Preparation method and application of deodorizing, antibacterial, moisture-absorbing and sweat-releasing porous polyester fibers
By mixing the modified deodorizing and antibacterial functional polyester with the modified water-soluble polyester and preparing blended fibers by melt spinning, the problem of poor hydrophilicity and moisture absorption and rapid drying performance of the polyester fibers is solved, and the efficient deodorization and antibacterial properties of the fibers are improved.
Patent Information
- Application Number
- CN202510028857.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-08
- Publication Date
- 2025-06-06
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Polyester fiber has poor hydrophilicity and moisture absorption and quick drying properties, and has poor antibacterial and deodorization properties.
The modified deodorizing and antibacterial functional polyester is mixed with the modified water-soluble polyester in a certain proportion, and blended fibers are prepared by melt spinning. After the blended fibers are dyed at high temperature and high pressure, the modified water-soluble polyester components are dissolved to form a nano-scale microporous structure, which improves the hydrophilic, moisture-absorbing and rapid drying properties of the fibers and deodorizing and antibacterial properties.
The hydrophilicity, moisture absorption and quick drying properties, deodorization and antibacterial properties of the fiber are significantly improved, and the method is environmentally friendly and convenient, and is suitable for large-scale production.
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Abstract
Description
Technical Field
[0001] The invention relates to the field of chemical fibers, and in particular to a preparation method and application of a deodorizing, antibacterial, moisture-absorbing and perspiration-releasing porous polyester fiber. Background Art
[0002] Polyester fiber has excellent physical, chemical and mechanical properties. Since industrialization, polyester fiber textiles have been deeply loved by consumers. With the development of modern science and technology, people are increasingly pursuing a comfortable and safe living environment. Polyethylene terephthalate (PET), which is currently the most widely used textile fiber, has the characteristics of high melting point, high strength, high hardness, excellent electrical properties, good chemical stability and transparency. The clothes made of its fiber are straight and wrinkle-free, and have good heat resistance and dimensional stability. Therefore, it has been widely used in fiber production. However, conventional polyester fiber is a hydrophobic fiber with a standard moisture regain of only 0.4%. It has poor hygroscopicity, which leads to easy static electricity, poor stain removal and poor wicking in daily wear, and can no longer meet people's increasing multifunctional demand for clothing. At the same time, with the development of the concept of green health, consumers have transformed from the initial pursuit of the practicality of textiles to the consumption concept of function, health and safety. Therefore, the development of antibacterial fibers and textiles has become a control measure to inhibit the growth and reproduction of harmful organisms such as bacteria or viruses, which can effectively reduce the invasion of human bodies by foreign pathogens. In addition to antibacterial properties, the odor produced by bacteria needs to be adsorbed, which requires the fiber to have good high adsorption. Currently, researchers mostly directly introduce nano-functional materials with porous structures, such as carbon materials, into polymer matrices to prepare modified fibers. However, the porous structure of the carbon material in the fiber is difficult to preserve. This is because during the fiber preparation process, the polyester melt will flow into the porous structure of the carbon material, making it unable to exert the adsorption function of the micropores.
[0003] A Chinese patent with application number CN202211001260.1 discloses a new type of modified hydrophilic polyester yarn fabric. A shaped polyester yarn is obtained by a shaped cross-section spinning method, and then a polyester polyether type hydrophilic finishing agent is added to the shaped polyester yarn for finishing to obtain a hydrophilic polyester yarn. The obtained fiber modulus is lower than that of conventional polyester, so that the fabric processed with it has good hygroscopicity, quick-drying properties, and skin affinity. It is suitable for processing various high-end moisture wicking fabrics. However, due to the use of a surface finishing modification method, the hydrophilic finishing agent on the surface of the fiber yarn is easily lost during the washing process, and there is a problem of short-lasting moisture absorption and quick-drying performance.
[0004] The Chinese patent application number CN201510164092.1 discloses a method for preparing hemp charcoal polyester fiber with high adsorption and hygroscopic properties, wherein nano-hemp charcoal and nano-silicon dioxide are added to polyester slices, and polyester fibers containing composite powders are prepared by melt spinning, and then the nano-silicon dioxide is removed by alkali treatment to obtain hemp charcoal / polyester fibers with a porous structure, achieving high adsorption and high hygroscopicity. However, this method uses alkali treatment to remove silicon dioxide to obtain fiber pores, which takes a long time to process and has environmental problems, making it difficult to implement in industrial production.
[0005] The Chinese patent application number CN202011247036.1 discloses a method for preparing an environmentally friendly high-adsorption fine-denier polyester filament, in which cellulose grafted and coated hollow microspheres are prepared by reacting oleic acid-coated nano bamboo charcoal powder with cellulose, and then the cellulose hollow microspheres are added to the polyester powder, mixed evenly, and then subjected to twin-screw extrusion granulation to obtain modified polyester masterbatch, which is then melt-spun to prepare polyester fibers, which have the ability to absorb odors. In order to retain the microporous structure of nano bamboo charcoal powder, this technology uses cellulose to chemically graft its oleic acid-coated surface, but the melt spinning temperature introduced into polyester is relatively high, which can easily cause thermal degradation of cellulose, etc., so that the polyester melt enters the micropores for filling and causes density, and the adsorption of the micropores cannot be exerted. Summary of the invention
[0006] In order to solve the technical problems mentioned in the above background technology that polyester fibers have poor hydrophilicity, moisture absorption and quick-drying properties, and poor antibacterial and deodorizing properties, the present invention provides a method for preparing and applying deodorizing, antibacterial, moisture absorption and perspiration porous polyester fibers, wherein modified deodorizing and antibacterial functional polyester and modified water-soluble polyester are mixed in a certain proportion and prepared through melt spinning to obtain blended fibers, wherein the water-soluble polyester component dissolves in water to form a microporous structure, which is environmentally friendly, convenient and meets the conditions for large-scale production.
[0007] The specific technical scheme of the present invention is: a method for preparing a deodorizing, antibacterial, moisture-absorbing and perspiration-releasing porous polyester fiber, comprising the following steps: 1) mixing terephthalic acid, isophthalic acid, sodium 5-sulfonate of isophthalic acid ester, antimony glycol, ethylene glycol and modified glycol, beating, raising the temperature, carrying out esterification reaction, and continuing to raise the temperature to cause polycondensation reaction to obtain modified water-soluble polyester; 2) mixing the deodorant and antibacterial agent with ethylene glycol in a mass ratio of (1.0-1.1):(0.9-1.0), adding terephthalic acid and hexylene glycol, and then beating the mixture and sequentially performing esterification reaction and polycondensation reaction to obtain a deodorant and antibacterial polyester; 3) The modified water-soluble polyester and the deodorizing antibacterial polyester are mixed in a mass ratio of (10-40): (60-90), and melt-spinned after crystallization and drying to obtain polyester fibers.
[0008] The present invention mixes modified deodorizing and antibacterial functional polyester and modified water-soluble polyester in a certain proportion and prepares blended fibers through melt spinning. After the blended fibers are dyed at high temperature and high pressure, the modified water-soluble polyester component in the fibers dissolves out in water, and nano-scale micropores are formed on the surface and inside, the specific surface area is increased, and the hydrophilic moisture absorption and quick-drying properties as well as the deodorizing and antibacterial properties are improved. Compared with traditional acid-dissolving, alkali-dissolving and other treatment methods, the method is more environmentally friendly and convenient, and is suitable for industrial large-scale production. The prepared modified water-soluble polyester and deodorizing and antibacterial polyester have both blending spinnability and functionality.
[0009] Furthermore, in step 1), the molar ratio of terephthalic acid, isophthalic acid, sodium 5-sulfonate of isophthalic acid ester, ethylene glycol and modified glycol is (0.84:~1.05):(0.18~0.23):(0.15~0.23):(0.80~0.95):(0.05~0.20).
[0010] Preferably, the intrinsic viscosity of the modified water-soluble polyester is 0.4 to 0.5 dl / g.
[0011] Furthermore, the modified diol is one or more of diethylene glycol, isosorbide and pentaerythritol.
[0012] Furthermore, the addition amount of antimony glycolate is 0.02-0.03% of the mass of terephthalic acid.
[0013] Furthermore, the preparation method of the deodorant and antibacterial agent is to add nano bamboo charcoal powder and nano zinc oxide in a mass ratio of (1 to 2:1) into ethylene glycol, add a dispersant, grind and disperse to obtain the deodorant and antibacterial agent.
[0014] Furthermore, the dispersant is one or more of PEG-2000, polyethylene wax, and ethylene methyl acrylate copolymer.
[0015] Preferably, the dispersant is ethylene methyl acrylate copolymer.
[0016] Furthermore, the added amount of the dispersant is 3-5% of the total mass of the nano zinc oxide and the nano bamboo charcoal powder.
[0017] Preferably, the particle size of nano zinc oxide is 100-200 nm.
[0018] Preferably, the particle size of the nano bamboo charcoal powder is 100-200 nm.
[0019] Preferably, the intrinsic viscosity of the deodorizing and antibacterial polyester is 0.55 to 0.65 dl / g.
[0020] Furthermore, in step 1) and step 2), the temperature of the esterification reaction is 230-250° C., and the time of the esterification reaction is 1-2 h.
[0021] Furthermore, in step 1) and step 2), the temperature of the polycondensation reaction is 270-275° C., the vacuum degree is greater than 1000 Pa, and the reaction time is 2-2.5 h.
[0022] Preferably, the drying and crystallization conditions in step 3) are: pre-crystallization at 70-90° C. for 1-3 h, and drying at 110-130° C. for 15-20 h, so that the moisture content of the slices is less than 0.008%.
[0023] Furthermore, an application of a deodorizing, antibacterial, moisture-absorbing and perspiration-releasing porous polyester fiber.
[0024] Preferably, a deodorizing, antibacterial, moisture-absorbing and perspiration-releasing porous polyester fiber fabric is prepared by weaving the polyester fibers obtained in the above steps, and obtaining the deodorizing, antibacterial, moisture-absorbing and perspiration-releasing porous polyester fiber fabric after high-temperature and high-pressure dyeing, reduction cleaning and heat setting. After the mixed fibers are dyed at high temperature and high pressure, the modified water-soluble components in the fibers are dissolved, and nano-scale micropores are formed on the surface and inside, thereby increasing the specific surface area, eliminating the internal stress, and improving the moisture absorption and quick-drying performance and the deodorizing and antibacterial performance.
[0025] Preferably, the high temperature and high pressure dyeing conditions are: starting dyeing at 20-30°C, heating to 85-95°C at a rate of 1.5-2.5°C / min, then heating to 100-150°C at a rate of 0.5-1.5°C / min, and dyeing at this temperature for 30-120 minutes; the dyeing pressure is 0.3-0.4MPa.
[0026] Preferably, the reduction cleaning step is as follows: the treatment temperature is 75-85°C, 1.5-2.5 g / L of NaOH and 1.5-2.5 g / L of hydrosulfur powder are added, and the time is 30-40 minutes.
[0027] Compared with the prior art, the beneficial effects of the present invention are: 1) Modified water-soluble polyester is used as a pore-forming agent, which can be dissolved in water to form a microporous structure. Compared with alkali dissolution, acid dissolution and other treatment methods, it is more environmentally friendly, more convenient and meets the conditions of large-scale production.
[0028] 2) Through monomer modification and process regulation, the prepared modified water-soluble polyester and modified deodorizing and antibacterial functional polyester have good blending spinnability and functionality.
[0029] 3) After the modified water-soluble polyester is dissolved, a porous honeycomb structure can be formed in the polyester fiber, and the specific surface area of the fiber is greatly improved. More antibacterial agents and deodorants can be exposed on the fiber surface to play a role, and the antibacterial and deodorizing effects are greatly improved. At the same time, the presence of a large number of micropores on the fiber surface and inside makes the fiber fabric have excellent moisture absorption and quick-drying properties. DETAILED DESCRIPTION
[0030] The present invention will be further described below in conjunction with the embodiments.
[0031] Example 1 1) Preparation of modified water-soluble polyester 290g of ethylene glycol and 76g of isosorbide were added to the reaction container, and then 0.35g of antimony ethylene glycol, 465g of terephthalic acid, 100g of isophthalic acid and 234g of sodium dimethyl 5-sulfonate were added. After pulping, the reactor was heated to 240°C for esterification reaction and kept warm for 2h. The reactor was further heated to 275°C and evacuated to a vacuum degree of 95Pa. The reaction was carried out for 2h to obtain a modified water-soluble polyester having a melt characteristic viscosity of 0.45dl / g.
[0032] 2) Preparation of deodorant and antibacterial functional polyester Nano bamboo charcoal powder and nano zinc oxide in a mass ratio of 2:1 are dispersed in ethylene glycol which is 5 times the total mass of the nano bamboo charcoal powder and nano zinc oxide, 4% of the total solid mass of PEG-2000 is added, and the mixture is ground and dispersed until the particle size of the nano bamboo charcoal powder and nano zinc oxide in the dispersion is 150 nm, thereby obtaining a deodorizing and antibacterial dispersion.
[0033] 172g of ethylene glycol, 172.8g of deodorizing and antibacterial dispersion, 0.35g of ethylene glycol antimony and 664g of terephthalic acid were added to the reactor. After pulping, the reactor was heated to 240°C and kept warm for 1.5h. The reactor was further heated to 275°C and evacuated to a vacuum degree of 1000Pa. The reactor was kept warm for 2h. The reactor was further heated to 278°C and evacuated to a vacuum degree of 95Pa to obtain a deodorizing and antibacterial polyester melt of 0.65dl / g.
[0034] 3) Preparation of polyester fiber The modified water-soluble polyester and the deodorant and antibacterial polyester were mixed in a mass ratio of 1:3, pre-crystallized at 80°C for 2h, dried at 120°C for 18h, melt-spun after passing through a 200-mesh filter and 40-mesh metal sand, and obtained pre-oriented yarns through a spinneret. After the precursor and elastic post-treatment, the polyester fiber that can be manufactured was obtained. The specific parameters of the spinning process are as follows: screw extruder process parameters: screw zone 1 temperature 280°C, zone 2 temperature 295°C, zone 3 temperature 290°C, zone 4 temperature 290°C, zone 5 temperature 290°C; filter screen size 300 mesh; spinning box temperature 285°C. Side blowing speed 0.4m / s; pre-network pressure 0.08MPa; first godet spinning speed 2793m / min; second godet spinning speed 2803m / min; main network pressure 0.3Mpa; winding speed 2800m / min.
[0035] 4) Preparation of knitted fabric After weaving the polyester fiber obtained in step 3), the initial dyeing temperature is 25° C., the temperature is increased to 90° C. at 2° C. / min, and then the temperature is increased to 130° C. at a heating rate of 1.5° C. / min, and the dyeing treatment is carried out at this temperature for 60 minutes; the dyeing pressure is 0.4 MPa, 1 g / L of degreasing agent is added, the amount of dye disperse black ECC is 5% owf, the bath ratio is 1:50, the pH value of the dye solution is 4, and then, at 80° C., 2 g / L of NaOH and 2 g / L of hydrosulfite are added, the holding time is 30 minutes, and then heat-setting is carried out at 175° C. for 1 minute to obtain a deodorizing, antibacterial, moisture-absorbing and sweat-releasing porous polyester fiber fabric.
[0036] 5) Performance testing The deodorizing, antibacterial, moisture wicking and perspiration-releasing functional polyester fiber fabric prepared in step 4) was tested for mechanical properties, specific surface area, moisture absorbing and quick-drying properties, antibacterial properties and deodorizing properties. Among them, the test method for fiber breaking strength refers to GB / T14344 "Standard Test Method for Tensile Properties of Chemical Fiber Filaments", the test steps for moisture absorption and quick-drying performance of cloth samples refer to GB / T21655.1-2023 "Evaluation of Moisture Absorption and Quick-drying of Textiles Part 1: Single Item Combination Test Method", the test method for moisture regain of cloth samples refers to GB / T6503-2017 "Test Method for Moisture Regain of Chemical Fibers", the test method for fiber specific surface area refers to GB / T19587-2017 "Determination of Specific Surface Area of Solid Substances by Gas Adsorption BET Method", the test method for antibacterial performance of cloth samples refers to GB / T20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Oscillation Method", and the deodorization test method of cloth samples refers to GB / T33610.2-2017 "Determination of Deodorization Performance of Textiles Part 2: Inspection Tube Method".
[0037] Comparative Example 1 The difference between this comparative example and Example 1 is that the modified water-soluble polyester is not added in this comparative example, and the rest of the process is the same as that of Example 1, and the specific steps are as follows: 1) Preparation of deodorant and antibacterial functional polyester Nano bamboo charcoal powder and nano zinc oxide in a mass ratio of 2:1 are dispersed in ethylene glycol which is 5 times the total mass of the nano bamboo charcoal powder and nano zinc oxide, 4% of the total solid mass of PEG-2000 is added, and the mixture is ground and dispersed until the particle size of the nano bamboo charcoal powder and nano zinc oxide in the dispersion is 150 nm, thereby obtaining a deodorizing and antibacterial dispersion.
[0038] 172g of ethylene glycol, 172.8g of deodorizing and antibacterial dispersion, 0.35g of ethylene glycol antimony and 664g of terephthalic acid were added to the reactor. After pulping, the reactor was heated to 240°C and kept warm for 1.5h. The reactor was further heated to 275°C and evacuated to a vacuum degree of 1000Pa. The reactor was kept warm for 2h. The reactor was further heated to 278°C and evacuated to a vacuum degree of 95Pa to obtain a deodorizing and antibacterial polyester melt of 0.65dl / g.
[0039] 2) Preparation of polyester fiber The deodorant and antibacterial polyester was pre-crystallized at 80°C for 2h, dried at 120°C for 18h, passed through a 200-mesh filter and 40-mesh metal sand for melt spinning, and passed through a spinneret to obtain pre-oriented yarns. After the precursor and elastic post-treatment, the polyester fiber that can be manufactured was obtained. The specific parameters of the spinning process are as follows: screw extruder process parameters: screw zone 1 temperature 280°C, zone 2 temperature 295°C, zone 3 temperature 290°C, zone 4 temperature 290°C, zone 5 temperature 290°C; filter screen size 300 mesh; spinning box temperature 285°C. Side blowing speed 0.4m / s; pre-netting device pressure 0.08MPa; first godet spinning speed 2793m / min; second godet spinning speed 2803m / min; main netting device pressure 0.3Mpa; winding speed 2800m / min.
[0040] 3) Preparation of knitted fabric After weaving the polyester fiber obtained in step 2), the temperature is raised to 90° C. at 2° C. / min at an initial dyeing temperature of 25° C., and then raised to 130° C. at a heating rate of 1.5° C. / min, and dyeing is performed at this temperature for 60 minutes; the dyeing pressure is 0.4 MPa, 1 g / L of degreasing agent is added, the amount of dye disperse black ECC is 5% owf, the bath ratio is 1:50, the pH value of the dye solution is 4, and then, at 80° C., 2 g / L of NaOH and 2 g / L of hydrosulfite are added, the holding time is 30 minutes, and then heat-setting is performed at 175° C. for 1 minute to obtain a polyester fiber fabric.
[0041] 4) Performance testing The deodorizing, antibacterial, moisture wicking and perspiration-releasing functional polyester fiber fabric prepared in step 3) was tested for mechanical properties, specific surface area, moisture absorbing and quick-drying properties, antibacterial properties and deodorizing properties.
[0042] Comparative Example 2 The difference between this comparative example and Example 1 is that in this comparative example, in step 3), the modified water-soluble polyester and the deodorizing antibacterial polyester are mixed in a mass ratio of 2:3, and the rest of the process is the same as that in Example 1, and the specific steps are as follows: 1) Preparation of modified water-soluble polyester 290g of ethylene glycol and 76g of isosorbide were added to the reaction container, and then 0.35g of antimony ethylene glycol, 465g of terephthalic acid, 100g of isophthalic acid and 234g of sodium dimethyl 5-sulfonate were added. After pulping, the reactor was heated to 240°C for esterification reaction and kept warm for 2h. The reactor was further heated to 275°C and evacuated to a vacuum degree of 95Pa. The reaction was carried out for 2h to obtain a modified water-soluble polyester having a melt characteristic viscosity of 0.45dl / g.
[0043] 2) Preparation of deodorant and antibacterial functional polyester Nano bamboo charcoal powder and nano zinc oxide in a mass ratio of 2:1 are dispersed in ethylene glycol which is 5 times the total mass of the nano bamboo charcoal powder and nano zinc oxide, 4% of the total solid mass of PEG-2000 is added, and the mixture is ground and dispersed until the particle size of the nano bamboo charcoal powder and nano zinc oxide in the dispersion is 150 nm, thereby obtaining a deodorizing and antibacterial dispersion.
[0044] 172g of ethylene glycol, 172.8g of deodorizing and antibacterial dispersion, 0.35g of ethylene glycol antimony and 664g of terephthalic acid were added to the reactor. After pulping, the reactor was heated to 240°C and kept warm for 1.5h. The reactor was further heated to 275°C and evacuated to a vacuum degree of 1000Pa. The reactor was kept warm for 2h. The reactor was further heated to 278°C and evacuated to a vacuum degree of 95Pa to obtain a deodorizing and antibacterial polyester melt of 0.65dl / g.
[0045] 3) Preparation of polyester fiber The modified water-soluble polyester and the deodorant antibacterial polyester are mixed in a mass ratio of 2:3, pre-crystallized at 80°C for 2h, dried at 120°C for 18h, melt-spun after passing through a 200-mesh filter and 40-mesh metal sand, and obtained through a spinneret to obtain pre-oriented yarns. After the precursor and elastic post-treatment, the polyester fiber that can be manufactured is obtained. The specific parameters of the spinning process are as follows: screw extruder process parameters: screw zone 1 temperature 280°C, zone 2 temperature 295°C, zone 3 temperature 290°C, zone 4 temperature 290°C, zone 5 temperature 290°C; filter screen size 300 mesh; spinning box temperature 285°C. Side blowing speed 0.4m / s; pre-netting device pressure 0.08MPa; first godet spinning speed 2793m / min; second godet spinning speed 2803m / min; main netting device pressure 0.3Mpa; winding speed 2800m / min.
[0046] 4) Preparation of knitted fabric After weaving the polyester fiber obtained in step 3), the initial dyeing temperature is 25° C., the temperature is increased to 90° C. at 2° C. / min, and then the temperature is increased to 130° C. at a heating rate of 1.5° C. / min, and the dyeing treatment is carried out at this temperature for 60 minutes; the dyeing pressure is 0.4 MPa, 1 g / L of degreasing agent is added, the amount of dye disperse black ECC is 5% owf, the bath ratio is 1:50, the pH value of the dye solution is 4, and then, at 80° C., 2 g / L of NaOH and 2 g / L of hydrosulfite are added, the holding time is 30 minutes, and then heat-setting is carried out at 175° C. for 1 minute to obtain a deodorizing, antibacterial, moisture-absorbing and sweat-releasing porous polyester fiber fabric.
[0047] 5) Performance testing The deodorizing, antibacterial, moisture absorption and perspiration wicking functional polyester fiber fabric prepared in step 4) was tested for mechanical properties, specific surface area, moisture absorption and quick-drying properties, antibacterial properties, and deodorizing properties. Table 1 Effect of the mixing ratio of modified water-soluble polyester and deodorizing antibacterial polyester on the properties of modified fibers (1) Table 2 Effect of the mixing ratio of modified water-soluble polyester and deodorizing antibacterial polyester on the properties of modified fibers (2) According to the data in Table 1 and Table 2, compared with Comparative Example 1, the hydrophilicity, moisture absorption and quick-drying performance, antibacterial performance and deodorization performance of the porous polyester fiber fabric prepared by adding water-soluble polyester for blending spinning dissolution and pore making are significantly improved. The addition of modified water-soluble polyester can improve the hydrophilicity of polyester fiber. After dyeing treatment, part of the modified water-soluble polyester is dissolved under hot water conditions, and micropores are formed on the surface and inside of the fiber. The formation of micropores increases the specific surface area of the fiber, which is beneficial to the conduction and evaporation of water and improves the moisture absorption and quick-drying performance of polyester fiber. On the other hand, it is beneficial to the naked leakage of deodorant and antibacterial agent, increases the contact probability between deodorant and odor, antibacterial agent and bacteria, and improves the deodorization and antibacterial performance of polyester fiber. In Comparative Example 2, too much modified water-soluble polyester is added, and the number of micropores formed in the fiber after water-soluble pore making is too large, distributed on the surface and inside of the fiber, resulting in a serious decrease in the mechanical properties of the fiber.
[0048] Comparative Example 3 The difference between this comparative example and Example 1 is that in this comparative example, in step 4), the dyeing time is 120 min, and the rest of the process is the same as that in Example 1, and the specific steps are as follows: 1) Preparation of modified water-soluble polyester 290g of ethylene glycol and 76g of isosorbide were added to the reaction container, and then 0.35g of antimony ethylene glycol, 465g of terephthalic acid, 100g of isophthalic acid and 234g of sodium dimethyl 5-sulfonate were added. After pulping, the reactor was heated to 240°C for esterification reaction and kept warm for 2h. The reactor was further heated to 275°C and evacuated to a vacuum degree of 95Pa. The reaction was carried out for 2h to obtain a modified water-soluble polyester having a melt characteristic viscosity of 0.45dl / g.
[0049] 2) Preparation of deodorant and antibacterial functional polyester Nano bamboo charcoal powder and nano zinc oxide in a mass ratio of 2:1 are dispersed in ethylene glycol which is 5 times the total mass of the nano bamboo charcoal powder and nano zinc oxide, 4% of the total solid mass of PEG-2000 is added, and the mixture is ground and dispersed until the particle size of the nano bamboo charcoal powder and nano zinc oxide in the dispersion is 150 nm, thereby obtaining a deodorizing and antibacterial dispersion.
[0050] 172g of ethylene glycol, 172.8g of deodorizing and antibacterial dispersion, 0.35g of ethylene glycol antimony and 664g of terephthalic acid were added to the reactor. After pulping, the reactor was heated to 240°C and kept warm for 1.5h. The reactor was further heated to 275°C and evacuated to a vacuum degree of 1000Pa. The reactor was kept warm for 2h. The reactor was further heated to 278°C and evacuated to a vacuum degree of 95Pa to obtain a deodorizing and antibacterial polyester melt of 0.65dl / g.
[0051] 3) Preparation of polyester fiber The modified water-soluble polyester and the deodorant and antibacterial polyester were mixed in a mass ratio of 1:3, pre-crystallized at 80°C for 2h, dried at 120°C for 18h, melt-spun after passing through a 200-mesh filter and 40-mesh metal sand, and obtained pre-oriented yarns through a spinneret. After the precursor and elastic post-treatment, the polyester fiber that can be manufactured was obtained. The specific parameters of the spinning process are as follows: screw extruder process parameters: screw zone 1 temperature 280°C, zone 2 temperature 295°C, zone 3 temperature 290°C, zone 4 temperature 290°C, zone 5 temperature 290°C; filter screen size 300 mesh; spinning box temperature 285°C. Side blowing speed 0.4m / s; pre-network pressure 0.08MPa; first godet spinning speed 2793m / min; second godet spinning speed 2803m / min; main network pressure 0.3Mpa; winding speed 2800m / min.
[0052] 4) Preparation of knitted fabric After weaving the polyester fiber obtained in step 3), the initial dyeing temperature is 25° C., the temperature is increased to 90° C. at 2° C. / min, and then the temperature is increased to 130° C. at a heating rate of 1.5° C. / min, and the dyeing treatment is carried out at this temperature for 120 minutes; the dyeing pressure is 0.4 MPa, 1 g / L of degreasing agent is added, the amount of dye disperse black ECC is 5% owf, the bath ratio is 1:50, the pH value of the dye solution is 4, and then, at 80° C., 2 g / L of NaOH and 2 g / L of hydrosulfite are added, the holding time is 30 minutes, and then heat-setting is carried out at 175° C. for 1 minute to obtain a deodorizing, antibacterial, moisture-absorbing and sweat-releasing porous polyester fiber fabric.
[0053] 5) Performance testing The deodorizing, antibacterial, moisture wicking and perspiration-releasing functional polyester fiber fabric prepared in step 4) was tested for mechanical properties, specific surface area, moisture absorbing and quick-drying properties, antibacterial properties and deodorizing properties.
[0054] Comparative Example 4 The difference between this comparative example and Example 1 is that in this comparative example, in step 4), the dyeing time is 30 minutes, and the rest of the process is the same as that in Example 1, and the specific steps are as follows: 1) Preparation of modified water-soluble polyester 290g of ethylene glycol and 76g of isosorbide were added to the reaction container, and then 0.35g of antimony ethylene glycol, 465g of terephthalic acid, 100g of isophthalic acid and 234g of sodium dimethyl 5-sulfonate were added. After pulping, the reactor was heated to 240°C for esterification reaction and kept warm for 2h. The reactor was further heated to 275°C and evacuated to a vacuum degree of 95Pa. The reaction was carried out for 2h to obtain a modified water-soluble polyester having a melt characteristic viscosity of 0.45dl / g.
[0055] 2) Preparation of deodorant and antibacterial functional polyester Nano bamboo charcoal powder and nano zinc oxide in a mass ratio of 2:1 are dispersed in ethylene glycol which is 5 times the total mass of the nano bamboo charcoal powder and nano zinc oxide, 4% of the total solid mass of PEG-2000 is added, and the mixture is ground and dispersed until the particle size of the nano bamboo charcoal powder and nano zinc oxide in the dispersion is 150 nm, thereby obtaining a deodorizing and antibacterial dispersion.
[0056] 172g of ethylene glycol, 172.8g of deodorizing and antibacterial dispersion, 0.35g of ethylene glycol antimony and 664g of terephthalic acid were added to the reactor. After pulping, the reactor was heated to 240°C and kept warm for 1.5h. The reactor was further heated to 275°C and evacuated to a vacuum degree of 1000Pa. The reactor was kept warm for 2h. The reactor was further heated to 278°C and evacuated to a vacuum degree of 95Pa to obtain a deodorizing and antibacterial polyester melt of 0.65dl / g.
[0057] 3) Preparation of polyester fiber The modified water-soluble polyester and the deodorant and antibacterial polyester were mixed in a mass ratio of 1:3, pre-crystallized at 80°C for 2h, dried at 120°C for 18h, melt-spun after passing through a 200-mesh filter and 40-mesh metal sand, and obtained pre-oriented yarns through a spinneret. After the precursor and elastic post-treatment, the polyester fiber that can be manufactured was obtained. The specific parameters of the spinning process are as follows: screw extruder process parameters: screw zone 1 temperature 280°C, zone 2 temperature 295°C, zone 3 temperature 290°C, zone 4 temperature 290°C, zone 5 temperature 290°C; filter screen size 300 mesh; spinning box temperature 285°C. Side blowing speed 0.4m / s; pre-network pressure 0.08MPa; first godet spinning speed 2793m / min; second godet spinning speed 2803m / min; main network pressure 0.3Mpa; winding speed 2800m / min.
[0058] 4) Preparation of knitted fabric After weaving the polyester fiber obtained in step 3), the initial dyeing temperature is 25° C., the temperature is increased to 90° C. at 2° C. / min, and then the temperature is increased to 130° C. at a heating rate of 1.5° C. / min, and the dyeing treatment is carried out at this temperature for 30 minutes; the dyeing pressure is 0.4 MPa, 1 g / L of degreasing agent is added, the amount of dye disperse black ECC is 5% owf, the bath ratio is 1:50, the pH value of the dye solution is 4, and then, at 80° C., 2 g / L of NaOH and 2 g / L of hydrosulfite are added, the holding time is 30 minutes, and then heat-setting is carried out at 175° C. for 1 minute to obtain a deodorizing, antibacterial, moisture-absorbing and sweat-releasing porous polyester fiber fabric.
[0059] 5) Performance testing The deodorizing, antibacterial, moisture wicking and perspiration-releasing functional polyester fiber fabric prepared in step 4) was tested for mechanical properties, specific surface area, moisture absorbing and quick-drying properties, antibacterial properties and deodorizing properties.
[0060] Table 3 Effect of dyeing time on modified fiber properties (1) Table 4 Effect of dyeing time on modified fiber properties (2) From the data in Table 3 and Table 4, in Comparative Example 3, the dyeing time is too long, the water-soluble pore-making conditions are relatively severe, and the number of micropores formed in the fiber is too large and distributed on the fiber surface and inside. Although the antibacterial performance, deodorization performance and moisture absorption and quick-drying performance are good, compared with Example 1, the improvement is limited, and the mechanical properties of the fiber are seriously reduced, which is not conducive to the use of subsequent products; in Comparative Example 4, the dyeing time is short, the water-soluble pore-making conditions are relatively mild, the number of micropores formed in the fiber is limited, the fiber specific surface area is improved, and the fiber moisture absorption and quick-drying performance, deodorization performance and antibacterial performance are limited.
[0061] The raw materials and equipment used in the present invention, unless otherwise specified, are all commonly used raw materials and equipment in the art; the methods used in the present invention, unless otherwise specified, are all conventional methods in the art.
[0062] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent transformation made to the above embodiment based on the technical essence of the present invention still falls within the protection scope of the technical solution of the present invention.
Claims
1. A method for preparing a deodorizing, antibacterial, moisture-absorbing and perspiration-releasing porous polyester fiber, characterized in that: The following steps are involved: 1) terephthalic acid, isophthalic acid, sodium isophthalate-5-sulfonate, ethylene glycol antimony, ethylene glycol and modified glycol are mixed, beaten, the temperature is increased, an esterification reaction is carried out, and the temperature is continued to be increased to cause a polycondensation reaction to obtain a modified water-soluble polyester; 2) Mixing the deodorant and antibacterial agent with ethylene glycol in a mass ratio of (1.0-1.1):(0.9-1.0), adding terephthalic acid and hexylene glycol, and then beating the mixture to sequentially perform esterification reaction and polycondensation reaction to obtain a deodorant and antibacterial polyester; 3) The modified water-soluble polyester and the deodorizing antibacterial polyester are mixed in a mass ratio of (10-40): (60-90), and after crystallization and drying, melt spinning is performed to obtain polyester fibers.
2. The method for preparing a deodorizing, antibacterial, moisture absorbing and perspiration wicking porous polyester fiber according to claim 1, characterized in that: In step 1), the molar ratio of terephthalic acid, isophthalic acid, sodium 5-sulfonate of isophthalic acid ester, ethylene glycol and modified glycol is (0.84:~1.05):(0.18~0.23):(0.15~0.23):(0.80~0.95):(0.05~0.20).
3. The method for preparing a deodorizing, antibacterial, moisture absorbing and perspiration wicking porous polyester fiber according to claim 1 or 2, characterized in that: The modified diol is one or more of diethylene glycol, isosorbide and pentaerythritol.
4. The method for preparing a deodorizing, antibacterial, moisture absorbing and perspiration wicking porous polyester fiber according to claim 1, characterized in that: The amount of antimony glycol added is 0.02~0.03% of the mass of terephthalic acid.
5. The method for preparing a deodorizing, antibacterial, moisture absorbing and perspiration wicking porous polyester fiber according to claim 1, characterized in that: The preparation method of the deodorant and antibacterial agent comprises the following steps: adding nano bamboo charcoal powder and nano zinc oxide in a mass ratio of (1-2:1) into ethylene glycol, adding a dispersant, and grinding and dispersing to obtain the deodorant and antibacterial agent.
6. The method for preparing a deodorizing, antibacterial, moisture-absorbing and perspiration-releasing porous polyester fiber according to claim 5, characterized in that: The dispersant is one or more of PEG-2000, polyethylene wax, and ethylene methyl acrylate copolymer.
7. The method for preparing a deodorizing, antibacterial, moisture absorbing and perspiration wicking porous polyester fiber according to claim 5 or 6, characterized in that: The added amount of the dispersant is 3-5% of the total mass of the nano zinc oxide and nano bamboo charcoal powder.
8. The method for preparing a deodorizing, antibacterial, moisture absorbing and perspiration wicking porous polyester fiber according to claim 1, characterized in that: In step 1) and step 2), the temperature of the esterification reaction is 230-250° C., and the time of the esterification reaction is 1-2 h.
9. The method for preparing a deodorizing, antibacterial, moisture absorbing and perspiration wicking porous polyester fiber according to claim 1, characterized in that: In step 1) and step 2), the temperature of the polycondensation reaction is 270-275° C., the vacuum degree is greater than 1000 Pa, and the reaction time is 2-2.5 h.
10. An application of the preparation method of the deodorizing, antibacterial, moisture absorbing and perspiration wicking porous polyester fiber according to any one of claims 1 to 9.
Citation Information
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