CN106757517A - One kind regeneration low melting point polyester fiber and preparation method thereof - Google Patents
One kind regeneration low melting point polyester fiber and preparation method thereof Download PDFInfo
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- CN106757517A CN106757517A CN201710017248.2A CN201710017248A CN106757517A CN 106757517 A CN106757517 A CN 106757517A CN 201710017248 A CN201710017248 A CN 201710017248A CN 106757517 A CN106757517 A CN 106757517A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, or compounds thereof
- C08G63/866—Antimony or compounds thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Polymers & Plastics (AREA)
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- General Chemical & Material Sciences (AREA)
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- Multicomponent Fibers (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention relates to one kind regeneration low melting point polyester fiber and preparation method thereof, regeneration low melting point polyester fiber is skin-core structure, and cortex is low-melting point polyester, and sandwich layer is reworked material；Low-melting point polyester is made up of terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol segment, diethylene glycol (DEG) segment and molecular weight regulator segment；The corresponding molecular weight regulator of molecular weight regulator segment is specially monoacid series or binary acid series；Regeneration low melting point polyester fiber preparation method includes that low-melting point polyester is polymerized and core-sheath spinning step, and spinning afterwards uses draft process, and low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.The fusing point that rises of obtained regeneration low melting point polyester fiber of the invention decreases and melts speed quickening, melts at once at the corresponding temperature, and melting effect is good.
Description
Technical field
The invention belongs to regenerate low melting point polyester fiber field, it is related to a kind of regeneration 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.
World resource is forever a big hot topic topic of the mankind, and the slogan for economizing on resources is regenerated with being slowly deep into the popular feeling
The awakening of material is also inevitable, the recycling that people pass through resource, real could accomplish environmental protection and energy saving.Reworked material maximum
Advantage is exactly resource recycling, although its performance and attribute on the whole is all strong not as virgin material, but we are much producing
Product making aspect just need not make it using that each side attribute and all good material of performance, so waste much very
Attribute more unnecessary, and reworked material is just different, according to difference the need for, it is only necessary to process the attribute in terms of certain, can
Corresponding product is produced, resource loss will not be so allowed.But because reworked material impurity is more, obtained product is dim
It is unglazed.
The content of the invention
The purpose of the present invention is that the low-melting point polyester fusing point of the regeneration low melting point polyester fiber for overcoming prior art is high, is melted
Melt speed it is slow the problems such as, realize the production of large-scale, there is provided one kind regeneration low melting point polyester fiber and preparation method thereof.This hair
Bright regeneration low melting point polyester fiber is skin-core structure, and cortex is low-melting point polyester, and sandwich layer is reworked material, and obtained regeneration is low
The fusing point that rises of melt polyester fibers decreases and melts speed quickening, melts at once at the corresponding temperature, and melting effect is good.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of regeneration 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 reworked material；The reworked material is the reworked material of a bottle piece, waste silk, foam material；
The low-melting point polyester by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol segment, diethylene glycol (DEG) segment and
Molecular weight regulator segment is 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 and methyl esters or ethyl ester corresponding to them, Huo Zhewei
Saturated fatty acid and 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, the regularity of addition saboteur's structure of diethylene glycol (DEG) segment, so as to reduce 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, the molecular weight distribution of high polymer is widened, works 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, improve the melting behaviour of low-melting point polyester.
Selection carbon number is the saturated fatty acid of 9-30, because the boiling point of the low saturated fatty acid of carbon number is relatively low, during polycondensation
Can deviate from, influence the stability of its content；Carbon number saturated fatty acid high, the activity decrease of its carboxylic acid can influence its anti-
Answer degree.
As preferred technical scheme：
Regeneration low melting point polyester fiber as described above a kind of, filament number is 1.7~3.3dtex, fracture strength >=
3.30cN/dtex；The core-skin area ratio of the skin-core structure is 40~60:60~40.
Regeneration low melting point polyester fiber as described above a kind of, the fusing point of the low-melting point polyester 100 DEG C~160 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 >=67%；It is described
The number-average molecular weight of low-melting point polyester is 22000-38000, the molecular weight distributing index D=2.6 of the low-melting point polyester~
4.4.The fusing point of the low-melting point polyester refers to that it plays fusing point.
One kind as described above regenerates low melting point polyester fiber, the 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 segment is terephthalic acid (TPA) segment and isophthalic two
Formic acid segment.
The present invention also provides a kind of preparation method for regenerating low melting point polyester fiber as described above, including step：
A) low-melting point polyester polymerization；
(1) terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG) and molecular weight regulator are carried out into esterification；
(2) and then, carry out polycondensation reaction, be obtained low-melting point polyester；
B) reworked material melting；
Reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material mass ratio
0.05%~0.1%.Fresh degree of reflecting is a kind of characteristic manner of bright and new degree, and the addition of zinc stearate improves the light of product colour
Fresh degree, zinc stearate floats over the surface of core fibers, can reduce the roughness on surface, improves the fresh degree of reflecting on surface, described
Fresh degree of reflecting DOI values 85~80；The test of the fresh degree of reflecting makes to measure sandwich layer fibre by WGB-4816wave scan DOI detectors
Dimension table face.
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with PET as sandwich layer；Spin afterwards and use
Draft process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
A kind of preparation method for regenerating low melting point polyester fiber as described above, it is terephthalic acid (TPA), M-phthalic acid, two sweet
Alcohol is 1 with the mol ratio of ethylene glycol:0.4~0.6:0.1~0.3:1.8~2.5；
A kind of preparation method for regenerating low melting point polyester fiber as described above, the specific steps of low-melting point polyester polymerization
For：
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG) and molecular weight regulator are made into slurry, ester is carried out
Change reaction, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure~0.3MPa, temperature is 230 DEG C~250 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；
(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.
A kind of preparation method for regenerating low melting point polyester fiber as described above, the main technologic parameters of the spinning are：
Spinning temperature：262-275 DEG C of cortex, 280-288 DEG C of sandwich layer, spinning speed：500-1100m/min；
Drawing-off uses oil bath drawing-off, and the temperature of the oil bath is 65 DEG C~75 DEG C, and drafting multiple is 2.0~2.5 times；
50-60 DEG C of coiling temperature, the main pressure 0.4-0.6MPa of curling, curling back pressure 0.2-0.4MPa, crispation number 8-13/
25mm, crimpness 11-13%, drying temperature are 65 DEG C~75 DEG C, time 10min~20min.
A kind of preparation method for regenerating 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 regeneration low-melting point polyester of the invention is terephthalic acid (TPA) segment and ethylene glycol segment, between adding wherein
Phthalic acid segment, diethylene glycol (DEG) segment, molecular weight regulator saboteur's structure, make it be changed into from the ordered structure of high-sequential
Unordered chaotic structure, the addition of M-phthalic acid segment changes ratio and chi between the different Asia macro crystallization forms of polyester
Very little size, makes crystallizing polyester difficult, is intended to unformed mode and exists；The addition of diethylene glycol (DEG) segment increases copolyesters macromolecular chain
Compliance, reduce fusing point；The addition of the monoacid series in molecular weight regulator reduces the molecular weight of low-melting point polyester, two
The addition of first acid series increases space steric effect, and the group on ortho position occupies larger locus, hinders to carboxyl
The attack of carbon atom, is unfavorable for the growth of molecular weight；The molecular weight of low-melting point polyester is reduced, the molecular weight point of high polymer is widened
Cloth, when relative molecular weight distribution broadens, the flowing temperature of low-melting point polyester melt declines, and this is because now strand occurs
The temperature range of relative displacement broadens, and especially low relative molecular mass component serves internally plasticized effect, makes polyester fondant
The temperature drop of flowing takes place, therefore low-melting point polyester is melted rapidly at corresponding temperature, improve low melting point
The melting behaviour of polyester, 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
>=67%, show as melting speed and accelerate；And the low-melting point polyester of routine is under same Elevated Temperature Conditions, in this temperature range
Melting degree≤20%；Reducing low-melting point polyester part macromolecular weight can reduce softening and flowing temperature, be conducive to
Low melting point infiltrates adherend, increased bond effect；Changed by M-phthalic acid segment, diethylene glycol (DEG) segment and molecular weight regulator etc.
Property component add prepared low-melting point polyester, with rising, melting temperature is low, the advantages of melting speed is fast.
Beneficial effect：
(1) addition of zinc stearate improves the bright-coloured degree of product colour in the present invention, and zinc stearate floats over core fibers
Surface, can reduce the roughness on surface, improve the fresh degree of reflecting on surface, fresh degree of the reflecting DOI values 85~80；
(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 and molecular weight regulator, prepared low-melting point polyester, with a 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；The molecular weight of low-melting point polyester is reduced, the molecular weight distribution of high polymer is widened, when relative molecular weight distribution broadens,
The flowing temperature of polyester fondant declines, this be because the temperature range that now strand occurs relative displacement broadens, it is especially low
Relative molecular mass component serves internally plasticized effect, makes polyester fondant that the temperature drop of flowing takes place, therefore make low
Melt polyester can rapidly be melted at corresponding temperature, improve the melting behaviour of low-melting point polyester.In 5 DEG C/min of programming rate
When, more than the fusing point in the range of 20 DEG C, low-melting point polyester melting degree >=67% shows as melting speed and accelerates；And it is conventional
Low-melting point polyester under same Elevated Temperature Conditions, melting degree≤20% in this temperature range；Reduce low-melting point polyester portion
Dividing macromolecular weight can reduce softening and flowing temperature, be conducive to low melting point to infiltrate adherend, increased bond effect.
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 for regenerating low melting point polyester fiber：
A) low-melting point polyester polymerization；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), benzoic acid are made into slurry, esterification is carried out,
Compressive reaction under nitrogen atmosphere, moulding pressure is normal pressure, and temperature is 230 DEG C, when the quantity of distillate of the water in esterification reaches
Theoretical value more than 90% when be esterification terminal, obtain esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid, two sweet
Alcohol is 1 with the mol ratio of ethylene glycol:0.4:0.1:1.8；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) reworked material melting；
Dry reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material
The 0.05% of mass ratio；Fresh degree of the reflecting DOI values 75 of sandwich layer；
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with reworked material as sandwich layer；Spin afterwards and adopt
With draft process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
The main technologic parameters of spinning are：
Spinning temperature：262 DEG C of cortex, 280 DEG C of sandwich layer, spinning speed：500m/min；
Drawing-off uses oil bath drawing-off, and the temperature of oil bath is 65 DEG C；
Drafting multiple is 2.0 times；
50 DEG C of coiling temperature, crimps main pressure 0.4MPa, crimps back pressure 0.2MPa, 8/25mm of crispation number, crimpness 11%.
The regeneration 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 reworked material；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, second
Glycol segment, diethylene glycol (DEG) segment, benzoic acid segment section composition；Benzoic acid segment is the 0.01% of phthalic acid 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 67%；The number-average molecular weight of low-melting point polyester is 22000, the molecular weight point of low-melting point polyester
Cloth index D=2.6.The filament number for regenerating low melting point polyester fiber is 1.7dtex, and fracture strength is 3.50cN/dtex；Core-skin
The core-skin area ratio of structure is 40:60.
Embodiment 2
A kind of preparation method for regenerating low melting point polyester fiber：
A) low-melting point polyester polymerization；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), p-methylbenzoic acid are made into slurry, it is esterified
React, under nitrogen atmosphere compressive reaction, moulding pressure is 0.3MPa, and temperature is 250 DEG C, when distillating for the water in esterification
It is esterification terminal to measure when reaching more than the 90% of theoretical value, obtains esterification products；Wherein, terephthalic acid (TPA), isophthalic diformazan
The mol ratio of acid, diethylene glycol (DEG) and ethylene glycol is 1:0.6:0.3:2.5；The addition of p-methylbenzoic acid is phthalic acid molal quantity
0.5%.
(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) reworked material melting；
Dry reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material
The 0.1% of mass ratio；Fresh degree of the reflecting DOI values 80 of sandwich layer；
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with reworked material as sandwich layer；Spin afterwards and adopt
With draft process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
The main technologic parameters of spinning are：
Spinning temperature：275 DEG C of cortex, 288 DEG C of sandwich layer, spinning speed：1100m/min；
Drawing-off uses oil bath drawing-off, and the temperature of oil bath is 75 DEG C；
Drafting multiple is 2.5 times；
60 DEG C of coiling temperature, crimps main pressure 0.6MPa, crimps back pressure 0.4MPa, 13/25mm of crispation number, crimpness
13%.
The regeneration 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 reworked material；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, second
Glycol segment, diethylene glycol (DEG) segment, p-methylbenzoic acid segment composition；P-methylbenzoic acid segment is phthalic acid segment molal quantity
0.5%, 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 68%；The number-average molecular weight of low-melting point polyester is 25000, low-melting point polyester
Molecular weight distributing index D=3.The filament number of regeneration regeneration low melting point polyester fiber is 3.3dtex, and fracture strength is
3.50cN/dtex；The core-skin area ratio of skin-core structure is 60:40.
Embodiment 3
A kind of preparation method for regenerating low melting point polyester fiber：
A) low-melting point polyester polymerization；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), p-ethylbenzoic acid are made into slurry, it is esterified
React, under nitrogen atmosphere compressive reaction, moulding pressure is 0.1MPa, and temperature is 240 DEG C, when distillating for the water in esterification
It is esterification terminal to measure when reaching more than the 90% of theoretical value, obtains esterification products；Wherein, terephthalic acid (TPA), isophthalic diformazan
The mol ratio of acid, diethylene glycol (DEG) and ethylene glycol is 1:0.5:0.2:2；The addition of p-ethylbenzoic acid is phthalic acid molal quantity
0.1%.
(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) reworked material melting；
Dry reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material
The 0.08% of mass ratio；Fresh degree of the reflecting DOI values 78 of sandwich layer；
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with reworked material as sandwich layer；Spin afterwards and adopt
With draft process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
The main technologic parameters of spinning are：
Spinning temperature：265 DEG C of cortex, 285 DEG C of sandwich layer, spinning speed：1000m/min；
Drawing-off uses oil bath drawing-off, and the temperature of oil bath is 70 DEG C；
Drafting multiple is 2.4 times；
55 DEG C of coiling temperature, crimps main pressure 0.5MPa, crimps back pressure 0.3MPa, 9/25mm of crispation number, crimpness 12%.
The regeneration 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 reworked material；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, second
Glycol segment, diethylene glycol (DEG) segment, p-ethylbenzoic acid segment composition；P-ethylbenzoic acid segment is phthalic acid segment molal quantity
0.1%, the fusing point of low-melting point polyester is at 150 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 70%；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 for regenerating low melting point polyester fiber is 2.0dtex, and fracture strength is 3.40cN/
dtex；The core-skin area ratio of skin-core structure is 50:50.
Embodiment 4
A kind of preparation method for regenerating low melting point polyester fiber：
A) low-melting point polyester polymerization；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), pelargonic acid are made into slurry, esterification is carried out,
Compressive reaction under nitrogen atmosphere, moulding pressure is 0.2MPa, and temperature is 245 DEG C, when the quantity of distillate of the water in esterification reaches
To theoretical value more than 90% when be esterification terminal, obtain esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid, two
Glycol is 1 with the mol ratio of ethylene glycol:0.5:0.25:2.2；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) reworked material melting；
Dry reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material
The 0.07% of mass ratio；Fresh degree of the reflecting DOI values 77 of sandwich layer；
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with reworked material as sandwich layer；Spin afterwards and adopt
With draft process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
The main technologic parameters of spinning are：
Spinning temperature：270 DEG C of cortex, 284 DEG C of sandwich layer, spinning speed：700m/min；
Drawing-off uses oil bath drawing-off, and the temperature of oil bath is 72 DEG C；
Drafting multiple is 2.35 times；
55 DEG C of coiling temperature, crimps main pressure 0.55MPa, crimps back pressure 0.25MPa, 9/25mm of crispation number, crimpness
12%.
The regeneration 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 reworked material；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, second
Glycol segment, diethylene glycol (DEG) segment, pelargonic acid segment composition；Pelargonic acid segment is the 0.2% of phthalic acid segment molal quantity, eutectic
The fusing point of point polyester is at 130 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, eutectic
The melting degree of point polyester is 72%；The number-average molecular weight of low-melting point polyester is 35000, and the molecular weight distribution of low-melting point polyester refers to
Number D=4.4.The filament number for regenerating low melting point polyester fiber is 2.4dtex, and fracture strength is 3.60cN/dtex；Skin-core structure
Core-skin area ratio be 45:55.
Embodiment 5
A kind of preparation method for regenerating low melting point polyester fiber：
A) low-melting point polyester polymerization；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), capric acid are made into slurry, esterification is carried out,
Compressive reaction under nitrogen atmosphere, moulding pressure is 0.1MPa, and temperature is 245 DEG C, when the quantity of distillate of the water in esterification reaches
Theoretical value more than 90% when be esterification terminal, obtain esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid, two sweet
Alcohol is 1 with the mol ratio of ethylene glycol:0.5:0.15:2.3；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) reworked material melting；
Dry reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material
The 0.06% of mass ratio；Fresh degree of the reflecting DOI values 76 of sandwich layer；
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with reworked material as sandwich layer；Spin afterwards and adopt
With draft process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
The main technologic parameters of spinning are：
Spinning temperature：274 DEG C of cortex, 285 DEG C of sandwich layer, spinning speed：900m/min；
Drawing-off uses oil bath drawing-off, and the temperature of oil bath is 70 DEG C；
Drafting multiple is 2.2 times；
55 DEG C of coiling temperature, crimps main pressure 0.55MPa, crimps back pressure 0.3MPa, 10/25mm of crispation number, crimpness
13%.
The regeneration 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 reworked material；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, second
Glycol segment, diethylene glycol (DEG) segment, capric acid segment composition；Capric acid segment is the 0.4% of phthalic acid segment molal quantity, and low melting point is gathered
The fusing point of ester is at 120 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 is gathered
The melting degree of ester is 69%；The number-average molecular weight of low-melting point polyester is 38000, the molecular weight distributing index D of low-melting point polyester
=3.5.The filament number for regenerating low melting point polyester fiber is 1.9dtex, and fracture strength is 3.40cN/dtex；Skin-core structure
Core-skin area ratio is 55:45.
Embodiment 6
A kind of preparation method for regenerating low melting point polyester fiber：
A) low-melting point polyester polymerization；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), benzoic acid formicester are made into slurry, be esterified instead
Answer, under nitrogen atmosphere compressive reaction, moulding pressure is 0.3MPa, and temperature is 250 DEG C, when the quantity of distillate of the water in esterification
It is esterification terminal when reaching more than the 90% of theoretical value, obtains esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid,
Diethylene glycol (DEG) is 1 with the mol ratio of ethylene glycol:0.4:0.3:1.8；The addition of benzoic acid formicester is phthalic acid molal quantity
0.09%.
(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) reworked material melting；
Dry reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material
The 0.06% of mass ratio；Fresh degree of the reflecting DOI values 77 of sandwich layer；
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with reworked material as sandwich layer；Spin afterwards and adopt
With draft process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
The main technologic parameters of spinning are：
Spinning temperature：268 DEG C of cortex, 283 DEG C of sandwich layer, spinning speed：600m/min；
Drawing-off uses oil bath drawing-off, and the temperature of oil bath is 70 DEG C；
Drafting multiple is 2.5 times；
60 DEG C of coiling temperature, crimps main pressure 0.4MPa, crimps back pressure 0.4MPa, 9/25mm of crispation number, crimpness 12%.
The regeneration 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 reworked material；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, second
Glycol segment, diethylene glycol (DEG) segment, benzoic acid formicester segment composition；Benzoic acid formicester segment is phthalic acid segment molal quantity
0.09%, the fusing point of low-melting point polyester is at 160 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 74%；The number-average molecular weight of low-melting point polyester is 28000, low-melting point polyester
Molecular weight distributing index D=3.The filament number for regenerating low melting point polyester fiber is 2.5dtex, and fracture strength is 3.30cN/
dtex；The core-skin area ratio of skin-core structure is 48:52.
Embodiment 7
A kind of preparation method for regenerating low melting point polyester fiber：
A) low-melting point polyester polymerization；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), benzoic acid second fat are made into slurry, be esterified instead
Answer, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure, and temperature is 250 DEG C, when the quantity of distillate of the water in esterification reaches
To theoretical value more than 90% when be esterification terminal, obtain esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid, two
Glycol is 1 with the mol ratio of ethylene glycol:0.4:0.3:1.8；The addition of benzoic acid second fat is phthalic acid molal quantity
0.5%.
(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) reworked material melting；
Dry reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material
The 0.1% of mass ratio；Fresh degree of the reflecting DOI values 75 of sandwich layer；
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with reworked material as sandwich layer；Spin afterwards and adopt
With draft process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
The main technologic parameters of spinning are：
Spinning temperature：262 DEG C of cortex, 288 DEG C of sandwich layer, spinning speed：1100m/min；
Drawing-off uses oil bath drawing-off, and the temperature of oil bath is 70 DEG C；
Drafting multiple is 2.1 times；
55 DEG C of coiling temperature, crimps main pressure 0.5MPa, crimps back pressure 0.3MPa, 10/25mm of crispation number, crimpness
11%.
The regeneration 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 reworked material；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, second
Glycol segment, diethylene glycol (DEG) segment, benzoic acid second fat chain section composition；Benzoic acid second fat chain section is phthalic acid segment molal quantity
0.5%, the fusing point of low-melting point polyester is at 155 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 73%；The number-average molecular weight of low-melting point polyester is 34000, low-melting point polyester
Molecular weight distributing index D=3.8.The filament number for regenerating low melting point polyester fiber is 2.3dtex, and fracture strength is 3.50cN/
dtex；The core-skin area ratio of skin-core structure is 55:45.
Embodiment 8-44
A kind of preparation method for regenerating 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, the mol ratio of terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG) and ethylene glycol is 1:0.4~0.6:0.1~0.3:1.8~
2.5；The addition of molecular weight regulator is the 0.01%~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 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) reworked material melting；
Dry reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material
The 0.1% of mass ratio；Fresh degree of the reflecting DOI values 80 of sandwich layer；
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with reworked material as sandwich layer；Spin afterwards and adopt
With draft process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
The main technologic parameters of spinning are：
Spinning temperature：265 DEG C of cortex, 288 DEG C of sandwich layer, spinning speed：1000m/min；
Drawing-off uses oil bath drawing-off, and the temperature of oil bath is 70 DEG C；
Drafting multiple is 2.4 times；
55 DEG C of coiling temperature, crimps main pressure 0.5MPa, crimps back pressure 0.3MPa, 9/25mm of crispation number, crimpness 12%.
The regeneration 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 reworked material；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, second
Glycol segment, diethylene glycol (DEG) segment, molecular weight regulator segment composition；Low-melting point polyester is 5 DEG C/min, low melting point in programming rate
When more than melting point polyester in the range of 20 DEG C, melting degree >=67% of low-melting point polyester.
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 low melting point polyester fiber, filament number, fracture strength and skin-core structure
Core-skin area than etc. particular product performance parameters it is as shown in the table：
Claims (9)
1. it is a kind of to regenerate low melting point polyester fiber, it is characterized in that：The regeneration 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 reworked material；The reworked material is bottle piece, waste silk
Or the reworked material of foam material；
The low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol segment, diethylene glycol (DEG) segment and molecule
Amount conditioning agent segment composition；
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 and methyl esters or ethyl ester corresponding to them, or is saturation
Aliphatic acid and 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. one kind according to claim 1 regenerates low melting point polyester fiber, it is characterised in that the regeneration low-melting point polyester
The filament number of fiber is 1.7~3.3dtex, fracture strength >=3.30cN/dtex；The core-skin area ratio of the skin-core structure is
40~60:60~40.
3. a kind of regeneration 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~160 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 >=67%；The number-average molecular weight of the low-melting point polyester is 22000-38000, the molecular weight of the low-melting point polyester
Profile exponent D=2.6~4.4.
4. one kind according to claim 1 regenerates low melting point polyester fiber, 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. the preparation method of a kind of regeneration low melting point polyester fiber as described in claim 1-4 is any, it is characterized in that including step
Suddenly：
A) low-melting point polyester polymerization；
(1) terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG) and molecular weight regulator are carried out into esterification；
(2) and then, carry out polycondensation reaction, be obtained low-melting point polyester；
B) reworked material melting；
Dry reworked material is melted, while adding zinc stearate；The content of described zinc stearate is reworked material quality
The 0.05%~0.1% of ratio；Fresh degree of the reflecting DOI values 75~80 of the sandwich layer；
C) spinning；
Preceding spinning uses core-sheath spinning technique, with the low-melting point polyester as cortex, with reworked material as sandwich layer；Spin to use afterwards and lead
Stretching process, low melting point polyester fiber is regenerated through curling, cut-out and dry acquisition.
6. it is according to claim 5 it is a kind of regenerate low melting point polyester fiber preparation method, it is characterised in that terephthaldehyde
The mol ratio of acid, M-phthalic acid, diethylene glycol (DEG) and ethylene glycol is 1:0.4~0.6:0.1~0.3:1.8~2.5.
7. it is according to claim 5 it is a kind of regenerate low melting point polyester fiber preparation method, it is characterised in that low melting point gather
Polyisocyanate polyaddition is concretely comprised the following steps：
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG) and molecular weight regulator are made into slurry, be esterified instead
Answer, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure~0.3MPa, temperature is 230 DEG C~250 DEG C, works as esterification
In the quantity of distillate of water be esterification terminal when reaching more than the 90% of theoretical value, obtain 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 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.
8. it is according to claim 5 it is a kind of regenerate low melting point polyester fiber preparation method, it is characterised in that the spinning
Main technologic parameters be：
Spinning temperature：262-275 DEG C of cortex, 280-288 DEG C of sandwich layer, spinning speed：500-1100m/min；
Drawing-off uses oil bath drawing-off, and the temperature of the oil bath is 65 DEG C~75 DEG C；Drafting multiple is 2.0~2.5 times；
50-60 DEG C of coiling temperature, the main pressure 0.4-0.6MPa of curling, curling back pressure 0.2-0.4MPa, crispation number 8-13/25mm,
Crimpness 11-13%.
9. it is according to claim 7 it is a kind of regenerate low melting point polyester fiber preparation method, 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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| 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 |
| CN111440294A (en) * | 2019-01-16 | 2020-07-24 | 远东新世纪股份有限公司 | Copolyester with low melting point and high crystallinity, manufacturing method thereof and low-melting-point polyester fiber |
| CN111560114A (en) * | 2020-06-11 | 2020-08-21 | 太仓逸枫化纤有限公司 | Synthesis and spinning preparation process of low-melting-point polyester |
| CN115726057A (en) * | 2022-12-06 | 2023-03-03 | 扬州富威尔复合材料有限公司 | Regenerated low-melting-point polyester composite fiber with ultraviolet shielding function and preparation method thereof |
| CN116536794A (en) * | 2023-05-05 | 2023-08-04 | 优彩环保资源科技股份有限公司 | Preparation method of sheath-core composite three-dimensional curled low-melting-point polyester fiber |
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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 |
| CN111440294A (en) * | 2019-01-16 | 2020-07-24 | 远东新世纪股份有限公司 | Copolyester with low melting point and high crystallinity, manufacturing method thereof and low-melting-point polyester fiber |
| CN111440294B (en) * | 2019-01-16 | 2022-10-04 | 远东新世纪股份有限公司 | Copolyester with low melting point and high crystallinity, manufacturing method thereof and low-melting-point polyester fiber |
| CN111560114A (en) * | 2020-06-11 | 2020-08-21 | 太仓逸枫化纤有限公司 | Synthesis and spinning preparation process of low-melting-point polyester |
| CN115726057A (en) * | 2022-12-06 | 2023-03-03 | 扬州富威尔复合材料有限公司 | Regenerated low-melting-point polyester composite fiber with ultraviolet shielding function and preparation method thereof |
| CN116536794A (en) * | 2023-05-05 | 2023-08-04 | 优彩环保资源科技股份有限公司 | Preparation method of sheath-core composite three-dimensional curled low-melting-point polyester fiber |
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Application publication date: 20170531 |