Negative oxygen ion polyester fiber and method for producing the same

Abstract

The application provides a negative oxygen ion polyester fiber and a preparation method thereof. The preparation method of the negative oxygen ion polyester fiber comprises the following steps: S1. Tourmaline powder is soaked in a hydrochloric acid solution, taken out, washed to neutral, dried, and pretreated tourmaline powder is obtained; hydrochloric acid is added to a tetrabutyl titanate ethanol solution, an ethanol-water mixture is added after stirring, and the system is transparent until a treatment solution is obtained; S2. The pretreated tourmaline powder is added to the treatment solution, stirred, ultrasonically treated, filtered, dried, and calcined in a protective gas atmosphere to obtain a composite; S3. The composite is mixed with stearic acid and polyester powder to obtain a mixture, and the mixture is melt blended, extruded, and granulated to obtain a master batch; and S4. The polyester chip and the master batch are mixed and melt spun and stretched to obtain the negative oxygen ion polyester fiber. The application can improve the negative oxygen ion release effect.

Description

Technical Field

[0001] This invention relates to the field of textile technology, and in particular to negative oxygen ion polyester fiber and its preparation method. Background Technology

[0002] Polyester fiber, also known as polyester, is a fiber spun from a fiber-forming polymer whose segments are linked by ester groups in a macromolecular chain. Polyester fiber is one of the most widely used synthetic fibers. It possesses advantages such as high breaking strength and elastic modulus, moderate resilience, excellent heat setting, good heat and light resistance, and resistance to organic solvents, making it widely used in home textiles and other fields.

[0003] As living standards improve, people have higher demands for textiles. For example, they want textiles to have negative ion release effects.

[0004] In related technologies, tourmaline and other negative ion powders are added during the fiber preparation process to impart negative oxygen ion release effects to polyester fibers. However, the negative oxygen ion release effect of polyester fibers needs further improvement. Summary of the Invention

[0005] This invention provides negative oxygen ion polyester fiber and its preparation method to solve the above-mentioned technical problems.

[0006] To achieve the above objectives, the technical solution of the present invention is as follows: This invention provides a method for preparing negative oxygen ion polyester fiber, comprising the following steps: S1. Soak tourmaline powder in hydrochloric acid solution, remove it, wash until neutral, and dry it to obtain pretreated tourmaline powder; Hydrochloric acid was added to an ethanol solution containing tetrabutyl titanate, and after stirring, an ethanol-water mixture was added until the system became transparent, thus obtaining the treatment solution. S2. Add the pretreated tourmaline powder to the treatment solution, stir, sonicate, filter, dry, and calcine under a protective gas atmosphere to obtain the composite. S3. The composite is mixed with stearic acid and polyester powder to obtain a mixture. The mixture is then melt-blended, extruded, and granulated to obtain a masterbatch. S4. The polyester chips and masterbatch are mixed, melt-spun, and stretched to obtain the negative oxygen ion polyester fiber.

[0007] In one embodiment of the present invention, step S1 is performed according to at least one of the following requirements (1)-(8): (1) The particle size of the tourmaline powder is 5nm-20nm, preferably 5-15nm; (2) The mass ratio of tourmaline powder to hydrochloric acid solution is 1:20-30, preferably 1:25-30; (3) The concentration of the hydrochloric acid solution is 0.3 mol / L-0.5 mol / L, preferably 0.4 mol / L-0.5 mol / L; (4) The soaking time is 12h-24h, preferably 18h-24h; (5) The drying temperature is 60℃-70℃, preferably 65℃-70℃; the drying time is 30min-40min, preferably 35min-40min; (6) In the ethanol solution, the concentration of tetrabutyl titanate is 18 g / L-25 g / L, preferably 20 g / L-25 g / L; (7) The mass ratio of hydrochloric acid to tetrabutyl titanate is 0.01-0.02:0.3-0.4, preferably 0.015-0.02:0.3-0.4.

[0008] (8) In the ethanol-water mixture, the volume percentage of ethanol is 10%-30%, preferably 15%-30%.

[0009] In one embodiment of the present invention, step S2 is performed according to at least one of the following requirements (9)-(12): (9) The mass ratio of the pretreated tourmaline powder to tetrabutyl titanate is 1:0.3-0.4, preferably 1:0.35-0.4; (10) During the ultrasonic treatment, the power is 150W-250W, preferably 200W-250W; the ultrasonic treatment time is 45min-60min, preferably 50min-60min; (11) The drying temperature is 90℃-100℃, preferably 95℃-100℃; the drying time is 20min-30min, preferably 25min-30min; (12) The calcination temperature is 500℃-550℃, preferably 520℃-550℃; the calcination time is 2h-3h, preferably 2.5h-3h.

[0010] In one embodiment of the present invention, in step S3, the mass ratio of stearic acid to the complex is 0.2-0.4:4-5, preferably 0.3-0.4:4-5.

[0011] In one embodiment of the present invention, in step S3, the mass ratio of the polyester powder to the composite is 90-95:4-5, preferably 90-95:4.5-5.

[0012] In one embodiment of the present invention, during the melt blending process in step S3, the temperature is 240℃-250℃, preferably 245℃-250℃.

[0013] In another embodiment of the present invention, an epoxy silane coupling agent is also added to the mixture in step S3.

[0014] In one embodiment of the present invention, in step S3, the mass ratio of the epoxy silane coupling agent to the complex is 0.02-0.05:4-5, preferably 0.03-0.05:4-5.

[0015] In one embodiment of the present invention, in step S3, the epoxy silane coupling agent includes 3-glycidoxypropyltrimethoxysilane (i.e., KH560).

[0016] In one embodiment of the present invention, in step S4, the mass ratio of the masterbatch to the polyester chips is 1-5:99-95, preferably 2-5:98-95.

[0017] In one embodiment of the present invention, during the melt spinning process in step S4, the temperature is 260℃-270℃, preferably 265℃-270℃; the speed is 2500m / min-3500m / min, preferably 2800m / min-3500m / min.

[0018] In one embodiment of the present invention, during the stretching process in step S4, the temperature is 105℃-115℃, preferably 105℃-115℃; the stretching ratio is 2-3 times, preferably 2.5-3 times.

[0019] The present invention also provides a negative oxygen ion polyester fiber prepared according to the method described above.

[0020] The beneficial effects of this invention are: In this application, hydrochloric acid solution can remove impurities from the surface of tourmaline and increase the density of surface active sites, resulting in pretreated tourmaline powder. Tetrabutyl titanate hydrolyzes under acidic conditions to generate hydroxylated titanium intermediates. These hydroxylated titanium intermediates polymerize and form a titanium dioxide gel layer on the tourmaline surface. During subsequent drying and calcination, the organic components in the gel layer are gradually removed, transforming into crystalline titanium dioxide, thus obtaining the composite. The composite is then formulated into a masterbatch, which is further processed into polyester fibers. The composite is then incorporated into the polyester fibers, imparting a negative oxygen ion release effect to the fibers.

[0021] Under light, the band structure changes of titanium dioxide cause photogenerated electrons to be tightly adsorbed onto tourmaline, inhibiting the recombination of photogenerated electron-void pairs and generating superoxide radicals and hydroxyl radicals. These radicals can degrade organic pollutants attached to the fabric made of the fiber and volatile organic compounds in the air into water and carbon dioxide. The micro-electric field generated by tourmaline has a polarization effect; under polarization, water ionizes to generate hydrogen ions and hydroxide ions. Hydroxide ions can combine with oxygen in the air to form negative oxygen ions. In short, titanium dioxide enhances the negative oxygen ion release effect of tourmaline, thereby improving the negative oxygen ion release effect of the polyester fibers made from it.

[0022] In this application, epoxy groups are introduced into the composite through an epoxy silane coupling agent. During the melt blending process, the epoxy groups can react with the terminal hydroxyl groups of the polyester, thereby increasing the bonding strength between the composite and the polyester and preventing the poor compatibility between the two from causing the composite to precipitate during processing, thus further improving the negative oxygen ion release effect. Detailed Implementation

[0023] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0024] One embodiment of this application provides a method for preparing negative oxygen ion polyester fiber, which includes the following steps: S1. Soak tourmaline powder in hydrochloric acid solution, remove it, wash until neutral, and dry it to obtain pretreated tourmaline powder; Hydrochloric acid was added to an ethanol solution containing tetrabutyl titanate, and after stirring, an ethanol-water mixture was added until the system became transparent, thus obtaining the treatment solution. S2. Add pretreated tourmaline powder to the treatment solution, stir, sonicate, filter, dry, and calcine under a protective gas atmosphere to obtain the composite. S3. The composite is mixed with stearic acid and polyester powder to obtain a mixture. The mixture is then melt-blended, extruded, and granulated to obtain a masterbatch. S4. Polyester chips and masterbatch are mixed, melt-spun, and stretched to obtain negative oxygen ion polyester fibers.

[0025] In this application, hydrochloric acid solution can remove impurities from the surface of natural tourmaline and increase the density of surface active sites, resulting in pretreated tourmaline powder. Tetrabutyl titanate hydrolyzes under acidic conditions to generate hydroxylated titanium intermediates. These hydroxylated titanium intermediates polymerize and form a titanium dioxide gel layer on the tourmaline surface. During subsequent drying and calcination, the organic components in the gel layer are gradually removed, transforming into crystalline titanium dioxide, thus obtaining the composite. The composite is then made into a masterbatch, which is further processed into polyester fibers. The composite is then incorporated into the polyester fibers, imparting a negative oxygen ion release effect to the fibers.

[0026] In this application, the protective gas may include substances such as nitrogen, argon, and helium.

[0027] The mechanism of this scheme is as follows: Under light, the band structure changes of titanium dioxide cause photogenerated electrons to be tightly adsorbed onto tourmaline, inhibiting the recombination of photogenerated electron-void pairs and generating superoxide radicals and hydroxyl radicals. These radicals can degrade organic pollutants adhering to fabrics made of fibers and volatile organic compounds in the air into water and carbon dioxide. The micro-electric field generated by tourmaline has a polarization effect; under this polarization, water ionizes to generate hydrogen ions and hydroxide ions. Hydroxide ions can combine with oxygen in the air to form negative oxygen ions. In short, titanium dioxide enhances the negative oxygen ion release effect of tourmaline.

[0028] In one embodiment of this application, in step S1, the particle size of the tourmaline powder is 5nm-20nm, preferably 5-15nm. The mass ratio of tourmaline powder to hydrochloric acid solution is 1:20-30, preferably 1:25-30. The concentration of the hydrochloric acid solution is 0.3mol / L-0.5mol / L, preferably 0.4mol / L-0.5mol / L. The soaking time is 12h-24h, preferably 18h-24h. The drying temperature is 60℃-70℃, preferably 65℃-70℃; the drying time is 30min-40min, preferably 35min-40min. In the ethanol solution, the concentration of tetrabutyl titanate is 18g / L-25g / L, preferably 20g / L-25g / L. The mass ratio of hydrochloric acid to tetrabutyl titanate is 0.01-0.02:0.3-0.4, preferably 0.015-0.02:0.3-0.4. In the ethanol-water mixture, the volume percentage of ethanol is 10%-30%, preferably 15%-30%.

[0029] In one embodiment of this application, in step S2, the mass ratio of pretreated tourmaline powder to tetrabutyl titanate is 1:0.3-0.4, preferably 1:0.35-0.4. During ultrasonic treatment, the power is 150W-250W, preferably 200W-250W; the ultrasonic treatment time is 45min-60min, preferably 50min-60min. The drying temperature is 90℃-100℃, preferably 95℃-100℃; the drying time is 20min-30min, preferably 25min-30min. The calcination temperature is 500℃-550℃, preferably 520℃-550℃; the calcination time is 2h-3h, preferably 2.5h-3h.

[0030] In one embodiment of this application, in step S3, the mass ratio of stearic acid to the composite is 0.2-0.4:4-5, preferably 0.3-0.4:4-5. The mass ratio of polyester powder to the composite is 90-95:4-5, preferably 90-95:4.5-5. During the melt blending process, the temperature is 240℃-250℃, preferably 245℃-250℃.

[0031] In one embodiment of this application, in step S4, the mass ratio of masterbatch to polyester chips is 1-5:99-95, preferably 2-5:98-95. During melt spinning, the temperature is 260℃-270℃, preferably 265℃-270℃; the speed is 2500m / min-3500m / min, preferably 2800m / min-3500m / min. During drawing, the temperature is 105℃-115℃, preferably 105℃-115℃; the draw ratio is 2-3 times, preferably 2.5-3 times.

[0032] In another embodiment of this application, in step S3, an epoxy silane coupling agent is further added to the mixture. The mass ratio of the epoxy silane coupling agent to the complex is 0.02-0.05:4-5, preferably 0.03-0.05:4-5. The epoxy silane coupling agent includes 3-glycidoxypropyltrimethoxysilane (i.e., epoxy silane coupling agent KH560).

[0033] In this application, by adding an epoxy silane coupling agent to the mixture, epoxy groups can be introduced into the composite through the epoxy silane coupling agent. During the melt blending process, the epoxy groups can react with the terminal hydroxyl groups of the polyester, thereby improving the bonding strength between the composite and the polyester and avoiding the poor compatibility between the two, which would cause the composite to precipitate during processing, and thus further improving the negative oxygen ion release efficiency.

[0034] Another embodiment of this application also provides a negative oxygen ion polyester fiber prepared according to the method described above.

[0035] Furthermore, the term "and / or" in this application is merely a description of the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, or B existing alone. Additionally, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed by this invention.

[0036] Example 1 S1. Tourmaline powder with a particle size of 5 nm was soaked in a 0.5 mol / L hydrochloric acid solution for 12 h. The mass ratio of tourmaline powder to hydrochloric acid solution was 1:30. The powder was taken out, washed until neutral (i.e., pH 7.0), and dried in an oven at 60 °C for 40 min to obtain pretreated tourmaline powder. Tetrabutyl titanate was added to ethanol and stirred to obtain an ethanol solution with a tetrabutyl titanate concentration of 25 g / L. Hydrochloric acid was added to the ethanol solution, with a mass ratio of hydrochloric acid to tetrabutyl titanate of 0.01:0.4. After stirring, an ethanol-water mixture (in which the volume percentage of ethanol is 30%) was added until the system became transparent, thus obtaining the treatment solution. S2. Add pretreated tourmaline powder to the treatment solution. The mass ratio of pretreated tourmaline powder to tetrabutyl titanate is 1:0.3. Stir, sonicate at 250W for 45 minutes, filter, and dry in an oven at 100℃ for 20 minutes. Next, the compound was calcined at 550°C for 2 hours in a nitrogen atmosphere to obtain the composite. S3. The composite, stearic acid and polyester powder are mixed at a mass ratio of 5:0.4:95 to obtain a mixture. The mixture is then melt-blended, extruded and granulated to obtain a masterbatch. The temperature during the melt-blending process is 250℃. S4. The polyester chips and masterbatch are mixed at a mass ratio of 99:1, and then melt-spun at a temperature of 270°C and a speed of 2500 m / min. Then, the fibers were stretched three times at 115°C to obtain negative oxygen ion polyester fibers.

[0037] Example 2 S1. Tourmaline powder with a particle size of 20 nm was soaked in a 0.3 mol / L hydrochloric acid solution for 24 h. The mass ratio of tourmaline powder to hydrochloric acid solution was 1:20. The powder was taken out, washed until neutral (i.e., pH 7.0), and dried in an oven at 70 °C for 30 min to obtain pretreated tourmaline powder. Tetrabutyl titanate was added to ethanol and stirred to obtain an ethanol solution with a tetrabutyl titanate concentration of 18 g / L. Hydrochloric acid was added to the ethanol solution, with a mass ratio of hydrochloric acid to tetrabutyl titanate of 0.02:0.3. After stirring, an ethanol-water mixture (in which the volume percentage of ethanol is 10%) was added until the system became transparent, thus obtaining the treatment solution. S2. Add pretreated tourmaline powder to the treatment solution. The mass ratio of pretreated tourmaline powder to tetrabutyl titanate is 1:0.4. Stir, sonicate at 150W for 60 minutes, filter, and dry in an oven at 90℃ for 30 minutes. Next, the compound was calcined at 500°C for 3 hours in a nitrogen atmosphere to obtain the composite. S3. The composite, stearic acid and polyester powder are mixed at a mass ratio of 4:0.2:90 to obtain a mixture. The mixture is then melt-blended, extruded and granulated to obtain a masterbatch. The temperature during the melt-blending process is 240℃. S4. The polyester chips and masterbatch are mixed at a mass ratio of 95:5, and then melt-spun at a temperature of 260℃ and a speed of 3500m / min. Then, the fibers were stretched twice at 105°C to obtain negative oxygen ion polyester fibers.

[0038] Example 3 S1. Tourmaline powder with a particle size of 10 nm was soaked in a 0.4 mol / L hydrochloric acid solution for 18 h. The mass ratio of tourmaline powder to hydrochloric acid solution was 1:25. The powder was taken out, washed until neutral (i.e., pH 7.0), and dried in an oven at 65 °C for 35 min to obtain pretreated tourmaline powder. Tetrabutyl titanate was added to ethanol and stirred to obtain an ethanol solution with a tetrabutyl titanate concentration of 20 g / L. Hydrochloric acid was added to the ethanol solution, with a mass ratio of hydrochloric acid to tetrabutyl titanate of 0.015:0.35. After stirring, an ethanol-water mixture (in which the volume percentage of ethanol is 20%) was added until the system became transparent, thus obtaining the treatment solution. S2. Add pretreated tourmaline powder to the treatment solution. The mass ratio of pretreated tourmaline powder to tetrabutyl titanate is 1:0.35. Stir, sonicate at 200W for 50 minutes, filter, and dry in an oven at 95℃ for 25 minutes; Next, the compound was calcined at 520°C for 2.5 h in a nitrogen atmosphere to obtain the composite. S3. The composite, stearic acid and polyester powder are mixed in a mass ratio of 4.5:0.3:96 to obtain a mixture. The mixture is then melt-blended, extruded and granulated to obtain a masterbatch. The temperature during the melt-blending process is 245℃. S4. The polyester chips and masterbatch are mixed at a mass ratio of 98:2, and then melt-spun at a temperature of 265°C and a speed of 3000 m / min. Then, the fibers were stretched 2.5 times at 110°C to obtain negative oxygen ion polyester fibers.

[0039] Example 4 Except for the following conditions, negative oxygen ion polyester fibers were prepared in the same manner as in Example 3: S3. The complex, stearic acid, polyester powder and 3-glycidyl etheroxypropyltrimethoxysilane (i.e. epoxy silane coupling agent KH560) are mixed in a mass ratio of 4.5:0.3:96:0.02 to obtain a mixture. The mixture is then melt-blended, extruded and granulated to obtain a masterbatch. The temperature during the melt-blending process is 245℃.

[0040] The difference between this embodiment and Example 3 is that in step S3, 3-glycidoxypropyltrimethoxysilane (i.e., epoxy silane coupling agent KH560) is also added to the mixture, and the mass ratio of 3-glycidoxypropyltrimethoxysilane (i.e., epoxy silane coupling agent KH560) to the complex is 0.02:4.5.

[0041] Example 5 Except for the following conditions, negative oxygen ion polyester fibers were prepared in the same manner as in Example 3: S3. The complex, stearic acid, polyester powder and 3-glycidyl etheroxypropyltrimethoxysilane (i.e. epoxy silane coupling agent KH560) are mixed in a mass ratio of 4.5:0.3:96:0.05 to obtain a mixture. The mixture is then melt-blended, extruded and granulated to obtain a masterbatch. The temperature during the melt-blending process is 245℃.

[0042] The difference between this embodiment and Example 3 is that in step S3, 3-glycidoxypropyltrimethoxysilane (i.e., epoxy silane coupling agent KH560) is also added to the mixture, and the mass ratio of 3-glycidoxypropyltrimethoxysilane (i.e., epoxy silane coupling agent KH560) to the complex is 0.05:4.5.

[0043] Comparative Example 1 Except for the following conditions, negative oxygen ion polyester fibers were prepared in the same manner as in Example 3: S2. Add tourmaline powder with a particle size of 10 nm to the treatment solution. The mass ratio of tourmaline powder to tetrabutyl titanate is 1:0.35. Stir, sonicate at 200W for 50 minutes, filter, and dry in an oven at 95℃ for 25 minutes; Next, the composite was calcined at 520°C for 2.5 h in a nitrogen atmosphere to obtain the composite.

[0044] The difference between this comparative example and Example 3 is that the tourmaline powder was not pretreated.

[0045] Comparative Example 2 Except for the following conditions, negative oxygen ion polyester fibers were prepared in the same manner as in Example 3: S1. Tourmaline powder with a particle size of 10 nm was soaked in a 0.4 mol / L hydrochloric acid solution for 18 h. The mass ratio of tourmaline powder to hydrochloric acid solution was 1:25. The powder was taken out, washed until neutral (i.e., pH 7.0), and dried in an oven at 65 °C for 35 min to obtain pretreated tourmaline powder. S3. The pretreated tourmaline powder, stearic acid and polyester powder are mixed in a mass ratio of 4.5:0.3:96 to obtain a mixture. The mixture is then melt-blended, extruded and granulated to obtain a masterbatch. The temperature during the melt-blending process is 245℃.

[0046] The difference between this comparative example and Example 3 is that the pretreated tourmaline powder was not made into a composite.

[0047] test The negative oxygen ion polyester fibers obtained in Examples 1-5 and Comparative Examples 1-2 were made into fabrics of the same specifications. Under visible light irradiation (λ > 450 nm), the negative ion generation (i.e. negative oxygen ion generation) of each fabric was tested according to GB / T 30128-2013 "Detection and Evaluation of Negative Ion Generation in Textiles". The measurement time was 3 min, and the results are shown in Table 1.

[0048] Table 1 Test Results

[0049] As shown in Table 1, the amount of negative ions generated in Example 3 was significantly increased compared to Comparative Example 1. This result indicates that, in this application, pretreatment of tourmaline can enhance the negative oxygen ion release effect of the manufactured polyester fibers.

[0050] As shown in Table 1, the amount of negative ions generated in Examples 4 and 5 is significantly higher than that in Example 3. This result indicates that, in this application, by adding an epoxy silane coupling agent to the mixture, the negative oxygen ion release effect of the prepared polyester fiber can be improved.

[0051] The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in the present invention should still be covered by the claims of the present invention.

Claims

1. A method for preparing negative oxygen ion polyester fiber, characterized in that, The preparation method includes the following steps: S1. Soak tourmaline powder in hydrochloric acid solution, remove it, wash until neutral, and dry it to obtain pretreated tourmaline powder; Hydrochloric acid was added to an ethanol solution containing tetrabutyl titanate, and after stirring, an ethanol-water mixture was added until the system became transparent, thus obtaining the treatment solution. S2. Add the pretreated tourmaline powder to the treatment solution, stir, sonicate, filter, dry, and calcine under a protective gas atmosphere to obtain the composite. S3. The composite is mixed with stearic acid and polyester powder to obtain a mixture. The mixture is then melt-blended, extruded, and granulated to obtain a masterbatch. S4. The polyester chips and masterbatch are mixed, melt-spun, and stretched to obtain the negative oxygen ion polyester fiber.

2. The method for preparing negative oxygen ion polyester fiber as described in claim 1, characterized in that, Step S1 shall be performed in accordance with at least one of the following requirements (1)-(8): (1) The particle size of the tourmaline powder is 5nm-20nm; (2) The mass ratio of the tourmaline powder to the hydrochloric acid solution is 1:20-30; (3) The concentration of the hydrochloric acid solution is 0.3 mol / L-0.5 mol / L; (4) The soaking time is 12h-24h; (5) The drying temperature is 60℃-70℃, and the drying time is 30min-40min; (6) The concentration of tetrabutyl titanate in the ethanol solution is 18 g / L-25 g / L; (7) The mass ratio of hydrochloric acid to tetrabutyl titanate is 0.01-0.02:0.3-0.4; (8) The volume percentage of ethanol in the ethanol-water mixture is 10%-30%.

3. The method for preparing negative oxygen ion polyester fiber as described in claim 1, characterized in that, Step S2 shall be performed in accordance with at least one of the following requirements (9)-(12): (9) The mass ratio of the pretreated tourmaline powder to tetrabutyl titanate is 1:0.3-0.4; (10) During the ultrasonic treatment, the power is 150W-250W and the ultrasonic treatment time is 45min-60min; (11) The drying temperature is 90℃-100℃, and the drying time is 20min-30min; (12) The calcination temperature is 500℃-550℃ and the calcination time is 2h-3h.

4. The method for preparing negative oxygen ion polyester fiber as described in claim 1, characterized in that, In step S3, the mass ratio of stearic acid to the complex is 0.2-0.4:4-5; And / or, in step S3, the mass ratio of the polyester powder to the composite is 90-95:4-5.

5. The method for preparing negative oxygen ion polyester fiber as described in claim 1, characterized in that, During the melt blending process described in step S3, the temperature is 240℃-250℃.

6. The method for preparing negative oxygen ion polyester fiber as described in claim 1, characterized in that, The mixture described in step S3 also contains an epoxy silane coupling agent.

7. The method for preparing negative oxygen ion polyester fiber as described in claim 6, characterized in that, In step S3, the mass ratio of the epoxy silane coupling agent to the complex is 0.02-0.05:4-5; And / or, in step S3, the epoxy silane coupling agent includes 3-glycidoxypropyltrimethoxysilane.

8. The method for preparing negative oxygen ion polyester fiber as described in claim 1, characterized in that, In step S4, the mass ratio of the masterbatch to the polyester chips is 1-5:99-95; And / or, in the melt spinning process described in step S4, the temperature is 260℃-270℃ and the speed is 2500m / min-3500m / min.

9. The method for preparing negative oxygen ion polyester fiber as described in claim 1, characterized in that, During the stretching process described in step S4, the temperature is 105℃-115℃, and the stretching ratio is 2-3 times.

10. A negative oxygen ion polyester fiber prepared according to any one of claims 1-9.

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