CN106811821B - Multi-blade special-shaped polyester fiber FDY (fully drawn yarn) and preparation method thereof - Google Patents

Multi-blade special-shaped polyester fiber FDY (fully drawn yarn) and preparation method thereof Download PDF

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CN106811821B
CN106811821B CN201611249311.7A CN201611249311A CN106811821B CN 106811821 B CN106811821 B CN 106811821B CN 201611249311 A CN201611249311 A CN 201611249311A CN 106811821 B CN106811821 B CN 106811821B
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chain segment
profiled
polyester
polyester fiber
modified polyester
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CN106811821A (en
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韦开顺
朱冬妹
银少和
丛茂鹏
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Jiangsu Hengke Advanced Materials Co Ltd
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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
    • D01F6/88—Monocomponent 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
    • D01F6/92—Monocomponent 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16—Dicarboxylic acids and dihydroxy compounds
    • C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/181—Acids containing aromatic rings
    • C08G63/185—Acids containing aromatic rings containing two or more aromatic rings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16—Dicarboxylic acids and dihydroxy compounds
    • C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/181—Acids containing aromatic rings
    • C08G63/185—Acids containing aromatic rings containing two or more aromatic rings
    • C08G63/187—Acids containing aromatic rings containing two or more aromatic rings containing condensed aromatic rings
    • C08G63/189—Acids containing aromatic rings containing two or more aromatic rings containing condensed aromatic rings containing a naphthalene ring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16—Dicarboxylic acids and dihydroxy compounds
    • C08G63/20—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/66—Polyesters containing oxygen in the form of ether groups
    • C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/672—Dicarboxylic acids and dihydroxy compounds
    • 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
    • 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
    • D01D5/12—Stretch-spinning methods
    • 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
    • D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
    • 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
    • D01F1/10—Other agents for modifying properties

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Polyesters Or Polycarbonates (AREA)

Abstract

The invention belongs to the field of polyester spinning, and relates to a multi-blade profiled polyester fiber FDY (fully drawn yarn) and a preparation method thereof, wherein polyester is modified polyester, and a molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a rigid structure chain segment, wherein the rigid structure chain segment is a 2, 6-naphthalenedicarboxylic acid chain segment, a bisphenol A chain segment, a 1, 4-cyclohexanedimethanol chain segment, a 2, 2-biphenyldicarboxylic acid chain segment, a 4, 4-diphenylene dicarboxylic acid chain segment, a 2, 4-biphenyldicarboxylic acid chain segment, a 3, 4-biphenyldicarboxylic acid chain segment, a 4, 4-biphenyldicarboxylic acid chain segment or a p-hydroxybenzoic acid chain segment, the molar ratio of the rigid structure chain segment to the terephthalic acid chain segment is 0.02-0.05:1, and the extrusion expansion ratio of a modified polyester melt is 1.25-. The multi-leaf profiled polyester fiber FDY prepared by the invention has good shape-preserving effect.

Description

Multi-blade special-shaped polyester fiber FDY (fully drawn yarn) and preparation method thereof
Technical Field
The invention belongs to the field of polyester spinning, and relates to a multi-blade profiled polyester fiber FDY yarn and a preparation method thereof.
Background
Since the advent of polyethylene terephthalate (PET fiber or polyester fiber) fiber, the fiber has a series of excellent properties such as high breaking strength and elastic modulus, moderate resilience, excellent heat setting, good heat and light resistance, acid and alkali resistance, corrosion resistance and the like, and the fabric has the advantages of crease resistance, non-ironing property, good stiffness and the like, and is widely applied to the fields of clothing, home textiles and the like.
Household textiles are one of three final product fields in the textile industry, and along with improvement of life quality of people, comfort, functionality and environmental protection increasingly become new requirements of consumers for home textile products. The polyester filament yarn products for home textile production in the market mainly use conventional common polyester products, have certain defects in hand feeling, luster and subsequent processing difficulty, and cannot meet the ever-increasing requirements of comfort and functionality of people.
The abnormity of the fiber section can improve the glossiness, bulkiness, hygroscopicity, fuzzing resistance, pilling resistance, stain resistance, stiffness, elasticity, hand feeling and the like of textile products to different degrees, and the special-shaped fiber is widely applied in the fields of clothes, household and industrial textiles. Common shaped fibers are triangular, trilobal, multilobal, cruciform, hollow fibers, and the like.
The profiled fiber is prepared by a specially designed and manufactured profiled spinneret plate through a special spinning process, which is the most commonly used method for producing profiled fibers at home and abroad, and the profiled fiber with any section shape can be produced by improving and optimizing a spinneret plate guide hole and micropore processing technology and a spinning technology, but the profiled fiber can generate an extrusion and expansion effect due to melt viscosity, and the profile degree of a product is not high, so that the fiber can not achieve the designed effect.
Disclosure of Invention
The invention aims to overcome the problem of poor shape-preserving effect of multi-lobal profiled fibers prepared by the prior art, and provides a polyester spinning method for weakening the extrusion swelling effect.
In order to achieve the purpose, the invention adopts the technical scheme that:
a polyester spinning method for weakening the extrusion swelling effect is characterized in that according to a multi-blade profiled polyester fiber FDY spinning process, polyester is modified polyester, and a molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a rigid structure chain segment;
the rigid structure chain segment is a 2, 6-naphthalenedicarboxylic acid chain segment, a bisphenol A chain segment, a 1, 4-cyclohexanedimethanol chain segment, a 2, 2-biphenyldicarboxylic acid chain segment, a 4, 4-diphenyl ether dicarboxylic acid chain segment, a 2, 4-biphenyldicarboxylic acid chain segment, a 3, 4-biphenyldicarboxylic acid chain segment, a 4, 4-biphenyldicarboxylic acid chain segment or a p-hydroxybenzoic acid chain segment;
the molar ratio of the rigid structure chain segment to the terephthalic acid chain segment is 0.02-0.05:1, and the extrusion swelling ratio of the modified polyester melt is 1.25-1.35.
The method for testing the extrusion swell ratio comprises the following steps: the method comprises the steps of utilizing a high-speed camera to make circular motion around a spinneret plate, shooting a dynamic image of a melt extruded from a spinneret micropore of the spinneret plate, establishing a three-dimensional graph through three-dimensional simulation, calculating the ratio of the maximum cross section area of the melt extruded from the spinneret micropore to the cross section area of the spinneret micropore to be an extrusion swelling ratio B, obtaining an extrusion swelling value B1 of one experiment, continuously taking 50 groups of data, averaging and obtaining a final B value.
As a preferred technical scheme:
according to the preparation method of the multi-blade profiled polyester fiber FDY yarn, the modified polyester melt is metered, extruded, cooled, oiled, stretched, heat-set and wound to prepare the multi-blade profiled polyester fiber FDY yarn, and the main spinning process parameters of the multi-blade profiled polyester fiber FDY yarn are as follows:
extrusion temperature: 285 ℃ and 300 ℃;
cooling temperature: 20-25 ℃;
network pressure: 0.20-0.30 MPa;
a roll speed: 2200-2600 m/min;
first roll temperature: 75-90 ℃;
two roll speed: 3600-3900 m/min;
temperature of the two rolls: 115 ℃ and 135 ℃;
winding speed: 4000-4600 m/min.
According to the preparation method of the multi-blade profiled polyester fiber FDY, the spinneret plate is used for spinning the multi-blade profiled fiber.
The preparation method of the multi-lobal profiled polyester fiber FDY yarn has the advantages that the number average molecular weight of the modified polyester is 20000-28000.
The preparation method of the leafy profiled polyester fiber FDY yarn comprises the following steps:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and a monomer containing a rigid structure into slurry, adding a catalyst and a stabilizer, uniformly mixing, and then carrying out esterification reaction, wherein the esterification reaction is carried out in a nitrogen atmosphere under the pressure of normal pressure to 0.3MPa, the temperature of the esterification reaction is 250-260 ℃, and the end point of the esterification reaction is when the distilled amount of water in the esterification reaction reaches more than 90% of the theoretical value; the monomer containing the rigid structure is 2, 6-naphthalenedicarboxylic acid, di-p-phthalate of bisphenol A, 1, 4-cyclohexanedimethanol, 2-diphenyldicarboxylic acid, 4-diphenyletherdicarboxylic acid, 2, 4-diphenyldicarboxylic acid, 3, 4-diphenyldicarboxylic acid, 4-diphenyldicarboxylic acid or p-hydroxybenzoate of terephthalic acid; the molar ratio of the terephthalic acid to the ethylene glycol to the monomer containing the rigid structure is 1:1.2-2.0: 0.02-0.05;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to below 500Pa absolute pressure, the temperature is controlled at 260-270 ℃, and the reaction time is 30-50 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to be less than 100Pa, the reaction temperature is controlled to be 275-285 ℃, and the reaction time is 50-90min, thereby obtaining the modified polyester.
According to the preparation method of the leafy profiled polyester fiber FDY yarn, the catalyst is antimony trioxide, ethylene glycol antimony or antimony acetate, the adding amount of the catalyst is 0.01-0.05% of the weight of the terephthalic acid, the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite, and the adding amount of the stabilizer is 0.01-0.05% of the weight of the terephthalic acid.
The invention also provides the multi-blade profiled polyester fiber FDY filament which has excellent shape-preserving effect, the filament number of the multi-blade profiled polyester fiber FDY filament is 2.0-4.0dtex, the breaking strength is more than or equal to 3.8cN/dtex, and the elongation at break is 33.0 +/-3.0%; the linear density deviation rate of the multi-blade profiled polyester fiber FDY is less than or equal to 0.5 percent, the breaking strength CV value is less than or equal to 4.0 percent, the breaking elongation CV value is less than or equal to 8.0 percent, and the yarn evenness unevenness CV value is less than or equal to 2.0 percent.
The ideal design effect can not be achieved when the multi-lobal profiled fiber is prepared by adopting a melt spinning method, which is mainly caused by two reasons, on one hand, the polymer melt can generate an extrusion swelling effect when passing through a spinneret plate, on the other hand, the surface tension of the polymer melt is larger, the polyester melt is influenced by the surface tension, and the shape retention effect of the multi-lobal profiled fiber is poorer because the polyester melt is more 'round and smooth' and has no edge angle. The cross section shape of the polyester melt is changed all the time when the polyester melt is extruded from the spinneret micropores, the polyester melt begins to extrude and swell in an area within 2mm from the outlet of the spinneret micropores, the extrusion and swell reaches the maximum when the distance is 2mm from the outlet of the spinneret micropores, the influence of the extrusion and swell on the cross section shape is eliminated when the distance is more than 4mm from the outlet of the spinneret micropores, and the surface tension of the polyester melt begins to influence the cross section shape of the polyester melt. According to the invention, the rigidity of the polyester molecular chain is increased by introducing the rigid structure chain segment into the polyester molecule, so that the extrusion swelling effect is weakened, the surface tension is reduced, and the multi-lobal profiled fiber with a good shape-preserving effect is prepared.
The extrusion swelling of polyester melt is caused by elastic deformation effect or memory effect, when the melt enters a die, because of streamline contraction, a velocity gradient is generated in the flowing direction, namely stretching deformation, if the residence time in the die is short, the melt cannot be relaxed, and the shrinkage is generated after the die is removed, so the extrusion swelling is caused. The extrusion swelling of the polyester melt is also caused by the normal stress difference, the melt flows in a die and is subjected to shear deformation, and the normal stress exists in the direction vertical to the shear direction, so that the extrusion swelling is further caused. When a rigid structure chain segment is introduced into a polyester molecular chain, the rigidity of the polyester molecular chain is increased, when a polyester melt enters a spinning micropore, the compressibility of the polyester melt is reduced, the elastic deformation effect is reduced, the normal stress difference is reduced, and when the polyester melt is extruded from the spinning micropore, the memory effect is weakened, so that the extrusion swell ratio is reduced.
The surface tension of the polyester melt is formed by unbalanced intermolecular force on the surface molecules of the substance, the surface tension of the polymer melt is in direct proportion to the fourth power of the isospecific volume, the isospecific volume is the sum of contribution constants of each atom and group in a polymer unit structure, the isospecific volume has additivity, the contribution constants of different atoms and groups to the isospecific volume are different, and when a rigid structure chain segment is introduced into the polyester molecule, the surface tension of the polyester containing the rigid structure chain segment is smaller than that of common polyester because the isospecific volume of the rigid structure chain segment is far smaller than that of a terephthalic acid chain segment or a glycol chain segment.
Has the advantages that:
(1) the polyester spinning method can effectively weaken the extrusion swelling effect of the polyester melt when the polyester melt is extruded from the spinning micropores, and the extrusion swelling ratio of the modified polyester melt is 1.25-1.35 which is far less than that of the common polyester melt by 1.36-1.50;
(2) the polyester spinning method of the invention can reduce the surface tension of the polyester melt while weakening the extrusion swelling effect, and the isospecific volume of the rigid structure chain segment is smaller than that of the terephthalic acid chain segment or the ethylene glycol chain segment, and specifically comprises the following steps: the 2, 6-naphthalene dicarboxylic acid segment is 10m smaller than the terephthalic acid segment5/2·KJ1/4Per mol, bisphenol A segments are 51.4m smaller than ethylene glycol segments5/2·KJ1/4The 1, 4-cyclohexanedimethanol chain segment is 78.2m smaller than the ethylene glycol chain segment5/2·KJ1/4The chain length of the 2, 2-biphenyldicarboxylic acid is 0.7m less than that of the phthalic acid5/2·KJ1/4The/mol, 4, 4-diphenyl ether dicarboxylic acid chain segment is 31.4m smaller than that of the phthalic acid chain segment5/2·KJ1/4Per mol, the p-hydroxybenzoic acid segment was 32.3m smaller than the ethylene glycol segment5/2·KJ1/4The chain segment of the 2, 4-biphenyldicarboxylic acid is 8.6m smaller than that of the phthalic acid5/2·KJ1/4The per mol, 3, 4-biphenyldicarboxylic acid segment is 8.6m smaller than the phthalic acid segment5/2·KJ1/4The chain length of the 4, 4-biphenyldicarboxylic acid is 8.6m less than that of the phthalic acid5/2·KJ1/4/mol；
(3) The modified polyester has less content of a rigid structure chain segment, and can keep the excellent characteristics of a polyester body;
(4) the multi-blade profiled fiber with good shape-preserving effect and ideal design effect can be prepared by adopting the polyester spinning method.
Drawings
FIG. 1 is a schematic cross-sectional view of trilobal spinneret micro-holes, wherein c-the radius of the circumscribed circle, d-the radius of the arc at the tip of the blade, e-the radius of the inscribed circle, and f-the length of the blade;
FIG. 2 is a comparison of the cross-sections of fibers made in example 1 and comparative example 1, with the solid portion being the cross-section of the fiber of example 1 and the dashed portion being the cross-section of the fiber of comparative example 1;
FIG. 3 is a schematic cross-sectional view of five-lobed spinneret micro-holes, wherein a is the lobe length and b is the lobe width;
FIG. 4 is a comparison of the cross-sections of fibers made in example 2 and comparative example 2, with the solid portion being the cross-section of the fiber for example 2 and the dashed portion being the cross-section of the fiber for comparative example 2.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A preparation method of trilobal profiled polyester fiber FDY yarns comprises the following steps of:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and 2, 6-naphthalenedicarboxylic acid into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 2, 6-naphthalenedicarboxylic acid is 1:1.2:0.02, adding antimony trioxide and triphenyl phosphate, uniformly mixing, and performing esterification reaction, wherein the adding amount of the antimony trioxide is 0.01 percent of the weight of the terephthalic acid, the adding amount of the triphenyl phosphate is 0.01 percent of the weight of the terephthalic acid, the esterification reaction is performed in a nitrogen atmosphere, the pressurizing pressure is 0.1MPa, the temperature of the esterification reaction is 250 ℃, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches 90 percent of the theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to the absolute pressure of 500Pa, the temperature is controlled at 260 ℃, and the reaction time is 30 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to 99Pa, the reaction temperature is controlled at 275 ℃, and the reaction time is 50min, thereby obtaining the modified polyester.
The number average molecular weight of the finally prepared modified polyester is 20000, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a 2, 6-naphthalenedicarboxylic acid chain segment, and the molar ratio of the 2, 6-naphthalenedicarboxylic acid chain segment to the terephthalic acid chain segment is 0.02: 1.
Metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester melt to obtain the trilobal profiled polyester fiber FDY, wherein the main spinning process parameters are as follows:
extrusion temperature: 285 ℃;
cooling temperature: 20 ℃;
network pressure: 0.20 MPa;
a roll speed: 2200 m/min;
first roll temperature: 75 ℃;
two roll speed: 3600 m/min;
temperature of the two rolls: 115 ℃ is carried out;
winding speed: 4000 m/min.
The spinneret plate is a spinneret plate for spinning three-leaf profiled fibers, the cross section of each spinneret micropore is shown in figure 1, the radius c of an external circle is 80um, the radius d of a circular arc at a leaf end is 80um, the length f of each leaf is 460um, the radius e of an internal tangent circle is 104um, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinneret micropores of the spinneret plate is 1.35.
The finally prepared three-leaf profiled polyester fiber FDY has excellent shape-preserving effect, the M value (the radius of the circumscribed circle and the radius of the arc of the leaf end) is 4.04 percent, the profile degree is 75.28 percent, the profile degree test method is a chemical fiber profile degree test method, and specifically, the FZ/T50002-91 textile industry standard of the people's republic of China:
relative radial profile DR(％)。
Figure BDA0001197735170000071
The filament number of the three-blade special-shaped polyester fiber FDY is 2.0dtex, the breaking strength is 3.8cN/dtex, and the elongation at break is 30%; the linear density deviation rate of the trilobal profiled polyester fiber FDY is 0.5%, the breaking strength CV value is 4.0%, the breaking elongation CV value is 8.0%, and the yarn evenness unevenness CV value is 2.0%.
Comparative example 1
A preparation method of three-leaf profiled polyester fiber FDY yarns comprises the steps of preparing three-leaf profiled polyester fiber FDY yarns by using common polyester with the number average molecular weight of 20000 through the same spinning equipment and spinning process as those in example 1, wherein the extrusion swelling ratio of polyester melt extruded from spinning micropores of a spinneret plate is 1.40, the M value (the radius of a circumscribed circle and the radius of an arc at a leaf end) of the finally prepared three-leaf profiled polyester fiber FDY yarns is 2.84%, the profile degree is 64.78%, the profile degree of the fibers prepared in comparative example 1 is far lower than that in example 1 (75.28%), the filament number is 2.3dtex, the breaking strength is 3.5cN/dtex, and the breaking elongation is 25%; the linear density deviation rate of the trilobal profiled polyester fiber FDY is 0.8%, the breaking strength CV value is 5.0%, the breaking elongation CV value is 10.0%, and the yarn evenness unevenness CV value is 3.0%.
A comparison of the cross-sections of the fibers obtained in example 1 and comparative example 1 is shown in FIG. 2, wherein the solid part is the cross-section of the fiber obtained in example 1 and the dashed part is the cross-section of the fiber obtained in comparative example 1, and it can be seen that the cross-section area of the fiber obtained in example 1 is smaller than that of the fiber obtained in comparative example 1, the cross-section of the fiber obtained in comparative example 1 has three enlarged lobes, each lobe has a smaller lobe length than that of example 1, the camber between two adjacent lobes is larger than that of example 1, and the cross-section of the fiber obtained in example 1 is closer to a trilobal shape, which shows that the present invention effectively improves the shape-retaining effect of the fiber by reducing the die swell ratio of the melt.
Example 2
A preparation method of five-leaf profiled polyester fiber FDY (fully drawn yarn) comprises the following steps of firstly preparing modified polyester:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and bisphenol A di-p-phthalate into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the bisphenol A di-p-phthalate is 1:1.3:0.025, adding antimony trioxide and triphenyl phosphate, uniformly mixing, and performing esterification reaction, wherein the addition amount of the antimony trioxide is 0.015% of the weight of the terephthalic acid, the addition amount of the triphenyl phosphate is 0.015% of the weight of the terephthalic acid, the esterification reaction is performed in a nitrogen atmosphere, the pressurization pressure is 0.12MPa, the temperature of the esterification reaction is 251 ℃, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches 90% of the theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is steadily pumped from normal pressure to 495Pa absolute pressure, the temperature is controlled at 262 ℃, and the reaction time is 32 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to 98Pa, the reaction temperature is controlled at 276 ℃, and the reaction time is 55min, thereby obtaining the modified polyester.
The number average molecular weight of the finally prepared modified polyester is 21000, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, a glycol chain segment and a bisphenol A chain segment, and the molar ratio of the bisphenol A chain segment to the terephthalic acid chain segment is 0.025: 1.
The modified polyester melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare five-leaf profiled polyester fiber FDY yarns, and the main spinning process parameters are as follows:
extrusion temperature: 286 ℃;
cooling temperature: 20 ℃;
network pressure: 0.21 MPa;
a roll speed: 2250 m/min;
first roll temperature: 76 ℃;
two roll speed: 3630 m/min;
temperature of the two rolls: 118 ℃;
winding speed: 4100 m/min.
The spinneret plate is a spinneret plate for five-leaf profiled fiber spinning, the cross section shape of a spinning micropore is shown in figure 3, the leaf length a is 400um, the leaf width is 80um, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinning micropore of the spinneret plate is 1.34.
The finally prepared five-leaf special-shaped polyester fiber FDY has excellent shape-preserving effect, the M value (the radius of the circumscribed circle and the radius of the arc of the leaf end) is 1.74 percent, the special-shaped degree is 42.63 percent, the single filament number of the five-leaf special-shaped polyester fiber FDY is 2.2dtex, the breaking strength is 3.82cN/dtex, and the elongation at break is 30.5 percent; the linear density deviation rate of the five-leaf profiled polyester fiber FDY is 0.48%, the breaking strength CV value is 3.8%, the breaking elongation CV value is 7.8%, and the yarn evenness CV value is 1.9%.
Comparative example 2
A preparation method of five-leaf profiled polyester fiber FDY yarns comprises the steps of preparing five-leaf profiled polyester fiber FDY yarns from common polyester with the number average molecular weight of 21000 by adopting the same spinning equipment and spinning process as those in the embodiment 2, wherein the extrusion swelling ratio of polyester melt extruded from a spinning micropore of a spinneret plate is 1.45, the M value (circumscribed circle radius and leaf end arc radius) of the finally prepared five-leaf profiled polyester fiber FDY yarns is 1.42%, the profile degree is 29.38%, the profile degree of the fibers prepared in the comparative example 2 is far lower than that in the embodiment 2 (42.63%), the single-filament number is 2.3dtex, the breaking strength is 3.5cN/dtex, and the breaking elongation is 25%; the linear density deviation rate of the five-leaf profiled polyester fiber FDY is 0.8%, the breaking strength CV value is 5.0%, the breaking elongation CV value is 10.0%, and the yarn evenness CV value is 3.0%.
A comparison of the cross-sections of the fibers obtained in example 2 and comparative example 2 is shown in FIG. 4, wherein the solid line part is the cross-section of the fiber obtained in example 2 and the dashed line part is the cross-section of the fiber obtained in comparative example 2, and it can be seen that the cross-sectional area of the fiber obtained in example 2 is smaller than that of the fiber obtained in comparative example 2, and the cross-section of the fiber obtained in comparative example 2 includes the cross-section of the fiber obtained in example 2, each of the five lobes of the cross-section of the fiber obtained in comparative example 2 is relatively large compared to example 2, the radian between two adjacent lobes is relatively large compared to example 2, and the cross-section of the fiber obtained in example 2 is more nearly in the shape of five lobes, which illustrates that the present invention effectively improves the shape-retaining effect of the fiber by reducing.
Example 3
A preparation method of trilobal profiled polyester fiber FDY yarns comprises the following steps of:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and 1, 4-cyclohexanedimethanol into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 1, 4-cyclohexanedimethanol is 1:1.4:0.03, adding antimony trioxide and triphenyl phosphate, uniformly mixing, and then carrying out esterification reaction, wherein the addition amount of the antimony trioxide is 0.02% of the weight of the terephthalic acid, the addition amount of the triphenyl phosphate is 0.02% of the weight of the terephthalic acid, the esterification reaction is carried out in a nitrogen atmosphere under the pressure of 0.14MPa, the temperature of the esterification reaction is 252 ℃, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches 90% of a theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to absolute pressure of 490Pa, the temperature is controlled at 263 ℃, and the reaction time is 34 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to 97Pa, the reaction temperature is controlled at 278 ℃, and the reaction time is 59min, thereby obtaining the modified polyester.
The finally prepared modified polyester has the number average molecular weight of 22000, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a 1, 4-cyclohexanedimethanol chain segment, and the molar ratio of the 1, 4-cyclohexanedimethanol chain segment to the terephthalic acid chain segment is 0.03: 1.
Metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester melt to obtain the trilobal profiled polyester fiber FDY, wherein the main spinning process parameters are as follows:
extrusion temperature: 288 ℃;
cooling temperature: 21 ℃;
network pressure: 0.22 MPa;
a roll speed: 2300 m/min;
first roll temperature: 78 ℃;
two roll speed: 3660 m/min;
temperature of the two rolls: 120 ℃;
winding speed: 4200 m/min.
Wherein, the spinneret plate is a spinneret plate for spinning trilobal profiled fibers, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinneret micropores of the spinneret plate is 1.33.
The finally prepared three-blade special-shaped polyester fiber FDY has excellent shape-preserving effect, the filament number of the three-blade special-shaped polyester fiber FDY is 2.4dtex, the breaking strength is 3.84cN/dtex, and the elongation at break is 31%; the linear density deviation rate of the trilobal profiled polyester fiber FDY is 0.47%, the breaking strength CV value is 3.7%, the breaking elongation CV value is 7.6%, and the yarn evenness CV value is 1.8%.
Example 4
A preparation method of trilobal profiled polyester fiber FDY yarns comprises the following steps of:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and 2, 2-biphenyldicarboxylic acid into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 2, 2-biphenyldicarboxylic acid is 1:1.5:0.035, adding ethylene glycol antimony and trimethyl phosphate, uniformly mixing, and then carrying out esterification reaction, wherein the adding amount of the ethylene glycol antimony is 0.025 percent of the weight of the terephthalic acid, the adding amount of the trimethyl phosphate is 0.025 percent of the weight of the terephthalic acid, the esterification reaction is carried out in a nitrogen atmosphere under the pressure of 0.16MPa, the temperature of the esterification reaction is 254 ℃, and the end point of the esterification reaction is determined when the water distillate in the esterification reaction reaches 91 percent of the theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to 488Pa, the temperature is controlled at 264 ℃, and the reaction time is 36 min; then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to 96Pa, the reaction temperature is controlled at 279 ℃, and the reaction time is 64min, thus obtaining the modified polyester.
The number average molecular weight of the finally prepared modified polyester is 23000, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a 2, 2-biphenyldicarboxylic acid chain segment, and the molar ratio of the 2, 2-biphenyldicarboxylic acid chain segment to the terephthalic acid chain segment is 0.035: 1.
Metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester melt to obtain the trilobal profiled polyester fiber FDY, wherein the main spinning process parameters are as follows:
extrusion temperature: 290 ℃;
cooling temperature: 22 ℃;
network pressure: 0.23 MPa;
a roll speed: 2350 m/min;
first roll temperature: 80 ℃;
two roll speed: 3700 m/min;
temperature of the two rolls: 122 ℃;
winding speed: 4250 m/min.
Wherein, the spinneret plate is a spinneret plate for spinning trilobal profiled fibers, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinneret micropores of the spinneret plate is 1.32.
The finally prepared three-blade special-shaped polyester fiber FDY has excellent shape-preserving effect, the filament number of the three-blade special-shaped polyester fiber FDY is 2.6dtex, the breaking strength is 3.85cN/dtex, and the elongation at break is 32%; the linear density deviation rate of the trilobal profiled polyester fiber FDY is 0.45%, the breaking strength CV value is 3.6%, the breaking elongation CV value is 7.5%, and the yarn evenness unevenness CV value is 1.7%.
Example 5
A preparation method of trilobal profiled polyester fiber FDY yarns comprises the following steps of:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and 4, 4-diphenyl ether dicarboxylic acid into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 4, 4-diphenyl ether dicarboxylic acid is 1:1.5:0.038, adding ethylene glycol antimony and trimethyl phosphate, uniformly mixing, and performing esterification reaction, wherein the addition amount of the ethylene glycol antimony is 0.03 percent of the weight of the terephthalic acid, the addition amount of the trimethyl phosphate is 0.03 percent of the weight of the terephthalic acid, the esterification reaction is performed in a nitrogen atmosphere under the pressure of 0.18MPa, the temperature of the esterification reaction is 255 ℃, and the end point of the esterification reaction is determined when the water distillate in the esterification reaction reaches 91 percent of the theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to 486Pa absolute pressure, the temperature is controlled at 265 ℃, and the reaction time is 38 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to 95Pa, the reaction temperature is controlled at 280 ℃, and the reaction time is 68min, thereby obtaining the modified polyester.
The number average molecular weight of the finally prepared modified polyester is 24000, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a 4, 4-diphenyl ether dicarboxylic acid chain segment, and the molar ratio of the 4, 4-diphenyl ether dicarboxylic acid chain segment to the terephthalic acid chain segment is 0.038: 1.
Metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester melt to obtain the trilobal profiled polyester fiber FDY, wherein the main spinning process parameters are as follows:
extrusion temperature: 291 deg.C;
cooling temperature: 23 ℃;
network pressure: 0.25 MPa;
a roll speed: 2400 m/min;
first roll temperature: 82 ℃;
two roll speed: 3730 m/min;
temperature of the two rolls: 125 ℃;
winding speed: 4300 m/min.
Wherein, the spinneret plate is used for spinning three-leaf profiled fiber, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinneret micropores of the spinneret plate is 1.31.
The finally prepared three-blade special-shaped polyester fiber FDY has excellent shape-preserving effect, the filament number of the three-blade special-shaped polyester fiber FDY is 2.8dtex, the breaking strength is 3.86cN/dtex, and the elongation at break is 33%; the linear density deviation rate of the trilobal profiled polyester fiber FDY is 0.43%, the breaking strength CV value is 3.5%, the breaking elongation CV value is 7.4%, and the yarn unevenness CV value is 1.6%.
Example 6
A preparation method of trilobal profiled polyester fiber FDY yarns comprises the following steps of:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and 2, 4-biphenyldicarboxylic acid into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 2, 4-biphenyldicarboxylic acid is 1:1.6:0.04, adding ethylene glycol antimony and trimethyl phosphate, uniformly mixing, and then carrying out esterification reaction, wherein the adding amount of the ethylene glycol antimony is 0.035% of the weight of the terephthalic acid, the adding amount of the trimethyl phosphate is 0.035% of the weight of the terephthalic acid, the esterification reaction is carried out in a nitrogen atmosphere under the pressure of 0.2MPa, the temperature of the esterification reaction is 256 ℃, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches 92% of a theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to 485Pa, the temperature is controlled at 266 ℃, and the reaction time is 40 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to 94Pa, the reaction temperature is controlled to 281 ℃, and the reaction time is 73min, thus obtaining the modified polyester.
The number average molecular weight of the finally prepared modified polyester is 2450, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a 2, 4-biphenyldicarboxylic acid chain segment, and the molar ratio of the 2, 4-biphenyldicarboxylic acid chain segment to the terephthalic acid chain segment is 0.04: 1.
Metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester melt to obtain the trilobal profiled polyester fiber FDY, wherein the main spinning process parameters are as follows:
extrusion temperature: 293 ℃;
cooling temperature: 24 ℃;
network pressure: 0.26 MPa;
a roll speed: 2450 m/min;
first roll temperature: 83 ℃;
two roll speed: 3750 m/min;
temperature of the two rolls: 128 ℃;
winding speed: 4350 m/min.
Wherein, the spinneret plate is used for spinning three-leaf profiled fiber, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinneret micropores of the spinneret plate is 1.30.
The finally prepared three-blade special-shaped polyester fiber FDY has excellent shape-preserving effect, the filament number of the three-blade special-shaped polyester fiber FDY is 3.0dtex, the breaking strength is 3.88cN/dtex, and the elongation at break is 33.5%; the linear density deviation rate of the trilobal profiled polyester fiber FDY is 0.41%, the breaking strength CV value is 3.4%, the breaking elongation CV value is 7.3%, and the yarn evenness CV value is 1.5%.
Example 7
A preparation method of four-leaf profiled polyester fiber FDY (fully drawn yarn) comprises the following steps of firstly preparing modified polyester:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and 3, 4-biphenyldicarboxylic acid into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 3, 4-biphenyldicarboxylic acid is 1:1.7:0.045, adding antimony acetate and trimethyl phosphite, uniformly mixing, and then carrying out esterification reaction, wherein the adding amount of the antimony acetate is 0.04% of the weight of the terephthalic acid, the adding amount of the trimethyl phosphite is 0.04% of the weight of the terephthalic acid, the esterification reaction is carried out in a nitrogen atmosphere under the pressure of 0.22MPa, the temperature of the esterification reaction is 257 ℃, and the end point of the esterification reaction is determined when the water distillation amount in the esterification reaction reaches 92% of a theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is smoothly pumped from normal pressure to absolute pressure of 484Pa, the temperature is controlled at 267 ℃, and the reaction time is 42 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the reaction pressure is reduced to 93Pa, the reaction temperature is controlled at 282 ℃, and the reaction time is 77min, thereby obtaining the modified polyester.
The finally prepared modified polyester has a number average molecular weight of 25000, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a 3, 4-biphenyldicarboxylic acid chain segment, and the molar ratio of the 3, 4-biphenyldicarboxylic acid chain segment to the terephthalic acid chain segment is 0.045: 1.
The modified polyester melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare four-leaf profiled polyester fiber FDY yarns, and the main spinning process parameters are as follows:
extrusion temperature: 295 ℃;
cooling temperature: 24 ℃;
network pressure: 0.27 MPa;
a roll speed: 2480 m/min;
first roll temperature: 85 ℃;
two roll speed: 3800 m/min;
temperature of the two rolls: 130 ℃;
winding speed: 4400 m/min.
Wherein, the spinneret plate is used for spinning four-leaf profiled fiber, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinneret micropores of the spinneret plate is 1.28.
The finally prepared four-leaf profiled polyester fiber FDY has excellent shape-preserving effect, the filament number of the four-leaf profiled polyester fiber FDY is 3.2dtex, the breaking strength is 3.92cN/dtex, and the elongation at break is 33.8%; the linear density deviation rate of the four-leaf profiled polyester fiber FDY is 0.39%, the breaking strength CV value is 3.3%, the breaking elongation CV value is 7.1%, and the yarn evenness CV value is 1.4%.
Example 8
A preparation method of four-leaf profiled polyester fiber FDY (fully drawn yarn) comprises the following steps of firstly preparing modified polyester:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and 4, 4-biphenyldicarboxylic acid into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 4, 4-biphenyldicarboxylic acid is 1:1.8:0.046, adding antimony acetate and trimethyl phosphite, uniformly mixing, and then carrying out esterification reaction, wherein the adding amount of the antimony acetate is 0.045% of the weight of the terephthalic acid, the adding amount of the trimethyl phosphite is 0.045% of the weight of the terephthalic acid, the esterification reaction is carried out in a nitrogen atmosphere under the pressure of 0.24MPa, the temperature of the esterification reaction is 258 ℃, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches 93% of a theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to 481Pa absolute pressure, the temperature is controlled at 268 ℃, and the reaction time is 45 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to 92Pa, the reaction temperature is controlled to 283 ℃, and the reaction time is 82min, thereby obtaining the modified polyester.
The number average molecular weight of the finally prepared modified polyester is 26000, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a 4, 4-biphenyldicarboxylic acid chain segment, and the molar ratio of the 4, 4-biphenyldicarboxylic acid chain segment to the terephthalic acid chain segment is 0.046: 1.
The modified polyester melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare four-leaf profiled polyester fiber FDY yarns, and the main spinning process parameters are as follows:
extrusion temperature: 296 deg.C;
cooling temperature: 25 ℃;
network pressure: 0.28 MPa;
a roll speed: 2500 m/min;
first roll temperature: 88 ℃;
two roll speed: 3820 m/min;
temperature of the two rolls: 132 ℃;
winding speed: 4500 m/min.
Wherein, the spinneret plate adopts a four-leaf profiled fiber spinning spinneret plate, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinneret micropores of the spinneret plate is 1.27.
The finally prepared four-leaf profiled polyester fiber FDY has excellent shape-preserving effect, the filament number of the four-leaf profiled polyester fiber FDY is 3.4dtex, the breaking strength is 3.95cN/dtex, and the elongation at break is 34%; the linear density deviation rate of the four-leaf profiled polyester fiber FDY is 0.37%, the breaking strength CV value is 3.2%, the breaking elongation CV value is 6.9%, and the yarn evenness CV value is 1.3%.
Example 9
A preparation method of five-leaf profiled polyester fiber FDY (fully drawn yarn) comprises the following steps of firstly preparing modified polyester:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and p-hydroxybenzoate into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the p-hydroxybenzoate is 1:1.9:0.048, adding antimony acetate and trimethyl phosphite, uniformly mixing, and carrying out esterification reaction, wherein the adding amount of the antimony acetate is 0.05% of the weight of the terephthalic acid, the adding amount of the trimethyl phosphite is 0.05% of the weight of the terephthalic acid, the esterification reaction is carried out under the pressure of 0.26MPa in a nitrogen atmosphere, the temperature of the esterification reaction is 259 ℃, and the end point of the esterification reaction is determined when the water distillation amount in the esterification reaction reaches 93% of a theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to 480Pa, the temperature is controlled at 269 ℃, and the reaction time is 48 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to 91Pa, the reaction temperature is controlled to be 284 ℃, and the reaction time is 86min, thereby obtaining the modified polyester.
The number average molecular weight of the finally prepared modified polyester is 27000, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, a glycol chain segment and a p-hydroxybenzoic acid chain segment, and the molar ratio of the p-hydroxybenzoic acid chain segment to the terephthalic acid chain segment is 0.048: 1.
The modified polyester melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare five-leaf profiled polyester fiber FDY yarns, and the main spinning process parameters are as follows:
extrusion temperature: 298 deg.C;
cooling temperature: 25 ℃;
network pressure: 0.29 MPa;
a roll speed: 2550 m/min;
first roll temperature: 89 ℃;
two roll speed: 3860 m/min;
temperature of the two rolls: 133 ℃;
winding speed: 4550 m/min.
Wherein, the spinneret plate adopts a spinneret plate for five-leaf profiled fiber spinning, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinneret micropores of the spinneret plate is 1.26.
The shape-preserving effect of the finally prepared five-leaf special-shaped polyester fiber FDY is excellent, the filament number of the five-leaf special-shaped polyester fiber FDY is 3.8dtex, the breaking strength is 3.95cN/dtex, and the elongation at break is 35%; the linear density deviation rate of the five-leaf profiled polyester fiber FDY is 0.36%, the breaking strength CV value is 3.1%, the breaking elongation CV value is 6.8%, and the yarn evenness CV value is 1.2%.
Example 10
A preparation method of six-leaf profiled polyester fiber FDY (fully drawn yarn) comprises the following steps of firstly preparing modified polyester:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and 2, 6-naphthalenedicarboxylic acid into slurry, wherein the molar ratio of the terephthalic acid to the ethylene glycol to the 2, 6-naphthalenedicarboxylic acid is 1:2.0:0.05, adding antimony trioxide and triphenyl phosphate, uniformly mixing, and performing esterification reaction, wherein the adding amount of the antimony trioxide is 0.05% of the weight of the terephthalic acid, the adding amount of the triphenyl phosphate is 0.05% of the weight of the terephthalic acid, the esterification reaction is performed in a nitrogen atmosphere, the pressurizing pressure is 0.3MPa, the temperature of the esterification reaction is 260 ℃, and the end point of the esterification reaction is determined when the distilled amount of water in the esterification reaction reaches 93% of the theoretical value;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to 478Pa under absolute pressure, the temperature is controlled at 270 ℃, and the reaction time is 50 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to 90Pa, the reaction temperature is controlled at 285 ℃, and the reaction time is 90min, thereby obtaining the modified polyester.
The finally prepared modified polyester has the number average molecular weight of 28000, the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a 2, 6-naphthalenedicarboxylic acid chain segment, and the molar ratio of the 2, 6-naphthalenedicarboxylic acid chain segment to the terephthalic acid chain segment is 0.05: 1.
The modified polyester melt is subjected to metering, extrusion, cooling, oiling, stretching, heat setting and winding to prepare six-leaf profiled polyester fiber FDY yarns, and the main spinning process parameters are as follows:
extrusion temperature: 300 ℃;
cooling temperature: 25 ℃;
network pressure: 0.30 MPa;
a roll speed: 2600 m/min;
first roll temperature: 90 ℃;
two roll speed: 3900 m/min;
temperature of the two rolls: 135 deg.C;
winding speed: 4600 m/min.
Wherein the spinneret plate is a spinneret plate for six-leaf profiled fiber spinning, and the extrusion swelling ratio of the modified polyester melt when the modified polyester melt is extruded from the spinneret micropores of the spinneret plate is 1.25.
The finally prepared six-leaf profiled polyester fiber FDY has excellent shape-preserving effect, the filament number of the six-leaf profiled polyester fiber FDY is 4.0dtex, the breaking strength is 4.2cN/dtex, and the elongation at break is 36%; the linear density deviation rate of the six-leaf profiled polyester fiber FDY is 0.35%, the breaking strength CV value is 3.0%, the breaking elongation CV value is 6.5%, and the yarn evenness CV value is 1.0%.

Claims (7)

1. A preparation method of multi-leaf profiled polyester fiber FDY yarns is characterized by comprising the following steps: according to the spinning process of the multi-leaf profiled polyester fiber FDY, wherein the polyester is modified polyester, and a molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a rigid structure chain segment;
the rigid structure chain segment is a bisphenol A chain segment, a 1, 4-cyclohexanedimethanol chain segment, a 2, 2-biphenyldicarboxylic acid chain segment, a 4, 4-diphenyl ether dicarboxylic acid chain segment, a 2, 4-biphenyldicarboxylic acid chain segment, a 3, 4-biphenyldicarboxylic acid chain segment, a 4, 4-biphenyldicarboxylic acid chain segment or a p-hydroxybenzoic acid chain segment;
the molar ratio of the rigid structure chain segment to the terephthalic acid chain segment is 0.02-0.048:1, and the extrusion swelling ratio of the modified polyester melt is 1.25-1.35;
the extrusion swell ratio test method comprises the following steps: the method comprises the steps of utilizing a high-speed camera to make circular motion around a spinneret plate, shooting a dynamic image of a melt extruded from a spinneret micropore of the spinneret plate, establishing a three-dimensional graph through three-dimensional simulation, calculating the ratio of the maximum cross section area of the melt extruded from the spinneret micropore to the cross section area of the spinneret micropore to be an extrusion swelling ratio B, obtaining an extrusion swelling value B1 of one experiment, continuously taking 50 groups of data, averaging and obtaining a final B value.
2. The preparation method of the multi-lobal profiled polyester fiber FDY filament according to claim 1, wherein the modified polyester melt is metered, extruded, cooled, oiled, stretched, heat-set and wound to prepare the multi-lobal profiled polyester fiber FDY filament, and the main spinning process parameters of the multi-lobal profiled polyester fiber FDY filament are as follows:
extrusion temperature: 285 ℃ and 300 ℃;
cooling temperature: 20-25 ℃;
network pressure: 0.20-0.30 MPa;
a roll speed: 2200-2600 m/min;
first roll temperature: 75-90 ℃;
two roll speed: 3600-3900 m/min;
temperature of the two rolls: 115 ℃ and 135 ℃;
winding speed: 4000-4600 m/min.
3. The method for preparing poly-lobal profiled polyester FDY filaments according to claim 1, wherein the spinneret plate is used for spinning poly-lobal profiled fibers.
4. The preparation method of poly-lobal profiled polyester FDY filament according to claim 1, wherein the number average molecular weight of the modified polyester is 20000-28000.
5. The preparation method of multilobal profiled polyester FDY filament according to claim 1, wherein the preparation steps of the modified polyester are as follows:
(1) esterification reaction to prepare dibasic acid dihydric alcohol ester;
preparing terephthalic acid, ethylene glycol and a monomer containing a rigid structure into slurry, adding a catalyst and a stabilizer, uniformly mixing, and then carrying out esterification reaction, wherein the esterification reaction is carried out in a nitrogen atmosphere under the pressure of normal pressure to 0.3MPa, the temperature of the esterification reaction is 250-260 ℃, and the end point of the esterification reaction is when the distilled amount of water in the esterification reaction reaches more than 90% of the theoretical value; the monomer containing the rigid structure is di-p-phthalate of bisphenol A, 1, 4-cyclohexanedimethanol, 2-diphenyldicarboxylic acid, 4-diphenyl ether dicarboxylic acid, 2, 4-diphenyldicarboxylic acid, 3, 4-diphenyldicarboxylic acid, 4-diphenyldicarboxylic acid or p-hydroxybenzoate terephthalate; the molar ratio of the terephthalic acid to the ethylene glycol to the monomer containing the rigid structure is 1:1.2-2.0: 0.02-0.048;
(2) performing polycondensation reaction to obtain modified polyester;
after the esterification reaction in the step (1) is finished, starting the polycondensation reaction in a low vacuum stage under the condition of negative pressure, wherein the pressure in the stage is stably pumped from normal pressure to below 500Pa absolute pressure, the temperature is controlled at 260-270 ℃, and the reaction time is 30-50 min; and then continuously vacuumizing, and carrying out the polycondensation reaction in a high vacuum stage, so that the absolute pressure is reduced to be less than 100Pa, the reaction temperature is controlled to be 275-285 ℃, and the reaction time is 50-90min, thereby obtaining the modified polyester.
6. The method for preparing poly-lobal profiled polyester fiber FDY filament of claim 5, characterized in that the catalyst is antimony trioxide, ethylene glycol antimony or antimony acetate, the amount of catalyst added is 0.01-0.05% of the weight of terephthalic acid, the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite, and the amount of stabilizer added is 0.01-0.05% of the weight of terephthalic acid.
7. Multilobal profiled polyester fiber FDY yarn produced by the production process according to any one of claims 1 to 6, characterized in that: the shape-preserving effect of the multi-blade profiled polyester fiber FDY is excellent, the filament number of the multi-blade profiled polyester fiber FDY is 2.0-4.0dtex, the breaking strength is more than or equal to 3.8cN/dtex, and the elongation at break is 33.0 +/-3.0%; the linear density deviation rate of the multi-blade profiled polyester fiber FDY is less than or equal to 0.5 percent, the breaking strength CV value is less than or equal to 4.0 percent, the breaking elongation CV value is less than or equal to 8.0 percent, and the yarn evenness unevenness CV value is less than or equal to 2.0 percent.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102797068A (en) * 2011-05-24 2012-11-28 江苏鹰翔化纤股份有限公司 Preparation method of 2,6-naphthalenedicarboxylic acid modified polyester fiber
CN105177748A (en) * 2015-10-20 2015-12-23 浙江金霞新材料科技有限公司 Colored flame-retardant flashing profiled polyester filament and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102797068A (en) * 2011-05-24 2012-11-28 江苏鹰翔化纤股份有限公司 Preparation method of 2,6-naphthalenedicarboxylic acid modified polyester fiber
CN105177748A (en) * 2015-10-20 2015-12-23 浙江金霞新材料科技有限公司 Colored flame-retardant flashing profiled polyester filament and preparation method thereof

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