Extinction PET fiber chip spinning preparation process

By adding modified coconut shell, nanosilver, nanosilica and other components to the precipitation PET fiber preparation process and adopting specific spinning steps, the problem of poor mechanical properties of precipitation PET fibers is solved, significantly improving the tensile strength, wear resistance and antibacterial properties of the fibers, and extending the service life.

CN119956520APending Publication Date: 2025-05-09ZHEJIANG HENGBAIHUA CHEMICAL FIBER CO LTD
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Patent Information

Application Number
CN202510249200.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-04
Publication Date
2025-05-09

AI Technical Summary

Technical Problem

The mechanical properties of the extinct PET fibers are poor and are prone to fracture and deformation, which affects their performance during use.

Method used

A homogenized PET fiber slice spinning preparation process is adopted to fully mix the hypogenized PET slices, modified coconut shells, nanosilver, nanosilica, masterbatches, triethyl phosphate, modified diatomaceous earth and antioxidants to form a uniform mixture, and fibers are prepared by melt extrusion, spinning, cooling, oiling, stretching and shaping and winding.

Benefits of technology

It significantly improves the tensile strength, wear resistance, antibacterial properties and thermal stability of the fiber, so that the fiber maintains good performance in high temperature environments and extends the service life of the fiber.

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Abstract

The invention belongs to the technical field of fiber preparation, and particularly discloses a matt PET fiber chip spinning preparation technology. The matt PET fiber chip spinning preparation process comprises the following steps: (1) uniformly mixing matt PET chips, modified coconut shells, nano silver, nano silicon dioxide, color master batches, triethyl phosphate, modified diatomite and an antioxidant, and carrying out melt extrusion to obtain a melt; and (2) spinning, cooling, oiling, stretching, shaping and winding the melt with the crimpness of 9-13% to obtain the extinction PET fiber. The delustering PET fiber prepared in the invention has good strength, wear resistance and antibacterial property, the components and steps jointly form the high-performance and high-durability fiber, and it is ensured that the delustering PET fiber is not prone to fracture and deformation in the use process.
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Description

Technical Field

[0001] The present application relates to the technical field of fiber preparation, and in particular to a matte PET fiber chip spinning preparation process. Background Art

[0002] Matt PET fiber is a fiber made by adding a matting agent (such as titanium dioxide) to polyethylene terephthalate (PET). The difference in refractive index between the matting agent and the PET matrix causes light to scatter on the fiber surface, reducing the glossiness. It is widely used in clothing fabrics, household textiles, industrial fabrics and other fields.

[0003] The existing preparation process usually includes mixing PET chips with a matting agent and then preparing fibers through a melt spinning process. During the melt spinning process, the PET melt is extruded through a spinneret to form fibers. After spinning, the fibers usually need to be stretched, shaped, and oiled to obtain finished fibers in order to improve their mechanical properties and processing properties.

[0004] By adding matting agent titanium dioxide to PET, a high matting effect can be achieved, giving the fiber a better visual effect. However, the matting agent will weaken the orientation of the PET molecular chain, resulting in reduced strength, which in turn affects the mechanical properties of the fiber, making it more susceptible to breakage and deformation during use. Summary of the invention

[0005] In order to improve the problem of poor mechanical properties of matt PET fibers, the present application provides a matt PET fiber chip spinning preparation process.

[0006] The present application provides a matte PET fiber chip spinning preparation process, which adopts the following technical solution: A matte PET fiber chip spinning preparation process, comprising the following steps: (1) mixing matt PET slices, modified coconut shell, nano silver, nano silicon dioxide, masterbatch, triethyl phosphate, modified diatomaceous earth, and antioxidant uniformly, and melt-extruding to obtain a melt; (2) spinning the melt at a spinning temperature of 280-290° C. and a spinning speed of 2800-3000 m / min, cooling, oiling, stretching, shaping and winding, with a curl of 9-13%, to obtain matte PET fibers.

[0007] By adopting the above technical scheme, matt PET slices, modified coconut shells, nano titanium dioxide, nano silicon dioxide, masterbatch, triethyl phosphate, modified diatomaceous earth, and antioxidant are fully mixed to form a uniform mixture. Matt PET slices are the main raw material for preparing PET fibers. As the main body of the fiber, they have high strength, high modulus and good wear resistance. Moreover, the matt PET slices contain matt titanium dioxide, which can effectively scatter light, reduce the glossiness of the fiber, and make it have a matt effect. Modified coconut shells have high hardness and strength, can be embedded in the structure of matt PET slices, significantly improve the mechanical properties such as tensile strength and wear resistance of the fiber, as well as heat resistance and thermal stability, so that the fiber maintains good performance under high temperature environment. Nanosilver has excellent antibacterial properties, can effectively inhibit the growth of bacteria, fungi and viruses, and improve the antibacterial properties of the fiber. Nano-silicon dioxide has stable chemical properties, small particle size, and large specific surface area, which can improve the mechanical properties of the fiber such as tensile strength and modulus. It also has high hardness and wear resistance, which can improve the wear resistance of the fiber and make it less prone to wear during use.

[0008] Masterbatch gives the fiber a specific color, providing the fiber with a uniform and stable color to meet the color requirements of the fiber in different application fields. Triethyl phosphate, as a plasticizer, can improve the flexibility and processing performance of the fiber. It also has good heat resistance and can improve the heat resistance and thermal stability of the fiber. Modified diatomaceous earth has good adsorption properties, mechanical properties and dispersibility, which allows the various components to be mixed evenly, and also improves the dimensional stability of the fiber, reducing the shrinkage and deformation of the fiber during processing and use. Antioxidants can prevent oxidative degradation of the fiber during processing and use, maintain the stability of the fiber's performance, delay the aging process of the fiber, and extend the service life of the fiber. Multiple components are mixed together to improve the mechanical properties, wear resistance and stability of the fiber.

[0009] The mixture is melt-extruded to obtain a melt, which is spun to form fibers. The spun fibers are cooled to solidify rapidly to ensure the stability and uniformity of the fibers. The cooled fibers are oiled to improve the lubricity and bundling properties of the fibers. The oiled fibers are stretched and heat-set to improve the strength and stability of the fibers. The set fibers are wound to form matte PET fibers to ensure the uniformity and stability of the fibers.

[0010] Preferably, the preparation method of the modified coconut shell comprises the following steps: (1) washing and crushing the coconut shell, dispersing it in a sodium hydroxide aqueous solution, soaking it at a temperature of 70-75° C. for 1-2 h, washing it with water, dispersing it in a silane coupling agent KH550 aqueous solution, stirring it for 25-30 min, filtering it, and drying it to obtain pretreated coconut shell powder; (2) dispersing the pretreated coconut shell powder in step (1) in deionized water, adding modified oak powder, malic acid, and sodium dodecylbenzene sulfonate, stirring at a stirring rate of 500-550 r / min for 1-2 h, filtering, and drying to obtain a mixture; (3) Spraying chitosan-sodium alginate-zinc oxide solution onto the surface of the mixture in step (2), stirring evenly, and drying to obtain modified coconut shell.

[0011] By adopting the above technical solution, the coconut shell is treated with sodium hydroxide aqueous solution to remove non-cellulose substances on the surface of the coconut shell and make the surface rougher, which is conducive to the subsequent combination with the coupling agent. The silane coupling agent KH550 is used for surface modification of coconut shell powder, which can react with the hydroxyl groups on the surface of coconut shell powder to form a complex, thereby improving the dispersibility of coconut shell powder and making the coconut shell powder evenly dispersed in the solvent.

[0012] Modified oak powder has good mechanical properties and heat resistance, and can be loaded on the surface or pores of pretreated coconut shell powder, improving the mechanical properties and heat resistance of modified coconut shell, and enhancing the strength and stability of the fiber. Malic acid adjusts the pH value of the system, allowing the pretreated coconut shell powder and modified oak powder to combine better. The carboxylic acid group in malic acid esterifies and cross-links with the -OH on the surface of pretreated coconut shell powder / modified oak powder to form a three-dimensional network, further increasing the structural strength of the mixture. Sodium dodecylbenzene sulfonate can reduce the surface tension of the solution, improve the dispersibility of pretreated coconut shell powder and its modified oak powder in water, ensure the uniformity of the mixture, and make each component evenly loaded.

[0013] Spray chitosan-sodium alginate-zinc oxide solution on the surface of the mixture. The chitosan-sodium alginate-zinc oxide solution can form a uniform coating on the surface of the mixture, so that the coconut shell powder and the modified oak powder are tightly bonded, further increasing the mechanical properties and functionality of the modified coconut shell, and improving the tensile modulus, tensile strength, toughness and other mechanical properties of the modified coconut shell.

[0014] Preferably, the mass ratio of the coconut shell, the modified oak powder and the chitosan-sodium alginate-zinc oxide solution is 1:0.5-0.6:0.2-0.3.

[0015] By adopting the above technical scheme, the mass ratio of coconut shell, modified oak powder and chitosan-sodium alginate-zinc oxide solution is further limited within a certain range, thereby increasing the comprehensive performance of modified coconut shell. After pretreatment, coconut shell has high hardness and strength, which can significantly improve the mechanical properties, heat resistance and thermal stability of the fiber, such as tensile strength and wear resistance. Modified oak powder has high flexibility and elasticity, which can significantly improve the mechanical properties of the fiber, such as tensile strength and wear resistance. Modified oak powder can be loaded in the pretreated coconut shell structure to increase the structural strength and wear resistance of the modified coconut shell. Chitosan-sodium alginate-zinc oxide solution is sprayed on the surface of coconut shell to form a uniform coating, which can further enhance the mechanical properties and functionality of the fiber, improve the mechanical properties, thermal stability and chemical stability of the prepared modified coconut shell, and improve the durability and application range of the fiber.

[0016] Preferably, the preparation method of the modified oak powder comprises the following steps: crushing the oak, dispersing it in an ethanol aqueous solution, heating and refluxing extraction at 80-85°C to obtain a crude oak extract, concentrating and drying to obtain oak powder; dispersing the oak powder in deionized water, adding alkali-free glass fiber, nanocellulose and sodium silicate, stirring at a temperature of 70-75°C for 2-3h, and drying to obtain modified oak powder.

[0017] By adopting the above technical scheme, the oak is crushed, heated and refluxed to extract, and the oak powder is obtained, which has good elasticity, wear resistance, flexibility and mechanical properties, and alkali-free glass fiber, nano cellulose and sodium silicate are added. The alkali-free glass fiber has high strength and high modulus, can be loaded in the structure of rubber powder, form a mesh structure, and can significantly improve the tensile strength and stability of the fiber. Nano cellulose has good flexibility and elasticity, forms a network structure with oak powder and alkali-free glass fiber, increases the mechanical properties and wear resistance of the system, and makes it difficult to break and damage during use. Sodium silicate has good bonding properties, can bond oak powder, alkali-free glass fiber and nano cellulose together, form a uniform composite material, and improve the uniformity and stability of the fiber. The modified oak powder obtained has good mechanical properties, wear resistance and thermal stability.

[0018] Preferably, the method for preparing the modified diatomite comprises the following steps: (1) dispersing diatomaceous earth in a hydrochloric acid solution, stirring for 1-2 hours, washing with water, drying, calcining at 450-500° C. for 1-2 hours, and sieving to obtain pretreated diatomaceous earth; (2) Dispersing the modified polyethylene fiber in ethanol, adding the pretreated diatomaceous earth in step (1), ultrasonicating for 2-3 hours, then adding polyvidone and Tween-20, stirring for 4-5 hours, and drying to obtain modified diatomaceous earth.

[0019] By adopting the above technical scheme, the diatomite is pretreated with a hydrochloric acid solution, the hydrochloric acid solution erodes the surface of the diatomite to a certain extent and removes some surface impurities, thereby increasing the surface roughness and specific surface area of ​​the diatomite, increasing the adsorption capacity of the diatomite, and facilitating the subsequent mixing of the diatomite with other components. Roasting can further remove organic impurities in the diatomite and make its structure more stable. The temperature range of 450-500°C can ensure that the structure of the diatomite is not destroyed, while achieving a good roasting effect. The pretreated diatomite has a porous structure, heat resistance and wear resistance.

[0020] The modified polyethylene fiber is mixed with pretreated diatomaceous earth, and then polyvidone and Tween-20 are added. The modified polyethylene fiber has high strength and toughness, can be loaded in the diatomaceous earth structure, and forms a network structure in the diatomaceous earth structure, so that the modified polyethylene fiber and diatomaceous earth are better combined, which can significantly improve the strength, flexibility and elasticity of diatomaceous earth, and make the diatomaceous earth have better mechanical properties and chemical stability.

[0021] Povidone has good bonding properties and can bond diatomaceous earth and modified polyethylene fibers together to form a uniform composite material, thereby improving the mechanical properties and wear resistance of the modified diatomaceous earth. Tween-20 can reduce the surface tension of the liquid, promote the dispersion and mixing of diatomaceous earth and modified polyethylene fibers, and make the modified polyethylene fibers uniformly loaded in the diatomaceous earth structure. The obtained modified diatomaceous earth has good mechanical properties and chemical stability.

[0022] Preferably, the mass ratio of the diatomaceous earth, the modified polyethylene fiber and the polyvinylpyrrolidone is 1:0.4-0.5:0.1-0.2.

[0023] By adopting the above technical scheme, the mass ratio of diatomite, modified polyethylene fiber and polyvinylpyrrolidone is further limited within a certain range, the obtained modified diatomite has excellent mechanical properties and thermal stability, the diatomite has a large specific surface area and porosity, the modified polyethylene fiber has good strength and toughness, the modified polyethylene fiber can be loaded on the surface and pores of the diatomite, and the mechanical properties of the diatomite are increased. The modified polyethylene fiber and the diatomite form a network structure, and the structural strength and stability of the diatomite are further improved. Polyvinylpyrrolidone has good bonding properties, and can bond the diatomite and the modified polyethylene fiber together, so that the modified polyethylene fiber is stably adhered to the surface of the diatomite, and the performance stability of the modified diatomite is increased. The obtained modified diatomite has good mechanical properties, thermal stability and wear resistance.

[0024] Preferably, the preparation method of the modified polyethylene fiber comprises the following steps: mixing polyethylene masterbatch, carbon fiber, polyethylene grafted maleic anhydride compatibilizer, and talcum powder, melt extruding, and spinning to obtain polyethylene fiber; dispersing the polyethylene fiber in a nitric acid solution and soaking it for 1-2 hours, washing it with water, and then dispersing it in deionized water, adding graphene and water-based polyurethane adhesive, stirring it for 2-3 hours, and drying it to obtain modified polyethylene fiber.

[0025] By adopting the above technical solution, polyethylene masterbatch is used as the base polymer to provide the main structure of the fiber, which has good flexibility and chemical stability. The carbon fiber has high strength and high modulus, which can significantly improve the mechanical properties of polyethylene fiber, such as tensile strength and modulus. Polyethylene grafted maleic anhydride compatibilizer can improve the compatibility between polyethylene and carbon fiber, promote the combination of the two, form chemical bonds or physical interactions between polyethylene and carbon fiber, enhance the interface bonding force, and improve the overall performance of the composite material. Talc can be filled in the structure of polyethylene masterbatch, which can improve the mechanical properties of polyethylene fiber, such as tensile strength and wear resistance, and can also improve the dimensional stability and thermal stability of the fiber.

[0026] The polyethylene fiber is treated with nitric acid to chemically treat the fiber surface, increase the surface active groups, and improve the fiber's reactivity and ability to combine with other materials. Graphene and water-based polyurethane adhesive are added. Graphene has excellent mechanical properties and thermal stability, and can be loaded on the surface of polyethylene fibers to increase the tensile strength, modulus, heat resistance and thermal stability of polyethylene fibers. The water-based polyurethane adhesive has good adhesion and can evenly adhere graphene to the surface of polyethylene fibers to form a stable composite material, so that the modified polyethylene fibers have good mechanical properties, flexibility and elasticity, improve the durability and service life of the modified polyethylene fibers, and maintain good performance in various environments.

[0027] Preferably, the antioxidant is selected from a combination of one or more of antioxidant 168, antioxidant 1010, antioxidant 1076, and antioxidant 1222.

[0028] By adopting the above technical solution, the antioxidant can significantly delay or inhibit the oxidation reaction of the fiber during processing and use, prevent the performance degradation and aging of the fiber due to oxidation, maintain the mechanical properties, color and appearance of the fiber, and extend its service life.

[0029] Preferably, the matt PET fiber has a fineness of 6.2-6.5 dtex, a fiber strength of 3.8-4.8 cN / dtex, and an elongation at break of 23.4-27.5%.

[0030] By adopting the above technical solution, the matt PET fiber has good mechanical properties, toughness and spinnability, so that the matt PET fiber shows good durability and reliability in various applications.

[0031] Preferably, the extrusion rotation speed is 300-350 r / min, and the extrusion heating temperature is 190-220°C.

[0032] By adopting the above technical solution, the parameters of each step are further limited, which is helpful to obtain a matte PET fiber with better comprehensive performance.

[0033] In summary, this application has the following beneficial effects: 1. The modified coconut shell in this application has high hardness and strength, and can be embedded in the matte PET slice structure, significantly improving the mechanical properties such as tensile strength and wear resistance of the fiber as well as the heat resistance and thermal stability, so that the fiber maintains good performance in a high temperature environment.

[0034] 2. The modified diatomaceous earth in the present application has good adsorption properties, mechanical properties and dispersibility, so that the various components are mixed evenly, and the dimensional stability of the fiber is improved, and the shrinkage and deformation of the fiber during processing and use are reduced.

[0035] 3. In the present application, matte PET fiber is formed to ensure the uniformity and stability of the fiber, improve the mechanical properties, wear resistance and antibacterial properties of the fiber, and make it less likely to break and deform during use. DETAILED DESCRIPTION

[0036] The present application is further described in detail below with reference to the embodiments.

[0037] The raw materials used in the examples and comparative examples can all be obtained commercially.

[0038] Preparation example of modified coconut shell Preparation Example 1-1 The preparation method of modified coconut shell comprises the following steps: (1) 70 kg of coconut shells were washed and crushed to 200 mesh, then dispersed in 90 L of 12% sodium hydroxide aqueous solution, soaked at 73° C. for 1.5 h, washed with water, then dispersed in 95 L of 0.3% silane coupling agent KH550 aqueous solution, stirred for 28 min, filtered and dried to obtain pretreated coconut shell powder; (2) dispersing the pretreated coconut shell powder in step (1) in 180 L of deionized water, adding modified oak powder, 10 kg of malic acid, and 8 kg of sodium dodecylbenzene sulfonate, stirring at a stirring rate of 540 r / min for 1.6 h, filtering, and drying to obtain a mixture; (3) Spraying chitosan-sodium alginate-zinc oxide solution onto the surface of the mixture in step (2), stirring evenly, and drying to obtain modified coconut shell.

[0039] Disperse 20 kg of chitosan in 20 L of 6% acetic acid aqueous solution, add 6 kg of sodium alginate, stir evenly to obtain a chitosan solution-sodium alginate solution, mix the chitosan solution-sodium alginate solution with 3 kg of zinc oxide, stir evenly to obtain a chitosan-sodium alginate-zinc oxide solution, and take the required amount for preparing modified coconut shell.

[0040] The mass ratio of coconut shell, modified oak powder and chitosan-sodium alginate-zinc oxide solution is 1:0.5:0.3.

[0041] The preparation method of modified oak powder comprises the following steps: crushing 260 kg of oak, dispersing it in 960 L of 65% ethanol aqueous solution, heating and refluxing extraction at 82° C. to obtain a crude oak extract, concentrating and drying to obtain oak powder; dispersing the oak powder in 90 L of deionized water, adding 11 kg of alkali-free glass fiber, 5 kg of nanocellulose and 8 kg of sodium silicate, stirring at 73° C. for 3 hours, and drying to obtain modified oak powder.

[0042] Preparation Example 1-2 The difference from Preparation Example 1-1 is that in step (2), no modified oak powder is added.

[0043] Preparation Example 1-3 The difference from Preparation Example 1-1 is that in step (3), no chitosan-sodium alginate-zinc oxide solution is added.

[0044] Preparation Example 1-4 The difference from Preparation Example 1-1 is that the mass ratio of coconut shell, modified oak powder and chitosan-sodium alginate-zinc oxide solution is 1:0.6:0.2.

[0045] Preparation Example 1-5 The difference from Preparation Example 1-1 is that the mass ratio of coconut shell, modified oak powder and chitosan-sodium alginate-zinc oxide solution is 1:0.1:0.6.

[0046] Preparation Example 1-6 The difference from Preparation Example 1-1 is that, in the preparation method of the modified oak powder, no alkali-free glass fiber is added.

[0047] Preparation Example 1-7 The difference from Preparation Example 1-1 is that no sodium silicate is added in the preparation method of the modified oak powder.

[0048] Preparation example of modified diatomite Preparation Example 2-1 The preparation method of modified diatomite comprises the following steps: (1) 40 kg of diatomaceous earth was dispersed in 66 L of 8% hydrochloric acid solution, stirred for 1.5 h, washed with water, dried, calcined at 470° C. for 1.6 h, and passed through a 100-mesh sieve to obtain pretreated diatomaceous earth; (2) Dispersing the modified polyethylene fiber in 100 L of ethanol, adding the pretreated diatomaceous earth in step (1), ultrasonicating for 3 h, then adding povidone and 3 kg of Tween-20, stirring for 4.5 h, and drying to obtain modified diatomaceous earth.

[0049] The mass ratio of diatomaceous earth, modified polyethylene fiber and povidone is 1:0.4:0.2.

[0050] The preparation method of modified polyethylene fiber comprises the following steps: mixing 35kg polyethylene masterbatch, 11kg carbon fiber, 3kg polyethylene grafted maleic anhydride compatibilizer and 7kg talcum powder at a temperature of 190°C, melt extruding at a melt extrusion temperature of 220°C, and spinning to obtain polyethylene fiber; dispersing the polyethylene fiber in 60L of 12% nitric acid solution by mass, soaking for 1.7h, washing with water, and then dispersing in 120L deionized water, adding 10kg graphene and 6kg water-based polyurethane adhesive, stirring for 2.5h, and drying to obtain modified polyethylene fiber; the water-based polyurethane adhesive is purchased from Shandong Tengyuan Chemical Technology Co., Ltd.

[0051] Preparation Example 2-2 The difference from Preparation Example 2-1 is that in step (2), no modified polyethylene fiber is added.

[0052] Preparation Example 2-3 The difference from Preparation Example 2-1 is that in step (2), no povidone is added.

[0053] Preparation Example 2-4 The difference from Preparation Example 2-1 is that the mass ratio of diatomaceous earth, modified polyethylene fiber and povidone is 1:0.5:0.1.

[0054] Preparation Example 2-5 The difference from Preparation Example 2-1 is that the mass ratio of diatomaceous earth, modified polyethylene fiber and povidone is 1:0.11:0.56.

[0055] Preparation Example 2-6 The difference from Preparation Example 2-1 is that graphene is not added in the preparation method of the modified polyethylene fiber.

[0056] Preparation Example 2-7 The difference from Preparation Example 2-1 is that no water-based polyurethane adhesive is added in the preparation method of the modified polyethylene fiber. Example

[0057] Example 1 A matte PET fiber chip spinning preparation process, comprising the following steps: (1) 100 kg of matte PET chips, 35 kg of modified coconut shells, 10 kg of nano-silver, 5 kg of nano-silicon dioxide, 3 kg of masterbatch, 4 kg of triethyl phosphate, 30 kg of modified diatomaceous earth, and 3 kg of antioxidant are mixed uniformly, melt-extruded, and obtain a melt; (2) The melt is spun at a spinning temperature of 290° C. and a spinning speed of 3000 m / min, and then cooled, oiled, stretched, shaped and wound with a curl of 9% to obtain matte PET fibers.

[0058] The antioxidant is selected from antioxidant 168, the extrusion rotation speed is 350r / min, and the extrusion heating temperature is 220°C.

[0059] The modified coconut shell was prepared by using Preparation Example 1-1; the modified diatomaceous earth was prepared by using Preparation Example 2-1.

[0060] Example 2 A matte PET fiber chip spinning preparation process, which differs from Example 1 in that it comprises the following steps: (1) 98 kg of matte PET chips, 33 kg of modified coconut shells, 9 kg of nano-silver, 6 kg of nano-silicon dioxide, 4 kg of masterbatch, 3 kg of triethyl phosphate, 29 kg of modified diatomaceous earth, and 2 kg of antioxidant were mixed and melt-extruded to obtain a melt; (2) The melt is spun at a spinning temperature of 280° C. and a spinning speed of 2800 m / min, and then cooled, oiled, stretched, shaped and wound with a curl of 13% to obtain matte PET fibers.

[0061] The extrusion speed was 300 r / min, and the extrusion heating temperature was 190°C.

[0062] Example 3 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified coconut shell is prepared using Preparation Example 1-2.

[0063] Example 4 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified coconut shell is prepared using Preparation Examples 1-3.

[0064] Example 5 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified coconut shell is prepared using Preparation Examples 1-4.

[0065] Example 6 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified coconut shell is prepared using Preparation Examples 1-5.

[0066] Example 7 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified coconut shell is prepared using Preparation Examples 1-6.

[0067] Example 8 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified coconut shell is prepared using Preparation Examples 1-7.

[0068] Example 9 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified diatomaceous earth is prepared using Preparation Example 2-2.

[0069] Example 10 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified diatomaceous earth is prepared using Preparation Example 2-3.

[0070] Embodiment 11 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified diatomaceous earth is prepared using Preparation Examples 2-4.

[0071] Example 12 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified diatomaceous earth is prepared using Preparation Examples 2-5.

[0072] Example 13 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified diatomaceous earth is prepared using Preparation Examples 2-6.

[0073] Embodiment 14 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified diatomaceous earth is prepared using Preparation Examples 2-7.

[0074] Comparative Example Comparative Example 1 A matte PET fiber chip spinning preparation process, which differs from Example 1 in that modified coconut shell is not added.

[0075] Comparative Example 2 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified coconut shell is replaced by an equal amount of coconut shell.

[0076] Comparative Example 3 A process for spinning and preparing matt PET fiber chips, which differs from Example 1 in that modified diatomaceous earth is not added.

[0077] Comparative Example 4 A matte PET fiber chip spinning preparation process, which is different from Example 1 in that the modified diatomaceous earth is replaced by an equal amount of diatomaceous earth.

[0078] Performance testing The matt PET fiber chip spinning preparation process prepared in Examples 1-14 and Comparative Examples 1-4 was subjected to performance testing; The fiber fineness, strength and elongation at break were tested according to GB / T 14337-2008 test method for tensile properties of chemical fiber staple fibers; the matte PET fibers prepared in the examples and comparative examples were woven on a loom to obtain fabrics, and the fabrics were tested for wear resistance according to GB / T21196.3-2007 "Determination of the abrasion resistance of textile fabrics by the Martindale method - Part 3: Determination of mass loss"; the antibacterial rate of matte PET fibers against Escherichia coli and Staphylococcus aureus was tested with reference to standard GB / T 20944.3-2008; the test results are shown in Table 1.

[0079] Table 1 Test data of embodiments and comparative examples It can be seen from Table 1 that the matt PET fibers prepared in Examples 1-2 of the present application have good mechanical properties and wear resistance, wherein the fiber fineness of Example 1 is 6.3 dtex, the fiber strength is 4.8 cN / dtex, the elongation at break is 27.5%, the Escherichia coli is 98.9%, the Staphylococcus aureus is 98.8%, and the wear resistance index is 0.95 mg / time. This indicates that the matt PET fibers prepared in the present application have good mechanical properties, mechanical strength, antibacterial properties and wear resistance, and the various components and processing steps cooperate with each other to jointly improve the wear resistance, antibacterial properties and mechanical properties of the matt PET fibers, thereby making the matt PET fibers less likely to break and deform during use.

[0080] In the preparation method of modified coconut shell of Examples 3-4, modified oak powder and chitosan-sodium alginate-zinc oxide solution were not added respectively. In Examples 5-6, the mass ratio of coconut shell, modified oak powder and chitosan-sodium alginate-zinc oxide solution was changed. As can be seen from Table 1, the test results of fiber strength, elongation at break and wear resistance index of Examples 3-4 were significantly worse than those of Examples 1-2 and Example 5. The test results of Escherichia coli and Staphylococcus aureus of Example 3 were basically unchanged, and the test results of Escherichia coli and Staphylococcus aureus of Example 4 were significantly lower than those of Example 1-2 and Example 5. The results are worse than those of Examples 1-2 and 5, while the performance tests of fiber strength, elongation at break, Escherichia coli, Staphylococcus aureus, and wear resistance index of Example 6 are better than those of Examples 3-4, but worse than those of Examples 1-2 and 5, indicating that the modified oak powder has higher flexibility and elasticity, and is loaded in the pretreated coconut shell structure to increase the structural strength and wear resistance of the modified coconut shell; the chitosan-sodium alginate-zinc oxide solution is sprayed on the surface of the coconut shell to form a uniform coating, which can further enhance the mechanical properties and antibacterial properties of the fiber.

[0081] In the preparation method of the modified oak powder in Examples 7-8, alkali-free glass fiber and sodium silicate are not added respectively. As can be seen from Table 1, the test results of Escherichia coli and Staphylococcus aureus remain basically unchanged, but the test results of fiber strength, elongation at break and wear resistance index are significantly better than those in Example 3, but worse than those in Examples 1-2, indicating that the alkali-free glass fiber has high strength and high modulus, can be loaded in the structure of rubber powder to form a network structure, and improve the tensile strength and stability of the fiber; sodium silicate has good bonding properties, and can bond oak powder, alkali-free glass fiber and nanocellulose together to form a uniform composite material, thereby improving the mechanical properties, wear resistance and stability of the fiber.

[0082] In the preparation methods of modified diatomite in Examples 9-10, modified polyethylene fiber and polyvinylpyrrolidone are not added respectively. In Examples 11-12, the mass ratio of diatomite, modified polyethylene fiber and polyvinylpyrrolidone is changed. As can be seen from Table 1, the test results of fiber strength, elongation at break and wear resistance index of Examples 9-10 are significantly worse than those of Examples 1-2 and Example 11. The test results of Escherichia coli and Staphylococcus aureus in Example 10 are basically unchanged. The test results of Escherichia coli and Staphylococcus aureus in Example 9 are worse than those in Examples 1-2 and Example 11, while the test results of fiber strength, elongation at break and wear resistance index in Example 12 are significantly worse than those in Example 1-2 and Example 11. The performance tests of dimensional strength, elongation at break, Escherichia coli, Staphylococcus aureus, and wear resistance index are better than those of Examples 9-10, but worse than those of Examples 1-2 and Example 11, indicating that the modified polyethylene fiber has good strength and toughness, and the modified polyethylene fiber can be loaded on the surface and pores of diatomaceous earth to increase the mechanical properties and antibacterial properties of diatomaceous earth; polyvidone has good bonding properties, and can bond diatomaceous earth and modified polyethylene fiber together, thereby increasing the performance stability of the modified diatomaceous earth, and the obtained modified diatomaceous earth has good mechanical properties, thermal stability and wear resistance.

[0083] In the preparation method of the modified polyethylene fiber of Examples 13-14, graphene and water-based polyurethane adhesive are not added respectively. It can be seen from Table 1 that the test results of Escherichia coli and Staphylococcus aureus in Example 14 are basically unchanged, and the test results of Escherichia coli and Staphylococcus aureus in Example 13 are deteriorated, but the test results of fiber strength, elongation at break and wear resistance index of Examples 13-14 are significantly better than those of Example 9, but worse than those of Examples 1-2, indicating that graphene has excellent mechanical properties, thermal stability and antibacterial properties, can be loaded on the surface of polyethylene fibers, and increase the tensile strength, antibacterial properties, heat resistance and thermal stability of polyethylene fibers; the water-based polyurethane adhesive has good adhesion, and can evenly adhere graphene to the surface of polyethylene fibers, improve the durability, mechanical properties, antibacterial properties and service life of the modified polyethylene fibers, and enable them to maintain good performance under various environments.

[0084] In Comparative Example 1 and Comparative Example 3, no modified coconut shell or modified diatomaceous earth is added. As can be seen from Table 1, the test results of Escherichia coli, Staphylococcus aureus, fiber strength, elongation at break, and wear resistance index of Comparative Example 1 and Comparative Example 3 are significantly worse than those of Examples 1-2, indicating that the modified coconut shell has higher hardness and strength, can be embedded in the matte PET slice structure, significantly improves the mechanical properties such as tensile strength and wear resistance of the fiber, and antibacterial properties, so that the fiber maintains good performance under high temperature environment; modified diatomaceous earth has good adsorption properties, mechanical properties and dispersibility, so that the various components are mixed evenly, and the mechanical properties, wear resistance and antibacterial properties of the fiber are improved.

[0085] In Comparative Examples 2 and 4, the modified coconut shell is replaced by an equal amount of coconut shell, and the modified diatomaceous earth is replaced by an equal amount of diatomaceous earth. As can be seen from Table 1, the test results of Escherichia coli, Staphylococcus aureus, fiber strength, elongation at break, and wear resistance index of Comparative Examples 2 and 4 are significantly worse than those of Examples 1-2, but better than those of Comparative Examples 1 and 3, indicating that the modified coconut shell and modified diatomaceous earth of the present application have good mechanical properties, wear resistance and antibacterial properties, thereby improving the mechanical properties of the matt PET fiber and keeping the matt PET fiber from being easily broken and deformed during use.

[0086] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A matte PET fiber chip spinning preparation process, characterized in that: The steps include: (1) Evenly mixing matte PET chips, modified coconut shell, nano silver, nano silicon dioxide, masterbatch, triethyl phosphate, modified diatomaceous earth and antioxidant, and melt-extruding to obtain a melt; (2) The melt is spun at a spinning temperature of 280-290° C. and a spinning speed of 2800-3000 m / min, and then cooled, oiled, stretched, shaped and wound with a curl of 9-13% to obtain matte PET fibers.

2. A matte PET fiber chip spinning preparation process according to claim 1, characterized in that: The preparation method of the modified coconut shell comprises the following steps: (1) Washing and crushing the coconut shell, dispersing it in a sodium hydroxide aqueous solution, soaking it at a temperature of 70-75°C for 1-2 hours, washing it with water, dispersing it in a silane coupling agent KH550 aqueous solution, stirring it for 25-30 minutes, filtering it, and drying it to obtain pretreated coconut shell powder; (2) dispersing the pretreated coconut shell powder in step (1) in deionized water, adding modified oak powder, malic acid, and sodium dodecylbenzene sulfonate, stirring at a stirring rate of 500-550 r / min for 1-2 h, filtering, and drying to obtain a mixture; (3) Spraying chitosan-sodium alginate-zinc oxide solution onto the surface of the mixture in step (2), stirring evenly, and drying to obtain modified coconut shell.

3. A matte PET fiber chip spinning preparation process according to claim 2, characterized in that: The mass ratio of the coconut shell, the modified oak powder and the chitosan-sodium alginate-zinc oxide solution is 1:0.5-0.6:0.2-0.

3.

4. A matte PET fiber chip spinning preparation process according to claim 2, characterized in that: The preparation method of the modified oak powder comprises the following steps: crushing oak, dispersing the oak in an ethanol aqueous solution, heating and refluxing extraction at 80-85°C to obtain a crude oak extract, concentrating and drying to obtain oak powder; dispersing the oak powder in deionized water, adding alkali-free glass fiber, nanocellulose and sodium silicate, stirring at a temperature of 70-75°C for 2-3 hours, and drying to obtain the modified oak powder.

5. A matte PET fiber chip spinning preparation process according to claim 1, characterized in that: The preparation method of the modified diatomite comprises the following steps: (1) Dispersing diatomaceous earth in a hydrochloric acid solution, stirring for 1-2 hours, washing with water, drying, calcining at 450-500° C. for 1-2 hours, and sieving to obtain pretreated diatomaceous earth; (2) Dispersing the modified polyethylene fiber in ethanol, adding the pretreated diatomaceous earth in step (1), ultrasonicating for 2-3 hours, then adding polyvidone and Tween-20, stirring for 4-5 hours, and drying to obtain modified diatomaceous earth.

6. A matte PET fiber chip spinning preparation process according to claim 5, characterized in that: The mass ratio of the diatomaceous earth, the modified polyethylene fiber and the polyvidone is 1:0.4-0.5:0.1-0.

2.

7. The process for preparing matt PET fiber chips according to claim 5, characterized in that: The preparation method of the modified polyethylene fiber comprises the following steps: mixing polyethylene masterbatch, carbon fiber, polyethylene grafted maleic anhydride compatibilizer and talcum powder, melt extruding, spinning to obtain polyethylene fiber; dispersing the polyethylene fiber in a nitric acid solution and soaking for 1-2 hours, washing with water, and then dispersing it in deionized water, adding graphene and water-based polyurethane adhesive, stirring for 2-3 hours, and drying to obtain the modified polyethylene fiber.

8. The process for preparing matt PET fiber chips according to claim 1, characterized in that: The antioxidant is selected from one or more combinations of antioxidant 168, antioxidant 1010, antioxidant 1076, and antioxidant 1222.

9. The process for preparing matt PET fiber chips according to claim 1, characterized in that: The matt PET fiber has a fineness of 6.2-6.5 dtex, a fiber strength of 3.8-4.8 cN / dtex, and a breaking elongation of 23.4-27.5%.

10. The process for preparing matt PET fiber chips according to claim 1, characterized in that: The extrusion speed is 300-350r / min, and the extrusion heating temperature is 190-220°C.

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