Preparation method and application of polyester staple fiber with deodorizing and antibacterial functions

Abstract

This invention relates to the field of functional fiber technology, specifically to a method for preparing polyester staple fibers with deodorizing and antibacterial functions. The method includes preparing hydroxyl-loaded polyester masterbatch, preparing polyester fibers and grafting them, and post-treatment. This invention prepares hydroxyl-rich polyester masterbatch by adding high-temperature resistant hydroxyl-rich nanoparticles to polyester powder, and then adds the hydroxyl-rich polyester masterbatch to the spinning of polyester staple fibers. This increases the number of active hydroxyl groups on the surface of the polyester fibers, solving the problem that polyester itself does not have active groups and cannot be directly grafted onto the surface of pure polyester fibers. The active hydroxyl groups of modified cyclodextrin undergo nucleation and addition reactions with isocyanate groups, replacing high-temperature esterification and radiation crosslinking reactions, resulting in low energy consumption and environmental friendliness. The desealing temperature of the water-based end-capped polyisocyanate is consistent with the drying and relaxation setting temperatures in polyester staple fiber production, triggering the nucleation and addition reaction and solving the problem of side reactions caused by excessively active isocyanate groups.

Description

Technical Field

[0001] This invention relates to the field of functional fiber technology, and in particular to a method for preparing and applying polyester staple fiber with deodorizing and antibacterial functions. Background Technology

[0002] With economic and social development, textiles are being used in a wider range of fields. As people's living standards improve, the demand for textiles in various fields has shifted from traditional durability to functionality, comfort, and the need for green, healthy and safe products.

[0003] Polyester fiber is widely used in clothing, home textiles, furniture, and industrial applications due to its excellent physical properties, chemical stability, ease of processing, and low price, accounting for approximately 70% of global textile fiber consumption. However, as people's pursuit of quality of life continues to increase, the shortcomings of ordinary polyester fiber in terms of comfort, functionality, and hygiene are becoming increasingly apparent.

[0004] In daily life, textiles, especially home textiles, are prone to harboring microorganisms due to their fabric structure and internal fiber fillings. Furthermore, human sweat, oils, and dander provide ideal breeding grounds for microorganisms and bacteria. The decomposition of these substances by microorganisms and bacteria produces odors and causes discomfort. Simultaneously, with the increasing aging population, the release of nonenal by the elderly at certain concentrations can also cause unpleasant odors. The odors emitted by pet cats or dogs also affect people's daily lives and pose certain health risks. Therefore, antibacterial and deodorizing fibers and textiles are increasingly attracting consumer attention and demand, and represent one of the directions for the development of functional fibers and textiles.

[0005] Cyclodextrin is a natural deodorant with a cone-shaped molecular structure containing hydrophobic cavities and a hydrophilic surface. Figure 1 and Figure 2 As shown, the inner diameter of β-cyclodextrin molecules is 0.68 nm, and the inner diameter of γ-cyclodextrin molecules is 0.8 nm. This special structure allows cyclodextrin to encapsulate most of the odorous small molecules, such as sweat odor (ammonia, acetic acid, isovaleric acid), aging odor (2-nonenal), pet odor, and household garbage odor (indole, methanethiol, hydrogen sulfide), thereby achieving the deodorizing effect. Furthermore, cyclodextrin has good biocompatibility and stability and is non-toxic and harmless to the human body.

[0006] Currently, methods for deodorizing textile fabrics using cyclodextrin (such as Chinese patents CN109667137B, CN118272986B, CN120830248A) or fibers (such as Chinese patent CN112176728B) include: 1. Using an impregnation process, cyclodextrin is bonded to the fabric or fiber using an adhesive. This method cannot solve the problem of washability, and the adhesive coating of cyclodextrin also affects the deodorizing effect. Furthermore, the presence of the adhesive severely affects the fabric's hand feel. 2. Using high-temperature esterification or irradiation crosslinking. This technology requires the fiber or fabric to be rich in hydroxyl groups. High-temperature esterification requires a catalyst, making production environmentally unfriendly. High temperatures also cause yellowing of the fiber or fabric and a stiffening of the fabric's hand feel. Irradiation requires specialized radiation equipment, which is sophisticated, requires large investments, and has high production costs, making large-scale mass production impractical. 3. Published and even authorized patents do not consider the extremely low solubility of cyclodextrin in water. At 25°C, the solubility of α-cyclodextrin is 12.7 g / 100 mL, β-cyclodextrin is 1.8 g / 100 mL, and γ-cyclodextrin is 23.2~25.6 g / 100 mL. However, the processing techniques all use aqueous solutions. In actual treatment processes, due to the extremely low solubility of cyclodextrin, it cannot fully penetrate the fiber surface or the yarn interface of the fabric, and therefore cannot fully combine with the fiber or fabric, resulting in an inadequate deodorization effect.

[0007] Polyester staple fiber is the most widely used filling material in home textiles such as quilts, mattress pads, pillows, sofa cushions, backrests, and pet beds. These filling applications are more prone to bacterial growth and odor due to their low washing frequency and long service life, making deodorization and antibacterial properties more urgent. However, polyester fiber itself does not have active groups that can bind with cyclodextrin, and adhesives cannot solve the problems of washability and poor deodorization.

[0008] Therefore, how to environmentally friendly, efficient and strong grafting of functional components such as cyclodextrin onto the surface of polyester fibers is an urgent problem that is of great economic and social significance. Summary of the Invention

[0009] To address the aforementioned problems, this invention constructs a chemical reaction in situ on the surface of polyester staple fibers during the manufacturing process, thereby crosslinking modified cyclodextrin onto the surface of the polyester staple fibers in the form of a covalently bonded chemical graft network.

[0010] In a first aspect, the present invention provides a method for preparing polyester staple fiber with deodorizing and antibacterial functions, comprising the following steps: (1) Preparation of hydroxyl-loaded polyester masterbatch The dried PET chips or powders are thoroughly mixed in a high-speed mixer with at least one or more of the following nanoparticles: nano-kaolin, montmorillonite, diatomaceous earth, nano zinc oxide, and nano aluminum hydroxide, which are rich in hydroxyl groups or have undergone hydroxylation surface treatment. The mixture is then melt-blended, extruded, cooled, and pelletized through a twin-screw extruder to obtain polyester masterbatch loaded with active hydroxyl groups. This step aims to introduce reactive active sites (-OH) into the polyester matrix. (2) Deodorizing polyester spinning and surface grafting a. Pre-spinning: The loaded active hydroxyl polyester masterbatch obtained in step (1) and conventional polyester chips are dried in advance to ensure that the moisture content of the loaded active hydroxyl polyester masterbatch and conventional polyester chips is controlled below 50ppm. Spinning is carried out on the polyester staple fiber production line. The dried loaded hydroxyl polyester masterbatch and conventional polyester chips are fed into the screw extruder in a certain proportion to be fully mixed and melted. After being stretched through the melt pipe, spinning assembly and drawing roller, nascent fiber bundles with active hydroxyl groups are obtained. b. Surface grafting pretreatment: The nascent fiber bundles enter the polyester staple fiber post-spinning production through the bundling frame. During the fiber crimping stage, a certain amount of deodorizing treatment liquid is uniformly and high-pressurely sprayed onto the upper and lower surfaces of the crimped fiber bundles through multiple rows of microporous channels densely distributed on the upper and lower pressure plates and bottom plates of the crimping machine's filling box using a metering pump. The deodorizing treatment liquid is a mixed aqueous solution of modified cyclodextrin, nano zinc oxide, and water-based end-capped polyisocyanate. Under high-pressure spraying, the deodorizing treatment liquid quickly penetrates into the surface of each fiber in the fiber bundle, ensuring that each fiber surface is coated with a layer of deodorizing treatment liquid. c. Drying and Graft Network Curing: After being sprayed with deodorizing liquid, the wet fiber bundles are laid flat on a stainless steel mesh screen and placed in a multi-zone oven for drying and graft network curing. The temperature in the front zone (1-4) of the oven is 90-110℃, mainly to quickly evaporate the moisture on the surface of the fiber bundles, while the deodorizing liquid adheres more evenly to the fiber surface. The temperature in the middle zone (zones 5-8) is 140-150℃. At this temperature, the end-capping agent of the water-based end-capped polyisocyanate begins to gradually decapsulate, releasing active isocyanate groups (-NCO). The active -NCO groups undergo rapid nucleophilic addition reactions with the active hydroxyl groups on the modified cyclodextrin molecular chain, the active hydroxyl groups of zinc oxide, and the active hydroxyl groups on the fiber surface to form stable urethane bonds (-NHCOO-). The temperature in the back zone (zones 9-10) is 160-180℃. At this high temperature, the nucleophilic addition reaction is further intensified until the -NCO is exhausted. The modified cyclodextrin and zinc oxide are firmly cured on the surface of the polyester fiber in a network. After drying and curing, the fiber bundles are cut by a cutting machine and packaged to obtain deodorizing polyester staple fibers.

[0011] Preferably, in step (1), the total amount of hydroxylated nanoparticle material added is 10%-20% of the weight of PET chips. If the amount added is too low, there will be insufficient surface active hydroxyl sites; if it is too high, the filtration pressure difference (DF) value will be too high, affecting the long-cycle production of spinning.

[0012] Preferably, in step (2), the proportion of the loaded hydroxyl polyester masterbatch added to the total spinning feed is 3%-20wt%. This proportion determines the density of hydroxyl groups that can be grafted onto the final fiber surface.

[0013] Preferably, in step (2), the concentration of the deodorizing treatment liquid is 5%-50%, wherein the mass concentration of modified cyclodextrin is 2%-35%, the mass concentration of nano zinc oxide is 0.5%-5%, the mass concentration of water-based end-capped polyisocyanate is 1%-15%, and the molar ratio of isocyanate group -NCO to hydroxyl group -OH is 1:(1~10). This ratio ensures sufficient -NCO group addition reaction to fix the cyclodextrin, while avoiding excessive -NCO groups causing changes in fiber style due to side reactions. However, too low a -NCO ratio results in insufficient curing and crosslinking of modified cyclodextrin and nano zinc oxide, failing to meet the requirements for deodorization, antibacterial effect, and washability.

[0014] Preferably, in step (2), the modified cyclodextrin satisfies the following requirements: the inner diameter of the molecular pores is greater than 0.6 nm, and the solubility in water exceeds 100%. It is one or more mixtures of hydroxypropyl-β-cyclodextrin, hydroxyethyl-β-cyclodextrin, carboxymethyl-β-cyclodextrin, and hydroxypropyl-γ-cyclodextrin. The cyclodextrin is selected using β-cyclodextrin and γ-cyclodextrin to ensure that the inner diameter and depth of the cavity match the size of the odor molecules, achieving sufficient adsorption and deodorization. The modification of the cyclodextrin with hydroxypropyl, hydroxyethyl, and carboxymethyl groups is to address the problem that the water solubility of β-cyclodextrin and γ-cyclodextrin is too low, making it impossible to ensure the concentration of cyclodextrin in aqueous solution and to allow it to quickly penetrate and coat the surface of polyester fibers.

[0015] Preferably, in step (2), the aqueous capped polyisocyanate is a capped product based on hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI), or toluene diisocyanate (MDI), and the capping agent is an oxime, imidazole, or lactam, etc., with a decapping temperature of 105℃-160℃, a solid content greater than 70%, and an isocyanate group -NCO content greater than 10%. The selection of polyisocyanate and capping agent takes into account the consistency between the -NCO group content and the decapping temperature and the relaxation and setting temperature of polyester fiber production. The nucleophilic addition reaction is completed simultaneously with the drying and relaxation setting of polyester fiber, while avoiding the decapping temperature being too low, which would cause -NCO to react with water, and the decapping temperature being too high, which would lead to excessively high production costs and be uneconomical and environmentally unfriendly.

[0016] Preferably, in step (2), the liquid carrying rate of the deodorizing treatment liquid on the fiber bundle is 15%-50%. If the liquid carrying rate is too low, the concentration of the deodorizing treatment liquid is required to be high, the viscosity of the deodorizing treatment liquid is too high, the fluidity is poor, which is not conducive to the rapid and uniform penetration of the deodorizing treatment liquid to the surface of each fiber; if the liquid carrying rate is too high, although the concentration of the deodorizing treatment liquid can be reduced, the fluidity is good and it is easy to penetrate to the fiber surface, but the subsequent water drying pressure is too high, which causes the water on the fiber surface to not be completely evaporated when entering the medium and high temperature zone, participate in the -NCO reaction, and reduce the addition reaction with modified cyclodextrin and zinc oxide.

[0017] Secondly, the present invention provides an odor-deodorizing nonwoven fabric sheet, which is made from the above-mentioned polyester short fibers with deodorizing and antibacterial functions and other ordinary fibers or functional fibers through a nonwoven fabric sheet equipment or a ball cotton equipment. In the odor-deodorizing nonwoven fabric sheet, the proportion of polyester short fibers with deodorizing and antibacterial functions is 30wt% to 100wt%.

[0018] Thirdly, the present invention provides the application of the above-mentioned deodorizing non-woven fabric wadding in the field of textiles, and is particularly suitable for filling textiles with high requirements for hygiene and comfort, such as quilts, quilted pads, backrest cushions, pillows, mattresses, pet beds and clothing.

[0019] The technical advantages of this invention are as follows: 1. Innovative Grafting Method: This invention prepares hydroxyl-rich polyester masterbatch by adding high-temperature resistant hydroxyl-rich nanoparticles to PET powder. A certain proportion of this hydroxyl-rich polyester masterbatch is then added to the spinning of polyester staple fibers, thereby increasing the number of active hydroxyl groups on the polyester fiber surface. This solves the operational problem of directly grafting the masterbatch onto the surface of pure PET fibers because polyester itself lacks active groups. The invention utilizes the nucleation and addition reaction between the active hydroxyl groups of cyclodextrin and isocyanate groups, replacing the drawbacks of high-temperature esterification and radiation crosslinking reactions, achieving a low-energy, high-efficiency, and environmentally friendly process. Furthermore, the invention leverages the consistent drying and relaxation temperatures of water-based end-capped polyisocyanates and polyester staple fiber production processes to trigger the nucleation and addition reaction, solving the problem of side reactions caused by the high reactivity of isocyanate groups with water and other substances.

[0020] 2. Highly efficient and long-lasting deodorization: Cyclodextrin is firmly grafted onto the surface of polyester fibers through chemical bonds, avoiding the problem of easy detachment in post-treatment methods. Washability is significantly improved. The cavity structure of cyclodextrin can physically encapsulate a variety of polar and non-polar odor molecules, resulting in a broad deodorization spectrum and long-lasting deodorization function, greatly enhancing the user experience of products containing this fiber.

[0021] 3. Process Integration and Innovation: By modifying the crimping machine and adding a metering spray unit integrated into the equipment, the surface chemical modification process is innovatively integrated into the crimping-drying process of polyester staple fiber post-spinning production. This satisfies the need to achieve deodorization for different types and specifications of polyester staple fibers, while realizing continuous production of "spinning-functionalization". It is highly efficient, requires no additional equipment or processing steps, and saves energy and reduces consumption. The water-based treatment solution is more environmentally friendly than organic solvent systems, has high chemical grafting reaction efficiency, low residual monomer, and ensures the stability and reliability of the fiber in subsequent processing and use.

[0022] 4. Wide range of applications: The polyester staple fiber prepared by this invention has deodorizing function, antibacterial properties and good mechanical properties. It can be widely used in all types of filled textiles, including clothing, home textiles and home furnishings. It is widely used in comforters, fiber mattresses, fiber pillows and home furnishings such as sofa cushions, backrests and pet beds, meeting people's demand for high-quality and multifunctional products, and has broad market application prospects. Attached Figure Description

[0023] Figure 1 This is a schematic diagram of the molecular structure of β-cyclodextrin, with an inner diameter of 0.68 nm.

[0024] Figure 2 This is a schematic diagram of the molecular structure of γ-cyclodextrin, with an inner diameter of 0.8 nm.

[0025] Figure 3 This is an SEM image of the deodorizing polyester staple fiber obtained in Example 1. Detailed Implementation

[0026] The present invention will be described below with reference to examples. These examples are only used to explain the present invention and are not intended to limit the scope of the present invention.

[0027] I. Preparation of deodorizing polyester fiber 1. Raw material preparation Conventional PET chips (intrinsic viscosity 0.65 dl / g) and conventional PBT chips (intrinsic viscosity 1.0 dl / g) are ground to obtain powder with a particle size of 200-500 mesh. Hydroxylated nano-kaolin, montmorillonite, diatomaceous earth, nano-zinc oxide, and nano-aluminum hydroxide are used, requiring nanoparticles with a particle size below 1 μm (D90) and a surface hydroxyl content greater than 2 (-OH / nm). 2The hydroxyl content was calculated by quantitative analysis of the specific surface area of ​​the nanoparticles combined with Fourier transform infrared spectroscopy (FT-IR). The coupling agent was one of vinyltriethoxysilane coupling agent, triisostearoyl titanate isopropyl acetate coupling agent, aluminum-titanium composite coupling agent, stearate coupling agent, or phosphate ester coupling agent. The dispersant was one of polyether ester polymer, pentaerythritol stearate, or polyethylene wax.

[0028] 2. Polyester masterbatch (1) Formulation design The granulation formulation of the hydroxyl-loaded polyester masterbatch is shown in Table 1.

[0029] Table 1. Deodorizing Treatment Solution Formulation Design raw material Masterbatch-1# Masterbatch-2# Masterbatch-3# PET powder 83 copies 46 copies 50 copies PBT powder 40 copies 37 copies Nano zinc oxide 3 copies 1 copy 2 copies Nano aluminum hydroxide 1 copy 3 copies 2 copies Nano diatomite 10 copies Nano-kaolin 8 copies Nano-montmorillonite 5 copies HEDIS®200 dispersant (polyether ester) 2 copies 2 copies 2 copies Coupling agent KH550 (silane-based) 1 copy 1 copy 2 copies (2) Granulation process ① Raw material drying The polymer chips used for granulation are dried in a rotary drum oven to ensure that the moisture content of the material is less than 50 ppm, and then pulverized to 200-500 mesh in a high-speed pulverizing device, and sealed and packaged for later use; other nanopowders are dried during hydroxylation and pre-dispersion treatment, and then sealed and packaged for later use. ② Preparation of pre-dispersion The hydroxylated nanoparticles were thoroughly mixed with half the amount of dispersant and coupling agent in a mixer according to the formulation ratio in Table 1 to prepare a pre-dispersion. ③ Premix preparation According to the formula in Table 1, mix the PET or PBT powder with the remaining half of the dispersant and coupling agent thoroughly, so that the dispersant and coupling agent fully coat the surface of the polyester chips. Then add the pre-dispersed material obtained in step ② and mix thoroughly and evenly under high-speed stirring of a high-speed mixer. The stirring time is set to 7-30 minutes to obtain the premixed material. ④ Granulation The premix obtained in step ③ is added to the hopper of a twin-screw extruder and fed into the melting and mixing zones of each twin-screw section through the feed port. The temperatures of each twin-screw section are set as follows: 120-150℃, 180-210℃, 190-235℃, 190-243℃, 190-250℃, 190-250℃, 190-250℃, 190-255℃, 190-255℃. The temperature settings of each zone are designed to be higher than the melting point of the polymer to ensure that the polymer and functional powder are fully and uniformly mixed under high viscosity. The ratio of the internal mixing section to the compression section of the screw needs to be adjusted appropriately depending on the powder ratio and the characteristics of the polymer chips. The length-to-diameter ratio of the screw is 1:35-45. After extrusion, the mixture is cooled in a water tank, blown by a blower, and cut into granules to obtain hydroxyl-loaded PET (1-3#) masterbatch. To improve filtration accuracy, two 200-mesh filters are installed at the screw extrusion die, with the mesh size arranged in a cross pattern. The masterbatch undergoes a filtration differential pressure test, and the DF value is required to be less than 2.

[0030] 3. Deodorizing treatment solution (1) Preparation of raw materials for deodorization treatment solution Modified cyclodextrins: hydroxypropyl-β-cyclodextrin (water solubility 240 g / ml), hydroxypropyl-γ-cyclodextrin (water solubility 130 g / ml); Nano zinc oxide aqueous solution: solid content 50%, zinc oxide particle size 30nm; Water-based capped polyisocyanates: HD-750 (HDMI type, solid content 75%, -NCO content 10%, decapsulation temperature 105℃); HD-850 (HDMI type, solid content 85%, NCO content 12%, decapsulation temperature 120℃).

[0031] (2) Configuration The formulation of the deodorizing treatment solution is shown in Table 2. According to the formulation table in Table 2, first, deionized water is metered into the mixing tank, the stirrer is turned on, the stirring speed is 150 r / min, and the temperature of the mixing tank is controlled to 40℃. Then, modified cyclodextrin is metered in, and after stirring for 20 minutes, nano zinc oxide aqueous solution is metered in, and stirred for another 20 minutes. Finally, water-based end-capped polyisocyanate is metered in, and stirring is continued for 60 minutes. It is then ready for use.

[0032] Table 2. Deodorizing Treatment Solution Formulation Design formula Deodorizing solution formula and ratio Fiber bundle liquid coverage (%) Formula-1# Hydroxypropyl-β-cyclodextrin: 15 parts; Nano zinc oxide aqueous solution: 5 parts; Aqueous capped polyisocyanate HD-750: 8 parts; Deionized water: 82 parts 25% Formula-2# Hydroxypropyl-β-cyclodextrin: 10 parts; Nano zinc oxide aqueous solution: 2 parts; Aqueous capped polyisocyanate HD-750: 6 parts; Deionized water: 88 parts 30% Formula-3# Hydroxypropyl-γ-cyclodextrin: 10 parts; Nano zinc oxide aqueous solution: 2 parts; Aqueous capped polyisocyanate HD-850: 5 parts; Deionized water: 83 parts 23% 4. Spinning (pre-spinning of short fibers) The prepared hydroxyl-loaded PET masterbatch (1-3#) was dried at 140℃ for 4 hours and then used to produce three types of hydroxyl-loaded polyester staple fibers by pre-spinning with conventional PET chips at a weight ratio of 5:95. The masterbatch and chips were fed into a screw extruder through a metering screw and pre-spun using a conventional PET staple fiber spinning production line. After multi-stage hot roller drawing, three three-dimensional hollow nascent fiber bundles numbered 1-3# with a density of 15 dtex were obtained.

[0033] 5. Surface pretreatment before grafting The nascent fiber bundles, numbered 1-3#, are fed into the polyester staple fiber spinning process in batches. After passing through a bundling frame and undergoing three stages of drafting (total draft ratio controlled at 3-4 times), the bundles enter the fiber crimping stage. In the fiber crimping stage, after the fiber bundles are crimped in the crimping box, a metering pump sprays the deodorizing liquid, formulated in Table 2, evenly and under high pressure onto the upper and lower surfaces of the crimped fiber bundles through multiple rows of microporous channels densely distributed on the upper and lower pressure plates and bottom plates at the crimping machine's filling box outlet. Under high pressure, the deodorizing liquid rapidly penetrates the surface of each fiber in the bundle, ensuring that each fiber surface is coated with a layer of deodorizing liquid. The liquid carry-over rate of the fiber bundles is controlled according to the liquid carry-over rate requirements of each formula in Table 2, with the metering pump speed adjusted accordingly.

[0034] 6. Drying and curing of grafted networks After being sprayed with deodorizing liquid, the wet fiber bundles enter the drying and grafting network curing process. The fiber bundles are then evenly spread on a stainless steel mesh screen via a left-right oscillating conveyor before entering a multi-zone drying oven for drying and grafting network curing. The temperature in the front zone (zones 1-4) of the oven is 90-110℃, primarily for rapid evaporation of moisture from the fiber bundle surface. Simultaneously, the deodorizing liquid rapidly penetrates and evenly adheres to the fiber surface as the moisture evaporates. The temperature in the middle zone (zones 5-8) is 140-150℃. At this temperature, the water-based end-capping agent of the polyisocyanate begins to open. The process begins with gradual unsealing, releasing active isocyanate groups (-NCO). These active -NCO groups undergo rapid nucleophilic addition reactions with the active hydroxyl groups on the modified cyclodextrin molecular chain, the active hydroxyl groups of zinc oxide, and the active hydroxyl groups on the fiber surface, forming stable carbamate bonds (-NHCOO-). The temperature in the back zone (zones 9-10) is 160-180℃. At this high temperature, the nucleophilic addition reaction is further intensified until the -NCO groups are exhausted, and the modified cyclodextrin and zinc oxide are firmly fixed to the surface of the polyester fiber in a network structure. The total residence time of the fiber in the oven is 15 minutes. After drying and curing, the fiber bundles are cut by a cutting machine and packaged to obtain deodorized polyester staple fibers.

[0035] Using the above process, the deodorizing polyester fiber technology combinations of Examples 1 to 9 (Fiber-1 to Fiber-9) of the present invention are shown in Table 3.

[0036] Table 3. Examples 1-9: Deodorizing Polyester Fiber Technology Combination Deodorizing fibers Fiber-1 Fiber-2 Fiber-3 Fiber-4 Fiber-5 Fiber-6 Fiber-7 Fiber-8 Fiber-9 Masterbatch Masterbatch-1# Masterbatch-1# Masterbatch-1# Masterbatch-2# Masterbatch-2 Masterbatch-2# Masterbatch-3# Masterbatch-3# Masterbatch-3# Deodorizing solution Formula-1# Formula-2# Formula-3# Formula-1# Formula-2# Formula-3# Formula-1# Formula-2# Formula-3# Figure 3 The image shown is an SEM image of the deodorizing polyester staple fiber obtained in Example 1. It can be seen that after the water-based capped polyisocyanate HD-750 is decapsulated, it reacts with hydroxypropyl-β-cyclodextrin and the active hydroxyl groups on the fiber to form a uniform film on the fiber surface, which uniformly embeds the nano zinc oxide, giving the fiber continuous and long-lasting deodorizing and antibacterial properties.

[0037] II. Preparation of Deodorizing Nonwoven Fabric Sheets To expand its application in fiber filling, a certain proportion of deodorizing polyester fiber can be added during the nonwoven fabric preparation process and mixed with various other filling fibers (such as cotton fiber, viscose fiber, ordinary polyester fiber, etc.) to obtain deodorizing nonwoven fabric flakes.

[0038] This invention uses the deodorizing polyester fibers (fiber specifications: 3D*64mm three-dimensional crimped hollow) from Examples 1 to 9. The deodorizing polyester fibers are uniformly mixed with ordinary polyester staple fibers (fiber specifications: 3D*64mm three-dimensional crimped hollow) at a ratio of 50%. The deodorizing nonwoven wadding with a weight of 200 g / m² is produced on the wadding cotton production line. These are Application Examples 1 to 9, and the corresponding wadding codes are NonW-1 to NonW-9.

[0039] Comparative Example Using 100% ordinary PET chips and the same spinning process as in the example, but without spraying deodorizing liquid during the crimping process, ordinary polyester staple fiber sample Fiber-C was obtained.

[0040] Using 100% ordinary polyester staple fiber and the same ordinary fiber and wadding production line as in the application example, a standard 200GSM nonwoven wadding sample, NonW-C, was obtained.

[0041] III. Performance Testing 1. Test the wash resistance of the samples: The prepared fibers and non-woven fabric sheets were washed 20 times according to the simplified washing conditions and procedures in Appendix C4 of standard FZ / T73023-2006, and then the deodorization and antibacterial properties were tested.

[0042] 2. Odor deodorization performance test Ammonia and acetic acid: Tested using the test tube method according to the Japanese SEK mark fiber product certification standard (JEC301-2013) and GBT33610.2-2017 standard; Isovalerate, 2-nonenal, and indole: determined using gas chromatography (GC) according to the Japanese SEK certification standards for fiber products (JEC301-2013) and GBT33610.3-2019.

[0043] 3. Antibacterial performance test The test was conducted according to Japanese standard JIS L1902:2008, "Test Methods for Antimicrobial Properties of Textiles - Antimicrobial Effect".

[0044] 4. Fiber moisture regain test The determination was carried out in accordance with GB / T9995-1997 "Determination of Moisture Content and Moisture Regain of Textile Materials - Oven Drying Method".

[0045] The test results are shown in Tables 4 and 5. Table 4, which tests 100% of the fibers, shows that the deodorizing polyester fiber prepared in this embodiment of the invention has good deodorizing and antibacterial effects, is washable, has a moisture regain rate of about 1%, and improves comfort. Table 5, which tests the performance of nonwoven wadding with nine types of deodorizing polyester fibers prepared in the embodiment by adding a certain proportion, shows that adding a certain proportion of the deodorizing polyester fiber of this invention in the production of nonwoven wadding can achieve deodorizing and antibacterial effects, and is washable, meeting the needs of different wadding and their end-use scenarios. Therefore, the deodorizing polyester staple fiber of this invention can be widely used in all types of filling textiles.

[0046] Table 4. Fiber Performance Testing Table 5. Performance Testing of Flocs 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 within the protection scope of the present invention.

Claims

1. A method for preparing polyester staple fiber with deodorizing and antibacterial functions, characterized in that, Includes the following steps: 1) Preparation of hydroxyl-loaded polyester masterbatch Polyester raw materials, active hydroxyl carriers, dispersants and coupling agents are mixed evenly in proportion and then melt-blended, extruded and granulated to obtain hydroxyl-loaded polyester masterbatch. 2) Preparation of polyester fibers and grafting The hydroxyl-loaded polyester masterbatch obtained in step 1) and pure PET chips are dried separately, mixed evenly in proportion, and then prepared into nascent fiber bundles by a screw extruder. The nascent fiber bundles are then further spun. In the fiber crimping stage, a deodorizing treatment liquid containing modified cyclodextrin and water-based end-capped diisocyanate is uniformly and high-pressure sprayed onto the fiber surface. The crimped PET fibers are dried in three stages in an oven, with the drying temperatures of the three stages controlled at 90~110℃, 140~150℃, and 160~180℃, respectively. 3) Post-processing After the fibers from step 2) are naturally cooled, they are cut into filaments to obtain short fibers of the required length.

2. The method according to claim 1, characterized in that, In step 1), the active hydroxyl carrier is one or more of the following nanoparticles: nano-kaolin, montmorillonite, diatomaceous earth, nano-zinc oxide, nano-aluminum hydroxide, etc.

3. The method according to claim 1, characterized in that, In step 1), the weight proportions of the polyester raw material, active hydroxyl carrier, dispersant, and coupling agent are as follows: 80-90 parts polyester raw material, 10-20 parts active hydroxyl carrier, 0.5-2 parts dispersant, and 0.5-3 parts coupling agent; the polyester raw material is PET or PBT, in chips or powder; the dispersant is one of polyether ester polymer, pentaerythritol stearate, or polyethylene wax; the coupling agent is one or a combination of vinyltriethoxysilane coupling agent, triisostearoyl titanate isopropyl acetate coupling agent, aluminum-titanium composite coupling agent, stearate coupling agent, or phosphate ester coupling agent.

4. The method according to claim 1, characterized in that, In step 2), the hydroxyl-loaded polyester masterbatch is added to the spinning raw material at a ratio of 3wt% to 20wt%.

5. The method according to claim 1, characterized in that, In step 2), the deodorizing treatment liquid contains the following components in the following proportions: 2wt%~35wt% modified cyclodextrin, 0.5wt%~5wt% nano zinc oxide, 1wt%~15wt% aqueous end-capped polyisocyanate, and the balance being water; in the deodorizing treatment liquid, the molar ratio of isocyanate groups to hydroxyl groups is 1:(1~10).

6. The method according to claim 5, characterized in that, The modified cyclodextrin has a molecular pore inner diameter greater than 0.6 nm and a solubility in water greater than 100 g / 100 mL. It is one or more of hydroxypropyl-β-cyclodextrin, hydroxyethyl-β-cyclodextrin, carboxymethyl-β-cyclodextrin, or hydroxypropyl-γ-cyclodextrin.

7. The method according to claim 5, characterized in that, The aqueous end-capped polyisocyanate has a decapsulation temperature of 105℃~160℃, a solid content of more than 70%, and an isocyanate group content of more than 10%.

8. The method according to claim 7, characterized in that, The aqueous capped polyisocyanate is a capped product based on hexamethylene diisocyanate, isophorone diisocyanate or toluene diisocyanate, and the capping agent is an oxime, imidazole or lactam.

9. A deodorizing nonwoven fabric sheet, characterized in that, The deodorizing and antibacterial polyester staple fiber and other ordinary or functional fibers prepared by any one of claims 1 to 8 are prepared by a nonwoven fabric wadding device or a ball cotton device. In the deodorizing nonwoven fabric wadding, the proportion of the deodorizing and antibacterial polyester staple fiber is 30wt% to 100wt%.

10. The application of the deodorizing nonwoven fabric wadding as described in claim 9 in quilt cores, quilted pads, seat cushions, pillows, mattresses, pet beds, and clothing.

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