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CN106757518B - 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
CN106757518B
CN106757518B CN201710018827.9A CN201710018827A CN106757518B CN 106757518 B CN106757518 B CN 106757518B CN 201710018827 A CN201710018827 A CN 201710018827A CN 106757518 B CN106757518 B CN 106757518B
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melting point
point polyester
low
glycol
carbon
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CN106757518A (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, sandwich layer PET;Low-melting point polyester is made 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 branch;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.Long filament low melting point polyester fiber produced by the present invention plays fusing point and decreases and melt speed quickening, melts at once at the corresponding temperature, 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 technique
Currently, Non-Woven Fabric Industry is quickly grown, 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 usually we pass through to conventional polyester Modification prepare low-melting point polyester.
Copolyester with low melting point is to carry out a kind of lower melting-point polyester obtained from chemical modification to conventional polyester, due to it Structure is similar to the chemical structure of conventional polyester, therefore its part of properties for remaining conventional polyester, has with conventional polyester good Good compatibility.Not only fusing point is low for this modified copolyester, mobility is 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 The well-flushing truck energy of wool blend improvement worsted fabric;The heat bondable fibre of especially copolyester with low melting point spinning is applied to non-knit It makes 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, Excellent performance with water-fastness dry-cleaning, sand washing, easy strike-through, peel strength is high, is a kind of high-grade bonding raw material.In addition, eutectic Point copolyesters also is used as Masterbatch, hot melt adhesive, 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, has a certain gap on raw material, technology and equipment with product leading in the world, most of production domestic at present Product also rest on the development phase, also face many difficulties on the road for realizing industrialization.On the one hand existing low melting point is poly- Ester to play fusing point higher, on the other hand its slow, strong influence use of low-melting point polyester that melts speed.It is high to play fusing point, melts It is slow to melt speed.
Long filament low melting point polyester fiber is mainly used for home textile articles, housing, jacket and auxiliary material.
Summary of the invention
The purpose of the present invention is overcoming the low-melting point polyester of the long filament low melting point polyester fiber of the prior art to play fusing point height, melt 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, a kind of long filament be provided 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 long filament low melting point polyester fiber obtained, which decreases and melts speed, to be accelerated, It melts at once at the corresponding temperature, melting effect is good.
For achieving the above object, the present invention adopts the following technical scheme:
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 containing branch 12 carbon glycol segments composition;
The corresponding molecular weight regulator of the molecular weight regulator segment is specially monoacid series or binary acid series;Institute State monoacid be benzoic acid, p-methylbenzoic acid or p-ethylbenzoic acid, perhaps for corresponding to them methyl esters or ethyl ester or Methyl esters or ethyl ester for saturated fatty acid or corresponding to it;The binary acid series be 1,8- naphthalenedicarboxylic acid, phthalic acid, 1, 2- cyclopentane dicarboxylic acid or 1,2- cyclohexane cyclohexanedimethanodibasic and dimethyl ester or diethylester corresponding to them;
The saturated fatty acid refers to that carbon atom number is the fatty acid of 9-30.
Wherein the addition of M-phthalic acid segment, diethylene glycol (DEG) segment, 12 carbon glycol segments containing branch destroys molecule knot The regularity of structure, to reduce fusing point;The addition of monoacid series in molecular weight regulator reduces point of low-melting point polyester Son amount, the addition of binary acid series increase space steric effect, and the group on ortho position occupies biggish spatial position, hinders Attack to carboxyl carbon atom is unfavorable for the growth of molecular weight, reduces the molecular weight of low-melting point polyester, widens point of high polymer Son amount distribution, when relative molecular weight distribution broadens, the flowing temperature of low-melting point polyester melt declines, this is because molecule at this time The temperature range that relative displacement occurs for chain broadens, and especially low relative molecular mass component plays the role of internally plasticized, makes to gather The temperature decline of flowing takes place in ester melt, therefore low-melting point polyester is enable to melt rapidly at corresponding temperature, improves The melting behaviour of low-melting point polyester.It selects carbon atom number for the saturated fatty acid of 9-30, is because of the low saturated fat of carbon atom number The boiling point of fat acid is relatively low, and when polycondensation can deviate from, and influences the stability of its content;The high saturated fatty acid of carbon atom number, carboxylic acid Activity decline, will affect its extent of reaction.
As a preferred technical scheme:
A kind of long filament low melting point polyester fiber as described above, 2.0~4.0dtex of filament number, breaking strength >= 3.00cN/dtex, elongation at break are 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 heating rate is 5 DEG C/min, more than fusing point in the range of 20 DEG C, low-melting point polyester melting degree >=82%;It is described The number molecular weight of low-melting point polyester is 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 Amount is the 1.5%~3% of phthalic acid segment molal quantity;The 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 branch refer to branch position On a non-end group carbon in 12 carbon glycol segments and branch is 12 carbon of the linear carbon chain containing 5-10 carbon atom Glycol segment;The corresponding 12 carbon glycol containing branch of 12 carbon glycol segments containing branch are specially 2- amyl -1,12 12 Carbon glycol, the 12 carbon glycol of 2- hexyl -1,12, the 12 carbon glycol of 2- heptyl -12, the 12 carbon glycol of 2- octyl -1,12,2- nonyl The 12 carbon glycol of base -1,12, the 12 carbon glycol of 2- decyl -1,12, the 12 carbon glycol of 3- amyl -1,12,3- hexyl -1,12 12 Carbon glycol, the 12 carbon glycol of 3- heptyl -12, the 12 carbon glycol of 3- octyl -1,12, the 12 carbon glycol of 3- nonyl -1,12, the 3- last of the ten Heavenly stems The 12 carbon glycol of base -1,12, the 12 carbon glycol of 4- amyl -1,12, the 12 carbon glycol of 4- hexyl -1,12,12 carbon of 4- heptyl -12 Glycol, the 12 carbon glycol of 4- octyl -1,12, the 12 carbon glycol of 4- nonyl -1,12, the 12 carbon glycol of 4- decyl -1,12,5- penta The 12 carbon glycol of base -1,12, the 12 carbon glycol of 5- hexyl -1,12, the 12 carbon glycol of 5- heptyl -12,12 carbon of 5- octyl -1,12 Glycol, the 12 carbon glycol of 5- nonyl -1,12, the 12 carbon glycol of 5- decyl -1,12, the 12 carbon glycol of 6- amyl -1,12,6- oneself The 12 carbon glycol of base -1,12, the 12 carbon glycol of 6- heptyl -12, the 12 carbon glycol of 6- octyl -1,12,12 carbon of 6- nonyl -1,12 One or more of 12 carbon glycol of glycol or 6- decyl -1,12;The 12 carbon glycol segments containing branch 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, low-melting point polyester and PET are measured, are squeezed Out, it cools down, oil, stretching, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin are made;
A) low-melting point polyester polymerize;
(1) by terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon containing branch Glycol carries out esterification;
(2) then, polycondensation reaction is carried out, low-melting point polyester is made;
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using 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 Alcohol, the pure and mild ethylene glycol of 12 carbon two containing branch molar ratio be 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 Are as follows:
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon two containing branch After alcohol is made into slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure~0.3MPa, and temperature is 230 DEG C~250 DEG C, it is esterification terminal when the quantity of distillate of the water in esterification reaches 90% or more of theoretical value, obtains To esterification products;
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure; The staged pressure by normal pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 260~270 DEG C, and the reaction time is 30~ 50 minutes;It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure and be less than 100Pa, reaction temperature are controlled at 275~280 DEG C, the reaction time 50~90 minutes, and low-melting point polyester is made.
The main spinning technology parameter of long filament low melting point polyester fiber FDY are as follows:
Spinning temperature: 262-275 DEG C of cortex, 280-288 DEG C of sandwich layer;
Cooling temperature: 25-30 DEG C;
One roller speed: 2000-2200m/min;
One roll temperature: 65-70 DEG C;
Two roller speeds: 2500-2700m/min;
Two roll temperatures: 70-75 DEG C;
Winding speed: 2500-2700m/min.
A kind of preparation method of long filament low melting point polyester fiber as described above, the catalyst are antimony oxide, second Glycol antimony or antimony acetate, catalyst charge are the 0.01%~0.05% of phthalic acid total weight;The stabilizer is phosphoric acid Triphenylmethyl methacrylate, trimethyl phosphate or Trimethyl phosphite, stabilizer additional amount be the phthalic acid total weight 0.01%~ 0.05%.
The principle of the present invention are as follows:
Unbranched for no modified component, the conventional polyester of no molecular weight regulator, molecular chain structure is containing phenyl ring The regular linear macromolecule of structure, 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 melting 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 destroy molecular structure, it is made to become unordered chaotic structure from the ordered structure of high-sequential, The addition of phthalic acid segment changes the ratio and size between the different sub- 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 flexibility of copolyesters macromolecular chain, reduces molten Point;The addition of 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 biggish spatial position, hinders the attack to carboxyl carbon atom, no Conducive to the growth of molecular weight, the molecular weight of low-melting point polyester is reduced, the molecular weight distribution of high polymer is widened, works as relative molecular weight When distribution broadens, the flowing temperature decline of low-melting point polyester melt, this is because the temperature of relative displacement occurs for strand at this time Range broadens, and especially low relative molecular mass component plays the role of internally plasticized, makes polyester fondant that flowing take place Temperature decline, therefore low-melting point polyester is enable to melt rapidly at corresponding temperature, the melting behaviour of low-melting point polyester is improved, In 5 DEG C/min of heating rate, more than fusing point in the range of 20 DEG C, low-melting point polyester melting degree >=82% shows as melting Melt speed quickening;And conventional low-melting point polyester is under same Elevated Temperature Conditions, melting degree≤20% in this temperature range; Softening and flowing temperature can be reduced by reducing low-melting point polyester part macromolecular weight, be conducive to low melting point infiltration and glued Object increases bond effect;The addition of the 12 carbon glycol segments containing branch, when temperature is higher than glass transition temperature, branch is first In backbone motion, so that the increasing degree of free volume is far longer than the characteristic of unbranched polyester macromolecule chain, be conducive to melt The increase of speed;By M-phthalic acid segment, diethylene glycol (DEG) segment, molecular weight regulator and 12 carbon glycol segments containing branch etc. Prepared low-melting point polyester is added in modified component, has had many advantages, such as that melting temperature is low, and melting speed is fast.Long filament low melting point is poly- Ester fiber key property is that coating fitting effect is good, has good morphological stability and resilience, easily controllable thawing speed.
The utility model has the advantages that
(1) long filament low melting point polyester fiber 2.0~4.0dtex of filament number produced by the present invention, breaking strength >= 3.00cN/dtex, elongation at break are 40.0 ± 5.0%;Line density deviation ratio≤1.0%;Coating fitting effect is good, has good Good morphological stability and resilience, easily controllable thawing speed.
(2) raw material of low-melting point polyester produced by 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 branch, prepared low melting point Polyester has had many advantages, such as that melting temperature is low, and melting speed is fast.
(3) raw material of low-melting point polyester produced by the present invention is terephthalic acid (TPA) segment and ethylene glycol segment, molecular weight tune The addition of 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 occupy biggish spatial position, hinder the attack to carboxyl carbon atom, be unfavorable for molecular weight Increase, reduces 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, this is because the temperature range that relative displacement occurs for strand at this time broadens, especially It is internally plasticized that it is that low relative molecular mass component plays the role of, and makes polyester fondant that the temperature decline of flowing take place, because This enables low-melting point polyester to melt rapidly at corresponding temperature, improves the melting behaviour of low-melting point polyester, in heating rate 5 DEG C/min when, more than fusing point in the range of 20 DEG C, low-melting point polyester melting degree >=82%, show as melting speed accelerate; And conventional low-melting point polyester 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 infiltration adherend, increase viscous Tie effect.
(4) raw material of low-melting point polyester produced by the present invention is terephthalic acid (TPA) segment and ethylene glycol segment, containing branch The addition of 12 carbon glycol segments, when temperature is higher than glass transition temperature, branch 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 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 long filament low melting point polyester fiber:
A) low-melting point polyester polymerize;
(1) esterification;
Terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), benzoic acid and the 12 carbon glycol of 2- amyl -1,12 are matched After slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure, and temperature is 230 DEG C, works as esterification The quantity of distillate of water in reaction is esterification terminal when reaching 90% of theoretical value or more, obtains esterification products;Wherein, to benzene Dioctyl phthalate, M-phthalic acid, diethylene glycol (DEG), the 12 carbon glycol containing branch, ethylene glycol molar ratio be 1:0.4:0.1:0.05: 1.8;The additional amount of benzoic acid is the 0.01% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure; The staged pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 260 DEG C by normal pressure, and the reaction time is 30 minutes;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Low-melting point polyester is made at 275 DEG C, the reaction time 50 minutes in degree control.Catalyst is antimony oxide, and catalyst charge is The 0.01% of phthalic acid total weight.Stabilizer is triphenyl phosphate, and stabilizer additional amount is phthalic acid total weight 0.01%.
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer, low-melting point polyester and PET through metering, extrusion, cooling, oil, stretch, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin are made;
Main spinning technology parameter are as follows:
Spinning temperature: 262 DEG C of cortex, 280 DEG C of sandwich layer;
Cooling temperature: 25 DEG C;
One roller speed: 2000m/min;
One roll temperature: 65 DEG C;
Two roller speeds: 2500m/min;
Two roll temperatures: 70 DEG C;
Winding speed: 2500m/min.
The long filament low melting point polyester fiber prepared through the above 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 12 carbon glycol segment of 2- amyl -1,12 composition;Benzoic acid segment is benzene two 0.01%, 2- amyl -1,12, the 12 carbon glycol segment of formic acid segment molal quantity is 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 heating 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, breaking strength 3.00cN/dtex, fracture are stretched Long rate 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 polymerize;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, 12 carbon of diethylene glycol (DEG), p-methylbenzoic acid and 2- hexyl -1,12 After glycol is made into slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure 0.3MPa, temperature 250 DEG C, it is esterification terminal when the quantity of distillate of the water in esterification reaches 90% or more of theoretical value, obtains esterification products; Wherein, terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), 12 carbon glycol of 2- hexyl -1,12, ethylene glycol molar ratio be 1: 0.6:0.3:0.1:2.5;The additional amount of p-methylbenzoic acid is the 0.5% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure; The staged pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 270 DEG C by normal pressure, and the reaction time is 50 minutes;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Low-melting point polyester is made at 280 DEG C, the reaction time 90 minutes in degree control.Catalyst is antimony glycol, and catalyst charge is benzene The 0.05% of dioctyl phthalate total weight.Stabilizer is trimethyl phosphate, and stabilizer additional amount is the 0.05% of phthalic acid total weight.
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer, low-melting point polyester and PET through metering, extrusion, cooling, oil, stretch, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin are made;
Main spinning technology parameter are as follows:
Spinning temperature: 275 DEG C of cortex, 288 DEG C of sandwich layer;
Cooling temperature: 30 DEG C;
One roller speed: 2200m/min;
One roll temperature: 70 DEG C;
Two roller speeds: 2700m/min;
Two roll temperatures: 75 DEG C;
Winding speed: 2700m/min.
The long filament low melting point polyester fiber prepared through the above 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 12 carbon glycol segment of 2- hexyl -1,12 composition;To methylbenzene first Sour segment is that 0.5%, 2- hexyl -1,12, the 12 carbon glycol segment of phthalic acid segment molal quantity is that terephthalic acid (TPA) segment rubs 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 heating 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 poly- The molecular weight distributing index D=4.1 of ester.The filament number 4.0dtex of long filament low melting point polyester fiber, breaking strength are 3.30cN/dtex, elongation at break 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 polymerize;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, 12 carbon two of diethylene glycol (DEG), p-ethylbenzoic acid and 2- heptyl -12 After alcohol is made into slurry, esterification being carried out, under nitrogen atmosphere compressive reaction, moulding pressure 0.1MPa, temperature is 240 DEG C, It is esterification terminal when the quantity of distillate of the water in esterification reaches 90% or more of theoretical value, obtains esterification products;Its In, terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), the 12 carbon glycol of 2- heptyl -12, ethylene glycol molar ratio be 1:0.5: 0.2:0.07:2;The additional amount of p-ethylbenzoic acid is the 0.1% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure; The staged pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 265 DEG C by normal pressure, and the reaction time is 40 minutes;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Low-melting point polyester is made at 278 DEG C, the reaction time 60 minutes in degree control.Catalyst is antimony acetate, and catalyst charge is benzene two The 0.03% of formic acid total weight.Stabilizer is Trimethyl phosphite, and stabilizer additional amount is the 0.02% of phthalic acid total weight.
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer, low-melting point polyester and PET through metering, extrusion, cooling, oil, stretch, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin are made;
Main spinning technology parameter are as follows:
Spinning temperature: 270 DEG C of cortex, 284 DEG C of sandwich layer;
Cooling temperature: 28 DEG C;
One roller speed: 2100m/min;
One roll temperature: 68 DEG C;
Two roller speeds: 2600m/min;
Two roll temperatures: 71 DEG C;
Winding speed: 2600m/min.
The long filament low melting point polyester fiber prepared through the above 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 12 carbon glycol segment of 2- heptyl -12 composition;P-ethylbenzoic acid Segment is that 0.1%, 2- heptyl -12, the 12 carbon glycol segment of phthalic acid segment molal quantity is terephthalic acid (TPA) segment molal quantity 7%;The fusing point of low-melting point polyester is at 150 DEG C;It is 5 DEG C/min in heating rate, more than low-melting point polyester fusing point 20 DEG C of model 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, breaking strength 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 polymerize;
(1) esterification;
Terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), pelargonic acid and the 12 carbon glycol of 2- octyl -1,12 are matched After slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure 0.2MPa, temperature is 245 DEG C, works as ester The quantity of distillate of water in change reaction is esterification terminal when reaching 90% of theoretical value or more, obtains esterification products;Wherein, right Phthalic acid, M-phthalic acid, diethylene glycol (DEG), the 12 carbon glycol of 2- octyl -1,12, ethylene glycol molar ratio be 1:0.5:0.25: 0.08:2.2;The additional amount of pelargonic acid is the 0.2% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure; The staged pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 260 DEG C by normal pressure, and the reaction time is 45 minutes;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Low-melting point polyester is made at 275 DEG C, the reaction time 70 minutes in degree control.Catalyst is antimony oxide, and catalyst charge is The 0.04% of phthalic acid total weight.Stabilizer is triphenyl phosphate, and stabilizer additional amount is phthalic acid total weight 0.03%.
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer, low-melting point polyester and PET through metering, extrusion, cooling, oil, stretch, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin are made;
Main spinning technology parameter are as follows:
Spinning temperature: 268 DEG C of cortex, 286 DEG C of sandwich layer;
Cooling temperature: 28 DEG C;
One roller speed: 2050m/min;
One roll temperature: 67 DEG C;
Two roller speeds: 2650m/min;
Two roll temperatures: 72 DEG C;
Winding speed: 2650m/min.
The long filament low melting point polyester fiber prepared through the above 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 12 carbon glycol segment of 2- octyl -1,12 composition;Pelargonic acid segment is benzene two 0.2%, 2- octyl -1,12, the 12 carbon glycol segment of formic acid segment molal quantity is 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 heating 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, breaking strength 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 polymerize;
(1) esterification;
Terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), capric acid and the 12 carbon glycol of 2- nonyl -1,12 are made into After slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure 0.1MPa, temperature is 245 DEG C, works as esterification The quantity of distillate of water in reaction is esterification terminal when reaching 90% of theoretical value or more, obtains esterification products;Wherein, to benzene Dioctyl phthalate, M-phthalic acid, diethylene glycol (DEG), the 12 carbon glycol of 2- nonyl -1,12, ethylene glycol molar ratio be 1:0.5:0.15: 0.09:2.3;The additional amount of capric acid is the 0.4% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure; The staged pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 265 DEG C by normal pressure, and the reaction time is 45 minutes;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Low-melting point polyester is made at 279 DEG C, the reaction time 80 minutes in degree control.Catalyst is antimony oxide, and catalyst charge is The 0.04% of phthalic acid total weight.Stabilizer is triphenyl phosphate, and stabilizer additional amount is phthalic acid total weight 0.04%.
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer, low-melting point polyester and PET through metering, extrusion, cooling, oil, stretch, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin are made;
Main spinning technology parameter are as follows:
Spinning temperature: 271 DEG C of cortex, 282 DEG C of sandwich layer;
Cooling temperature: 26 DEG C;
One roller speed: 2000m/min;
One roll temperature: 65 DEG C;
Two roller speeds: 2700m/min;
Two roll temperatures: 75 DEG C;
Winding speed: 2700m/min.
The long filament low melting point polyester fiber prepared through the above 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 12 carbon glycol segment of 2- nonyl -1,12 composition;Capric acid segment is phthalic acid 0.4%, 2- nonyl -1,12, the 12 carbon glycol segment of segment molal quantity is 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 heating 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, breaking strength 3.20cN/dtex, elongation at break are 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 polymerize;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, 12 carbon two of diethylene glycol (DEG), benzoic acid formicester and 2- decyl -1,12 After alcohol is made into slurry, esterification being carried out, under nitrogen atmosphere compressive reaction, moulding pressure 0.3MPa, temperature is 250 DEG C, It is esterification terminal when the quantity of distillate of the water in esterification reaches 90% or more of theoretical value, obtains esterification products;Its In, terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), 12 carbon glycol of 2- decyl -1,12, ethylene glycol molar ratio be 1:0.4: 0.3:0.1:1.8;The additional amount of benzoic acid formicester is the 0.09% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure; The staged pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 270 DEG C by normal pressure, and the reaction time is 30 minutes;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Low-melting point polyester is made at 275 DEG C, the reaction time 90 minutes in degree control.Catalyst is antimony glycol, and catalyst charge is benzene The 0.05% of dioctyl phthalate total weight.Stabilizer is triphenyl phosphate, and stabilizer additional amount is the 0.01% of phthalic acid total weight.
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer, low-melting point polyester and PET through metering, extrusion, cooling, oil, stretch, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin are made;
Main spinning technology parameter are as follows:
Spinning temperature: 262 DEG C of cortex, 280 DEG C of sandwich layer;
Cooling temperature: 25 DEG C;
One roller speed: 2200m/min;
One roll temperature: 65 DEG C;
Two roller speeds: 2700m/min;
Two roll temperatures: 75 DEG C;
Winding speed: 2500m/min.
The long filament low melting point polyester fiber prepared through the above 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 12 carbon glycol segment of 2- decyl -1,12 composition;Benzoic acid formicester chain Section is that 0.09%, 2- decyl -1,12, the 12 carbon glycol segment of phthalic acid segment molal quantity is 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 heating 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, breaking strength are 3.30cN/dtex, elongation at break 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 polymerize;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, 12 carbon two of diethylene glycol (DEG), benzoic acid second rouge and 3- amyl -1,12 After alcohol is made into slurry, esterification being carried out, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure, and temperature is 250 DEG C, when The quantity of distillate of water in esterification is esterification terminal when reaching 90% of theoretical value or more, obtains esterification products;Wherein, Terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), the 12 carbon glycol of 3- amyl -1,12, ethylene glycol molar ratio be 1:0.4:0.3: 0.05:1.8;The additional amount of benzoic acid second rouge is the 0.5% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure; The staged pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 270 DEG C by normal pressure, and the reaction time is 30 minutes;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Low-melting point polyester is made at 275 DEG C, the reaction time 50 minutes in degree control.Catalyst is antimony acetate, and catalyst charge is benzene two The 0.05% of formic acid total weight.Stabilizer is Trimethyl phosphite, and stabilizer additional amount is the 0.01% of phthalic acid total weight.
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer, low-melting point polyester and PET through metering, extrusion, cooling, oil, stretch, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin are made;
Main spinning technology parameter are as follows:
Spinning temperature: 2685 DEG C of cortex, 284 DEG C of sandwich layer;
Cooling temperature: 28 DEG C;
One roller speed: 2100m/min;
One roll temperature: 67 DEG C;
Two roller speeds: 2600m/min;
Two roll temperatures: 71 DEG C;
Winding speed: 2600m/min.
The long filament low melting point polyester fiber prepared through the above 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 12 carbon glycol segment of 3- amyl -1,12 composition;Benzoic acid second fat chain Section is that 0.5%, 3- amyl -1,12, the 12 carbon glycol segment of phthalic acid segment molal quantity is 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 in heating rate, more than low-melting point polyester fusing point 20 DEG C of model 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, breaking strength 3.30cN/ Dtex, elongation at break 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 polymerize;
(1) esterification;
By terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon two containing branch After alcohol is made into slurry, esterification being carried out, under nitrogen atmosphere compressive reaction, moulding pressure 0.2MPa, temperature is 230 DEG C, It is esterification terminal when the quantity of distillate of the water in esterification reaches 90% or more of theoretical value, obtains esterification products;Its In, terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG), the 12 carbon glycol containing branch, ethylene glycol molar ratio be 1:0.5: 0.25:0.08:2.2;The additional amount of molecular weight regulator is the 0.3% of phthalic acid molal quantity.
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure; The staged pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 265 DEG C by normal pressure, and the reaction time is 40 minutes;So After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure less than 100Pa, reaction temperature Low-melting point polyester is made at 280 DEG C, the reaction time 70 minutes in degree control.Catalyst is antimony glycol, and catalyst charge is benzene The 0.03% of dioctyl phthalate total weight.Stabilizer is triphenyl phosphate, and stabilizer additional amount is the 0.02% of phthalic acid total weight.
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer, low-melting point polyester and PET through metering, extrusion, cooling, oil, stretch, thermal finalization and winding, long filament low melting point polyester fiber FDY of core-skin are made;
Main spinning technology parameter are as follows:
Spinning temperature: 275 DEG C of cortex, 284 DEG C of sandwich layer;
Cooling temperature: 28 DEG C;
One roller speed: 2200m/min;
One roll temperature: 65 DEG C;
Two roller speeds: 2700m/min;
Two roll temperatures: 75 DEG C;
Winding speed: 2500m/min.
The long filament low melting point polyester fiber prepared through the above 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 composition containing branch.
Fusing point, the number of the molecular-weight adjusting and finally prepd low-melting point polyester that use in the above embodiment of the present invention are equal The acetaldehyde of molecular weight and molecualr weight distribution and long filament low melting point polyester fiber, filament number, breaking strength and core-skin knot The particular product performance parameters such as the core-skin area ratio of structure are 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 Measure regulator segment and the 12 carbon glycol segments composition containing branch;
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, perhaps for the methyl esters or ethyl ester corresponding to them or be full Methyl esters or ethyl ester with fatty acid or corresponding to it;The binary acid series is 1,8- naphthalenedicarboxylic acid, phthalic acid, 1,2- ring Pentane dioctyl phthalate or 1,2- cyclohexane cyclohexanedimethanodibasic and dimethyl ester or diethylester corresponding to them;
The saturated fatty acid refers to that carbon atom number is the fatty acid of 9-30.
2. a kind of long filament low melting point polyester fiber according to claim 1, which is characterized in that the long filament low-melting point polyester 2.0~4.0dtex of filament number of fiber, breaking strength >=3.00cN/dtex, elongation at break are 40.0 ± 5.0%;Line is close Spend 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, which is characterized in that the low-melting point polyester melts O'clock between 100 DEG C~170 DEG C;When heating rate is 5 DEG C/min, more than fusing point in the range of 20 DEG C, low-melting point polyester Melting degree >=82%;The number molecular weight of the low-melting point polyester is 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, which is characterized in that the molecular weight regulator chain The content of 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, which is characterized in that 12 carbon containing branch Glycol segment refers on a non-end group carbon that branch is located in 12 carbon glycol segments and branch is containing 5-10 carbon atom Linear carbon chain 12 carbon glycol segments;The corresponding 12 carbon glycol containing branch of 12 carbon glycol segments containing branch are specific For the 12 carbon glycol of 2- amyl -1,12, the 12 carbon glycol of 2- hexyl -1,12, the 12 carbon glycol of 2- heptyl -12,2- octyl -1,12 12 carbon glycol, the 12 carbon glycol of 2- nonyl -1,12, the 12 carbon glycol of 2- decyl -1,12, the 12 carbon glycol of 3- amyl -1,12, The 12 carbon glycol of 3- hexyl -1,12, the 12 carbon glycol of 3- heptyl -12, the 12 carbon glycol of 3- octyl -1,12,3- nonyl -1,12 ten Two carbon glycol, the 12 carbon glycol of 3- decyl -1,12, the 12 carbon glycol of 4- amyl -1,12, the 12 carbon glycol of 4- hexyl -1,12,4- The 12 carbon glycol of heptyl -12, the 12 carbon glycol of 4- octyl -1,12, the 12 carbon glycol of 4- nonyl -1,12,4- decyl -1,12 12 Carbon glycol, the 12 carbon glycol of 5- amyl -1,12, the 12 carbon glycol of 5- hexyl -1,12, the 12 carbon glycol of 5- heptyl -12,5- are pungent The 12 carbon glycol of base -1,12, the 12 carbon glycol of 5- nonyl -1,12, the 12 carbon glycol of 5- decyl -1,12,6- amyl -1,12 12 Carbon glycol, the 12 carbon glycol of 6- hexyl -1,12, the 12 carbon glycol of 6- heptyl -12, the 12 carbon glycol of 6- octyl -1,12,6- nonyl One or more of 12 carbon glycol of the 12 carbon glycol of base -1,12 or 6- decyl -1,12;The 12 carbon glycol chains containing branch Section is the 5~10% of terephthalic acid (TPA) segment molal quantity.
6. the preparation method of -5 any a kind of long filament low melting point polyester fibers according to claim 1, it is characterized in that including Step: low-melting point polyester and PET through metering, extrusion, cooling, oil, stretch, thermal finalization and winding, the long filament that core-skin is made it is low Melt polyester fibers FDY;
A) low-melting point polyester polymerize;
(1) by terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon glycol containing branch Carry out esterification;
(2) then, polycondensation reaction is carried out, low-melting point polyester is made;
B) spinning;
Using core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer.
7. a kind of preparation method of long filament low melting point polyester fiber according to claim 6, which is characterized in that terephthaldehyde Acid, M-phthalic acid, diethylene glycol (DEG), the pure and mild ethylene glycol of 12 carbon two containing branch molar ratio be 1:0.4~0.6:0.1~0.3: 0.05~0.1:1.8~2.5.
8. a kind of preparation method of long filament low melting point polyester fiber according to claim 6, which is characterized in that low melting point is poly- The specific steps of polyisocyanate polyaddition are as follows:
(1) esterification;
Terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), molecular weight regulator and 12 carbon glycol containing branch are matched After slurry, esterification is carried out, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure~0.3MPa, and temperature is 230 DEG C ~250 DEG C, it is esterification terminal when the quantity of distillate of the water in esterification reaches 90% or more of theoretical value, is esterified Product;
(2) polycondensation reaction;
Then, under the action of catalyst and stabilizer, start the polycondensation reaction of low vacuum stage under conditions of negative pressure;The rank Section pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 260~270 DEG C by normal pressure, and the reaction time is 30~50 points Clock;It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be down to absolute pressure less than 100Pa, instead It answers temperature control at 275~280 DEG C, the reaction time 50~90 minutes, low-melting point polyester is made;
The main spinning technology parameter of long filament low melting point polyester fiber FDY are as follows:
Spinning temperature: 262-275 DEG C of cortex, 280-288 DEG C of sandwich layer;
Cooling temperature: 25-30 DEG C;
One roller speed: 2000-2200m/min;
One roll temperature: 65-70 DEG C;
Two roller speeds: 2500-2700m/min;
Two roll temperatures: 70-75 DEG C;
Winding speed: 2500-2700m/min.
9. a kind of preparation method of long filament low melting point polyester fiber according to claim 8, which is characterized 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 total weight; The stabilizer is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite, and stabilizer additional amount is that the phthalic acid is total The 0.01%~0.05% of weight.
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CN109722731B (en) * 2018-12-27 2020-10-16 江苏恒力化纤股份有限公司 Modified polyester POY fiber and preparation method thereof
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