizers, 10g of defoamer, 20g of antioxidant, and 20g of corrosion inhibitor. The preparation method includes the following steps: S100. Add smooth base oil to the reactor and dehydrate it for 60 min at 70℃ and a vacuum of -0.08MPa to obtain dehydrated base oil with a water content of no more than 0.3wt%. S200, add emulsifier, antistatic agent, clustering agent, defoamer, antioxidant, corrosion inhibitor and 90g compatibility stabilizer to dehydrated base oil, control the temperature inside the reactor at 60℃, stir for 45min to obtain base oil phase; S300. Add the first antibacterial component, the second antibacterial component and the remaining 60g of compatibility stabilizer to another container, stir and mix at 45℃ for 30min to obtain the antibacterial mother liquor. S400. The antibacterial mother liquor is added to the base oil phase by metering over a period of 30 minutes, while maintaining the system temperature at 45°C during the addition process. After the addition is complete, the mixture is aged at 55°C for 40 minutes. Subsequently, vacuum degassing is performed, followed by 7μm filtration and 2μm filtration to obtain the antibacterial and deodorizing polyester FDY special oil agent. Example 3

[0050] This embodiment provides an antibacterial and deodorizing polyester FDY special oil and its preparation method. By weight percentage, it comprises: 4700g of pentaerythritol tetra(2-ethylhexanoic acid) ester as a smoothing base oil; 1200g of fatty alcohol polyoxyethylene ether and 800g of fatty acid polyoxyethylene ester as emulsifiers; 1000g of fatty alcohol polyether phosphate salt as an antistatic agent; 800g of polyethylene glycol fatty acid ester as a bridging agent; 60g of benzisothiazolinone and 100g of iodopropynyl butylcarbamate as a first antibacterial component; 640g of quaternized aminosiloxane as a second antibacterial component; 500g of polyether-modified siloxane as a compatibility stabilizer; 50g of defoamer; 90g of antioxidant; and 60g of corrosion inhibitor. The preparation method includes the following steps: S100. Add smooth base oil to the reactor and dehydrate it for 120 min at 95℃ and a vacuum of -0.095MPa to obtain dehydrated base oil with a moisture content of no more than 0.3wt%. S200, add emulsifier, antistatic agent, clustering agent, defoamer, antioxidant, corrosion inhibitor and 400g compatibility stabilizer to the dehydrated base oil, control the temperature inside the reactor to 80℃, stir for 90min to obtain the base oil phase; S300. Add the first antibacterial component, the second antibacterial component and the remaining 100g of compatibility stabilizer to another container, stir and mix at 70℃ for 60min to obtain the antibacterial mother liquor. S400. The antibacterial mother liquor is slowly added to the base oil phase over a period of 60 minutes, while maintaining the system temperature at 60°C during the addition process. After the addition is complete, the mixture is aged at 70°C for 90 minutes. Subsequently, vacuum degassing is performed, followed by 10μm filtration and 3μm filtration to obtain the antibacterial and deodorizing polyester FDY special oil agent. Example 4

[0051] This embodiment provides an antibacterial and deodorizing polyester FDY special oil agent and its preparation method. The formula is as shown in Example 3, but the steps are different from those in Example 3: In S100, dehydration was carried out at 85°C and a vacuum of -0.09 MPa for 90 min to obtain dehydrated base oil; In S200, add 200g of compatibility stabilizer, keep the other materials unchanged, control the temperature inside the reactor at 70℃, stir for 60min, and obtain the base oil phase; Add the remaining 300g of compatibility stabilizer to S300, keeping the other materials unchanged, and stir at 60℃ for 40min to obtain antibacterial mother liquor; In S400, 1100g of antibacterial mother liquor was metered and added to the base oil phase at 50°C over 40 minutes; after addition, it was aged at 60°C for 60 minutes.

[0052] Comparative Example 1 This comparative example provides an antibacterial and deodorizing polyester FDY special oil agent and its preparation method. The formula and preparation method are as shown in Example 2. The difference is that there is no second antibacterial component, that is, the first antibacterial component is 120g of benzisothiazolinone and 80g of iodopropynyl butylcarbamate.

[0053] Comparative Example 2 This comparative example provides an antibacterial and deodorizing polyester FDY special oil agent and its preparation method. The formula and preparation method are as shown in Example 2. The difference is that there is no first antibacterial component, that is, the second antibacterial component is 200g of quaternized aminosiloxane.

[0054] Comparative Example 3 This comparative example provides an antibacterial and deodorizing special oil agent for polyester FDY and its preparation method. The formulation and preparation method are as shown in Example 2, except that: In S200, 150g of compatibility stabilizer is added to the dehydrated base oil in one go, and mixed with emulsifier, antistatic agent, cleaving agent and additives to obtain the base oil phase; No S300; In S400, 100g of the first antibacterial component and 100g of the second antibacterial component are directly added to the base oil phase and mixed, and then degassed and filtered to obtain the finished oil product.

[0055] Comparative Example 4 This comparative example provides an antibacterial and deodorizing polyester FDY special oil agent and its preparation method. The formula and preparation method are as shown in Example 2, except that: there is no compatibility stabilizer and the smoothing base oil is adjusted to 8500g.

[0056] Comparative Example 5 This comparative example provides an antibacterial and deodorizing polyester FDY special oil agent and its preparation method. The formula and preparation method are as shown in Example 2, except that the mass ratio of the first antibacterial component to the second antibacterial component is adjusted to 1:6, that is, the first antibacterial component is 17.14g of benzisothiazolinone and 11.43g of iodopropynyl butylcarbamate; the second antibacterial component is 171.43g of quaternized aminosiloxane.

[0057] Comparative Example 6 This comparative example provides an antibacterial and deodorizing polyester FDY special oil agent and its preparation method. The formulation and preparation method are as shown in Example 2. The difference is that in S400, after the antibacterial mother liquor is added to the base oil phase and mixed evenly, no aging treatment is performed; at the same time, no graded filtration is used, only 1μm single-stage filtration is used.

[0058] Performance testing Initial antibacterial rate test: The oils obtained in Examples 1-4 and Comparative Examples 1-6 were used to apply the oils evenly to the surface of polyester FDY raw yarns of the same specification using an oiling device. The oiling rate was controlled at 0.80±0.05wt%, and the yarns were placed at 25℃ for 24 hours before use. 0.75g of the oiled FDY yarn samples were then inoculated with Staphylococcus aureus and Escherichia coli suspensions to achieve an initial bacterial inoculation of 1×10⁻⁶ on the sample surface. 5 ~1×10 6 CFU / sample was incubated at 37℃ for 24 h, and the number of surviving bacteria was determined by elution counting method; Antibacterial retention rate test after placement: Each oil sample was sealed and placed at 25±2℃ for 90 days. After placement, the antibacterial rate was determined according to the same oiling method and antibacterial test method as described above. Antibacterial retention rate test after heat treatment: FDY filaments after oiling were placed in a heat treatment device and treated at 180°C for 2 minutes. After cooling to room temperature, the antibacterial rate after heat treatment was determined according to the above antibacterial rate test method.

[0059] Table 1 As shown in Table 1, Examples 1-4 all exhibited good antibacterial properties, indicating that the combination of the first and second antibacterial components, along with the stepwise introduction of a compatibility stabilizer into the FDY oil system, effectively imparted high initial antibacterial activity to the silk samples. Overall, Examples 3 and 2 showed the highest initial average antibacterial rates, followed by Example 4. Although Example 1 had a slightly lower rate due to the lower addition of the antibacterial composite system, it was still significantly better than the comparative examples, indicating that the present invention still has a good basic antibacterial effect even at lower addition levels. In contrast, Comparative Examples 1 and 2 showed a significant decrease in antibacterial retention due to the lack of the second or first antibacterial component, respectively, indicating that a single antibacterial component is difficult to simultaneously achieve both immediate antibacterial action and sustained adhesion. Comparative Examples 3, 4, and 6, lacking steps such as mother liquor method, compatibility stabilizer, or aging and graded filtration, showed a further decrease in antibacterial retention rates after standing and heat treatment, indicating that the complete process significantly promotes the maintenance of antibacterial performance.

[0060] Oil storage stability test: Take 100 mL of each oil sample and place it in a transparent, stoppered glass bottle. Store it at 25±2℃. Observe its appearance changes at 30 days and 90 days, and record whether layering, turbidity, precipitation, and sedimentation occur. At the same time, take samples after preparation and 90 days later, and use a laser particle size analyzer to measure its average particle size. (Appearance evaluation criteria are as follows: Excellent: The sample is uniform and transparent, with no layering, turbidity, or precipitation; Good: The sample is basically uniform, slightly turbid, but with no obvious layering or precipitation; Medium: The sample is turbid or has a small amount of precipitation; Poor: The sample has obvious layering, precipitation, or sedimentation.) Filtration passability test: Take 500g of each oil sample and conduct filtration test using a laboratory pressure filtration device at 25℃; Table 2 Table 2 shows that Examples 1-4 all exhibited good appearance stability and low particle size growth during storage. Examples 2 and 3 showed the most uniform appearance, maintaining an excellent grade after 90 days, and exhibited the smallest change in average particle size, indicating that the antibacterial composite system was more stable in the oil-based system. Regarding filtration performance, Examples 1-4 all had shorter filtration times and lower filter membrane residue, indicating that the stepwise addition of the compatibility stabilizer, pre-compounding of the antibacterial mother liquor, maturation, and staged filtration helped reduce local aggregates and insoluble matter, improving filtration stability. In contrast, Comparative Example 3, with direct feeding, easily generated localized high concentrations and interfacial impacts, leading to a significant increase in particle size and a prolonged filtration time. Comparative Example 4, without the addition of a compatibility stabilizer, had the worst appearance stability and filtration performance. Although Comparative Example 6 contained complete components, due to the lack of maturation and the use of only single-stage filtration, its particle size growth and filter membrane residue were significantly higher than those of the Examples.

[0061] Oiling process: After applying each oil sample to FDY yarn of the same specification, the yarn was equilibrated for 24 hours under standard temperature and humidity conditions. The dynamic friction coefficient between the yarn bundle and the metal guide was measured using a yarn friction coefficient tester. Bundle performance test: Under the same tension, same filament speed and same guide path conditions, observe the filament bundle operation status, and characterize the bundle performance by the filament bundle diffusion width and bundle level (the bundle level is evaluated from 1 to 5, and the higher the value, the better the bundle performance). Breakage rate test: Under the same spinning and winding conditions, run continuously for 8 hours and record the number of breakages during the operation; Fiber rate test: The number of fibrous hairs in a unit length of silk sample is counted using a fibrous hair detector and converted into fibrous hair rate, with the unit being hairs / 100,000m.

[0062] Table 3 As shown in Table 3, Examples 1-4 exhibited good overall processing performance in terms of dynamic friction coefficient, filament diffusion width, bundle grade, breakage rate, fuzz rate, and oiling uniformity CV value. This indicates that while introducing antibacterial and deodorizing functions, the present invention can still maintain the lubricity, bundle properties, and oiling stability required by FDY oil. Overall, Examples 2 and 3 performed best, followed by Example 4. Although Example 1's performance was slightly inferior due to the lower addition amount of each component, it was still better than all comparative examples. Comparative Examples 1 and 2, lacking a type of antibacterial component, retained some basic performance, but were inferior to the complete examples in terms of friction, bundle properties, and breakage control. In Comparative Example 5, the ratio of the first antibacterial component to the second antibacterial component exceeded the preferred range, which adversely affected the interface state and oil film structure, resulting in a decrease in processing performance. Comparative Examples 3 and 4, lacking a mother liquor method or compatibility stabilizer, were most prone to oiling fluctuations, local aggregation, and interface unevenness, resulting in significantly worse breakage rate, fuzz rate, and oiling uniformity CV value.

[0063] Odor suppression and deodorization test: FDY filaments after oiling were collected, artificial sweat was added, and a mixed bacterial solution was inoculated. After 48 hours of sealed incubation at 37°C, odor was evaluated. Evaluation involved both scoring the odor level by evaluators and detecting the ammonia and isovaleric acid content in the headspace gas. (Odor levels range from 0 to 5: 0 indicates no odor, and 5 indicates a very noticeable odor). Table 4 As shown in Table 4, Examples 1-4 all exhibit good odor suppression capabilities. Examples 3 and 2 show the lowest odor levels, lowest ammonia and isovaleric acid concentrations, and highest odor suppression rates, indicating that under optimal antibacterial composite system and compatibility-stabilized system conditions, the present invention can more effectively inhibit microbial reproduction and the production of their metabolites. Although Example 4 is slightly lower than Examples 2 and 3, it still maintains a high odor suppression rate. Example 1 also shows significantly better deodorizing effects than the comparative examples under low addition conditions, indicating that the present invention still has a certain odor control capability even near the lower limit of the formulation. In contrast, Comparative Examples 1 and 2, due to incomplete antibacterial systems, cannot simultaneously achieve rapid antibacterial action and sustained antibacterial action on the fiber surface, resulting in limited deodorizing effects. Comparative Examples 3 and 4, lacking a mother liquor method or compatibility stabilizer, suffer from poor dispersion of antibacterial components, further reducing their deodorizing effect. Although Comparative Examples 5 and 6 are better than Comparative Examples 3 and 4, they are still inferior to the examples of the present invention.

[0064] In summary, this invention constructs an antibacterial composite system consisting of a first antibacterial component and a second antibacterial component, and combines this with preparation methods such as stepwise addition of compatibility stabilizers, pre-compounding of antibacterial mother liquor, maturation, and graded filtration, enabling the antibacterial components to be stably introduced into the FDY oiling system. This not only improves the antibacterial and deodorizing effects on the oil and fiber surface, but also reduces problems such as turbidity, precipitation, stratification, and decreased filtration permeability caused by insufficient system compatibility, while maintaining good oiling uniformity, frictional properties, bundling properties, and spinning processing stability, thereby achieving a balance between antibacterial performance, storage stability, and FDY processability. Any person skilled in the art can make various modifications and alterations without departing from the spirit and scope of this invention; therefore, the scope of protection of this invention should be determined by the scope defined in the claims.

Claims

1. A special oiling agent for antibacterial and deodorizing polyester FDY, characterized in that, By weight percentage, including: Emulsifier 2~20%; Antistatic agent 0.5~10%; Clustering agent 0.1-8%; Antibacterial complex system 0.05~8%; Compatibility stabilizer 0.1-5%; The remainder is a smoothing base oil; The antibacterial complex system includes a first antibacterial component and a second antibacterial component. The first antibacterial component includes at least one of benzisothiazolinone and iodopropynyl butylcarbamate; The second antibacterial component includes quaternized aminosiloxane.

2. The special oiling agent for polyester FDY according to claim 1, characterized in that, The emulsifier includes at least one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, and phosphate salt; and / or The antistatic agent includes at least one of fatty alcohol polyether phosphate salt and alkyl sulfonyl succinate salt; and / or The slugging agent includes at least one of isotridecyl polyoxyethylene ether and polyethylene glycol fatty acid ester; and / or The compatibility stabilizer includes at least one of polyether-modified siloxane and EO / PO block polyether; and / or The smoothing base oil includes at least one of fatty acid esters, diesters, polyol esters, polyethers, polyether esters, and siloxane-modified esters.

3. The special oiling agent for polyester FDY according to claim 1, characterized in that, The mass ratio of the first antibacterial component to the second antibacterial component is 1:(0.3~4).

4. The special oiling agent for polyester FDY according to any one of claims 1 to 3, characterized in that, The polyester FDY special oil agent also includes 0.01 to 2% of additives by weight, including at least one of defoamer, antioxidant, and corrosion inhibitor.

5. A method for preparing the antibacterial and deodorizing polyester FDY special oil agent according to any one of claims 1 to 4, characterized in that, The preparation method is used to prepare a special oiling agent for polyester FDY, and includes the following steps: S100. The smoothing base oil is added to a reaction vessel for dehydration treatment to obtain dehydrated base oil; S200: Add the emulsifier, the antistatic agent, the clustering agent and 40-80% of the compatibility stabilizer to the dehydrated base oil, and mix to obtain the base oil phase; S300: The first antibacterial component, the second antibacterial component and the remaining compatibility stabilizer are compounded to obtain an antibacterial mother liquor; S400. The antibacterial mother liquor is added to the base oil phase and mixed evenly, and then degassed and filtered to obtain the polyester FDY special oil agent.

6. The preparation method according to claim 5, characterized in that, In S100, the dehydration treatment temperature is 50~95℃, the vacuum degree is -0.06~-0.095MPa, and the time is 20~120min.

7. The preparation method according to claim 5, characterized in that, In S200, the mixing process is carried out at a temperature of 40~80°C for 20~90 minutes.

8. The preparation method according to claim 5, characterized in that, In S300, the temperature for the compounding treatment is 25~70℃ and the time is 10~60min.

9. The preparation method according to claim 5, characterized in that, In S400, The antibacterial mother liquor accounts for 1-12% of the total mass of the base oil phase; and / or The filtration process is a staged filtration, using 5~10μm filtration and 1~3μm filtration sequentially.

10. The preparation method according to any one of claims 5 to 9, characterized in that, After the antibacterial mother liquor described in S400 is added, it is aged at 40~70℃ for 20~90min.

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