KR101865394B1 - A manufacturing method of polyester yarn - Google Patents
A manufacturing method of polyester yarn Download PDFInfo
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- KR101865394B1 KR101865394B1 KR1020150191444A KR20150191444A KR101865394B1 KR 101865394 B1 KR101865394 B1 KR 101865394B1 KR 1020150191444 A KR1020150191444 A KR 1020150191444A KR 20150191444 A KR20150191444 A KR 20150191444A KR 101865394 B1 KR101865394 B1 KR 101865394B1
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- flame retardant
- polyester
- master batch
- phosphorus
- resin
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D4/00—Spinnerette packs; Cleaning thereof
- D01D4/02—Spinnerettes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/06—Load-responsive characteristics
- D10B2401/063—Load-responsive characteristics high strength
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2505/00—Industrial
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2507/00—Sport; Military
Abstract
Mixing a master batch chip comprising a polyester base resin having an intrinsic viscosity (IV) of 1.0 dl / g or more and a flame retardant into a polyester resin and melt-spinning the mixture through a spinneret to form an undrawn yarn; Supplying and supplying a radial emulsion to the undrawn yarn; And a step of stretching and winding the non-drawn filament to which the emulsion is adhered.
Description
The present invention relates to a method for producing a polyester fiber, and more particularly, to a method for producing a polyester fiber capable of high-strength development and having excellent flame retardancy.
Recently, polyester fibers have excellent physical and chemical properties, and their use as industrial fibers has continued to expand. Especially, industrial polyester fiber is widely used as a material for use in the harsh industrial environments such as safety nets and protective nets at construction sites, ropes for large ships, hoses for automobiles, seamstrips, and safety belts, as well as various leisure products such as tents, hammocks, · It is being used in various fields ranging from sporting goods. In the above-mentioned various industrial and leisure environments, heat resistance characteristics that can be used at a predetermined temperature or higher are required, and in particular, a flame retardant performance is required to prevent flames from being transferred to a large fire in advance. Basically, the polyester fiber has heat resistance that maintains its shape even at about 200 DEG C, but since it has flammability and flammability to catch fire when toxic smoke is generated at the ignition temperature of about 500 DEG C or more, flame retardancy Are being attempted.
Three types of polymerization type, postflame type and master batch type can be cited as examples for producing environmentally friendly polyester flame retarded fibers. First, the polymerization type is a method of producing a flame-retardant polyester resin chip in which a phosphorus-containing flame retardant containing a carboxyl group is polycondensed with terephthalic acid or dimethyl terephthalate and ethylene glycol in a raw material polymerization step and then melt-spun. However, for industrial use, a high strength of 7.0 g / d or more is required. Therefore, it is necessary to conduct a process of passing the polymerized resin chip again through solid-state polymerization. In this case, the efficiency of the solid- There is a problem in that it is not suitable for manufacturing a substantially high strength industrial flame retardant polyester fiber.
The post flame retardant type is a method of treating a liquid post-flame retardant on the surface of the fiber that is melt-spun. In this case, since the flame retardant is applied to the surface of the fiber, the flame retardant durability is lowered, so that it is not suitable for industrial roads used in most harsh environments.
Finally, the masterbatch type is the most economical and efficient method among the three methods of adding the flame retardant masterbatch to the raw material during the spinning. In order to exhibit the flame retardant performance, a halogen flame retardant which is not environmentally friendly is used, or a high- It is difficult to produce environmentally friendly high-strength flame retardant fibers.
Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made to solve the above problems, and it is an object of the present invention to provide a polyester production process which is environmentally friendly and capable of exhibiting strength suitable for industrial and leisure sports applications, and having excellent flame retardant properties.
According to an aspect of the present invention, there is provided a method of producing a polyester fiber of the following embodiments.
In a first embodiment, a master batch chip comprising a polyester base resin having an intrinsic viscosity (IV) of 1.0 dl / g or more and a flame retardant is mixed with a polyester resin and melt spun through the spinneret to form an undrawn yarn step;
Supplying and supplying a radial emulsion to the undrawn yarn; And
And a step of stretching and winding the non-drawn filament with the emulsion attached thereto.
In a second embodiment, in the first embodiment, the polyester resin is at least one selected from the group consisting of a polyethylene terephthalate resin, a polytrimethylene terephthalate resin, and a polybutylene terephthalate resin. To a process for producing an ester fiber.
The third embodiment relates to a method for producing a polyester fiber, wherein the polyester resin has an intrinsic viscosity of 0.9 to 1.0 dl / g in the first embodiment or the second embodiment.
In a fourth embodiment, in any one of the first to third embodiments, the content of the master batch chip is 1 to 30 parts by weight based on 100 parts by weight of the polyester resin. And a method for producing the same.
A fifth embodiment of the present invention relates to a method for producing a polyester fiber, wherein the flame retardant contained in the master batch chip is a phosphorus flame retardant in any one of the first to fourth embodiments.
A sixth embodiment is, in the fifth embodiment, characterized in that, in the fifth embodiment, the phosphorus flame retardant is a phosphoric acid ester compound, a pyrophosphate flame retardant, a phosphonate flame retardant, a phosphinate flame retardant, a non-halogen condensate phosphorus flame retardant, And at least one selected from the group consisting of polyester fibers.
The seventh embodiment is the method according to the fifth or sixth embodiment, wherein the content of phosphorus in the flame retardant is 10,000 to 100,000 ppm with respect to 100% by weight of the master batch chip will be.
An eighth embodiment is, in any one of the first to seventh embodiments, characterized in that the content of phosphorus in the flame retardant is at least 2,000 ppm based on 100% by weight of the polyester fiber ≪ / RTI >
The ninth embodiment is directed to the method for producing a polyester fiber according to any one of the first to eighth embodiments, wherein the strength of the polyester fiber is 7.0 g / d or more.
The tenth embodiment is characterized in that, in any one of the first to ninth embodiments, the master batch chip contains at least one of an ultraviolet stabilizer, an antioxidant, an antistatic agent, an organic colorant and an inorganic colorant in addition to the flame retardant The present invention relates to a method for producing a polyester fiber.
According to one embodiment of the present invention, it is possible to provide a polyester fiber which is eco-friendly, can exhibit strength suitable for industrial and leisure sports applications, and has excellent flame retardant properties.
In addition, it is possible to freely adjust the phosphorus content required for shortening the production process and the product characteristics, and to flexibly apply the production process without producing any additional copolymerization and solid phase polymerization in the production of industrial polyester fibers requiring flame retardancy have.
1 is a schematic view of a polyester fiber manufacturing apparatus used in the production method of the present invention.
Hereinafter, the method for producing a polyester fiber of the present invention will be described in detail. Prior to this, terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms, and the inventor should appropriately interpret the concepts of the terms appropriately It should be interpreted in accordance with the meaning and concept consistent with the technical idea of the present invention based on the principle that it can be defined.
In order to produce polyester fibers which are required to have excellent flame retardancy in industry, it is very important not only to produce flame-retardant products themselves but also to produce high-quality products uniformly at the time of production and to solve economic problems due to use of expensive flame retardants. However, as described above, there are many problems such as a decrease in strength and environmental hazard when using a halogen flame retardant, and thus it is difficult to produce a polyester yarn having high strength and flame retardancy suitable for industrial use.
Accordingly, the present invention is a method devised to solve all of these problems, and it is a method of manufacturing an industrial polyester fiber that requires flame retardancy by a highly effective method without greatly changing existing manufacturing facilities.
A method for producing a polyester fiber according to one aspect of the present invention comprises mixing a master batch chip comprising a polyester base resin having an intrinsic viscosity of 1.0 or more and a flame retardant into a polyester resin and melt- ; Supplying and supplying a radial emulsion to the undrawn yarn; And stretching and winding the non-drawn filament to which the emulsion is adhered.
First, a master batch chip comprising a polyester base resin having an intrinsic viscosity (IV) of 1.0 dl / g or more and a flame retardant is mixed with a polyester resin and melt-spun through a spinneret to form an undrawn yarn.
The polyester base resin and the polyester resin may each independently use at least one selected from the group consisting of a polyethylene terephthalate resin, a polytrimethylene terephthalate resin, and a polybutylene terephthalate resin, but is not limited thereto . Preferably, a polyethylene terephthalate resin which is excellent in heat resistance, mechanical strength and molding processability and is economically advantageous is used.
According to one embodiment of the present invention, the polyester resin may be one prepared by condensation polymerization of at least one dicarboxylic acid compound and at least one glycol compound. Preferably, the dicarboxylic acid compound may be an aromatic, aliphatic or alicyclic dicarboxylic acid, and the glycol compound may be an aliphatic or alicyclic glycol. More preferably, the aromatic dicarboxylic acid is an aromatic dicarboxylic acid having 6 to 20 carbon atoms, and the aliphatic or alicyclic dicarboxylic acid is an aliphatic or alicyclic dicarboxylic acid having 3 to 20 carbon atoms, The group Glycol is an aliphatic or cycloaliphatic glycol having 2 to 20 carbon atoms.
More specifically, as the dicarboxylic acid compound, terephthalic acid, isophthalic acid, 1,4-cyclohexanedicarboxylic acid, 1,3-cyclohexanedicarboxylic acid, succinic acid, glutaric acid, adipic acid, (1,4-, 1,5-, 2,3-, 2,6- or 2,7-) naphthalene dicarboxylic acid, 4,4'-biphenyldicarboxylic acid, 4,4 ' - dibenzyldicarboxylic acid, and the like, but the present invention is not limited thereto. Preferably, terephthalic acid, isophthalic acid or a mixture thereof is used. Examples of the glycol compound include ethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, (1,2-, 1,3- or 1,4-) cyclohexanedimethanol, neopentyl glycol, 2,2,4,4-tetramethyl-1,3-cyclobutanediol and the like can be used, It is not. Preferably, ethylene glycol, cyclohexanedimethanol or a mixture thereof is used.
The polyester resin can be synthesized by using the dicarboxylic acid compound and the glycol compound as described above. The production of a polyester resin using a dicarboxylic acid compound and a glycol compound is usually carried out in two stages of an esterification reaction and a polycondensation reaction, and the production process thereof is already well known in the art.
The polyester base resin preferably has an intrinsic viscosity (IV) of 1.0 dl / g or more, preferably 1.0 to 2.0 dl / g, more preferably 1.0 to 2.0 dl / g, in order to minimize the viscosity drop due to thermal decomposition and shearing stress during the production process 1.0 to 1.4 dl / g is used.
The flame retardant may be a non-halogen flame retardant, but may preferably be a phosphorus flame retardant.
The phosphorus-based flame retardant is eco-friendly since it does not generate a halogen-based gas at the time of processing or molding and combustion of the resin composition, and can be used in combination with a nitrogen-based flame retardant described later to minimize the deterioration of the mechanical and thermal properties of the composition.
The phosphorus-based flame retardant usable in the present invention is preferably one selected from a phosphoric acid ester compound, a pyrophosphate-based flame retardant, a phosphonate-based flame retardant, a phosphinate-based flame retardant, a non-halogenated condensed phosphorus- Mixtures of two or more species may be used.
Examples of the phosphoric acid ester compound include, but are not limited to, a monomer compound having one aromatic group such as triphenyl phosphate (TPP), trixylenyl phosphate (TXP), or tricresyl phosphate (Tricresyl phosphate, TCP); A monomer compound having two or more aromatic groups such as resorcinyl diphenyl phosphate (RDP), phenyl diresorcinyl phosphate, cresyl diphenyl phosphate, xylylenyl Xylenyl diphenyl phosphate or phenyl di (isopropylphenyl) phosphate; And oligomers or polyphosphates having a dimer or more.
As the phosphonate-based flame retardant, a flame retardant copolymerized with a polycarbonate having a crosslinked polyphosphonate structure which is reactive by introducing phosphoric acid ester bond into the molecule is preferably used.
As the phosphinate-based flame retardant, metal-substituted monophosphinate or diphosphinate flame retardant may preferably be used alone or in combination.
The content of phosphorus in the flame retardant may be 10,000 to 100,000 ppm, preferably 40,000 to 80,000 ppm, more preferably 60,000 to 80,000 ppm with respect to 100 wt% of the master batch chip. When the content of phosphorus satisfies the above range, there is an advantage that the addition amount can be reduced at the time of inputting the master batch chip, and the flame retardancy can be effectively imparted without deteriorating mechanical properties such as heat distortion temperature and tensile strength.
The master batch chip may further contain at least one of an ultraviolet stabilizer, an antioxidant, an antistatic agent, an organic colorant and an inorganic colorant in addition to the flame retardant, depending on the required physical properties.
According to an embodiment of the present invention, in order to produce an industrial polyester fiber having a flame retardant performance superior to that of a conventional commercial product, it is preferable to use a polyester resin having a hole diameter of 0.4 mm or more, preferably 0.2 to 1.2 mm, more preferably 0.4 to 0.8 mm , A nozzle having 40 to 400 holes, preferably 144 to 192 holes can be assembled into a pack and applied as a spin-block.
The polyester resin may have an intrinsic viscosity (IV) of 0.9 to 1.0 dl / g to produce a high strength fiber.
The polyester resin having such an intrinsic viscosity can be easily produced by a known method such as a method of solid-phase polymerization of a conventional polyester chip having an intrinsic viscosity of about 0.6.
The content of the master batch chip may be 1 to 30 parts by weight, preferably 3 to 15 parts by weight, more preferably 5 to 10 parts by weight based on 100 parts by weight of the polyester resin. When the content of the master batch chip satisfies the above range, the flame retardancy can be effectively imparted without deteriorating the mechanical properties such as the heat distortion temperature and the tensile strength, the problem of lowering of workability in the injection and molding at the time of extrusion does not occur, And can be produced in fibrous form.
According to one embodiment of the present invention, the temperature of the melt spinning is, for example, 300 DEG C, preferably 290 to 310 DEG C, and the spinning temperature can be appropriately determined in consideration of the melt index of the polyester resin. The melt-spun fibers are cooled to form undrawn yarn.
The filament fineness (D.P.F., denier per filament) of the melt-spun non-drawn filament can be adjusted to 5 to 120 denier, preferably 30 to 60 denier.
At this time, the number of holes in the spinneret may be 40 to 400, preferably 144 to 192.
The size of the hole of the spinneret is 0.2 to 1.2 mm, more preferably 0.4 to 0.8 mm, and the depth of the spinneret hole is 0.8 to 4.8 mm, more preferably 1.6 to 3.2 mm.
Thereafter, the undrawn yarn discharged through the spinneret is subjected to a cooling process through a quenching zone, and the cooling temperature can be adjusted to 15 to 30 ° C, more preferably 20 to 25 ° C.
In addition, the wind speed during cooling can be adjusted to 1.0 to 2.0 m / sec, more preferably 0.8 to 1.5 m / sec.
Then, the spinning oil is supplied to the undrawn yarn and attached.
At this stage, the linear velocity and the spinning oil during running of the polyester undrawn yarn can be applied according to a conventional method.
According to one embodiment of the present invention, the polyester undrawn yarn is run at a linear velocity of 200 to 600 m / min, and a radial emulsion containing a lubricant having a viscosity of 90 to 1000 cps is supplied to the undrawn yarn, .
By controlling the running speed of the polyester undrawn yarn in the range of 200 to 600 m / min as described above, scattering of the emulsion can be suppressed. Further, when the viscosity of the lubricant contained in the emulsion is in the range of 90 to 1000 cps, the lubricant can be controlled at a low viscosity through the temperature control when mixed with the spinning emulsion, and is excellent in heat resistance. In the subsequent drawing process, It is possible to prevent scum from being generated on the surface of the roller when passing through the roller.
Examples of such a high viscosity lubricant include paraffin wax having 24 to 40 carbon atoms, silicon wax having a weight average molecular weight of 1,000 to 8,000, or a mixture thereof.
Specific examples of the paraffin wax include polymethylene-based, polyethylene-based, and polypropylene-based waxes, or a mixture thereof.
Such a lubricant has a high viscosity and therefore raises the viscosity of the whole mixed emulsion. If the viscosity of the mixed radial emulsion is too high, the uniform adhesion of the emulsion to the fiber may be deteriorated, so that the radial emulsion can be heated and fed to the fiber so that the viscosity remains below 10 cps.
The radial emulsion may contain 50 to 80% by weight of the high viscosity lubricant, and when the content of the high viscosity lubricant satisfies the above range, the uniform adhesion of the radial emulsion can be improved.
In addition to the high-viscosity lubricant, conventional emulsion additive components such as mineral oil, antistatic agent, surfactant and the like may be further added to the spinning emulsion, and known components imparting various properties to the polyester fiber such as rubber adhesion property and water repellency Of course, can be added.
The unstretched fiber to which the oil-repellent oil is adhered is fed to a stretching process according to a conventional production process of a polyester fiber and stretched. The OPU of the polyester fiber produced here may be 0.7 to 2.0%. If the OPU value of the fiber satisfies the above range, the abrasion resistance effect is enhanced and the problem of increased contamination due to high OPU in the drawing and winding process can be prevented.
Next, the unstretched yarn to which the emulsion is adhered is stretched.
The heat treatment conditions and the stretching ratio in the stretching process can be easily adjusted by those skilled in the art depending on the intrinsic viscosity of the raw material resin, the intended use and strength of the polyester fiber, and the like.
According to an embodiment of the present invention, in the previous step, the non-drawn yarn can be supplied to the drawn hot rollers controlled at a temperature of 80 to 250 DEG C at an initial feeding speed of 400 to 700 m / min by using a feeding roller. At this time, the stretching ratio can be stretched by about 4 to 7 times in accordance with the feeding roller speed.
Further, if necessary, the stretched polyester fiber may undergo additional relaxation treatment.
Then, the interlaced pressure used to wind up the drawn yarn and to engage the existing filaments in the winding step can be focused at a pressure of 5.0 to 9.0 bar, more preferably a pressure of 6.0 to 8.0 bar .
The single fiber fineness of the polyester fiber according to one embodiment of the present invention may be 4 to 10 denier, preferably 5 to 7 denier.
The strength of the polyester fiber according to an embodiment of the present invention may be 7.0 g / d or more, preferably 7.5 to 8.5 g / d, and the elongation may be 10 to 30%, preferably 15 to 25%.
The phosphorus content of the flame retardant may be 2,000 ppm or more, preferably 3,000 to 90,000 ppm, more preferably 3,000 to 7,000 ppm, based on 100% by weight of the polyester fiber according to an embodiment of the present invention. When the phosphorus content satisfies this range, the flame retardancy can be effectively imparted to the polyester fiber according to the embodiment of the present invention without deteriorating the mechanical properties such as the heat distortion temperature and the tensile strength.
Further, the polyester fiber according to the production method of the present invention can be applied to industrial materials, leisure and sports applications requiring sufficient strength and flame retardancy.
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail with reference to examples. However, the embodiments according to the present invention can be modified into various other forms, and the scope of the present invention should not be construed as being limited to the embodiments described below. Embodiments of the present invention are provided to more fully describe the present invention to those skilled in the art.
Example One
A polyester fiber was produced as follows using an apparatus for producing a polyester fiber according to an embodiment of the present invention shown in FIG.
First, a polyethylene terephthalate master batch chip having an intrinsic viscosity of 1.0, which contains 15,000 ppm of phosphorus, was mixed in a proportion of 20 parts by weight with respect to 100 parts by weight of a polyester resin having an intrinsic viscosity of 0.9 to 1.0 using a dosing machine (11) And the mixture was fed into an
Thereafter, the extrudate was cooled with quench air at 20 to 25 DEG C using a high-
Next, the untreated yarn is uniformly focused while the radial
At this time, the air pressure in the
As a result, finally, the single fiber fineness was 2.5 Polyethylene terephthalate fibers having a total fineness of 1,000 denier were produced.
Example 2
A polyethylene terephthalate fiber was prepared in the same manner as in Example 1, except that 10 parts by weight of a polyethylene terephthalate base resin master batch chip having an intrinsic viscosity of 1.0 and containing 60,000 ppm of phosphorus was used.
Comparative Example 1
(2-Carboxylethyl (phenyl) phosphinic acid) in a molar ratio of dimethyl terephthalate and ethylene glycol of 1: 1.5 to a stainless steel reactor equipped with a condenser and stirrer, The temperature was raised to 220 ° C to 230 ° C while heating and stirring, and the ester stirring reaction was carried out. After the ester stirring reaction, the temperature was gradually increased to make the final temperature 285 ° C, And the reaction was carried out for 120 minutes so that the flame retardant polyethylene terephthalate resin precursor having a phosphorus content of 6,500 ppm and an intrinsic viscosity of 0.70 was prepared. Thereafter, the flame retardant polyethylene terephthalate resin precursor was solidified in a solid state polymerizer at 220 DEG C for 40 hours to prepare a flame retardant polyethylene terephthalate resin having an intrinsic viscosity of 0.90.
The produced flame-retardant polyethylene terephthalate resin had a melt viscosity of about 3,000 poise at the same temperature and was about 1/2, so that the polyester fiber was prepared in the same manner as in Example 1 except that the spinning temperature was 290 ° C.
Comparative Example 2
A polyethylene terephthalate fiber was prepared in the same manner as in Example 2, except that a polyethylene terephthalate base resin having an intrinsic viscosity of 0.64 was used.
Property evaluation
1. Intrinsic viscosity (I.V.)
0.1 g of the sample was dissolved in a reagent (90 ° C.) mixed with phenol and 1,1,2,2-tetrachloroethanol 6: 4 (weight ratio) for 90 minutes, transferred to a Ubbelohde viscometer, Hold the solution in a thermostatic chamber for 10 minutes and use a viscometer and an aspirator to determine the number of drops of the solution. The number of drops of the solvent was determined in the same manner as described above, and then the intrinsic viscosity (I.V.) value was calculated.
2. Evaluation of flame retardancy (UL94-VTM)
The flame retardant performance evaluation method for thin plastic materials is as follows. After the sample is placed vertically, a burner is used. The amount of residual flue generated from the sample through two complexes per sample, the time of the residue, The evaluation is carried out three times in total, and VTM-0, VTM-1, VTM-2, and grade 4 are evaluated.
3. Evaluation of flame retardancy (KS F 8081)
The sample was placed on a slope of 45 degrees with a flame-retardant evaluation standard for a thin bubble, and a micro-burner was used to measure the degree of coagulation, residue, residual salt, and carbonization distance.
The test was carried out three times per sample, and when it satisfied the criterion of less than 3 seconds of residual flushing time, less than 5 seconds of staying time, and less than 20 cm of carbonization distance, it was judged as acceptable.
4. How to measure the strength of yarn
The yarn was allowed to stand for 24 hours in a standard temperature condition, i.e., a constant temperature and humidity room at a temperature of 25 DEG C and a relative humidity of 65%, and then measured by a tensile tester by the method of ASTM D-885.
The polyester fibers produced in Examples 1 and 2 and Comparative Examples 1 and 2 and the fabric obtained by weaving the polyester fibers in plain weave of the fabric density shown in Table 2 were each evaluated for physical properties by the aforementioned method, Table 1 shows the results.
(IV)
(Total Residual Flush Time Comparison)
Referring to Table 1, it can be seen that the polyester fibers of Examples 1 and 2 have excellent flame retardancy and high strength characteristics.
On the other hand, in Comparative Example 1, the polyphosphoric acid added during the copolymerization adversely affected the solid phase polymerization, so that sufficient solid phase polymerization was not performed for high strength development, resulting in low fiber strength. In the case of Comparative Example 2, although the flame retardancy was excellent, the strength of the final fiber was found to be low due to the effect of the master batch base resin having a low viscosity.
10: extruder, 11: injection machine, 20: spinneret, 30: nozzle, 40: cooling device
50: Radial emulsion applying device, 60: Gold detector roller, 70: Box
80: interlocking device 90: winder
Claims (10)
Supplying and supplying a radial emulsion to the undrawn yarn; And
And stretching and winding the undrawn yarn to which the radiation protective agent is attached.
Wherein the polyester resin is at least one selected from the group consisting of a polyethylene terephthalate resin, a polytrimethylene terephthalate resin, and a polybutylene terephthalate resin.
Wherein the content of the master batch chip is 1 to 30 parts by weight based on 100 parts by weight of the polyester resin.
Wherein the flame retardant contained in the master batch chip is a phosphorus flame retardant.
Wherein the phosphorus flame retardant is at least one member selected from the group consisting of a phosphoric acid ester compound, a pyrophosphate flame retardant, a phosphonate flame retardant, a phosphinate flame retardant, a non-halogenated condensed phosphorus flame retardant, ≪ / RTI >
Wherein the content of phosphorus in the flame retardant is 10,000 to 100,000 ppm based on 100% by weight of the master batch chip.
Wherein the content of phosphorus in the flame retarder is 2,000 ppm or more with respect to 100 wt% of the polyester fiber.
Wherein the polyester fiber has a strength of not less than 7.0 g / d.
Wherein the master batch chip further comprises at least one of an ultraviolet stabilizer, an antioxidant, an antistatic agent, an organic colorant and an inorganic colorant in addition to the flame retardant.
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KR102103533B1 (en) * | 2018-06-01 | 2020-04-22 | 김익 | Method for preparing polyester fibers for reinforcing concrete and concrete comprising polyester fibers |
KR102183240B1 (en) * | 2019-03-28 | 2020-11-26 | 주식회사 휴비스 | High Strength Flame Retardant Composite Yarn |
CN110373732A (en) * | 2019-07-09 | 2019-10-25 | 长乐佳纶纺织实业有限公司 | A kind of production technology of coloured flame-retardant dacron thread |
CN111926398B (en) * | 2020-06-22 | 2021-10-08 | 湖州市中跃化纤有限公司 | Technological method of super-elastic flame-retardant coarse denier porous PET-DTY |
KR102619704B1 (en) * | 2021-11-22 | 2023-12-28 | 도레이첨단소재 주식회사 | Heavy metal free-antimicrobial polyester draw textured yarn and Manufacturing method thereof |
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