Preparation method of regenerated polyester composite antibacterial filament

Abstract

According to the preparation method of the regenerated polyester composite antibacterial filament, regenerated PET bottle flakes and PET slices are used as raw materials, modified montmorillonite and nano particles are used as modified antibacterial agents, the interlayer spacing of Na-montmorillonite is remarkably increased through quaternary ammonium salt intercalation, and the Na-montmorillonite is stripped under the action of polyethyl phosphate glyceride to obtain a single-layer montmorillonite structure; the single-layer montmorillonite structure can be used as a nanoparticle carrier, the agglomeration problem of nanoparticles is effectively solved, and the single-layer montmorillonite structure is effectively dispersed under the action of polyvinylpyrrolidone and is tightly combined with polyester through the interfacial compatibilizer; the nano particles can also form hydrogen bonds with the surface of the single-layer montmorillonite structure, so that the antibacterial effect of the regenerated polyester is greatly improved. The regenerated polyester filament yarn prepared by the method has the characteristics of good mechanical property and strong and lasting antibacterial effect.

Description

Technical Field

[0001] The present invention relates to the technical field of differentiated regenerated environmentally friendly fiber preparation, and in particular to a method for preparing regenerated polyester composite antibacterial filament. Background Art

[0002] Recycled polyester refers to a new type of recycled fiber produced from recycled polyester fiber waste through a series of physical and chemical processes. Recycled polyester fiber waste mainly refers to polyethylene terephthalate (PET). As a recyclable fiber product, recycled polyester has many advantages. It can reduce resource waste, reduce waste emissions, and save costs. Compared with polyester fibers, recycled polyester products are soft, breathable, and easy to dry.

[0003] In recent years, with the rapid development of my country's economy, resource shortages and environmental degradation have become increasingly prominent and have become a major bottleneck restricting economic development. The rapid growth of polyester production has further increased the amount of waste plastic bottles and waste fibers. Due to its strong chemical properties, polyester is difficult to degrade in nature, which has a certain impact on the environment. At the same time, international fashion trends are increasingly focusing on environmental protection and sustainable development. However, the petroleum raw material for polyester fabrics is a non-renewable resource, which is not conducive to the sustainable development of the textile industry. Therefore, various industries have conducted relevant research on recycling in recent years. It is now possible to recycle waste plastic bottles and fibers into polyester fibers with stable quality and excellent performance, giving waste plastics and fibers a second life, achieving resource recycling and environmental protection.

[0004] However, recycled polyester also has some limitations. Usually, the antibacterial properties of recycled polyester usually involve nanosilver particles. When nanosilver is applied to the fabric, the nanosilver lacks sufficient adhesion to the fibers, resulting in a loose bond with the fibers. As a result, only a small amount of nanosilver ions can be adsorbed on the fibers. Nanosilver is not easy to enter the fabric and is easily washed away. As a result, the antibacterial properties of recycled polyester cannot meet people's needs.

[0005] In view of this, we disclose a method for preparing regenerated polyester composite antibacterial filament. Summary of the Invention

[0006] In view of the deficiencies of the prior art, the present invention provides a method for preparing regenerated polyester composite antibacterial filament.

[0007] To achieve the above objectives, the present invention proposes the following technical solutions:

[0008] A method for preparing a regenerated polyester composite antibacterial filament, comprising the following raw material components in parts by weight:

[0009] 65-75 PET slices;

[0010] 25-35 parts of recycled PET bottle flakes;

[0011] 3-5 parts of interfacial compatibilizer;

[0012] 1.2-1.8 parts of modified antibacterial agent;

[0013] 0.1-0.3 parts of compound antioxidant;

[0014] 5-9 parts of color paste.

[0015] Furthermore, the intrinsic viscosity of the PET chips is 0.85±0.05 dl / g.

[0016] Furthermore, the intrinsic viscosity of the recycled PET bottle flakes is 0.60±0.03 dl / g.

[0017] Furthermore, the interfacial compatibilizer is one of styrene / MAH random copolymer, styrene / acrylonitrile / MAH terpolymer, butyl acrylate or maleic anhydride.

[0018] Furthermore, the modified antibacterial agent is a mixture of modified montmorillonite and nanoparticles.

[0019] Furthermore, the preparation method of the modified montmorillonite is:

[0020] A1. Add sodium montmorillonite to deionized water at a mass ratio of 1:(10-20) and perform ultrasonic treatment to obtain a sodium montmorillonite dispersion.

[0021] A2. Dissolve octadecyldimethylallyl ammonium chloride in deionized water in a ratio of 1:(2-5) by weight of octadecyldimethylallyl ammonium chloride to sodium montmorillonite. Adjust the pH of the solution to 3-4 with dilute hydrochloric acid and stir until completely dissolved to obtain an aqueous solution of octadecyldimethylallyl ammonium chloride.

[0022] A3, slowly adding the octadecyldimethylallyl ammonium chloride aqueous solution dropwise to the sodium montmorillonite dispersion, heating to 80-90 ° C, stirring at 500-1000 rpm for 20-24 hours, centrifuging to obtain a solid, washing the solid with deionized water several times, drying in a vacuum drying oven at 60 ° C, grinding and sieving to 200 mesh to obtain a solid mixture;

[0023] A4, drying the solid mixture and polyethyl phosphate glyceride in a vacuum drying oven for 8 h;

[0024] A5, mixing the dried solid mixture in A4 and the polyethyl glycerol phosphate in a mass ratio of 1:1, and stirring at room temperature for 3-5 minutes to obtain a mixture;

[0025] A6. The mixture in A5 was washed with anhydrous ethanol for multiple times and centrifuged at 3000-3500 rpm to obtain the modified montmorillonite.

[0026] Furthermore, the nanoparticles are one of nanosilver, nanocopper oxide or nanozinc oxide.

[0027] Furthermore, the compound antioxidant is a mixture of antioxidant 1010 and antioxidant 168, and the ratio of antioxidant 1010 to antioxidant 168 is 1:(1-2) in parts by weight.

[0028] Furthermore, the method for preparing the regenerated polyester composite antibacterial filament comprises the following steps:

[0029] S1. Material pre-treatment

[0030] Washing recycled PET bottle flakes and PET chips, drying them with hot air, and preparing modified antimicrobial agents at the same time;

[0031] S2. Preparation of modified antimicrobial agent

[0032] The nanoparticles and the modified montmorillonite are dispersed in deionized water at a mass ratio of 1:(5-8), and then a 1.5-3% polyvinyl pyrrolidone aqueous solution is added to prepare the modified antibacterial agent;

[0033] S3. Material combination

[0034] The recycled PET bottle flakes, PET chips, interfacial compatibilizer, modified antibacterial agent, and compound antioxidant are mixed at a high speed of 900-1200 rpm for 5 minutes, then kept at 80-120° C. for 0.5 hours, and then stirred and mixed at the same stirring speed for 5 minutes to obtain a premix;

[0035] S4, extrusion granulation

[0036] The premix is ​​melt-blended and extruded through a twin-screw extruder, followed by pulling, granulation, and drying to prepare a recycled polyester antibacterial functional masterbatch;

[0037] S5. Spinning process

[0038] The dried regenerated polyester antibacterial functional masterbatch is placed in a vacuum drum, first heated to 130°C at a rate of 2°C / min for pre-crystallization for 3 hours; then heated to 150°C at a rate of 9°C / min and kept warm for 4-5 hours, and then put into a spinning machine for spinning treatment. The spinning temperature is 300-310°C and the spinning speed is 3000-4500m / min to obtain regenerated polyester composite antibacterial filament.

[0039] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0040] The present invention provides a method for preparing a regenerated polyester composite antibacterial filament. The method uses recycled PET bottle flakes and PET chips as raw materials, and uses modified montmorillonite and nanoparticles as modified antibacterial agents. The sodium-based montmorillonite undergoes quaternary ammonium salt intercalation to significantly increase the interlayer spacing, and is then exfoliated under the action of polyethyl phosphate glyceride to obtain a single-layer montmorillonite structure. The single-layer montmorillonite structure can serve as a nanoparticle carrier, effectively solving the problem of nanoparticle agglomeration. The single-layer montmorillonite structure is effectively dispersed under the action of polyvinyl pyrrolidone and tightly bonded to the polyester through an interfacial compatibilizer. The nanoparticles can also form hydrogen bonds with the surface of the single-layer montmorillonite structure, greatly enhancing the antibacterial effect of the regenerated polyester. The regenerated polyester filament prepared by the present invention has the characteristics of excellent mechanical properties and strong and long-lasting antibacterial effect.

[0041] It should be appreciated that all combinations of the foregoing concepts, as well as additional concepts described in greater detail below, to the extent such concepts are not mutually inconsistent, can be considered to be part of the present subject matter disclosure.

[0042] The foregoing and other aspects, embodiments and features of the present invention will be more fully understood from the following description. Other additional aspects of the present invention, such as the features and / or beneficial effects of the exemplary embodiments, will become apparent from the following description or will be learned from the practice of the specific embodiments according to the present invention. DETAILED DESCRIPTION

[0043] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the described embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Unless otherwise defined, the technical terms or scientific terms used herein should be the common meanings understood by people with ordinary skills in the field to which the present invention belongs.

[0044] The words "first", "second" and similar words used in the patent application specification and claims of the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. Similarly, unless the context clearly indicates otherwise, the singular forms of "a", "an" or "the" and similar words do not indicate a quantitative limitation, but rather indicate the presence of at least one. Words such as "include" or "comprise" mean that the elements or objects appearing before "include" or "comprise" cover the features, wholes, steps, operations, elements and / or components listed after "include" or "comprise", and do not exclude the existence or addition of one or more other features, wholes, steps, operations, elements, components and / or their collections. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly. The experimental methods or test methods described in the following examples / comparative examples are all conventional methods unless otherwise specified; the reagents and materials are all obtained from conventional commercial channels or prepared by conventional methods unless otherwise specified.

[0045] In this invention, in order to achieve the antibacterial function of the regenerated polyester filament, we added montmorillonite as one of the additives. Montmorillonite (English name montmorillonite) is a natural silicate mineral and the main mineral component of bentonite. It contains Al2O316.54%, MgO4.65%, SiO250.95%, and has the structural formula (Al, Mg)2(SiO 10 )(OH)2nH2O, a monoclinic crystal with multiple crystal positions, aggregates in soil-like, spherical, and other forms. Its volume expands several times upon addition of water, becoming a paste; upon thermal dehydration, its volume shrinks. It possesses strong adsorption capacity and cation exchange properties and is primarily found in the weathering crust of volcanic tuff. Montmorillonite (including calcium-based, sodium-based, sodium-calcium-based, and magnesium-based montmorillonite) undergoes exfoliation, dispersion, purification, modification, ultrafine grading, and special organic compounding, resulting in an average chip thickness of less than 25nm. It can be used as a bleaching agent, adsorbent filler, and is known as a "universal material." In the present invention, montmorillonite primarily serves as a carrier for nanosilver ions, preventing the nanosilver particles from agglomerating and effectively dispersing them within the regenerated polyester filament. The nanosilver particles form hydrogen bonds with the montmorillonite surface, achieving long-lasting and potent antibacterial properties.

[0046] Montmorillonite exhibits oleophobicity due to the large number of inorganic ions between its layers, which hinders its dispersion in a polymer matrix. Therefore, it requires organic modification. The goal is to change the high polarity of the montmorillonite surface, converting the interlayers from hydrophilic to oleophilic, reducing its surface energy. Simultaneously, the interlayer spacing is increased, allowing polymer chains or monomers to enter the interlayers, thereby producing a nanocomposite material. The present invention treats sodium montmorillonite with the cationic surfactant octadecyldimethylallylammonium chloride, causing a cation exchange reaction. This allows organic groups to cover the montmorillonite surface or intercalate between its layers, changing its surface energy and increasing the interlayer spacing, thereby converting its original hydrophilicity to oleophilicity. Natural montmorillonite is rich in silanol (-SiOH) groups on its surface, making it poorly compatible with the hydrophobic PET matrix. Direct addition can lead to particle agglomeration and interfacial defects. Furthermore, the CEC (cation exchange capacity) of natural montmorillonite is approximately 80-120 meq / 100g, making it difficult to load sufficient amounts of antimicrobial ingredients. In the present invention, sodium montmorillonite is peeled off under the action of polyethyl phosphate glyceride to obtain a single-layer montmorillonite structure, which can effectively make up for the above-mentioned defects, can load sufficient antibacterial components and is well compatible with the PET matrix.

[0047] The addition of recycled PET reduces production costs and aligns with my country's green development philosophy. However, during processing, recycled PET bottles experience molecular chain breakage, leading to reduced molecular weight, low intrinsic viscosity, poor flow stability, difficulty in demolding, and poor impact resistance. These issues can affect the performance and durability of recycled PET, necessitating the addition of PET chips to the recycled material. PET chips improve melt strength and spinnability, compensating for the chain breakage defects of the recycled material.

[0048] Example 1

[0049] A method for preparing a regenerated polyester composite antibacterial filament, comprising the following raw material components in parts by weight:

[0050] 65 PET slices;

[0051] 25 parts of recycled PET bottle flakes;

[0052] 3 parts of interfacial compatibilizer;

[0053] 1.2 parts of modified antimicrobial agent;

[0054] 0.1 part of compound antioxidant;

[0055] 5 parts of color paste.

[0056] Furthermore, the intrinsic viscosity of the PET chips is 0.80 dl / g.

[0057] Furthermore, the intrinsic viscosity of the recycled PET bottle flakes is 0.57 dl / g.

[0058] Furthermore, the preparation method of the modified montmorillonite is:

[0059] A1. Add sodium montmorillonite to deionized water in a mass ratio of 1:10, and ultrasonically treat to obtain a sodium montmorillonite dispersion;

[0060] A2. Dissolve octadecyl dimethyl allyl ammonium chloride in deionized water in a ratio of 1:2 by weight of octadecyl dimethyl allyl ammonium chloride to sodium montmorillonite. Adjust the pH of the solution to 3 with dilute hydrochloric acid and stir until completely dissolved to obtain an aqueous solution of octadecyl dimethyl allyl ammonium chloride.

[0061] A3, slowly adding the octadecyldimethylallyl ammonium chloride aqueous solution dropwise to the sodium montmorillonite dispersion, heating to 80 ° C, stirring at 500 rpm for 20 h, centrifuging to obtain a solid, washing the solid with deionized water several times, drying in a vacuum drying oven at 60 ° C, grinding and sieving to 200 mesh, to obtain a solid mixture;

[0062] A4, drying the solid mixture and polyethyl phosphate glyceride in a vacuum drying oven for 8 h;

[0063] A5, mixing the dried solid mixture in A4 and the polyethyl glycerol phosphate in a mass ratio of 1:1, and stirring at room temperature for 3 minutes to obtain a mixture;

[0064] A6. The mixture in A5 was washed with anhydrous ethanol for multiple times and centrifuged at 3000 rpm to obtain the modified montmorillonite.

[0065] Furthermore, the compound antioxidant is a mixture of antioxidant 1010 and antioxidant 168, with the ratio of antioxidant 1010 to antioxidant 168 being 1:1 in parts by weight.

[0066] Furthermore, the modified antibacterial agent is a mixture of modified montmorillonite and nano-silver particles.

[0067] Furthermore, the method for preparing the regenerated polyester composite antibacterial filament comprises the following steps:

[0068] S1. Material pre-treatment

[0069] Washing recycled PET bottle flakes and PET chips, drying them with hot air, and preparing modified antimicrobial agents at the same time;

[0070] S2. Preparation of modified antimicrobial agent

[0071] The modified antibacterial agent is prepared by dispersing the nanosilver particles and the modified montmorillonite in deionized water at a mass ratio of 1:5, and then adding a 1.5% polyvinyl pyrrolidone aqueous solution;

[0072] S3. Material combination

[0073] The recycled PET bottle flakes, PET slices, interfacial compatibilizer, modified antimicrobial agent, and compound antioxidant were mixed at a high speed of 900 r for 5 min, then kept at 80°C for 0.5 h, and then stirred and mixed at the same stirring rate for 5 min to obtain a premix;

[0074] S4, extrusion granulation

[0075] The premix is ​​melt-blended and extruded through a twin-screw extruder, followed by pulling, granulation, and drying to prepare a recycled polyester antibacterial functional masterbatch;

[0076] S5. Spinning process

[0077] The dried regenerated polyester antibacterial functional masterbatch was placed in a vacuum drum, first heated to 130°C at a rate of 2°C / min for pre-crystallization for 3 hours; then heated to 150°C at a rate of 9°C / min and kept warm for 4 hours, and then put into a spinning machine for spinning treatment. The spinning temperature was 300°C and the spinning speed was 3000m / min to obtain regenerated polyester composite antibacterial filament.

[0078] Example 2

[0079] A method for preparing a regenerated polyester composite antibacterial filament, comprising the following raw material components in parts by weight:

[0080] 70 pieces of PET slices;

[0081] 30 parts of recycled PET bottle flakes;

[0082] 4 parts of interfacial compatibilizer;

[0083] 1.5 parts of modified antibacterial agent;

[0084] 0.2 parts of compound antioxidant;

[0085] 7 parts of color paste.

[0086] Furthermore, the intrinsic viscosity of the PET chips is 0.85 dl / g.

[0087] Furthermore, the intrinsic viscosity of the recycled PET bottle flakes is 0.60 dl / g.

[0088] Furthermore, the preparation method of the modified montmorillonite is:

[0089] A1. Add sodium montmorillonite to deionized water in a mass ratio of 1:15, and ultrasonically treat to obtain a sodium montmorillonite dispersion.

[0090] A2. Dissolve octadecyl dimethyl allyl ammonium chloride in deionized water in a ratio of 1:4 by weight of octadecyl dimethyl allyl ammonium chloride to sodium montmorillonite. Adjust the pH of the solution to 3.5 with dilute hydrochloric acid and stir until completely dissolved to obtain an aqueous solution of octadecyl dimethyl allyl ammonium chloride.

[0091] A3, slowly adding the octadecyldimethylallyl ammonium chloride aqueous solution dropwise to the sodium montmorillonite dispersion, heating to 85 ° C, stirring at 800 rpm for 22 h, centrifuging to obtain a solid, washing the solid with deionized water several times, placing it in a vacuum drying oven at 60 ° C, and grinding and sieving to 200 mesh to obtain a solid mixture;

[0092] A4, drying the solid mixture and polyethyl phosphate glyceride in a vacuum drying oven for 10 h;

[0093] A5, mixing the dried solid mixture in A4 and the polyethyl glycerol phosphate in a mass ratio of 1:1, and stirring at room temperature for 4 minutes to obtain a mixture;

[0094] A6. The mixture in A5 was washed with anhydrous ethanol for multiple times and centrifuged at 3300 rpm to obtain the modified montmorillonite.

[0095] Furthermore, the compound antioxidant is a mixture of antioxidant 1010 and antioxidant 168, with the ratio of antioxidant 1010 to antioxidant 168 being 1:1 in parts by weight.

[0096] Furthermore, the method for preparing the regenerated polyester composite antibacterial filament comprises the following steps:

[0097] S1. Material pre-treatment

[0098] Washing recycled PET bottle flakes and PET chips, drying them with hot air, and preparing modified antimicrobial agents at the same time;

[0099] S2. Preparation of modified antimicrobial agent

[0100] The nanoparticles and modified montmorillonite are dispersed in deionized water at a mass ratio of 1:7, and then a 2% polyvinyl pyrrolidone aqueous solution is added to prepare the modified antibacterial agent;

[0101] S3. Material combination

[0102] The recycled PET bottle flakes, PET chips, interfacial compatibilizer, modified antimicrobial agent, and compound antioxidant were mixed at a high speed of 1100r for 5 minutes, then kept at 100°C for 0.5 hours, and then stirred and mixed at the same stirring speed for 5 minutes to obtain a premix;

[0103] S4, extrusion granulation

[0104] The premix is ​​melt-blended and extruded through a twin-screw extruder, followed by pulling, granulation, and drying to prepare a recycled polyester antibacterial functional masterbatch;

[0105] S5. Spinning process

[0106] The dried regenerated polyester antibacterial functional masterbatch was placed in a vacuum drum, first heated to 130°C at a rate of 2°C / min for pre-crystallization for 3 hours; then heated to 150°C at a rate of 9°C / min and kept warm for 4.5 hours, and put into a spinning machine for spinning treatment. The spinning temperature was 305°C and the spinning speed was 3800m / min to obtain regenerated polyester composite antibacterial filament.

[0107] Example 3

[0108] A method for preparing a regenerated polyester composite antibacterial filament, comprising the following raw material components in parts by weight:

[0109] 75 PET slices;

[0110] 35 parts of recycled PET bottle flakes;

[0111] 5 parts of interfacial compatibilizer;

[0112] 1.8 parts of modified antibacterial agent;

[0113] 0.3 parts of compound antioxidant;

[0114] 9 parts of color paste.

[0115] Furthermore, the intrinsic viscosity of the PET sliced ​​bottle flakes is 0.90 dl / g.

[0116] Furthermore, the intrinsic viscosity of the PET bottle flakes is 0.63 dl / g.

[0117] Furthermore, the preparation method of the modified montmorillonite is:

[0118] A1. Add sodium montmorillonite to deionized water in a mass ratio of 1:20, and ultrasonically treat to obtain a sodium montmorillonite dispersion;

[0119] A2. Dissolve octadecyl dimethyl allyl ammonium chloride in deionized water in a ratio of 1:5 by weight of octadecyl dimethyl allyl ammonium chloride to sodium montmorillonite. Adjust the pH of the solution to 4 with dilute hydrochloric acid and stir until completely dissolved to obtain an aqueous solution of octadecyl dimethyl allyl ammonium chloride.

[0120] A3, slowly adding the octadecyldimethylallyl ammonium chloride aqueous solution dropwise to the sodium montmorillonite dispersion, heating to 90 ° C, stirring at 1000 rpm for 24 hours, centrifuging to obtain a solid, washing the solid with deionized water several times, placing it in a vacuum drying oven at 60 ° C, drying it, grinding and sieving it to 200 mesh, to obtain the modified montmorillonite;

[0121] A4, drying the solid mixture and polyethyl phosphate glyceride in a vacuum drying oven for 12 h;

[0122] A5, mixing the dried solid mixture in A4 and the polyethyl glycerol phosphate in a mass ratio of 1:1, and stirring at room temperature for 5 minutes to obtain a mixture;

[0123] A6. The mixture in A5 was washed with anhydrous ethanol for multiple times and centrifuged at 3500 rpm to obtain the modified montmorillonite.

[0124] Furthermore, the compound antioxidant is a mixture of antioxidant 1010 and antioxidant 168, with the ratio of antioxidant 1010 to antioxidant 168 being 1:1 in parts by weight.

[0125] Furthermore, the modified antibacterial agent is a mixture of modified montmorillonite and nano-silver particles.

[0126] Furthermore, the method for preparing the regenerated polyester composite antibacterial filament comprises the following steps:

[0127] S1. Material pre-treatment

[0128] Washing recycled PET bottle flakes and PET chips, drying them with hot air, and preparing modified antimicrobial agents at the same time;

[0129] S2. Preparation of modified antimicrobial agent

[0130] The nanoparticles and modified montmorillonite are dispersed in deionized water at a mass ratio of 1:8, and a 3% polyvinyl pyrrolidone aqueous solution is added to prepare the modified antibacterial agent;

[0131] S3. Material combination

[0132] The recycled PET bottle flakes, PET chips, interfacial compatibilizer, modified antimicrobial agent, and compound antioxidant were mixed at a high speed of 1200r for 5 minutes, then kept at 120°C for 0.5 hours, and then stirred and mixed at the same stirring speed for 5 minutes to obtain a premix;

[0133] S4, extrusion granulation

[0134] The premix is ​​melt-blended and extruded through a twin-screw extruder, followed by pulling, granulation, and drying to prepare a recycled polyester antibacterial functional masterbatch;

[0135] S5. Spinning process

[0136] The dried regenerated polyester antibacterial functional masterbatch was placed in a vacuum drum, first heated to 130°C at a rate of 2°C / min for pre-crystallization for 3 hours; then heated to 150°C at a rate of 9°C / min and kept warm for 5 hours, and then put into a spinning machine for spinning treatment. The spinning temperature was 310°C and the spinning speed was 4500m / min to obtain regenerated polyester composite antibacterial filament.

[0137] Comparative Example 1

[0138] The difference from Example 1 is that the modified antibacterial agent is modified montmorillonite, and the other steps refer to Example 1.

[0139] Comparative Example 2

[0140] The difference from Example 1 is that the modified antibacterial agent is nanosilver particles, and the other steps refer to Example 1.

[0141] Comparative Example 3

[0142] The difference from Example 1 is that the modified antibacterial agent is a mixture of modified montmorillonite and nanosilver particles without adding polyvinyl pyrrolidone aqueous solution. The other steps refer to Example 1.

[0143] Comparative Example 4

[0144] The difference from Example 1 is that octadecyldimethylallyl ammonium chloride is not added in the preparation method of the modified montmorillonite, and the other steps refer to Example 1.

[0145] Comparative Example 5

[0146] Different from Example 1, polyethyl phosphate glyceride is not added in the preparation method of the modified montmorillonite, and other steps refer to Example 1.

[0147] Performance Testing

[0148] Mechanical properties testing

[0149] With reference to GB / T14337-2008 “Test method for tensile properties of chemical staple fibers”, the yarns were cut into the same test length, and the mechanical properties of the sample yarns were evaluated using an electronic single-filament strength tester (LLY-06E) purchased from Laizhou Electronic Instrument Co., Ltd. in China, with breaking strength (unit: cN / dtex) as the evaluation standard.

[0150] Long-lasting antibacterial

[0151] Refer to GB / T31713-2015 "Safety and Hygiene Requirements for Antimicrobial Textiles", use standard detergent to wash at 40°C, conduct the initial antibacterial rate test (wash 0 times), perform multiple washes (such as 5 times, 10 times, 20 times, 50 times), retest the antibacterial rate after washing, and observe the attenuation.

[0152] Antibacterial properties

[0153] The yarns were woven into fabric using the same process and then cut into fabrics of equal area for testing. The antibacterial properties of the PET composite antibacterial fiber were tested according to GB / T 20944.3-2008, "Evaluation of Antimicrobial Properties of Textiles - Part 3: Oscillation Method." The antibacterial activity of the regenerated polyester filament was expressed as inhibition rate (%) against Staphylococcus aureus (ATCC 6538), Escherichia coli (ATCC 25922), and Candida albicans (ATCC 10231).

[0154] The regenerated polyester filament samples of Examples 1-3 and Comparative Examples 1-5 were sampled and then characterized according to relevant performance test standards. Detailed comparison of relevant tests is shown in Table 1.

[0155] Table 1 Comparison of relevant test characteristics

[0156] From the comparison in the above table, it can be seen that the regenerated polyester filament prepared by the present invention has the characteristics of good mechanical properties and strong and long-lasting antibacterial effect.

[0157] As for mechanical properties, the present invention mainly uses breaking strength as the evaluation standard. The breaking strength is mainly related to the structure of the polyester filament. In Examples 1-3, as the proportion of recycled PET bottle flakes increases,

[0158] The breaking strength of recycled polyester shows a downward trend for the following reasons: 1. The recycled raw materials undergo multiple melt processing, and the molecular chains break, resulting in a decrease in polymerization degree and a decrease in intrinsic viscosity; 2. Impurities (such as dyes and additives) remain during the regeneration process, destroying the structural uniformity; 3. The recycled PET composition is complex, and the intrinsic viscosity fluctuates greatly, affecting the strength stability.

[0159] For antimicrobial agents, the modified antimicrobial agent used in the present invention is a mixture of modified montmorillonite and nanoparticles. After being treated with a polyvinyl pyrrolidone aqueous solution, the modified antimicrobial agent is combined with regenerated polyester filaments. The synergistic effect of the modified montmorillonite and the nanoparticles imparts excellent antimicrobial properties to the regenerated polyester filaments. In Comparative Examples 1-5, the incomplete structure of the modified antimicrobial agent significantly impacts its antimicrobial properties. The nanosilver particles provide potent antimicrobial properties. The modified montmorillonite acts as a carrier for the nanoparticles, preventing them from agglomerating. The polyvinyl pyrrolidone disperses the monolayer montmorillonite structure, and the PET structure influences the stability of the modified antimicrobial agent's binding to it.

[0160] While the present invention has been disclosed above with reference to preferred embodiments, this is not intended to limit the present invention. Persons skilled in the art will readily appreciate that various modifications and variations can be made without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention shall be determined by the claims.

Claims

1. A method for preparing regenerated polyester composite antibacterial filament, characterized in that: Calculated by weight, it includes the following raw materials: 65-75 PET slices; 25-35 parts of recycled PET bottle flakes; 3-5 parts of interfacial compatibilizer; 1.2-1.8 parts of modified antibacterial agent; 0.1-0.3 parts of compound antioxidant; 5-9 parts of color paste.

2. The method for preparing a regenerated polyester composite antibacterial filament according to claim 1, characterized in that: The intrinsic viscosity of the PET chips is 0.85±0.05 dl / g.

3. The method for preparing a regenerated polyester composite antibacterial filament according to claim 1, characterized in that: The intrinsic viscosity of the recycled PET bottle flakes is 0.60±0.03 dl / g.

4. The method for preparing a regenerated polyester composite antibacterial filament according to claim 1, characterized in that: The interfacial compatibilizer is one of styrene / MAH random copolymer, styrene / acrylonitrile / MAH terpolymer, butyl acrylate or maleic anhydride.

5. The method for preparing a regenerated polyester composite antibacterial filament according to claim 1, characterized in that: The modified antibacterial agent is a mixture of modified montmorillonite and nanoparticles.

6. The method for preparing a regenerated polyester composite antibacterial filament according to claim 5, characterized in that: The preparation method of the modified montmorillonite is: A1. Add sodium montmorillonite to deionized water at a mass ratio of 1:(10-20) and perform ultrasonic treatment to obtain a sodium montmorillonite dispersion. A2. Dissolve octadecyldimethylallyl ammonium chloride in deionized water in a ratio of 1:(2-5) by weight of octadecyldimethylallyl ammonium chloride to sodium montmorillonite. Adjust the pH of the solution to 3-4 with dilute hydrochloric acid and stir until completely dissolved to obtain an aqueous solution of octadecyldimethylallyl ammonium chloride. A3, slowly adding the octadecyldimethylallyl ammonium chloride aqueous solution dropwise to the sodium montmorillonite dispersion, heating to 80-90 ° C, stirring at 500-1000 rpm for 20-24 hours, centrifuging to obtain a solid, washing the solid with deionized water several times, drying in a vacuum drying oven at 60 ° C, grinding and sieving to 200 mesh to obtain a solid mixture; A4, drying the solid mixture and polyethyl phosphate glyceride in a vacuum drying oven for 8-12 hours; A5, mixing the dried solid mixture in A4 and the polyethyl glycerol phosphate in a mass ratio of 1:1, and stirring at room temperature for 3-5 minutes to obtain a mixture; A6. The mixture in A5 was washed with anhydrous ethanol for multiple times and centrifuged at 3000-3500 rpm to obtain the modified montmorillonite.

7. The method for preparing a regenerated polyester composite antibacterial filament according to claim 5, characterized in that: The nanoparticles are one of nanosilver, nanocopper oxide or nanozinc oxide.

8. The method for preparing a regenerated polyester composite antibacterial filament according to claim 1, characterized in that: The compound antioxidant is a mixture of antioxidant 1010 and antioxidant 168, and the ratio of antioxidant 1010 to antioxidant 168 is 1:(1-2) by weight.

9. A method for preparing a regenerated polyester composite antibacterial filament according to any one of claims 1 to 8, characterized in that: The following steps are involved: S1. Material pre-treatment Washing recycled PET bottle flakes and PET chips, drying them with hot air, and preparing modified antimicrobial agents at the same time; S2. Preparation of modified antimicrobial agent The nanoparticles and the modified montmorillonite are dispersed in deionized water at a mass ratio of 1:(5-8), and then a 1.5-3% polyvinyl pyrrolidone aqueous solution is added to prepare the modified antibacterial agent; S3. Material combination The recycled PET bottle flakes, PET chips, interfacial compatibilizer, modified antibacterial agent, and compound antioxidant are mixed at a high speed of 900-1200 rpm for 5 minutes, then kept at 80-120° C. for 0.5 hours, and then stirred and mixed at the same stirring speed for 5 minutes to obtain a premix; S4, extrusion granulation The premix is ​​melt-blended and extruded through a twin-screw extruder, followed by pulling, granulation, and drying to prepare a recycled polyester antibacterial functional masterbatch; S5. Spinning process The dried regenerated polyester antibacterial functional masterbatch is placed in a vacuum drum, first heated to 130°C at a rate of 2°C / min for pre-crystallization for 3 hours; then heated to 150°C at a rate of 9°C / min and kept warm for 4-5 hours, and then put into a spinning machine for spinning treatment. The spinning temperature is 300-310°C and the spinning speed is 3000-4500m / min to obtain regenerated polyester composite antibacterial filament.

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