CN108130605B - A kind of polyester Wool-Like abnormal contraction composite filament and preparation method thereof - Google Patents

A kind of polyester Wool-Like abnormal contraction composite filament and preparation method thereof Download PDF

Info

Publication number
CN108130605B
CN108130605B CN201711340316.5A CN201711340316A CN108130605B CN 108130605 B CN108130605 B CN 108130605B CN 201711340316 A CN201711340316 A CN 201711340316A CN 108130605 B CN108130605 B CN 108130605B
Authority
CN
China
Prior art keywords
modified poly
poly ester
spinneret orifice
spinneret
composite filament
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201711340316.5A
Other languages
Chinese (zh)
Other versions
CN108130605A (en
Inventor
张元华
丁竹君
张学东
沈建根
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Hengli Chemical Fiber Co Ltd
Original Assignee
Jiangsu Hengli Chemical Fiber Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Hengli Chemical Fiber Co Ltd filed Critical Jiangsu Hengli Chemical Fiber Co Ltd
Priority to CN201711340316.5A priority Critical patent/CN108130605B/en
Publication of CN108130605A publication Critical patent/CN108130605A/en
Application granted granted Critical
Publication of CN108130605B publication Critical patent/CN108130605B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02—Heat treatment
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/08—Melt spinning methods
    • D01D5/098—Melt spinning methods with simultaneous stretching
    • 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
    • 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
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
    • D02G1/02—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Artificial Filaments (AREA)

Abstract

The present invention relates to a kind of polyester Wool-Like abnormal contraction composite filaments and preparation method thereof, modified poly ester POY and FDY is made respectively first, then by POY and FDY compound obtained polyester Wool-Like abnormal contraction composite filament, the color difference Δ E of composite filament obtained is less than 0.200, the a branch of POY squeezed out through same spinneret contains diesis shape monofilament and trilobal monofilament in FDY simultaneously, it include branched dihydric alcohol segment, the structural formula of branched dihydric alcohol in the strand of modified poly ester are as follows:In formula, R1And R2The straight-chain alkyl-sub for being 1~3 for carbon atom number, R3The alkyl for being 1~5 for carbon atom number, R4The alkyl for being 2~5 for carbon atom number, the matt agent dispersed in modified poly ester are the mixture of unformed titanium dioxide and amorphous silica or calcium carbonate and amorphous silica.The method of the present invention advantages of simple, composite filament obtained have good fluffy and moisture absorbing and sweat releasing performance.

Description

A kind of polyester Wool-Like abnormal contraction composite filament and preparation method thereof
Technical field
The invention belongs to fiber preparation field, it is related to a kind of polyester Wool-Like abnormal contraction composite filament and preparation method thereof.
Background technique
Polyethylene terephthalate (PET fiber or polyester fiber) fiber since the advent of the world, due to having fracture strong Degree is high, elasticity modulus is high, resilience is moderate, thermal finalization is excellent, heat-resisting light resistance is good and a system such as acid-fast alkali-proof corrosion resistance Column excellent performance is widely used in the fields such as clothes and home textile.
As the development of modern textile technology and people's living standard are continuously improved, people are to taking, decorate and industrial Yield, performance and the quality of chemical fibre used by textile are put forward higher requirements, and therefore, in recent years, researcher causes Power is in the research and development of the new varieties of chemical fibre, to meet people to the market demand of the fiber with high added value.PET is fine Strong durable and wash and wear is tieed up, but its sucting wet air permeability is poor, affects the sense comfortable and easy to wear of fabric, therefore improve fabric Fluffy and sucting wet air permeability has a very important significance.
Profiled filament is made of spinning melt spins after the spinneret orifice with certain geometrical shape squeezes out with special The chemical fibre of cross sectional shape and function.The cross sectional shape of fiber affects the performance of yarn and fabric, using with not similar shape The composite spinneret of shape and the spinneret orifice of size can spin out the profiled filament with different cross section shape, the material of fiber with Shape feature influences the performance of fiber, and the arrangement of fiber and fiber in the yarn influences the performance of yarn, and yarn and yarn are being knitted Arrangement in object influences the performance of fabric, thus the shape feature of fiber is the essence for influencing yarn and fabric property.With not The improvement played with the fiber of cross sectional shape for yarn and fabric is different, profiled filament class textile research side Also there is also some difficult and deficiencies in face, are that solution is existing different with the double profiled filaments of plate or with the more double profiled filaments of plate in recent years The insufficient important means of shape fiber, meets people to profiled filament class textile at the advantages of capable of integrating two kinds of profiled filaments The demand of high quality and functional diversities.Although however researcher to the double profiled filament of same plate or with the more double profiled filaments of plate into A large amount of research is gone, but difficult in actual production with the double profiled filaments of plate or with the more double profiled filaments of plate.Due to Polyester fondant is non-newtonian fluid, is viscoelastic fluid, and while making stickiness flowing in spinneret orifice, elastic shape will occur Become, form certain pressure, therefore, polyester fondant, which goes out after spinneret orifice, can generate certain pressure drop, the shape of spinneret orifice, big Small, length and mutual relationship can all have a huge impact its pressure drop, and existing research generally only takes into account The shape of spinneret orifice is identical or cross-sectional area is equal, and shape, size and the mutual influence of length are without reference to this The pressure drop that sample will result in when polyester fondant is flowed out from the spinneret orifice of different shapes of same spinneret is inconsistent, so that section There is difference in extruded velocity between different fibers, therefore either POY or FDY can all occur that fiber number is irregular, intensity Not phenomena such as uniform uneven dyeing, going on smoothly for fibre spinning processing is influenced.
Therefore, study a kind of fiber with good bulkiness and moisture absorbing and sweat releasing performance for capableing of smoothly spinning processing at For current urgent problem to be solved.
Summary of the invention
The purpose of the invention is to overcome the prior art cannot smoothly spinning process to obtain have good bulkiness and The problem of fiber of moisture absorbing and sweat releasing performance, provide it is a kind of be capable of smoothly spinning processing there is good fluffy and moisture absorbing and sweat releasing property The polyester Wool-Like abnormal contraction composite filament and preparation method thereof of energy.The introducing of branched dihydric alcohol in modified poly ester of the present invention, Reduce the cyclic oligomer generated in polyester side reaction；Using the spinneret orifice for being provided with two kinds of special shapes and two kinds spray The size of the microcell length of wire hole, cross-sectional area and section girth has the composite spinneret of certain connection, ensure that Spinning smoothly stable progress, contains diesis shape monofilament and trilobal list simultaneously from the mass of fibers that same spinneret squeezes out Silk, the cross sectional shape of monofilament influence its performance, and the cross sectional shape of monofilament influences its performance, and diesis shape fiber is along fiber axis side There is groove to the section of the groove for having tubulose, i.e. fiber, provide pipeline for the migration of moisture, fabric as made from it can be made to produce Raw wicking, wicking is that extensive hygroscopic effect between fiber is betided on the basis of wet fabric, so that fabric With good moisture absorption sweat discharging functions, trefoil fiber is since section is in trilobal, so that obvolvent is loose between monofilament, gas permeability It is good.Therefore when diesis shape fiber and trefoil fiber are combined, due to the fibre of diesis shape fiber and trefoil fiber It being had differences between degree, and the voidage of diesis shape fiber is big, trefoil fiber is easy to be embedded in the groove of diesis shape fiber, Reduce the voidage of fiber, so that combining fabric obtained by the two not only has good moisture absorption sweat discharging functions, it can The moisture of skin is discharged rapidly, also there is good bulkiness, keeps fabric dress ventilative without the bored sense of heat；The addition of matt agent, makes Fiber is more nearly the texture of natural cotton, the performance with better moisture absorbing and sweat releasing.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of polyester Wool-Like abnormal contraction composite filament, polyester Wool-Like abnormal contraction composite filament are modified poly ester POY and change The composite filament of property polyester FDY；
Contain diesis shape list simultaneously in a branch of modified poly ester POY or modified poly ester FDY that same spinneret squeezes out Silk and trilobal monofilament；
The strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and branched dihydric alcohol segment, band The structural formula of the dihydric alcohol of branch is as follows:
Figure GDA0001618979150000021
In formula, R1And R2It is each independently selected from the straight-chain alkyl-sub that carbon atom number is 1~3, R3It is 1 selected from carbon atom number ~5 alkyl, R4The alkyl for being 2~5 selected from carbon atom number, the purpose that carbon atom number limits: due to introducing branch in dihydric alcohol Chain structure and backbone can be such that the electronegativity of alkoxy portion weakens, and the carbon atom number of branched structure is too small, to alkoxy Partial electronegativity influence is small, has little significance to the generation for reducing cyclic oligomer；The carbon atom number of branched structure is excessive, meeting Intermolecular entanglement is generated, the distribution of molecular weight is had an impact, the principle that the present invention reduces cyclic oligomer is specific as follows:
In organic compound, the angle between two chemical bonds that intramolecular atom is formed is known as bond angle, and bond angle is usually used Degree indicates that the electronegativity of central atom and coordination atom, will affect the bond angle of molecule in organic compound molecule.When with center When the electronegativity of the coordination atom of atomistic binding increases, the enhancing of coordination atom electron-withdrawing ability, bond electron pair will be to ligand Direction is mobile, farther out from central atom, makes between key pair because that repulsion reduces is close to each other, so that bond angle also reduces therewith, on the contrary, When the electronegativity for the coordination atom being bonded with central atom reduces, coordination atom electron donation enhancing, bond electron pair will It is mobile to central atom direction, it is closer from central atom, make to be located remotely from each other between key pair because repulsion increases, so that bond angle is also therewith Increase；
According to Pauling Electronegativity, the electronegativity of C, H and O atom is respectively 2.55,2.20 and 3.44, and according to Valence electron balancing energy is theoretical, and the calculation formula of Group Electronegativity is shown below:
Figure GDA0001618979150000031
In formula, xiFor the electronegativity of i atom neutral atom before bonding, NVe, iFor valence electron number in i atom, niFor i The number of atom in the molecule.It is main for the calculating step of more complex Group Electronegativity are as follows: to calculate simple group first Electronegativity, then regard simple group as electronegativity that quasiatom calculates more complex group again, such successive iteration, finally Obtain the electronegativity of Targeting groups.It should be noted that when calculating the electronegativity of quasiatom, base (for example, group- Base of OH is O atom) in the valence electron of non-bonding regard the valence electron of quasiatom as；
C atom can be with the O atom knot of hydroxyl in dihydric alcohol after the C-O key fracture of carboxyl in terephthalic acid (TPA) in the present invention The new C-O key formed in ester group is closed, the C atom key C-C formed and the chemical bond newly formed on the C atom and phenyl ring in ester group Bond angle between C-O is denoted as α, and the change of bond angle α will affect annulation, and when α is less than 109 °, molecule is easy to cyclic, and with The increase of α, the probability of molecule cyclization can decline.Present invention introduces branched dihydric alcohol, structural formula, should as shown in above formula Diol structure can be such that the electronegativity of its alkoxy portion weakens due to introducing branched structure and backbone, pass through group electricity The calculation formula of negativity can also obtain the electronegativity for the group being connected in the diol structure with carbonyl in diacid 2.59~2.79 Between, and the group-OCH being connected in ethylene glycol with carbonyl in diacid2CH2Electronegativity be 3.04, thus its alkoxy compares second - OCH in glycol2CH2There is stronger electron, so that the bond electron pair on the chemical bond C-O key newly formed Will be mobile to center C atomic orientation, it is closer from central atom, make to be located remotely from each other between key pair because repulsion increases, so that key Angle α is greater than 109 °, and the probability for generating linear polymer increases, to reduce the generation of cyclic oligomer；
It is dispersed with matt agent in modified poly ester, matt agent is the mixed of unformed titanium dioxide and unformed silica Close object, or the mixture for calcium carbonate and unformed silica；
Pure PET fiber, since the glossiness on surface is very high, usually translucent body, the strong and weak of gloss both depend on table Face reflected light, but it is related with transmitted light, while the gloss of fiber is also by fiber surface state, fiber cross-sectional shapes and fiber The influence of the factors such as portion's structure, such as the fiber that macromolecular orientation degree is good, internal structure is more uniform, the reflective light intensity of fiber, light Pool is bright, therefore, can by addition inorganic particulate delustring or by adjusting fiber cross-sectional shapes and surface texture etc. come pair The gloss of fiber is regulated and controled.In order to make the gloss of PET fiber close to the gloss of cotton fiber, delustring can be added in the course of the polymerization process Agent, common PET delustrant are the Detitanium-ore-types of titanium dioxide, in order to reduce titanium dioxide anatase crystal to polyester light The influence in pool, using the mixture or calcium carbonate of unformed titanium dioxide and unformed silica and unformed two The mixture of silica is inorganic matt particle, and inorganic particulate is dispersed in PET, and fiber is made to be more nearly natural cotton Texture.
The color difference Δ E of polyester Wool-Like abnormal contraction composite filament is less than 0.200.
As a preferred technical scheme:
A kind of polyester Wool-Like abnormal contraction composite filament as described above, the fiber number of the diesis shape monofilament is 0.7~ 0.9dtex, the fiber number of the trilobal monofilament are 0.90~1.1dtex；
The bending stiffness of the diesis shape monofilament is 0.78 × 10-5~0.90 × 10-5cN·cm2, the trilobal list The bending stiffness of silk is 0.79 × 10-5~0.96 × 10-5cN·cm2；
Modified poly ester POY and modified poly ester FDY the ratio between fiber numbers are 1 in the polyester Wool-Like abnormal contraction composite filament ~1.5:1；
The fiber number of the polyester Wool-Like abnormal contraction composite filament be 150~300dtex, breaking strength >=2.1cN/dtex, Elongation at break is 15.0 ± 2.0%, and crimp contraction is 5.50 ± 3.0%, and internet pricing is 90 ± 5/m, line density deviation Rate≤2.0%, breaking strength CV value≤7.0%, extension at break CV value≤8.0%, crimp contraction coefficient of variation CV value≤ 8.0%, boiling water shrinkage is 5.0 ± 1.0%, and oil content is 1.0 ± 0.2%, glossiness<50%, capillary parameter>=0.15.Often The capillary parameter for advising fiber is 0.08~0.12, and the capillary parameter that fiber is made in the present invention is apparently higher than conventional products, therefore makes The moisture absorption sweat discharging functions of the fiber obtained achieve significant progress compared with the prior art.
A kind of polyester Wool-Like abnormal contraction composite filament as described above, the content of cyclic oligomer in the modified poly ester≤ 0.6wt%, the amount of cyclic oligomer is 1.5~2.1wt% in polyester made from the prior art, and the present invention is compared with the existing technology Significantly reduce the production quantity of cyclic oligomer；
The number-average molecular weight 20000~27000 of the modified poly ester, molecular weight distributing index are 1.8~2.2, modified poly- The molecular weight of ester is higher, and molecular weight distribution is relatively narrow, can satisfy the demand of spinning processing, and it is excellent to be conducive to processability Fiber；
The molar content of branched dihydric alcohol segment is the 3 of terephthalic acid (TPA) segment molar content in the modified poly ester ~5%；
The branched dihydric alcohol is 2- Ethyl-2-Methyl -1,3- propylene glycol, 2,2- diethyl -1,3- propylene glycol, 2- Butyl -2- ethyl -1,3- propylene glycol, 3,3- diethyl -1,5- pentanediol, 4,4- diethyl -1,7- heptandiol, 4,4- bis- (1, - Methylethyl) -1,7- heptandiol, 3,3- dipropyl -1,5- pentanediol, 4,4- dipropyl -1,7- heptandiol, 4- methyl -4- (1, 1- dimethyl ethyl) -1,7- heptandiol, 3- methyl -3- amyl -1,6-HD or 3,3- diamyl -1,5- pentanediol.
A kind of polyester Wool-Like abnormal contraction composite filament as described above, the modified poly ester the preparation method comprises the following steps: will be to benzene Dioctyl phthalate, ethylene glycol and the branched dihydric alcohol successively carry out esterification after mixing and polycondensation reaction is modified Polyester；Specific step is as follows:
(1) esterification；
Terephthalic acid (TPA), ethylene glycol and the branched dihydric alcohol are made into slurry, catalyst, delustering agent and steady is added Determine agent after mixing, pressurization carries out esterification in nitrogen atmosphere, and moulding pressure is normal pressure~0.3MPa, esterification Temperature is 250~260 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches 90% or more of theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure 30~ Absolute pressure 500Pa being steadily evacuated to by normal pressure in 50min hereinafter, reaction temperature is 260~270 DEG C, the reaction time is 30~ 50min then proceedes to vacuumize, and carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure For 100Pa hereinafter, reaction temperature is 275~285 DEG C, the reaction time is 50~90min, and modified poly ester is made.
A kind of polyester Wool-Like abnormal contraction composite filament as described above, in step (1), terephthalic acid (TPA), ethylene glycol and institute The molar ratio for stating branched dihydric alcohol is 1:1.2~2.0:0.03~0.06, and the additional amount of the catalyst is terephthaldehyde The 0.01~0.05% of sour weight, the additional amount of the delustering agent are the 0.20~0.25% of terephthalic acid (TPA) weight, described steady The additional amount for determining agent is the 0.01~0.05% of terephthalic acid (TPA) weight；
The catalyst is antimony oxide, antimony glycol or antimony acetate, and the delustering agent is titanium dioxide, the stabilization Agent is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite.
A kind of polyester Wool-Like abnormal contraction composite filament as described above, content of the matt agent in modified poly ester are 1.0~1.5wt%, the content of unformed silica is 13~50wt% in the matt agent.
The present invention also provides a kind of method of polyester Wool-Like abnormal contraction composite filament as described above is prepared, by spinning melt It is squeezed out through metering, composite spinneret, is cooling, oiled and wound, being made modified poly ester POY；Spinning melt is measured, is compound Spinneret squeezes out, cools down, oils, stretching, thermal finalization and winding, is made modified poly ester FDY；By modified poly ester POY and change Property polyester FDY through plying network, heating stretchings, false twisting, thermal finalization and coiling and molding, the obtained different contraction of polyester Wool-Like is compound Silk；
The spinning melt includes the modified poly ester and the matt agent；
Diesis shape spinneret orifice and trilobal spinneret orifice, the diesis shape spinneret are equipped on the composite spinneret simultaneously The microcell length ratio of hole and trilobal spinneret orifice is equal to the ratio between the equivalent diameter of diesis shape spinneret orifice and trilobal spinneret orifice With the product of COEFFICIENT K, the equivalent diameter is the cross-sectional area of spinneret orifice and the ratio of section girth, and the COEFFICIENT K takes Being worth range is 0.97~1.03.
As a preferred technical scheme:
The microcell length of method as described above, the diesis shape spinneret orifice or trilobal spinneret orifice be 0.50~ The equivalent diameter of 1.44mm, the diesis shape spinneret orifice or trilobal spinneret orifice is 0.25~0.36mm；
All spinneret orifices concentric arrays on spinneret, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located at same On heart circle, the concentric circles is equidistant concentric circles, and the spinneret orifice on same annulus equidistantly arranges.
Method as described above contains diesis shape spinneret orifice and trilobal spinneret orifice, same circle on same annulus simultaneously Diesis shape spinneret orifice and the quantity ratio of trilobal spinneret orifice or the quantity of trilobal spinneret orifice and diesis shape spinneret orifice on ring Than for 3~5:2.
Method as described above, described modified poly ester POY main spinning technology parameters are as follows:
Spinning temperature: 280~290 DEG C；
Cooling temperature: 18~22 DEG C；
Winding speed: 3200~3600m/min；
Described modified poly ester FDY main spinning technology parameters are as follows:
Spinning temperature: 280~290 DEG C；
Cooling temperature: 20~25 DEG C；
Network pressure: 0.20~0.30MPa；
One roller speed: 2200~2600m/min；
One roll temperature: 75~85 DEG C；
Two roller speeds: 3650~3850m/min；
Two roll temperatures: 115~135 DEG C；
Winding speed: 3600~3800m/min；
The main spinning technology parameter of the polyester Wool-Like abnormal contraction composite filament is as follows:
Spin speed: 400~800m/min；
Overfeed rate of setting: 3.5~5.5%；
Winding overfeed rate: 2.5~5.0%；
T1:180~220 DEG C；
T2:150~180 DEG C；
DR:1.6~1.8；
D/Y:1.6~2.0；
Network pressure: 0.05~0.3MPa.
Invention mechanism:
Polyester fondant is non-newtonian fluid, is viscoelastic fluid, while making stickiness flowing in spinneret orifice, will be occurred Elastic deformation, and elastically-deformable presence is unstable one of the key factor of spinning.The microcell length of spinneret orifice and cross section Perimeter and spinneret orifice cross-sectional area etc. to elasticity in melt can storage and relaxation degree have a significant impact, the present invention is logical It crosses and the microcell length of two kinds of spinneret orifices, cross-sectional area and section girth on same spinneret is set and by two kinds of spinneret orifices Size establishes certain connection, realizes the relaxation of melt elasticity energy, so that its pressure during by different spinneret orifices Power drop is identical, melt is reduced in the pressure drop and extruding in exit, to ensure that melt spinning smoothly steadily carries out.
When polyester fondant passes through the spinneret orifice of spinneret, the calculation formula of melt pressure drop is as follows:
Figure GDA0001618979150000071
In formula, Δ P is that the pressure of melt drops, and is spinneret orifice inner wall area in S, value be equal to the microcell length of spinneret orifice with The product of the section girth of spinneret orifice, SIt cutsFor the cross-sectional area of spinneret orifice, τ is the viscous fluid shear stress of material.
For the polyester fondant by variform spinneret orifice A and spinneret orifice B on same spinneret, to make melt never It is consistent with the speed squeezed out in spinneret orifice or difference is smaller, it is necessary to assure its pressure drop during by different spinneret orifices It is identical or difference in a certain range, i.e. Δ PA=K Δ PB, wherein therefore COEFFICIENT K=0.97~1.03 can derive different sprays The microcell length of wire hole and the perimeter of its spinneret orifice cross section and the relationship of spinneret orifice cross-sectional area, it may be assumed that
Figure GDA0001618979150000081
In formula, D is the microcell length of spinneret orifice, and S is the cross-sectional area of spinneret orifice, and L is the week of the cross section of spinneret orifice Long, B is the equivalent diameter of spinneret orifice.
Spinneret is arranged in the present invention in such a way, realize from same spinneret and meanwhile squeeze out diesis shape monofilament and Trilobal monofilament, the cross sectional shape of monofilament influence its performance, and diesis shape fiber has the groove of tubulose along fiber axis direction, i.e., There is groove in the section of fiber, provides pipeline for the migration of moisture, and fabric as made from it can be made to generate wicking, and wicking is Extensive hygroscopic effect between fiber is betided on the basis of wet fabric, so that fabric has good moisture absorbing and sweat releasing Function, trefoil fiber is since section is in trilobal, so that obvolvent is loose between monofilament, good permeability.Therefore, diesis shape fiber When being combined with trefoil fiber, since the fiber number of diesis shape fiber and trefoil fiber has differences, and diesis The voidage of shape fiber is big, and trefoil fiber is easy to be embedded in the voidage for reducing fiber in the groove of diesis shape fiber, from And making fabric as made from it not only has good moisture absorption sweat discharging functions, can discharge rapidly the moisture of skin, also has good Good bulkiness keeps fabric dress ventilative without the bored sense of heat.
The utility model has the advantages that
(1) preparation method of a kind of polyester Wool-Like abnormal contraction composite filament of the invention, by being arranged on same spinneret The size of two kinds of spinneret orifices is simultaneously established certain connection by microcell length, cross-sectional area and the section girth of two kinds of spinneret orifices System ensure that pressure drop of polyester fondant during by different spinneret orifices is essentially identical, so that melt is from spinneret Extruded velocity in hole is almost the same, to ensure that its spinning smoothly steadily carries out；
(2) preparation method of a kind of polyester Wool-Like abnormal contraction composite filament of the invention, using unformed titanium dioxide It is inorganic matt particle with the mixture or calcium carbonate of unformed silica and the mixture of unformed silica, Inorganic particulate is dispersed in PET, and fiber is made to be more nearly the texture of natural cotton, the property with better moisture absorbing and sweat releasing Energy；
(3) preparation method of a kind of polyester Wool-Like abnormal contraction composite filament of the invention, by being introduced in modified poly ester Branched dihydric alcohol, changes the bond angle of polyester molecule, to significantly reduce cyclic oligomer in process of polyester synthesizing It generates；
(4) a kind of polyester Wool-Like abnormal contraction composite filament of the invention, preparation flow advantages of simple, polyester obtained imitate hair Type abnormal contraction composite filament has good fluffy and moisture absorbing and sweat releasing performance, has fabulous promotional value.
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 preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) esterification；Terephthalic acid (TPA), ethylene glycol and Ethyl-2-Methyl -1 2- for being 1:1.2:0.03 by molar ratio, 3-propanediol is made into slurry, and antimony oxide, titanium dioxide and triphenyl phosphate is added after mixing, adds in nitrogen atmosphere Pressure carries out esterification, and moulding pressure is normal pressure, and the temperature of esterification is 250 DEG C, when the water quantity of distillate in esterification reaches To theoretical value 90% when be esterification terminal, wherein the additional amount of antimony oxide is terephthalic acid (TPA) weight 0.01%, the additional amount of titanium dioxide is the 0.20% of terephthalic acid (TPA) weight, and the additional amount of triphenyl phosphate is terephthaldehyde The 0.05% of sour weight, wherein 2- Ethyl-2-Methyl -1,3-PD structural formula is as follows:
Figure GDA0001618979150000091
(b) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 500Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 30min, and reaction temperature is 260 DEG C, reaction time 40min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is further reduced to absolute pressure 100Pa, instead Answering temperature is 275 DEG C, reaction time 70min, and modified poly ester is made.Wherein the strand of modified poly ester includes terephthalic acid (TPA) Segment, ethylene glycol segment and 2- Ethyl-2-Methyl -1,3-PD segment, the content of cyclic oligomer is in modified poly ester 0.6wt%, number-average molecular weight 20000, molecular weight distributing index 2.0,2- Ethyl-2-Methyl -1,3- the third two in modified poly ester The molar content of alcohol segment is the 3% of terephthalic acid (TPA) segment molar content；
(1.2) disperse matt agent in modified poly ester, matt agent is unformed titanium dioxide and unformed silica Mixture, wherein content of the matt agent in modified poly ester is 1.0wt%, the content of unformed silica in matt agent For 13wt%；
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter are as follows: spinning temperature is 280 DEG C；Cooling temperature is 22 DEG C；Winding speed is 3600m/min, wherein together Contain diesis shape monofilament and trilobal monofilament, diesis shape list simultaneously in a branch of modified poly ester POY that one spinneret squeezes out The fiber number of silk is 0.81dtex, and bending stiffness is 0.82 × 10-5cN·cm2, the fiber number of trilobal monofilament is 1.01dtex, bending Rigidity is 0.96 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 280 DEG C；Cooling temperature is 22 DEG C；Network pressure is 0.20MPa；One roller speed is 2300m/min；One roll temperature is 83 DEG C；Two roller speeds are 3750m/min；Two roll temperatures are 115 ℃；Winding speed is 3600m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.8dtex, and bending stiffness is 0.67 × 10-5cN·cm2, three The fiber number of leaf monofilament is 1.0dtex, and bending stiffness is 0.86 × 10-5cN·cm2,；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 0.97, and the microcell length of diesis shape spinneret orifice is 0.85mm, three The microcell length of leaf spinneret orifice is 0.85mm, equivalent diameter 0.26mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 4:2；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 400m/min；Sizing is super The rate of feeding is 3.5%；Winding overfeed rate is 3.5%；T1 is 200 DEG C；T2 is 170 DEG C；DR is 1.7；D/Y is 1.8；Network pressure is 0.3MPa, the ratio between modified poly ester POY and modified poly ester FDY fiber number is 1:1 in polyester Wool-Like abnormal contraction composite filament.
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.100, fiber number 230dtex, and fracture is strong Degree is 2.2cN/dtex, and elongation at break 15%, crimp contraction 5.50%, internet pricing is 90/m, line density deviation Rate is 1.9%, and breaking strength CV value is 6.5%, and extension at break CV value is 7.5%, and crimp contraction coefficient of variation CV value is 7.4%, boiling water shrinkage 5.0%, oil content 1.0%, glossiness 47%, capillary parameter is 0.155.
Embodiment 2
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) esterification；Terephthalic acid (TPA), ethylene glycol and the 2,2- diethyl -1,3- for being 1:1.3:0.04 by molar ratio Propylene glycol is made into slurry, and antimony glycol, titanium dioxide and trimethyl phosphate is added after mixing, pressurize in nitrogen atmosphere into Row esterification, moulding pressure are normal pressure, and the temperature of esterification is 260 DEG C, when the water quantity of distillate in esterification reaches reason By value 91% when be esterification terminal, wherein the additional amount of antimony glycol be terephthalic acid (TPA) weight 0.02%, dioxy The additional amount for changing titanium is the 0.21% of terephthalic acid (TPA) weight, and the additional amount of trimethyl phosphate is terephthalic acid (TPA) weight 0.03%, wherein the structural formula of 2,2- diethyl -1,3-PD is as follows:
Figure GDA0001618979150000111
(b) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 490Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 35min, and reaction temperature is 261 DEG C, reaction time 30min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is further reduced to absolute pressure 100Pa, instead Answering temperature is 277 DEG C, reaction time 85min, and modified poly ester is made.Wherein the strand of modified poly ester includes terephthalic acid (TPA) Segment, ethylene glycol segment and 2,2- diethyl -1,3-PD segment, the content of cyclic oligomer is in modified poly ester 0.6wt%, number-average molecular weight 27000, molecular weight distributing index 1.8,2,2- diethyl -1,3-PD chain in modified poly ester The molar content of section is the 5% of terephthalic acid (TPA) segment molar content；
(1.2) dispersing matt agent in modified poly ester, matt agent is the mixture of calcium carbonate and unformed silica, Content of the middle matt agent in modified poly ester is 1.2wt%, and the content of unformed silica is 22wt% in matt agent；
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature is 282 DEG C；Cooling temperature is 18 DEG C；Winding speed is 3200m/min, wherein Contain diesis shape monofilament and trilobal monofilament, diesis shape simultaneously in a branch of modified poly ester POY that same spinneret squeezes out The fiber number of monofilament is 0.7dtex, and bending stiffness is 0.78 × 10-5cN·cm2, the fiber number of trilobal monofilament is 0.90dtex, curved Stiffness is 0.86 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 281 DEG C；Cooling temperature is 20 DEG C；Network pressure is 0.30MPa；One roller speed is 2500m/min；One roll temperature is 80 DEG C；Two roller speeds are 3800m/min；Two roll temperatures are 115 ℃；Winding speed is 3800m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.71dtex, and bending stiffness is 0.62 × 10-5cN·cm2, three The fiber number of leaf monofilament is 0.89dtex, and bending stiffness is 0.86 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 0.99, and the microcell length of trilobal spinneret orifice is 0.93mm, double ten The microcell length of font spinneret orifice is 0.93mm, equivalent diameter 0.25mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 3:2；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 500m/min；Sizing is super The rate of feeding is 5.0%；Winding overfeed rate is 4.0%；T1 is 180 DEG C；T2 is 150 DEG C；DR is 1.6；D/Y is 1.6；Network pressure is 0.25MPa, modified poly ester POY and modified poly ester FDY the ratio between fiber numbers are 1.2 in polyester Wool-Like abnormal contraction composite filament: 1。
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.180, fiber number 150dtex, and fracture is strong Degree is 2.1cN/dtex, and elongation at break 13%, crimp contraction 2.5%, internet pricing is 85/m, line density deviation ratio It is 2.0%, breaking strength CV value is 7.0%, and extension at break CV value is 8.0%, and crimp contraction coefficient of variation CV value is 8.0%, boiling water shrinkage 4.0%, oil content 0.8%, glossiness 45%, capillary parameter is 0.15.
Embodiment 3
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) esterification；Terephthalic acid (TPA), ethylene glycol and ethyl -1 2- butyl -2- for being 1:1.4:0.05 by molar ratio, 3-propanediol is made into slurry, and antimony acetate, titanium dioxide and Trimethyl phosphite is added after mixing, pressurizes in nitrogen atmosphere Esterification is carried out, moulding pressure 0.1MPa, the temperature of esterification is 252 DEG C, when the water quantity of distillate in esterification reaches To theoretical value 92% when be esterification terminal, wherein the additional amount of antimony acetate be terephthalic acid (TPA) weight 0.03%, two The additional amount of titanium oxide is the 0.23% of terephthalic acid (TPA) weight, and the additional amount of Trimethyl phosphite is terephthalic acid (TPA) weight 0.01%, wherein 2- butyl -2- ethyl -1,3-PD structural formula is as follows:
Figure GDA0001618979150000131
(b) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 495Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 40min, and reaction temperature is 263 DEG C, reaction time 45min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure made to be further reduced to absolute pressure 95Pa, react Temperature is 278 DEG C, reaction time 60min, modified poly ester is made, wherein the strand of modified poly ester includes terephthalic acid (TPA) chain Section, ethylene glycol segment and 2- butyl -2- ethyl -1,3-PD segment, the content of cyclic oligomer is in modified poly ester 0.5wt%, number-average molecular weight 21000, molecular weight distributing index 2.2,2- butyl -2- ethyl -1,3- the third two in modified poly ester The molar content of alcohol segment is the 4% of terephthalic acid (TPA) segment molar content；
(1.2) disperse matt agent in modified poly ester, matt agent is unformed titanium dioxide and unformed silica Mixture, wherein content of the matt agent in modified poly ester is 1.3wt%, the content of unformed silica in matt agent For 34wt%.
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature is 286 DEG C；Cooling temperature is 22 DEG C；Winding speed is 3300m/min, wherein Contain diesis shape monofilament and trilobal monofilament, diesis shape simultaneously in a branch of modified poly ester POY that same spinneret squeezes out The fiber number of monofilament is 0.9dtex, and bending stiffness is 0.90 × 10-5cN·cm2, the fiber number of trilobal monofilament is 1.1dtex, bending It is just 0.90 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 283 DEG C；Cooling temperature is 22 DEG C；Network pressure is 0.25MPa；One roller speed is 2600m/min；One roll temperature is 78 DEG C；Two roller speeds are 3650m/min；Two roll temperatures are 115 ℃；Winding speed is 3800m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.86dtex, and bending stiffness is 0.75 × 10-5cN·cm2, three The fiber number of leaf monofilament is 1.05dtex, and bending stiffness is 0.92 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 1.03, and the microcell length of trilobal spinneret orifice is 1.20mm, double ten The microcell length of font spinneret orifice is 1.20mm, and the microcell length of trilobal spinneret orifice is 1.22mm, equivalent diameter 0.36mm, All spinneret orifices concentric arrays on spinneret, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, Wherein concentric circles is equidistant concentric circles, and same annulus contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant simultaneously It arranges, the quantity ratio of diesis shape spinneret orifice and trilobal spinneret orifice is 5:2 on same annulus；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 800m/min；Sizing is super The rate of feeding is 4.5%；Winding overfeed rate is 2.5%；T1 is 220 DEG C；T2 is 180 DEG C；DR is 1.8；D/Y is 2.0；Network pressure is 0.05MPa, modified poly ester POY and modified poly ester FDY the ratio between fiber numbers are 1.5 in polyester Wool-Like abnormal contraction composite filament: 1。
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.165, fiber number 300dtex, and fracture is strong Degree is 2.3cN/dtex, and elongation at break 17.0%, crimp contraction 8.50%, internet pricing is 95/m, and line density is inclined Rate is 1.8%, and breaking strength CV value is 6.3%, and extension at break CV value is 7.2%, and crimp contraction coefficient of variation CV value is 7.2%, boiling water shrinkage 6.0%, oil content 0.8%, glossiness 49%, capillary parameter is 0.159.
Embodiment 4
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) 3,3- diethyl -1,5- pentanediol is prepared；At 95 DEG C, under nitrogen atmosphere, by 3,3- diethyl-propionic aldehyde, acetaldehyde 20min is reacted with triethylamine, then concentrate is added in the hydrogenator for having thunder girl's Raney nickel, in 2.914MPa hydrogen pressure It is reacted at 100 DEG C, reaction is finished, and it is cooling, catalyst is precipitated, after the processing of solution spent ion exchange resin, water is steamed in decompression, point From purification obtains 3,3- diethyl -1,5-PD, wherein the structural formula of 3,3- diethyl -1,5-PD is as follows:
Figure GDA0001618979150000141
(b) esterification；Terephthalic acid (TPA), ethylene glycol and the 3,3- diethyl -1,5- for being 1:1.5:0.06 by molar ratio Pentanediol is made into slurry, and antimony oxide, titanium dioxide and triphenyl phosphate is added after mixing, pressurizes in nitrogen atmosphere Esterification is carried out, moulding pressure 0.3MPa, the temperature of esterification is 255 DEG C, when the water quantity of distillate in esterification reaches To theoretical value 95% when be esterification terminal, wherein the additional amount of antimony oxide is terephthalic acid (TPA) weight 0.04%, the additional amount of titanium dioxide is the 0.25% of terephthalic acid (TPA) weight, and the additional amount of triphenyl phosphate is terephthaldehyde The 0.01% of sour weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 400Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 50min, and reaction temperature is 265 DEG C, reaction time 33min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure made to be further reduced to absolute pressure 90Pa, react Temperature is 280 DEG C, reaction time 50min, modified poly ester is made, wherein the strand of modified poly ester includes terephthalic acid (TPA) chain Section, ethylene glycol segment and 3,3- diethyl -1,5-PD segment, the content of cyclic oligomer is 0.2wt% in modified poly ester, Number-average molecular weight 23000, molecular weight distributing index 1.9,3,3- diethyl -1,5-PD segment mole in modified poly ester Content is the 3.5% of terephthalic acid (TPA) segment molar content；
(1.2) disperse matt agent in modified poly ester, matt agent is unformed titanium dioxide and unformed silica Mixture, wherein content of the matt agent in modified poly ester is 1.15wt%, and unformed silica contains in matt agent Amount is 15wt%；
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature is 290 DEG C；Cooling temperature is 18 DEG C；Winding speed is 3200m/min, wherein Contain diesis shape monofilament and trilobal monofilament, diesis shape simultaneously in a branch of modified poly ester POY that same spinneret squeezes out The fiber number of monofilament is 0.79dtex, and bending stiffness is 0.80 × 10-5cN·cm2, the fiber number of trilobal monofilament is 0.98dtex, curved Stiffness is 0.88 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 288 DEG C；Cooling temperature is 21 DEG C；Network pressure is 0.26MPa；One roller speed is 2200m/min；One roll temperature is 77 DEG C；Two roller speeds are 3700m/min；Two roll temperatures are 130 ℃；Winding speed is 3650m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.79dtex, and bending stiffness is 0.74 × 10-5N·cm2, three The fiber number of leaf monofilament is 0.80dtex, and bending stiffness is 0.95 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 1.00, and the microcell length of diesis shape spinneret orifice is 0.50mm, three The microcell length of leaf spinneret orifice is 0.51mm, equivalent diameter 0.25mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 3:2；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 600m/min；Sizing is super The rate of feeding is 3.5%；Winding overfeed rate is 4.5%；T1 is 185 DEG C；T2 is 155 DEG C；DR is 1.7；D/Y is 1.7；Network pressure is 0.15MPa, modified poly ester POY and modified poly ester FDY the ratio between fiber numbers are 1.3 in polyester Wool-Like abnormal contraction composite filament: 1。
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.120, fiber number 160dtex, and fracture is strong Degree is 2.12cN/dtex, and elongation at break 13.5%, crimp contraction 3.0%, internet pricing is 86/m, and line density is inclined Rate is 1.82%, and breaking strength CV value is 6.9%, and extension at break CV value is 7.9%, and crimp contraction coefficient of variation CV value is 7.85%, boiling water shrinkage 4.1%, oil content 0.85%, glossiness 48%, capillary parameter is 0.153.
Embodiment 5
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) 4,4- diethyl -1,7- heptandiol is prepared；At 95 DEG C, under nitrogen atmosphere, by 4,4- diethyl-butyraldehyde, propionic aldehyde 20min is reacted with triethylamine, then concentrate is added in the hydrogenator for having thunder girl's Raney nickel, in 2.914MPa hydrogen pressure It is reacted at 100 DEG C, reaction is finished, and it is cooling, catalyst is precipitated, after the processing of solution spent ion exchange resin, water is steamed in decompression, point From purification obtains 4,4- diethyl -1,7- heptandiol, wherein the structural formula of 4,4- diethyl -1,7- heptandiols is as follows:
(b) esterification；Terephthalic acid (TPA), ethylene glycol and the 4,4- diethyl -1,7- for being 1:1.6:0.03 by molar ratio Heptandiol is made into slurry, and antimony glycol, titanium dioxide and trimethyl phosphate is added after mixing, pressurize in nitrogen atmosphere into Row esterification, moulding pressure are normal pressure, and the temperature of esterification is 257 DEG C, when the water quantity of distillate in esterification reaches reason By value 92% when be esterification terminal, wherein the additional amount of antimony glycol be terephthalic acid (TPA) weight 0.05%, dioxy The additional amount for changing titanium is the 0.20% of terephthalic acid (TPA) weight, and the additional amount of trimethyl phosphate is terephthalic acid (TPA) weight 0.04%；
(c) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 450Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 33min, and reaction temperature is 270 DEG C, reaction time 30min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure made to be further reduced to absolute pressure 95Pa, react Temperature is 275 DEG C, reaction time 60min, modified poly ester is made, wherein the strand of modified poly ester includes terephthalic acid (TPA) chain Section, ethylene glycol segment and 4,4- diethyl -1,7- heptandiol segment, the content of cyclic oligomer is 0.5wt% in modified poly ester, Number-average molecular weight 25000, molecular weight distributing index 2.1, mole of 4,4- diethyl -1,7- heptandiol segment in modified poly ester Content is the 5% of terephthalic acid (TPA) segment molar content.
(1.2) dispersing matt agent in modified poly ester, matt agent is the mixture of calcium carbonate and unformed silica, Content of the middle matt agent in modified poly ester is 1.2wt%, and the content of unformed silica is 40wt% in matt agent.
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature is 280 DEG C；Cooling temperature is 22 DEG C；Winding speed is 3250m/min, wherein Contain diesis shape monofilament and trilobal monofilament, diesis shape simultaneously in a branch of modified poly ester POY that same spinneret squeezes out The fiber number of monofilament is 0.81dtex, and bending stiffness is 0.82 × 10-5cN·cm2, the fiber number of trilobal monofilament is 1.0dtex, curved Stiffness is 0.79 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 290 DEG C；Cooling temperature is 25 DEG C；Network pressure is 0.20MPa；One roller speed is 2400m/min；One roll temperature is 75 DEG C；Two roller speeds are 3850m/min；Two roll temperatures are 135 ℃；Winding speed is 3700m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.84dtex, and bending stiffness is 0.78 × 10-5cN·cm2, three The fiber number of leaf monofilament is 1.05dtex, and bending stiffness is 0.88 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 0.98, and the microcell length of trilobal spinneret orifice is 0.50mm, double ten The microcell length of font spinneret orifice is 0.50mm, equivalent diameter 0.26mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 5:2；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 700m/min；Sizing is super The rate of feeding is 4.0%；Winding overfeed rate is 5.0%；T1 is 190 DEG C；T2 is 160 DEG C；DR is 1.8；D/Y is 1.8；Network pressure is 0.2MPa, the ratio between modified poly ester POY and modified poly ester FDY fiber number is 1.5:1 in polyester Wool-Like abnormal contraction composite filament.
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.160, fiber number 180dtex, and fracture is strong Degree is 2.14cN/dtex, and elongation at break 14%, crimp contraction 3.5%, internet pricing is 87/m, line density deviation Rate is 1.92%, and breaking strength CV value is 6.8%, and extension at break CV value is 7.8%, and crimp contraction coefficient of variation CV value is 7.85%, boiling water shrinkage 4.5%, oil content 0.88%, glossiness 48%, capillary parameter is 0.153.
Embodiment 6
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) 4,4- bis- (1,-Methylethyl) -1,7- heptandiol is prepared；At 90 DEG C, under nitrogen atmosphere, by (the 1- first of 4,4- bis- Base ethyl)-butyraldehyde, propionic aldehyde and triethylamine reaction 20min, then concentrate is added to the hydrogenator for having thunder girl's Raney nickel In, it is reacted at 2.914MPa hydrogen pressure and 100 DEG C, reaction is finished, and it is cooling, catalyst is precipitated.At solution spent ion exchange resin After reason, water is steamed in decompression, separates, and purification obtains 4,4- bis- (1,-Methylethyl) -1,7- heptandiol, wherein 4,4- bis- (1,-methyl Ethyl) -1,7- heptandiol structural formula it is as follows:
Figure GDA0001618979150000181
(b) esterification；By molar ratio be the terephthalic acid (TPA) of 1:1.7:0.05, ethylene glycol and 4,4- bis- (1 ,-methyl second Base) -1,7- heptandiol is made into slurry, antimony acetate, titanium dioxide and Trimethyl phosphite is added after mixing, in nitrogen atmosphere Middle pressurization carries out esterification, and moulding pressure 0.2MPa, the temperature of esterification is 253 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 96% of theoretical value, and wherein the additional amount of antimony acetate is terephthalic acid (TPA) weight 0.01%, the additional amount of titanium dioxide is the 0.20% of terephthalic acid (TPA) weight, and the additional amount of Trimethyl phosphite is to benzene two The 0.05% of formic acid weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 480Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 38min, and reaction temperature is 262 DEG C, reaction time 38min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure made to be further reduced to absolute pressure 98Pa, react Temperature is 279 DEG C, reaction time 80min, modified poly ester is made, wherein the strand of modified poly ester includes terephthalic acid (TPA) chain Section, ethylene glycol segment and 4,4- bis- (1,-Methylethyl) -1,7- heptandiol segment, the content of cyclic oligomer in modified poly ester For 0.55wt%, number-average molecular weight 27000, molecular weight distributing index 2.2,4,4- bis- (1 ,-Methylethyl)-in modified poly ester The molar content of 1,7- heptandiol segment is the 4% of terephthalic acid (TPA) segment molar content；
(1.2) disperse matt agent in modified poly ester, matt agent is unformed titanium dioxide and unformed silica Mixture, wherein content of the matt agent in modified poly ester is 1.5wt%, the content of unformed silica in matt agent For 38wt%；
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature is 289 DEG C；Cooling temperature is 20 DEG C；Winding speed is 3300m/min, wherein Contain diesis shape monofilament and trilobal monofilament, diesis shape simultaneously in a branch of modified poly ester POY that same spinneret squeezes out The fiber number of monofilament is 0.83dtex, and bending stiffness is 0.83 × 10-5cN·cm2, the fiber number of trilobal monofilament is 1.03dtex, curved Stiffness is 0.82 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 281 DEG C；Cooling temperature is 25 DEG C；Network pressure is 0.28MPa；One roller speed is 2600m/min；One roll temperature is 79 DEG C；Two roller speeds are 3850m/min；Two roll temperatures are 120 ℃；Winding speed is 3600m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.84dtex, and bending stiffness is 0.88 × 10-5cN·cm2, three The fiber number of leaf monofilament is 1.03dtex, and bending stiffness is 0.82 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 0.97, and the microcell length of trilobal spinneret orifice is 1.22mm, double ten The microcell length of font spinneret orifice is 1.22mm, equivalent diameter 0.28mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 5:2；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 500m/min；Sizing is super The rate of feeding is 5.5%；Winding overfeed rate is 3.0%；T1 is 195 DEG C；T2 is 165 DEG C；DR is 1.6；D/Y is 2.0；Network pressure is 0.05MPa, modified poly ester POY and modified poly ester FDY the ratio between fiber numbers are 1.1 in polyester Wool-Like abnormal contraction composite filament: 1。
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.130, fiber number 190dtex, and fracture is strong Degree is 2.14cN/dtex, and elongation at break 13.8%, crimp contraction 3.8%, internet pricing is 90/m, and line density is inclined Rate is 1.9%, and breaking strength CV value is 6.7%, and extension at break CV value is 7.7%, and crimp contraction coefficient of variation CV value is 7.6%, boiling water shrinkage 4.6%, oil content 0.89%, glossiness 47%, capillary parameter is 0.156.
Embodiment 7
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) 3,3- dipropyl -1,5- pentanediol is prepared；At 94 DEG C, under nitrogen atmosphere, by 3,3- dipropyl-propionic aldehyde, acetaldehyde 20min is reacted with triethylamine, then concentrate is added in the hydrogenator for having thunder girl's Raney nickel, in 2.914MPa hydrogen pressure It is reacted at 100 DEG C, reaction is finished, and it is cooling, catalyst is precipitated.After the processing of solution spent ion exchange resin, water is steamed in decompression, point From purification obtains 3,3- dipropyl -1,5-PD, wherein the structural formula of 3,3- dipropyl -1,5-PD is as follows:
(b) esterification；Terephthalic acid (TPA), ethylene glycol and the 3,3- dipropyl -1,5- for being 1:1.8:0.03 by molar ratio Pentanediol is made into slurry, and antimony oxide, titanium dioxide and triphenyl phosphate is added after mixing, pressurizes in nitrogen atmosphere Esterification is carried out, moulding pressure 0.3MPa, the temperature of esterification is 250 DEG C, when the water quantity of distillate in esterification reaches To theoretical value 90% when be esterification terminal, wherein the additional amount of antimony oxide is terephthalic acid (TPA) weight 0.03%, the additional amount of titanium dioxide is the 0.24% of terephthalic acid (TPA) weight, and the additional amount of triphenyl phosphate is terephthaldehyde The 0.02% of sour weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 455Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 42min, and reaction temperature is 264 DEG C, reaction time 45min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure made to be further reduced to absolute pressure 85Pa, react Temperature is 285 DEG C, reaction time 75min, modified poly ester is made, wherein the strand of modified poly ester includes terephthalic acid (TPA) chain Section, ethylene glycol segment and 3,3- dipropyl -1,5-PD segment, the content of cyclic oligomer is in modified poly ester 0.45wt%, number-average molecular weight 26500, molecular weight distributing index 2.2,3,3- dipropyl -1,5-PD in modified poly ester The molar content of segment is the 4.5% of terephthalic acid (TPA) segment molar content.
(1.2) disperse matt agent in modified poly ester, matt agent is the mixture of unformed silica, wherein matt agent Content in modified poly ester is 1.25wt%, and the content of unformed silica is 27wt% in matt agent.
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature is 280 DEG C；Cooling temperature is 20 DEG C；Winding speed is 3350m/min, wherein Contain diesis shape monofilament and trilobal monofilament, diesis shape simultaneously in a branch of modified poly ester POY that same spinneret squeezes out The fiber number of monofilament is 0.85dtex, and bending stiffness is 0.85 × 10-5cN·cm2, the fiber number of trilobal monofilament is 0.92dtex, curved Stiffness is 0.96 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 284 DEG C；Cooling temperature is 25 DEG C；Network pressure is 0.25MPa；One roller speed is 2500m/min；One roll temperature is 82 DEG C；Two roller speeds are 3650m/min；Two roll temperatures are 125 ℃；Winding speed is 3650m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.84dtex, and bending stiffness is 0.69 × 10-5cN·cm2, three The fiber number of leaf monofilament is 0.91dtex, and bending stiffness is 0.86 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 1.03, and the microcell length of diesis shape spinneret orifice is 1.44mm, three The microcell length of leaf spinneret orifice is 1.44mm, equivalent diameter 0.29mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 5:2；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 400m/min；Sizing is super The rate of feeding is 4.5%；Winding overfeed rate is 4.0%；T1 is 200 DEG C；T2 is 170 DEG C；DR is 1.8；D/Y is 1.6；Network pressure is 0.3MPa, the ratio between modified poly ester POY and modified poly ester FDY fiber number is 1:1 in polyester Wool-Like abnormal contraction composite filament.
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.125, fiber number 200dtex, and fracture is strong Degree is 2.16cN/dtex, and elongation at break 13.9%, crimp contraction 3.9%, internet pricing is 92/m, and line density is inclined Rate is 1.88%, and breaking strength CV value is 6.6%, and extension at break CV value is 7.5%, and crimp contraction coefficient of variation CV value is 7.6%, boiling water shrinkage 4.9%, oil content 0.9%, glossiness 47%, capillary parameter is 0.157.
Embodiment 8
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) 4,4- dipropyl -1,7- heptandiol is prepared；At 93 DEG C, under nitrogen atmosphere, by 4,4- dipropyl-butyraldehyde, acetaldehyde 20min is reacted with triethylamine, then concentrate is added in the hydrogenator for having thunder girl's Raney nickel, in 2.914MPa hydrogen pressure It is reacted at 100 DEG C, reaction is finished, and it is cooling, catalyst is precipitated.After the processing of solution spent ion exchange resin, water is steamed in decompression, point From purification obtains 4,4- dipropyl -1,7- heptandiol, wherein the structural formula of 4,4- dipropyl -1,7- heptandiols is as follows:
Figure GDA0001618979150000221
(b) esterification；Terephthalic acid (TPA), ethylene glycol and the 4,4- dipropyl -1,7- for being 1:1.9:0.04 by molar ratio Heptandiol is made into slurry, and antimony glycol, titanium dioxide and trimethyl phosphate is added after mixing, pressurize in nitrogen atmosphere into Row esterification, moulding pressure 0.3MPa, the temperature of esterification is 260 DEG C, when the water quantity of distillate in esterification reaches Theoretical value 93% when be esterification terminal, wherein the additional amount of antimony glycol be terephthalic acid (TPA) weight 0.04%, two The additional amount of titanium oxide is the 0.21% of terephthalic acid (TPA) weight, and the additional amount of trimethyl phosphate is terephthalic acid (TPA) weight 0.03%；
(c) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 475Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 45min, and reaction temperature is 265 DEG C, reaction time 48min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure made to be further reduced to absolute pressure 88Pa, react Temperature is 283 DEG C, reaction time 80min, modified poly ester is made, wherein the strand of modified poly ester includes terephthalic acid (TPA) chain Section, ethylene glycol segment and 4,4- dipropyl -1,7- heptandiol segment, the content of cyclic oligomer is 0.6wt% in modified poly ester, Number-average molecular weight 23000, molecular weight distributing index 2.0, mole of 4,4- dipropyl -1,7- heptandiol segment in modified poly ester Content is the 3% of terephthalic acid (TPA) segment molar content；
(1.2) dispersing matt agent in modified poly ester, matt agent is the mixture of calcium carbonate and unformed silica, Content of the middle matt agent in modified poly ester is 1.4wt%, and the content of unformed silica is 50wt% in matt agent；
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature is 290 DEG C；Cooling temperature is 21 DEG C；Winding speed is 3500m/min, wherein Contain diesis shape monofilament and trilobal monofilament, diesis shape simultaneously in a branch of modified poly ester POY that same spinneret squeezes out The fiber number of monofilament is 0.83dtex, and bending stiffness is 0.86 × 10-5cN·cm2, the fiber number of trilobal monofilament is 0.93dtex, curved Stiffness is 0.90 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 285 DEG C；Cooling temperature is 24 DEG C；Network pressure is 0.30MPa；One roller speed is 2400m/min；One roll temperature is 85 DEG C；Two roller speeds are 3800m/min；Two roll temperatures are 115 ℃；Winding speed is 3800m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.84dtex, and bending stiffness is 0.86 × 10-5cN·cm2, three The fiber number of leaf monofilament is 0.94dtex, and bending stiffness is 0.90 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 0.99, and the microcell length of diesis shape spinneret orifice is 0.52mm, three The microcell length of leaf spinneret orifice is 0.52mm, equivalent diameter 0.36mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 5:2；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 600m/min；Sizing is super The rate of feeding is 3.5%；Winding overfeed rate is 4.5%；T1 is 205 DEG C；T2 is 175 DEG C；DR is 1.8；D/Y is 1.8；D/Y is 2.0； Network pressure is 0.25MPa, modified poly ester POY and modified poly ester FDY fiber numbers in polyester Wool-Like abnormal contraction composite filament The ratio between be 1.4:1.
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.144, fiber number 220dtex, and fracture is strong Degree is 2.16cN/dtex, and elongation at break 15.4%, crimp contraction 6.5%, internet pricing is 93/m, and line density is inclined Rate is 1.85%, and breaking strength CV value is 6.5%, and extension at break CV value is 7.4%, and crimp contraction coefficient of variation CV value is 7.4%, boiling water shrinkage 5.5%, oil content 1.1%, glossiness 46%, capillary parameter is 0.157.
Embodiment 9
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) 4- methyl -4- (1,1- dimethyl ethyl) -1,7- heptandiol is prepared；At 92 DEG C, under nitrogen atmosphere, by 4- first Base -4- (1,1- dimethyl ethyl)-butyraldehyde, propionic aldehyde and triethylamine react 20min, and concentrate addition is then had the catalysis of thunder girl's nickel In the hydrogenator of agent, to be reacted at 2.914MPa hydrogen pressure and 100 DEG C, reaction is finished, and it is cooling, catalyst is precipitated, solution is used After ion exchange resin treatment, water is steamed in decompression, separates, purification, obtains 4- methyl -4- (1,1- dimethyl ethyl) -1,7- heptan two Alcohol, wherein 4- methyl -4- (1,1- dimethyl ethyl) -1,7- heptandiol structural formula is as follows:
(b) esterification；Terephthalic acid (TPA), ethylene glycol and the 4- methyl -4- (1,1- bis- for being 1:2.0:0.05 by molar ratio Methylethyl) -1,7- heptandiol is made into slurry, antimony acetate, titanium dioxide and trimethyl phosphate is added after mixing, in nitrogen Pressurization carries out esterification in atmosphere, and moulding pressure is normal pressure MPa, and the temperature of esterification is 251 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 96% of theoretical value, and wherein the additional amount of antimony acetate is terephthalic acid (TPA) weight 0.05%, the additional amount of titanium dioxide is the 0.22% of terephthalic acid (TPA) weight, and the additional amount of trimethyl phosphate is terephthaldehyde The 0.04% of sour weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 420Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 30min, and reaction temperature is 267 DEG C, reaction time 50min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure made to be further reduced to absolute pressure 80Pa, react Temperature is 280 DEG C, reaction time 90min, modified poly ester is made, wherein the strand of modified poly ester includes terephthalic acid (TPA) chain Section, ethylene glycol segment and 4- methyl -4- (1,1- dimethyl ethyl) -1,7- heptandiol segment, cyclic oligomer in modified poly ester Content be 0.25wt%, number-average molecular weight 24000, molecular weight distributing index 2.2,4- methyl -4- (1,1- in modified poly ester Dimethyl ethyl) -1,7- heptandiol segment molar content be terephthalic acid (TPA) segment molar content 4%；
(1.2) disperse matt agent in modified poly ester, matt agent is unformed titanium dioxide and unformed silica Mixture, wherein content of the matt agent in modified poly ester is 1.0wt%, the content of unformed silica in matt agent For 23wt%；
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature is 283 DEG C；Cooling temperature is 21 DEG C；Winding speed is 3600m/min, wherein Contain diesis shape monofilament and trilobal monofilament, curved diesis simultaneously in a branch of modified poly ester POY that same spinneret squeezes out The fiber number of shape monofilament is 0.85dtex, and bending stiffness is 0.87 × 10-5cN·cm2, the fiber number of trilobal monofilament is 0.96dtex, Stiffness is 0.95 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；
Spinning melt is squeezed out, cooled down, oiled, stretched through metering, composite spinneret, thermal finalization and winding, main spinning Technological parameter is as follows: spinning temperature is 290 DEG C；Cooling temperature is 23 DEG C；Network pressure is 0.20MPa；One roller speed is 2400m/min；One roll temperature is 80 DEG C；Two roller speeds are 3750m/min；Two roll temperatures are 135 DEG C；Winding speed is 3800m/ Min, wherein contain diesis shape monofilament and trilobal monofilament simultaneously in a branch of modified poly ester FDY of same spinneret extrusion, The fiber number of diesis shape monofilament is 0.85dtex, and bending stiffness is 0.79 × 10-5cN·cm2, the fiber number of trilobal monofilament is 0.98dtex, bending stiffness are 0.96 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 1.02, and the microcell length of diesis shape spinneret orifice is 0.85mm, three The microcell length of leaf spinneret orifice is 0.85mm, equivalent diameter 0.25mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 4:2；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 800m/min；Sizing is super The rate of feeding is 4.5%；Winding overfeed rate is 2.5%；T1 is 215 DEG C；T2 is 178 DEG C；DR is 1.6；D/Y is 1.9；Network pressure is 0.05MPa, modified poly ester POY and modified poly ester FDY the ratio between fiber numbers are 1.3 in polyester Wool-Like abnormal contraction composite filament: 1。
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.174, fiber number 240dtex, and fracture is strong Degree is 2.17cN/dtex, and elongation at break 16%, crimp contraction 7.50%, internet pricing is 94/m, line density deviation Rate is 1.83%, and breaking strength CV value is 6.4%, and extension at break CV value is 7.4%, and crimp contraction coefficient of variation CV value is 7.3%, boiling water shrinkage 5.7%, oil content 1.2%, glossiness 46%, capillary parameter is 0.158.
Embodiment 10
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) 3- methyl -3- amyl -1,6-HD is prepared；At 90 DEG C, under nitrogen atmosphere, by 3- methyl -3- amyl-the third Aldehyde, propionic aldehyde and triethylamine react 20min, then concentrate are added in the hydrogenator for having thunder girl's Raney nickel, It is reacted at 2.914MPa hydrogen pressure and 100 DEG C, reaction is finished, and it is cooling, catalyst is precipitated.After the processing of solution spent ion exchange resin, Water is steamed in decompression, separates, and purification obtains 3- methyl -3- amyl -1,6- hexylene glycol, wherein 3- methyl -3- amyl -1,6- hexylene glycol Structural formula it is as follows:
Figure GDA0001618979150000261
(b) esterification；Terephthalic acid (TPA), ethylene glycol and amyl -1 3- methyl -3- for being 1:1.2:0.06 by molar ratio, 6- hexylene glycol is made into slurry, and antimony glycol, titanium dioxide and Trimethyl phosphite is added after mixing, adds in nitrogen atmosphere Pressure carries out esterification, and moulding pressure 0.1MPa, the temperature of esterification is 255 DEG C, when the water quantity of distillate in esterification It is esterification terminal when reaching the 92% of theoretical value, wherein the additional amount of antimony glycol is terephthalic acid (TPA) weight 0.01%, the additional amount of titanium dioxide is the 0.20% of terephthalic acid (TPA) weight, and the additional amount of Trimethyl phosphite is to benzene two The 0.01% of formic acid weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 490Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 50min, and reaction temperature is 269 DEG C, reaction time 30min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is further reduced to absolute pressure 100Pa, instead Answering temperature is 281 DEG C, reaction time 55min, modified poly ester is made, wherein the strand of modified poly ester includes terephthalic acid (TPA) Segment, ethylene glycol segment and 3- methyl -3- amyl -1,6- hexylene glycol segment, the content of cyclic oligomer is in modified poly ester 0.1wt%, number-average molecular weight 20000, molecular weight distributing index 1.9, in modified poly ester 3- methyl -3- amyl -1,6- oneself two The molar content of alcohol segment is the 3.5% of terephthalic acid (TPA) segment molar content；
(1.2) dispersing matt agent in modified poly ester, matt agent is the mixture of calcium carbonate and unformed silica, Content of the middle matt agent in modified poly ester is 1.3wt%, and the content of unformed silica is 44wt% in matt agent；
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature is 290 DEG C；Cooling temperature is 21 DEG C；Winding speed is 3600m/min, wherein Contain diesis shape monofilament and trilobal monofilament, diesis shape simultaneously in a branch of modified poly ester POY that same spinneret squeezes out The fiber number of monofilament is 0.87dtex, and bending stiffness is 0.89 × 10-5cN·cm2, the fiber number of trilobal monofilament is 1.06dtex, curved Stiffness is 0.79 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 284 DEG C；Cooling temperature is 20 DEG C；Network pressure is 0.28MPa；One roller speed is 2200m/min；One roll temperature is 77 DEG C；Two roller speeds are 3650m/min；Two roll temperatures are 120 ℃；Winding speed is 3600m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.88dtex, and bending stiffness is 0.78 × 10-5cN·cm2, three The fiber number of leaf monofilament is 1.07dtex, and bending stiffness is 0.79 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 1.02, and the microcell length of trilobal spinneret orifice is 1.35mm, double ten The microcell length of font spinneret orifice is 1.35mm, equivalent diameter 0.33mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 5:2；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 700m/min；Sizing is super The rate of feeding is 5.5%；Winding overfeed rate is 5.0%；T1 is 220 DEG C；T2 is 178 DEG C；DR is 1.6；D/Y is 2.0；Network pressure is 0.3MPa, the ratio between modified poly ester POY and modified poly ester FDY fiber number is 1:1 in polyester Wool-Like abnormal contraction composite filament.
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.163, fiber number 250dtex, and fracture is strong Degree is 2.23cN/dtex, and elongation at break 16%, crimp contraction 7.9%, internet pricing is 95/m, line density deviation Rate is 1.82%, and breaking strength CV value is 6.3%, and extension at break CV value is 7.3%, and crimp contraction coefficient of variation CV value is 7.2%, boiling water shrinkage 5.9%, oil content 1.2%, glossiness 45%, capillary parameter is 0.159.
Embodiment 11
A kind of preparation method of polyester Wool-Like abnormal contraction composite filament, the specific steps are as follows:
(1) prepared by spinning melt；
(1.1) modified poly ester is prepared:
(a) 3,3- diamyl -1,5- pentanediol is prepared；At 90 DEG C, under nitrogen atmosphere, by 3,3- diamyl-propionic aldehyde, acetaldehyde 20min is reacted with triethylamine, then concentrate is added in the hydrogenator for having thunder girl's Raney nickel, in 2.914MPa hydrogen pressure It is reacted at 100 DEG C, reaction is finished, and it is cooling, catalyst is precipitated.After the processing of solution spent ion exchange resin, water is steamed in decompression, point From purification obtains 3,3- diamyl -1,5-PD, wherein the structural formula of 3,3- diamyl -1,5-PD is as follows:
Figure GDA0001618979150000281
(b) esterification；Terephthalic acid (TPA), ethylene glycol and the 3,3- diamyl -1,5- for being 1:2.0:0.03 by molar ratio Pentanediol is made into slurry, and antimony acetate, titanium dioxide and Trimethyl phosphite is added after mixing, pressurize in nitrogen atmosphere into Row esterification, moulding pressure 0.2MPa, the temperature of esterification is 250 DEG C, when the water quantity of distillate in esterification reaches Theoretical value 97% when be esterification terminal, wherein the additional amount of antimony acetate be terephthalic acid (TPA) weight 0.01%, dioxy The additional amount for changing titanium is the 0.23% of terephthalic acid (TPA) weight, and the additional amount of Trimethyl phosphite is terephthalic acid (TPA) weight 0.05%；
(c) polycondensation reaction；After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, It is 500Pa that pressure, which is steadily evacuated to absolute pressure by normal pressure, in 45min, and reaction temperature is 260 DEG C, reaction time 40min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure made to be further reduced to absolute pressure 92Pa, react Temperature is 277 DEG C, reaction time 80min, modified poly ester is made, wherein the strand of modified poly ester includes terephthalic acid (TPA) chain Section, ethylene glycol segment and 3,3- diamyl -1,5-PD segment, the content of cyclic oligomer is in modified poly ester 0.35wt%, number-average molecular weight 25500, molecular weight distributing index 1.8,3,3- diamyl -1,5-PD in modified poly ester The molar content of segment is the 5% of terephthalic acid (TPA) segment molar content；
(1.2) dispersing matt agent in modified poly ester, matt agent is the mixture of calcium carbonate and unformed silica, Content of the middle matt agent in modified poly ester is 1.45wt%, and the content of unformed silica is 41wt% in matt agent；
(2) modified poly ester POY preparations；Spinning melt is squeezed out through metering, composite spinneret, is cooling, oils and winds, Main spinning technology parameter is as follows: spinning temperature: 285 DEG C；Cooling temperature: 20 DEG C；Winding speed: 3600m/min, wherein same Contain diesis shape monofilament and trilobal monofilament, diesis shape monofilament simultaneously in a branch of modified poly ester POY that spinneret squeezes out Fiber number be 0.89dtex, bending stiffness be 0.89 × 10-5cN·cm2, the fiber number of trilobal monofilament is 1.08dtex, and bending is rigid Degree is 0.88 × 10-5cN·cm2；
(3) modified poly ester FDY preparations；Spinning melt is squeezed out through metering, composite spinneret, cools down, oil, stretching, Thermal finalization and winding, main spinning technology parameter are as follows: spinning temperature is 280 DEG C；Cooling temperature is 20 DEG C；Network pressure is 0.30MPa；One roller speed is 2200m/min；One roll temperature is 76 DEG C；Two roller speeds are 3800m/min；Two roll temperatures are 125 ℃；Winding speed is 3700m/min, wherein containing diesis simultaneously in a branch of modified poly ester FDY of same spinneret extrusion Shape monofilament and trilobal monofilament, the fiber number of diesis shape monofilament are 0.88dtex, and bending stiffness is 0.68 × 10-5cN·cm2, three The fiber number of leaf monofilament is 1.07dtex, and bending stiffness is 0.88 × 10-5cN·cm2；
Wherein composite spinneret refers to same spinneret in step (2) and step (3), is equipped with double ten simultaneously on composite spinneret The microcell length ratio of font spinneret orifice and trilobal spinneret orifice, diesis shape spinneret orifice and trilobal spinneret orifice is equal to diesis Product of the ratio between the equivalent diameter of shape spinneret orifice and trilobal spinneret orifice with COEFFICIENT K, wherein equivalent diameter is the transversal of spinneret orifice The ratio of area and section girth, the value of COEFFICIENT K are 0.99, and the microcell length of trilobal spinneret orifice is 1.44mm, double ten The microcell length of font spinneret orifice is 1.44mm, equivalent diameter 0.26mm, all spinneret orifices concentric circles row on spinneret Column, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located on concentric circles, and wherein concentric circles is equidistant concentric circles, same circle Ring contains diesis shape spinneret orifice and trilobal spinneret orifice and equidistant arrangement simultaneously, on same annulus diesis shape spinneret orifice with The quantity ratio of trilobal spinneret orifice is 1:1；
(4) by modified poly ester POY and modified poly ester FDY through plying network, heating stretching, false twisting, thermal finalization and volume Around molding, polyester Wool-Like abnormal contraction composite filament is made, main spinning technology parameter is as follows: spinning speed is 800m/min；Sizing is super The rate of feeding is 3.5%；Winding overfeed rate is 5.0%；T1 is 220 DEG C；T2 is 180 DEG C；DR is 1.8；D/Y is 1.6；Network pressure is 0.2MPa, the ratio between modified poly ester POY and modified poly ester FDY fiber number is 1.4:1 in polyester Wool-Like abnormal contraction composite filament.
The color difference Δ E of final polyester Wool-Like abnormal contraction composite filament obtained is 0.190, fiber number 285dtex, and fracture is strong Degree is 2.27cN/dtex, and elongation at break 16.8%, crimp contraction 8.2%, internet pricing is 95/m, and line density is inclined Rate is 1.8%, and breaking strength CV value is 6.35%, and extension at break CV value is 7.3%, and crimp contraction coefficient of variation CV value is 7.2%, boiling water shrinkage 6.0%, oil content 1.2%, glossiness 45%, capillary parameter is 0.159.

Claims (10)

1. a kind of preparation method of polyester Wool-Like abnormal contraction composite filament, it is characterized in that: by spinning melt through metering, compound spinneret Plate squeezes out, is cooling, oiling and wind, and is made modified poly ester POY；Spinning melt is squeezed out through metering, composite spinneret, is cold But, oil, stretch, thermal finalization and winding, being made modified poly ester FDY；By POY and modified poly ester FDY warps of modified poly ester Combine network, heating stretching, false twisting, thermal finalization and coiling and molding, polyester Wool-Like abnormal contraction composite filament is made；
The spinning melt includes modified poly ester and matt agent；
The strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and branched dihydric alcohol segment, band branch Dihydric alcohol structural formula it is as follows:
Figure FDA0002142808550000011
In formula, R1And R2It is each independently selected from the straight-chain alkyl-sub that carbon atom number is 1~3, R3It is 1~5 selected from carbon atom number Alkyl, R4The alkyl for being 2~5 selected from carbon atom number；
Matt agent is the mixture of unformed titanium dioxide and unformed silica, or is calcium carbonate and unformed The mixture of silica；
On the composite spinneret simultaneously be equipped with diesis shape spinneret orifice and trilobal spinneret orifice, the diesis shape spinneret orifice with The microcell length ratio of trilobal spinneret orifice is equal to the ratio between diesis shape spinneret orifice and the equivalent diameter of trilobal spinneret orifice and is The product of number K, the equivalent diameter are the cross-sectional area of spinneret orifice and the ratio of section girth, the value model of the COEFFICIENT K Enclose is 0.97~1.03.
2. a kind of preparation method of polyester Wool-Like abnormal contraction composite filament according to claim 1, which is characterized in that described The microcell length of diesis shape spinneret orifice or trilobal spinneret orifice is 0.50~1.44mm, the diesis shape spinneret orifice or three leaves The equivalent diameter of shape spinneret orifice is 0.25~0.36mm；
All spinneret orifices concentric arrays on spinneret, the center of circle or the circumscribed circle center of circle of all spinneret orifices are located at concentric circles On, the concentric circles is equidistant concentric circles, and the spinneret orifice on same annulus equidistantly arranges.
3. a kind of preparation method of polyester Wool-Like abnormal contraction composite filament according to claim 2, which is characterized in that same Contain diesis shape spinneret orifice and trilobal spinneret orifice on annulus simultaneously, diesis shape spinneret orifice and trilobal are sprayed on same annulus The quantity ratio or trilobal spinneret orifice of wire hole and the quantity ratio of diesis shape spinneret orifice are 3~5:2.
4. the preparation method of described in any item a kind of polyester Wool-Like abnormal contraction composite filaments according to claim 1~3, feature It is, described modified poly ester POY main spinning technology parameters are as follows:
Spinning temperature: 280~290 DEG C；
Cooling temperature: 18~22 DEG C；
Winding speed: 3200~3600m/min；
Described modified poly ester FDY main spinning technology parameters are as follows:
Spinning temperature: 280~290 DEG C；
Cooling temperature: 20~25 DEG C；
Network pressure: 0.20~0.30MPa；
One roller speed: 2200~2600m/min；
One roll temperature: 75~85 DEG C；
Two roller speeds: 3650~3850m/min；
Two roll temperatures: 115~135 DEG C；
Winding speed: 3600~3800m/min；
The main spinning technology parameter of the polyester Wool-Like abnormal contraction composite filament is as follows:
Spin speed: 400~800m/min；
Overfeed rate of setting: 3.5~5.5%；
Winding overfeed rate: 2.5~5.0%；
T1:180~220 DEG C；
T2:150~180 DEG C；
DR:1.6~1.8；
D/Y:1.6~2.0；
Network pressure: 0.05~0.3MPa.
5. the preparation method of a kind of polyester Wool-Like abnormal contraction composite filament according to claim 1, it is characterized in that: polyester is imitative The composite filament that wool type abnormal contraction composite filament is modified poly ester POY and modified poly ester FDY；
Contain simultaneously in a branch of modified poly ester POY or modified poly ester FDY that same spinneret squeezes out diesis shape monofilament with Trilobal monofilament；
Matt agent is dispersed in modified poly ester；
The color difference Δ E of polyester Wool-Like abnormal contraction composite filament is less than 0.200.
6. a kind of preparation method of polyester Wool-Like abnormal contraction composite filament according to claim 5, which is characterized in that described The fiber number of diesis shape monofilament is 0.7~0.9dtex, and the fiber number of the trilobal monofilament is 0.90~1.1dtex；
The bending stiffness of the diesis shape monofilament is 0.78 × 10-5~0.90 × 10-5cN·cm2, the trilobal monofilament Bending stiffness is 0.79 × 10-5~0.96 × 10-5cN·cm2；
In the polyester Wool-Like abnormal contraction composite filament the ratio between modified poly ester POY and modified poly ester FDY fiber number be 1~ 1.5:1；
The fiber number of the polyester Wool-Like abnormal contraction composite filament is 150~300dtex, breaking strength >=2.1cN/dtex, fracture Elongation be 15.0 ± 2.0%, crimp contraction be 5.50 ± 3.0%, internet pricing be 90 ± 5/m, line density deviation ratio≤ 2.0%, breaking strength CV value≤7.0%, extension at break CV value≤8.0%, crimp contraction coefficient of variation CV value≤8.0%, Boiling water shrinkage is 5.0 ± 1.0%, and oil content is 1.0 ± 0.2%, glossiness<50%, capillary parameter>=0.15.
7. a kind of preparation method of polyester Wool-Like abnormal contraction composite filament according to claim 5 or 6, which is characterized in that Content≤0.6wt% of cyclic oligomer in the modified poly ester；
The number-average molecular weight 20000~27000 of the modified poly ester, molecular weight distributing index are 1.8~2.2；
In the modified poly ester molar content of branched dihydric alcohol segment be terephthalic acid (TPA) segment molar content 3~ 5%；
The branched dihydric alcohol is 2- Ethyl-2-Methyl -1,3- propylene glycol, 2,2- diethyl -1,3- propylene glycol, 2- fourth Base -2- ethyl -1,3- propylene glycol, 3,3- diethyl -1,5- pentanediol, 4,4- diethyl -1,7- heptandiol, 4,4- bis- (1,-first Base ethyl) -1,7- heptandiol, 3,3- dipropyl -1,5- pentanediol, 4,4- dipropyl -1,7- heptandiol, 4- methyl -4- (1,1- Dimethyl ethyl) -1,7- heptandiol, 3- methyl -3- amyl -1,6-HD or 3,3- diamyl -1,5- pentanediol.
8. a kind of preparation method of polyester Wool-Like abnormal contraction composite filament according to claim 7, which is characterized in that described Modified poly ester the preparation method comprises the following steps: by terephthalic acid (TPA), ethylene glycol and the branched dihydric alcohol after mixing first it is laggard Row esterification and polycondensation reaction obtain modified poly ester；Specific step is as follows:
(1) esterification；
Terephthalic acid (TPA), ethylene glycol and the branched dihydric alcohol are made into slurry, catalyst, delustering agent and stabilizer is added After mixing, pressurization carries out esterification in nitrogen atmosphere, and moulding pressure is normal pressure~0.3MPa, the temperature of esterification It is 250~260 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches 90% or more of theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 30~50min Interior to be steadily evacuated to absolute pressure 500Pa hereinafter, reaction temperature is 260~270 DEG C by normal pressure, the reaction time is 30~50min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is further reduced to absolute pressure 100Pa hereinafter, Reaction temperature is 275~285 DEG C, and the reaction time is 50~90min, and modified poly ester is made.
9. a kind of preparation method of polyester Wool-Like abnormal contraction composite filament according to claim 8, which is characterized in that step (1) in, the molar ratio of terephthalic acid (TPA), ethylene glycol and the branched dihydric alcohol is 1:1.2~2.0:0.03~0.06, institute The additional amount for stating catalyst is the 0.01~0.05% of terephthalic acid (TPA) weight, and the additional amount of the delustering agent is terephthalic acid (TPA) The 0.20~0.25% of weight, the additional amount of the stabilizer are the 0.01~0.05% of terephthalic acid (TPA) weight；
The catalyst is antimony oxide, antimony glycol or antimony acetate, and the delustering agent is titanium dioxide, and the stabilizer is Triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite.
10. a kind of preparation method of polyester Wool-Like abnormal contraction composite filament according to claim 5 or 6, which is characterized in that Content of the matt agent in modified poly ester is 1.0~1.5wt%, the content of unformed silica in the matt agent For 13~50wt%.
CN201711340316.5A 2017-12-14 2017-12-14 A kind of polyester Wool-Like abnormal contraction composite filament and preparation method thereof Active CN108130605B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711340316.5A CN108130605B (en) 2017-12-14 2017-12-14 A kind of polyester Wool-Like abnormal contraction composite filament and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711340316.5A CN108130605B (en) 2017-12-14 2017-12-14 A kind of polyester Wool-Like abnormal contraction composite filament and preparation method thereof

Publications (2)

Publication Number Publication Date
CN108130605A CN108130605A (en) 2018-06-08
CN108130605B true CN108130605B (en) 2019-10-15

Family

ID=62390194

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711340316.5A Active CN108130605B (en) 2017-12-14 2017-12-14 A kind of polyester Wool-Like abnormal contraction composite filament and preparation method thereof

Country Status (1)

Country Link
CN (1) CN108130605B (en)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108130613B (en) 2017-12-14 2020-05-05 江苏恒力化纤股份有限公司 Double-profile fiber and preparation method thereof
CN109629033A (en) * 2018-12-25 2019-04-16 南通东屹高新纤维科技有限公司 A kind of manufacture craft of 56 hydroscopic fast-drying fiber of super delustring novel nylon
CN109750372B (en) * 2018-12-27 2020-05-22 江苏恒力化纤股份有限公司 Wool-like polyester filament and preparation method thereof
CN109750378B (en) * 2018-12-27 2020-07-07 江苏恒力化纤股份有限公司 Silk for silk-like polyester silk and preparation method thereof
CN110983465B (en) * 2019-12-24 2021-12-21 江苏恒力化纤股份有限公司 Method for preparing self-curling elastic combined filament yarn for knitting
CN111101264B (en) * 2019-12-24 2021-06-25 江苏恒力化纤股份有限公司 Shrink-proof non-ironing wool-like fabric and preparation method thereof
CN110983597B (en) * 2019-12-29 2021-08-13 江苏恒力化纤股份有限公司 Preparation method of knitted underwear fabric
CN111041632B (en) * 2019-12-29 2021-06-25 江苏恒力化纤股份有限公司 Preparation method of worsted wool fabric
CN110983598B (en) * 2019-12-29 2021-08-13 江苏恒力化纤股份有限公司 Preparation method of vamp fabric
CN111118697B (en) * 2019-12-29 2021-06-25 江苏恒力化纤股份有限公司 Preparation method of woolen fabric
CN115323550B (en) * 2022-08-02 2024-05-14 山东岱银纺织集团股份有限公司 Composite yarn and application thereof in preparation of moisture-absorbing breathable anti-wrinkle fabric
CN116623334B (en) * 2023-07-26 2023-10-03 江苏德力化纤有限公司 Double-rotation layered deformed polyester yarn and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1826373A (en) * 2003-07-03 2006-08-30 罗狄亚特性纤维公司 Mineral fillers for enhancing opacity of thermoplastic polymers
CN201857453U (en) * 2010-10-08 2011-06-08 太仓荣文合成纤维有限公司 Spinneret plate for producing low-temperature chromophilous polyester
CN205398792U (en) * 2015-11-30 2016-07-27 扬州锦辉化纤有限公司 Profile polyester fiber
CN106319679A (en) * 2016-08-31 2017-01-11 江苏恒力化纤股份有限公司 Soft wool-like porous polyester and preparation method thereof
CN106381547A (en) * 2016-08-31 2017-02-08 江苏恒力化纤股份有限公司 Porous soft polyester fiber FDY yarn and preparing method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014088636A (en) * 2012-10-30 2014-05-15 Toray Monofilament Co Ltd Formative monofilament and binding material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1826373A (en) * 2003-07-03 2006-08-30 罗狄亚特性纤维公司 Mineral fillers for enhancing opacity of thermoplastic polymers
CN201857453U (en) * 2010-10-08 2011-06-08 太仓荣文合成纤维有限公司 Spinneret plate for producing low-temperature chromophilous polyester
CN205398792U (en) * 2015-11-30 2016-07-27 扬州锦辉化纤有限公司 Profile polyester fiber
CN106319679A (en) * 2016-08-31 2017-01-11 江苏恒力化纤股份有限公司 Soft wool-like porous polyester and preparation method thereof
CN106381547A (en) * 2016-08-31 2017-02-08 江苏恒力化纤股份有限公司 Porous soft polyester fiber FDY yarn and preparing method thereof

Also Published As

Publication number Publication date
CN108130605A (en) 2018-06-08

Similar Documents

Publication Publication Date Title
CN108130605B (en) A kind of polyester Wool-Like abnormal contraction composite filament and preparation method thereof
CN108130624A (en) A kind of polyester imitates linen look abnormal contraction composite filament and preparation method thereof
CN108385226A (en) A kind of polyester imitates cotton abnormal contraction composite filament and preparation method thereof
CN102978724B (en) Dual-component parallel composite fiber and preparation method thereof
CN103526323B (en) Copolyester melt direct-spinning controllable multiple differential shrinkage composite fiber and preparation method thereof
CN105133082A (en) Low-melting-point sheath-core-type polylactic acid composite fiber and preparation method thereof
CN102517680A (en) Multi-hole superfine denier polyamide 6 POY/FDY interlacing composite fiber, its preparation method and its device
CN103320923B (en) A kind of cationic compound imitates the production method of cotton
CN108048939B (en) One step spins elastic force composite filament and preparation method thereof
CN109735940B (en) Preparation method of deep-float linen-like polyester fiber
CN108130611A (en) It is a kind of high to stretch low-shrinkage type polyester industrial fiber and preparation method thereof
CN101748512A (en) Polyester composite fiber and method for producing same
CN106337212A (en) Side-by-side composite PBT polyester fiber and preparation method thereof
WO2021135083A1 (en) Cotton-like polyester fiber and preparation method therefor
CN105926060A (en) Melt direct spinning superfine denier polyester filament and making method thereof
CN102517660A (en) Manufacture method of super-cotton-feeling super-softness flock fiber of polyester
CN105586660A (en) A production method for hydrophilic moisture-transmitting polyester staple fibers specially used for vortex spinning
CN107904682B (en) Elastic force imitates linen-cotton polyester fiber and preparation method thereof
CN103603071A (en) Fine-denier flat yarn and manufacturing method thereof
CN103122500B (en) A kind of Splittable conjugate fiber and obtained Superfine Fibre Fabric thereof
CN103572399B (en) A kind of core-sheath compound fibre and production method thereof
CN110029408B (en) Elastic composite fiber and manufacturing method thereof
CN102877155B (en) High-simulated-cotton porous superfine-denier polyester fiber and preparation method thereof and preparation equipment
CN108624986A (en) Novel PLA/PET bi-component sheath-cores structural fibers and preparation method thereof
CN110106582A (en) A kind of preparation method of SSY-FDY composite fibre

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant