Preparation method of antibacterial porous polyester DTY (Draw Textured Yarn) composite yarn

Abstract

The invention belongs to the technical field of fiber spinning, and particularly discloses a preparation method of an antibacterial porous polyester DTY composite yarn. Comprising the following steps: (1) mixing 60-65 parts of waste polyester chips, 2-4 parts of an antibacterial agent, 6-8 parts of diphenyl silane glycol, 18-25 parts of nano-particle modified pearl powder, 5-9 parts of zinc acetate and 12-16 parts of polyethylene glycol, and carrying out melt extrusion, cooling, oiling and heat setting to obtain polyester POY (Polyester Pre-Oriented Yarn) filaments; and (2) carrying out heating stretching, false twisting and heat setting on the polyester POY filaments to obtain the antibacterial porous polyester DTY composite filaments. The antibacterial porous polyester DTY composite yarn prepared in the invention has good strength and wear resistance, so that the fiber is not easy to break in the use process, and the wear resistance and durability of the fiber are ensured.

Description

Technical Field

[0001] This application relates to the technical field of fiber spinning, and particularly to a preparation method of antibacterial porous polyester DTY composite filaments. Background Art

[0002] Polyester DTY composite filaments are a type of polyester drawn textured yarn prepared through a draw texturing process, with properties such as bulkiness, high elasticity, and multifunctionality, and are widely used in the fields of clothing, home textiles, and industry. With the widespread application of polyester DTY composite filaments, people's requirements for DTY composite filaments are also getting higher and higher, and there is an increasing pursuit of functional DTY composite filaments.

[0003] In the prior art, polyester chips are used as the basic raw material, and through melt blending, spinning, drawing, and false twist setting, polyester DTY composite filaments are obtained. For functional modification technologies, conductive materials are also added to reduce static electricity accumulation, pore-forming agents are added to increase the moisture absorption and sweat discharge properties of polyester DTY composite filaments, and antibacterial particles are added to increase the antibacterial properties of polyester DTY composite filaments.

[0004] The polyester DTY composite filaments obtained through the above method have good elasticity and anti-fusing properties, can maintain a stable shape at high temperatures, are not easily deformed, and have good corrosion resistance and light resistance. However, during the subsequent use of the fibers, due to the action of external stress and friction, the surface of the fibers is prone to wear, which in turn affects subsequent use. Summary of the Invention

[0005] In order to improve the problem that the fiber surface is prone to wear, this application provides a preparation method of antibacterial porous polyester DTY composite filaments.

[0006] This application provides a preparation method of antibacterial porous polyester DTY composite filaments, adopting the following technical solution: A preparation method of antibacterial porous polyester DTY composite filaments, comprising the following steps: (1) Mix 60 - 65 parts of waste polyester chips, 2 - 4 parts of antibacterial agent, 6 - 8 parts of diphenylsilanediol, 18 - 25 parts of nano-particle modified pearl powder, 5 - 9 parts of zinc acetate, and 12 - 16 parts of polyethylene glycol, melt extrude, cool, oil, and heat set to obtain polyester POY filaments; (2) Heat draw, false twist, and heat set the polyester POY filaments obtained in step (1) to obtain antibacterial porous polyester DTY composite filaments.

[0007] By adopting the above technical solution, waste polyester chips are used as the matrix material to provide basic physical structure and mechanical properties, improving the recyclability and environmental friendliness of the material. The antibacterial agent is combined with zinc acetate to inhibit the growth of bacteria, prevent odor and microbial contamination, and extend the service life of the filament. Diphenylsilanediol improves the flexibility and elasticity of the filament, improves the interfacial bonding between the nanoparticle-modified pearl powder and the waste polyester chips, and enhances the thermal stability and mechanical properties of the filament. The nanoparticle-modified pearl powder enhances the antibacterial property of the filament, improves the luster and appearance of the filament, and increases the surface hardness, mechanical properties and wear resistance of the filament. Polyethylene glycol helps other components to be evenly dispersed in the system, improves the uniformity and stability of the system, and further enhances the flexibility and elasticity of the filament.

[0008] The mixed materials are melt-extruded to form polyester POY filaments. The extruded polyester POY filaments are cooled to stabilize the fiber morphology. An oil agent is applied to the surface of the filaments to improve the processing performance and handle of the fibers. The filaments are heat-set to improve the dimensional stability and thermal stability of the filaments.

[0009] The polyester POY filaments are heated and stretched, false-twisted, and heat-set. Heating and stretching improve the orientation degree and strength of the filaments. False-twisting increases the crimp degree and elasticity of the filaments. The false-twisted filaments are heat-set again to further improve the dimensional stability and thermal stability of the filaments. The obtained antibacterial porous polyester DTY composite filaments have good antibacterial properties, wear resistance, high strength and elasticity, and improve the air permeability and moisture absorption of the composite filaments.

[0010] Preferably, the pretreatment method of the waste polyester chips includes the following steps: (1) The waste polyester chips are crushed to obtain fragments with a size of 0.5-1 mm. The fragments are dispersed in a sodium hydroxide solution, stirred for 1-2 h, washed with water, then dispersed in a cleaning solution, and cleaned at a rotation speed of 400-450 rpm for 30-35 min, and dried to obtain cleaned fragments; (2) The modified seaweed fibers are dispersed in deionized water, and the cleaned fragments obtained in step (1), 5-sulfonatophthalic acid ester, and pentaerythritol tetra are added, and stirred at a temperature of 60-65 °C for 20-25 min, and filtered to obtain a mixture; (3) An ethylene glycol solution of barium sulfate is sprayed on the surface of the mixture obtained in step (2), and dried to obtain the pretreated waste polyester chips; The cleaning solution includes benzyl alcohol, alkylbenzene sulfonate, polyoxyethylene styrenated phenyl ether, and amino acid type surfactant.

[0011] By adopting the above technical solution, the waste polyester chips are crushed into fragments of 0.5 - 1 mm, increasing the surface area and facilitating subsequent cleaning and chemical treatment. The sodium hydroxide solution effectively removes the oil stains and impurities on the surface of the polyester chips, causing the oil stains and impurities to separate from the chip surface. The cleaning solution further removes the residual impurities and fine particles on the chip surface, ensuring the purity of the chips.

[0012] In the cleaning solution, benzyl alcohol has good solubility and can effectively remove the oil stains and organic impurities on the surface of the polyester chips; alkylbenzene sulfonate can combine with the oil stains and impurities on the surface of the polyester chips, causing them to separate from the chip surface and enhancing the permeability and dispersibility of the cleaning solution. Polyoxyethylene styrenated phenyl ether has good dispersibility and can evenly disperse the solid particles in the cleaning solution, preventing particle agglomeration, solubilizing the oil stains and impurities into the cleaning solution, and improving the cleaning efficiency. Amino acid-based surfactants have good biocompatibility and mildness, effectively removing the oil stains and impurities on the chip surface while protecting the surface quality of the chips.

[0013] The modified seaweed fiber, cleaning fragments, 5-sodium sulfoisophthalate, and pentaerythritol tetra are mixed. The modified seaweed fiber has good dispersibility, flexibility, and wear resistance and can be loaded on the surface of the cleaning fragment particles, increasing the flexibility and mechanical properties of the cleaning fragments. The addition of pentaerythritol tetra improves the thermal stability and antioxidant performance of the system. 5-Sodium sulfoisophthalate has good dispersibility and plasticizing properties, enabling the modified seaweed fiber to be evenly loaded in the cleaning fragment structure and improving the flexibility and processing performance of the mixture.

[0014] A glycol solution of barium sulfate is sprayed on the surface of the mixture. The glycol solution of barium sulfate has high density, good dispersibility, and adhesiveness. Barium sulfate adheres evenly to the surface of the mixture, forming a protective layer, making the modified seaweed fiber and the cleaning fragments adhere tightly, improving the stability and mechanical properties of the mixture. The pretreated waste polyester chips obtained have excellent mechanical properties, wear resistance, thermal stability, and antioxidant performance.

[0015] Preferably, the mass ratio of the waste polyester chips, the modified seaweed fiber, and the glycol solution of barium sulfate is 1:0.5 - 0.6:0.08 - 0.09.

[0016] By adopting the above technical solution, further limiting the mass ratio of waste polyester chips, modified seaweed fiber and ethylene glycol solution of barium sulfate within a certain range can improve the mechanical strength, wear resistance and flexibility of waste polyester chips. The modified seaweed fiber has good flexibility and biocompatibility, can be loaded on the surface and pores of waste polyester chips to improve the mechanical properties of waste polyester chips. The ethylene glycol solution of barium sulfate has good wear resistance and mechanical properties, can coat the waste polyester chips, making the waste polyester chips adhere tightly to the modified seaweed fiber, increasing the mechanical properties, flexibility and wear resistance of the waste polyester chips, and subsequently improving the corresponding properties of the antibacterial porous polyester DTY composite filament.

[0017] Preferably, the preparation method of the modified seaweed fiber includes the following steps: subject the seaweed fiber to oxygen plasma treatment under the conditions of a temperature of 45 - 48 °C, a vacuum degree of 800 - 850 Pa, and a plasma power source of 260 - 280 W, then immerse it in the graphene modified solution, add glutaraldehyde and nano-activated carbon, stir at a temperature of 90 - 95 °C for 2 - 3 h, and dry to obtain the modified seaweed fiber.

[0018] Graphene modified solution: Disperse graphene in deionized water, add chitosan, wheat straw powder, silane coupling agent and p-toluenesulfonic acid catalyst, stir at a temperature of 80 - 85 °C for 35 - 40 min, and ultrasonically disperse for 25 - 30 min to obtain the graphene modified solution.

[0019] By adopting the above technical solution, plasma treatment can effectively remove impurities on the surface of seaweed fiber, change its surface morphology, and there appear many obvious gaps, which is helpful for subsequent impregnation and modification treatments.

[0020] In the graphene modified solution, chitosan forms hydrogen bonds with the surface of graphene, enhancing the dispersibility and stability of graphene. Wheat straw powder has good adsorption and enhancement properties, can be embedded in the network structure formed by chitosan and graphene, and forms a synergistic effect with chitosan and graphene, further improving the stability and functionality of the solution. The silane coupling agent can react with the functional groups on the surface of graphene to form chemical bonds, enhancing the compatibility of graphene with other materials. The p-toluenesulfonic acid catalyst can promote the chemical reaction between graphene and other materials, improving the reaction efficiency.

[0021] Immerse the seaweed fiber in the graphene modified solution, and the active components in the solution can be loaded on the surface of the seaweed fiber. Add glutaraldehyde and nano-activated carbon, and glutaraldehyde undergoes a cross-linking reaction with the active groups in the seaweed fiber and the graphene modified solution to form a stable network structure, which is further loaded in the seaweed fiber structure, enhancing the stability and mechanical properties of the fiber. The obtained modified seaweed fiber has excellent wear resistance, antibacterial property and mechanical properties.

[0022] Preferably, the preparation method of the nanoparticle-modified pearl powder comprises the following steps: (1) Sieve the pearl powder, disperse it in acetone, add aluminum distearate and lauroyl lysine, stir for 2 - 3 h, filter, wash, and dry to obtain the treated pearl powder; (2) Disperse the modified loofah sponge in deionized water, add the treated pearl powder, metal framework material, xanthan gum, and sodium hexametaphosphate obtained in step (1), stir at 60 - 65 °C for 1 - 2 h, and dry to obtain the nanoparticle-modified pearl powder.

[0023] By adopting the above technical solution, the pearl powder is dispersed in absolute ethanol, and aluminum distearate and lauroyl lysine are added. The combination of aluminum distearate and lauroyl lysine improves the dispersibility, processing performance, and biocompatibility of the pearl powder, making the subsequent combination of the pearl powder with other components uniform.

[0024] The modified loofah sponge, treated pearl powder, metal framework material, xanthan gum, and sodium hexametaphosphate are mixed. The modified loofah sponge has good adsorption and a porous structure, with a large surface area, adsorbing on the surface of the pearl powder particles, enhancing the adsorption of the pearl powder. The metal framework material can be embedded in the structures of the modified loofah sponge and the pearl powder, further increasing the connectivity of the modified loofah sponge and the pearl powder, improving the mechanical strength, wear resistance, and stability of the pearl powder, and also preventing particle agglomeration. Xanthan gum has good antioxidant and adhesive properties, can prevent the oxidation of the pearl powder during the treatment process, maintain its activity, and can also increase the adhesion between the pearl powder, modified loofah sponge, and metal framework material. Sodium hexametaphosphate has good dispersibility and stability, making the components in the system disperse evenly, and improving the dispersibility and stability of the pearl powder.

[0025] Through the synergistic effect of absolute ethanol, lauroyl lysine, and sodium hexametaphosphate, the uniform dispersion of the pearl powder in the system is ensured. The addition of lauroyl lysine and xanthan gum improves the biocompatibility, adhesion, and antioxidant properties of the pearl powder. The addition of the metal framework material enhances the mechanical strength and stability of the pearl powder. The modified loofah sponge provides a porous structure, increasing the surface area and adsorption performance of the pearl powder. The various compositions in the system cooperate synergistically, improving the wear resistance, breathability, antibacterial property, and mechanical properties of the nanoparticle-modified pearl powder.

[0026] Preferably, the mass ratio of the pearl powder, modified loofah sponge, metal framework material, and xanthan gum is 1:0.4 - 0.5:0.2 - 0.3:0.1 - 0.2.

[0027] By adopting the above technical solutions, the mass ratio of pearl powder, modified loofah sponge, metal framework material and xanthan gum is further limited within a certain range. Pearl powder has good biological activity and osteogenic effect. Modified loofah sponge has a natural three-dimensional porous structure, which can adsorb on the surface of pearl powder particles, increasing the surface area, mechanical properties and adsorption properties of pearl powder, and helping to improve the air permeability and moisture absorption of the fiber subsequently. The metal framework material can be embedded in the structures of pearl powder and modified loofah sponge, not only increasing the adhesion between pearl powder and modified loofah sponge, but also improving the mechanical strength, wear resistance and stability of pearl powder. Xanthan gum has good antioxidant performance and adhesiveness, which can prevent the fiber from oxidation during processing and use, making pearl powder, modified loofah sponge and metal framework material adhere tightly, further increasing the mechanical properties, biocompatibility, antibacterial properties and antioxidant properties of pearl powder, and helping to improve the corresponding properties of the composite filament subsequently.

[0028] Preferably, the preparation method of the modified loofah sponge includes the following steps: cutting the loofah sponge into pieces, dispersing it in a sodium hydroxide solution, heating at 70 - 75 °C for 2 - 3 h, washing with water and drying to obtain the pretreated loofah sponge; dispersing the pretreated loofah sponge in a citric acid solution, adding cocamidopropyl betaine, stirring evenly, washing with deionized water and drying to obtain the post-treated loofah sponge; dispersing the post-treated loofah sponge in deionized water, adding konjac gum and nano-nickel, stirring at 70 - 75 °C for 2 - 3 h and drying to obtain the modified loofah sponge.

[0029] By adopting the above technical solutions, treating the loofah sponge with a sodium hydroxide solution can remove the wax and impurities on the surface of the loofah sponge through alkali treatment, increasing its specific surface area and thus improving its adsorption performance. Dispersing the pretreated loofah sponge in a citric acid solution and adding cocamidopropyl betaine, the citric acid undergoes an esterification reaction with the hydroxyl groups on the surface of the loofah sponge to improve its surface chemical properties, and cocamidopropyl betaine improves the wettability and dispersibility of the loofah sponge, making it easier to combine with other components in subsequent treatments.

[0030] The post-treated loofah sponge, konjac gum and nano-nickel are mixed. Nano-nickel has good mechanical properties and antibacterial properties and can be loaded in the pores of the post-treated loofah sponge, increasing the mechanical strength and antibacterial properties of the post-treated loofah sponge. Konjac gum has good wrapping and stabilizing effects, which can enhance the adsorption performance of the loofah sponge, making nano-nickel adhere stably in the loofah sponge structure, increasing the adsorption, mechanical and antibacterial properties of the modified loofah sponge, and subsequently improving the corresponding properties of the nano-particle modified pearl powder.

[0031] Preferably, in step (1), the temperature of melt extrusion is 250 - 260 °C, the extrusion pressure is 50 - 60 MPa, and the temperature of heat setting is 120 - 125 °C.

[0032] By adopting the above technical solution and further limiting the conditions of melt extrusion, oiling and heat setting, the obtained polyester POY filaments have good mechanical strength, flexibility and chemical resistance, so that the filaments have better applications.

[0033] Preferably, in step (2), the temperature of heating and stretching is 200-210° C., the drafting ratio is 1.03-1.06; and the single fiber fineness of the DTY composite yarn is 3-4 dtex.

[0034] By adopting the above technical solution, the heating and stretching temperature, the drafting multiple and the single filament fineness are set, so that the fiber has good flexibility and comfort while maintaining high strength and modulus.

[0035] In summary, this application has the following beneficial effects: 1. In this application, waste polyester chips are used as base materials to provide basic physical structure and mechanical properties, and improve the recyclability and environmental friendliness of the materials.

[0036] 2. The nanoparticle-modified pearl powder in the present application enhances the antibacterial properties of the filaments, improves the gloss and appearance of the filaments, and increases the surface hardness, mechanical properties and wear resistance of the filaments.

[0037] 3. The antibacterial porous polyester DTY composite yarn in the present application has good antibacterial properties, wear resistance, high strength and elasticity, and improves the air permeability and moisture absorption of the composite yarn. DETAILED DESCRIPTION

[0038] The present application is further described in detail below with reference to the embodiments.

[0039] The raw materials used in the examples and comparative examples can all be obtained commercially.

[0040] Preparation example of nanoparticle modified pearl powder Preparation Example 1-1 The preparation method of nanoparticle modified pearl powder comprises the following steps: (1) 30 kg of pearl powder was passed through a 20-mesh sieve, dispersed in 50 L of acetone, 2 kg of aluminum distearate and 3 kg of lauroyl lysine were added, stirred for 2.5 h, filtered, washed, and dried to obtain treated pearl powder; (2) Dispersing the modified loofah in 80 L of deionized water, adding the treated pearl powder of step (1), metal skeleton material, xanthan gum and 2 kg of sodium hexametaphosphate, stirring at 63 ° C for 1.5 h, and drying to obtain nanoparticle modified pearl powder; the metal skeleton material is ZIF-8 purchased from Xi'an Qiyue Biotechnology Co., Ltd., and the xanthan gum is purchased from Jinan Hongyuan Chemical Co., Ltd.

[0041] The mass ratio of pearl powder, modified loofah sponge, metal framework material and xanthan gum is 1:0.4:0.3:0.2.

[0042] The preparation method of the modified loofah sponge includes the following steps: Chop 50 kg of loofah sponge into pieces, disperse it in 100 L of sodium hydroxide solution with a mass fraction of 20%, heat it at 72 °C for 2.6 h, wash it with water and dry it to obtain the pretreated loofah sponge; Disperse the pretreated loofah sponge in 90 L of citric acid solution with a mass fraction of 4%, add 3 kg of coconut oil amide propyl betaine, stir evenly, wash it with deionized water and dry it to obtain the post-treated loofah sponge; Disperse the post-treated loofah sponge in 70 L of deionized water, add 4 kg of konjac gum and 9 kg of nano-nickel, stir at 74 °C for 2.5 h and dry it to obtain the modified loofah sponge.

[0043] Preparation Examples 1-2 The difference from Preparation Example 1-1 is that in step (2), no modified loofah sponge is added.

[0044] Preparation Example 1-3 The difference from Preparation Example 1-1 is that in step (2), no metal framework material is added.

[0045] Preparation Example 1-4 The difference from Preparation Example 1-1 is that in step (2), no xanthan gum is added.

[0046] Preparation Example 1-5 The difference from Preparation Example 1-1 is that the mass ratio of pearl powder, modified loofah sponge, metal framework material and xanthan gum is 1:0.5:0.2:0.1.

[0047] Preparation Example 1-6 The difference from Preparation Example 1-1 is that the mass ratio of pearl powder, modified loofah sponge, metal framework material and xanthan gum is 1:0.1:0.05:0.6.

[0048] Preparation Example 1-7 The difference from Preparation Example 1-1 is that in the preparation method of the modified loofah sponge, no konjac gum is added.

[0049] Preparation Example 1-8 The difference from Preparation Example 1-1 is that in the preparation method of the modified loofah sponge, no nano-nickel is added. Examples

[0050] Example 1 A preparation method of an antibacterial porous polyester DTY composite filament includes the following steps: (1) Mix 60 kg of waste polyester chips, 2 kg of antibacterial agent, 6 kg of diphenylsilanediol, 25 kg of nano-particle modified pearl powder, 5 kg of zinc acetate, and 12 kg of polyethylene glycol, melt-extrude, cool, oil, and heat-set to obtain polyester POY filaments; the antibacterial agent is nano-silver; (2) Heat-draw, false-twist, and heat-set the polyester POY filaments obtained in step (1) to obtain antibacterial porous polyester DTY composite filaments.

[0051] The waste polyester chips are for the product wig fibers.

[0052] In step (1), the temperature of melt-extrusion is 250 °C, the extrusion pressure is 60 MPa, and the temperature of heat-setting is 125 °C.

[0053] In step (2), the temperature of heat-drawing is 200 °C, the draw ratio is 1.03, and the denier per filament of the DTY composite filaments is 3 dtex.

[0054] The nano-particle modified pearl powder adopts Preparation Example 1-1.

[0055] Example 2 A method for preparing antibacterial porous polyester DTY composite filaments, which is different from Example 1, includes the following steps: (1) Mix 65 kg of waste polyester chips, 4 kg of antibacterial agent, 8 kg of diphenylsilanediol, 18 kg of nano-particle modified pearl powder, 9 kg of zinc acetate, and 16 kg of polyethylene glycol, melt-extrude, cool, oil, and heat-set to obtain polyester POY filaments; (2) Heat-draw, false-twist, and heat-set the polyester POY filaments obtained in step (1) to obtain antibacterial porous polyester DTY composite filaments.

[0056] In step (1), the temperature of melt-extrusion is 260 °C, the extrusion pressure is 50 MPa, and the temperature of heat-setting is 120 °C.

[0057] In step (2), the temperature of heat-drawing is 210 °C, the draw ratio is 1.06, and the denier per filament of the DTY composite filaments is 4 dtex.

[0058] Example 3 A method for preparing antibacterial porous polyester DTY composite filaments, which is different from Example 1, is that the nano-particle modified pearl powder is prepared by Preparation Example 1-2.

[0059] Example 4 A method for preparing antibacterial porous polyester DTY composite filaments, which is different from Example 1, is that the nano-particle modified pearl powder is prepared by Preparation Example 1-3.

[0060] Example 5 A method for preparing an antibacterial porous polyester DTY composite yarn is different from Example 1 in that the nanoparticle-modified pearl powder is prepared using Preparation Examples 1-4.

[0061] Example 6 A method for preparing an antibacterial porous polyester DTY composite yarn is different from Example 1 in that the nanoparticle-modified pearl powder is prepared using Preparation Examples 1-5.

[0062] Example 7 A method for preparing an antibacterial porous polyester DTY composite yarn is different from Example 1 in that the nanoparticle-modified pearl powder is prepared using Preparation Examples 1-6.

[0063] Example 8 A method for preparing an antibacterial porous polyester DTY composite yarn is different from Example 1 in that the nanoparticle-modified pearl powder is prepared using Preparation Examples 1-7.

[0064] Example 9 A method for preparing an antibacterial porous polyester DTY composite yarn is different from Example 1 in that the nanoparticle-modified pearl powder is prepared using Preparation Examples 1-8.

[0065] Example 10 A method for preparing an antibacterial porous polyester DTY composite yarn, which is different from Example 1 in that the pretreatment method of waste polyester chips comprises the following steps: (1) 100 kg of waste polyester chips were crushed to obtain fragments with a size of 0.8 mm, the fragments were dispersed in 130 L of a 7% sodium hydroxide solution, stirred for 1.5 h, washed with water, and then dispersed in a cleaning solution, washed at a rotation speed of 420 rpm for 32 min, and dried to obtain cleaned fragments; (2) dispersing the modified seaweed fiber in 200 L of deionized water, adding the cleaned fragments of step (1), 8 kg of 5-sodium sulfonate isophthalate, and 3 kg of pentaerythritol tetrachloride, stirring at a temperature of 62° C. for 23 min, and filtering to obtain a mixture; (3) spraying a barium sulfate ethylene glycol solution on the surface of the mixture in step (2), and drying to obtain pretreated waste polyester chips; The cleaning liquid is obtained by uniformly mixing 140L benzyl alcohol, 8kg alkylbenzene sulfonate, 10kg polyoxyethylene styrenated phenyl ether, and 15kg amino acid type surfactant; the alkylbenzene sulfonate is sodium dodecylbenzene sulfonate, and the amino acid type surfactant is sodium lauroyl glutamate.

[0066] The mass ratio of waste polyester chips, modified seaweed fiber and ethylene glycol solution of barium sulfate is 1:0.5:0.09.

[0067] Preparation method of modified seaweed fiber, comprising the following steps: subject 70 kg of seaweed fiber to oxygen plasma treatment under the conditions of a temperature of 47 °C, a vacuum degree of 820 Pa, and a plasma power supply of 270 W, then immerse it in a graphene modified solution, add 5 kg of glutaraldehyde and 10 kg of nano-activated carbon, stir at a temperature of 92 °C for 2.5 h, and dry to obtain the modified seaweed fiber.

[0068] Graphene modified solution: Disperse 10 kg of graphene in 100 L of deionized water, add 3 kg of chitosan, 6 kg of wheat straw powder, 2 kg of silane coupling agent kh550, and 1 kg of p-toluenesulfonic acid catalyst, stir at a temperature of 82 °C for 37 min, and perform ultrasonic dispersion for 26 min to obtain the graphene modified solution.

[0069] Example 11 A preparation method of an antibacterial porous polyester DTY composite filament, different from Example 10 in that the mass ratio of waste polyester chips, modified seaweed fiber, and ethylene glycol solution of barium sulfate is 1:0.6:0.08.

[0070] Example 12 A preparation method of an antibacterial porous polyester DTY composite filament, different from Example 10 in that no modified seaweed fiber is added.

[0071] Example 13 A preparation method of an antibacterial porous polyester DTY composite filament, different from Example 10 in that no ethylene glycol solution of barium sulfate is added.

[0072] Example 14 A preparation method of an antibacterial porous polyester DTY composite filament, different from Example 10 in that the mass ratio of waste polyester chips, modified seaweed fiber, and ethylene glycol solution of barium sulfate is 1:0.1:0.3.

[0073] Example 15 A preparation method of an antibacterial porous polyester DTY composite filament, different from Example 10 in that in the preparation method of the modified seaweed fiber, no graphene modified solution is added.

[0074] Example 16 A preparation method of an antibacterial porous polyester DTY composite filament, different from Example 10 in that in the preparation method of the modified seaweed fiber, no nano-activated carbon is added.

[0075] Comparative example Comparative example 1 A preparation method of an antibacterial porous polyester DTY composite filament, different from Example 1 in that no nano-particle modified pearl powder is added.

[0076] Comparative Example 2 A method for preparing an antibacterial porous polyester DTY composite filament, which is different from Example 1 in that the nano-particle modified pearl powder is replaced with an equal amount of pearl powder.

[0077] Performance detection test Perform performance tests on the preparation methods of an antibacterial porous polyester DTY composite filament prepared in Examples 1-16 and Comparative Examples 1-2; Refer to FZ / T 54085-2016 "Flame Retardant Polyester DTY Yarn" to determine the breaking strength and breaking elongation of the examples and comparative examples; Refer to the experimental method of "Determination of Martindale fabric abrasion resistance of textiles - Part 3: Determination of mass loss" in GB / T 21196.3-2007 to detect the examples and comparative examples. Weigh the weight of the sample before the experiment as m1, use a Martindale abrasion tester to conduct abrasion experiments on the sample. After 530 abrasion times, weigh the weight of the sample m2, and calculate the wear rate of the sample = (m1 - m2) / m1 × 100%.

[0078] Use a circular trajectory pilling and fuzzing tester. According to the standard provisions of GB / T 4802.1-2008 "Textiles - Pilling of fabrics", under a pressure of 500 cN, along a circular motion trajectory, first fuzz with a nylon brush, and then interact with a fabric abrasive to rub and pill. Fuzz 60 times and pill 60 times, and visually describe and evaluate the pilling and fuzzing performance of the sample; the rating ranges from 1-5 levels, with level 1 being the worst (the most serious pilling and fuzzing), and level 5 being the best (no pilling phenomenon). Half-levels are allowed. To better compare the differences in pilling and fuzzing performance between fabrics, 0.1 is used as the minimum precision in actual rating.

[0079] The disperse dye Disperse Red 167 is used for dyeing. Use a high-temperature and high-pressure machine to dye the DTY composite filament. The dye dosage is 2.5%, the dosage of dispersant AEO-7 is 1.7 g / L, the pH value is 6.5, the bath ratio is 1:78, dye at 60 °C, heat up uniformly at a speed of 1.5 °C / min to 115 °C, keep the temperature constant for dyeing for 35 min, cool down uniformly at a speed of 2.5 °C to 45 °C, wash and dry; the percentage of dye uptake is determined by the residual liquid colorimetric method. Absorb the original dyeing solution and the dyeing residual solution, add N, N-2 methylformamide (DMF) and distilled water. The volume ratio of DMF to water in the test dye solution is 40 / 60. The absorbance of the dye solution is measured by a 721-type ultraviolet-visible spectrophotometer. Calculate according to the percentage of dye uptake = (1 - absorbance of the residual liquid - absorbance of the pre-dyeing solution) * 100%. The test results are shown in Table 1.

[0080] Table 1 Test data of examples and comparative examples As can be seen from Table 1, an antibacterial porous polyester DTY composite filament prepared in Examples 1-2 of the present application has good mechanical properties and wear resistance. Among them, the breaking strength of Example 1 is 6.98 cN / dtex, the elongation at break is 20.96%, the wear rate is 0.21%, the pilling resistance rating is 4.2, and the dye uptake rate is 93.6%. It shows that the prepared antibacterial porous polyester DTY composite filament has good mechanical properties, wear resistance, pilling resistance and dyeability. With the cooperation of various components, the obtained antibacterial porous polyester DTY composite filament has good wear resistance, high strength and elasticity, making the composite filament not prone to wear, reducing the wear rate and prolonging the service life of the composite filament.

[0081] In the preparation methods of the nano-particle modified pearl powder in Examples 3-5, modified loofah sponge, metal skeleton material and xanthan gum are not added respectively. In Examples 6-7, the mass ratios of pearl powder, modified loofah sponge, metal skeleton material and xanthan gum are changed. As can be seen from Table 1, the test results of the breaking strength, elongation at break, wear rate, pilling resistance rating and dye uptake rate in Examples 3-5 are significantly worse than those in Examples 1-2 and Example 6, while the corresponding performance tests in Example 7 are better than those in Examples 3-5 but worse than those in Examples 1-2. It shows that the modified loofah sponge has a natural three-dimensional porous structure and can adsorb on the surface of pearl powder particles. The metal skeleton material can be embedded in the structures of pearl powder and modified loofah sponge, which not only increases the adhesion between pearl powder and modified loofah sponge, but also improves the mechanical strength, wear resistance and stability of pearl powder. Xanthan gum makes pearl powder, modified loofah sponge and metal skeleton material adhere tightly, further increasing the mechanical properties, biocompatibility, antibacterial properties and antioxidant properties of pearl powder, which helps to improve the corresponding properties of the composite filament subsequently.

[0082] In the preparation methods of the modified loofah sponge in Examples 8-9, konjac gum and nano-nickel are not added respectively. As can be seen from Table 1, the test results of the breaking strength, elongation at break, wear rate, pilling resistance rating and dye uptake rate in Examples 8-9 are significantly better than those in Example 3 but worse than those in Examples 1-2. It shows that nano-nickel has good mechanical properties and antibacterial properties and can be loaded in the pores of the post-treated loofah sponge, increasing the mechanical strength and antibacterial properties of the post-treated loofah sponge. Konjac gum has a good wrapping and stabilizing effect, making nano-nickel stably adhere to the loofah sponge structure, increasing the adsorption, mechanical properties and antibacterial properties of the modified loofah sponge, and subsequently improving the corresponding properties of the nano-particle modified pearl powder.

[0083] Example 10-11 pre-treats waste polyester chips. It can be seen from Table 1 that the test results of the breaking strength, elongation at break, wear rate, pilling resistance rating, and dye uptake rate of Examples 10-11 are significantly better than those of Examples 1-2, indicating that the pre-treated waste polyester chips have excellent mechanical properties, wear resistance, thermal stability, and antioxidant properties, thereby improving the comprehensive properties of the antibacterial porous polyester DTY composite filaments.

[0084] In the pre-treatment methods of Examples 12-13, the ethylene glycol solutions of modified seaweed fiber and barium sulfate are not added respectively. In Example 14, the mass ratios of waste polyester chips, modified seaweed fiber, and the ethylene glycol solution of barium sulfate are changed. It can be seen from Table 1 that the test results of the breaking strength, elongation at break, wear rate, pilling resistance rating, and dye uptake rate of Examples 12-13 are significantly worse than those of Examples 10-11, but better than those of Examples 1-2, while the test results of Example 14 are significantly better than those of Examples 12-13, but worse than those of Examples 10-11. It shows that the modified seaweed fiber has good flexibility and biocompatibility, can be loaded on the surface and pores of the waste polyester chips, and improves the mechanical properties of the waste polyester chips. The ethylene glycol solution of barium sulfate has good wear resistance and mechanical properties, can coat the waste polyester chips, make the waste polyester chips adhere tightly to the modified seaweed fiber, increase the mechanical properties, flexibility, and wear resistance of the waste polyester chips, and subsequently improve the corresponding properties of the antibacterial porous polyester DTY composite filaments.

[0085] In the preparation methods of Examples 15-16, the graphene modification solution and nano-activated carbon are not added respectively. It can be seen from Table 1 that the test results of the breaking strength, elongation at break, wear rate, pilling resistance rating, and dye uptake rate of Examples 15-16 are significantly worse than those of Examples 10-11, but better than those of Example 12. It shows that when the seaweed fiber is impregnated in the graphene modification solution, the active components in the solution can be loaded on the surface of the seaweed fiber. By adding glutaraldehyde and nano-activated carbon, glutaraldehyde reacts with the active groups in the seaweed fiber and the graphene modification solution to form a stable network structure, which is further loaded in the seaweed fiber structure, enhancing the stability and mechanical properties of the fiber. The obtained modified seaweed fiber has excellent wear resistance, antibacterial properties, and mechanical properties, and subsequently improves the corresponding properties of the composite filaments.

[0086] In Comparative Example 1, no nanoparticle-modified pearl powder was added. In Comparative Example 2, the nanoparticle-modified pearl powder was replaced with an equal amount of pearl powder. As can be seen from Table 1, the test results of the breaking strength, elongation at break, wear rate, pilling resistance rating, and dye uptake rate of Comparative Example 1 were significantly worse than those of Examples 1-2. The corresponding test results of Comparative Example 2 were worse than those of Examples 1-2 but better than those of Comparative Example 1. It shows that the nanoparticle-modified pearl powder enhances the antibacterial properties, mechanical properties, and wear resistance of the composite filament, and improves the surface hardness and wear resistance of the composite filament; the nanoparticle-modified pearl powder of the present application has good mechanical properties, wear resistance, and stability, thereby improving the mechanical properties of the composite filament and keeping the composite from being easily worn during use.

[0087] This specific embodiment is only an explanation of the present application and does not limit the present application. Those skilled in the art can make modifications without creative contributions to this embodiment according to needs after reading this specification, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A preparation method of an antibacterial porous polyester DTY composite filament, characterized in that, It includes the following steps: (1) Mix 60 - 65 parts of waste polyester chips, 2 - 4 parts of antibacterial agent, 6 - 8 parts of diphenylsilanediol, 18 - 25 parts of nanoparticle - modified pearl powder, 5 - 9 parts of zinc acetate, and 12 - 16 parts of polyethylene glycol, then perform melt extrusion, cooling, oiling, and heat setting to obtain polyester POY filaments; (2) Heat - stretch, false - twist, and heat - set the polyester POY filaments obtained in step (1) to obtain antibacterial porous polyester DTY composite filaments.

2. The preparation method of an antibacterial porous polyester DTY composite filament according to claim 1, characterized in that, The pretreatment method of the waste polyester chips includes the following steps: (1) Crush the waste polyester chips to obtain fragments with a size of 0.5 - 1 mm, disperse the fragments in a sodium hydroxide solution, stir for 1 - 2 h, wash with water, then disperse in a cleaning solution, clean at a rotation speed of 400 - 450 rpm for 30 - 35 min, and dry to obtain cleaned fragments; (2) Disperse the modified seaweed fiber in deionized water, add the cleaned fragments obtained in step (1), 5 - sodium sulfoisophthalate, and pentaerythritol tetra, stir at a temperature of 60 - 65 °C for 20 - 25 min, and filter to obtain a mixture; (3) Spray an ethylene glycol solution of barium sulfate on the surface of the mixture in step (2), and dry to obtain pretreated waste polyester chips; The cleaning solution includes benzyl alcohol, alkylbenzene sulfonate, polyoxyethylene styrenated phenyl ether, and amino acid - type surfactant.

3. The preparation method of an antibacterial porous polyester DTY composite filament according to claim 3, characterized in that, The mass ratio of the waste polyester chips, modified seaweed fiber, and ethylene glycol solution of barium sulfate is 1:0.5 - 0.6:0.08 - 0.

09.

4. The preparation method of an antibacterial porous polyester DTY composite filament according to claim 3, characterized in that, The preparation method of the modified seaweed fiber includes the following steps: Perform oxygen plasma treatment on the seaweed fiber at a temperature of 45 - 48 °C, a vacuum degree of 800 - 850 Pa, and a plasma power supply of 260 - 280 W, then immerse it in a graphene - modified solution, add glutaraldehyde and nano - activated carbon, stir at a temperature of 90 - 95 °C for 2 - 3 h, and dry to obtain the modified seaweed fiber.

5. Graphene - modified solution: Disperse graphene in deionized water, add chitosan, wheat straw powder, silane coupling agent, and p - toluenesulfonic acid catalyst, stir at a temperature of 80 - 85 °C for 35 - 40 min, and perform ultrasonic dispersion for 25 - 30 min to obtain the graphene - modified solution.

6. The preparation method of an antibacterial porous polyester DTY composite filament according to claim 1, characterized in that, The preparation method of the nanoparticle - modified pearl powder includes the following steps: (1) Sieve the pearl powder, disperse it in acetone, add aluminum distearate and lauroyl lysine, stir for 2 - 3 h, filter, wash, and dry to obtain treated pearl powder; (2) Disperse the modified loofah sponge in deionized water, add the treated pearl powder obtained in step (1), metal framework material, xanthan gum, and sodium hexametaphosphate, stir at 60 - 65 °C for 1 - 2 h, and dry to obtain nanoparticle - modified pearl powder.

7. The preparation method of an antibacterial porous polyester DTY composite filament according to claim 6, characterized in that, The mass ratio of the pearl powder, modified loofah sponge, metal framework material, and xanthan gum is 1:0.4 - 0.5:0.2 - 0.3:0.1 - 0.

2.

8. The preparation method of an antibacterial porous polyester DTY composite filament according to claim 6, characterized in that, The preparation method of the modified loofah sponge includes the following steps: Cut the loofah sponge into pieces, disperse it in a sodium hydroxide solution, heat it at 70 - 75 °C for 2 - 3 h, wash it with water and dry it to obtain the pretreated loofah sponge; Disperse the pretreated loofah sponge in a citric acid solution, add cocamidopropyl betaine, stir evenly, wash it with deionized water and dry it to obtain the post-treated loofah sponge; Disperse the post-treated loofah sponge in deionized water, add konjac gum and nano-nickel, stir at 70 - 75 °C for 2 - 3 h, and dry it to obtain the modified loofah sponge.

9. The preparation method of an antibacterial porous polyester DTY composite filament according to claim 1, characterized in that In step (1), the temperature for melt extrusion is 250 - 260 °C, the extrusion pressure is 50 - 60 MPa, and the temperature for heat setting is 120 - 125 °C.

10. The preparation method of an antibacterial porous polyester DTY composite filament according to claim 1, characterized in that, In step (2), the temperature for heating and stretching is 200 - 210 °C, the draw ratio is 1.03 - 1.06; the fineness of the single filament of the DTY composite filament is 3 - 4 dtex.

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