Production method of full-dull flat polyester POY (Polyester Pre-Oriented Yarn) fiber

Abstract

The invention relates to the technical field of spinning, and particularly discloses a production method of full-dull flat polyester POY fibers. A production method of full-dull flat polyester POY (polyester pre-oriented yarn) fibers comprises the following specific steps: mixing terephthalic acid, ethylene glycol, modified titanium dioxide powder, ethylene glycol antimony, trimethyl phosphate and a catalyst, and sequentially performing esterification reaction, pre-polycondensation reaction and final polycondensation reaction to generate polyethylene terephthalate, so as to obtain polyester semi-dull melt; melting the full-dull master batch, then mixing the full-dull master batch with a polyester semi-dull solution for spinning, extruding from a flat spinneret plate to obtain a composite melt trickle, then carrying out circular blowing cooling and curing to form a nascent fiber, and then sequentially carrying out oiling and winding forming to obtain the full-dull flat polyester POY fiber; the surface of the prepared full-dull flat polyester POY fiber has a uniform dull effect, and meanwhile, the fiber system has relatively good dispersity and compatibility, so that the fiber can be promoted to keep relatively good strength.

Description

Technical Field

[0001] The present application relates to the field of spinning technology, and in particular to a method for producing full-dull flat polyester POY fibers. Background Art

[0002] Polyester fiber has excellent mechanical properties and heat resistance, and has a wide range of applications in clothing, home textiles, industrial use and other fields. As a high-end clothing fabric, polyester filaments have excellent light transmittance, so they need to be matted to achieve the effect of shading and luminescence, making the fabric opaque or reducing its light transmittance. Titanium dioxide is a commonly used matting agent for polyester filaments. At present, it is usually copolymerized by adding titanium dioxide as a matting agent in the process of copolymerization and pulping to prepare titanium dioxide products with matting properties.

[0003] In existing production, in order to improve the compatibility of titanium dioxide and polymers, a smaller amount of titanium dioxide is generally used. A smaller amount of titanium dioxide can reduce the gloss of the fiber, but it cannot completely eliminate the gloss and cannot meet the requirements of fully matte fiber. If the amount of titanium dioxide added is increased, although the full matte effect can be achieved, it is difficult to achieve a good dispersion of high-content titanium dioxide in the polyester melt, which increases the spinning pressure, increases the burden on the filter, affects the spinnability of the fiber, and the spinning process and equipment cannot meet the needs of long-term continuous production. Summary of the invention

[0004] In order to improve the full matt effect of polyester POY fiber, the present application provides a method for producing full matt flat polyester POY fiber.

[0005] The present application provides a method for producing a fully matte flat polyester POY fiber, which adopts the following technical solution: A method for producing full-dull flat polyester POY fiber comprises the following specific steps: Terephthalic acid and ethylene glycol, modified titanium dioxide powder, ethylene glycol antimony, trimethyl phosphate and a catalyst are mixed, and esterification reaction, pre-polycondensation reaction and final polycondensation reaction are carried out in sequence to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the fully-dull masterbatch is melted and mixed with the polyester semi-dull melt for spinning, and extruded from a flat spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a fully-dull flat polyester POY fiber.

[0006] By adopting the above technical solution, polyester semi-matt melt is mixed with molten full-matt masterbatch, the amount of titanium dioxide in the polyester semi-matt melt can be reduced by the full-matt masterbatch, and the uniformity of each component of the polyester POY fiber system can be improved. At the same time, full-matt flat polyester POY fiber is produced by melt direct spinning, which is conducive to long-term continuous production. The use of trimethyl phosphate can interact with polyester molecules, stabilize the polyester structure, improve the stability of polyester semi-matt melt in spinning, enhance the strength of polyester fibers, and reduce the phenomenon of polyester fiber breakage during processing and production. Flat polyester filament fibers have a large specific surface area and good adsorption, and have a capillary effect, which improves the moisture absorption and perspiration performance of the fiber.

[0007] Preferably, the polyethylene terephthalate comprises the following raw materials in parts by weight: 70-90 parts of terephthalic acid, 20-30 parts of ethylene glycol, 3-5 parts of modified titanium dioxide, 0.5-1 parts of ethylene glycol antimony, 1-3 parts of trimethyl phosphate, and 0.03-0.05 parts of a catalyst.

[0008] By adopting the above technical scheme, terephthalic acid and ethylene glycol are first subjected to an esterification reaction to generate ethylene terephthalate, and then a polyethylene terephthalate polymer chain is formed through pre-polycondensation and final polycondensation reactions. A small amount of modified titanium dioxide is used to participate in the copolymerization reaction of the polymer, which can enable the titanium dioxide to be evenly dispersed in the polyethylene terephthalate melt to form a polyester semi-matt melt with a semi-matt effect.

[0009] Preferably, the modified titanium dioxide is prepared by modifying titanium dioxide with a polyester dispersant.

[0010] By adopting the above technical solution, the polyester dispersant combines with the active sites on the surface of titanium dioxide to form a stable interface layer, reduce the mutual attraction between titanium dioxide particles, and improve the stable dispersion effect of titanium dioxide in the polymer melt. The polyester dispersant is similar to the polyester semi-matt melt polymer matrix and can improve the compatibility of the polymer matrix.

[0011] Preferably, the polyester dispersant comprises the following raw materials in parts by weight: 80-90 parts of 12-hydroxystearic acid, 20-30 parts of tetraethylenepentamine, 1-3 parts of stannous chloride, and 40-50 parts of solvent.

[0012] By adopting the above technical solution, 12-hydroxystearic acid is used as the main dispersant component to provide a long-chain fatty acid structure, which helps to form a stable interface layer on the surface of titanium dioxide and improve the dispersibility of titanium dioxide in the polymer melt. Tetraethylenepentamine reacts with the hydroxyl group of 12-hydroxystearic acid to form a cross-linked structure, which enhances the thermal stability and chemical stability of the polyester dispersant. At the same time, the amine group of tetraethylenepentamine can react with the hydroxyl group or carboxyl group on the surface of titanium dioxide, thereby improving the compatibility of titanium dioxide with the polymer, improving the strength of polyester fibers, and reducing the breakage of fibers during processing.

[0013] Preferably, the preparation method of the modified titanium dioxide comprises the following specific steps: mixing 12-hydroxystearic acid, stannous chloride and a solvent, heating to 160-180°C for reaction, performing reduced pressure distillation under the protection of nitrogen, adding tetraethylenepentamine and keeping warm at 140-150°C for reaction, and obtaining a polyester dispersant after reduced pressure distillation; mixing the polyester dispersant with titanium dioxide, stirring at high speed, removing the solvent, and vacuum drying to obtain the modified titanium dioxide.

[0014] Preferably, the full matte masterbatch comprises the following specific steps: 30-50 parts of polyurethane matrix resin, 20-30 parts of talcum powder, 20-40 parts of silicon dioxide, and 5-10 parts of dispersion liquid.

[0015] By adopting the above technical solution, the molecular structure of the polyurethane matrix resin is similar to that of polyester, and can be well compatible with polyester melt. At the same time, the high molecular weight and cross-linked structure of polyurethane help to improve the stability and dispersibility of the full matte masterbatch in the polyester fiber system. Talc can improve the fluidity of the full matte masterbatch, reduce the agglomeration phenomenon of the full matte masterbatch in the polyester semi-matte melt, and can also improve the thermal stability of the full matte masterbatch. Silicon dioxide makes the prepared full matte masterbatch have a good matte effect, and can synergize with titanium dioxide in the polyester semi-matte melt to enhance the matte effect of polyester POY fiber.

[0016] Preferably, the dispersion is a mixture of nanocellulose and ethanol aqueous solution, and the mass ratio of the nanocellulose to the ethanol aqueous solution is 1:(10-15).

[0017] By adopting the above technical solution, nanocellulose uses its high specific surface area and surface activity to adsorb on the surface of particles in the full matte masterbatch system, reduce the agglomeration between particles, form a stable dispersion system, improve the dispersion effect of the full matte masterbatch system, further improve the matte uniformity and strength of polyester POY fiber, and reduce the breakage of fibers during processing. The use of ethanol aqueous solution can reduce the viscosity of the system and improve fluidity. At the same time, the volatility of ethanol helps to evaporate quickly during processing, reduce residues, and improve the stability of the full matte masterbatch.

[0018] Preferably, the method for preparing the full matte masterbatch comprises the following specific steps: mixing a polyurethane matrix resin, talcum powder, silicon dioxide and a dispersion liquid, heating to 200-250° C. for melt extrusion, and granulating to obtain the full matte masterbatch.

[0019] In summary, this application has the following beneficial effects: 1. Since the present application reduces the amount of titanium dioxide in the polyester semi-matt melt by using full matt masterbatch, reduces the phenomenon of particle agglomeration caused by excessive use of titanium dioxide, improves the uniformity of the polyester POY fiber system, and produces full matt flat polyester POY fiber by melt direct spinning, it is conducive to long-term continuous production. Adding an appropriate amount of trimethyl phosphate to the polyethylene terephthalate system interacts with the polyester molecules, stabilizes the polyester structure, and improves the stability of the polyester semi-matt melt in spinning.

[0020] 2. In this application, polyester dispersant is used to disperse and modify titanium dioxide, reduce the mutual attraction between titanium dioxide particles, and improve the dispersibility and compatibility of titanium dioxide in polymer melt. Tetraethylenepentamine is used in the polyester dispersant system to react with the hydroxyl group of hydroxystearic acid to form a cross-linked structure, which reacts with the hydroxyl group or carboxyl group on the surface of titanium dioxide to improve the compatibility of titanium dioxide with the polymer. DETAILED DESCRIPTION

[0021] The present application is further described in detail below with reference to the embodiments.

[0022] All raw materials in the examples are commercially available. Example

[0023] Example 1 This embodiment provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 40 kg of polyurethane matrix resin, 25 kg of talcum powder and 30 kg of silicon dioxide were mixed, the polyurethane matrix resin CAS number was 68227-93-0, heated to 230°C for melt extrusion, and granulated to obtain full matte masterbatch.

[0024] S2: Mix titanium dioxide and 12-hydroxystearic acid evenly, with the mass ratio of titanium dioxide to 12-hydroxystearic acid being 1:0.8, and grind and dry to obtain modified titanium dioxide powder.

[0025] S3: 80kg of terephthalic acid, 25kg of ethylene glycol, 4kg of modified titanium dioxide powder, 0.8kg of ethylene glycol antimony, 2kg of trimethyl phosphate and 0.04kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the full-dull masterbatch is melted at 270°C and dynamically mixed with the polyester semi-dull melt, the mass ratio of the polyester semi-dull melt to the molten full-dull masterbatch is 10:1, and after spinning, it is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a full-dull flat polyester POY fiber.

[0026] Example 2 This embodiment provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 40 kg of polyurethane matrix resin, 25 kg of talcum powder and 30 kg of silicon dioxide were mixed, the polyurethane matrix resin CAS number was 68227-93-0, heated to 230°C for melt extrusion, and granulated to obtain full matte masterbatch.

[0027] S2: Mix titanium dioxide and 12-hydroxystearic acid evenly, with the mass ratio of titanium dioxide to 12-hydroxystearic acid being 1:0.8, and grind and dry to obtain modified titanium dioxide powder.

[0028] S3: 70kg of terephthalic acid, 20kg of ethylene glycol, 3kg of modified titanium dioxide powder, 0.5kg of ethylene glycol antimony, 1kg of trimethyl phosphate and 0.03kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the full-dull masterbatch is melted at 270°C and dynamically mixed with the polyester semi-dull melt, the mass ratio of the polyester semi-dull melt to the molten full-dull masterbatch is 10:1, and after spinning, it is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a full-dull flat polyester POY fiber.

[0029] Example 3 This embodiment provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 40 kg of polyurethane matrix resin, 25 kg of talcum powder and 30 kg of silicon dioxide were mixed, the polyurethane matrix resin CAS number was 68227-93-0, heated to 230°C for melt extrusion, and granulated to obtain full matte masterbatch.

[0030] S2: Mix titanium dioxide and 12-hydroxystearic acid evenly, with the mass ratio of titanium dioxide to 12-hydroxystearic acid being 1:0.8, and grind and dry to obtain modified titanium dioxide powder.

[0031] S3: 90kg of terephthalic acid, 30kg of ethylene glycol, 5kg of modified titanium dioxide powder, 1kg of ethylene glycol antimony, 3kg of trimethyl phosphate and 0.05kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the full-dull masterbatch is melted at 270°C and dynamically mixed with the polyester semi-dull melt, the mass ratio of the polyester semi-dull melt to the molten full-dull masterbatch is 10:1, and after spinning, it is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a full-dull flat polyester POY fiber.

[0032] Example 4 This embodiment provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 40 kg of polyurethane matrix resin, 25 kg of talcum powder and 30 kg of silicon dioxide were mixed, the polyurethane matrix resin CAS number was 68227-93-0, heated to 230°C for melt extrusion, and granulated to obtain full matte masterbatch.

[0033] S2: 85 kg of 12-hydroxystearic acid, 2 kg of stannous chloride and 45 kg of solvent are mixed, wherein the solvent is xylene, and the mixture is heated to 170°C for reaction for 20 hours, and then distilled under reduced pressure under the protection of nitrogen. Then, 25 kg of tetraethylenepentamine is added and the mixture is kept warm for reaction at 145°C for 3 hours, and a polyester dispersant is obtained after distillation under reduced pressure. The polyester dispersant is mixed with titanium dioxide, wherein the mass ratio of the polyester dispersant to titanium dioxide is 1:10, and the mixture is stirred at high speed, the solvent is removed, and the mixture is dried in vacuo to obtain modified titanium dioxide.

[0034] S3: 80kg of terephthalic acid, 25kg of ethylene glycol, 4kg of modified titanium dioxide powder, 0.8kg of ethylene glycol antimony, 2kg of trimethyl phosphate and 0.04kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the full-dull masterbatch is melted at 270°C and dynamically mixed with the polyester semi-dull melt, the mass ratio of the polyester semi-dull melt to the molten full-dull masterbatch is 10:1, and after spinning, it is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a full-dull flat polyester POY fiber.

[0035] Example 5 This embodiment provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 40 kg of polyurethane matrix resin, 25 kg of talcum powder and 30 kg of silicon dioxide were mixed, the polyurethane matrix resin CAS number was 68227-93-0, heated to 230°C for melt extrusion, and granulated to obtain full matte masterbatch.

[0036] S2: Mix 80kg 12-hydroxystearic acid, 1kg stannous chloride and 40kg solvent, wherein the solvent is xylene, heat to 170°C for reaction for 20h, distill under reduced pressure under the protection of nitrogen, add 20kg tetraethylenepentamine and keep warm for reaction at 145°C for 3h, and obtain polyester dispersant after distillation under reduced pressure; mix the polyester dispersant with titanium dioxide, wherein the mass ratio of the polyester dispersant to titanium dioxide is 1:10, stir at high speed, remove the solvent, and dry under vacuum to obtain modified titanium dioxide.

[0037] S3: 80kg of terephthalic acid, 25kg of ethylene glycol, 4kg of modified titanium dioxide powder, 0.8kg of ethylene glycol antimony, 2kg of trimethyl phosphate and 0.04kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the full-dull masterbatch is melted at 270°C and dynamically mixed with the polyester semi-dull melt, the mass ratio of the polyester semi-dull melt to the molten full-dull masterbatch is 10:1, and after spinning, it is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a full-dull flat polyester POY fiber.

[0038] Example 6 This embodiment provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 40 kg of polyurethane matrix resin, 25 kg of talcum powder and 30 kg of silicon dioxide were mixed, the polyurethane matrix resin CAS number was 68227-93-0, heated to 230°C for melt extrusion, and granulated to obtain full matte masterbatch.

[0039] S2: Mix 90kg 12-hydroxystearic acid, 3kg stannous chloride and 50kg solvent, wherein the solvent is xylene, heat to 170°C for reaction for 20h, distill under reduced pressure under the protection of nitrogen, then add 30kg tetraethylenepentamine and keep warm for reaction at 145°C for 3h, and obtain polyester dispersant after distillation under reduced pressure; mix the polyester dispersant with titanium dioxide, wherein the mass ratio of the polyester dispersant to titanium dioxide is 1:10, stir at high speed, remove the solvent, and dry under vacuum to obtain modified titanium dioxide.

[0040] S3: 80kg of terephthalic acid, 25kg of ethylene glycol, 4kg of modified titanium dioxide powder, 0.8kg of ethylene glycol antimony, 2kg of trimethyl phosphate and 0.04kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the full-dull masterbatch is melted at 270°C and dynamically mixed with the polyester semi-dull melt, the mass ratio of the polyester semi-dull melt to the molten full-dull masterbatch is 10:1, and after spinning, it is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a full-dull flat polyester POY fiber.

[0041] Example 7 This embodiment provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 40kg of polyurethane matrix resin, 25kg of talcum powder, 30kg of silicon dioxide and 8kg of dispersion liquid are mixed, the polyurethane matrix resin CAS number is 68227-93-0, the dispersion liquid is a mixture of nanocellulose and 95% ethanol aqueous solution by volume, the mass ratio of nanocellulose to 95% ethanol aqueous solution by volume is 1:13, heat to 230°C for melt extrusion, and granulate to obtain full matte masterbatch.

[0042] S2: Mix 80kg 12-hydroxystearic acid, 1kg stannous chloride and 40kg solvent, wherein the solvent is xylene, heat to 170°C for reaction for 20h, distill under reduced pressure under the protection of nitrogen, add 20kg tetraethylenepentamine and keep warm for reaction at 145°C for 3h, and obtain polyester dispersant after distillation under reduced pressure; mix the polyester dispersant with titanium dioxide, wherein the mass ratio of the polyester dispersant to titanium dioxide is 1:10, stir at high speed, remove the solvent, and dry under vacuum to obtain modified titanium dioxide.

[0043] S3: 80kg of terephthalic acid, 25kg of ethylene glycol, 4kg of modified titanium dioxide powder, 0.8kg of ethylene glycol antimony, 2kg of trimethyl phosphate and 0.04kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the full-dull masterbatch is melted at 270°C and dynamically mixed with the polyester semi-dull melt, the mass ratio of the polyester semi-dull melt to the molten full-dull masterbatch is 10:1, and after spinning, it is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a full-dull flat polyester POY fiber.

[0044] Example 8 This embodiment provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 30 kg of polyurethane matrix resin, 30 kg of talcum powder, 20 kg of silicon dioxide and 5 kg of dispersion liquid are mixed, the polyurethane matrix resin CAS number is 68227-93-0, the dispersion liquid is a mixture of nanocellulose and 95% ethanol aqueous solution by volume, the mass ratio of nanocellulose to 95% ethanol aqueous solution by volume is 1:13, heat to 230 ° C for melt extrusion, and granulate to obtain full matte masterbatch.

[0045] S2: Mix 80kg 12-hydroxystearic acid, 1kg stannous chloride and 40kg solvent, wherein the solvent is xylene, heat to 170°C for reaction for 20h, distill under reduced pressure under the protection of nitrogen, add 20kg tetraethylenepentamine and keep warm for reaction at 145°C for 3h, and obtain polyester dispersant after distillation under reduced pressure; mix the polyester dispersant with titanium dioxide, wherein the mass ratio of the polyester dispersant to titanium dioxide is 1:10, stir at high speed, remove the solvent, and dry under vacuum to obtain modified titanium dioxide.

[0046] S3: 80kg of terephthalic acid, 25kg of ethylene glycol, 4kg of modified titanium dioxide powder, 0.8kg of ethylene glycol antimony, 2kg of trimethyl phosphate and 0.04kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the full-dull masterbatch is melted at 270°C and dynamically mixed with the polyester semi-dull melt, the mass ratio of the polyester semi-dull melt to the molten full-dull masterbatch is 10:1, and after spinning, it is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a full-dull flat polyester POY fiber.

[0047] Example 9 This embodiment provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 50 kg of polyurethane matrix resin, 20 kg of talcum powder, 40 kg of silicon dioxide and 10 kg of dispersion liquid are mixed, the polyurethane matrix resin CAS number is 68227-93-0, the dispersion liquid is a mixture of nanocellulose and 95% ethanol aqueous solution by volume, the mass ratio of nanocellulose to 95% ethanol aqueous solution by volume is 1:13, heat to 230 ° C for melt extrusion, and granulate to obtain full matte masterbatch.

[0048] S2: Mix 80kg 12-hydroxystearic acid, 1kg stannous chloride and 40kg solvent, wherein the solvent is xylene, heat to 170°C for reaction for 20h, distill under reduced pressure under the protection of nitrogen, add 20kg tetraethylenepentamine and keep warm for reaction at 145°C for 3h, and obtain polyester dispersant after distillation under reduced pressure; mix the polyester dispersant with titanium dioxide, wherein the mass ratio of the polyester dispersant to titanium dioxide is 1:10, stir at high speed, remove the solvent, and dry under vacuum to obtain modified titanium dioxide.

[0049] S3: 80kg of terephthalic acid, 25kg of ethylene glycol, 4kg of modified titanium dioxide powder, 0.8kg of ethylene glycol antimony, 2kg of trimethyl phosphate and 0.04kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the full-dull masterbatch is melted at 270°C and dynamically mixed with the polyester semi-dull melt, the mass ratio of the polyester semi-dull melt to the molten full-dull masterbatch is 10:1, and after spinning, it is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a full-dull flat polyester POY fiber.

[0050] Comparative Example Comparative Example 1 Comparative Example 1 provides a method for producing a fully matte flat polyester POY fiber, comprising the following specific steps: S1: 40 kg of polyurethane matrix resin, 25 kg of talcum powder and 30 kg of silicon dioxide were mixed, the polyurethane matrix resin CAS number was 68227-93-0, heated to 230°C for melt extrusion, and granulated to obtain full matte masterbatch.

[0051] S2: 80kg of terephthalic acid, 25kg of ethylene glycol, 0.8kg of ethylene glycol antimony, 2kg of trimethyl phosphate and 0.04kg of catalyst are mixed, wherein the catalyst is germanium dioxide. Under the protection of nitrogen, esterification reaction and pre-polycondensation reaction are carried out in sequence at 245°C, and final polycondensation reaction is carried out at 270°C to generate polyethylene terephthalate to obtain a polyester melt; the full matte masterbatch is melted at 270°C and dynamically mixed with the polyester melt, wherein the mass ratio of the polyester melt to the molten full matte masterbatch is 10:1, and after spinning, a composite melt stream is extruded from a flat wavy spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, which is then oiled and wound in sequence to obtain a full matte flat polyester POY fiber.

[0052] Performance testing The following performance tests were performed on the full-dull flat polyester POY fibers provided in Examples 1-9 and Comparative Example 1 of the present application. The specific test results are shown in Table 1.

[0053] Detection Methods 1. Mechanical properties The monofilament fineness of the full-dull flat polyester POY fiber prepared in this application was tested with reference to the standard of GB / T14335-2008 "Test Method for Density of Chemical Staple Fibers". The breaking strength and breaking elongation of the full-dull flat polyester POY fiber prepared in this application were tested with reference to the standard of GB / T14334-2008 "Test Method for Tensile Properties of Chemical Staple Fibers".

[0054] 2. Glossiness The glossiness of the fully matte flat polyester POY fiber prepared in the present application was tested using a gloss tester.

[0055] Table 1: Performance test results data table It can be seen from the performance test results that the fully matte flat polyester POY fiber prepared in the present application has a uniform matte effect in appearance, and the glossiness reaches the full matte requirement. At the same time, under the synergistic effect of each component, it has good strength, and the stability of the polyester POY fiber is improved. By comparing Comparative Example 1 with Example 1, it can be seen that Comparative Example 1 does not use titanium dioxide in the polyester semi-matte melt. From the performance test results, it can be seen that the strength of the polyester fiber decreases, and the matte effect is also affected.

[0056] 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 method for producing full-dull flat polyester POY fiber, characterized in that: The specific steps include: Terephthalic acid and ethylene glycol, modified titanium dioxide powder, ethylene glycol antimony, trimethyl phosphate and a catalyst are mixed, and esterification reaction, pre-polycondensation reaction and final polycondensation reaction are carried out in sequence to generate polyethylene terephthalate to obtain a polyester semi-dull melt; the fully-dull masterbatch is melted and mixed with the polyester semi-dull melt for spinning, and extruded from a flat spinneret to obtain a composite melt stream, which is then cooled and solidified by annular blowing to form a primary fiber, and then oiled and wound in sequence to obtain a fully-dull flat polyester POY fiber.

2. The method for producing full-dull flat polyester POY fiber according to claim 1, characterized in that: The polyethylene terephthalate comprises the following raw materials in parts by weight: 70-90 parts of terephthalic acid, 20-30 parts of ethylene glycol, 3-5 parts of modified titanium dioxide, 0.5-1 parts of ethylene glycol antimony, 1-3 parts of trimethyl phosphate and 0.03-0.05 parts of a catalyst.

3. The method for producing full-dull flat polyester POY fiber according to claim 2, characterized in that: The modified titanium dioxide is prepared by modifying titanium dioxide with a polyester dispersant.

4. The method for producing full-dull flat polyester POY fiber according to claim 3, characterized in that: The polyester dispersant comprises the following raw materials in parts by weight: 80-90 parts of 12-hydroxystearic acid, 20-30 parts of tetraethylenepentamine, 1-3 parts of stannous chloride and 40-50 parts of solvent.

5. The method for producing full-dull flat polyester POY fiber according to claim 4, characterized in that: The preparation method of the modified titanium dioxide comprises the following specific steps: mixing 12-hydroxystearic acid, stannous chloride and a solvent, heating to 160-180°C for reaction, performing reduced pressure distillation under the protection of nitrogen, adding tetraethylenepentamine and performing heat preservation reaction at 140-150°C, and obtaining a polyester dispersant after reduced pressure distillation; mixing the polyester dispersant with titanium dioxide, stirring at high speed, removing the solvent, and vacuum drying to obtain the modified titanium dioxide.

6. The method for producing full-dull flat polyester POY fiber according to claim 1, characterized in that: The full matte masterbatch comprises the following specific steps: 30-50 parts of polyurethane matrix resin, 20-30 parts of talcum powder, 20-40 parts of silicon dioxide, and 5-10 parts of dispersion liquid.

7. The method for producing full-dull flat polyester POY fiber according to claim 6, characterized in that: The dispersion liquid is a mixed liquid of nanocellulose and ethanol aqueous solution, and the mass ratio of the nanocellulose to the ethanol aqueous solution is 1: (10-15).

8. The method for producing full-dull flat polyester POY fiber according to claim 6, characterized in that: The method for preparing the full matte masterbatch comprises the following specific steps: mixing a polyurethane matrix resin, talcum powder, silicon dioxide and a dispersion liquid, heating to 200-250° C. for melt extrusion, and granulating to obtain the full matte masterbatch.

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