Preparation method of polyester fiber and preparation method of catalyst

By preparing iron-doped zinc sulfide nano powder combined with polyester fiber, the safety hazards and high cost of existing antibacterial and UV fibers are solved, low-cost and efficient antibacterial and UV functions and harmful gas decomposition are achieved, and the competitiveness of textiles is enhanced.

CN119640432BActive Publication Date: 2025-07-01JIANGSU RUIBANG TECH CO LTD
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Patent Information

Application Number
CN202510167721.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-02-17
Publication Date
2025-07-01
Estimated Expiration
2045-02-17

AI Technical Summary

Technical Problem

The existing antibacterial and UV-resistant functional fibers have safety hazards, high costs, serious pollution and poor washing resistance, and cannot effectively remove harmful gases such as formaldehyde. The traditional post-tire finishing process affects the competitiveness of textiles.

Method used

The zinc oxide and sulfur source are used to react with trivalent iron compounds in a mixed solvent of ethylenediamine and ethanolamine to prepare iron-doped zinc sulfide nanopowders. By in-situ polymerization, they form antibacterial and anti-UV functional fibers, and use photon downconversion to achieve ultraviolet absorption and visible light emission, and decompose harmful gases.

Benefits of technology

It realizes safe and low-cost antibacterial and anti-ultraviolet functions, can effectively decompose harmful gases such as formaldehyde, reduce catalyst use, reduce pollution, and enhance the competitiveness and added value of textiles.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to a preparation method of polyester fiber and a preparation method of a catalyst. The preparation method of polyester fiber includes: (1) First, zinc oxide and a sulfur source are dissolved in a mixed solvent of ethylenediamine and ethanolamine, and then an organic acid and an iron-containing compound are added, and a functional powder is obtained by reaction. The iron in the iron-containing compound is trivalent iron, and the reaction temperature is controlled at 180-220 °C during the reaction; (2) The functional powder obtained in step (1) is mixed with polyester raw materials for in-situ polymerization reaction to obtain functional polyester chips, and then melt spinning is carried out to obtain polyester fibers. The polyester fibers prepared by the preparation method of polyester fiber of the present invention can realize the function of absorbing ultraviolet rays and emitting visible light through photon down-conversion, which can compensate for the human body's demand for visible light. After the polyester fibers are woven into fabrics, they have the function of decomposing formaldehyde, acetaldehyde, and propionaldehyde.
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Description

Technical Field

[0001] The present invention belongs to the field of polyester production, and particularly relates to a method for preparing polyester fibers and a method for preparing a catalyst. Background Art

[0002] Antibacterial and anti-ultraviolet functional materials have always been an important product in the functional development of chemical fiber fabrics and an important direction for the application and development of outdoor fabric products. At present, there are already some solutions, such as solving from the origin of the fiber, and antibacterial and anti-ultraviolet fibers can be prepared. For example, antibacterial and anti-ultraviolet functional fibers are prepared by using high addition amounts and composite spinning technologies, and nano zinc oxide, titanium dioxide or rare earths are used as functional additive materials to obtain functional fibers by melt spinning. Fabrics prepared from these fibers can meet the antibacterial and anti-ultraviolet requirements of the fabrics. However, such fibers also have irreparable defects as follows: First, the use of rare earth powders has the risk of radiation, and some rare earths have biological toxicity, so there are safety hazards in use; Second, simply adding zinc-based, silver-based and titanium dioxide in combination to obtain antibacterial and anti-ultraviolet functions, the high addition amount of zinc-based affects the spinning performance, and the addition cost of silver-based is high.

[0003] Currently, most fabrics on the market achieve the functions of the fabrics by antibacterial and anti-ultraviolet after-treatment. For example, organic antibacterial agents such as quaternary ammonium salts are used in combination with anti-ultraviolet auxiliaries. This method has a lower cost and more significant effects compared with using antibacterial and anti-ultraviolet functional fibers. However, although this method is inexpensive and effective, it also has inevitable defects: (1) additional pollution. Currently, antibacterial and anti-ultraviolet auxiliaries are generally used for after-treatment, which increases the pollution degree of wastewater and also increases the difficulty of wastewater treatment; (2) insufficient durability. The currently used antibacterial and anti-ultraviolet functional after-treatment methods have poor wash resistance, and generally few can meet the standard requirements of wash resistance, which is not conducive to the export of textiles, reduces the competitive advantage of textiles, and increases disputes in trade.

[0004] The existing antibacterial and anti-ultraviolet functional materials on the market cannot remove formaldehyde, have low added value, and some fabrics contain heavy metal elements, posing safety hazards. Summary of the Invention

[0005] The purpose of the present invention is to provide a method for preparing polyester fibers and a method for preparing a catalyst. The prepared polyester fibers can decompose formaldehyde, have antibacterial and anti-ultraviolet properties, are safe and non-toxic, and have high cost performance.

[0006] To achieve the above object, a technical solution adopted by the present invention is:

[0007] A method for preparing polyester fibers, comprising:

[0008] (1) First, dissolve zinc oxide and a sulfur source in a mixed solvent of ethylenediamine and ethanolamine, then add an organic acid and an iron-containing compound, and react to obtain a functional powder. The iron in the iron-containing compound is trivalent iron, and the reaction temperature is controlled at 180 - 220 °C during the reaction;

[0009] (2) Mix the functional powder obtained in step (1) with a polyester raw material for an in-situ polymerization reaction to obtain a functional polyester chip, and then perform melt spinning to obtain polyester fibers.

[0010] According to some embodiments of the present invention, in step (1), the sulfur source includes sulfur powder.

[0011] According to some embodiments of the present invention, in step (1), the iron-containing compound is a combination of one or more selected from ferric chloride or ferric sulfate.

[0012] According to a preferred embodiment of the present invention, in step (1), the iron-containing compound is ferric chloride hexahydrate. After the iron ions in ferric chloride hexahydrate dissociate during the reaction, under high temperature and high pressure conditions, hydrochloric acid can exist in a gaseous state.

[0013] According to some embodiments of the present invention, in step (1), the addition amount of the iron-containing compound is 0.2 - 2% of the sum of the masses of the zinc oxide and the sulfur source.

[0014] According to some embodiments of the present invention, in step (1), the organic acid is a combination of one or more selected from oxalic acid and acetic acid; the mixed solution of the added organic acid and the iron-containing compound is neutral or weakly acidic.

[0015] According to a preferred embodiment of the present invention, in step (1), the organic acid is oxalic acid.

[0016] Since amine substances are used in the preparation, it is known that amine substances (the surface of the functional powder is negatively charged with amino groups) will attack the ester bonds in the polyester to break the chain, resulting in a decrease in the degree of polymerization, and accelerating the degradation of polyester macromolecules during subsequent processing and use. Therefore, an organic acid is added to the solvent. The organic acid reacts with the -NH group in the amine substance to generate an amide bond, and adjusts the dissolution pH of the functional powder to neutral or weakly acidic, improving the compatibility and mechanical properties with the polyester resin.

[0017] According to some embodiments of the present invention, the addition amount of the organic acid is 0.05 - 0.2% of the sum of the masses of the zinc oxide and the sulfur source.

[0018] According to some embodiments of the present invention, in step (1), the mixed solvent of ethylenediamine and ethanolamine is beneficial to the synthesis of zinc sulfide (ZnS) and does not produce side reactions.

[0019] According to a preferred embodiment of the present invention, in step (1), the mass ratio of ethylenediamine to ethanolamine is (1:2)-(2:1). Preferably, the mass ratio of ethylenediamine to ethanolamine is 1:1.

[0020] According to some embodiments of the present invention, in step (1), the mass fraction of zinc oxide and sulfur source dissolved in the mixed solvent of ethylenediamine and ethanolamine is 5-25%.

[0021] According to some embodiments of the present invention, in step (1), zinc oxide and sulfur source are dissolved in a mixed solvent of ethylenediamine and ethanolamine in a certain proportion. A certain amount of organic acid is added to the mixed solvent. After magnetic stirring of the mixture, an iron-containing compound is added to the mixture, and the mixture is stirred and then transferred to a stainless steel autoclave with a polytetrafluoroethylene liner and stirred continuously. After sealing, the autoclave is heated to 180-220 °C and maintained at this temperature for 12-36 h, and then naturally cooled to room temperature. The precipitate is collected, washed several times with absolute ethanol and deionized water, and finally dried in a vacuum oven at a drying temperature of 50-100 °C for a drying time of 5-8 h.

[0022] According to a preferred embodiment of the present invention, in step (1), it is dried in a vacuum oven at 60 °C for 6 h.

[0023] According to a preferred embodiment of the present invention, in step (1), the reaction temperature is controlled to be 180-200 °C during the reaction.

[0024] According to a preferred embodiment of the present invention, in step (1), the pressure in the autoclave is 1-7.5 atmospheres.

[0025] According to some embodiments of the present invention, in step (2), the polyester raw materials include polyols and polyacids. First, the functional powder prepared in step (1) is prepared into nano-powder by liquid-phase grinding and dispersed in a polyol medium. Then, titanate esters are added as surface modifiers and dispersants to improve its dispersibility to obtain a blend. Then, the blend is subjected to in-situ polymerization with polyols and polyacids to obtain functional polyester chips.

[0026] According to some embodiments of the present invention, in step (2), the polyol includes ethylene glycol; the grinding is carried out using a liquid-phase ball milling device, the grinding time is 6-12 h, the particle size of the ground functional powder is 3-30 nm, and the mass fraction of the functional powder is 5-20%; the addition amount of the titanate ester surface modifier is 1-3% of the powder mass.

[0027] According to a preferred embodiment of the present invention, in step (2), the particle size of the ground functional powder is less than 10 nm.

[0028] According to some implementation aspects of the present invention, in step (2), the in-situ polymerization includes: first mixing the blend with ethylene glycol, and then performing in-situ polymerization with terephthalic acid to obtain functional polyester chips, wherein ethylene glycol and terephthalic acid are used as polymerization monomers, and nano-titanium dioxide is used as a catalyst for catalytic polymerization.

[0029] According to some implementation aspects of the present invention, in step (2), the polymerization is divided into prepolymerization, post-condensation polymerization, and final polymerization. The prepolymerization temperature is 170 - 200 °C, and the time is 40 - 80 min; the post-condensation polymerization temperature is 230 - 270 °C, and the time is 1 - 3 h; the final polymerization temperature is 260 - 290 °C, and the time is 1 - 4 h.

[0030] According to some implementation aspects of the present invention, in step (2), the molar ratio of ethylene glycol (the mixture of ethylene glycol and the blend) mixed with the blend to terephthalic acid is (1 - 1.2):1.

[0031] According to some implementation aspects of the present invention, in step (2), the mass fraction of the functional powder in the polyester chips is 0.1% - 2%, preferably 0.1 - 1.6%.

[0032] According to some implementation aspects of the present invention, in step (2), the dried polyester chips are fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 260 - 300 °C, the spinning speed is 600 - 3000 m / min, and the initial pressure of the spinning pack is 8 - 16 MPa.

[0033] According to some implementation aspects of the present invention, in step (2), the spinning temperature is 285 °C, and the spinning speed is 2800 m / min.

[0034] According to some implementation aspects of the present invention, in step (2), the molecular weight of the functional polyester chips is 20000 - 30000.

[0035] According to some implementation aspects of the present invention, in step (2), the molecular weight of the functional polyester chips is 23000 - 26000.

[0036] According to some implementation aspects of the present invention, in step (2), white / light-colored polyester fibers are prepared; the fineness of the single filament of the polyester fiber is 0.5 - 5 D.

[0037] Another technical solution adopted by the present invention is:

[0038] A preparation method of a catalyst includes: first dissolving zinc oxide and a sulfur source in a mixed solvent of ethylenediamine and ethanolamine, and then adding an organic acid and an iron-containing compound to react to obtain a functional powder, wherein the iron in the iron-containing compound is trivalent iron, and the reaction temperature is controlled at 180 - 220 °C during the reaction.

[0039] Another technical solution adopted by the present invention is as follows:

[0040] The catalyst prepared by the above-mentioned catalyst preparation method is applied to the preparation of polyester fibers.

[0041] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art:

[0042] In the preparation method of the polyester fiber of the present invention, first, an iron-doped zinc sulfide nano-functional powder is obtained. Iron exists in the form of surface modification groups on the surface of the nano-material. Among them, zinc sulfide can shield ultraviolet rays, and iron has antibacterial functions; the surface of the functional powder contains amino groups (NH groups), and organic acids react with amino groups to produce amide bonds. After the reaction, the pH of the functional powder can be adjusted without harming polyester; moreover, no complex is formed between iron ions and amino groups, and iron ions are doped into the zinc sulfide crystal lattice, which is beneficial to subsequent polyester polymerization. The molecular weight of the subsequent obtained functional polyester is suitable, and the antibacterial effect is better; and after doping with iron ions, the lattice defects of the zinc sulfide nano-material are increased. At the same time, the doping of trivalent iron ions increases the redox potential of zinc sulfide, and it is easy to generate singlet oxygen under the excitation of light, heat, etc., and decompose organic harmful gases such as formaldehyde, acetaldehyde, and propionaldehyde through oxidation.

[0043] The polyester fiber prepared by the preparation method of the polyester fiber of the present invention has a dual anti-ultraviolet function of shielding and converting ultraviolet rays, and realizes the function of absorbing ultraviolet rays and emitting visible light through photon down-conversion. The human body can absorb visible light, which is beneficial to the absorption of vitamin D and calcium, and can compensate for the human body's demand for visible light; the polyester fiber woven into a fabric has the function of decomposing formaldehyde, acetaldehyde, and propionaldehyde; the functional powder can play a role in catalytic polymerization in in-situ polymerization, reducing the use of catalysts; the mechanical properties of the polyester fiber reach the standards of ordinary fibers and fully meet the requirements of various weavings; compared with the currently used antibacterial and anti-ultraviolet fibers, the cost is reduced by 70%, and the cost is lower than the post-finishing process; pollution is reduced. Description of the Drawings

[0044] Appendix Figure 1 It is the excitation spectrum of the polyester fiber of Example 16;

[0045] Appendix Figure 2 It is the emission spectrum of the polyester fiber of Example 16 under illumination with different excitation wavelengths;

[0046] Appendix Figure 3 It is the fluorescence image of the polyester fiber of Example 16. Detailed Embodiments

[0047] The present invention will be further described below in conjunction with the shown embodiments.

[0048] Unless otherwise specified in the following examples, all raw materials are commercially available or prepared by conventional methods in the art.

[0049] Example 1

[0050] (1) Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) were dissolved in a mixed solvent of ethylenediamine and ethanolamine at a molar ratio of 1:1, and the mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine was 5%; 0.05% oxalic acid by mass was added to the mixed solution, and after the mixture was magnetically stirred for 10 min, 0.2% of ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder was added to the mixture, and the mixture was stirred for 15 min, then transferred to a stainless steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, within 30 min, the autoclave was heated to 180 °C and maintained at this temperature for 24 h, and finally naturally cooled to room temperature; the precipitate was collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0051] (2) Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) was prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium, and then titanate was added as a surface modifier and dispersant to improve its dispersibility to obtain a blend, where the addition amount of titanate was 1% of the mass of the functional powder prepared in step (1), the mass fraction of the functional powder prepared in step (1) in ethylene glycol medium was 10%, and the grinding time was 6 h;

[0052] (3) Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder dispersed in step (2) was added to ethylene glycol to form a mixture, and then in-situ polymerization was carried out with terephthalic acid at a molar ratio of 1.05 - 1, where the pre-polymerization temperature was 180 °C and the time was 60 min; the post-polycondensation temperature was 255 °C and the time was 2 h; the final polycondensation temperature was 275 °C and the time was 2 h; the mass fraction of the functional powder in the polyester chips was 0.1%;

[0053] (4) Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips were dried and then fed into the feeder of the spinning machine for melt spinning. The spinning temperature was 285 °C, the spinning speed was 2800 m / min, and the initial pressure of the spinning pack was 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0054] Example 2

[0055] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine in a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 10%; 0.1% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.4% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, the autoclave is heated to 180 °C within 30 min and maintained at this temperature for 24 h, and finally cooled naturally to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0056] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility to obtain a blend, where the addition amount of titanate is 1% of the mass of the functional powder prepared in step (1), the mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 10%, and the grinding time is 6 h;

[0057] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid in a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0058] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0059] Example 3

[0060] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine according to a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 15%; 0.15% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, ferric chloride hexahydrate (FeCl3·6H2O) accounting for 0.6% of the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, the autoclave is heated to 180 °C within 30 min and maintained at this temperature for 24 h, and finally naturally cooled to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0061] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility, and a blend is obtained. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 10%, and the grinding time is 6 h;

[0062] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerization is carried out with terephthalic acid according to a molar ratio of 1.05:1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0063] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0064] Example 4

[0065] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine according to a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 180 °C and maintained at this temperature for 24 h, and finally naturally cooled to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0066] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility, and a blend is obtained. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction concentration of the functional powder prepared in step (1) in the ethylene glycol medium is 10%, and the grinding time is 6 h;

[0067] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerization is carried out with terephthalic acid according to a molar ratio of 1.05:1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-condensation temperature is 255 °C and the time is 2 h; the final condensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0068] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0069] Example 5

[0070] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine according to a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 25%; 0.25% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, ferric chloride hexahydrate (FeCl3·6H2O) with a mass of 1% of the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min, and then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, the autoclave is heated to 180 °C within 30 min and maintained at this temperature for 24 h, and finally naturally cooled to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0071] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility, and a blend is obtained. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction concentration of the functional powder prepared in step (1) in the ethylene glycol medium is 10%, and the grinding time is 6 h;

[0072] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid according to a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0073] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0074] Example 6

[0075] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine according to a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 200 °C and maintained at this temperature for 18 h, and finally cooled naturally to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0076] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility, obtaining a blend. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 10%, and the grinding time is 6 h;

[0077] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid according to a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0078] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0079] Example 7

[0080] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine in a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, the autoclave is heated to 220 °C within 30 min and maintained at this temperature for 12 h, and finally cooled naturally to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0081] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility to obtain a blend. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 10%, and the grinding time is 6 h;

[0082] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid in a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0083] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0084] Example 8

[0085] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine in a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 200 °C and maintained at this temperature for 18 h, and finally naturally cooled to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0086] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility, and a blend is obtained. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 5%, and the grinding time is 6 h;

[0087] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid in a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0088] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0089] Example 9

[0090] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine in a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 200 °C and maintained at this temperature for 18 h, and finally naturally cooled to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0091] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, a titanate is added as a surface modifier and dispersant to improve its dispersibility, and a blend is obtained. The addition amount of the titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 15%, and the grinding time is 6 h;

[0092] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid in a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-condensation temperature is 255 °C and the time is 2 h; the final polymerization temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0093] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0094] Example 10

[0095] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine at a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min, then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene, and stirred for another 15 min. After sealing, the autoclave is heated to 200 °C within 30 min and maintained at this temperature for 18 h, and finally cooled naturally to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h;

[0096] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is ground into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility, and a blend is obtained. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 20%, and the grinding time is 6 h;

[0097] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid at a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0098] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa, obtaining antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0099] Example 11

[0100] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine at a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 200 °C and maintained at this temperature for 18 h, and finally naturally cooled to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0101] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is ground into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility, and a blend is obtained. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 15%, and the grinding time is 8 h;

[0102] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerization is carried out with terephthalic acid at a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0103] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0104] Example 12

[0105] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine at a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 200 °C and maintained at this temperature for 18 h, and finally naturally cooled to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0106] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility to obtain a blend, where the addition amount of titanate is 1% of the mass of the functional powder prepared in step (1), the mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 10%, and the grinding time is 10 h;

[0107] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid at a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.1%;

[0108] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0109] Example 13

[0110] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine at a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After magnetically stirring the mixture for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 200 °C and maintained at this temperature for 18 h, and finally cooled naturally to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0111] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is ground into nano-powder by liquid grinding and dispersed in ethylene glycol medium, and then titanate is added as a surface modifier and dispersant to improve its dispersibility to obtain a blend, where the addition amount of titanate is 1% of the mass of the functional powder prepared in step (1), the mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 15%, and the grinding time is 8 h;

[0112] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerization is carried out with terephthalic acid at a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.2%;

[0113] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0114] Example 14

[0115] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine according to a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 200 °C and maintained at this temperature for 18 h, and finally naturally cooled to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0116] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, a titanate is added as a surface modifier and dispersant to improve its dispersibility to obtain a blend. The addition amount of the titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 15%, and the grinding time is 8 h;

[0117] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid according to a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.4%;

[0118] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0119] Example 15

[0120] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine in a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur source in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% of ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, the autoclave is heated to 200 °C within 30 min and maintained at this temperature for 18 h, and finally cooled to room temperature naturally; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h;

[0121] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is ground into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility, and a blend is obtained. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 15%, and the grinding time is 8 h;

[0122] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerization is carried out with terephthalic acid in a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-condensation temperature is 255 °C and the time is 2 h; the final polymerization temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 0.8%;

[0123] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa, obtaining antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0124] Example 16

[0125] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine according to a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 200 °C and maintained at this temperature for 18 h, and finally cooled to room temperature naturally; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0126] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility to obtain a blend, where the addition amount of titanate is 1% of the mass of the functional powder prepared in step (1), the mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 15%, and the grinding time is 8 h;

[0127] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid according to a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-condensation temperature is 255 °C and the time is 2 h; the final polymerization temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 1.2%;

[0128] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0129] Example 17

[0130] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine according to a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution. After the mixture is magnetically stirred for 10 min, 0.8% ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder is added to the mixture. The mixture is stirred for 15 min, and then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, within 30 min, the autoclave is heated to 200 °C and maintained at this temperature for 18 h, and finally naturally cooled to room temperature; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0131] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate is added as a surface modifier and dispersant to improve its dispersibility, and a blend is obtained. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 15%, and the grinding time is 8 h;

[0132] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid according to a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 1.6%;

[0133] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0134] Comparative Example 1

[0135] This example is different from Example 16 in that oxalic acid and ferric chloride hexahydrate are not added, as follows.

[0136] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine in a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; the mixture is stirred for 15 min, and then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, the autoclave is heated to 200 °C within 30 min and maintained at this temperature for 18 h, and finally cooled to room temperature naturally; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain the functional powder;

[0137] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is ground into nano-powder by liquid grinding and dispersed in ethylene glycol medium, and then titanate is added as a surface modifier and dispersant to improve its dispersibility, obtaining a blend. The addition amount of titanate is 1% of the mass of the functional powder prepared in step (1), the mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 15%, and the grinding time is 8 h;

[0138] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid in a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chip is 1.2%;

[0139] (4)Spinning: The polyester chip with antibacterial and ultraviolet-absorbing and visible-light-emitting functions is dried and then fed into the feeder of the spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain polyester fibers.

[0140] Comparative Example 2

[0141] This example is different from Example 16 in that oxalic acid is not added, as follows.

[0142] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) were dissolved in a mixed solvent of ethylenediamine and ethanolamine at a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine was 20%; then, hexahydrate chloride (FeCl3·6H2O) with a molar ratio of 0.8% of the sum of the masses of zinc oxide and sulfur powder was added to the mixture. The mixture was stirred for 15 min, and then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, within 30 min, the autoclave was heated to 200 °C and maintained at this temperature for 18 h, and finally cooled to room temperature naturally; the precipitate was collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0143] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) was prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate was added as a surface modifier and dispersant to improve its dispersibility to obtain a blend. The addition amount of titanate was 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in ethylene glycol medium was 15%, and the grinding time was 8 h;

[0144] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The dispersed antibacterial and ultraviolet-absorbing and visible-light-emitting functional nano-powder ethylene glycol blend was added to ethylene glycol to form a mixture, and then in-situ polymerized with terephthalic acid at a molar ratio of 1.05-1. The pre-polymerization temperature was 180 °C and the time was 60 min; the post-polycondensation temperature was 255 °C and the time was 2 h; the final polycondensation temperature was 275 °C and the time was 2 h; the mass fraction of the functional powder in the polyester chips was 1.2%;

[0145] (4)Spinning: The polyester chips with antibacterial and ultraviolet-absorbing and visible-light-emitting functions were dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature was 285 °C, the spinning speed was 2800 m / min, and the initial pressure of the spinning pack was 9 MPa to obtain polyester fibers.

[0146] Comparative Example 3

[0147] This example is different from Example 16 in that ferric chloride hexahydrate was not added, as follows.

[0148] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) are dissolved in a mixed solvent of ethylenediamine and ethanolamine in a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine is 20%; 0.2% oxalic acid by mass is added to the mixed solution, and the mixture is magnetically stirred for 10 min, and then transferred to a stainless-steel autoclave with a polytetrafluoroethylene liner and stirred for another 15 min; after sealing, the autoclave is heated to 200 °C within 30 min and maintained at this temperature for 18 h, and finally cooled to room temperature naturally; the precipitate is collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain the functional powder;

[0149] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) is prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium, and then titanate is added as a surface modifier and dispersant to improve its dispersibility to obtain a blend, where the addition amount of titanate is 1% of the mass of the functional powder prepared in step (1), the mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium is 15%, and the grinding time is 8 h;

[0150] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder dispersed in step (2) is added to ethylene glycol to form a mixture, and then in-situ polymerization is carried out with terephthalic acid in a molar ratio of 1.05 - 1. The pre-polymerization temperature is 180 °C and the time is 60 min; the post-polycondensation temperature is 255 °C and the time is 2 h; the final polycondensation temperature is 275 °C and the time is 2 h; the mass fraction of the functional powder in the polyester chips is 1.2%;

[0151] (4)Spinning: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester chips are dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature is 285 °C, the spinning speed is 2800 m / min, and the initial pressure of the spinning pack is 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0152] Comparative Example 4

[0153] This example is different from Example 16 in that: ethylenediamine is not added, specifically as follows.

[0154] (1)Preparation of functional powder: Zinc oxide (ZnO) and sulfur powder (S) were dissolved in a solvent of ethanolamine according to a molar ratio of 1:1. The mass fraction of zinc oxide and sulfur powder in the mixed solvent of ethylenediamine and ethanolamine was 20%; 0.2% oxalic acid by mass was added to the mixed solution. After the mixture was magnetically stirred for 10 min, 0.8% of ferric chloride hexahydrate (FeCl3·6H2O) based on the sum of the masses of zinc oxide and sulfur powder was added to the mixture. The mixture was stirred for 15 min and then transferred to a stainless-steel autoclave lined with polytetrafluoroethylene and stirred for another 15 min; after sealing, within 30 min, the autoclave was heated to 200 °C and maintained at this temperature for 18 h, and finally cooled to room temperature naturally; the precipitate was collected, washed 3 times with absolute ethanol and deionized water, and dried in a vacuum oven at 60 °C for 6 h to obtain iron-doped zinc sulfide functional powder;

[0155] (2)Grinding and dispersion of functional powder: The antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder prepared in step (1) was prepared into nano-powder by liquid grinding and dispersed in ethylene glycol medium. Then, titanate was added as a surface modifier and dispersant to improve its dispersibility, and a blend was obtained. The addition amount of titanate was 1% of the mass of the functional powder prepared in step (1). The mass fraction of the functional powder prepared in step (1) in the ethylene glycol medium was 15%, and the grinding time was 8 h;

[0156] (3)Preparation of antibacterial and ultraviolet-absorbing and visible-light-emitting functional polyester by in-situ polymerization: The ethylene glycol blend of the antibacterial and ultraviolet-absorbing and visible-light-emitting functional powder dispersed in step (2) was added to ethylene glycol to form a mixture, and then in-situ polymerization was carried out with terephthalic acid according to a molar ratio of 1.05 - 1. The pre-polymerization temperature was 180 °C and the time was 60 min; the post-polycondensation temperature was 255 °C and the time was 2 h; the final polycondensation temperature was 275 °C and the time was 2 h; the mass fraction of the functional powder in the polyester chips was 1.2%;

[0157] (4)Spinning: The polyester chips with antibacterial and ultraviolet-absorbing and visible-light-emitting functions were dried and then fed into the feeder of a spinning machine for melt spinning. The spinning temperature was 285 °C, the spinning speed was 2800 m / min, and the initial pressure of the spinning pack was 9 MPa to obtain antibacterial and ultraviolet-absorbing and visible-light-emitting polyester fibers.

[0158] Performance testing

[0159] The particle sizes of the functional powders in step (1) of Examples 1-17 and Comparative Examples 1-4 were tested by a laser particle size analyzer. The antibacterial effects of the polyester fibers in Examples 1-17 and Comparative Examples 1-4 against Escherichia coli, Staphylococcus aureus, and Candida albicans / light-colored Candida were tested. The effects of absorbing ultraviolet light and emitting visible light were tested, and the fabrics woven were tested for formaldehyde removal. Among them, the antibacterial and ultraviolet light absorption and visible light emission effects of the prepared fibers were tested according to the test standard of GB / T 20944.3-2008, and the formaldehyde test was carried out according to JC / T 1004-2008.

[0160] The particle size of the functional powder and the absorption spectrum data and emission spectrum data of the polyester fibers in Examples 1-17 and Comparative Examples 1-4 are shown in Table 1 below:

[0161]

[0162] In Examples 1-5, the mass fraction of zinc oxide and sulfur powder dissolved in the mixed solvent of ethylenediamine and ethanolamine in Example 4 was 20%, and the obtained nano-functional powder had the smallest particle size and the best effect.

[0163] In Example 7, when the reaction temperature in step (1) was too high, the reaction rate increased, but the particle size of the generated functional powder increased instead. Compared with Example 6, the antibacterial effect decreased. The optimal reaction temperature was 200 °C and the reaction time was 18 h.

[0164] In Example 8, compared with Example 7, reducing the grinding concentration (the mass fraction of the functional powder prepared in step (1) dispersed into the ethylene glycol medium by liquid grinding) was beneficial to reducing the particle size of the powder. It was preferred to use a relatively high concentration for grinding, and the production efficiency was high.

[0165] In Example 10, compared with Example 9, increasing the grinding concentration (the mass fraction of the functional powder prepared in step (1) dispersed into the ethylene glycol medium by liquid grinding) increased the particle size of the powder instead, and the antibacterial and ultraviolet resistance decreased. Therefore, the grinding concentration was set at 15% as the best.

[0166] In Example 12, compared with Example 11, increasing the grinding time in step (2) did not change the particle size, indicating that the particle size had reached the lowest at this time. Considering the working efficiency, the grinding time was set at 8 h as the best.

[0167] The fabric woven in Example 16 was tested for formaldehyde removal, and the test was carried out according to JC / T 1004-2008. The formaldehyde removal efficiency was 87%. After iron ion doping, the lattice defects of the zinc sulfide nanomaterial were increased, and at the same time, the doping of trivalent iron ions increased the redox potential of zinc sulfide, which was easily excited by light and heat to generate singlet oxygen, and decomposed organic harmful gases such as formaldehyde, acetaldehyde, and propionaldehyde through oxidation.

[0168] In Example 17, when the content of nano-functional powder in the polyester chip was continuously increased, the antibacterial efficiency remained basically unchanged, the anti-ultraviolet performance increased insignificantly, and the increase of inorganic functional powder would affect the spinning efficiency and fiber mechanical properties, increasing the fiber cost. Therefore, the mass fraction of functional powder in the polyester chip was preferably 1.2%.

[0169] In Step (2) of Comparative Example 1, the molecular weight of the functional polyester obtained was 21,000, and the polyester molecular weight was relatively low, resulting in floating filaments during spinning.

[0170] In Comparative Example 2, since the pH of the system was not adjusted, complexation occurred between iron ions and amino groups, resulting in only partial participation of iron ions in zinc sulfide doping. Therefore, it had an impact on both the antibacterial effect and polyester polymerization, and the molecular weight was relatively low. The molecular weight of the functional polyester obtained in Step (2) was 20,000, and the polyester molecular weight was relatively low, resulting in floating filaments during spinning.

[0171] The formaldehyde removal efficiency of the fabric woven in Comparative Example 2 was less than that of the fabric woven in Example 16. Compared with Examples 1 - 12, the mass fraction of the functional powder in the polyester chip of Comparative Example 2 was relatively large, and the formaldehyde removal efficiency was relatively high.

[0172] In Comparative Example 3, oxalic acid was added, and oxalic acid reacted with the amino groups on the surface of the functional powder, resulting in a decrease in its antibacterial performance; however, the addition of oxalic acid prevented agglomeration, and the particle size of the functional powder decreased. The anti-ultraviolet performance of Comparative Example 3 was better than that of Comparative Example 1.

[0173] In addition, the reason why the polyesters of Comparative Example 1 and Comparative Example 3 had no formaldehyde removal efficiency was that: ferric chloride hexahydrate was not added in both Comparative Example 1 and Comparative Example 3. The iron-doped zinc sulfide functional powder had a photocatalytic degradation function and thus had a formaldehyde removal function. Zinc sulfide was a kind of quantum dot with a light conversion function, which could absorb ultraviolet light and convert it into visible light. After being doped with iron elements, the lattice of the zinc sulfide nanopowder had defects to form holes. At this time, it could absorb ultraviolet light and visible light to act on oxygen in the air to form free radicals. The oxygen free radicals had an oxidation function and could decompose formaldehyde in the air, thus endowing the iron-doped zinc sulfide with a formaldehyde removal function. Without iron element doping, zinc sulfide had no defects and thus no oxygen free radicals would be generated. Therefore, the polyesters of Comparative Example 1 and Comparative Example 3 did not have the function of removing formaldehyde.

[0174] For the fabric woven in Example 16, see Figure 1 and Figure 2 , which had the maximum absorption and emission under the excitation of ultraviolet light at 360 nm, and the wavelength of the emitted visible light was 450 nm. See Figure 1 and Figure 2, the polyester fiber of the present invention absorbs ultraviolet light and emits visible light, with the ultraviolet range being 200 - 400 nm and the visible light range being 400 - 800 nm. Figure 3 Among them, blue - green light is emitted. The polyester fiber of the present invention belongs to a fluorescent material, which is instantaneous. It emits visible light when there is excitation light and does not emit visible light when there is no excitation light, without delay.

[0175] The preparation method of the polyester fiber of the present invention is as follows: first, an iron - doped zinc sulfide nanomaterial is obtained as a functional powder, and then it is modified by chemical surface modification to improve its compatibility with the resin, having the properties of low addition amount and good effect; then polymerization is carried out through an in - situ polymerization process, and finally, an antibacterial and ultraviolet - absorbing and visible - light - emitting polyester fiber is obtained through a melt - spinning process. The fiber diameter can be made into ultrafine fibers, and the fiber can be made into light colors, having long - term antibacterial and ultraviolet - absorbing and visible - light - emitting functions; different from traditional ultraviolet - resistant fibers, it has a dual ultraviolet - resistant function of shielding and converting ultraviolet light, and realizes the function of ultraviolet - absorbing and visible - light - emitting through photon down - conversion, which can compensate for the human body's demand for visible light. Its mechanical properties reach the standards of ordinary fibers, fully meeting the requirements of various weaving. The cost is lower than that of post - finishing processes, and the functional powder can play a role in catalytic polymerization during in - situ polymerization, reducing the use of catalysts. Compared with the currently used antibacterial and ultraviolet - resistant fibers, the cost is reduced by 70%, reducing pollution, which can expand the export of textiles and increase the added value of textiles.

[0176] The above - mentioned embodiments are only for illustrating the technical concept and characteristics of the present invention, and their purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly, and cannot be used to limit the protection scope of the present invention. All equivalent changes or modifications made according to the spirit and essence of the present invention should be covered within the protection scope of the present invention.

Claims

1. A method for preparing polyester fiber, characterized in that: include: (1) firstly adding zinc oxide and a sulfur source into a mixed solvent of ethylenediamine and ethanolamine, and then adding an organic acid and an iron-containing compound to react to obtain a functional powder, wherein the iron in the iron-containing compound is trivalent iron, and the reaction temperature is controlled to be 180-220°C during the reaction; (2) The functional powder of step (1) is mixed with a polyester raw material to carry out an in-situ polymerization reaction to obtain functional polyester chips, which are then melt-spun to obtain polyester fibers, wherein the polyester raw material includes a polyol and a polyacid. The functional powder prepared in step (1) is firstly prepared into a nanopowder by liquid grinding and dispersed in a polyol medium, and then titanate is added as a surface modifier and a dispersant to improve its dispersibility to obtain a blend, and then the blend is in-situ polymerized with the polyol and the polyacid to obtain functional polyester chips.

2. The method for preparing polyester fiber according to claim 1, characterized in that: In step (1), the iron-containing compound is a combination of one or more selected from ferric chloride and ferric sulfate.

3. The method for preparing polyester fiber according to claim 1, characterized in that: In step (1), the amount of the iron-containing compound added is 0.2-2% of the sum of the mass of the zinc oxide and the sulfur source.

4. The method for preparing polyester fiber according to claim 1, characterized in that: In step (1), the organic acid is a combination of one or more selected from oxalic acid and acetic acid.

5. The method for preparing polyester fiber according to claim 1, characterized in that: In step (1), the amount of organic acid added is 0.05-0.2% of the sum of the mass of zinc oxide and sulfur source.

6. The method for preparing polyester fiber according to claim 1, characterized in that: In step (1), the mass ratio of ethylenediamine to ethanolamine is (1:2)-(2:1).

7. The method for preparing polyester fiber according to claim 1, characterized in that: In step (1), the molar ratio of the zinc oxide to the sulfur source is (1:1.1)-(1.1:1); and\or, the mass fraction of the zinc oxide and the sulfur source dissolved in the mixed solvent of ethylenediamine and ethanolamine is 5-25%.

8. The method for preparing polyester fiber according to claim 1, characterized in that: In step (2), the functional powder of step (1) is first dispersed in a polyol medium, and then a surface modifier is added to obtain a blend. The blend is then in-situ polymerized with a polyol and a polyacid to obtain a functional polyester chip, wherein the mass fraction of the functional powder in the polyester chip is 0.1%-2%.

9. The method for preparing polyester fiber according to claim 8, characterized in that: In step (2), the blend is added to a polyol and then in-situ polymerized with a polyacid, wherein the molar ratio of the polyol mixed with the blend to the polyacid is (1-1.2):1; and\or, in step (2), the polymerization is divided into prepolymerization, post-condensation polymerization, and final polymerization, the prepolymerization temperature is 170-200°C, and the time is 40-80min; the post-condensation temperature is 230-270°C, and the time is 1-3h; the final polymerization temperature is 260-290°C, and the time is 1-4h.

Citation Information

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