CN111118651B - Preparation method of flame-retardant polyester fiber - Google Patents

Preparation method of flame-retardant polyester fiber Download PDF

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CN111118651B
CN111118651B CN202010087843.5A CN202010087843A CN111118651B CN 111118651 B CN111118651 B CN 111118651B CN 202010087843 A CN202010087843 A CN 202010087843A CN 111118651 B CN111118651 B CN 111118651B
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flame
polyester fiber
retardant polyester
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CN111118651A (en
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王倩倩
朱美芳
周家良
相恒学
俞森龙
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Donghua University
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/07Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments

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Abstract

The invention provides a preparation method of flame-retardant polyester fiber, which comprises the following steps: firstly, constructing metal oxide with ultra-small particle size, uniform and stable dispersion and capable of catalyzing polyester polycondensation reaction on a micron-sized template to generate a micro-nano material; secondly, introducing the micro-nano material into a polyester polymerization system, and introducing alkyl phosphinic acid metal salt to prepare flame-retardant resin: and finally, obtaining the flame-retardant polyester fiber by a melt spinning method, wherein the spinning speed is 800-4500 m/min. The micro-nano material realizes the dual functions of catalytic polycondensation and synergistic flame retardance, effectively improves the flame retardance of the polyester fiber, enlarges the application range of the polyester fiber, and is used for improving the production efficiency of the flame-retardant polyester fiber in industrial production.

Description

Preparation method of flame-retardant polyester fiber
Technical Field
The invention belongs to the technical field of preparation of flame-retardant polyester fibers, and particularly relates to a preparation method of a micro-nano structure material synergistic flame-retardant polyester fiber.
Background
Polyester fiber, commonly known as "dacron", is a synthetic fiber obtained by spinning polyester obtained by polycondensation of organic dibasic acid and dihydric alcohol, and belongs to a high molecular compound. The polyester fiber has good crease resistance and shape retention, and high strength and elastic recovery capability; therefore, polyester fiber is widely used in human life and industrial production due to its excellent properties of fastness, anti-wrinkle, easy-care, and non-hair-sticking, etc., and at a low price. However, the flame retardant capability of the polyester fiber is poor, and the limit oxygen index is only 20-22%, which greatly limits the application range of the polyester fiber.
At present, the problem of poor flame retardant property of polyester fiber is mainly that the flame retardant capability of the polyester fiber is improved by a flame retardant modification mode. Common flame retardant modifiers include halogen flame retardants, phosphorus flame retardants, inorganic flame retardants, and organic-inorganic hybrid flame retardants. The organic-inorganic hybrid flame retardant is a flame-retardant modified material with a wide application range at present, multiple flame retardance can be realized through the synergistic effect of organic components and inorganic components in the combustion process of the polyester fiber, however, the inorganic components of the currently adopted hybrid flame retardant are high in addition amount, poor in dispersion and low in efficiency, and the processing and forming of the flame-retardant polyester fiber are greatly limited due to the problems.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a preparation method of flame-retardant polyester fiber, so that inorganic flame-retardant components with high performance, easy dispersion and low addition are constructed on the polyester fiber, and the purposes of improving the flame-retardant capability of the polyester fiber and the production efficiency of the polyester fiber are achieved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of flame-retardant polyester fiber comprises the following steps of:
(1) constructing metal oxide on the micron-sized template to generate a micro-nano material;
(2) simultaneously introducing a micro-nano material and alkyl phosphinic acid metal salt into a polyester polymerization system to obtain flame-retardant resin;
(3) and spinning the flame-retardant resin to prepare the flame-retardant polyester fiber.
As a limitation of the present invention, the step (1) comprises the following steps performed in sequence:
s1, dispersing the micron-sized template in a polar solvent to prepare a solution A;
s2, adding a chelating agent into the solution A, and reacting for 3.5-5.0 h at 36-43 ℃ to obtain a solution B;
s3, adding germanium chloride or n-butyl titanate into the solution B, and reacting for 3.2-4.5 h at 53-65 ℃ to obtain a product C;
and S4, cleaning the product C with ethanol, then placing the product C in a muffle furnace under a nitrogen atmosphere, and reacting for 4.2-6.6 h at 380-450 ℃ to obtain a product D.
As a further limitation of the present invention, in the step (1):
the weight part ratio of the micron-sized template to the polar solvent is 1: 80-120 parts;
the weight part ratio of the micron-sized template to the chelating agent is 1: 0.09-0.2;
the weight part ratio of the micron-sized template to the germanium chloride or the n-butyl titanate is 1: 0.5-1.0.
As a further limitation of the invention, the micron-sized template is selected from any one of halloysite nanotubes, montmorillonite and zirconium phosphate, and the size of the micron-sized template is 200-700 nm.
As still further defined in the present invention, the polar solvent is deionized water or absolute ethanol; the chelating agent used for constructing the micro-nano material is phytic acid.
As another limitation of the present invention, the step (2) comprises the following steps performed in sequence:
s1', mixing the product D with terephthalic acid, ethylene glycol and alkyl phosphinic acid metal salt to obtain a mixture E;
s2', adding the mixture E into a polymerization reactor, and reacting for 2-3 h at 200-250 ℃;
and S3', carrying out reduced pressure polycondensation, and reacting for 2-3 h at 260-300 ℃ to obtain the composite flame-retardant resin.
As a further limitation of the present invention, in the step (2): the weight ratio of the product D to the p-dibenzoic acid, the glycol and the alkyl phosphinic acid metal salt is 0.5-2.5: 43-48: 43-46: 6-8.
As a further limitation of the invention, the metal alkyl phosphinate is zinc alkyl phosphinate or aluminum alkyl phosphinate.
As still further limitation of the present invention, in the step (3): and spinning the composite flame-retardant resin at 260-300 ℃ by adopting a melt spinning method to prepare the flame-retardant polyester fiber, wherein the spinning speed is 800-4500 m/min.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, a nanoscale metal oxide is constructed on the surface of a micron-sized material by utilizing a molecular chelation technology, the metal oxide has small particle size and uniform and stable dispersion, and can play a catalytic role in polyester polycondensation reaction, so that the problem of agglomeration of a nano material in the use process is solved, and the efficiency of the micro-nano hybrid material is effectively ensured.
(2) The micro-nano hybrid material plays a dual role in the preparation process of the flame-retardant polyester, and is used as a catalyst for polycondensation reaction, so that the nano material in the micro-nano hybrid material has good dispersibility and can play a better catalytic role; secondly, in the combustion process, the nanometer-scale component can catalyze the alkyl phosphinate to form small-scale ceramic microspheres to be flame-retardant with the alkyl phosphinate in a synergistic manner, and the micron-scale component plays a role in blocking and supporting the carbon layer, so that the strength of the carbon layer after combustion is improved, heat release and oxygen circulation are inhibited, and the flame-retardant capability of the polyester fiber is effectively improved.
In conclusion, the synthesis method disclosed by the invention is low in cost and remarkable in flame-retardant effect of the product, and is used for improving the production efficiency of the flame-retardant polyester fiber in industrial production.
Drawings
FIG. 1 is a graph of the heat release rate of PET and flame retardant polyester of example 1 of the present invention;
FIG. 2 is a graph of the total heat release curve for PET and flame retardant polyester of example 1 of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the description of the preferred embodiment is only for purposes of illustration and understanding, and is not intended to limit the invention.
Example 1 preparation method of flame retardant polyester fiber
The preparation method is carried out according to the following steps:
(1): constructing metal oxide on micron-sized template to prepare micro-nano material
S1, drying halloysite nanotubes with the particle size of 500nm, and fully dispersing the halloysite nanotubes in deionized water to prepare a solution A. Wherein the weight part ratio of the halloysite nanotube to the deionized water is 1: 100.
S2, adding phytic acid into the solution A, and reacting for 4 hours at 40 ℃ to obtain a solution B. Wherein the weight part ratio of the halloysite nanotube to the phytic acid is 1: 0.1.
S3, adding germanium chloride into the solution B, and reacting for 4 hours at 60 ℃ to obtain a product C. Wherein the weight part ratio of the halloysite nanotube to the germanium chloride is 1: 0.5.
S4, washing the product C with ethanol for three times, placing the product C in a muffle furnace under nitrogen atmosphere, and reacting for 6h at 400 ℃ to obtain a product D (germanium oxide @ halloysite nanotubes).
(2): simultaneously introducing micro-nano material and alkyl phosphinic acid metal salt into polyester polymerization system to prepare composite flame-retardant resin
S1', mixing the germanium oxide @ halloysite nanotube with terephthalic acid, ethylene glycol and diethyl aluminum hypophosphite according to the weight ratio of 0.5:46:45.5:8 to obtain a mixture E.
S2', adding the mixture E into a polymerization reactor, and reacting for 3h at 240 ℃.
S3', and then carrying out reduced pressure polycondensation and reacting for 2h at 275 ℃ to obtain the composite flame-retardant resin.
(3): composite flame-retardant resin spinning and preparation of flame-retardant polyester fiber
And (3) spinning the composite flame-retardant resin at 285 ℃ by adopting a melt spinning method, wherein the spinning speed is 3500m/min, so as to obtain the flame-retardant polyester fiber. The limit oxygen index of the flame-retardant polyester fiber is 32.6, and UL-94 reaches V0 grade.
Fig. 1 to fig. 2 comparatively illustrate that the flame-retardant polyester prepared by the present invention can effectively reduce the heat release rate and the total heat release amount in the PET combustion process, thereby reducing the generation of volatile combustible substances in the combustion process, and slowing down the propagation of flame, thereby improving the flame-retardant ability of the polyester fiber.
Examples 2 to 6A method for preparing flame retardant polyester fiber
The preparation methods in examples 2 to 6 are the same as the preparation steps in example 1, except that the parameters involved in the respective steps are different, as shown in table 1.
Figure DEST_PATH_IMAGE001
Figure 387509DEST_PATH_IMAGE002
The limited oxygen index of the flame-retardant polyester fiber prepared in example 2 is 33.5, and UL-94 reaches V0 grade.
The limited oxygen index of the flame-retardant polyester fiber prepared in example 3 is 34, and UL-94 reaches grade V0.
The limited oxygen index of the flame-retardant polyester fiber prepared in example 4 is 35, and UL-94 reaches grade V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 5 is 34.6, and UL-94 reaches grade V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 6 was 32, and UL-94 reached grade V0.
Example 7 preparation method of flame retardant polyester fiber
The preparation method is carried out according to the following steps:
(1): constructing metal oxide on micron-sized template to prepare micro-nano material
S1, drying halloysite nanotubes with the particle size of 300nm, and fully dispersing the halloysite nanotubes in absolute ethyl alcohol to obtain a solution A. Wherein the weight part ratio of the halloysite nanotube to the deionized water is 1: 100.
S2, adding phytic acid into the solution A, and reacting for 4 hours at 40 ℃ to obtain a solution B. Wherein the weight part ratio of the halloysite nanotube to the phytic acid is 1: 0.1.
S3, adding tetrabutyl titanate into the solution B, dropwise adding deionized water for one minute at the speed of 5 drops/second, and reacting for 4 hours at the temperature of 60 ℃ to obtain a product C. Wherein the weight part ratio of the halloysite nanotube to the n-butyl titanate is 1: 0.5.
S4, washing the product C with ethanol for three times, placing the product C in a muffle furnace under nitrogen atmosphere, and reacting for 4 hours at 400 ℃ to obtain a product D (titanium dioxide @ halloysite nanotubes).
(2): simultaneously introducing micro-nano material and alkyl phosphinic acid metal salt into polyester polymerization system to prepare composite flame-retardant resin
S1', mixing the titanium dioxide @ halloysite nanotubes with terephthalic acid, ethylene glycol and zinc diethylphosphinate according to the weight ratio of 1:46:45:8 to obtain a mixture E.
S2', adding the mixture E into a polymerization reactor, and reacting for 2.5h at 240 ℃.
S3', and then carrying out reduced pressure polycondensation and reacting at 275 ℃ for 2.5h to obtain the composite flame-retardant resin.
(3): composite flame-retardant resin spinning and preparation of flame-retardant polyester fiber
And (3) spinning the composite flame-retardant resin at 285 ℃ by adopting a melt spinning method, wherein the spinning speed is 3500m/min, so as to obtain the flame-retardant polyester fiber. The limit oxygen index of the flame-retardant polyester fiber is 34, and UL-94 reaches V0 grade.
EXAMPLES 8 to 12A method for preparing a flame-retardant polyester fiber
The preparation procedures in examples 8-12 were the same as those in example 7 except that the parameters involved in the respective procedures were different, as shown in Table 2.
Figure DEST_PATH_IMAGE003
Figure 25688DEST_PATH_IMAGE004
The limited oxygen index of the flame-retardant polyester fiber prepared in example 8 is 31.8, and UL-94 reaches grade V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 9 was 32, and UL-94 reached grade V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 10 was 34.9, and UL-94 reached grade V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 11 was 36, and UL-94 reached grade V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 12 was 33.8, and UL-94 reached grade V0.
Example 13 preparation of a flame retardant polyester fiber
The preparation method is carried out according to the following steps:
(1): constructing metal oxide on micron-sized template to prepare micro-nano material
S1, drying zirconium phosphate with the particle size of 700nm, and fully dispersing the zirconium phosphate in deionized water to obtain a solution A. Wherein the weight part ratio of the zirconium phosphate to the deionized water is 1: 100.
S2, adding phytic acid into the solution A, and reacting for 5 hours at 40 ℃ to obtain a solution B. Wherein the weight part ratio of the zirconium phosphate to the phytic acid is 1: 0.1.
S3, adding germanium chloride into the solution B, and reacting for 4 hours at 60 ℃ to obtain a product C. Wherein the weight part ratio of the zirconium phosphate to the germanium chloride is 1: 1.
S4, washing the product C with ethanol for three times, placing the product C in a muffle furnace under a nitrogen atmosphere, and reacting for 6h at 400 ℃ to obtain a product D (germanium oxide @ zirconium phosphate).
(2): simultaneously introducing micro-nano material and alkyl phosphinic acid metal salt into polyester polymerization system to prepare composite flame-retardant resin
S1', mixing germanium oxide @ zirconium phosphate with terephthalic acid, ethylene glycol and diethyl aluminum hypophosphite in a weight ratio of 0.5:46:45.5:8 to obtain a mixture E.
S2', adding the mixture E into a polymerization reactor, and reacting for 3h at 240 ℃.
S3', and then carrying out reduced pressure polycondensation and reacting for 2h at 275 ℃ to obtain the composite flame-retardant resin.
(3): composite flame-retardant resin spinning and preparation of flame-retardant polyester fiber
And (3) spinning the composite flame-retardant resin at 285 ℃ by adopting a melt spinning method, wherein the spinning speed is 4000m/min, so as to obtain the flame-retardant polyester fiber. The limit oxygen index of the flame-retardant polyester fiber is 33, and UL-94 reaches V0 grade.
EXAMPLES 14 to 18A method for preparing a flame retardant polyester fiber
The preparation procedures in examples 14 to 18 were the same as those in example 13 except that the parameters involved in the respective procedures were different, as shown in Table 3.
Figure DEST_PATH_IMAGE005
Figure 398900DEST_PATH_IMAGE006
The limited oxygen index of the flame retardant polyester fiber prepared in example 14 was 35, and UL-94 reached grade V0.
The flame retardant polyester fiber prepared in example 15 had a limiting oxygen index of 34.5 and a UL-94 rating of V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 16 was 33 and UL-94 reached grade V0.
The flame retardant polyester fiber prepared in example 17 had a limiting oxygen index of 32.9 and a UL-94 rating of V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 18 was 34, and UL-94 reached grade V0.
Example 19A method for preparing a flame retardant polyester fiber
The preparation method is carried out according to the following steps:
(1): constructing metal oxide on micron-sized template to prepare micro-nano material
S1, drying montmorillonite with the particle size of 500nm, and fully dispersing in absolute ethyl alcohol to prepare solution A. Wherein the weight portion ratio of the montmorillonite to the absolute ethyl alcohol is 1: 100.
S2, adding phytic acid into the solution A, and reacting for 4 hours at 40 ℃ to obtain a solution B. Wherein the weight portion ratio of the montmorillonite to the phytic acid is 1: 0.1.
S3, adding tetrabutyl titanate into the solution B, dropwise adding deionized water for one minute at the speed of 5 drops/second, and reacting for 4 hours at the temperature of 60 ℃ to obtain a product C. Wherein the weight part ratio of the montmorillonite to the n-butyl titanate is 1: 1.
S4, washing the product C with ethanol for three times, placing the product C in a muffle furnace under nitrogen atmosphere, and reacting for 6h at 600 ℃ to obtain a product D (titanium dioxide @ montmorillonite).
(2): simultaneously introducing micro-nano material and alkyl phosphinic acid metal salt into polyester polymerization system to prepare composite flame-retardant resin
S1', mixing titanium dioxide @ montmorillonite with terephthalic acid, ethylene glycol and diethyl aluminum hypophosphite according to the weight ratio of 2.5:45:44.5:8 to obtain a mixture E.
S2', adding the mixture E into a polymerization reactor, and reacting for 3h at 240 ℃.
S3', and then carrying out reduced pressure polycondensation and reacting for 2h at 275 ℃ to obtain the composite flame-retardant resin.
(3): composite flame-retardant resin spinning and preparation of flame-retardant polyester fiber
And (3) spinning the composite flame-retardant resin at 285 ℃ by adopting a melt spinning method, wherein the spinning speed is 3200m/min, so as to obtain the flame-retardant polyester fiber. The limit oxygen index of the flame-retardant polyester fiber is 35, and UL-94 reaches V0 grade.
EXAMPLES 20 to 24A method for preparing a flame-retardant polyester fiber
The preparation procedures in examples 20 to 24 were the same as those in example 19 except that the parameters involved in the respective procedures were different, as shown in Table 4.
Figure DEST_PATH_IMAGE007
Figure 512219DEST_PATH_IMAGE008
The limited oxygen index of the flame retardant polyester fiber prepared in example 20 was 33, and UL-94 reached grade V0.
The flame retardant polyester fiber prepared in example 21 had a limiting oxygen index of 32.4 and a UL-94 rating of V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 22 was 35, and UL-94 reached grade V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 23 was 36 and UL-94 reached grade V0.
The limited oxygen index of the flame retardant polyester fiber prepared in example 24 was 34.2 and UL-94 reached grade V0.
Although the present invention has been described in detail with reference to the above embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described above, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A preparation method of flame-retardant polyester fiber is characterized by comprising the following steps: comprises the following steps which are carried out in sequence:
(1) constructing metal oxide on the micron-sized template by utilizing a molecular chelation technology to generate a micro-nano material;
(2) simultaneously introducing a micro-nano material and alkyl phosphinic acid metal salt into a polyester polymerization system to obtain flame-retardant resin;
(3) and spinning the flame-retardant resin to prepare the flame-retardant polyester fiber.
2. The method for preparing flame retardant polyester fiber according to claim 1, wherein: the step (1) comprises the following steps which are carried out in sequence:
s1, dispersing the micron-sized template in a polar solvent to prepare a solution A;
s2, adding a chelating agent into the solution A, and reacting for 3.5-5.0 h at 36-43 ℃ to obtain a solution B;
s3, adding germanium chloride or n-butyl titanate into the solution B, and reacting for 3.2-4.5 h at 53-65 ℃ to obtain a product C;
and S4, cleaning the product C with ethanol, then placing the product C in a muffle furnace under a nitrogen atmosphere, and reacting for 4.2-6.6 h at 380-450 ℃ to obtain a product D.
3. The method for preparing flame retardant polyester fiber according to claim 2, wherein: in the step (1):
the weight part ratio of the micron-sized template to the polar solvent is 1: 80-120 parts;
the weight part ratio of the micron-sized template to the chelating agent is 1: 0.09-0.2;
the weight part ratio of the micron-sized template to the germanium chloride or the n-butyl titanate is 1:0.5 to 1.0.
4. The method for preparing a flame retardant polyester fiber according to claim 2 or 3, wherein: the micron-sized template is selected from any one of halloysite nanotubes, montmorillonite and zirconium phosphate, and the size of the micron-sized template is 200-700 nm.
5. The method for preparing flame retardant polyester fiber according to claim 4, wherein: the polar solvent is deionized water or absolute ethyl alcohol; the chelating agent used for constructing the micro-nano material is phytic acid.
6. The method for preparing a flame retardant polyester fiber according to any one of claims 1 to 3 and 5, wherein: the step (2) comprises the following steps which are carried out in sequence:
s1', mixing the product D with terephthalic acid, ethylene glycol and alkyl phosphinic acid metal salt to obtain a mixture E;
s2', adding the mixture E into a polymerization reactor, and reacting for 2-3 h at 200-250 ℃;
and S3', carrying out reduced pressure polycondensation, and reacting for 2-3 h at 260-300 ℃ to obtain the composite flame-retardant resin.
7. The method for preparing flame retardant polyester fiber according to claim 6, wherein: in the step (2): the weight ratio of the product D to the p-dibenzoic acid, the glycol and the alkyl phosphinic acid metal salt is 0.5-2.5: 43-48: 43-46: 6-8.
8. The method for preparing flame retardant polyester fiber according to claim 6, wherein: the metal alkyl phosphinate is zinc alkyl phosphinate or aluminum alkyl phosphinate.
9. The method for preparing a flame retardant polyester fiber according to claim 7 or 8, wherein: in the step (3): and spinning the composite flame-retardant resin at 260-300 ℃ by adopting a melt spinning method to prepare the flame-retardant polyester fiber, wherein the spinning speed is 800-4500 m/min.
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