CN103451761A - Phosphorus flame-retardant cationic dyeable polyester fiber and production method thereof - Google Patents

Phosphorus flame-retardant cationic dyeable polyester fiber and production method thereof Download PDF

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CN103451761A
CN103451761A CN201310356115XA CN201310356115A CN103451761A CN 103451761 A CN103451761 A CN 103451761A CN 201310356115X A CN201310356115X A CN 201310356115XA CN 201310356115 A CN201310356115 A CN 201310356115A CN 103451761 A CN103451761 A CN 103451761A
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polyester fiber
cationic dyeable
dyeable polyester
flame retardant
retardant
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徐醒我
关乐
赵满才
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Suzhou Longjie Special Fiber Co Ltd
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Suzhou Longjie Special Fiber Co Ltd
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Abstract

The invention discloses a production method of a phosphorus flame-retardant cationic dyeable polyester fiber. The production method is characterized by comprising the steps: in the copolymerization process of polyester, a phosphorus flame-retardant agent and isophthalic acid component containing metal sulfonate are added, wherein relative to the weight of the polyester fiber, the content of phosphorus atoms of the phosphorus flame-retardant agent is 500ppm-15000ppm, and the content of the isophthalic acid component containing the metal sulfonate is 0.5mol%-5.0mol%; then melt spinning is carried out on the formed flame-retardant cationic dyeable polyester at the spinning temperature of 260-295 DEG C.

Description

A kind of phosphorous flame-retardant cationic dyeable polyester fiber and production method thereof
Technical field
The present invention relates to a kind of flame retardant cationic dyeable polyester fiber and manufacture method thereof.
Background technology
It is high that polyester fiber (being terylene) has intensity, good springiness, and wrinkle resistance is strong, dimensionally stable, ABRASION RESISTANCE is good, stable chemical performance, quick-drying washable, the performances such as heat resistance and weather fastness are good, so leapt to as global output maximum most widely used fiber species since modern age.But because the limited oxygen index of common PET is 20~24, can under usual conditions, burn, and also can melting drip under burning or high temperature, thereby limit its application in aviation, public place of entertainment, family's decorations art work and some special industry occasion.
Fire-retardant polyester fibre mainly makes by following several method at present, and the first is processed with fire retardant on the surface of fiber; The second is to add fire retardant to carry out blending and modifying; The third is to use fire proofing to carry out copolyreaction.Although having superiority on manufacturing cost, first method has the not shortcoming of the poor durability such as wash resistant; Second method, owing to having added fire retardant, exists viscosity and color distortion, may cause the problems such as the bad and physical property reduction of spinnability; The third method is to manufacture flame retardant polyester by copolyreaction, and its durability of fire-retardant is good, good spinnability and have physical and mechanical properties preferably.
Aspect fire retardant, a lot of patents have all related to the fire retardant of halogen system.Although this based flame retardant, after interpolation, can play flame retardant effect preferably really, have quite serious shortcoming: the color variation of polymer, light fastness reduces, and produces toxic gas, major polluting atmosphere environment in combustion process.Phosphorus flame retardant has overcome some shortcomings of halogen flame, and not only flame retarding efficiency is high, and can effectively reduce the release of corrosion or toxic gas.
From the phosphorus flame retardant combination, divide, a kind of is directly with main chain, to be combined and to form main chain phosphorus to also have a kind of be to be combined formation side chain phosphorus with side chain with phosphorus atoms with phosphorus atoms, flame retardant effect be take main chain as excellent, but the add anti-dyeability and the anti-hydrolytic performance that make polyester of side chain phosphorus fire retardant are better than main chain phosphorus.At present the side chain phosphonium flame retardant is mainly by preparing phosphorous epoxy resin, P elements to be introduced, wherein with
Figure BDA0000367426810000011
10-oxidation-(9,10-2 hydrogen-9-oxygen-10-phosphorus) assorted luxuriant and rich with fragrance (DOPO) is excellent, because be firm ring phosphorus structure, is a fire retardant that character is pretty good.Because the hydrogen of P-H in the DOPO structure is an active atomic, DOPO directly can be imported to the main body of epoxy resin, relate to a kind of side chain phosphorus fire retardant in patent CN200410084108.X,
Figure BDA0000367426810000012
This fire retardant is to adopt DOPO and itaconic acid (ITA) or its derivative to carry out the meter Xie Er addition to synthesize, and still, due to the existence of the methylene that is connected with phosphorus atoms, makes side chain elongated, and phosphorus atoms and main chain are distant, and fire resistance is affected; Introducing with duration side chain phosphorus fire retardant makes the polyester macromolecule short texture, and structural regularity is influenced, makes its crystallization difficulty, melting point depression, shaping and the physical property of impact silk; And the synthetic cost of itaconic acid and derivative thereof is higher.
Because the PET molecular structure is regular, degree of crystallinity and the degree of orientation are higher in addition, without easily dying functional group, polarity is less, lack hydrophily, the gap that there is no suitably to hold dye molecule between the polyester long-chain molecule, so dye particles is difficult for entering fiber, its dyeability is poor, can use the kind of dyestuff few, can only adopt the methods such as DISPERSE DYES carrier dyeing, high-temp dyeing and pad-dry-cure dyeing, but the working condition harshness, production cost is high, and product colour is undesirable.
Summary of the invention
The purpose of this invention is to provide a kind of have good flame retardant effect and chromatic phosphorous flame-retardant cationic dyeable polyester fiber and production method thereof.
Technical solution of the present invention:
A kind of phosphorous flame-retardant cationic dyeable polyester fiber, the phosphorous flame-retardant composition and the sulfur-bearing copolyester section that contain Chemical formula 1 or Chemical formula 2 in main body, wherein with respect to polyester fiber weight, the phosphorus atoms content of phosphorus flame retardant is 500~15000ppm, with respect to sulfur-bearing copolyester section element sulphur content, is 0.05~1.50wt%.
Chemical formula 1
R1 in Chemical formula 1, R2 are the hydroxy alkylidenes of hydrogen atom or C1~C10;
Chemical formula 2:
Figure BDA0000367426810000022
R3 in Chemical formula 2 is the alkyl of C1~C6 or the aryl of C6~C9; R4 is the alkylidene of C1~C6; R5 and R6 are the hydroxy alkylidenes of hydrogen atom or C2~C4.
This fire retardant (Chemical formula 1) makes the P atom directly be connected with main chain, improved fire resistance, and can not affect the structural regularity of polyester macromolecule, physical property and the common PET of silk are suitable, and, under the condition of identical P atom content, the amount of required fire retardant still less.
The content of phosphorus flame retardant phosphorus atoms is preferably 2500~8000ppm.
In described sulfur-bearing copolyester section, the M-phthalic acid composition that described element sulphur comes from the M-phthalic acid compound containing metal sulfonate containing sulphonate-base of the formula that is shown below is the compound with following formula:
Figure BDA0000367426810000023
The open chain that R1, R2 are C1~C15 or cyclic alkyl, M is alkali metallic sodium, lithium or potassium.
The M-phthalic acid component content of containing metal sulfonate is preferably 1.0mol~3.0mol%.
Described phosphorous flame-retardant cationic dyeable polyester fiber, have following characteristic,
The filament number of (1) 0.5~15dtex;
(2) intensity of 1.8cN/dtex~4.5cN/dtex.
A kind of production method of phosphorous flame-retardant cationic dyeable polyester fiber, in the polyethylene terephthalate copolymer process, the M-phthalic acid composition that adds phosphorus flame retardant and containing metal sulfonate, wherein with respect to polyester fiber weight, the phosphorus atoms content of phosphorus flame retardant is 500~15000ppm, and the content of the M-phthalic acid composition of containing metal sulfonate is 0.5mol~5.0mol%, then by the flame retardant cationic dyeable polyester formed, carry out melt spinning, spinning temperature is 260~295 ℃.
The spun tow of melting can first be made pre-oriented yarn, then through false twisting hot-stretch processing, thereby make flame retardant cationic dyeable polyester fiber DTY false twist yarn.
The spun tow of melting also can spray by spinnerets, cooling after, with the speed of 800~4000m/min through the first hot-rolling, speed with 3000~6000m/min is batched after the second hot-rolling, thereby make flame retardant cationic dyeable polyester fiber FDY, extends silk.
Gained fiber of the present invention has good flame retardant effect and dyeability.
This modified polyester fiber, wherein the M-phthalic acid content containing sulphonate-base is 0.5~5.0mol%, wherein is preferably 1.0mol~3.0mol%.Adopt 5-sulfonic acid Metal Substrate-dimethyl isophthalate (SIPM) or with 5-sulfonic acid Metal Substrate-ethylene isophthalate (SIPE) containing the M-phthalic acid composition of metal organic sulfonate base.Wherein preferred SIPE, for the metal ingredient in SIPE, can be used the alkali metals such as sodium, potassium, lithium, but be most preferably sodium.The content of 5-sulfonic acid Metal Substrate-ethylene isophthalate has a significant impact melt spinning stability, if SIPE is greater than 5.0mol%, can produce tackify, gelation because of the charge effect of SIPE, and spinnability descends; If SIPE is less than 0.5mol%, copolymer has just lost the easy molten characteristic of alkali lye.Only have content in 0.5~5.0mol% scope, can realize that the molten characteristic of easy alkali of copolymer has the generation that can avoid tackify and gelation.
Content about P in phosphorus flame retardant in fiber is preferably 500~15000ppm, and preferably phosphorus atoms content is 2500~8000ppm, and when content is less than 500ppm, fire resistance is not obvious; And, when content is greater than 15000ppm, fire resistance is good, but manufacturing cost increases greatly, and the physical property of fiber significantly reduces.Only have when P content in 500~15000ppm scope, the fire resistance of fiber physical property and common PET excellent and fiber is suitable.
Analysis on dyeing properties
Dyeing prescription:
Dyestuff: cationic blue CB546, the percentage by weight 1% of dyestuff to fiber, bath raio: 1: 30.
Dyeing flow:
Figure BDA0000367426810000031
The mensuration of dye uptake:
Get dye liquor before above-mentioned dyeing flow, measure its absorbance A 0, then sample dye liquor after cloth dyeing, measure its absorbance A 1, according to (A0-A1)/A0 * 100%, be dye uptake.
Fire resistance is measured
Described fire-retardant evaluation method can adopt JIS standard A-4 method, D method
Burning A-4 method:
Sample size: cylinder is compiled thing or fabric (8.9*25.4cm)
Experiment condition: scorching high: 38mm
Ignition time: 3S
Estimate burning length and residual scorching time.
Burning D method (connecing scorching method)
Sample size: cylinder is compiled thing or fabric (the long 10cm of width, weight is 1g)
Evaluation criterion: connect the difficult combustion product that scorching number of times is greater than 3 times.
The fiber that this patent relates to connects scorching number of times and reaches more than 3 times.
Flame retardant cationic dyeable polyester fiber of the present invention has good spinning property, and physical property is close with general polyester fiber.The fibre number made is thin, powerful large, and has fire resistance and good stainability.The method production cost is low in addition, easy operating.
Below in conjunction with embodiment, the invention will be further described:
The specific embodiment:
Embodiment 1:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Addition is 6000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 290 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.88 times, heter temperature is at 170 ℃, intensity 3.6cN/dtex, elongation at break 26%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Embodiment 2:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000042
Addition is 6000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 285 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.86 times, heter temperature is at 170 ℃, intensity 3.6cN/dtex, elongation at break 27%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Embodiment 3:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000043
Addition is 6000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 290 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.88 times, heter temperature is at 170 ℃, intensity 3.8cN/dtex, elongation at break 24%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Embodiment 4:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000051
Addition is 500ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 290 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.87 times, heter temperature is at 170 ℃, intensity 3.8cN/dtex, elongation at break 27%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Embodiment 5:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000052
Addition is 3000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 290 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.88 times, heter temperature is at 170 ℃, intensity 3.8cN/dtex, elongation at break 26%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Embodiment 6:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000053
Addition is 8000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 290 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.88 times, heter temperature is at 170 ℃, intensity 3.6cN/dtex, elongation at break 25%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Embodiment 7:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000061
Addition is 15000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 280 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.88 times, heter temperature is at 160 ℃, intensity 3.3cN/dtex, elongation at break 24%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Embodiment 8:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Addition is 6000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 0.5mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 280 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.88 times, heter temperature is at 170 ℃, intensity 3.7cN/dtex, elongation at break 25%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Embodiment 9:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000063
Addition is 6000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 4.5mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 290 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.88 times, heter temperature is at 160 ℃, intensity 3.3cN/dtex, elongation at break 23%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Embodiment 10:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000071
Addition is 6000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, addition is 2mol%, make section and carry out melt spinning, 290 ℃ of spinning temperatures, the spun tow of melting by spinnerets spray, cooling after, with the speed of 1480m/min through the first hot-rolling, speed with 4700m/min is batched after the second hot-rolling, wherein the first heat roller temperature is 100 ℃, the second heat roller temperature is 140 ℃, thereby make flame retardant cationic dyeable polyester fiber FDY and extend silk, intensity 3.9cN/dtex, elongation at break 35%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Comparative example 1:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000072
Addition is 300ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 290 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.88 times, heter temperature is at 170 ℃, intensity 3.7cN/dtex, elongation at break 28%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Comparative example 2:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000073
Addition is 20000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 275 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.86 times, heter temperature is at 150 ℃, intensity 2.2cN/dtex, elongation at break 23%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Comparative example 3:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000081
Addition is 6000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 0.3mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 290 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.88 times, heter temperature is at 170 ℃, intensity 3.5cN/dtex, elongation at break 25%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Comparative example 4:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000082
Addition is 6000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 6.0mol%.Make section and carry out melt spinning, can not become silk.
Comparative example 5:
Take terephthalic acid (TPA) and ethylene glycol as polymerization single polymerization monomer, in polymerization process, add phosphorus flame retardant to reach the M-phthalic acid composition containing sulphonate-base, wherein the structure of phosphorus flame retardant is
Figure BDA0000367426810000083
Addition is 6000ppm.Wherein the M-phthalic acid composition containing the metal organic sulfonate base adopts 5-sodium sulfonate-ethylene isophthalate, and addition is 2.0mol%.Make section and carry out melt spinning, make fiber precursor, and further through reel stretching, network etc., obtain flame retardant cationic dyeable polyester filament, i.e. flame retardant cationic dyeable polyester fiber; 275 ℃ of spinning temperatures, spinning speed is that 2700m/min ,Hou road DTY multiplying power is 1.86 times, heter temperature is at 160 ℃, intensity 2.6cN/dtex, elongation at break 24%.The flame retardant cationic dyeable polyester fiber made is carried out to cylinder and compile processing, dyeing, estimate its dye-uptake; The flame retardant cationic dyeable polyester fiber made is carried out to fabric processing, estimate its anti-flammability.
Figure BDA0000367426810000091

Claims (8)

1. a phosphorous flame-retardant cationic dyeable polyester fiber, it is characterized in that: the phosphorous flame-retardant composition and the sulfur-bearing copolyester section that contain Chemical formula 1 or Chemical formula 2 in its main body, wherein with respect to polyester fiber weight, the phosphorus atoms content of phosphorus flame retardant is 500~15000ppm, with respect to sulfur-bearing copolyester section element sulphur content, is 0.05~1.50wt%.
Chemical formula 1
Figure FDA0000367426800000011
R1 in Chemical formula 1, R2 are the hydroxy alkylidenes of hydrogen atom or C1~C10;
Chemical formula 2:
R3 in Chemical formula 2 is the alkyl of C1~C6 or the aryl of C6~C9; R4 is the alkylidene of C1~C6; R5 and R6 are the hydroxy alkylidenes of hydrogen atom or C2~C4.
2. phosphorous flame-retardant cationic dyeable polyester fiber according to claim 1, it is characterized in that: with respect to polyester fiber weight, the content of phosphorus flame retardant phosphorus atoms is preferably 2500~8000ppm.
3. phosphorous flame-retardant cationic dyeable polyester fiber according to claim 1 is characterized in that: in the sulfur-bearing copolyester section, described element sulphur comes from the M-phthalic acid compound containing sulphonate-base of the formula that is shown below
Figure FDA0000367426800000013
The open chain that R1, R2 are C1~C15 or cyclic alkyl, M is alkali metallic sodium, lithium or potassium.
4. phosphorous flame-retardant cationic dyeable polyester fiber according to claim 3, it is characterized in that: with respect to polyester fiber weight, the M-phthalic acid component content of containing metal sulfonate is preferably 1.0mol~3.0mol%.
5. according to claim 1,2 or 3 described phosphorous flame-retardant cationic dyeable polyester fibers, it is characterized in that: fiber has following characteristic,
The filament number of (1) 0.5~15dtex;
(2) intensity of 1.8cN/dtex~4.5cN/dtex.
6. the production method of a phosphorous flame-retardant cationic dyeable polyester fiber claimed in claim 1, it is characterized in that: in the polyethylene terephthalate copolymer process, the M-phthalic acid composition that adds phosphorus flame retardant and containing metal sulfonate, wherein with respect to polyester fiber weight, the phosphorus atoms content of phosphorus flame retardant is 500~15000ppm, the content of the M-phthalic acid composition of containing metal sulfonate is 0.5mol~5.0mol%, then by the flame retardant cationic dyeable polyester formed, carry out melt spinning, spinning temperature is 260~295 ℃.
7. the production method of phosphorous flame-retardant cationic dyeable polyester fiber according to claim 6 is characterized in that: melt spinning is made the orientation silk, then, through false twisting hot-stretch processing, makes flame retardant cationic dyeable polyester fiber DTY false twist yarn.
8. the production method of phosphorous flame-retardant cationic dyeable polyester fiber according to claim 6, it is characterized in that: the spun tow of melting by spinnerets spray, cooling after, with the speed of 800~4000m/min through the first hot-rolling, speed with 3000~6000m/min is batched after the second hot-rolling, thereby make flame retardant cationic dyeable polyester fiber FDY, extends silk.
CN201310356115XA 2013-08-15 2013-08-15 Phosphorus flame-retardant cationic dyeable polyester fiber and production method thereof Pending CN103451761A (en)

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CN114000226A (en) * 2021-12-31 2022-02-01 江苏新视界先进功能纤维创新中心有限公司 Preparation method of cationic dyeable flame-retardant high-strength polyester fiber
CN115821418A (en) * 2022-10-18 2023-03-21 浙江恒逸石化研究院有限公司 Method for preparing high-sulfonate-content antibacterial flame-retardant cationic dye dyeable polyester fiber based on autocatalysis

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CN102061533A (en) * 2009-11-18 2011-05-18 东丽纤维研究所(中国)有限公司 Easy cation-dyeable polyester (ECDP) fibers and production method thereof
CN103122501A (en) * 2011-11-18 2013-05-29 东丽纤维研究所(中国)有限公司 Method for preparing dyeable polyester fibers with phosphorus-containing flame-retarding cations

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CN101851810A (en) * 2009-04-03 2010-10-06 东丽纤维研究所(中国)有限公司 Phosphorous flame-retardant cationic dyeable polyester fiber and production method thereof
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CN114000226A (en) * 2021-12-31 2022-02-01 江苏新视界先进功能纤维创新中心有限公司 Preparation method of cationic dyeable flame-retardant high-strength polyester fiber
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Application publication date: 20131218