Antibacterial and deodorant polyester fiber and preparation method thereof

By introducing triethanolamine, g-C3N4/X, and polyethylene glycol of different molecular weights during the synthesis of polyester fibers, an antibacterial and deodorizing polyester fiber with a permeable microporous structure is formed, which solves the problem that it is difficult to balance antibacterial and deodorizing performance with fiber mechanical properties in the existing technology, and achieves efficient and stable antibacterial and deodorizing effect.

CN121629554APending Publication Date: 2026-03-10FUJIAN CHANGLE CITY CHANGYUAN TEXTILE
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-22
Publication Date
2026-03-10

AI Technical Summary

Technical Problem

In the current process of modifying polyester fibers for antibacterial and deodorization, it is difficult to achieve both high-efficiency antibacterial and deodorization functions and the stability of fiber mechanical properties. Furthermore, existing methods are prone to causing damage to the fiber structure or limiting its functionality.

Method used

By introducing triethanolamine, g-C3N4/X (X is Ag⁺, Cu²⁺ or Fe³⁺) and polyethylene glycol of different molecular weights into the polyester fiber synthesis process, and through esterification, pre-condensation and final condensation reactions, combined with hollow profile spinning and water treatment, antibacterial and deodorizing polyester fibers with a through-hole microporous structure are formed.

Benefits of technology

It achieves highly efficient antibacterial and deodorizing performance while maintaining the mechanical properties of the fiber, and its functional stability is good and does not decrease with washing and use.

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Abstract

The invention discloses an antibacterial and deodorant polyester fiber and a preparation method thereof, and belongs to the technical field of functional polyester fiber preparation. The method comprises the following steps: preparing a mixed slurry containing triethanolamine, g-C3N4 / X (X is one or more of Ag < + > or Cu < 2 + > or Fe < 3 + >), terephthalic acid and ethylene glycol, sequentially carrying out esterification reaction, pre-polycondensation reaction and final polycondensation reaction to obtain modified polyester, and carrying out hollow special-shaped melt spinning and water treatment with a sodium hydroxide aqueous solution to obtain the hollow g-C3N4 / X / terephthalic acid modified polyester. The antibacterial and deodorant polyester fiber with the micro-porous penetrating structure is obtained. Through a'copolymerization + blending 'composite modification mode, the mechanical property and the antibacterial deodorization function of the fiber are synergistically improved, the mechanical strength of the fiber is larger than or equal to 3.0 cN / dtex, the antibacterial rate to candida albicans, escherichia coli and staphylococcus aureus is larger than or equal to 95%, the reduction rate of isovaleric acid is larger than or equal to 90%, the reduction rate of ammonia gas is larger than or equal to 85%, the function is long-acting and stable, and the fiber can be widely applied to the fields of clothes, home textiles and the like.
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Description

Technical Field

[0001] This invention relates to the field of functional polyester fiber preparation technology, specifically to an antibacterial and deodorizing polyester fiber and its preparation method. Background Technology

[0002] Polyester fiber is currently the largest category of synthetic fibers. Due to its high molecular chain rigidity and elastic modulus, fabrics made from polyester fiber are wrinkle-free, strong, crisp, easy to wash and dry, and possess good heat resistance, sun resistance, and abrasion resistance, making it widely used in clothing, home textiles, and industrial applications. However, polyester fiber can easily become a medium for the spread of microorganisms during use. Pathogenic bacteria such as Staphylococcus aureus, Escherichia coli, and Candida albicans, as well as "odor-causing bacteria" (such as Staphylococcus epidermidis and Corynebacterium) that decompose human sweat metabolites, will multiply rapidly in high temperature and humidity environments. Their metabolic products can lead to fiber degradation and discoloration, and generate volatile malodorous substances such as acetic acid and ammonia. This not only affects the user experience but may also cause human diseases. Therefore, antibacterial and deodorizing modification of polyester fiber is particularly necessary.

[0003] In existing technologies, the antibacterial and deodorizing modification of polyester fibers mainly focuses on two approaches: one is to introduce inorganic antibacterial materials during the polyester synthesis or spinning stage, and improve the utilization rate of functional materials through methods such as core-sheath composite spinning or masterbatch carrier migration; the other is to introduce functional components through in-situ polymerization or blending, followed by a washing treatment of the fiber to increase the contact area between the functional components and external small molecules. However, both of these methods have obvious drawbacks: the former has limited improvement in antibacterial and deodorizing performance, while the latter easily leads to a significant decrease in fiber mechanical properties, making it difficult to balance functionality and structural stability.

[0004] For example, Chinese invention patent 201210491230.3 discloses a core-sheath type antibacterial and deodorizing polyester fiber, which is prepared by blending or copolymerizing a composite antibacterial agent with polyester and then spinning it into a composite. However, the core-sheath structure limits the full contact of the antibacterial components, resulting in limited functional efficiency. Chinese invention patent 202011123881.8 improves the antibacterial and deodorizing efficiency by eluting water-soluble polyester to form a microporous structure. However, the elution process will damage the integrity of the fiber structure, leading to a decrease in mechanical properties. Chinese invention patent 202411355640.4 uses acid washing modification to obtain acid-base buffer groups. Although it has wash resistance, the antibacterial function depends on the antibacterial masterbatch, and the deodorization mechanism is singular, making it difficult to achieve efficient synergy.

[0005] Therefore, developing a polyester fiber preparation technology that can achieve efficient antibacterial and deodorizing functions, retain the excellent mechanical properties of the fiber, and maintain long-term stable function has become an urgent technical problem to be solved in this field. Summary of the Invention

[0006] The purpose of this invention is to provide an antibacterial and deodorizing polyester fiber and its preparation method, so as to solve the problems of existing polyester fibers having difficulty in balancing mechanical properties and functions, and insufficient functional stability.

[0007] The technical solution of the present invention to solve the above-mentioned technical problems is as follows: A method for preparing antibacterial and deodorizing polyester fiber includes the following steps: S1: Preparation of mixed slurry: Triethanolamine, g-C3N4 / X, terephthalic acid and ethylene glycol are mixed, wherein X is one or more of Ag⁺, Cu²⁺ or Fe³⁺; S2: The reaction proceeds sequentially: the mixed slurry first undergoes an esterification reaction, then enters the pre-condensation reaction stage, and finally undergoes a final condensation reaction, wherein polyethylene glycol is introduced in the pre-condensation reaction stage; S3: Spinning and post-treatment: The modified polyester obtained by final polycondensation is processed into fibers by hollow shaped melt spinning process. After water treatment, antibacterial and deodorizing polyester fibers with microporous structure are prepared.

[0008] In a further proposed scheme, the molar ratio of terephthalic acid to ethylene glycol is 1:1.2-1.5.

[0009] In the mixed slurry: the molar ratio of triethanolamine to ethylene glycol is 0.01-0.1:1; the mass fraction of g-C3N4 / X relative to terephthalic acid is 0.5-2.0%.

[0010] In a further embodiment, triethanolamine is mixed with g-C3N4 / X and then added together with terephthalic acid and ethylene glycol. The mixed slurry contains a catalyst, which is one or more of tetrabutyl titanate, titanium glycol, and antimony glycol. The mass fraction of the catalyst relative to terephthalic acid is 10-200 ppm.

[0011] A further proposed approach involves the following specific preparation process for g-C3N4 / X: S11: Under ambient pressure in air, melamine is placed in a covered crucible and heated to 500-650℃ in a muffle furnace at a heating rate of 5-20℃ / min, and held for 2-5 hours to obtain block g-C3N4 / X; S12: After natural cooling, grind into powder, then heat to 500-600℃ at a heating rate of 1-5℃ / min, and keep warm for 2-4 hours to obtain powdered g-C3N4; S13: Disperse powdered g-C3N4 / X in deionized water for 15-60 minutes under ultrasonic conditions, wherein the mass of the deionized water is 25-80% of the mass of g-C3N4 / X; then add dropwise 0.1-0.5 mol / L AgNO3, Cu(NO3)2 or Fe(NO3)3 standard solution, stir for 3-6 hours, centrifuge, wash 3 times with deionized water and anhydrous ethanol, and finally dry to constant weight.

[0012] In a further proposed approach, the esterification reaction temperature is 235-245℃, the reaction pressure is positive pressure 0-300kPa, and the reaction time is 2.5-5.0h.

[0013] In a further embodiment, the pre-polymerization reaction temperature is 250-265℃, the reaction pressure is 100-1000Pa, and the reaction time is 1.0-2.5h; the amount of polyethylene glycol added is 2.5-10% of the mass fraction of terephthalic acid, and the polyethylene glycol is composed of polyethylene glycol with a relative number average molecular weight of 1000-4000g / mol and 12000-20000g / mol, with a mass ratio of 2:8-8:2.

[0014] In a further embodiment, the final polycondensation reaction temperature is 265-285℃, the reaction pressure is 0-100Pa, and the reaction time is 1.5-3.0h; the modified polyester prepared after the final polycondensation reaction has an intrinsic viscosity of 0.60-0.70dL / g and a terminal carboxyl group content of 10-20mol / t.

[0015] In a further embodiment, melt spinning employs a hollow-structured shaped spinneret, with a spinning speed of 2000-3200 m / min, and the spun fiber monofilament specifications are 0.5-3.0 dtex; the water treatment involves placing the spun fibers in a 0.1-0.5 mol / L sodium hydroxide aqueous solution at a temperature of 65-85℃ for 15-45 min.

[0016] An antibacterial and deodorizing polyester fiber prepared by the above preparation method: the fiber has a mechanical strength ≥3.0cN / dtex, an antibacterial rate of ≥95% against Candida albicans, Escherichia coli and Staphylococcus aureus, an isovaleric acid reduction rate ≥90%, and an ammonia reduction rate ≥85%.

[0017] The triethanolamine introduced in this invention is a monomer containing a trihydroxyl structure, which can participate in the polyester esterification reaction. Triethanolamine can undergo esterification with terephthalic acid to form a product with an esterified structure. The purpose of introducing triethanolamine is to enhance the strength of the final synthesized polyester melt, ensuring that the spun fibers still have good mechanical properties after water treatment. The amount of triethanolamine introduced is 0.01-0.1:1 relative to ethylene glycol. If the amount of triethanolamine introduced is too high, it will lead to severe crosslinking during the polyester synthesis stage, making it impossible to form and process. If the amount introduced is too low, the improvement in the melt strength of the polyester will be limited, and the mechanical properties of the spun fibers will decrease significantly after water treatment.

[0018] The g-C3N4 / X of this invention is an antibacterial material with excellent photocatalytic activity. It is a chelate formed by a semiconductor and a metal ion, wherein X is one or more of Ag+, Cu2+, or Fe3+. The mass fraction of g-C3N4 / X relative to terephthalic acid is 0.5-2.0%. Under light-free conditions, g-C3N4 / X can exert normal antibacterial function. Under visible light conditions, it can be excited to form a photoresponsive effect to enhance the antibacterial effect, achieving antibacterial and deodorizing effects. g-C3N4 / X is introduced into terephthalic acid and ethylene glycol for esterification together with triethanolamine, wherein triethanolamine plays a pre-dispersing role to prevent the agglomeration of g-C3N4 / X. When the amount of g-C3N4 / X added is too low, the antibacterial and deodorizing effect is limited and cannot meet the effective deodorizing function; when the content is too high, on the one hand, the dispersion requirements increase, the spinnability of the prepared polyester will be significantly affected, and the cost will increase.

[0019] This invention involves a mixture of triethanolamine, g-C3N4 / X, terephthalic acid, and ethylene glycol. After esterification, the mixture undergoes a polycondensation reaction, which is divided into two stages: pre-polymerization and final polycondensation. The pre-polymerization reaction is carried out under relatively low vacuum conditions to prevent the product from being carried out of the system along with the ethylene glycol, thus avoiding waste of raw materials and blockage of the vacuum pipeline. After the pre-polymerization reaction, the molecular weight of the product has increased to a certain extent. When it enters the high-vacuum tube for final polycondensation, the molecular weight continues to increase and will not be extracted due to the negative vacuum pressure. Without the pre-polymerization stage, the product and polyethylene glycol would directly enter the final polycondensation stage, easily causing blockage of the vacuum pipeline system.

[0020] This invention introduces a polyethylene glycol (PEG) component during the prepolymerization reaction stage, with the addition amount being 2.5-10% of the mass fraction of terephthalic acid. The PEG component consists of PEGs with a relative number average molecular weight of 1000-4000 g / mol and 12000-20000 g / mol, in a mass ratio of 2:8-8:2. The PEGs with relative number average molecular weights of 1000-4000 g / mol and 12000-20000 g / mol play different roles. The PEG with a relative number average molecular weight of 1000-4000 g / mol undergoes transesterification with the esterification reaction product and copolymerizes into the polyester backbone. The PEG with a relative number average molecular weight of 12000-20000 g / mol is blended into the polyester melt. When the functional polyester fibers obtained through melt spinning are treated with alkaline water, the polyethylene glycol (PEG) blended in the polyester dissolves and detaches from the fibers. The PEG copolymerized in the polyester enhances the hydrophilicity of the polyester, facilitating water penetration into the matrix and thus better dissolving the PEG blended within. This combination allows for the formation of microporous structures deep within the fiber surface, creating a pervasive connection with the hollow spun structure. This pervasive connection significantly enhances the adsorption rate and amount of odor molecules. Introducing only PEG with a number-average molecular weight of 1000-4000 g / mol improves the hydrophilicity of the fiber, but it is difficult to achieve micropore formation on the fiber surface during water treatment. Introducing only PEG with a number-average molecular weight of 12000-20000 g / mol allows micropores to form on the fiber surface during water treatment, but it is difficult to achieve a pervasive connection with the hollow structure.

[0021] The present invention has the following beneficial effects: This invention introduces different types of components at different stages of polyester synthesis. Triethanolamine and low molecular weight polyethylene glycol components are copolymerized, while g-C3N4 / X and high molecular weight polyethylene glycol are blended, each playing a different role. Ultimately, this achieves fibers with antibacterial and deodorizing functions while retaining their original mechanical properties.

[0022] This invention introduces modified substances with specific properties during the polyester synthesis stage, combined with fiber water treatment, to ultimately achieve a fiber structure with a through-linked connection. This structure enables rapid adsorption of small odor molecules and increases the adsorption capacity. It also facilitates the rapid decomposition of odor molecules by photoresponsive antibacterial components, thereby achieving deodorization of the fiber. Furthermore, this antibacterial and deodorizing function is permanent and will not diminish with washing or other usage conditions. Attached Figure Description

[0023] Figure 1 This is a flowchart of the preparation method of the present invention. Detailed Implementation

[0024] The principles and features of the present invention are described below with reference to the accompanying drawings. The examples given are only for explaining the present invention and are not intended to limit the scope of the present invention.

[0025] Example 1: Preparation of g-C3N4 / Ag⁺ antibacterial and deodorizing polyester fiber Preparation of g-C3N4 / Ag⁺: Place 10g of melamine into a covered alumina crucible, place it in a muffle furnace, heat it to 550℃ at a heating rate of 10℃ / min, keep it at that temperature for 3 hours, and grind it into powder after natural cooling. The powder was placed back into the muffle furnace and heated to 550°C at a heating rate of 3°C / min, and held for 3 hours to obtain powdered g-C3N4. Take 5g of powdered g-C3N4 / and disperse it in 2g of deionized water (40% of the mass fraction of g-C3N4) under ultrasonic conditions for 30 minutes; then add 0.3mol / L AgNO3 standard solution dropwise, stir for 4 hours, centrifuge, wash with deionized water and anhydrous ethanol three times alternately, and dry at 80℃ to constant weight to obtain g-C3N4 / Ag⁺.

[0026] Mixed slurry preparation: Weigh out 1 mol of terephthalic acid (166 g) and 1.3 mol of ethylene glycol (80.6 g) according to the molar ratio of terephthalic acid to ethylene glycol of 1:1.3. Weigh 0.065 mol of triethanolamine (11.7 g) according to a triethanolamine to ethylene glycol molar ratio of 0.05:1, mix it evenly with 0.83 g-C3N4 / Ag⁺ (relative to 0.5% terephthalic acid mass fraction), and then add it to the mixture of terephthalic acid and ethylene glycol. Add 0.0166g of tetrabutyl titanate (100ppm relative to terephthalic acid by mass) and stir to form a uniform slurry.

[0027] Esterification reaction: The mixed slurry was transferred into the esterification reactor, heated to 240°C, maintained at a reaction pressure of 200 kPa, and reacted for 3.5 hours until no condensate was generated, thus completing the esterification reaction.

[0028] Pre-condensation reaction: The esterification product was transferred into a prepolymerization reactor, evacuated to 500 Pa, heated to 260 °C, and reacted for 1.5 h. During the process, 8.3g of polyethylene glycol (5% relative to the mass fraction of terephthalic acid) was added. The polyethylene glycol was composed of polyethylene glycol with a number average molecular weight of 2000g / mol and 15000g / mol in a mass ratio of 4:6. The mixture was stirred until the reaction was complete.

[0029] Final condensation reaction: The prepolymerization product was transferred into the final polymerization reactor, evacuated to 50 Pa, heated to 275 °C, and reacted for 2.0 h to obtain the modified polyester. The modified polyester was tested and found to have an intrinsic viscosity of 0.65 dL / g and a terminal carboxyl group content of 15 mol / t.

[0030] Melt spinning and water treatment: A hollow-structured shaped spinneret was used to melt-spin modified polyester at a spinning speed of 2800 m / min, producing fibers with a single filament specification of 1.5 dtex. The spun fibers were placed in a 0.3 mol / L sodium hydroxide aqueous solution and treated at 75°C for 30 min. After washing and drying, antibacterial and deodorizing polyester fibers were obtained.

[0031] Performance testing: Mechanical strength: 3.2 cN / dtex; Antibacterial rate: 96.5% against Candida albicans, 97.2% against Escherichia coli, and 98.1% against Staphylococcus aureus; Deodorization rate: Isovalerate reduction rate 92.3%, ammonia reduction rate 87.5%.

[0032] Example 2: Preparation of g-C3N4 / Cu²⁺ antibacterial and deodorizing polyester fiber Preparation of g-C3N4 / Cu²⁺: Place 10g of melamine into a covered alumina crucible, heat it to 600℃ at a heating rate of 15℃ / min, hold it at that temperature for 2.5 hours, and grind it into powder after natural cooling. The powder was heated to 580℃ at a heating rate of 2℃ / min and held at that temperature for 2.5 hours to obtain powdered g-C3N4. Take 5g of powdered g-C3N4 and ultrasonically disperse it in 4g of deionized water (80% of the mass fraction of g-C3N4) for 45 minutes; add 0.4mol / L Cu(NO3)2 standard solution, stir for 5 hours, centrifuge, wash 3 times and dry to constant weight to obtain g-C3N4 / Cu²⁺.

[0033] Mixed slurry preparation: The molar ratio of terephthalic acid to ethylene glycol is 1:1.4. Weigh out 1 mol of terephthalic acid (166 g) and 1.4 mol of ethylene glycol (86.8 g). The molar ratio of triethanolamine to ethylene glycol is 0.08:1. Weigh 0.112 mol of triethanolamine (20.16 g), mix it with 3.32 g g-C3N4 / Cu²⁺ (relative to terephthalic acid mass fraction 2.0%), and add it to the system. Add 0.0332g of antimony glycol (200ppm relative to terephthalic acid mass fraction) and stir to form a slurry.

[0034] Esterification reaction: 245℃, 300kPa, reaction time 3.0h.

[0035] Pre-condensation reaction: vacuum degree 300Pa, 265℃, reaction time 1.0h; add 16.6g polyethylene glycol (relative to 10% of terephthalic acid mass fraction), which is composed of polyethylene glycol with a number average molecular weight of 3000g / mol and 18000g / mol in a mass ratio of 6:4.

[0036] Final polycondensation reaction: vacuum degree 30Pa, 280℃, reaction time 1.8h; modified polyester intrinsic viscosity 0.68dL / g, end carboxyl group content 12mol / t.

[0037] Melt spinning and water treatment: spinning speed 3000 m / min, single filament specification 2.0 dtex; 0.4 mol / L sodium hydroxide aqueous solution, treated at 80℃ for 25 min.

[0038] Performance testing: Mechanical strength: 3.1 cN / dtex; Antibacterial rate: 95.8% against Candida albicans, 96.7% against Escherichia coli, and 97.5% against Staphylococcus aureus; Deodorization rate: Isovalerate reduction rate 93.1%, ammonia reduction rate 88.2%.

[0039] Example 3: Preparation of g-C3N4 / Fe³⁺ antibacterial and deodorizing polyester fiber Preparation of g-C3N4 / Fe³⁺: Melamine was heated to 580°C at 8°C / min, held for 4 hours, cooled and ground, and then heated to 520°C at 4°C / min and held for 3 hours. 5g of powdered g-C3N4 was ultrasonically dispersed in 1.25g of deionized water (25% of g-C3N4 by mass) for 20 minutes; 0.2mol / L Fe(NO3)3 standard solution was added dropwise, and the mixture was stirred for 3 hours before centrifugation, washing, and drying.

[0040] Mixed slurry preparation: The molar ratio of terephthalic acid to ethylene glycol is 1:1.2, with 1 mol of terephthalic acid (166 g) and 1.2 mol of ethylene glycol (74.4 g). Triethanolamine and ethylene glycol in a molar ratio of 0.03:1, 0.036 mol of triethanolamine (6.48 g), and 1.66 g of C3N4 / Fe³⁺ (relative to 1.0% terephthalic acid mass fraction) were mixed. Add 0.00166g of titanium glycol (10ppm relative to terephthalic acid mass fraction).

[0041] Esterification reaction: 235℃, 100kPa, reaction time 4.0h.

[0042] Pre-condensation reaction: vacuum degree 800Pa, 255℃, reaction time 2.0h; add 4.15g polyethylene glycol (relative to terephthalic acid mass fraction 2.5%), which is composed of polyethylene glycol with a number average molecular weight of 1000g / mol and 12000g / mol in a mass ratio of 3:7.

[0043] Final polycondensation reaction: vacuum degree 80Pa, 270℃, reaction time 2.5h; modified polyester intrinsic viscosity 0.62dL / g, end carboxyl group content 18mol / t.

[0044] Melt spinning and water treatment: spinning speed 2500 m / min, single filament specification 1.0 dtex; 0.2 mol / L sodium hydroxide aqueous solution, treated at 70℃ for 40 min.

[0045] Performance testing: Mechanical strength: 3.3 cN / dtex; Antibacterial rate: 95.5% against Candida albicans, 96.3% against Escherichia coli, and 97.0% against Staphylococcus aureus; Deodorization rate: Isovalerate reduction rate 91.2%, ammonia reduction rate 86.8%.

[0046] Comparative Example 1: Preparation method without the addition of triethanolamine Except for the absence of triethanolamine in the mixed slurry, the other conditions were the same as in Example 1, and polyester fibers were prepared. Performance test results: mechanical strength 2.2 cN / dtex, antibacterial rate 94.8% (Staphylococcus aureus), isovaleric acid reduction rate 88.5%, ammonia reduction rate 83.2%; after 50 washes, the mechanical strength decreased to 1.8 cN / dtex, and the antibacterial rate decreased to 89.3%.

[0047] Comparative Example 2: Preparation method with only addition of polyethylene glycol of a single molecular weight Except for the addition of polyethylene glycol with a number average molecular weight of 2000 g / mol during the pre-polymerization stage, the other conditions were the same as in Example 1, and polyester fibers were prepared. Performance test results: mechanical strength 3.1 cN / dtex, antibacterial rate 95.2% (Staphylococcus aureus), isovaleric acid reduction rate 78.3%, ammonia reduction rate 75.6%; the fibers have no obvious through-hole microporous structure.

[0048] The above embodiments and comparative examples show that the present invention significantly improves the mechanical properties, antibacterial and deodorizing efficiency, and functional stability of fibers through the introduction of triethanolamine, the dual-functional design of polyethylene glycol, and synergistic optimization of the process. Its overall performance is superior to that of the prior art.

[0049] 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 antibacterial and deodorizing polyester fiber, characterized in that, The method comprises the following steps: S1: configuring a mixed slurry: mixing triethanolamine, g-C3N4 / X, terephthalic acid and ethylene glycol, wherein X is one or more of Ag+, Cu2+ or Fe3+; S2: sequentially performing reactions: the mixed slurry is subjected to esterification, then enters a pre-polycondensation reaction stage, and finally is subjected to a final polycondensation reaction, wherein the pre-polycondensation reaction stage introduces a polyethylene glycol component; S3: spinning and post-processing: the modified polyester prepared through the final polycondensation is subjected to a hollow special-shaped melt spinning process to obtain a fiber, and the fiber is subjected to water treatment to prepare an antibacterial and deodorizing polyester fiber with a micro-porous structure.

2. The method of making an antimicrobial deodorant polyester fiber according to claim 1, wherein, The molar ratio of terephthalic acid to ethylene glycol is 1:1.2-1.

5.

3. The method of making an antimicrobial deodorant polyester fiber according to claim 1, wherein, In the mixed slurry: the molar ratio of triethanolamine to ethylene glycol is 0.01-0.1:1; and the mass fraction of g-C3N4 / X to terephthalic acid is 0.5-2.0%.

4. The method of making an antimicrobial deodorant polyester fiber according to claim 1, wherein, The triethanolamine and g-C3N4 / X are mixed and then added to the terephthalic acid and ethylene glycol, and the mixed slurry contains a catalyst, wherein the catalyst is one or more of tetrabutyl titanate, titanium glycolate and antimony glycolate, and the mass fraction of the catalyst to terephthalic acid is 10-200 ppm.

5. The method of making an antimicrobial deodorant polyester fiber according to claim 1, wherein, The specific preparation process of g-C3N4 / X is as follows: S11: under the ambient pressure in air, melamine is placed in a covered crucible, heated to 500-650℃ at a heating rate of 5-20℃ / min in a muffle furnace, and kept for 2-5 hours to obtain blocky g-C3N4 / X; S12: after natural cooling, the blocky g-C3N4 / X is ground into powder, heated to 500-600℃ at a heating rate of 1-5℃ / min, and kept for 2-4 hours to obtain powder-like g-C3N4; S13: the powder-like g-C3N4 / X is dispersed in deionized water under ultrasonic conditions for 15-60 minutes, wherein the mass of the deionized water is 25-80% of the mass of the g-C3N4 / X; then 0.1-0.5 mol / L of AgNO3, Cu(NO3)2 or Fe(NO3)3 standard solution is added dropwise, stirred for 3-6 hours, centrifuged, washed with deionized water and anhydrous ethanol for 3 times, and finally dried to constant weight.

6. The method of making an antimicrobial deodorant polyester fiber according to claim 1, wherein, The temperature of the esterification reaction is 235-245℃, the reaction pressure is 0-300 kPa, and the reaction time is 2.5-5.0 hours.

7. The method of making an antimicrobial deodorant polyester fiber according to claim 1, wherein, The temperature of the pre-polycondensation reaction is 250-265℃, the reaction pressure is 100-1000 Pa, and the reaction time is 1.0-2.5 hours; the addition amount of the polyethylene glycol is 2.5-10% of the mass fraction of terephthalic acid, and the polyethylene glycol is composed of polyethylene glycol with a relative number-average molecular weight of 1000-4000 g / mol and 12000-20000 g / mol, and the mass ratio of the two is 2:8-8:

2.

8. The method of making an antimicrobial deodorizing polyester fiber according to claim 1, wherein, The temperature of the final polycondensation reaction is 265-285℃, the reaction pressure is 0-100 Pa, and the reaction time is 1.5-3.0 hours; after the final polycondensation reaction, the modified polyester prepared has a specific viscosity of 0.60-0.70 dL / g and a carboxyl end group content of 10-20 mol / t.

9. The method of making an antimicrobial deodorant polyester fiber according to claim 1, wherein, The melt spinning uses a hollow structure of a special-shaped spinneret, the spinning speed is 2000-3200 m / min, and the spun fiber single filament specification is 0.5-3.0 dtex; the water treatment is to place the spun fiber in a 0.1-0.5 mol / L sodium hydroxide aqueous solution for treatment, the treatment temperature is 65-85 ℃, and the treatment time is 15-45 min.

10. An antibacterial deodorizing polyester fiber, characterized by, Prepared by the preparation method of any one of claims 1-9.

Citation Information

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