Environment-friendly flame-retardant polyester yarn and preparation method thereof

By using flame retardant polymers and other additives containing organic salt structures in flame retardant polyester yarns, the problems of phase separation and environmental pollution during use are solved, and better Flame retardant properties, UV aging resistance and mechanical strength.

CN119392399AInactive Publication Date: 2025-02-07YANGZHOU LEKANG TEXTILE TECH CO LTD

Patent Information

Application Number
CN202411523206.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-30
Publication Date
2025-02-07
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing flame retardant polyester yarns are prone to phase separation during use, which affects the service life. The flame retardant used is highly polluted to the environment, and the mechanical strength and UV aging resistance are insufficient.

Method used

The flame-retardant polymer containing organic salt structure is used as the flame-retardant active ingredient, combined with polyester slices, antioxidants, lubricants, benzotriazole sodium and quinoline yellow, and prepared environmentally friendly through ion exchange treatment and drafting processing. Flame-retardant polyester yarn.

Benefits of technology

It improves the flame retardant performance, UV aging resistance and mechanical strength of the yarn, avoids environmental pollution and phase separation problems of the flame retardant, and extends the service life.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses an environment-friendly flame-retardant polyester yarn and a preparation method thereof, and relates to the technical field of textile, and the environment-friendly flame-retardant polyester yarn is prepared from the following raw materials in parts by weight: 100 parts of polyester chips, 10-15 parts of a flame-retardant polymer containing an organic salt structure, 1-3 parts of an antioxidant, 0.8-2 parts of a lubricant, 1-2 parts of benzotriazole sodium and 0.8-1.2 parts of quinoline yellow. The flame-retardant polymer containing the organic salt structure comprises a structural unit introduced by the following monomers: bis (3-aminophenyl) (3, 5-bis (trifluoromethyl) phenyl) phosphine oxide, 3, 7-diamino-5-phenylphenazine chloride and 3, 5-isoxazole dicarboxylic acid. The environment-friendly flame-retardant polyester yarn is good in ultraviolet aging resistance and flame retardance, high in strength and sufficient in softness.
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Description

Technical Field

[0001] The invention relates to the technical field of textiles, and in particular to an environmentally friendly flame-retardant polyester yarn and a preparation method thereof. Background Art

[0002] Polyester is the simplest of the three major synthetic fibers, and its price is relatively cheap. It is a very common chemical fiber clothing fabric in daily life. Its biggest advantage is its good wrinkle resistance and shape retention. Therefore, it is suitable for outerwear, various bags, tents and other outdoor products. With the improvement of people's awareness of fire hazards and the strengthening of safety awareness, the flame retardant function of various multifunctional fibers and textiles has become a standard for measuring the excellent performance of materials. Flame retardant polyester yarn has become a new hot spot in my country's textile market and has good development prospects.

[0003] At present, flame-retardant polyester yarn is mainly achieved by adding flame retardants. However, the combustion of existing flame retardants will cause great pollution to the environment, and due to the compatibility problem between the flame retardant and the polyester substrate, the produced polyester yarn is prone to phase separation during long-term use, affecting the service life.

[0004] In order to solve the above problems, the Chinese invention patent with authorization announcement number CN115506062B discloses an environmentally friendly flame-retardant polyester yarn, including the following weight percentages of fibers: 60-70% polyester outer solid thread and 30-40% cotton inner core thread. A method for preparing an environmentally friendly flame-retardant polyester yarn comprises the following steps: S1, pre-treating the polyester outer solid thread and the cotton inner core thread respectively; S2, subjecting the pre-treated polyester outer solid thread and the cotton inner core thread to carding, blending and twisting in turn to obtain the environmentally friendly flame-retardant polyester yarn. The invention discloses an environmentally friendly flame-retardant polyester yarn and a method for making the same, which have good softness and flame retardancy. However, the mechanical strength and UV aging resistance of the polyester yarn still need to be further improved. Summary of the invention

[0005] In view of this, the purpose of the present invention is to provide an environmentally friendly flame-retardant polyester yarn and a preparation method thereof, which has good ultraviolet aging resistance and flame retardant properties, and has high strength. No toxic flame retardants that are not compatible with polyester substrates are used in the preparation process, thereby avoiding the release and volatilization of flame retardant residues that affect human health and the atmospheric environment; it also avoids the insufficient performance stability caused by compatibility problems.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] An environmentally friendly flame-retardant polyester yarn comprises the following raw materials in parts by weight: 100 parts of polyester chips, 10-15 parts of flame-retardant polymers containing organic salt structures, 1-3 parts of antioxidants, 0.8-2 parts of lubricants, 1-2 parts of sodium benzotriazole, and 0.8-1.2 parts of quinoline yellow; the flame-retardant polymer containing organic salt structures comprises structural units introduced by the following monomers: bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, and 3,5-isoxazoledicarboxylic acid.

[0008] Preferably, the polyester chips are industrial yarn-specific polyester chips 224 produced by Sinopec.

[0009] Preferably, the preparation method of the flame-retardant polymer containing an organic salt structure comprises the following steps: adding bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazoledicarboxylic acid, and a catalyst to a high boiling point solvent and mixing them evenly to obtain a mixed material, then adding the mixed material to a reaction kettle, replacing the air in the kettle with an inert gas, reacting at 120-130°C under normal pressure for 3-5 hours, then heating to 235-255°C, and performing a condensation reaction at 100-400 Pa for 15-22 hours, then cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the crude product with ethanol 3-6 times, and then placing it in a vacuum drying oven at 85-95°C to dry to constant weight to obtain a flame-retardant polymer containing an organic salt structure.

[0010] Preferably, the molar ratio of the bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazoledicarboxylic acid, catalyst and high boiling point solvent is 0.8:0.2:1:(0.8-1.2):(6-10).

[0011] Preferably, the catalyst is at least one of thiophosphonate, phosphorous acid, and thiophosphoramide; the high boiling point solvent is dimethyl sulfoxide; and the inert gas is any one of nitrogen, helium, neon, and argon.

[0012] Preferably, the antioxidant is at least one of antioxidant 1010 and antioxidant 168; the lubricant is at least one of pentaerythritol stearate and ethylene bisstearamide.

[0013] Another object of the present invention is to provide a method for preparing the environmentally friendly flame-retardant polyester yarn, comprising the following steps:

[0014] Step S1, mixing polyester slices, flame retardant polymers containing organic salt structures, antioxidants and lubricants uniformly to obtain spinning raw materials, drying and adding them into a composite spinning machine for spinning, and then stretching to obtain primary polyester fibers;

[0015] Step S2, soaking the nascent polyester fiber in an aqueous solution containing sodium benzotriazole and quinoline yellow for 1-2 hours for ion exchange treatment, then washing with deionized water for 3-6 times, and drying at room temperature to obtain polyester fiber;

[0016] Step S3, drying the polyester fiber in a drying device; and then making the dried polyester fiber into the polyester yarn in a yarn blending machine.

[0017] Preferably, the spinning temperature in step S1 is 265-295° C., and the spinning winding speed is 1000-2500 m / min.

[0018] Preferably, the stretching processing parameters in step S1 are a stretching multiple of 2-4 times, a hot plate temperature of 60-90°C, and a hot plate temperature of 110-210°C.

[0019] Preferably, the mass ratio of sodium benzotriazole to water in the aqueous solution containing sodium benzotriazole and quinoline yellow in step S2 is (5-8):100.

[0020] The beneficial effects of adopting the above technical solution are:

[0021] (1) The environmentally friendly flame-retardant polyester yarn provided by the present invention uses a flame-retardant polymer containing an organic salt structure as a flame-retardant active ingredient added to a polyester chip substrate, so that the flame-retardant active ingredient can be evenly dispersed in the yarn, making the flame-retardant effect of the yarn more excellent and lasting. The flame-retardant polymer containing an organic salt structure includes structural units introduced from the following monomers: bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, and 3,5-isoxazoledicarboxylic acid. Phenylphosphine oxide, phenylphenazine salt, isoxazole and amide structures are simultaneously introduced into its molecular structure, and their interaction can give the product more excellent flame-retardant properties, and the formed polymer has good compatibility with the polyester chip substrate, and the product has good performance stability.

[0022] (2) In the environmentally friendly flame-retardant polyester yarn provided by the present invention, the structural unit introduced by 3,7-diamino-5-phenylphenazine chloride can undergo ion exchange reaction with sodium benzotriazole and quinoline yellow during the ion exchange treatment to remove chloride ions, so that the halogen content in the manufactured yarn is low, the environmental protection performance is relatively good, and the use is safer and more environmentally friendly.

[0023] (3) The environmentally friendly flame-retardant polyester yarn provided by the present invention forms an interpenetrating network ionic cross-linked structure on the fiber surface by soaking in quinoline yellow, which cooperates with the simultaneous introduction of benzotriazole and quinolyl indane dione structures to give the product advantages such as better UV aging resistance and flame retardancy, and greater strength. DETAILED DESCRIPTION

[0024] In order to make the technical solution of the present invention better understood by the technical personnel in the field, and to make the above-mentioned features, purposes and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with the embodiments. The embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention.

[0025] Example 1

[0026] An environmentally friendly flame-retardant polyester yarn comprises the following raw materials in parts by weight: 100 parts of polyester chips, 10 parts of flame-retardant polymers containing organic salt structures, 1 part of antioxidants, 0.8 parts of lubricants, 1 part of sodium benzotriazole, and 0.8 parts of quinoline yellow; the flame-retardant polymer containing organic salt structures comprises structural units introduced by the following monomers: bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, and 3,5-isoxazoledicarboxylic acid; the polyester chips are polyester chips 224 for industrial yarns produced by Sinopec.

[0027] The preparation method of the flame-retardant polymer containing an organic salt structure comprises the following steps: adding bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazole dicarboxylic acid and a catalyst into a high boiling point solvent and mixing them evenly to obtain a mixed material, then adding the mixed material into a reaction kettle, replacing the air in the kettle with an inert gas, reacting at 120° C. for 3 hours at normal pressure, then heating to 235° C., performing a polycondensation reaction at 100 Pa for 15 hours, then cooling to room temperature, adjusting to normal pressure, precipitating in water, and rinsing with ethanol. The crude product was washed three times, and then placed in a vacuum drying oven at 85° C. and dried to constant weight to obtain a flame retardant polymer containing an organic salt structure; the molar ratio of the bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazoledicarboxylic acid, catalyst, and high boiling point solvent was 0.8:0.2:1:0.8:6; the catalyst was a thiophosphonate; the high boiling point solvent was dimethyl sulfoxide; the inert gas was nitrogen; the number average molecular weight of the polymer was 16890 g / mol through GPC testing, M W / M n=1.382; through elemental analysis and weight change calculation, the molar ratio of the structural units introduced by bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, and 3,5-isoxazoledicarboxylic acid is the same as the theoretical value.

[0028] The antioxidant is antioxidant 1010; the lubricant is pentaerythritol stearate.

[0029] A method for preparing the environmentally friendly flame-retardant polyester yarn comprises the following steps:

[0030] Step S1, mixing polyester slices, flame retardant polymers containing organic salt structures, antioxidants and lubricants uniformly to obtain spinning raw materials, drying and adding them into a composite spinning machine for spinning, and then stretching to obtain primary polyester fibers;

[0031] Step S2, soaking the nascent polyester fiber in an aqueous solution containing sodium benzotriazole and quinoline yellow for ion exchange treatment for 1 hour, then washing with deionized water for 3 times, and drying at room temperature to obtain polyester fiber;

[0032] Step S3, drying the polyester fiber in a drying device; and then making the dried polyester fiber into the polyester yarn in a yarn blending machine.

[0033] The spinning temperature of the spinning in step S1 is 265° C., and the spinning winding speed is 1000 m / min; the drawing processing parameters in step S1 are a drawing multiple of 3 times, a hot plate temperature of 60° C., and a hot plate temperature of 110° C.; the mass ratio of sodium benzotriazole to water in the aqueous solution containing sodium benzotriazole and quinoline yellow in step S2 is 5:100.

[0034] Example 2

[0035] An environmentally friendly flame-retardant polyester yarn comprises the following raw materials in parts by weight: 100 parts of polyester chips, 12 parts of flame-retardant polymers containing organic salt structures, 1.5 parts of antioxidants, 1 part of lubricants, 1.2 parts of sodium benzotriazole, and 0.9 parts of quinoline yellow; the flame-retardant polymer containing organic salt structures comprises structural units introduced by the following monomers: bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, and 3,5-isoxazoledicarboxylic acid; the polyester chips are polyester chips 224 for industrial yarns produced by Sinopec.

[0036] The method for preparing a flame-retardant polymer containing an organic salt structure comprises the following steps: adding bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazole dicarboxylic acid and a catalyst into a high boiling point solvent and mixing them evenly to obtain a mixed material; then adding the mixed material into a reaction kettle, replacing the air in the kettle with an inert gas, reacting at 123° C. under normal pressure for 3.5 hours, then heating to 240° C., performing a polycondensation reaction at 200 Pa for 17 hours, and then cooling the mixture. to room temperature, adjusted to normal pressure, precipitated in water, washed the crude product 4 times with ethanol, and then dried in a vacuum drying oven at 87° C. to constant weight to obtain a flame retardant polymer containing an organic salt structure; the molar ratio of the bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazoledicarboxylic acid, catalyst, and high boiling point solvent is 0.8:0.2:1:0.9:7; the catalyst is phosphorous acid; the high boiling point solvent is dimethyl sulfoxide; and the inert gas is helium.

[0037] The antioxidant is antioxidant 168; the lubricant is ethylene bisstearamide.

[0038] A method for preparing the environmentally friendly flame-retardant polyester yarn comprises the following steps:

[0039] Step S1, mixing polyester slices, flame retardant polymers containing organic salt structures, antioxidants and lubricants uniformly to obtain spinning raw materials, drying and adding them into a composite spinning machine for spinning, and then stretching to obtain primary polyester fibers;

[0040] Step S2, soaking the nascent polyester fiber in an aqueous solution containing sodium benzotriazole and quinoline yellow for 1.2 hours for ion exchange treatment, then washing with deionized water for 4 times, and drying at room temperature to obtain polyester fiber;

[0041] Step S3, drying the polyester fiber in a drying device; and then making the dried polyester fiber into the polyester yarn in a yarn blending machine.

[0042] The spinning temperature of the spinning in step S1 is 275° C., and the spinning winding speed is 1300 m / min; the drawing processing parameters in step S1 are a drawing multiple of 3 times, a hot plate temperature of 65° C., and a hot plate temperature of 130° C.; the mass ratio of sodium benzotriazole to water in the aqueous solution containing sodium benzotriazole and quinoline yellow in step S2 is 6:100.

[0043] Example 3

[0044] An environmentally friendly flame-retardant polyester yarn comprises the following raw materials in parts by weight: 100 parts of polyester chips, 13 parts of flame-retardant polymers containing organic salt structures, 2 parts of antioxidants, 1.4 parts of lubricants, 1.5 parts of sodium benzotriazole, and 1 part of quinoline yellow; the flame-retardant polymer containing organic salt structures comprises structural units introduced by the following monomers: bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, and 3,5-isoxazoledicarboxylic acid; the polyester chips are polyester chips 224 for industrial yarns produced by Sinopec.

[0045] The method for preparing a flame-retardant polymer containing an organic salt structure comprises the following steps: adding bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazole dicarboxylic acid and a catalyst into a high boiling point solvent and mixing them evenly to obtain a mixed material; then adding the mixed material into a reaction kettle, replacing the air in the kettle with an inert gas, reacting at 125° C. for 4 hours at normal pressure, then heating to 245° C., performing a polycondensation reaction at 250 Pa for 18 hours, and then cooling to The mixture is prepared from room temperature, adjusted to normal pressure, precipitated in water, washed with ethanol for 4 times, and then dried in a vacuum drying oven at 90° C. to constant weight to obtain a flame retardant polymer containing an organic salt structure; the molar ratio of the bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazoledicarboxylic acid, catalyst, and high boiling point solvent is 0.8:0.2:1:1:8; the catalyst is thiophosphoramide; the high boiling point solvent is dimethyl sulfoxide; and the inert gas is neon.

[0046] The antioxidant is antioxidant 1010; the lubricant is pentaerythritol stearate.

[0047] A method for preparing the environmentally friendly flame-retardant polyester yarn comprises the following steps:

[0048] Step S1, mixing polyester slices, flame retardant polymers containing organic salt structures, antioxidants and lubricants uniformly to obtain spinning raw materials, drying and adding them into a composite spinning machine for spinning, and then stretching to obtain primary polyester fibers;

[0049] Step S2, soaking the nascent polyester fiber in an aqueous solution containing sodium benzotriazole and quinoline yellow for ion exchange treatment for 1.5 hours, then washing with deionized water for 5 times, and drying at room temperature to obtain polyester fiber;

[0050] Step S3, drying the polyester fiber in a drying device; and then making the dried polyester fiber into the polyester yarn in a yarn blending machine.

[0051] The spinning temperature of the spinning in step S1 is 280° C., and the spinning winding speed is 1800 m / min; the drawing processing parameters in step S1 are a drawing multiple of 3 times, a hot plate temperature of 75° C., and a hot plate temperature of 180° C.; the mass ratio of sodium benzotriazole to water in the aqueous solution containing sodium benzotriazole and quinoline yellow in step S2 is 6.5:100.

[0052] Example 4

[0053] An environmentally friendly flame-retardant polyester yarn comprises the following raw materials in parts by weight: 100 parts of polyester chips, 14 parts of flame-retardant polymers containing organic salt structures, 2.5 parts of antioxidants, 1.8 parts of lubricants, 1.8 parts of sodium benzotriazole, and 1.1 parts of quinoline yellow; the flame-retardant polymer containing organic salt structures comprises structural units introduced by the following monomers: bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, and 3,5-isoxazoledicarboxylic acid; the polyester chips are polyester chips 224 for industrial yarns produced by Sinopec.

[0054] The method for preparing a flame-retardant polymer containing an organic salt structure comprises the following steps: adding bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazole dicarboxylic acid and a catalyst into a high boiling point solvent and mixing them evenly to obtain a mixed material; then adding the mixed material into a reaction kettle, replacing the air in the kettle with an inert gas, reacting at 128° C. for 4.5 hours at normal pressure, then heating to 253° C., performing a polycondensation reaction at 350 Pa for 21 hours, then cooling to room temperature, adjusting to normal pressure, and precipitating in water. , wash the crude product with ethanol for 6 times, and then dry it in a vacuum drying oven at 93°C to constant weight to obtain a flame retardant polymer containing an organic salt structure; the molar ratio of the bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazoledicarboxylic acid, catalyst, and high boiling point solvent is 0.8:0.2:1:1.1:9.5; the catalyst is a mixture of thiophosphonate, phosphorous acid, and thiophosphoramide in a mass ratio of 1:2:3; the high boiling point solvent is dimethyl sulfoxide; and the inert gas is argon.

[0055] The antioxidant is a mixture of antioxidant 1010 and antioxidant 168 in a mass ratio of 3:5; the lubricant is a mixture of pentaerythritol stearate and ethylene bisstearamide in a mass ratio of 1:3.

[0056] A method for preparing the environmentally friendly flame-retardant polyester yarn comprises the following steps:

[0057] Step S1, mixing polyester slices, flame retardant polymers containing organic salt structures, antioxidants and lubricants uniformly to obtain spinning raw materials, drying and adding them into a composite spinning machine for spinning, and then stretching to obtain primary polyester fibers;

[0058] Step S2, soaking the nascent polyester fiber in an aqueous solution containing sodium benzotriazole and quinoline yellow for ion exchange treatment for 1.8 hours, then washing with deionized water for 6 times, and drying at room temperature to obtain polyester fiber;

[0059] Step S3, drying the polyester fiber in a drying device; and then making the dried polyester fiber into the polyester yarn in a yarn blending machine.

[0060] The spinning temperature of the spinning in step S1 is 290° C., and the spinning winding speed is 2400 m / min; the drawing processing parameters in step S1 are a drawing multiple of 3 times, a hot plate temperature of 85° C., and a hot plate temperature of 200° C.; the mass ratio of sodium benzotriazole to water in the aqueous solution containing sodium benzotriazole and quinoline yellow in step S2 is 7.5:100.

[0061] Example 5

[0062] An environmentally friendly flame-retardant polyester yarn comprises the following raw materials in parts by weight: 100 parts of polyester chips, 15 parts of flame-retardant polymers containing organic salt structures, 3 parts of antioxidants, 2 parts of lubricants, 2 parts of sodium benzotriazole, and 1.2 parts of quinoline yellow; the flame-retardant polymer containing organic salt structures comprises structural units introduced by the following monomers: bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, and 3,5-isoxazoledicarboxylic acid; the polyester chips are polyester chips 224 for industrial yarns produced by Sinopec.

[0063] The method for preparing a flame-retardant polymer containing an organic salt structure comprises the following steps: adding bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazole dicarboxylic acid and a catalyst into a high boiling point solvent and mixing them evenly to obtain a mixed material; then adding the mixed material into a reaction kettle, replacing the air in the kettle with an inert gas, reacting at 130° C. under normal pressure for 5 hours, then heating to 255° C., performing a polycondensation reaction at 400 Pa for 22 hours, and then cooling to room temperature. , adjusted to normal pressure, precipitated in water, washed the crude product with ethanol 6 times, and then placed in a vacuum drying oven at 95°C to dry to constant weight to obtain a flame retardant polymer containing an organic salt structure; the molar ratio of the bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazoledicarboxylic acid, catalyst, and high boiling point solvent is 0.8:0.2:1:1.2:10; the catalyst is a thiophosphonate; the high boiling point solvent is dimethyl sulfoxide; and the inert gas is nitrogen.

[0064] The antioxidant is antioxidant 1010; the lubricant is pentaerythritol stearate.

[0065] A method for preparing the environmentally friendly flame-retardant polyester yarn comprises the following steps:

[0066] Step S1, mixing polyester slices, flame retardant polymers containing organic salt structures, antioxidants and lubricants uniformly to obtain spinning raw materials, drying and adding them into a composite spinning machine for spinning, and then stretching to obtain primary polyester fibers;

[0067] Step S2, soaking the nascent polyester fiber in an aqueous solution containing sodium benzotriazole and quinoline yellow for 2 hours for ion exchange treatment, then washing with deionized water for 6 times, and drying at room temperature to obtain polyester fiber;

[0068] Step S3, drying the polyester fiber in a drying device; and then making the dried polyester fiber into the polyester yarn in a yarn blending machine.

[0069] The spinning temperature of the spinning in step S1 is 295° C., and the spinning winding speed is 2500 m / min; the drawing processing parameters in step S1 are a drawing multiple of 3 times, a hot plate temperature of 90° C., and a hot plate temperature of 210° C.; the mass ratio of sodium benzotriazole to water in the aqueous solution containing sodium benzotriazole and quinoline yellow in step S2 is 8:100.

[0070] Comparative Example 1

[0071] An environmentally friendly flame-retardant polyester yarn and a preparation method thereof, which are basically the same as Example 1, except that an equal amount of bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide is used instead of 3,7-diamino-5-phenylphenazine chloride, and no quinoline yellow is added.

[0072] Comparative Example 2

[0073] An environmentally friendly flame-retardant polyester yarn and a preparation method thereof, which are basically the same as Example 1, except that an equal amount of 3,7-diamino-5-phenylphenazine chloride is used instead of bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, and no sodium benzotriazole is added.

[0074] The environmentally friendly flame-retardant polyester yarn samples described in Examples 1-5 and Comparative Examples 1-2 were subjected to performance tests. The test results are shown in Table 1. The test method is as follows:

[0075] Refer to GB / T 3916-1997 "Textiles, packaged yarn, single yarn - Determination of breaking strength and breaking elongation" standard for sampling and testing of yarn initial modulus. Take 250mm long yarns from the package yarn, a total of 20 yarns, fully pre-humidify and moisten the yarns, and test the conditioned yarns on the YG051 yarn electronic strength meter. Record the relevant data and calculate the average value of the initial modulus of the 20 yarns. The smaller the initial modulus, the better the softness of the yarn.

[0076] Refer to GB / T 5455-2014 "Determination of vertical damage length, smoldering and afterflaming time of textile combustion performance" to test the afterflaming time, flame retardant time and number of melt droplets.

[0077] Refer to GB / T 3916-2013 Method B for breaking strength test.

[0078] Heat aging resistance: Each polyester yarn sample was irradiated with a UV lamp with a wavelength of 350nm at room temperature for 48 hours, with the sample being 10cm away from the UV light source. The UV aging resistance was measured by the retention rate of breaking strength, and the larger the value, the better the UV aging resistance.

[0079] Table 1

[0080]

[0081] As can be seen from Table 1, the environmentally friendly flame-retardant polyester yarn disclosed in the embodiment of the present invention has better softness, flame retardancy, mechanical strength and UV aging resistance than the comparative example; the combined use of bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, quinoline yellow and sodium benzotriazole is beneficial to improving the above properties.

[0082] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions only describe the principles of the present invention. The present invention may be subject to various changes and improvements without departing from the spirit and scope of the present invention. These changes and improvements fall within the scope of the present invention. The scope of protection claimed by the present invention is defined by the attached claims and their equivalents.

Claims

1. An environmentally friendly flame-retardant polyester yarn, characterized in that: The invention comprises the following raw materials in parts by weight: 100 parts of polyester chips, 10-15 parts of flame-retardant polymers containing organic salt structures, 1-3 parts of antioxidants, 0.8-2 parts of lubricants, 1-2 parts of sodium benzotriazole, and 0.8-1.2 parts of quinoline yellow; the flame-retardant polymer containing organic salt structures comprises structural units introduced by the following monomers: bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, and 3,5-isoxazoledicarboxylic acid.

2. The environmentally friendly flame-retardant polyester yarn according to claim 1, characterized in that: The polyester chips are polyester chips 224 for industrial yarn produced by Sinopec.

3. The environmentally friendly flame-retardant polyester yarn according to claim 1, characterized in that: The preparation method of the flame-retardant polymer containing an organic salt structure comprises the following steps: adding bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazole dicarboxylic acid and a catalyst into a high boiling point solvent and mixing them evenly to obtain a mixed material, then adding the mixed material into a reaction kettle, replacing the air in the kettle with an inert gas, reacting at 120-130° C. under normal pressure for 3-5 hours, then heating to 235-255° C., carrying out a polycondensation reaction at 100-400 Pa for 15-22 hours, then cooling to room temperature, adjusting to normal pressure, precipitating in water, washing the crude product with ethanol for 3-6 times, and then drying it in a vacuum drying oven at 85-95° C. to constant weight to obtain the flame-retardant polymer containing an organic salt structure.

4. The environmentally friendly flame-retardant polyester yarn according to claim 3, characterized in that: The molar ratio of the bis(3-aminophenyl)(3,5-bis(trifluoromethyl)phenyl)phosphine oxide, 3,7-diamino-5-phenylphenazine chloride, 3,5-isoxazoledicarboxylic acid, catalyst and high boiling point solvent is 0.8:0.2:1:(0.8-1.2):(6-10).

5. The environmentally friendly flame-retardant polyester yarn according to claim 3, characterized in that: The catalyst is at least one of thiophosphonate, phosphorous acid, and thiophosphoramide; the high boiling point solvent is dimethyl sulfoxide; and the inert gas is any one of nitrogen, helium, neon, and argon.

6. The environmentally friendly flame-retardant polyester yarn according to claim 1, characterized in that: The antioxidant is at least one of antioxidant 1010 and antioxidant 168; the lubricant is at least one of pentaerythritol stearate and ethylene bisstearamide.

7. A method for preparing the environmentally friendly flame-retardant polyester yarn according to any one of claims 1 to 6, characterized in that: The steps include: Step S1, mixing polyester slices, flame retardant polymers containing organic salt structures, antioxidants and lubricants uniformly to obtain spinning raw materials, drying and adding them into a composite spinning machine for spinning, and then stretching to obtain primary polyester fibers; Step S2, soaking the nascent polyester fiber in an aqueous solution containing sodium benzotriazole and quinoline yellow for 1-2 hours for ion exchange treatment, then washing with deionized water for 3-6 times, and drying at room temperature to obtain polyester fiber; Step S3, drying the polyester fiber in a drying device; and then making the dried polyester fiber into the polyester yarn in a yarn blending machine.

8. The method for preparing the environmentally friendly flame-retardant polyester yarn according to claim 7, characterized in that: The spinning temperature of the spinning in step S1 is 265-295° C., and the spinning winding speed is 1000-2500 m / min.

9. The method for preparing the environmentally friendly flame-retardant polyester yarn according to claim 7, characterized in that: The drawing processing parameters in step S1 are a drawing multiple of 2-4 times, a hot plate temperature of 60-90°C, and a hot plate temperature of 110-210°C.

10. The method for preparing the environmentally friendly flame-retardant polyester yarn according to claim 7, characterized in that: The mass ratio of sodium benzotriazole to water in the aqueous solution containing sodium benzotriazole and quinoline yellow in step S2 is (5-8):100.

Citation Information

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