CN106835336B - A kind of FDY, square hollow polyester fiber and preparation method thereof - Google Patents
A kind of FDY, square hollow polyester fiber and preparation method thereof Download PDFInfo
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- CN106835336B CN106835336B CN201611247727.5A CN201611247727A CN106835336B CN 106835336 B CN106835336 B CN 106835336B CN 201611247727 A CN201611247727 A CN 201611247727A CN 106835336 B CN106835336 B CN 106835336B
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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
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- 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
- C08G63/183—Terephthalic acids
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- 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
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- 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
- C08G63/199—Acids or hydroxy compounds containing cycloaliphatic rings
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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
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; 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
- D01D5/253—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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- Polymers & Plastics (AREA)
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Abstract
The invention belongs to Direct-spinning of PET Fiber fields, it is related to a kind of FDY, square hollow polyester fiber and preparation method thereof, spinning melt includes saturated fat acid metal salt and modified poly ester, the mass ratio of saturated fat acid metal salt and modified poly ester is 0.0005-0.002:1, saturated fat acid metal salt refers to that carbon atom number is 12-22, fusing point is 100-180 DEG C and dynamic viscosity≤1Pas fatty acid metal salts, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and rigid structure segment, the molar ratio of rigid structure segment and terephthalic acid (TPA) segment is 0.02-0.05:1, the die swell ratio of the spinning melt is 1.21-1.32, pressure is 82-123kg/cm after filter when spinning2.FDY degree of hollowness with higher of square hollow polyester fiber produced by the present invention and preferable conformal effect.
Description
Technical field
The invention belongs to Direct-spinning of PET Fiber fields, are related to a kind of FDY, square hollow polyester fiber and preparation method thereof.
Background technique
Polyethylene terephthalate (PET fiber or polyester fiber) fiber since the advent of the world, have breaking strength and
Elasticity modulus is high, and resilience is moderate, and thermal finalization is excellent, and heat-resisting light resistance is good and acid-fast alkali-proof corrosion resistance etc. is a series of excellent
Performance, and fabric has many advantages, such as wash and wear, stiffness is good, is widely used in the fields such as clothes, home textile.
Household textiles is one of big final products field of textile industry three, with the improvement of people's quality of life, comfort,
The functional and feature of environmental protection has become new requirement of the consumer to home textile articles.Market is used for the polyester filament of home textile production
Product based on conventional ordinary polyester product, have the defects that on feel, gloss and rear road difficulty of processing it is certain,
It is not able to satisfy the growing comfort of people, functional requirement.
The abnormal shapeization of fibre section can make the glossiness, bulkiness, hygroscopicity, anti-fluffing, pilling tendency, resistant of textile product
Property, stiffness, elasticity, feel etc. obtain different degrees of improvement, profiled filament take, household and fabrics for industrial use field
Inside obtain very extensive application.Common profiled filament has triangle, trilobal, multi-leaf-shaped, cross, doughnut etc.
Deng.
Profiled filament is using the profile spinneret for being specifically designed manufacture, the method being prepared through special spinning technique,
This is the method that domestic and international production profiled filament most generally uses, by spinneret guide hole and capillary processing technology and spinning
The improvement and optimization of technology can produce the profiled filament of Arbitrary Shape Cross Section, but profiled filament is due to the original of melt viscosity
Effect is expanded because extrusion can be generated, and product will appear that degree of profile is not high, cause fiber that the effect of design is not achieved.
The appearance of doughnut is bionics application as a result, cavity provides still air to improve the warming of fiber
Property, the surface area in unit volume is increased, to improve the bulkiness of fiber, makes fiber that there is warmth retention property.In hollow type
The kind of hollow fiber and its abundant, quickly grows, and raw material is from design terylene, polyamide fibre etc.；Holes on synthetic fibres develops to four from single hole
Hole, 12 holes, 24 holes etc.；Also triangle, quadrangle, quincunx etc. are developed to from circle in section.But it is general hollow short
The degree of hollowness of fiber is lower than 20%, and the degree of hollowness of tubular filament is lower than 10%, makes fiber quality, warming and water vapour permeability also not very
It is ideal, it is difficult to meet the requirement of functional clothing fabric development and batch production.
Summary of the invention
The purpose of the present invention is overcoming the problems, such as that the conformal effect of prior art preparation profiled filament is poor, a kind of side is provided
Shape hollow polyester fibre FDY and preparation method thereof, the present invention introduces a small amount of rigid structure segment in polyester molecule and increases
Polyester molecule chain rigidity is able to maintain the good characteristic of polyester ontology on the one hand since the content of rigid structure segment is less,
Another aspect polyester molecule chain rigidity increase can weaken extrusion swelling effect while reduce surface tension, and then prepare conformal
FDY, effect preferable square hollow polyester fiber.The present invention joined saturated fat acid metal salt in spinning melt, quite
In joined lubricant, pressure after filter when can effectively reduce spinning, and then effectively reduce outlet expansion, i.e. decrease extrusion swelling
Than making product that there is good conformal effect；Saturated fat acid metal salt can also be used as nucleating agent simultaneously, promote polyester fiber
Crystallization, increases the curing rate of fiber, further increases the conformal effect of fiber；In addition saturated fat acid metal salt is to polyester fibre
The not big destruction of structural regularity is tieed up, the excellent performance of polyester fiber is maintained, index of refraction is 1.49 foldings for being less than polyester
Light rate 1.52-1.54, the transparency final to product do not have an impact.
In order to achieve the above objectives, the technical solution adopted by the present invention are as follows:
A kind of FDY, square hollow polyester fiber preparation methods, according to square hollow polyester fiber FDY spinning technique,
Wherein spinning melt includes saturated fat acid metal salt and modified poly ester, the mass ratio of saturated fat acid metal salt and modified poly ester
For 0.0005-0.002:1；
The saturated fat acid metal salt refers to that carbon atom number is 12-22, fusing point is 100-180 DEG C and dynamic viscosity≤
The fatty acid metal salts of 1Pas, the strand of the modified poly ester include terephthalic acid (TPA) segment, ethylene glycol segment and rigidity
Structure segment；
The rigid structure segment be 2,6- naphthalenedicarboxylic acid segment, bisphenol-A segment, 1,4 cyclohexane dimethanol segment, 2,
2- biphenyl dicarboxylic acid segment, 4,4- oxydibenzoic acid segment, 2,4- biphenyl dicarboxylic acid segment, 3,4- biphenyl dicarboxylic acid segment,
4,4- biphenyl dicarboxylic acid segment or P-hydroxybenzoic acid segment；
The molar ratio of the rigid structure segment and terephthalic acid (TPA) segment is 0.02-0.05:1, the spinning melt
Die swell ratio is 1.21-1.32, and pressure is 82-123kg/cm after filter when spinning2, conventional filter when spinning in the prior art
Pressure is 110-140kg/cm afterwards2。
Die swell ratio test method of the invention are as follows: moved in a circle, taken around spinneret using high-speed motion picture camera
Dynamic image when melt is squeezed out from the spinneret orifice of spinneret is established 3-D graphic by three-dimensional simulation, is calculated micro- from spinneret
The ratio between the maximum cross-section area and the cross-sectional area of spinneret orifice of the melt that hole squeezes out are set to die swell ratio B, obtain primary reality
The extrusion swelling value B1 tested, continuously takes 50 groups of data to be averaged, and obtains final B value.
As a preferred technical scheme:
A kind of FDY, square hollow polyester fiber preparation methods as described above, spinning melt is through metering, extrusion, cold
But, oil, stretch, FDY, square hollow polyester fiber, FDY, the square hollow polyester fiber is made in thermal finalization and winding
Main spinning technology parameter are as follows:
Extrusion temperature: 285-300 DEG C；
Cooling temperature: 20-25 DEG C；
Network pressure: 0.20-0.30MPa；
One roller speed: 2200-2600m/min；
One roll temperature: 75-90 DEG C；
Two roller speeds: 3600-3900m/min；
Two roll temperatures: 115-135 DEG C；
Winding speed: 4000-4600m/min.
A kind of FDY, square hollow polyester fiber preparation methods as described above, section of the spinneret orifice on spinneret
Face shape is made of four cross section slots of the same size, and four rectangles constitute a square, and rectangle is transversal
The ratio between the long side in face and short side are all 2-7:1, and the ratio between two neighboring rectangle distance and rectangular short side are all 0.2-0.8:
1。
A kind of FDY, square hollow polyester fiber preparation methods as described above, the equal molecule of the number of the modified poly ester
Amount is 20000-28000.
A kind of FDY, square hollow polyester fiber preparation methods as described above, the preparation step of the spinning melt
It is as follows:
(1) binary acid binary alcohol esters are made in esterification；
Terephthalic acid (TPA), ethylene glycol and monomer containing rigid structure are made into slurry, catalyst, stabilizer and saturation is added
Fatty acid metal salts after mixing, carry out esterification, esterification compressive reaction in nitrogen atmosphere, moulding pressure is normal
Pressure -0.3MPa, the temperature of esterification are 250-260 DEG C, when the water quantity of distillate in esterification reach the 90% of theoretical value with
It was esterification terminal when upper；The monomer containing rigid structure be 2,6- naphthalenedicarboxylic acid, bisphenol-A two terephthalates,
1,4 cyclohexane dimethanol, 2,2- biphenyl dicarboxylic acid, 4,4- oxydibenzoic acid, 2,4- biphenyl dicarboxylic acid, 3,4- biphenyl diformazan
Acid, 4,4- biphenyl dicarboxylic acid or terephthalic acid (TPA) p-hydroxybenzoate；The terephthalic acid (TPA), ethylene glycol and contain rigid structure
Monomer molar ratio be 1:1.2-2.0:0.02-0.05；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
Staged pressure by normal pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 260-270 DEG C, reaction time 30-
50min；It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure and be less than
100Pa, reaction temperature are controlled at 275-285 DEG C, reaction time 50-90min, and spinning melt is made.
A kind of FDY, square hollow polyester fiber preparation methods as described above, the catalyst be antimony oxide,
Antimony glycol or antimony acetate, catalyst charge are the 0.01-0.05% of terephthalic acid (TPA) weight, and the stabilizer is tricresyl phosphate
Phenyl ester, trimethyl phosphate or Trimethyl phosphite, stabilizer additional amount is the 0.01-0.05% of terephthalic acid (TPA) weight, described
Saturated fat acid metal salt is aluminum stearate, magnesium stearate, calcium stearate, zinc stearate, zinc laurate or behenic acid calcium.
The present invention also provides a kind of FDY, square hollow polyester fiber, in FDY, the square hollow polyester fiber
Reciprocal of duty cycle is 15-20%, conformal to work well.
A kind of FDY, square hollow polyester fiber as described above, the monofilament of FDY, the square hollow polyester fiber is fine
Degree is 3.0-5.0dtex, and breaking strength >=3.8cN/dtex, elongation at break is 33.0 ± 3.0%；The square hollow polyester
Fiber FDY line density deviation ratio≤0.5%, breaking strength CV value≤4.0%, extension at break CV value≤8.0%, item are dry not
Even rate CV value≤2.0%.
Ideal design effect is generally unable to reach when preparing profiled filament using melt spinning method, this is mainly due to
Caused by two aspect reasons, extrusion swelling effect can be generated when one side high polymer molten passes through spinneret, it is on the other hand high poly-
The surface tension of object melt is larger, and polyester fondant is influenced by surface tension, compares " mellow and full " without corner angle, leads to special-shaped fibre
The conformal effect of dimension is poor.Polyester fondant from spinneret orifice squeeze out when cross sectional shape changing always, polyester fondant away from
Start extrusion swelling from the region in spinneret orifice outlet 2mm, extrusion swelling reaches most when exporting 2mm apart from spinneret orifice
Greatly, when being greater than 4mm apart from spinneret orifice outlet, the influence of extrusion swelling pair cross-section shape is eliminated, at this time the surface of polyester fondant
Tension starts to have an impact the cross sectional shape of polyester fondant.The present invention by polyester molecule introduce rigid structure segment,
The reduction that saturated fat acid metal salt realizes the decrease and surface tension of extrusion swelling effect is added in polyester fondant simultaneously, into
And prepare the preferable profiled filament of conformal effect.
The extrusion swelling of polyester fondant is as caused by flexible deformation effect or memory effect, when melt enters mouth mold, by
It is shunk in streamline, generates velocity gradient, i.e. stretcher strain in the flowing direction, if the residence time is short in mouth mold, have little time
Relaxation leads to extrusion swelling from contraction is generated after mould.The extrusion swelling of polyester fondant can also be caused by normal stress difference, melt
In mouth mold flow by shear-deformable, there are direct stress on perpendicular to shear direction, further cause extrusion swelling.When poly-
When introducing rigid structure segment in ester molecule chain, polyester molecule chain rigidity increases, and when polyester fondant enters spinneret orifice, gathers
The degree of compressibility of ester melt is reduced, and flexible deformation effect reduces, and normal stress difference reduces, when polyester fondant is squeezed from spinneret orifice
When out, memory effect weakens, so as to cause die swell ratio reduction.Saturated fat acid metal salt is added in polyester fondant, by
Refer to that carbon atom number is 12-22, fusing point is 100-180 DEG C and dynamic viscosity≤1Pas fat in saturated fat acid metal salt
Acid metal salt, molecular weight is much smaller than the molecular weight with polyester, and the compatibility of saturated fat acid metal salt and polyester is bad, because
This, polyester fondant surface can be moved to by being saturated fatty acid metal salts in the flow process of spinning melt；In addition, due to saturated fat
The dynamic viscosity of fat acid metal salt can be effective when melt flows in spinneret orifice much smaller than the viscosity with polyester fondant
Therefore the friction for improving the hot metal surface of polymer melt and spinneret orifice moves to polyester fondant surface saturated fatty acid
Metal salt can play outer lubricating action, and melt is made to will appear the type of flow of wall slippage in spinneret orifice, and the wall surface is sliding
Shifting refers to a kind of complete sliding form, refers to melt with the form flowing of approximate " plug flow ".Of the invention joined saturated fat
The spinning melt of fat acid metal salt is easier to flow out from spinneret orifice relative to common spinning melt, therefore the present invention can be real
The reduction of existing spinning pressure (pressure after the filter when spinning pressure in the present invention refers both to spinning), after spinning pressure reduces, spinning
Pressure and the pressure drop of spinneret outlet pressure also decrease, and then corresponding normal stress difference can also reduce, micro- in spinneret
Flowing is also reduced by by shear-deformable perpendicular to direct stress existing for shear direction in hole, and outlet expansion reduces, that is, is squeezed
It is swollen out than reducing, is conducive to the conformal effect for improving fiber.In addition, the saturated fat acid metal salt being added in the present invention can also
To promote modified polyester fiber crystallization as nucleating agent, the curing rate for increasing fiber becomes larger, and it is cold to further increase offer fiber
But conformal effect, the present invention are added same as the prior art in spinning pressure after saturated fat acid metal salt in polyester fondant
Under conditions of, additionally it is possible to it realizes further increasing for spinning speed, is advantageously implemented high speed and super high-speed spinning.
The surface tension of polyester fondant is formed since material surface molecule is acted on by unbalanced molecular separating force,
The surface tension of high polymer molten and the biquadratic of parachor are directly proportional, and parachor is each original in polymer unit structure
The adduction of son and group contribution constant, parachor have additive property, not the contribution constant of homoatomic and group to parachor
Difference, when introducing rigid structure segment in polyester molecule, since the parachor of rigid structure segment is much smaller than glycol chain
The parachor of section makes the surface of polyester tension of the segment containing rigid structure be less than the surface tension of conventional polyester.
The utility model has the advantages that
(1) Direct-spinning of PET Fiber method of the invention can effectively weaken extrusion swelling when polyester fondant is squeezed out from spinneret orifice
The die swell ratio of effect, modified poly ester melt is 1.21-1.32, much smaller than the die swell ratio 1.36- of general polyester fondant
1.50；
(2) it can reduce the surface of polyester fondant while Direct-spinning of PET Fiber method of the invention weakens extrusion swelling effect
Power, rigid structure segment parachor are less than the parachor of terephthalic acid (TPA) segment or ethylene glycol segment, specifically: 2,6- naphthalenes
Dioctyl phthalate segment is 10m smaller than terephthalic acid (TPA) segment5/2·KJ1/4/ mol, bisphenol-A segment are 51.4m smaller than ethylene glycol segment5/2·
KJ1/4/ mol, 1,4-CHDM segment are 78.2m smaller than ethylene glycol segment5/2·KJ1/4/ mol, 2,2- biphenyl dicarboxylic acid chains
Section is 0.7m smaller than terephthalic acid (TPA) segment5/2·KJ1/4/ mol, 4,4- oxydibenzoic acid segments are smaller than terephthalic acid (TPA) segment
31.4m5/2·KJ1/4/ mol, P-hydroxybenzoic acid segment are 32.3m smaller than ethylene glycol segment5/2·KJ1/4/ mol, 2,4- biphenyl two
Formic acid segment is 8.6m smaller than terephthalic acid (TPA) segment5/2·KJ1/4/ mol, 3,4- biphenyl dicarboxylic acid segments are than terephthalic acid (TPA) segment
Small 8.6m5/2·KJ1/4/ mol, 4,4- biphenyl dicarboxylic acid segments are 8.6m smaller than terephthalic acid (TPA) segment5/2·KJ1/4/mol；
(3) content of rigid structure segment is less in modified poly ester of the present invention, is able to maintain the good characteristic of polyester ontology；
(4) it can prepare that conformal effect is good, the ideal profiled filament of design effect using Direct-spinning of PET Fiber method of the invention；
(5) degree of hollowness (15-20%) of the doughnut prepared using Direct-spinning of PET Fiber method of the invention is higher than common side
The doughnut (10-15%) of method preparation；
(6) present invention joined saturated fat acid metal salt in spinning melt, is equivalent to and joined lubricant, can be effective
Pressure after filter when reducing spinning, and then effectively reduce outlet expansion, that is, weaken die swell ratio, makes product that there is good guarantor
Shape effect；Saturated fat acid metal salt can also be used as nucleating agent simultaneously, promote polyester fiber crystallization, increase the solidification speed of fiber
Degree, further increases the conformal effect of fiber；In addition saturated fat acid metal salt is not big to polyester fiber structures regularity
It destroys, maintains the excellent performance of polyester fiber, index of refraction is the 1.49 index of refraction 1.52-1.54 for being less than polyester, to product
The final transparency does not have an impact；
(7) it is to be realized by reducing spinning melt viscosity, and it is logical for reducing viscosity that the prior art, which improves spinning speed,
It crosses and increases temperature to realize, and increasing temperature can be such that polyester thermally decomposes, and reduce the mechanical property of polyester；And the present invention is logical
After crossing addition saturated fat acid metal salt, spinning melt is set to pass through wall slippage to improve spinning speed, it is not necessary to increase spinning group
The heating temperature of part avoids polyester from generating thermal decomposition, makes the molecular weight remained steady of polyester, advantageously ensures that the raising of fiber is fine
The mechanical property of dimension reduces the irregularity of fiber；
(8) after the present invention is by being added saturated fat acid metal salt, pressure after filter when can effectively reduce spinning makes spinning
The replacement cycle of component extends, and saves production cost.In addition, process of the spinning melt of the present invention through pipeline to filament spinning component
In, the pressure being subject in the duct can also reduce, and be conducive to the stability for improving polyester fondant, reduce polyester fondant and conveying
Thermal degradation in the process.
Detailed description of the invention
Fig. 1 is the schematic cross-section of the spinneret orifice of spinneret；
Fig. 2 is fiber cross section made from embodiment 2 and comparative example 1, and wherein bold portion is that the fiber of embodiment 2 is transversal
Face figure, dotted portion are the fiber cross section figure of comparative example 1；
Wherein, a- leaf is long, b- leaf width, c- pitch of holes.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
Terephthalic acid (TPA), ethylene glycol and 2,6-naphthalenedicarboxylic acid are made into slurry, terephthalic acid (TPA), ethylene glycol and 2,6- naphthalene two
The molar ratio of formic acid is 1:1.2:0.02, and antimony oxide, triphenyl phosphate and aluminum stearate is added after mixing, carries out ester
Change reaction, antimony oxide additional amount is the 0.01% of terephthalic acid (TPA) weight, and triphenyl phosphate additional amount is terephthalic acid (TPA)
The temperature of the 0.01% of weight, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.1MPa, esterification is
250 DEG C, be esterification terminal when the water quantity of distillate in esterification reaches the 90% of theoretical value；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 500Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 260 DEG C, reaction time 30min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 99Pa, reaction temperature control exists
275 DEG C, reaction time 50min, spinning melt is made.
Spinning melt obtained includes aluminum stearate and modified poly ester, and the mass ratio of aluminum stearate and modified poly ester is
The fusing point of 0.0005:1, aluminum stearate are 100 DEG C, and the number-average molecular weight of dynamic viscosity 0.27Pas, modified poly ester are
20000, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and 2,6-naphthalenedicarboxylic acid segment, 2,6- naphthalenes
The molar ratio of dioctyl phthalate segment and terephthalic acid (TPA) segment is 0.02:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 285 DEG C；
Cooling temperature: 20 DEG C；
Network pressure: 0.20MPa；
One roller speed: 2200m/min；
One roll temperature: 75 DEG C；
Two roller speeds: 3600m/min；
Two roll temperatures: 115 DEG C；
Winding speed: 4000m/min.
Wherein the cross sectional shape of the spinneret orifice on spinneret is made of four cross section slots of the same size, and four
A rectangle constitutes a square, and the ratio between the long side of rectangular cross section and short side are all 2:1, two neighboring rectangle distance
It is all 0.2:1 with the ratio between rectangular short side, the length of short side is 75um, and the die swell ratio of spinning melt is 1.32, spinning
When filter after pressure be 123kg/cm2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 15%, and conformal to work well, square hollow is poly-
The filament number that ester fiber is FDY is 3.0dtex, breaking strength 3.8cN/dtex, elongation at break 30%；Square hollow
FDY, polyester fiber line density deviation ratios are 0.5%, and breaking strength CV value is 4.0%, and extension at break CV value is 8.0%, item
Dry irregularity CV value is 2.0%.
Embodiment 2
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
By terephthalic acid (TPA), ethylene glycol and 4,4- biphenyl dicarboxylic acid is made into slurry, terephthalic acid (TPA), ethylene glycol and 4,4- connection
The molar ratio of phthalic acid is 1:1.8:0.046, and antimony acetate, Trimethyl phosphite and zinc stearate is added after mixing, into
Row esterification, antimony acetate additional amount are the 0.045% of terephthalic acid (TPA) weight, and Trimethyl phosphite additional amount is terephthaldehyde
The 0.045% of sour weight, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.24MPa, the temperature of esterification
It is 258 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 93% of theoretical value；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 481Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 268 DEG C, reaction time 32min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 92Pa, reaction temperature control exists
283 DEG C, reaction time 82min, spinning melt is made.
Spinning melt obtained includes zinc stearate and modified poly ester, and the mass ratio of zinc stearate and modified poly ester is
The fusing point of 0.0019:1, zinc stearate are 118 DEG C, and the number-average molecular weight of dynamic viscosity 0.27Pas, modified poly ester are
26000, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and 4,4- biphenyl dicarboxylic acid segment, and 4,4-
The molar ratio of biphenyl dicarboxylic acid segment and terephthalic acid (TPA) segment is 0.046:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 296 DEG C；
Cooling temperature: 24 DEG C；
Network pressure: 0.28MPa；
One roller speed: 2550m/min；
One roll temperature: 87 DEG C；
Two roller speeds: 3850m/min；
Two roll temperatures: 132 DEG C；
Winding speed: 4450m/min.
As shown in Figure 1, the cross sectional shape of the spinneret orifice on spinneret is by four cross section slots of the same size
It constitutes, four rectangles constitute a square, the long side (i.e. the long a of leaf, 560um) and short side (i.e. leaf width of rectangular cross section
B, 80um) the ratio between be all 7:1, two neighboring rectangle distance (i.e. pitch of holes c, 60um) and rectangular short side (i.e. leaf width b,
It the ratio between 80um) is all 0.75:1, the length of short side is 75um, and the die swell ratio of spinning melt is 1.23, after filter when spinning
Pressure is 90kg/cm2。
The degree of hollowness of final obtained FDY, square hollow polyester fiber is 19.49%, conformal to work well, it is rectangular in
Empty polyester fiber FDY filament numbers are 4.5dtex, breaking strength 3.95cN/dtex, elongation at break 34%；Side
Shape hollow polyester fibre FDY line density deviation ratios are 0.38%, and breaking strength CV value is 2.8%, and extension at break CV value is
6.0%, yarn unevenness CV value is 1.2%.
Comparative example 1
A kind of FDY, square hollow polyester fiber preparation methods use the conventional polyester that number-average molecular weight is 26000
FDY, square hollow polyester fiber is made in device for spinning and spinning technique same as Example 2, wherein the extrusion of spinning melt
It swells than being 1.38, pressure is 120kg/cm after filter when spinning2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 14.31%, much smaller than made from embodiment 2
The degree of hollowness (19.49%) of fiber, the filament number that square hollow polyester fiber is FDY are 4.8dtex, and breaking strength is
3.8cN/dtex, elongation at break 30%；FDY, square hollow polyester fiber line density deviation ratios are 0.42%, fracture
Intensity CV value is 3.5%, and extension at break CV value is 6.5%, and yarn unevenness CV value is 1.5%.
The comparison diagram of fiber cross section made from embodiment 2 and comparative example 1 is as shown in Fig. 2, wherein bold portion is to implement
The fiber cross section figure of example 2, dotted portion are the fiber cross section figure of comparative example 1, and comparison is it can be seen that fibre made from embodiment 2
The cross-sectional area of dimension is less than the cross-sectional area of fiber made from comparative example 1, while the cross section of fiber made from embodiment 2
Closer rectangular, the arc length of connecting line and radian are smaller between adjacent both sides, and the cross section of fiber made from comparative example 1 is close
Circular ring shape, the arc length of connecting line and radian are larger between adjacent both sides, illustrate the present invention by reducing the die swell ratio of melt
Effectively improve the conformal effect of fiber.
Embodiment 3
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
Two terephthalates of terephthalic acid (TPA), ethylene glycol and bisphenol-A are made into slurry, terephthalic acid (TPA), ethylene glycol
Molar ratio with two terephthalates of bisphenol-A is 1:1.3:0.025, and antimony oxide, triphenyl phosphate and tristearin is added
Sour aluminium after mixing, carries out esterification, and antimony oxide additional amount is the 0.015% of terephthalic acid (TPA) weight, tricresyl phosphate
Phenyl ester additional amount is the 0.015% of terephthalic acid (TPA) weight, and esterification compressive reaction in nitrogen atmosphere, moulding pressure is
0.12MPa, the temperature of esterification are 251 DEG C, are esterification when the water quantity of distillate in esterification reaches the 90% of theoretical value
Reaction end；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 495Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 262 DEG C, reaction time 35min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 98Pa, reaction temperature control exists
276 DEG C, reaction time 55min, spinning melt is made.
Spinning melt obtained includes aluminum stearate and modified poly ester, and the mass ratio of aluminum stearate and modified poly ester is
The fusing point of 0.001:1, aluminum stearate are 100 DEG C, and the number-average molecular weight of dynamic viscosity 0.27Pas, modified poly ester are
21000, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and bisphenol-A segment, bisphenol-A segment with it is right
The molar ratio of phthalic acid segment is 0.025:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 286 DEG C；
Cooling temperature: 20 DEG C；
Network pressure: 0.21MPa；
One roller speed: 2250m/min；
One roll temperature: 76 DEG C；
Two roller speeds: 3645m/min；
Two roll temperatures: 117 DEG C；
Winding speed: 4060m/min.
Wherein the cross sectional shape of the spinneret orifice on spinneret is made of four cross section slots of the same size, and four
A rectangle constitutes a square, and the ratio between the long side of rectangular cross section and short side are all 2.5:1, two neighboring rectangle away from
From being all 0.25:1 with the ratio between rectangular short side, the length of short side is 76um, and the die swell ratio of spinning melt is 1.31, is spun
Pressure is 118kg/cm after filter when silk2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 15.3%, conformal to work well, square hollow
The filament number that polyester fiber is FDY is 3.2dtex, breaking strength 3.82cN/dtex, elongation at break 30.5%；Side
Shape hollow polyester fibre FDY line density deviation ratios are 0.48%, and breaking strength CV value is 3.8%, and extension at break CV value is
7.6%, yarn unevenness CV value is 1.8%.
Embodiment 4
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
Terephthalic acid (TPA), ethylene glycol and 1,4-CHDM are made into slurry, terephthalic acid (TPA), ethylene glycol and Isosorbide-5-Nitrae-
The molar ratio of cyclohexanedimethanol is 1:1.4:0.03, and antimony oxide, triphenyl phosphate and magnesium stearate is added and is uniformly mixed
Afterwards, esterification is carried out, antimony oxide additional amount is the 0.02% of terephthalic acid (TPA) weight, and triphenyl phosphate additional amount is pair
The 0.02% of phthalic acid weight, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.14MPa, esterification
Temperature be 252 DEG C, when the water quantity of distillate in esterification reaches the 90% of theoretical value be esterification terminal；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 490Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 263 DEG C, reaction time 37min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 97Pa, reaction temperature control exists
278 DEG C, reaction time 59min, spinning melt is made.
Spinning melt obtained includes magnesium stearate and modified poly ester, and the mass ratio of magnesium stearate and modified poly ester is
The fusing point of 0.0012:1, magnesium stearate are 130 DEG C, and the number-average molecular weight of dynamic viscosity 0.35Pas, modified poly ester are
22000, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and 1,4-CHDM segment, and 1,
The molar ratio of 4- cyclohexanedimethanol segment and terephthalic acid (TPA) segment is 0.03:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 288 DEG C；
Cooling temperature: 21 DEG C；
Network pressure: 0.22MPa；
One roller speed: 2300m/min；
One roll temperature: 78 DEG C；
Two roller speeds: 3680m/min；
Two roll temperatures: 120 DEG C；
Winding speed: 4100m/min.
Wherein the cross sectional shape of the spinneret orifice on spinneret is made of four cross section slots of the same size, and four
A rectangle constitutes a square, and the ratio between the long side of rectangular cross section and short side are all 2.8:1, two neighboring rectangle away from
From being all 0.3:1 with the ratio between rectangular short side, the length of short side is 76um, and the die swell ratio of spinning melt is 1.30, is spun
Pressure is 113kg/cm after filter when silk2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 15.8%, conformal to work well, square hollow
The filament number that polyester fiber is FDY is 3.5dtex, breaking strength 3.84cN/dtex, elongation at break 31%；It is rectangular
Hollow polyester fibre FDY line density deviation ratios are 0.45%, and breaking strength CV value is 3.6%, and extension at break CV value is
7.2%, yarn unevenness CV value is 1.7%.
Embodiment 5
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
By terephthalic acid (TPA), ethylene glycol and 2,2- biphenyl dicarboxylic acid is made into slurry, terephthalic acid (TPA), ethylene glycol and 2,2- connection
The molar ratio of phthalic acid is 1:1.5:0.035, and antimony glycol, trimethyl phosphate and magnesium stearate is added after mixing, into
Row esterification, antimony glycol additional amount are the 0.025% of terephthalic acid (TPA) weight, and trimethyl phosphate additional amount is terephthaldehyde
The 0.025% of sour weight, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.16MPa, the temperature of esterification
It is 254 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 91% of theoretical value；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 488Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 264 DEG C, reaction time 40min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 96Pa, reaction temperature control exists
279 DEG C, reaction time 64min, spinning melt is made.
Spinning melt obtained includes magnesium stearate and modified poly ester, and the mass ratio of magnesium stearate and modified poly ester is
The fusing point of 0.0014:1, magnesium stearate are 130 DEG C, and the number-average molecular weight of dynamic viscosity 0.35Pas, modified poly ester are
23000, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and 2,2- biphenyl dicarboxylic acid segment, and 2,2-
The molar ratio of biphenyl dicarboxylic acid segment and terephthalic acid (TPA) segment is 0.035:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 290 DEG C；
Cooling temperature: 21 DEG C；
Network pressure: 0.23MPa；
One roller speed: 2350m/min；
One roll temperature: 80 DEG C；
Two roller speeds: 3710m/min；
Two roll temperatures: 122 DEG C；
Winding speed: 4150m/min.
Wherein the cross sectional shape of the spinneret orifice on spinneret is made of four cross section slots of the same size, and four
A rectangle constitutes a square, and the ratio between the long side of rectangular cross section and short side are all 3:1, two neighboring rectangle distance
It is all 0.4:1 with the ratio between rectangular short side, the length of short side is 77um, and the die swell ratio of spinning melt is 1.28, spinning
When filter after pressure be 109kg/cm2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 16.4%, conformal to work well, square hollow
The filament number that polyester fiber is FDY is 3.7dtex, breaking strength 3.85cN/dtex, elongation at break 31.8%；Side
Shape hollow polyester fibre FDY line density deviation ratios are 0.44%, and breaking strength CV value is 3.5%, and extension at break CV value is
7.0%, yarn unevenness CV value is 1.6%.
Embodiment 6
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
By terephthalic acid (TPA), ethylene glycol and 4,4- oxydibenzoic acid is made into slurry, terephthalic acid (TPA), ethylene glycol and 4,4-
The molar ratio of oxydibenzoic acid is 1:1.5:0.038, and antimony glycol, trimethyl phosphate and calcium stearate is added and is uniformly mixed
Afterwards, esterification is carried out, antimony glycol additional amount is the 0.03% of terephthalic acid (TPA) weight, and trimethyl phosphate additional amount is to benzene
The 0.03% of dioctyl phthalate weight, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.18MPa, esterification
Temperature is 255 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 91% of theoretical value；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 486Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 265 DEG C, reaction time 42min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 95Pa, reaction temperature control exists
280 DEG C, reaction time 68min, spinning melt is made.
Spinning melt obtained includes calcium stearate and modified poly ester, and the mass ratio of calcium stearate and modified poly ester is
The fusing point of 0.0015:1, calcium stearate are 150 DEG C, and the number-average molecular weight of dynamic viscosity 0.32Pas, modified poly ester are
24000, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and 4,4- oxydibenzoic acid segment, and 4,
The molar ratio of 4- oxydibenzoic acid segment and terephthalic acid (TPA) segment is 0.038:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 291 DEG C；
Cooling temperature: 22 DEG C；
Network pressure: 0.25MPa；
One roller speed: 2400m/min；
One roll temperature: 82 DEG C；
Two roller speeds: 3750m/min；
Two roll temperatures: 125 DEG C；
Winding speed: 4200m/min.
Wherein the cross sectional shape of the spinneret orifice on spinneret is made of four cross section slots of the same size, and four
A rectangle constitutes a square, and the ratio between the long side of rectangular cross section and short side are all 4:1, two neighboring rectangle distance
It is all 0.45:1 with the ratio between rectangular short side, the length of short side is 78um, and the die swell ratio of spinning melt is 1.26, spinning
When filter after pressure be 105kg/cm2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 16.8%, conformal to work well, square hollow
The filament number that polyester fiber is FDY is 3.7dtex, breaking strength 3.86cN/dtex, elongation at break 32.5%；Side
Shape hollow polyester fibre FDY line density deviation ratios are 0.43%, and breaking strength CV value is 3.3%, and extension at break CV value is
6.8%, yarn unevenness CV value is 1.5%.
Embodiment 7
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
By terephthalic acid (TPA), ethylene glycol and 2,4- biphenyl dicarboxylic acid is made into slurry, terephthalic acid (TPA), ethylene glycol and 2,4- connection
The molar ratio of phthalic acid is 1:1.6:0.04, and antimony glycol, trimethyl phosphate and calcium stearate is added after mixing, is carried out
Esterification, antimony glycol additional amount are the 0.035% of terephthalic acid (TPA) weight, and trimethyl phosphate additional amount is terephthalic acid (TPA)
The temperature of the 0.035% of weight, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.2MPa, esterification is
256 DEG C, be esterification terminal when the water quantity of distillate in esterification reaches the 92% of theoretical value；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 485Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 266 DEG C, reaction time 44min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 94Pa, reaction temperature control exists
281 DEG C, reaction time 73min, spinning melt is made.
Spinning melt obtained includes calcium stearate and modified poly ester, and the mass ratio of calcium stearate and modified poly ester is
The fusing point of 0.0016:1, calcium stearate are 150 DEG C, and the number-average molecular weight of dynamic viscosity 0.32Pas, modified poly ester are
24500, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and 2,4- biphenyl dicarboxylic acid segment, and 2,4-
The molar ratio of biphenyl dicarboxylic acid segment and terephthalic acid (TPA) segment is 0.04:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 293 DEG C；
Cooling temperature: 22 DEG C；
Network pressure: 0.26MPa；
One roller speed: 2450m/min；
One roll temperature: 85 DEG C；
Two roller speeds: 3800m/min；
Two roll temperatures: 128 DEG C；
Winding speed: 4280m/min.
Wherein the cross sectional shape of the spinneret orifice on spinneret is made of four cross section slots of the same size, and four
A rectangle constitutes a square, and the ratio between the long side of rectangular cross section and short side are all 5:1, two neighboring rectangle distance
It is all 0.5:1 with the ratio between rectangular short side, the length of short side is 80um, and the die swell ratio of spinning melt is 1.25, spinning
When filter after pressure be 100kg/cm2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 17.5%, conformal to work well, square hollow
The filament number that polyester fiber is FDY is 4.0dtex, breaking strength 3.89cN/dtex, elongation at break 32.6%；Side
Shape hollow polyester fibre FDY line density deviation ratios are 0.42%, and breaking strength CV value is 3.2%, and extension at break CV value is
6.5%, yarn unevenness CV value is 1.4%.
Embodiment 8
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
By terephthalic acid (TPA), ethylene glycol and 3,4- biphenyl dicarboxylic acid is made into slurry, terephthalic acid (TPA), ethylene glycol and 3,4- connection
The molar ratio of phthalic acid is 1:1.7:0.045, and antimony acetate, Trimethyl phosphite and zinc stearate is added after mixing, into
Row esterification, antimony acetate additional amount are the 0.04% of terephthalic acid (TPA) weight, and Trimethyl phosphite additional amount is terephthaldehyde
The 0.04% of sour weight, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.22MPa, the temperature of esterification
It is 257 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 92% of theoretical value；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 484Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 267 DEG C, reaction time 46min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 93Pa, reaction temperature control exists
282 DEG C, reaction time 77min, spinning melt is made.
Spinning melt obtained includes zinc stearate and modified poly ester, and the mass ratio of zinc stearate and modified poly ester is
The fusing point of 0.0018:1, zinc stearate are 118 DEG C, and the number-average molecular weight of dynamic viscosity 0.27Pas, modified poly ester are
25000, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and 3,4- biphenyl dicarboxylic acid segment, and 3,4-
The molar ratio of biphenyl dicarboxylic acid segment and terephthalic acid (TPA) segment is 0.045:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 295 DEG C；
Cooling temperature: 23 DEG C；
Network pressure: 0.27MPa；
One roller speed: 2500m/min；
One roll temperature: 86 DEG C；
Two roller speeds: 3820m/min；
Two roll temperatures: 130 DEG C；
Winding speed: 4330m/min.
Wherein the cross sectional shape of the spinneret orifice on spinneret is made of four cross section slots of the same size, and four
A rectangle constitutes a square, and the ratio between the long side of rectangular cross section and short side are all 6:1, two neighboring rectangle distance
It is all 0.6:1 with the ratio between rectangular short side, the length of short side is 80um, and the die swell ratio of spinning melt is 1.24, spinning
When filter after pressure be 95kg/cm2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 18.2%, conformal to work well, square hollow
The filament number that polyester fiber is FDY is 4.2dtex, breaking strength 3.92cN/dtex, elongation at break 32.7%；Side
Shape hollow polyester fibre FDY line density deviation ratios are 0.4%, and breaking strength CV value is 3.0%, and extension at break CV value is
6.2%, yarn unevenness CV value is 1.3%.
Embodiment 9
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
Terephthalic acid (TPA), ethylene glycol and terephthalic acid (TPA) p-hydroxybenzoate are made into slurry, terephthalic acid (TPA), second two
The molar ratio of pure and mild terephthalic acid (TPA) p-hydroxybenzoate is 1:1.9:0.048, and antimony acetate, Trimethyl phosphite and the moon is added
Cinnamic acid zinc after mixing, carries out esterification, and antimony acetate additional amount is the 0.05% of terephthalic acid (TPA) weight, phosphorous acid front three
Ester additional amount is the 0.05% of terephthalic acid (TPA) weight, and esterification compressive reaction in nitrogen atmosphere, moulding pressure is
0.26MPa, the temperature of esterification are 259 DEG C, are esterification when the water quantity of distillate in esterification reaches the 93% of theoretical value
Reaction end；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 480Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 269 DEG C, reaction time 48min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 91Pa, reaction temperature control exists
284 DEG C, reaction time 86min, spinning melt is made.
Spinning melt obtained includes zinc laurate and modified poly ester, and the mass ratio of zinc laurate and modified poly ester is
The fusing point of 0.002:1, zinc laurate are 130 DEG C, and the number-average molecular weight of dynamic viscosity 0.27Pas, modified poly ester are
27000, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and P-hydroxybenzoic acid segment, to hydroxyl
The molar ratio of benzoic acid segment and terephthalic acid (TPA) segment is 0.048:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 298 DEG C；
Cooling temperature: 25 DEG C；
Network pressure: 0.29MPa；
One roller speed: 2580m/min；
One roll temperature: 88 DEG C；
Two roller speeds: 3880m/min；
Two roll temperatures: 133 DEG C；
Winding speed: 4520m/min.
Wherein the cross sectional shape of the spinneret orifice on spinneret is made of four cross section slots of the same size, and four
A rectangle constitutes a square, and the ratio between the long side of rectangular cross section and short side are all 7:1, two neighboring rectangle distance
It is all 0.8:1 with the ratio between rectangular short side, the length of short side is 80um, and the die swell ratio of spinning melt is 1.22, spinning
When filter after pressure be 88kg/cm2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 19.5%, conformal to work well, square hollow
The filament number that polyester fiber is FDY is 4.8dtex, breaking strength 3.96cN/dtex, elongation at break 35%；It is rectangular
Hollow polyester fibre FDY line density deviation ratios are 0.36%, and breaking strength CV value is 2.6%, and extension at break CV value is
5.8%, yarn unevenness CV value is 1.0%.
Embodiment 10
A kind of FDY, square hollow polyester fiber preparation methods, prepare spinning melt, steps are as follows first:
(1) binary acid binary alcohol esters are made in esterification；
Terephthalic acid (TPA), ethylene glycol and 2,6-naphthalenedicarboxylic acid are made into slurry, terephthalic acid (TPA), ethylene glycol and 2,6- naphthalene two
The molar ratio of formic acid is 1:2.0:0.05, and antimony oxide, triphenyl phosphate and behenic acid calcium is added after mixing, carries out ester
Change reaction, antimony oxide additional amount is the 0.05% of terephthalic acid (TPA) weight, and triphenyl phosphate additional amount is terephthalic acid (TPA)
The temperature of the 0.05% of weight, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.3MPa, esterification is
260 DEG C, be esterification terminal when the water quantity of distillate in esterification reaches the 93% of theoretical value；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should
It is 478Pa that staged pressure, which is steadily evacuated to absolute pressure by normal pressure, and temperature control is at 270 DEG C, reaction time 50min；Then after
It is continuous to vacuumize, the polycondensation reaction of high vacuum stage of Fig is carried out, reaction pressure is made to be down to absolute pressure 90Pa, reaction temperature control exists
285 DEG C, reaction time 90min, spinning melt is made.
Spinning melt obtained includes behenic acid calcium and modified poly ester, and the mass ratio of behenic acid calcium and modified poly ester is
The fusing point of 0.002:1, behenic acid calcium are 110 DEG C, and the number-average molecular weight of dynamic viscosity 0.33Pas, modified poly ester are
28000, the strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and 2,6-naphthalenedicarboxylic acid segment, 2,6- naphthalenes
The molar ratio of dioctyl phthalate segment and terephthalic acid (TPA) segment is 0.05:1.
Finally, spinning melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind square hollow polyester is made
Fiber FDY, main spinning technology parameter are as follows:
Extrusion temperature: 300 DEG C；
Cooling temperature: 25 DEG C；
Network pressure: 0.30MPa；
One roller speed: 2600m/min；
One roll temperature: 90 DEG C；
Two roller speeds: 3900m/min；
Two roll temperatures: 135 DEG C；
Winding speed: 4600m/min.
Wherein the cross sectional shape of the spinneret orifice on spinneret is made of four cross section slots of the same size, and four
A rectangle constitutes a square, and the ratio between the long side of rectangular cross section and short side are all 7:1, two neighboring rectangle distance
It is all 0.8:1 with the ratio between rectangular short side, the length of short side is 80um, and the die swell ratio of spinning melt is 1.21, spinning
When filter after pressure be 82kg/cm2。
The degree of hollowness of final FDY, square hollow polyester fiber obtained is 20%, and conformal to work well, square hollow is poly-
The filament number that ester fiber is FDY is 5.0dtex, breaking strength 3.98cN/dtex, elongation at break 36%；In rectangular
Empty polyester fiber FDY line density deviation ratios are 0.32%, and breaking strength CV value is 2.5%, and extension at break CV value is
5.5%, yarn unevenness CV value is 0.8%.
Claims (8)
1. a kind of FDY, square hollow polyester fiber preparation methods, it is characterized in that: being spun according to square hollow polyester fiber FDY
Silk technique, wherein spinning melt includes saturated fat acid metal salt and modified poly ester, saturated fat acid metal salt and modified poly ester
Mass ratio be 0.0005-0.002:1；
The saturated fat acid metal salt refers to that carbon atom number is 12-22, fusing point is 100-180 DEG C and dynamic viscosity≤
Aluminum stearate, zinc stearate, zinc laurate or the behenic acid calcium of 1Pas, the strand of the modified poly ester includes terephthaldehyde
Sour segment, ethylene glycol segment and rigid structure segment；
The rigid structure segment is bisphenol-A segment, 1,4 cyclohexane dimethanol segment, 2,2- biphenyl dicarboxylic acid segment, 4,4-
Oxydibenzoic acid segment, 2,4- biphenyl dicarboxylic acid segment, 3,4- biphenyl dicarboxylic acid segment, 4,4- biphenyl dicarboxylic acid segment or right
Hydroxybenzoic acid segment；
The molar ratio of the rigid structure segment and terephthalic acid (TPA) segment is 0.02-0.048:1, the extrusion of the spinning melt
It swells than for 1.21-1.32, pressure is 82-123kg/cm after filter when spinning2；
Die swell ratio test method are as follows: moved in a circle using high-speed motion picture camera around spinneret, take melt from spinneret
Dynamic image of spinneret orifice when squeezing out, 3-D graphic is established by three-dimensional simulation, calculates the melt squeezed out from spinneret orifice
The maximum cross-section area and the ratio between the cross-sectional area of spinneret orifice be set to die swell ratio B, obtain the extrusion swelling once tested
Value B1 continuously takes 50 groups of data to be averaged, and obtains final B value.
2. FDY, a kind of square hollow polyester fiber preparation methods according to claim 1, which is characterized in that spinning
Melt through metering, extrusion, cooling, oil, stretch, thermal finalization and wind FDY, square hollow polyester fiber is made, it is described rectangular
Hollow polyester fibre FDY main spinning technology parameters are as follows:
Extrusion temperature: 285-300 DEG C；
Cooling temperature: 20-25 DEG C；
Network pressure: 0.20-0.30MPa；
One roller speed: 2200-2600m/min；
One roll temperature: 75-90 DEG C；
Two roller speeds: 3600-3900m/min；
Two roll temperatures: 115-135 DEG C；
Winding speed: 4000-4600m/min.
3. FDY, a kind of square hollow polyester fiber preparation methods according to claim 1, which is characterized in that spinneret
The cross sectional shape of spinneret orifice on plate is made of four cross section slots of the same size, and four rectangles constitute one
Square, the ratio between the long side of rectangular cross section and short side are all 2-7:1, two neighboring rectangle distance and rectangular short side
The ratio between be all 0.2-0.8:1.
4. FDY, a kind of square hollow polyester fiber preparation methods according to claim 1, which is characterized in that described
The number-average molecular weight of modified poly ester is 20000-28000.
5. FDY, a kind of square hollow polyester fiber preparation methods according to claim 1, which is characterized in that described
The preparation step of spinning melt is as follows:
(1) binary acid binary alcohol esters are made in esterification；
Terephthalic acid (TPA), ethylene glycol and monomer containing rigid structure are made into slurry, catalyst, stabilizer and saturated fat is added
Acid metal salt after mixing, carries out esterification, esterification compressive reaction in nitrogen atmosphere, and moulding pressure is normal pressure-
0.3MPa, the temperature of esterification is 250-260 DEG C, when the water quantity of distillate in esterification reaches 90% or more of theoretical value
For esterification terminal；The monomer containing rigid structure be two terephthalates of bisphenol-A, 1,4 cyclohexane dimethanol,
2,2- biphenyl dicarboxylic acid, 4,4- oxydibenzoic acid, 2,4- biphenyl dicarboxylic acid, 3,4- biphenyl dicarboxylic acid, 4,4- biphenyl dicarboxylic acid
Or terephthalic acid (TPA) p-hydroxybenzoate；The molar ratio of the terephthalic acid (TPA), ethylene glycol and the monomer containing rigid structure is
1:1.2-2.0:0.02-0.048；
(2) spinning melt is made in polycondensation reaction；
After esterification in step (1), start the polycondensation reaction of low vacuum stage, the stage under conditions of negative pressure
Pressure by normal pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 260-270 DEG C, reaction time 30-50min；So
After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure less than 100Pa, reaction temperature
Spinning melt is made at 275-285 DEG C, reaction time 50-90min in degree control.
6. FDY, a kind of square hollow polyester fiber preparation methods according to claim 5, which is characterized in that described
Catalyst is antimony oxide, antimony glycol or antimony acetate, and catalyst charge is the 0.01- of terephthalic acid (TPA) weight
0.05%, the stabilizer is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite, and stabilizer additional amount is terephthaldehyde
The 0.01-0.05% of sour weight.
7. using FDY, square hollow polyester fiber made from preparation method as claimed in any one of claims 1 to 6, feature
Be: the degree of hollowness of FDY, the square hollow polyester fiber is 15-20%, conformal to work well.
8. FDY, a kind of square hollow polyester fiber according to claim 7, which is characterized in that the square hollow is poly-
The filament number that ester fiber is FDY be 3.0-5.0dtex, breaking strength >=3.8cN/dtex, elongation at break be 33.0 ±
3.0%；Line density deviation ratio≤0.5% of FDY, the square hollow polyester fiber, breaking strength CV value≤4.0%, fracture
Extend CV value≤8.0%, yarn unevenness CV value≤2.0%.
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