CN106757518A - A kind of long filament low melting point polyester fiber and preparation method thereof - Google Patents

A kind of long filament low melting point polyester fiber and preparation method thereof Download PDF

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Publication number
CN106757518A
CN106757518A CN201710018827.9A CN201710018827A CN106757518A CN 106757518 A CN106757518 A CN 106757518A CN 201710018827 A CN201710018827 A CN 201710018827A CN 106757518 A CN106757518 A CN 106757518A
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melting point
point polyester
low
glycol
carbon
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CN106757518B (en
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朱兴荣
高国
张盛
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Yangzhou Forwell Composite Materials Co Ltd
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Yangzhou Forwell Composite Materials Co Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/66Polyesters containing oxygen in the form of ether groups
    • C08G63/668Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/672Dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78Preparation processes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78Preparation processes
    • C08G63/82Preparation processes characterised by the catalyst used
    • C08G63/85Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
    • C08G63/86Germanium, antimony, or compounds thereof
    • C08G63/866Antimony or compounds thereof
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/28Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30Conjugate filaments; Spinnerette packs therefor
    • D01D5/34Core-skin structure; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Multicomponent Fibers (AREA)

Abstract

The present invention relates to a kind of long filament low melting point polyester fiber and preparation method thereof, long filament low melting point polyester fiber is skin-core structure, and cortex is low-melting point polyester, and sandwich layer is PET;Low-melting point polyester is made up of terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol segment, diethylene glycol (DEG) segment, molecular weight regulator and 12 carbon glycol segments containing side chain;The corresponding molecular weight regulator of molecular weight regulator segment is specially monoacid series or binary acid series;Long filament low melting point polyester fiber preparation method includes low-melting point polyester polymerization and core-sheath spinning step, obtains long filament low melting point polyester fiber.Obtained long filament low melting point polyester fiber of the invention plays fusing point and decreases and melt speed quickening, melts at once at the corresponding temperature, and melting effect is good.

Description

A kind of long filament low melting point polyester fiber and preparation method thereof
Technical field
The invention belongs to long filament low melting point polyester fiber field, it is related to a kind of long filament low melting point polyester fiber and its preparation side Method.
Background technology
Currently, Non-Woven Fabric Industry quickly grows, and especially polyester non-woven fabric industry needs a kind of fusing point more poly- than common Ester is low but has the polymer of excellent compatibility as heat-bondable fibre with conventional polyester, and generally we are by conventional polyester Modified prepare low-melting point polyester.
Copolyester with low melting point is that a kind of relatively low polyester of fusing point obtained from chemical modification is carried out to conventional polyester, due to it Structure is similar to the chemical constitution of conventional polyester, therefore it remains the part of properties of conventional polyester, has with conventional polyester good Good compatibility.Not only fusing point is low for this modified copolyester, mobility preferable, and moderate, therefore purposes is extremely wide.
Copolyester with low melting point can be made into core-skin composite fiber, be applied to the fields such as clothes, health care, it may also be used for sheep Wool blend improves the well-flushing truck energy of worsted fabric;The heat bondable fibre of particularly copolyester with low melting point spinning is applied to non-knitting Make in cloth industry, meiting powder can be made more soft, fluffy.Copolyester with low melting point can also develop into polyester hot-melt adhesive product, Premium properties with water-fastness, dry-cleaning, sand washing, easy strike-through, peel strength is high, is a kind of high-grade bonding raw material.Additionally, eutectic Point copolyesters also is used as Masterbatch, PUR, can also directly apply to the industries such as building materials, coating.
The market demand of low-melting point polyester is very big, and compared to foreign countries, the development of domestic low-melting fiber is started late, and Variety protection is single, also has certain gap with product leading in the world on raw material, technology and equipment, most of product domestic at present Product also rest on the development phase, and many difficulties are also faced on the road for realize industrialization.On the one hand existing low melting point is gathered Ester to play fusing point higher, on the other hand it to melt speed slow, the strong influence use of low-melting point polyester.Play fusing point high, melt Melt speed slow.
Long filament low melting point polyester fiber is mainly used in home textile articles for use, overcoat, jacket and auxiliary material.
The content of the invention
The purpose of the present invention is that the low-melting point polyester fusing point of the long filament low melting point polyester fiber for overcoming prior art is high, is melted Melt that speed is slow and low melting point polyester fiber in acetaldehyde it is high the problems such as, realize the production of large-scale, there is provided a kind of long filament Low melting point polyester fiber and preparation method thereof.Long filament low melting point polyester fiber of the invention is skin-core structure, and cortex is eutectic Point polyester, sandwich layer is conventional polyester, and a fusing point for obtained long filament low melting point polyester fiber decreases and melts speed and accelerates, Melt at once at the corresponding temperature, melting effect is good.
For achieving the above object, the present invention is adopted the following technical scheme that:
A kind of long filament low melting point polyester fiber of the invention, is skin-core structure;Cortex in the skin-core structure is eutectic Point polyester;Sandwich layer in the skin-core structure is PET;
The low-melting point polyester by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol segment, diethylene glycol (DEG) segment, Molecular weight regulator segment and the 12 carbon glycol segments containing side chain are constituted;
The corresponding molecular weight regulator of the molecular weight regulator segment is specially monoacid series or binary acid series;Institute Monoacid is stated for benzoic acid, p-methylbenzoic acid or p-ethylbenzoic acid, or methyl esters or ethyl ester corresponding to them, or It is saturated fatty acid or methyl esters or ethyl ester corresponding to it;Binary acid series is 1,8- naphthalenedicarboxylic acids, phthalic acid, 1, 2- pentamethylene dioctyl phthalate or 1,2- cyclohexane cyclohexanedimethanodibasics and dimethyl ester or diethylester corresponding to them;
The saturated fatty acid refers to the aliphatic acid that carbon number is 9-30.
Wherein M-phthalic acid segment, diethylene glycol (DEG) segment, the addition saboteur of the 12 carbon glycol segments containing side chain tie The regularity of structure, so as to reduce fusing point;The addition of the monoacid series in molecular weight regulator reduces dividing for low-melting point polyester Son amount, the addition of binary acid series increases space steric effect, and the group on ortho position occupies larger locus, hinders Attack to carboxyl carbon atom, is unfavorable for the growth of molecular weight, reduces the molecular weight of low-melting point polyester, widens dividing for high polymer Son amount distribution, when relative molecular weight distribution broadens, the flowing temperature of low-melting point polyester melt declines, and this is due to now molecule The temperature range that chain occurs relative displacement broadens, and especially low relative molecular mass component serves internally plasticized effect, makes to gather Ester melt takes place the temperature drop of flowing, therefore low-melting point polyester is melted rapidly at corresponding temperature, improves The melting behaviour of low-melting point polyester.Selection carbon number is the saturated fatty acid of 9-30, because the low saturated fat of carbon number The boiling point of fat acid is relatively low, can deviate from during polycondensation, influences the stability of its content;Carbon number saturated fatty acid high, its carboxylic acid Activity decrease, its extent of reaction can be influenceed.
As preferred technical scheme:
A kind of long filament low melting point polyester fiber as described above, 2.0~4.0dtex of filament number, fracture strength >= 3.00cN/dtex, elongation at break is 40.0 ± 5.0%;Line density deviation ratio≤1.0%;The core-skin face of the skin-core structure Product is than being 40~60:60~40.
A kind of long filament low melting point polyester fiber as described above, the fusing point of the low-melting point polyester 100 DEG C~170 DEG C it Between;When programming rate is 5 DEG C/min, more than the fusing point in the range of 20 DEG C, low-melting point polyester melting degree >=82%;It is described Several molecular weight of low-melting point polyester are 17000-35000, molecular weight distributing index D=2.4~4.1 of the low-melting point polyester. The fusing point of the low-melting point polyester refers to that it plays fusing point.
A kind of long filament low melting point polyester fiber as described above, monoacid segment in the molecular weight regulator segment Content is the 0.01%~0.05% of phthalic acid segment molal quantity, and binary acid segment contains in the molecular weight regulator segment Measure is the 1.5%~3% of phthalic acid segment molal quantity;Described phthalic acid is terephthalic acid (TPA) and M-phthalic acid;
A kind of long filament low melting point polyester fiber as described above, the 12 carbon glycol segments containing side chain refer to side chain position On a non-end group carbon in 12 carbon glycol segments and side chain is to contain 5-10 12 carbon of the linear carbon chain of carbon atom Glycol segment;The corresponding 12 carbon glycol containing side chain of 12 carbon glycol segments containing side chain are specially 2- amyl groups -1,12 12 Carbon glycol, the carbon glycol of 2- hexyls -1,12 12, the carbon glycol of 2- heptyl -12 12, the carbon glycol of 2- octyl groups -1,12 12,2- nonyls The carbon glycol of base -1,12 12, the carbon glycol of 2- decyls -1,12 12, the carbon glycol of 3- amyl groups -1,12 12,3- hexyls -1,12 12 Carbon glycol, the carbon glycol of 3- heptyl -12 12, the carbon glycol of 3- octyl groups -1,12 12, the carbon glycol of 3- nonyls -1,12 12, the 3- last of the ten Heavenly stems The carbon glycol of base -1,12 12, the carbon glycol of 4- amyl groups -1,12 12, the carbon glycol of 4- hexyls -1,12 12, the carbon of 4- heptyl -12 12 Glycol, the carbon glycol of 4- octyl groups -1,12 12, the carbon glycol of 4- nonyls -1,12 12, the carbon glycol of 4- decyls -1,12 12,5- penta The carbon glycol of base -1,12 12, the carbon glycol of 5- hexyls -1,12 12, the carbon glycol of 5- heptyl -12 12, the carbon of 5- octyl groups -1,12 12 Glycol, the carbon glycol of 5- nonyls -1,12 12, the carbon glycol of 5- decyls -1,12 12, the carbon glycol of 6- amyl groups -1,12 12,6- oneself The carbon glycol of base -1,12 12, the carbon glycol of 6- heptyl -12 12, the carbon glycol of 6- octyl groups -1,12 12, the carbon of 6- nonyls -1,12 12 One or more of glycol or the carbon glycol of 6- decyls -1,12 12;The 12 carbon glycol segments containing side chain are terephthaldehyde The 5~10% of sour segment molal quantity.
The present invention also provides a kind of preparation method of long filament low melting point polyester fiber, and low-melting point polyester and PET are through measuring, squeezing Go out, cool down, oiling, stretching, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin is obtained;
A) low-melting point polyester polymerization;
(1) by terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon containing side chain Glycol carries out esterification;
(2) and then, carry out polycondensation reaction, be obtained low-melting point polyester;
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer.
A kind of preparation method of long filament low melting point polyester fiber as described above, it is terephthalic acid (TPA), M-phthalic acid, two sweet The mol ratio of alcohol, the 12 carbon glycol containing side chain and ethylene glycol is 1:0.4~0.6:0.1~0.3:0.05~0.1:1.8~ 2.5。
A kind of preparation method of long filament low melting point polyester fiber as described above, the specific steps of low-melting point polyester polymerization For:
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon two containing side chain After alcohol is made into slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure~0.3MPa, temperature is 230 DEG C~250 DEG C, be esterification terminal when the quantity of distillate of the water in esterification reaches more than the 90% of theoretical value, is obtained To esterification products;
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure; The staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature control at 260~270 DEG C, the reaction time is 30~ 50 minutes;Then proceed to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure and be less than 100Pa, reaction temperature control in 50~90 minutes reaction time, is obtained low-melting point polyester at 275~280 DEG C.
The main spinning technology parameter of long filament low melting point polyester fiber FDY is:
Spinning temperature:262-275 DEG C of cortex, 280-288 DEG C of sandwich layer;
Chilling temperature:25-30℃;
One roller speed:2000-2200m/min;
One roll temperature:65-70℃;
Two roller speeds:2500-2700m/min;
Two roll temperatures:70-75℃;
Winding speed:2500-2700m/min.
A kind of preparation method of long filament low melting point polyester fiber as described above, the catalyst is antimony oxide, second Glycol antimony or antimony acetate, catalyst charge are the 0.01%~0.05% of phthalic acid gross weight;The stabilizer is phosphoric acid Triphenylmethyl methacrylate, trimethyl phosphate or Trimethyl phosphite, stabilizer addition be the phthalic acid gross weight 0.01%~ 0.05%.
Principle of the invention is:
Unbranched for without modified component, the conventional polyester without molecular weight regulator, its molecular chain structure is to contain phenyl ring The regular linear macromolecule of structure, the functional group's marshalling on strand, regularity is good, and flexible poor, crystallinity is high, this A little characteristics hinder the reduction of fusing point, thus melt temperature is high.
The raw material of polyester is terephthalic acid (TPA) segment and ethylene glycol segment, and M-phthalic acid segment, two sweet is added wherein Alcohol segment, molecular weight regulator saboteur's structure, make it be changed into unordered chaotic structure from the ordered structure of high-sequential, The addition of phthalic acid segment changes the ratio and size between the different Asia macro crystallization forms of polyester, makes crystallizing polyester Difficulty, is intended to unformed mode and exists;The addition of diethylene glycol (DEG) segment increases the compliance of copolyesters macromolecular chain, reduces molten Point;The addition of the monoacid series in molecular weight regulator reduces the molecular weight of low-melting point polyester, the addition of binary acid series Increase space steric effect, the group on ortho position occupies larger locus, hinders the attack to carboxyl carbon atom, no Beneficial to the growth of molecular weight, the molecular weight of low-melting point polyester is reduced, widen the molecular weight distribution of high polymer, work as relative molecular weight When distribution broadens, the flowing temperature of low-melting point polyester melt declines, and this is because now strand occurs the temperature of relative displacement Scope broadens, and especially low relative molecular mass component serves internally plasticized effect, makes polyester fondant that flowing takes place Temperature drop, therefore low-melting point polyester is melted rapidly at corresponding temperature, the melting behaviour of low-melting point polyester is improve, In 5 DEG C/min of programming rate, more than the fusing point in the range of 20 DEG C, low-melting point polyester melting degree >=82% shows as melting Melt speed quickening;And the low-melting point polyester of routine is under same Elevated Temperature Conditions, melting degree≤20% in this temperature range; Reducing low-melting point polyester part macromolecular weight can reduce softening and flowing temperature, be conducive to low melting point to infiltrate and glued Thing, increased bond effect;The addition of the 12 carbon glycol segments containing side chain, when temperature is higher than glass transition temperature, side chain elder generation In backbone motion, the increasing degree of free volume is far longer than the characteristic of unbranched polyester macromolecule chain, be conducive to melting The increase of speed;By M-phthalic acid segment, diethylene glycol (DEG) segment, molecular weight regulator and 12 carbon glycol segments containing side chain etc. Modified component adds prepared low-melting point polyester, and with rising, melting temperature is low, the advantages of melting speed is fast.Long filament low melting point is gathered Ester fiber key property is that coating laminating effect is good, with good morphological stability and resilience, it is easy to which speed is melted in control.
Beneficial effect:
(1) the obtained long filament low melting point polyester fiber 2.0~4.0dtex of filament number of the present invention, fracture strength >= 3.00cN/dtex, elongation at break is 40.0 ± 5.0%;Line density deviation ratio≤1.0%;Coating laminating effect is good, with good Good morphological stability and resilience, it is easy to which speed is melted in control.
(2) raw material of the obtained low-melting point polyester of the present invention is terephthalic acid (TPA) segment and ethylene glycol segment, in macromolecular Contain M-phthalic acid segment, diethylene glycol (DEG) segment, molecular weight regulator and 12 carbon glycol containing side chain, prepared low melting point Polyester, with rise melting temperature it is low, melting speed it is fast the advantages of.
(3) raw material of the obtained low-melting point polyester of the present invention is terephthalic acid (TPA) segment and ethylene glycol segment, and molecular weight is adjusted The addition of the monoacid series in section agent reduces the molecular weight of low-melting point polyester, and the addition of binary acid series increases steric hindrance Effect, the group on ortho position occupies larger locus, hinders the attack to carboxyl carbon atom, is unfavorable for molecular weight Increase, reduce the molecular weight of low-melting point polyester, widen the molecular weight distribution of high polymer, when relative molecular weight distribution broadens, The flowing temperature of low-melting point polyester melt declines, and this is because the temperature range that now strand occurs relative displacement broadens, especially It is that low relative molecular mass component serves internally plasticized effect, makes polyester fondant that the temperature drop of flowing takes place, because This enables low-melting point polyester to be melted rapidly at corresponding temperature, improves the melting behaviour of low-melting point polyester, in programming rate 5 DEG C/min when, more than the fusing point in the range of 20 DEG C, low-melting point polyester melting degree >=82% shows as melting speed and accelerates; And the low-melting point polyester of routine is under same Elevated Temperature Conditions, melting degree≤20% in this temperature range;Reduce low melting point Polyester portion macromolecular weight can reduce softening and flowing temperature, be conducive to low melting point to infiltrate adherend, increased viscous Knot effect.
(4) raw material of the obtained low-melting point polyester of the present invention is terephthalic acid (TPA) segment and ethylene glycol segment, containing side chain The addition of 12 carbon glycol segments, when temperature is higher than glass transition temperature, side chain makes the increase of free volume prior to backbone motion Amplitude is far longer than the characteristic of unbranched polyester macromolecule chain, effectively reduces fusing point.
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 Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, art technology Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Fixed scope.
Embodiment 1
A kind of preparation method of long filament low melting point polyester fiber:
A) low-melting point polyester polymerization;
(1) esterification;
Terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), benzoic acid and the carbon glycol of 2- amyl groups -1,12 12 are matched somebody with somebody Into after slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure, temperature is 230 DEG C, works as esterification It is esterification terminal when the quantity of distillate of the water in reaction reaches more than the 90% of theoretical value, obtains esterification products;Wherein, to benzene Dioctyl phthalate, M-phthalic acid, diethylene glycol (DEG), the 12 carbon glycol containing side chain, the mol ratio of ethylene glycol are 1:0.4:0.1:0.05: 1.8;The addition of benzoic acid is the 0.01% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure; The staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 260 DEG C, the reaction time is 30 minutes to temperature control;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Degree control in 50 minutes reaction time, is obtained low-melting point polyester at 275 DEG C.Catalyst is antimony oxide, and catalyst charge is The 0.01% of phthalic acid gross weight.Stabilizer is triphenyl phosphate, and stabilizer addition is phthalic acid gross weight 0.01%.
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer, low-melting point polyester and PET is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, and long filament low melting point polyester fiber FDY of core-skin is obtained;
Mainly spinning technology parameter is:
Spinning temperature:262 DEG C of cortex, 280 DEG C of sandwich layer;
Chilling temperature:25℃;
One roller speed:2000m/min;
One roll temperature:65℃;
Two roller speeds:2500m/min;
Two roll temperatures:70℃;
Winding speed:2500m/min.
The long filament low melting point polyester fiber prepared by above-mentioned steps is skin-core structure;Cortex in skin-core structure is eutectic Point polyester;Sandwich layer in skin-core structure is PET;Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol Segment, diethylene glycol (DEG) segment, benzoic acid segment and the carbon glycol segment of 2- amyl groups -1,12 12 composition;Benzoic acid segment is benzene two 0.01%, 2- amyl group -1 of formic acid segment molal quantity, 120 two carbon glycol segments are the 5% of terephthalic acid (TPA) segment molal quantity; The fusing point of low-melting point polyester is at 100 DEG C;It is 5 DEG C/min in programming rate, when more than low-melting point polyester fusing point in the range of 20 DEG C, The melting degree of low-melting point polyester is 82%;The number-average molecular weight of low-melting point polyester is 17000, the molecular weight point of low-melting point polyester Cloth index D=2.4.The filament number 2.0dtex of long filament low melting point polyester fiber, fracture strength is 3.00cN/dtex, and fracture is stretched Rate long is 35.0%;Line density deviation ratio is 1.0%;The core-skin area ratio of skin-core structure is 40:60.
Embodiment 2
A kind of preparation method of long filament low melting point polyester fiber:
A) low-melting point polyester polymerization;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), p-methylbenzoic acid and the carbon of 2- hexyls -1,12 12 After glycol is made into slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is 0.3MPa, temperature is 250 DEG C, it is esterification terminal when the quantity of distillate of the water in esterification reaches more than the 90% of theoretical value, obtain esterification products; Wherein, terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), 2- hexyl -1,120 two carbon glycol, the mol ratio of ethylene glycol are 1: 0.6:0.3:0.1:2.5;The addition of p-methylbenzoic acid is the 0.5% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure; The staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 270 DEG C, the reaction time is 50 minutes to temperature control;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Degree control in 90 minutes reaction time, is obtained low-melting point polyester at 280 DEG C.Catalyst is antimony glycol, and catalyst charge is benzene The 0.05% of dioctyl phthalate gross weight.Stabilizer is trimethyl phosphate, and stabilizer addition is the 0.05% of phthalic acid gross weight.
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer, low-melting point polyester and PET is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, and long filament low melting point polyester fiber FDY of core-skin is obtained;
Mainly spinning technology parameter is:
Spinning temperature:275 DEG C of cortex, 288 DEG C of sandwich layer;
Chilling temperature:30℃;
One roller speed:2200m/min;
One roll temperature:70℃;
Two roller speeds:2700m/min;
Two roll temperatures:75℃;
Winding speed:2700m/min.
The long filament low melting point polyester fiber prepared by above-mentioned steps is skin-core structure;Cortex in skin-core structure is eutectic Point polyester;Sandwich layer in skin-core structure is PET;Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol Segment, diethylene glycol (DEG) segment, p-methylbenzoic acid segment and the carbon glycol segment of 2- hexyls -1,12 12 composition;To methylbenzene first Sour segment is 0.5%, 2- hexyl -1 of phthalic acid segment molal quantity, and 120 two carbon glycol segments rub for terephthalic acid (TPA) segment The 10% of that number;The fusing point of low-melting point polyester is at 120 DEG C;It is 5 DEG C/min in programming rate, more than low-melting point polyester fusing point 20 DEG C In the range of when, the melting degree of low-melting point polyester is 84%;The number-average molecular weight of low-melting point polyester is 35000, and low melting point is gathered The molecular weight distributing index D=4.1 of ester.The filament number 4.0dtex of long filament low melting point polyester fiber, fracture strength is 3.30cN/dtex, elongation at break is 45.0%;Line density deviation ratio is 0.08%;The core-skin area ratio of skin-core structure is 60: 40。
Embodiment 3
A kind of preparation method of long filament low melting point polyester fiber:
A) low-melting point polyester polymerization;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), p-ethylbenzoic acid and the carbon two of 2- heptyl -12 12 After alcohol is made into slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is 0.1MPa, temperature is 240 DEG C, It is esterification terminal when the quantity of distillate of the water in esterification reaches more than the 90% of theoretical value, obtains esterification products;Its In, terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), the carbon glycol of 2- heptyl -12 12, the mol ratio of ethylene glycol are 1:0.5: 0.2:0.07:2;The addition of p-ethylbenzoic acid is the 0.1% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure; The staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 265 DEG C, the reaction time is 40 minutes to temperature control;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Degree control in 60 minutes reaction time, is obtained low-melting point polyester at 278 DEG C.Catalyst is antimony acetate, and catalyst charge is benzene two The 0.03% of formic acid gross weight.Stabilizer is Trimethyl phosphite, and stabilizer addition is the 0.02% of phthalic acid gross weight.
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer, low-melting point polyester and PET is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, and long filament low melting point polyester fiber FDY of core-skin is obtained;
Mainly spinning technology parameter is:
Spinning temperature:270 DEG C of cortex, 284 DEG C of sandwich layer;
Chilling temperature:28℃;
One roller speed:2100m/min;
One roll temperature:68℃;
Two roller speeds:2600m/min;
Two roll temperatures:71℃;
Winding speed:2600m/min.
The long filament low melting point polyester fiber prepared by above-mentioned steps is skin-core structure;Cortex in skin-core structure is eutectic Point polyester;Sandwich layer in skin-core structure is PET;Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol Segment, diethylene glycol (DEG) segment, p-ethylbenzoic acid segment and the carbon glycol segment of 2- heptyl -12 12 composition;P-ethylbenzoic acid Segment is terephthalic acid (TPA) segment molal quantity for the carbon glycol segment of 0.1%, 2- heptyl -12 12 of phthalic acid segment molal quantity 7%;The fusing point of low-melting point polyester is at 150 DEG C;It is 5 DEG C/min, more than low-melting point polyester fusing point 20 DEG C of model in programming rate When enclosing interior, the melting degree of low-melting point polyester is 83%;The number-average molecular weight of low-melting point polyester is 25000, low-melting point polyester Molecular weight distributing index D=4.The filament number 2.5dtex of long filament low melting point polyester fiber, fracture strength is 3.20cN/dtex, Elongation at break is 40.0%;Line density deviation ratio≤1.0%;The core-skin area ratio of skin-core structure is 50:50.
Embodiment 4
A kind of preparation method of long filament low melting point polyester fiber:
A) low-melting point polyester polymerization;
(1) esterification;
Terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), pelargonic acid and the carbon glycol of 2- octyl groups -1,12 12 are matched somebody with somebody Into after slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is 0.2MPa, temperature is 245 DEG C, works as ester It is esterification terminal when the quantity of distillate for changing the water in reaction reaches more than the 90% of theoretical value, obtains esterification products;Wherein, it is right Phthalic acid, M-phthalic acid, diethylene glycol (DEG), the carbon glycol of 2- octyl groups -1,12 12, the mol ratio of ethylene glycol are 1:0.5:0.25: 0.08:2.2;The addition of pelargonic acid is the 0.2% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure; The staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 260 DEG C, the reaction time is 45 minutes to temperature control;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Degree control in 70 minutes reaction time, is obtained low-melting point polyester at 275 DEG C.Catalyst is antimony oxide, and catalyst charge is The 0.04% of phthalic acid gross weight.Stabilizer is triphenyl phosphate, and stabilizer addition is phthalic acid gross weight 0.03%.
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer, low-melting point polyester and PET is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, and long filament low melting point polyester fiber FDY of core-skin is obtained;
Mainly spinning technology parameter is:
Spinning temperature:268 DEG C of cortex, 286 DEG C of sandwich layer;
Chilling temperature:28℃;
One roller speed:2050m/min;
One roll temperature:67℃;
Two roller speeds:2650m/min;
Two roll temperatures:72℃;
Winding speed:2650m/min.
The long filament low melting point polyester fiber prepared by above-mentioned steps is skin-core structure;Cortex in skin-core structure is eutectic Point polyester;Sandwich layer in skin-core structure is PET;Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol Segment, diethylene glycol (DEG) segment, pelargonic acid segment and the carbon glycol segment of 2- octyl groups -1,12 12 composition;Pelargonic acid segment is benzene two 0.2%, 2- octyl group -1 of formic acid segment molal quantity, 120 two carbon glycol segments are the 8% of terephthalic acid (TPA) segment molal quantity;It is low The fusing point of melt polyester is at 130 DEG C;It is 5 DEG C/min in programming rate, it is low when more than low-melting point polyester fusing point in the range of 20 DEG C The melting degree of melt polyester is 84%;The number-average molecular weight of low-melting point polyester is 30000, the molecular weight distribution of low-melting point polyester Index D=3.5.The filament number 2.5dtex of long filament low melting point polyester fiber, fracture strength is 3.30cN/dtex, extension at break Rate is 42.0%;Line density deviation ratio is 0.7%;The core-skin area ratio of the skin-core structure is 45:55.
Embodiment 5
A kind of preparation method of long filament low melting point polyester fiber:
A) low-melting point polyester polymerization;
(1) esterification;
Terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), capric acid and the carbon glycol of 2- nonyls -1,12 12 are made into After slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is 0.1MPa, temperature is 245 DEG C, works as esterification It is esterification terminal when the quantity of distillate of the water in reaction reaches more than the 90% of theoretical value, obtains esterification products;Wherein, to benzene Dioctyl phthalate, M-phthalic acid, diethylene glycol (DEG), the carbon glycol of 2- nonyls -1,12 12, the mol ratio of ethylene glycol are 1:0.5:0.15: 0.09:2.3;The addition of capric acid is the 0.4% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure; The staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 265 DEG C, the reaction time is 45 minutes to temperature control;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Degree control in 80 minutes reaction time, is obtained low-melting point polyester at 279 DEG C.Catalyst is antimony oxide, and catalyst charge is The 0.04% of phthalic acid gross weight.Stabilizer is triphenyl phosphate, and stabilizer addition is phthalic acid gross weight 0.04%.
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer, low-melting point polyester and PET is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, and long filament low melting point polyester fiber FDY of core-skin is obtained;
Mainly spinning technology parameter is:
Spinning temperature:271 DEG C of cortex, 282 DEG C of sandwich layer;
Chilling temperature:26℃;
One roller speed:2000m/min;
One roll temperature:65℃;
Two roller speeds:2700m/min;
Two roll temperatures:75℃;
Winding speed:2700m/min.
The long filament low melting point polyester fiber prepared by above-mentioned steps is skin-core structure;Cortex in skin-core structure is eutectic Point polyester;Sandwich layer in skin-core structure is PET;Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol Segment, diethylene glycol (DEG) segment, capric acid segment and the carbon glycol segment of 2- nonyls -1,12 12 composition;Capric acid segment is phthalic acid 0.4%, 2- nonyl -1 of segment molal quantity, 120 two carbon glycol segments are the 9% of terephthalic acid (TPA) segment molal quantity;Low melting point The fusing point of polyester is at 170 DEG C;It is 5 DEG C/min in programming rate, when more than low-melting point polyester fusing point in the range of 20 DEG C, low melting point The melting degree of polyester is 84%;The number-average molecular weight of low-melting point polyester is 30000, the molecular weight distributing index of low-melting point polyester D=3.5.The filament number 4.0dtex of long filament low melting point polyester fiber, fracture strength is 3.20cN/dtex, and elongation at break is 43.0%;Line density deviation ratio is 0.7%;The core-skin area ratio of the skin-core structure is 55:45.
Embodiment 6
A kind of preparation method of long filament low melting point polyester fiber:
A) low-melting point polyester polymerization;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), benzoic acid formicester and the carbon two of 2- decyls -1,12 12 After alcohol is made into slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is 0.3MPa, temperature is 250 DEG C, It is esterification terminal when the quantity of distillate of the water in esterification reaches more than the 90% of theoretical value, obtains esterification products;Its In, terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), 2- decyl -1,120 two carbon glycol, the mol ratio of ethylene glycol are 1:0.4: 0.3:0.1:1.8;The addition of benzoic acid formicester is the 0.09% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure; The staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 270 DEG C, the reaction time is 30 minutes to temperature control;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Degree control in 90 minutes reaction time, is obtained low-melting point polyester at 275 DEG C.Catalyst is antimony glycol, and catalyst charge is benzene The 0.05% of dioctyl phthalate gross weight.Stabilizer is triphenyl phosphate, and stabilizer addition is the 0.01% of phthalic acid gross weight.
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer, low-melting point polyester and PET is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, and long filament low melting point polyester fiber FDY of core-skin is obtained;
Mainly spinning technology parameter is:
Spinning temperature:262 DEG C of cortex, 280 DEG C of sandwich layer;
Chilling temperature:25℃;
One roller speed:2200m/min;
One roll temperature:65℃;
Two roller speeds:2700m/min;
Two roll temperatures:75℃;
Winding speed:2500m/min.
The long filament low melting point polyester fiber prepared by above-mentioned steps is skin-core structure;Cortex in skin-core structure is eutectic Point polyester;Sandwich layer in skin-core structure is PET;Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol Segment, diethylene glycol (DEG) segment, benzoic acid formicester segment and the carbon glycol segment of 2- decyls -1,12 12 composition;Benzoic acid formicester chain Section is 0.09%, 2- decyl -1 of phthalic acid segment molal quantity, and 120 two carbon glycol segments are terephthalic acid (TPA) segment mole Several 10%;The fusing point of low-melting point polyester is between 160 DEG C;It is 5 DEG C/min in programming rate, more than low-melting point polyester fusing point 20 When in the range of DEG C, the melting degree of low-melting point polyester is 82%;The number-average molecular weight of low-melting point polyester is 28000, low melting point The molecular weight distributing index D=3 of polyester.The filament number 3.5dtex of long filament low melting point polyester fiber, fracture strength is 3.30cN/dtex, elongation at break is 38.0%;Line density deviation ratio is 0.5%;The core-skin area ratio of skin-core structure is 45: 55。
Embodiment 7
A kind of preparation method of long filament low melting point polyester fiber:
A) low-melting point polyester polymerization;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), benzoic acid second fat and the carbon two of 3- amyl groups -1,12 12 After alcohol is made into slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure, temperature is 250 DEG C, when It is esterification terminal when the quantity of distillate of the water in esterification reaches more than the 90% of theoretical value, obtains esterification products;Wherein, Terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), the carbon glycol of 3- amyl groups -1,12 12, the mol ratio of ethylene glycol are 1:0.4:0.3: 0.05:1.8;The addition of benzoic acid second fat is the 0.5% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure; The staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 270 DEG C, the reaction time is 30 minutes to temperature control;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Degree control in 50 minutes reaction time, is obtained low-melting point polyester at 275 DEG C.Catalyst is antimony acetate, and catalyst charge is benzene two The 0.05% of formic acid gross weight.Stabilizer is Trimethyl phosphite, and stabilizer addition is the 0.01% of phthalic acid gross weight.
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer, low-melting point polyester and PET is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, and long filament low melting point polyester fiber FDY of core-skin is obtained;
Mainly spinning technology parameter is:
Spinning temperature:2685 DEG C of cortex, 284 DEG C of sandwich layer;
Chilling temperature:28℃;
One roller speed:2100m/min;
One roll temperature:67℃;
Two roller speeds:2600m/min;
Two roll temperatures:71℃;
Winding speed:2600m/min.
The long filament low melting point polyester fiber prepared by above-mentioned steps is skin-core structure;Cortex in skin-core structure is eutectic Point polyester;Sandwich layer in skin-core structure is PET;Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol Segment, diethylene glycol (DEG) segment, benzoic acid second fat chain section and the carbon glycol segment of 3- amyl groups -1,12 12 composition;Benzoic acid second fat chain Section is 0.5%, 3- amyl group -1 of phthalic acid segment molal quantity, and 120 two carbon glycol segments are terephthalic acid (TPA) segment molal quantity 5%;The fusing point of low-melting point polyester is at 130 DEG C;It is 5 DEG C/min, more than low-melting point polyester fusing point 20 DEG C of model in programming rate When enclosing interior, the melting degree of low-melting point polyester is 85%;The number-average molecular weight of low-melting point polyester is 25000, low-melting point polyester Molecular weight distributing index D=3.8.The filament number 2.8dtex of long filament low melting point polyester fiber, fracture strength is 3.30cN/ Dtex, elongation at break is 41.0%;Line density deviation ratio≤1.0%;The core-skin area ratio of skin-core structure is 54:46.
Embodiment 8-44
A kind of preparation method of long filament low melting point polyester fiber:
A) low-melting point polyester polymerization;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon two containing side chain After alcohol is made into slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is 0.2MPa, temperature is 230 DEG C, It is esterification terminal when the quantity of distillate of the water in esterification reaches more than the 90% of theoretical value, obtains esterification products;Its In, terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), the 12 carbon glycol containing side chain, the mol ratio of ethylene glycol are 1:0.5: 0.25:0.08:2.2;The addition of molecular weight regulator is the 0.3% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure; The staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 265 DEG C, the reaction time is 40 minutes to temperature control;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Degree control in 70 minutes reaction time, is obtained low-melting point polyester at 280 DEG C.Catalyst is antimony glycol, and catalyst charge is benzene The 0.03% of dioctyl phthalate gross weight.Stabilizer is triphenyl phosphate, and stabilizer addition is the 0.02% of phthalic acid gross weight.
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer, low-melting point polyester and PET is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, and long filament low melting point polyester fiber FDY of core-skin is obtained;
Mainly spinning technology parameter is:
Spinning temperature:275 DEG C of cortex, 284 DEG C of sandwich layer;
Chilling temperature:28℃;
One roller speed:2200m/min;
One roll temperature:65℃;
Two roller speeds:2700m/min;
Two roll temperatures:75℃;
Winding speed:2500m/min.
The long filament low melting point polyester fiber prepared by above-mentioned steps is skin-core structure;Cortex in skin-core structure is eutectic Point polyester;Sandwich layer in skin-core structure is PET;Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol Segment, diethylene glycol (DEG) segment, molecular weight regulator segment and the 12 carbon glycol segments containing side chain composition.
Molecular-weight adjusting and the fusing point of finally prepd low-melting point polyester, the number used in the above embodiment of the present invention are The acetaldehyde of molecular weight and molecualr weight distribution and long filament low melting point polyester fiber, filament number, fracture strength and core-skin knot The core-skin area of structure than etc. particular product performance parameters it is as shown in the table:

Claims (9)

1. a kind of long filament low melting point polyester fiber, it is characterized in that:The long filament low melting point polyester fiber is skin-core structure;The skin Cortex in cored structure is low-melting point polyester;Sandwich layer in the skin-core structure is PET;
The low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol segment, diethylene glycol (DEG) segment, molecule Amount conditioning agent segment and the composition of the 12 carbon glycol segments containing side chain;
The corresponding molecular weight regulator of the molecular weight regulator segment is specially monoacid series or binary acid series;Described one First acid is benzoic acid, p-methylbenzoic acid or p-ethylbenzoic acid, or methyl esters or ethyl ester corresponding to them, or is full With aliphatic acid or methyl esters or ethyl ester corresponding to it;The binary acid series is 1,8- naphthalenedicarboxylic acids, phthalic acid, 1,2- rings Pentane dioctyl phthalate or 1,2- cyclohexane cyclohexanedimethanodibasics and dimethyl ester or diethylester corresponding to them;
The saturated fatty acid refers to the aliphatic acid that carbon number is 9-30.
2. a kind of long filament low melting point polyester fiber according to claim 1, it is characterised in that the long filament low-melting point polyester 2.0~the 4.0dtex of filament number of fiber, fracture strength >=3.00cN/dtex, elongation at break is 40.0 ± 5.0%;Line is close Degree deviation ratio≤1.0%;The core-skin area ratio of the skin-core structure is 40~60:60~40.
3. a kind of long filament low melting point polyester fiber according to claim 1, it is characterised in that the low-melting point polyester it is molten O'clock between 100 DEG C~170 DEG C;When programming rate is 5 DEG C/min, more than the fusing point in the range of 20 DEG C, low-melting point polyester Melting degree >=82%;Several molecular weight of the low-melting point polyester are 17000-35000, the molecular weight point of the low-melting point polyester Cloth index D=2.4~4.1.
4. a kind of long filament low melting point polyester fiber according to claim 1, it is characterised in that the molecular weight regulator chain The content of the monoacid segment in section is the 0.01%~0.05% of phthalic acid segment molal quantity, the molecular weight regulator chain The content of binary acid segment is the 1.5%~3% of phthalic acid segment molal quantity in section.
5. a kind of long filament low melting point polyester fiber according to claim 1, it is characterised in that 12 carbon containing side chain Glycol segment refers to side chain on a non-end group carbon in 12 carbon glycol segments and side chain is to contain 5-10 carbon atom Linear carbon chain 12 carbon glycol segments;The corresponding 12 carbon glycol containing side chain of 12 carbon glycol segments containing side chain are specific It is the carbon glycol of 2- amyl groups -1,12 12, the carbon glycol of 2- hexyls -1,12 12, the carbon glycol of 2- heptyl -12 12,2- octyl groups -1,12 12 carbon glycol, the carbon glycol of 2- nonyls -1,12 12, the carbon glycol of 2- decyls -1,12 12, the carbon glycol of 3- amyl groups -1,12 12, The carbon glycol of 3- hexyls -1,12 12, the carbon glycol of 3- heptyl -12 12, the carbon glycol of 3- octyl groups -1,12 12,3- nonyls -1,12 ten Two carbon glycol, the carbon glycol of 3- decyls -1,12 12, the carbon glycol of 4- amyl groups -1,12 12, the carbon glycol of 4- hexyls -1,12 12,4- The carbon glycol of heptyl -12 12, the carbon glycol of 4- octyl groups -1,12 12, the carbon glycol of 4- nonyls -1,12 12,4- decyls -1,12 12 Carbon glycol, the carbon glycol of 5- amyl groups -1,12 12, the carbon glycol of 5- hexyls -1,12 12, the carbon glycol of 5- heptyl -12 12,5- are pungent The carbon glycol of base -1,12 12, the carbon glycol of 5- nonyls -1,12 12, the carbon glycol of 5- decyls -1,12 12,6- amyl groups -1,12 12 Carbon glycol, the carbon glycol of 6- hexyls -1,12 12, the carbon glycol of 6- heptyl -12 12, the carbon glycol of 6- octyl groups -1,12 12,6- nonyls One or more of the carbon glycol of base -1,12 12 or the carbon glycol of 6- decyls -1,12 12;The 12 carbon glycol chains containing side chain Section is the 5~10% of terephthalic acid (TPA) segment molal quantity.
6. according to a kind of preparation method of any described long filament low melting point polyester fibers of claim 1-5, it is characterized in that including Step:Low-melting point polyester and PET are through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, and the long filament that core-skin is obtained is low Melt polyester fibers FDY;
A) low-melting point polyester polymerization;
(1) by terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon glycol containing side chain Carry out esterification;
(2) and then, carry out polycondensation reaction, be obtained low-melting point polyester;
B) spinning;
Using core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer.
7. a kind of preparation method of long filament low melting point polyester fiber according to claim 6, it is characterised in that terephthaldehyde The mol ratio of acid, M-phthalic acid, diethylene glycol (DEG), the 12 carbon glycol containing side chain and ethylene glycol is 1:0.4~0.6:0.1~0.3: 0.05~0.1:1.8~2.5.
8. the preparation method of a kind of long filament low melting point polyester fiber according to claim 6, it is characterised in that low melting point is gathered Polyisocyanate polyaddition is concretely comprised the following steps:
(1) esterification;
Terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon glycol containing side chain are matched somebody with somebody Into after slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure~0.3MPa, temperature is 230 DEG C ~250 DEG C, be esterification terminal when the quantity of distillate of the water in esterification reaches more than the 90% of theoretical value, is esterified Product;
(2) polycondensation reaction;
Then, in the presence of catalyst and stabilizer, the polycondensation reaction in low vacuum stage is started under conditions of negative pressure;The rank Section pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 260~270 DEG C, the reaction time is 30~50 points to temperature control Clock;Then proceed to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is down to absolute pressure and be less than 100Pa, instead Answer temperature control at 275~280 DEG C, in 50~90 minutes reaction time, low-melting point polyester is obtained;
The main spinning technology parameter of long filament low melting point polyester fiber FDY is:
Spinning temperature:262-275 DEG C of cortex, 280-288 DEG C of sandwich layer;
Chilling temperature:25-30℃;
One roller speed:2000-2200m/min;
One roll temperature:65-70℃;
Two roller speeds:2500-2700m/min;
Two roll temperatures:70-75℃;
Winding speed:2500-2700m/min.
9. a kind of preparation method of long filament low melting point polyester fiber according to claim 8, it is characterised in that the catalysis Agent is antimony oxide, antimony glycol or antimony acetate, and catalyst charge is the 0.01%~0.05% of phthalic acid gross weight; The stabilizer is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite, and stabilizer addition is that the phthalic acid is total The 0.01%~0.05% of weight.
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CN109680359A (en) * 2018-12-27 2019-04-26 江苏恒力化纤股份有限公司 The preparation method of the fluffy snow Neil silk of low boiling water
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CN109853082A (en) * 2018-12-27 2019-06-07 江苏恒力化纤股份有限公司 Core-skin thermo-fuse and preparation method thereof
CN110923843A (en) * 2019-12-16 2020-03-27 扬州富威尔复合材料有限公司 Polyester FDY hot-melt fiber and preparation method thereof
CN110952161A (en) * 2019-12-16 2020-04-03 扬州富威尔复合材料有限公司 Low-melting-point elastic polyester fiber and preparation method thereof
CN111441100A (en) * 2020-05-26 2020-07-24 无锡佳成纤维有限公司 Spinning forming process of low-melting-point polyester chip
CN111534889A (en) * 2020-06-24 2020-08-14 江苏微笑新材料科技有限公司 Antistatic and moisture-absorbing dyeable sheath-core composite fiber and preparation method thereof
CN112760743A (en) * 2020-12-31 2021-05-07 扬州富威尔复合材料有限公司 Preparation method of colored low-melting-point polyester fiber
CN115398054A (en) * 2020-03-31 2022-11-25 可隆工业株式会社 Spunbonded nonwoven fabric and modular carpet using the same
CN117448984A (en) * 2023-11-21 2024-01-26 南京禾素时代抗菌材料科技集团有限公司 PHBV composite fiber based on modified low-melting-point PET

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CN109735929A (en) * 2018-12-27 2019-05-10 江苏恒力化纤股份有限公司 Binary acid modified polyester fibre and preparation method thereof with tert-butyl side group
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CN109750378A (en) * 2018-12-27 2019-05-14 江苏恒力化纤股份有限公司 Terylene silk like fabric silk and preparation method thereof
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CN115398054A (en) * 2020-03-31 2022-11-25 可隆工业株式会社 Spunbonded nonwoven fabric and modular carpet using the same
CN111441100A (en) * 2020-05-26 2020-07-24 无锡佳成纤维有限公司 Spinning forming process of low-melting-point polyester chip
CN111534889A (en) * 2020-06-24 2020-08-14 江苏微笑新材料科技有限公司 Antistatic and moisture-absorbing dyeable sheath-core composite fiber and preparation method thereof
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