CN110644073B - Preparation method of polyester-nylon parallel composite elastic fiber - Google Patents
Preparation method of polyester-nylon parallel composite elastic fiber Download PDFInfo
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- CN110644073B CN110644073B CN201910850269.1A CN201910850269A CN110644073B CN 110644073 B CN110644073 B CN 110644073B CN 201910850269 A CN201910850269 A CN 201910850269A CN 110644073 B CN110644073 B CN 110644073B
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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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
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- 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
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
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- 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
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
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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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/32—Side-by-side structure; Spinnerette packs therefor
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- 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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- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
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Abstract
The invention relates to the field of chemical fibers and discloses a preparation method of a polyester-nylon parallel composite elastic fiber. Compared with the existing polyester-nylon composite fiber, the polyester-nylon composite fiber has better elasticity, the product has higher added value, and the problem of parallel polyester-nylon composite fiber splitting is solved.
Description
Technical Field
The invention relates to the field of chemical fibers, in particular to a preparation method of a polyester-nylon parallel composite elastic fiber.
Background
The elastic fiber is stretched to 2 times of the original length at room temperature, and can finally return to the original length after the tensile force is released. Elastic fibers can be divided into two main categories from the elastic mechanism, one is intrinsic elastic fibers, and the fibers are made of high polymers with soft segments and hard segments linked together, such as Polyurethane (PU) fibers and polytrimethylene terephthalate (PTT) fibers; another class is the shape-derived elastic fibers, including the post-processed and inherently crimp-structured fibers, also known as self-crimping fibers, such as PTT/PET (T400) fibers, PBT/PET fibers. Unlike the tight binding provided by PU fibers, the elasticity provided by such fibers provides a comfortable, snug feel.
Polyester (PET) is the most widely used synthetic fiber variety with the largest world output, and accounts for more than 60% of the world synthetic fiber output. The terylene has the advantages of high strength, good heat resistance, stiffness, uneasiness, difficult deformation, elasticity and the like, but is easy to pill, difficult to dye, poor in air permeability and poorer in moisture absorption. At present, terylene is widely used for clothing, bedding and the like. Chinlon (PA6) is the third largest chemical fiber of synthetic fiber and plays a significant role. The nylon has high strength and high abrasion, is light and thin in texture, is easy to dye, is soft in hand feeling, but has poor heat resistance and is easy to deform. The knitted fabric is mainly used for knitted socks, cords, high-grade fabrics and the like. As two varieties of synthetic fibers with larger yield and mature process, the self-crimping elastic fiber is prepared by adopting an eccentric sheath-core composite spinning process and the superfine fiber is prepared by adopting a split or island composite spinning process at present. At present, because the compatibility of the two components is poor, parallel compounding can not be realized all the time, and the two components are split to cause spinning failure. The elasticity of the eccentric sheath-core polyester-polyamide composite fiber is not as good as that of parallel fibers, and the eccentric sheath-core polyester-polyamide composite fiber is difficult to be compared with high-low viscosity PET parallel composite and the like.
The compatibility problem of terylene and chinlon is firstly solved when the parallel polyester-chinlon composite fiber is prepared, and two methods are common at present. Firstly, the terylene or the chinlon is modified to obtain better compatibility. And secondly, a specially designed spinneret plate is selected for spinning preparation. Application number CN201811103894.1 discloses a preparation method of polyester-nylon composite elastic fiber, wherein a third monomer is added in a polyester synthesis process to prepare a modified polyester slice, after the modified polyester and nylon are melt blended, the compatibility of polyester and nylon is improved, the cross section of the fiber obtained after composite spinning with nylon is in a dumbbell-shaped parallel structure, and the fiber has good curling elasticity. Meanwhile, due to the existence of the polyester and nylon components, the fiber can show good dyeing property and elastic effect. The application number CN201720443234.2 also discloses a parallel composite fiber and a preparation method thereof, the two-component parallel composite fiber is characterized in that in the cross section, the shapes of two components which are parallel are respectively fan-shaped ring and circular or elliptical, and the fan-shaped ring is externally connected with the circular or elliptical. However, the polyamide-polyester composite yarn prepared by the method disclosed by the patent aims to improve the moisture absorption of the fiber, and the fiber does not have excellent elasticity. In addition, the existing polyamide-polyester composite fiber has single functionality and low added value of products, and a new functional polyamide-polyester composite fiber needs to be developed.
Disclosure of Invention
The invention provides a preparation method of a polyester-polyamide parallel composite elastic fiber, aiming at the problems of poor compatibility of terylene and chinlon, easy fiber opening of parallel composite fiber and the like. The cross section of the polyester-nylon parallel composite elastic fiber is dumbbell-shaped, the surface of one side of the polyester component is coated with the nylon 6 layer and then is parallel compounded with the nylon 6 component, so that the PA6 and PET are not easy to split, the skin layer of the PA6 enables the fiber to have the characteristics of good dyeing property, good wear resistance, pilling resistance and strong moisture absorption capacity, and the core layer of the polyester enables the fiber to have the advantages of high modulus and good elasticity. In addition, the invention endows the fiber with more functionality by selecting the modified PET slices.
The specific technical scheme of the invention is as follows: a preparation method of polyester-nylon parallel composite elastic fibers comprises the following steps: 1) and respectively drying the PET slices and the nylon 6 slices, and then melting by a screw extruder to obtain a PET spinning melt and a nylon 6 spinning melt.
2) The two spinning melts respectively enter the two-component composite spinning assembly through respective corresponding pipelines to be spun, and the two spinning melts are sprayed out from the sheath-core composite spinneret to form filaments.
3) Cooling, oiling, stretching, shaping and winding the strand silk to obtain the polyester-nylon parallel composite elastic fiber; the two components in the polyester-nylon parallel composite elastic fiber are combined in parallel, and the cross section of the polyester-nylon parallel composite elastic fiber is dumbbell-shaped; and the surface of the terylene component is coated with a nylon 6 layer.
The sheath-core composite spinneret plate comprises a spinneret plate, and a circle of spinneret holes are formed in the spinneret plate; each spinneret orifice consists of a dumbbell-shaped nylon 6 spinneret orifice and a terylene spinneret orifice arranged at the center of one side of the nylon 6 spinneret orifice.
The PET chips and the nylon 6 chips are used as two components, and then the specially designed sheath-core composite spinneret plate is adopted, so that the polyester-nylon parallel composite elastic fiber is prepared. The cross section of the polyester-nylon parallel composite elastic fiber is dumbbell-shaped, the surface of one side of the polyester component is coated with the nylon 6 layer and then is parallel compounded with the nylon 6 component, so that the PA6 and PET are not easy to split, the skin layer of the PA6 enables the fiber to have the characteristics of good dyeing property, good wear resistance, pilling resistance and strong moisture absorption capacity, and the core layer of the polyester enables the fiber to have the advantages of high modulus and good elasticity.
Preferably, the number of the spinneret holes of the sheath-core composite spinneret plate is 24-36.
Preferably, the intrinsic viscosity of the PET slices is 0.65 +/-0.2 dL/g, the melting point is 240-265 ℃, and the water content of the dry slices is less than 50 ppm.
Preferably, the relative viscosity of the nylon 6 slice is 2.47 +/-0.2, the melting point is 215-225 ℃, and the water content of the dry slice is less than 100 ppm.
Preferably, the mass ratio of the PET slices to the PA6 slices is 25:75-45: 55.
Preferably, in the step 1), the screw temperature of the screw extruder is 260-285 ℃.
Preferably, in the step 2), the temperature of a spinning box body of the two-component composite spinning assembly is 260-285 ℃; the temperature of a first hot roller is 75-95 ℃ and the temperature of a second hot roller is 130-150 ℃ during stretching and shaping; the stretching ratio is 3.0 to 4.0.
Preferably, the PET slices are normal PET slices or modified PET slices. In order to further provide the additional value of the polyester-nylon parallel composite elastic fiber and enable the polyester-nylon parallel composite elastic fiber to have functionality, the invention also provides a modified PET slice, and the preparation method comprises the following steps:
a) adding terephthalic acid, ethylene glycol, a catalyst, an ethylene glycol solution of phosphorus flame retardant ester and an ethylene glycol solution of maleic anhydride ester into a reaction vessel, and pulping.
b) Introducing nitrogen into the reaction vessel to remove air, then filling nitrogen, adding initial pressure to 0.08-0.12Mpa, heating to 235-; after esterification, adding ethylene glycol suspension containing vinyl nano silicon spheres into a reaction container, stirring for 30-45 min, carrying out pre-polycondensation reaction at 260-270 ℃ under vacuum of-0.09-0.1 Mpa for 0.5-1 h, then carrying out polycondensation at 273-278 ℃ under high vacuum of less than 70pa for 2-3 h, after the reaction is finished, extruding melt by using nitrogen, cooling by water, and carrying out grain cutting to obtain the modified PET slice.
The modified PET chips prepared by the method have excellent flame retardance and anti-dripping property. One way to make the fibers flame retardant is to add flame retardants. In actual use, although the product of the most effective polyester phosphorus flame retardant CEPPA in the existing market has a higher oxygen index, the melt drip promoting flame retardant principle of the product causes a large amount of melt drip phenomenon during combustion of flame retardant polyester, so that people can be scalded and secondary burn can be caused. In fact, most phosphorus flame retardants realize flame retardance by taking away heat through molten drops, so that the problem of mutual contradiction between flame retardance and molten drop resistance exists, and the research on flame-retardant and molten drop-resistant polyester becomes a difficult problem. Some of the research results disclosed so far are that some anti-dropping agents, such as polytetrafluoroethylene and its derivatives, etc., are used, or inorganic fillers, such as metal hydroxides, glass fibers, etc., are added. The addition of these materials, while effective, has greatly limited the use of polyesters and, in addition, is not desirable because of the tendency of these inorganic fillers to clog the spinneret during high speed melt spinning production, which is particularly difficult to use in fibers.
Aiming at the problems of common flame retardant property and obvious molten drop phenomenon of the conventional flame retardant polyester, the invention provides a modified PET. The PET of the invention is compounded with vinyl nano silicon spheres, phosphorus flame retardant ester and maleic anhydride ester. The maleic anhydride esterified monomer can be crosslinked by taking the vinyl nano silicon spheres as a crosslinking agent under the action of high temperature during combustion, so that the original linear high polymer is converted into a body-shaped high polymer which is more combustible to be burnt into carbon, and part of the vinyl nano silicon spheres can be crosslinked mutually to form a reticular silane network, so that the effects of hindering heat conduction and limiting polymer melting and dropping are achieved, and the excellent flame-retardant and anti-dripping effect is reflected by matching with the flame-retardant effect of a phosphorus flame retardant.
Because the structural unit of the modified PET provided by the invention is provided with the high-temperature self-crosslinking structure, the high-temperature self-crosslinking structure is stable at the temperature of polyester synthesis and processing, and the synthesis and processing of the polyester cannot be influenced by crosslinking. But before it reaches the pyrolysis temperature in the burning process of being heated, can take place quick chemical crosslinking or radiation crosslinking under the high temperature radiation, form the polymer crosslinked network to can interconnect between the silicon ball, form inorganic coating, improve the fuse-element viscosity of copolyester under the high temperature rapidly, promote the copolyester to become charcoal under the high temperature, form the barrier layer, hinder the heat further diffusion, thereby obtain excellent fire-retardant and anti-molten drop effect.
Preferably, the catalyst comprises at least one of ethylene glycol antimony, antimony trioxide, a titanium-silicon composite catalyst, and a titanate.
Preferably, the specification of the polyester-nylon parallel composite elastic fiber is 100 dtex/36-48 f.
Compared with the prior art, the invention has the beneficial effects that:
the PET and PA6 with excellent performance are selected as two components of the polyester-nylon parallel composite elastic fiber, and the obtained polyester-nylon parallel composite elastic fiber has the advantages of light weight, wear resistance, fatigue resistance, high strength, easiness in dyeing, moisture absorption and the like of nylon, and also has the advantages of high elasticity, high elastic resilience, high oil absorption, high impact resistance and the like of polyester. And after the fiber is subjected to heat treatment, the high-elasticity self-curling effect can be generated due to the asymmetrical structure of the cross section and the shrinkage difference of the two components. Can be compared with other polyester parallel composite fibers to create high value-added fibers.
The special sheath-core parallel spinneret plate effectively solves the problem of compatibility of the polyester-nylon composite fiber, and the PA6 is coated with PET through the sheath-core structure, so that the problem of fiber splitting is avoided.
(3) The invention can select modified PET slices with high-temperature self-crosslinking function, and the polyester is compounded with vinyl nano silicon spheres, phosphorus flame retardant ester and maleic anhydride ester. The maleic anhydride esterified monomer can be crosslinked by taking the vinyl nano silicon spheres as a crosslinking agent under the action of high temperature during combustion, so that the original linear high polymer is converted into a body-shaped high polymer which is more combustible to be burnt into carbon, and part of the vinyl nano silicon spheres can be crosslinked mutually to form a reticular silane network, so that the effects of hindering heat conduction and limiting polymer melting and dropping are achieved, and the excellent flame-retardant and anti-dripping effect is reflected by matching with the flame-retardant effect of a phosphorus flame retardant.
Drawings
Fig. 1 is a cross-sectional view of a sheath-core composite spinneret of the present invention;
FIG. 2 is a schematic cross-sectional view of the polyester-nylon parallel composite elastic fiber of the invention.
The reference signs are: a spinneret plate 1, a polyester spinneret orifice 2, a nylon spinneret orifice 3, a polyester component A and a nylon 6 component B.
Detailed Description
The present invention will be further described with reference to the following examples.
The preparation method of the polyester-nylon parallel composite elastic fiber (the fiber specification is 100 dtex/36-48 f) in the general embodiment comprises the following steps:
1) respectively drying the PET slices and the nylon 6 slices according to the mass ratio of 25:75-45:55, and then melting the PET slices and the nylon 6 slices by a screw extruder (260-285 ℃) to obtain a PET spinning melt and a nylon 6 spinning melt.
2) The two spinning melts respectively enter the two-component composite spinning assembly through respective corresponding pipelines to be spun (the temperature of a spinning box body is 260-285 ℃), and the two spinning melts are sprayed out from a sheath-core composite spinneret to form filaments.
3) Cooling, oiling and stretching and shaping the strand silk (the temperature of a first hot roller is 75-95 ℃, and the temperature of a second hot roller is 130-150 ℃; stretching times of 3.0-4.0) and winding to obtain the polyester-nylon parallel composite elastic fiber; two components (a polyester component A and a nylon 6 component B) in the polyester-nylon parallel composite elastic fiber are combined in parallel, and the cross section of the polyester-nylon parallel composite elastic fiber is dumbbell-shaped; and the surface of the polyester component is coated with a nylon 6 layer (as shown in fig. 2).
As shown in fig. 1, the sheath-core composite spinneret plate comprises a spinneret plate 1, wherein a circle of (24-36 holes) spinneret holes are formed in the spinneret plate; each spinneret orifice consists of a dumbbell-shaped nylon 6 spinneret orifice 2 and a terylene spinneret orifice 1 arranged at the center of one side of the nylon 6 spinneret orifice.
Wherein the intrinsic viscosity of the PET slices is 0.65 +/-0.2 dL/g, the melting point is 240-265 ℃, and the water content of the dry slices is less than 50 ppm. The relative viscosity of the nylon 6 slice is 2.47 +/-0.2, the melting point is 215-225 ℃, and the water content of the dry slice is less than 100 ppm.
Preferably, the PET slices are normal PET slices or modified PET slices. In order to further provide the additional value of the polyester-nylon parallel composite elastic fiber and enable the polyester-nylon parallel composite elastic fiber to have functionality, the invention also provides a modified PET slice, and the preparation method comprises the following steps:
a) adding terephthalic acid, ethylene glycol, a catalyst (at least one of ethylene glycol antimony, antimony trioxide, a titanium-silicon composite catalyst and titanate), an ethylene glycol solution of a phosphorus flame retardant esterified substance and an ethylene glycol solution of a maleic anhydride esterified substance into a reaction vessel, and then pulping.
b) Introducing nitrogen into the reaction vessel to remove air, then filling nitrogen, adding initial pressure to 0.08-0.12Mpa, heating to 235-; after esterification, adding ethylene glycol suspension containing vinyl nano silicon spheres into a reaction container, stirring for 30-45 min, carrying out pre-polycondensation reaction at 260-270 ℃ under vacuum of-0.09-0.1 Mpa for 0.5-1 h, then carrying out polycondensation at 273-278 ℃ under high vacuum of less than 70pa for 2-3 h, after the reaction is finished, extruding melt by using nitrogen, cooling by water, and carrying out grain cutting to obtain the modified PET slice.
Example 1
The raw materials comprise: PET slices (intrinsic viscosity 0.65 +/-0.2 dL/g, melting point 260-265 ℃ C.)
PA6 slice (relative viscosity 2.47 +/-0.2, melting point 215-225 ℃ C.)
Respectively drying the Polyester (PET) slices and the chinlon 6(PA6) slices. The drying temperature of the polyester chips is 130 ℃, the drying time is 20h, and the water content of the polyester chips after drying treatment is less than 50 ppm. The drying temperature of the nylon 6 slices is 95 ℃, the drying time is 24 hours, and the water content of the dried nylon 6 slices is less than 100 ppm.
Respectively feeding the dried terylene slices and the dried chinlon slices into a double-screw extruder for melt extrusion according to a set composite ratio (40: 60), respectively feeding the melts of the two components into a composite spinning assembly through melt pipelines by two sets of metering pumps, spraying the melts out of a spinneret plate (shown in figure 1), and then performing side-blowing cooling, oiling, winding, first hot rollers, second hot rollers and FDY winding to form a finished product.
Wherein PET is used as a component A, and the temperature of each zone of the screw is 260-285 ℃; PA6 is used as a component B, the temperature of each zone of the screw is 260-270 ℃, the temperature of a spinning box body is 275 ℃, and the air speed of cross-blown air is 0.7 m/s; the spinning speed of a first hot roller is 1200m/min, and the temperature is 75 ℃; the temperature of the second hot roll is 130 ℃, and the stretching ratio is 3.0.
The self-curling composite filament prepared by the process has the specification of 100dtex/36 f.
Example 2
The present embodiment is the same as embodiment 1 in arrangement and operation principle, and the difference is that:
wherein PET is used as a component A, and the temperature of each zone of the screw is 260-285 ℃; PA6 is used as a component B, the temperature of each zone of the screw is 260-270 ℃, the temperature of a spinning box body is 275 ℃, and the air speed of cross-blown air is 0.7 m/s; the spinning speed of a first hot roller is 1200m/min, and the temperature is 75 ℃; the temperature of the second hot roll is 150 ℃, and the stretching ratio is 3.0.
The self-crimping composite filament prepared by the process has the specification of 100dtex/24 f.
Example 3
The present embodiment is the same as embodiment 1 in arrangement and operation principle, and the difference is that:
wherein PET is used as a component A, and the temperature of each zone of the screw is 260-285 ℃; PA6 is used as a component B, the temperature of each zone of the screw is 260-270 ℃, the temperature of a spinning box body is 275 ℃, and the air speed of cross-blown air is 0.7 m/s; the spinning speed of a first hot roller is 1200m/min, and the temperature is 95 ℃; the temperature of the second hot roll is 150 ℃, and the stretching ratio is 3.0.
The self-curling composite filament prepared by the process has the specification of 100dtex/36 f.
Example 4
The present embodiment is the same as embodiment 1 in arrangement and operation principle, and the difference is that:
wherein PET is used as a component A, and the temperature of each zone of the screw is 260-285 ℃; PA6 is used as a component B, the temperature of each zone of the screw is 260-270 ℃, the temperature of a spinning box body is 275 ℃, and the air speed of cross-blown air is 0.7 m/s; the spinning speed of a first hot roller is 1200m/min, and the temperature is 95 ℃; the temperature of the second hot roll is 150 ℃, and the stretching ratio is 3.8.
The self-curling composite filament prepared by the process has the specification of 100dtex/36 f.
Comparative example 1 (side-by-side, but not sheath-core, clad structure)
The raw materials comprise: PET slices (intrinsic viscosity 0.65 +/-0.2 dL/g, melting point 260-265 ℃ C.)
PA6 slice (relative viscosity 2.47 +/-0.2, melting point 215-225 ℃ C.)
Respectively drying the Polyester (PET) slices and the chinlon 6(PA6) slices. The drying temperature of the polyester chips is 130 ℃, the drying time is 20h, and the water content of the polyester chips after drying treatment is less than 50 ppm. The drying temperature of the nylon 6 slices is 95 ℃, the drying time is 24 hours, and the water content of the dried nylon 6 slices is less than 100 ppm.
Respectively feeding the dried terylene slices and the dried chinlon slices into a double-screw extruder according to a set composite ratio (50: 50) for melt extrusion, wherein melts of the two components are respectively subjected to two sets of metering pumps, wherein PET is used as a component A, and the temperature of each zone of a screw is 260-285 ℃; PA6 is used as a component B, the temperature of each zone of the screw is 260-270 ℃, and the temperature of the spinning manifold is 275 ℃. The two components enter a composite spinning assembly through a melt pipeline and are sprayed out by a conventional 36f parallel composite spinneret plate. At this time, the non-oil yarn is drawn, and the fiber is stripped into 2 pieces, so that the obvious fiber opening phenomenon occurs, and the subsequent spinning operation is not continued.
Comparative example 2 (side by side sheath core construction, polyester and nylon ratio outside the scope of claims)
The raw materials comprise: PET slices (intrinsic viscosity 0.65 +/-0.2 dL/g, melting point 260-265 ℃ C.)
PA6 slice (relative viscosity 2.47 +/-0.2, melting point 215-225 ℃ C.)
Respectively drying the Polyester (PET) slices and the chinlon 6(PA6) slices. The drying temperature of the polyester chips is 130 ℃, the drying time is 20h, and the water content of the polyester chips after drying treatment is less than 50 ppm. The drying temperature of the nylon 6 slices is 95 ℃, the drying time is 24 hours, and the water content of the dried nylon 6 slices is less than 100 ppm.
Respectively feeding the dried terylene slices and the dried chinlon slices into a double-screw extruder for melt extrusion according to a set composite ratio (55: 45), respectively feeding the melts of the two components into a composite spinning assembly through melt pipelines by two sets of metering pumps, spraying the melts out of a spinneret plate (shown in figure 1), and then performing side-blowing cooling, oiling, winding, first hot rollers, second hot rollers and FDY winding to form a finished product.
Wherein PET is used as a component A, and the temperature of each zone of the screw is 260-285 ℃; PA6 is used as a component B, the temperature of each zone of the screw is 260-270 ℃, the temperature of a spinning box body is 275 ℃, and the air speed of cross-blown air is 0.7 m/s; the spinning speed of a first hot roller is 1200m/min, and the temperature is 75 ℃; the temperature of the second hot roll is 130 ℃, and the stretching ratio is 3.0.
The self-curling composite filament prepared by the process has the specification of 100dtex/36 f.
Comparative example 3 (parallel sheath-core construction, but part of the process parameters in the spinning process are outside the scope of the claims)
The raw materials comprise: PET slices (intrinsic viscosity 0.65 +/-0.2 dL/g, melting point 260-265 ℃ C.)
PA6 slice (relative viscosity 2.47 +/-0.2, melting point 215-225 ℃ C.)
Respectively drying the Polyester (PET) slices and the chinlon 6(PA6) slices. The drying temperature of the polyester chips is 130 ℃, the drying time is 20h, and the water content of the polyester chips after drying treatment is less than 50 ppm. The drying temperature of the nylon 6 slices is 95 ℃, the drying time is 24 hours, and the water content of the dried nylon 6 slices is less than 100 ppm.
Respectively feeding the dried terylene slices and the dried chinlon slices into a double-screw extruder for melt extrusion according to a set composite ratio (40: 60), respectively feeding the melts of the two components into a composite spinning assembly through melt pipelines by two sets of metering pumps, spraying the melts out of a spinneret plate (shown in figure 1), and then performing side-blowing cooling, oiling, winding, first hot rollers, second hot rollers and FDY winding to form a finished product.
Wherein PET is used as a component A, and the temperature of each zone of the screw is 270-290 ℃; PA6 is used as a component B, the temperature of each zone of the screw is 255-270 ℃, the temperature of the spinning box is 290 ℃, and the air speed of the cross-blown air is 0.7 m/s; the spinning speed of a first hot roller is 1200m/min, and the temperature is 105 ℃; the temperature of the second hot roll is 150 ℃, and the stretching ratio is 3.0.
The self-curling composite filament prepared by the process has the specification of 100dtex/36 f.
The filaments prepared in the above examples were tested for physical properties according to the method for testing tensile properties of filament GB/T-14337, the method for testing crimp properties of filament GB/T-14338 and the method for testing thermal shrinkage of filament GB/T-6505-2008 chemical fiber-filament, as shown in Table 1.
TABLE 1 Main preparation Process and fiber physical index
It can be seen from the comparison of the above examples and table 1 that the polyester-nylon parallel elastic fiber with the advantages of moisture absorption, air permeability, pilling resistance, bulkiness, high elasticity, stiff and smooth fabric is prepared by using polyethylene terephthalate (PET) and nylon 6(PA6) as two parallel components, respectively melt-extruding the two components by a screw extruder, feeding the melt into a two-component composite spinning device and a specially designed parallel composite spinneret orifice, and cooling, oiling, drafting, heat-setting and winding the sprayed melt.
The fiber obtained in the comparative example 2 has improper proportions of the PET component and the PA6 component, so that fiber part is split, the mechanical property is seriously reduced, and the fiber cannot be used for subsequent processing treatment. The fiber obtained in the comparative example 3 has poor performance because the spinning temperature is high, the performance of the fiber is influenced, the winding temperature is high, the fiber is not beneficial to fiber forming.
The mechanical properties of the fibers obtained in the embodiments 1 to 4 meet related standard requirements, and the PET and PA6 with excellent properties are adopted as the two components, so that the obtained polyester-nylon parallel composite elastic fiber has the advantages of light weight, wear resistance, fatigue resistance, high strength, easiness in dyeing, moisture absorption and the like of nylon, and also has the advantages of high elasticity, high elastic recovery, high oil absorption, high impact resistance and the like of polyester. After the fiber is subjected to heat treatment, the high-elasticity self-curling effect can be generated due to the asymmetrical structure of the cross section and the shrinkage difference of the two components. Can be compared with other polyester parallel composite fibers to create high value-added fibers.
Example 5
In order to enable the polyester-nylon parallel composite elastic fiber to further have functionality, the modified PET slice is adopted in the invention.
Preparing vinyl nano silicon spheres: adding 3.8g of vinyltriethoxysilane into 30g of water, adding 0.05g of 25 mass percent ammonia water, adjusting the pH to 9, stirring at room temperature for 12 hours to obtain a transparent and uniform dispersion, adding 6.9mmol/L sodium dodecyl benzene sulfonate, continuing stirring for 12 hours, centrifuging, washing, preparing an ethylene glycol suspension of 10 mass percent vinyl nano silicon spheres in ethylene glycol, and measuring the particle size of the vinyl nano silicon spheres prepared by a gel method by using a particle size potentiometer to be 1000nm, wherein D90 to be 500 nm. In the above process, the particle size of the vinyl nano silicon spheres needs to be controlled by strictly limiting the pH value, the stirring speed and the stirring time. The grain diameter of the silicon spheres is also controlled at 200-1000nm, and the polyester spinning is not influenced, so that the silicon spheres can be directly used as flame-retardant anti-dripping polyester for fibers.
Preparation of ethylene glycol solution of CEPPA esterified product (phosphorus flame retardant esterified product): adding CEPPA powder and ethylene glycol into a reaction kettle according to the molar ratio of 1: 4.14, stirring at 185 ℃ under normal pressure for esterification reaction, maintaining for 30 minutes, adding ethylene glycol to dilute the CEPPA to 30 wt%, discharging, collecting with a beaker, and cooling for later use. The method controls the ratio of alcohol to acid and the reaction temperature, maintains enough time at a certain temperature to reach esterification balance, and finally leads the acid value of the product to reach proper value through ethylene glycol dilution.
Preparation of glycol solution of maleic anhydride esterified substance: adding maleic anhydride and ethylene glycol into a reaction kettle according to the molar ratio of 1: 5, stirring at 140 ℃ under normal pressure to perform ester exchange ring-opening reaction, reacting for 30 minutes until the reaction product is clear and transparent, finishing the reaction, collecting by using a beaker, and cooling for later use. The invention maintains enough time to reach esterification balance at a certain temperature by controlling the ratio of alcohol to acid and the reaction temperature.
Preparing a modified PET slice: 664g of terephthalic acid, 306.8g of ethylene glycol, 128.7g of ethylene glycol solution of CEPPA esterified substance, 96.5g of ethylene glycol solution of maleic anhydride esterified substance and 0.5g of ethylene glycol antimony are beaten and added into a reaction kettle, nitrogen is filled to discharge the air in the kettle, the operation is repeated for three times, and finally the pressure is increased to 0.1 MPa; heating to 245 ℃ to start esterification, controlling the water outlet speed to be slow and stable, controlling the pressure in the kettle to be 0.3MPa, maintaining for 1.5h, then, starting to reduce the pressure, gradually increasing the temperature to 255 ℃, and ending the esterification when the water outlet amount is 140ml and the pressure is recovered to normal pressure; and after the esterification reaction is finished, slowly introducing nitrogen into the reaction kettle, adding 77.2g of ethylene glycol suspension of the vinyl nano silicon spheres into the reaction kettle, stirring for 0.5h, performing low-vacuum polycondensation for 0.5h at 260 ℃, heating to 275 ℃ to perform high-vacuum polycondensation (70pa) for 2.5h, discharging after the melt viscosity reaches the standard, cooling by water, and pelletizing.
The modified PET chip has excellent flame-retardant and anti-dripping characteristics, the oxygen index of the modified PET chip is 32.0 percent, the vertical combustion grade of a sample strip is V-1, the number of molten drops after ignition for two times in vertical combustion until the molten drops are extinguished is 1, but absorbent cotton is not ignited, and the content of agglutinated particles in the chip is 0; the cloth sample oxygen index is 33.0%, the vertical combustion grade is B-1, and the cloth sample oxygen index is ignited twice in the combustion until the cloth sample oxygen index is extinguished and no molten drop exists.
Preparing polyester-nylon parallel composite elastic fibers:
the raw materials comprise: modified PET (polyethylene terephthalate) slice
PA6 slicing
And respectively drying the modified Polyester (PET) slices and the chinlon 6(PA6) slices. The drying temperature of the modified polyester chip is 130 ℃, the drying time is 20h, and the water content of the modified polyester chip after drying treatment is less than 50 ppm. The drying temperature of the nylon 6 slices is 95 ℃, the drying time is 24 hours, and the water content of the dried nylon 6 slices is less than 100 ppm.
And respectively feeding the dried modified polyester chips and the dried polyamide chips into a double-screw extruder for melt extrusion according to a set composite ratio (40: 60), feeding the melts of the two components into a composite spinning assembly through a melt pipeline by using two sets of metering pumps, spraying the melts out of a spinneret plate, and performing side-blowing cooling, oiling, winding, first hot rollers, second hot rollers and FDY winding to form a finished product.
Wherein the modified PET is used as a component A, and the temperature of each zone of the screw is 260-285 ℃; PA6 is used as a component B, the temperature of each zone of the screw is 260-270 ℃, the temperature of a spinning box body is 265 ℃, and the air speed of cross-blown air is 0.7 m/s; the spinning speed of a first hot roller is 1200m/min, and the temperature is 75 ℃; the temperature of the second hot roll is 130 ℃, and the stretching ratio is 3.0.
The self-curling composite filament prepared by the process has the specification of 100dtex/36 f.
The polyester-nylon parallel composite elastic fiber obtained in the embodiment has excellent flame retardant and anti-dripping performances.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (9)
1. A preparation method of polyester-nylon parallel composite elastic fiber is characterized by comprising the following steps:
1) respectively drying the PET slices and the nylon 6 slices, and then melting by a screw extruder to obtain a PET spinning melt and a nylon 6 spinning melt;
2) the two spinning melts respectively enter the two-component composite spinning assembly through respective corresponding pipelines to be spun, and the two spinning melts are sprayed out from the sheath-core composite spinneret to form filaments;
3) cooling, oiling, stretching, shaping and winding the strand silk to obtain the polyester-nylon parallel composite elastic fiber; the two components in the polyester-nylon parallel composite elastic fiber are combined in parallel, and the cross section of the polyester-nylon parallel composite elastic fiber is dumbbell-shaped; and the surface of the terylene component is coated with a nylon 6 layer;
the sheath-core composite spinneret plate comprises a spinneret plate, and a circle of spinneret holes are formed in the spinneret plate; each spinneret orifice consists of a dumbbell-shaped nylon 6 spinneret orifice and a polyester spinneret orifice arranged in the center of one side of the nylon 6 spinneret orifice;
the PET slices are modified PET slices; the preparation method comprises the following steps:
a) adding terephthalic acid, ethylene glycol, a catalyst, an ethylene glycol solution of a phosphorus flame retardant esterified substance and an ethylene glycol solution of a maleic anhydride esterified substance into a reaction container, and pulping;
b) introducing nitrogen into the reaction vessel to remove air, then filling nitrogen, adding initial pressure to 0.08-0.12Mpa, heating to 235-; after esterification, adding ethylene glycol suspension of vinyl nano silicon spheres into a reaction container, stirring for 30-45 min, carrying out pre-polycondensation reaction at 260-270 ℃ under vacuum of-0.09 to-0.1 Mpa for 0.5-1 h, then carrying out polycondensation at 273-278 ℃ under high vacuum of less than 70pa for 2-3 h, after the reaction is finished, extruding melt by using nitrogen, cooling by water, and carrying out grain cutting to obtain the modified PET slice.
2. The method according to claim 1, wherein the number of the holes of the sheath-core composite spinneret is 24 to 48.
3. The preparation method according to claim 1, wherein in the step 1), the screw temperature of the screw extruder is 260 to 285 ℃.
4. The preparation method according to claim 1, wherein in the step 2), the temperature of a spinning beam of the two-component composite spinning assembly is 260-285 ℃; the temperature of a first hot roller is 75-95 ℃ and the temperature of a second hot roller is 130-150 ℃ during stretching and shaping; the stretching ratio is 3.0 to 4.0.
5. The method of claim 1, wherein the mass ratio of the PET chip to the PA6 chip is 25:75 to 45: 55.
6. The process according to claim 1, wherein the PET chip has an intrinsic viscosity of 0.65 ± 0.2dL/g, a melting point of 240-265 ℃, and a water content of less than 50ppm in a dry chip.
7. The method of claim 1 or 6, wherein the nylon 6 chip has a relative viscosity of 2.47 ± 0.2, a melting point of 215-225 ℃, and a water content of less than 100ppm in a dried chip.
8. The method of claim 1, wherein the catalyst comprises at least one of ethylene glycol antimony, antimony trioxide, titanium-silicon composite catalyst, and titanate.
9. The preparation method of claim 1, wherein the polyester-nylon side-by-side conjugate elastic fiber has a specification of 100 dtex/24-48 f.
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| CN112538668B (en) * | 2020-12-10 | 2023-05-23 | 浙江理工大学 | Preparation method of antistatic ultraviolet-resistant fiber |
| CN112760749A (en) * | 2020-12-29 | 2021-05-07 | 嘉兴市凯邦锦纶科技股份有限公司 | Manufacturing method of parallel superfine denier modified polyester fancy spun yarn |
| CN114150390A (en) * | 2021-10-14 | 2022-03-08 | 江苏嘉通能源有限公司 | Production equipment and production method of polyester-nylon composite yarn shaped like Chinese character' mi |
| CN114108113B (en) * | 2021-12-27 | 2022-10-18 | 浙江昊能科技有限公司 | Manufacturing method of superfine denier easy-to-dye polyester-nylon composite filament fiber |
| CN114351268B (en) * | 2022-01-06 | 2023-02-28 | 浙江昊能科技有限公司 | Preparation method of flame-retardant anti-dripping polyester-nylon composite fiber |
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