CN106757444B - A kind of low melting point polyester fiber and preparation method thereof - Google Patents
A kind of low melting point polyester fiber and preparation method thereof Download PDFInfo
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- CN106757444B CN106757444B CN201710018733.1A CN201710018733A CN106757444B CN 106757444 B CN106757444 B CN 106757444B CN 201710018733 A CN201710018733 A CN 201710018733A CN 106757444 B CN106757444 B CN 106757444B
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- Prior art keywords
- melting point
- low
- point polyester
- polyester fiber
- low melting
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- 238000002844 melting Methods 0.000 title claims abstract description 241
- 229920000728 polyester Polymers 0.000 title claims abstract description 218
- 230000008018 melting Effects 0.000 title claims abstract description 132
- 239000000835 fiber Substances 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 520
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 148
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 96
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000009987 spinning Methods 0.000 claims abstract description 53
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 37
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 32
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 32
- 238000005406 washing Methods 0.000 claims abstract description 23
- 239000005711 Benzoic acid Substances 0.000 claims abstract description 16
- 235000010233 benzoic acid Nutrition 0.000 claims abstract description 16
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 16
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluic acid Chemical compound CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005520 cutting process Methods 0.000 claims abstract description 11
- 150000004671 saturated fatty acids Chemical class 0.000 claims abstract description 7
- 125000004494 ethyl ester group Chemical group 0.000 claims abstract description 6
- 150000004702 methyl esters Chemical class 0.000 claims abstract description 6
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 70
- 230000032050 esterification Effects 0.000 claims description 48
- 238000005886 esterification reaction Methods 0.000 claims description 48
- 238000006068 polycondensation reaction Methods 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 34
- 239000003054 catalyst Substances 0.000 claims description 30
- 239000003381 stabilizer Substances 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 23
- 208000011580 syndromic disease Diseases 0.000 claims description 23
- 230000035484 reaction time Effects 0.000 claims description 20
- 238000007664 blowing Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000009471 action Effects 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 6
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical group C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 6
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 5
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical group [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 5
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 claims description 4
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 150000004665 fatty acids Chemical class 0.000 claims description 3
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- ZQVKTHRQIXSMGY-UHFFFAOYSA-N 4-Ethylbenzoic acid Chemical compound CCC1=CC=C(C(O)=O)C=C1 ZQVKTHRQIXSMGY-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006116 polymerization reaction Methods 0.000 abstract description 5
- 150000002148 esters Chemical class 0.000 description 18
- 239000000047 product Substances 0.000 description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 8
- 125000003827 glycol group Chemical group 0.000 description 8
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 description 8
- 229920001634 Copolyester Polymers 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 4
- 239000005643 Pelargonic acid Substances 0.000 description 4
- 150000001721 carbon Chemical group 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 239000004831 Hot glue Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- WSXIMVDZMNWNRF-UHFFFAOYSA-N antimony;ethane-1,2-diol Chemical compound [Sb].OCCO WSXIMVDZMNWNRF-UHFFFAOYSA-N 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000739 chaotic effect Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005108 dry cleaning Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—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
-
- 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
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
- D01D5/092—Cooling filaments, threads or the like, leaving the spinnerettes in shafts or chimneys
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Multicomponent Fibers (AREA)
Abstract
The present invention relates to a kind of low melting point polyester fiber and preparation method thereof, low melting point polyester fiber is skin-core structure, and cortex is low-melting point polyester, sandwich layer PET；The low-melting point polyester is made of terephthalic acid (TPA) segment, M-phthalic acid segment, ethylene glycol segment, diethylene glycol (DEG) segment and molecular weight regulator end-capping group；The corresponding molecular weight regulator of molecular weight regulator end-capping group is specially benzoic acid, p-methylbenzoic acid or p-ethylbenzoic acid, is perhaps the methyl esters or ethyl ester corresponding to them or methyl esters or ethyl ester for saturated fatty acid or corresponding to it；The content < 0.5ppm of acetaldehyde in the low melting point polyester fiber.Preparation method includes low-melting point polyester polymerization and core-sheath spinning step, and rear spinning uses drawing-off-washing process, and drawing-off is using the oil bath drawing-off that sodium sulfite is added, through curling, cutting and dry acquisition low melting point polyester fiber.Low melting point polyester fiber fusing point produced by the present invention is low, and acetaldehyde is low.
Description
Technical field
The invention belongs to low melting point polyester fiber field, it is related to a kind of low melting point polyester fiber and preparation method thereof, especially
It is to be related to a kind of low melting point polyester fiber and preparation method thereof of low acetaldehyde.
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,
Have the characteristics that water-fastness, dry-cleaning, the excellent performance of sand washing and easy strike-through, peel strength are high, is a kind of high-grade bonding raw material.This
Outside, copolyester with low melting point 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.
A series of side reaction can occur in the esterification of low-melting point polyester and polycondensation process, generate many by-products
Object, wherein being affected is acetaldehyde, acetaldehyde can cause uncomfortable symptom.The application of low-melting point polyester generates unfavorable shadow
It rings, especially limits its application in automobile, closed environment.By-product of the acetaldehyde as polymerization reaction can not polymerize
In completely eliminate, therefore how to reduce the difficult point that the content of acetaldehyde in low melting point polyester fiber is production process.
Summary of the invention
The purpose of the present invention is overcoming the low-melting point polyester of the low melting point polyester fiber of the prior art to rise, fusing point is high, and melting is fast
The problems such as acetaldehyde is high in slow and low melting point polyester fiber is spent, realizes the production of large-scale, it is poly- to provide a kind of low melting point
Ester fiber and preparation method thereof.Low melting point polyester fiber of the invention is skin-core structure, and cortex is low-melting point polyester, and sandwich layer is
The fusing point that rises of conventional polyester, low melting point polyester fiber obtained decreases and melts speed quickening, at the corresponding temperature at once
Melting, melting effect are good.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of low melting point polyester fiber of the invention is skin-core structure；Cortex in the skin-core structure is poly- for low melting point
Ester；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 and
Molecular weight regulator end-capping group composition；
The corresponding molecular weight regulator of the molecular weight regulator end-capping group be specially benzoic acid, p-methylbenzoic acid or
P-ethylbenzoic acid, perhaps for the methyl esters or ethyl ester corresponding to them or the methyl esters for saturated fatty acid or corresponding to it or
Ethyl ester；
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 destroys the regularity of molecular structure, to reduce fusing point；
The molecular weight distribution of high polymer is widened in the addition of molecular weight regulator, and when relative molecular weight distribution broadens, low-melting point polyester is molten
The flowing temperature of body declines, this is because the temperature range that relative displacement occurs for strand at this time broadens, it is opposite point especially low
Protonatomic mass component plays the role of internally plasticized, makes polyester fondant that the temperature decline of flowing take place, therefore keep low melting point poly-
Ester can melt rapidly at corresponding temperature, improve the melting behaviour of low-melting point polyester.Select carbon atom number for the full of 9-30
And fatty acid, if being because the boiling point of the too low saturated fatty acid of carbon atom number is relatively low, when polycondensation, can deviate from, and influence its content
Stability；If the excessively high saturated fatty acid of carbon atom number, the activity decline of carboxylic acid will affect its extent of reaction.
The content < 0.5ppm of acetaldehyde in the low melting point polyester fiber.
As a preferred technical scheme:
A kind of low melting point polyester fiber as described above, filament number are 1.5~3.0dtex, breaking strength >=3.00cn/
dtex；The core-skin area ratio of the skin-core structure is 40~60:60~40.
A kind of low melting point polyester fiber as described above, the fusing point of the low-melting point polyester is between 100 DEG C~180 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 >=63%；It is described low
The number-average molecular weight of melt polyester is 15000-35000, molecular weight distributing index D=2.5~4.5 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 low melting point polyester fiber as described above, the molecular weight regulator end-capping group are that phthalic acid segment rubs
The 0.01%~0.5% of that number.Phthalic acid segment refers to terephthalic acid (TPA) segment and M-phthalic acid segment.
The present invention also provides the preparation methods of low melting point polyester fiber as described above, comprising steps of
A) low-melting point polyester polymerize；
(1) terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG) and molecular weight regulator are subjected to esterification；
(2) then, polycondensation reaction is carried out, low-melting point polyester is made；
B) spinning；
Preceding spin uses core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer；It spins and uses afterwards
Drawing-off-washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.The purpose of washing is to be further reduced acetaldehyde
Amount, while also cleaning the sodium sulfite that carries on fiber surface.
A kind of preparation method of low melting point polyester fiber as described above, terephthalic acid (TPA), M-phthalic acid, diethylene glycol (DEG) with
The molar ratio of ethylene glycol is 1:0.4~0.6:0.1~0.3:1.8~2.5；The content of the molecular weight regulator is phthalic acid
The 0.01%~0.5% of molal quantity.
A kind of preparation method of low melting point polyester fiber as described above, the specific steps of low-melting point polyester polymerization are as follows:
(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, and temperature is 230 DEG C~250 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；
(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.
A kind of preparation method of low melting point polyester fiber as described above, the main technologic parameters of the spinning are as follows: spinning
Temperature: 262-275 DEG C of cortex, 280-288 DEG C of sandwich layer, spinning speed: 500-1100m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 50 DEG C~80 DEG C, and circular blow wind wind speed is 1.0m/
S~3.0m/s；Second circular blow wind-warm syndrome is 14 DEG C~20 DEG C, and circular blow wind wind speed is 2.0m/s~4.0m/s；Twice cool down circular blow
30~50cm of wind interval；
Drawing-off uses oil bath drawing-off, and the sodium sulfite of 5~10wt% is added in oil bath, and the temperature of oil bath is 65 DEG C~75
℃；The temperature of washing is 65 DEG C~75 DEG C；
Drafting multiple is 2.5~2.7 times；
It 50-60 DEG C of coiling temperature, crimps main pressure 0.4-0.6MPa, crimps back pressure 0.2-0.4MPa, crispation number 8-10/
25mm, crimpness 11-13%, drying temperature are 65 DEG C~75 DEG C, time 10min~20min.
A kind of preparation method of low melting point polyester fiber as described above, the catalyst are antimony oxide, ethylene glycol
Antimony or antimony acetate, catalyst charge are the 0.01%~0.05% of phthalic acid total weight；The stabilizer is phosphoric acid triphen
Ester, trimethyl phosphate or Trimethyl phosphite, stabilizer additional amount are the 0.01%~0.05% of the phthalic acid total weight.
The principle of the present invention are as follows:
For no modified component, unbranched, without molecular weight regulator conventional polyester, molecular chain structure is containing phenyl ring
The regular linear macromolecule of structure, functional group's marshalling on strand, regularity is good, flexibility is poor, crystallinity is high, this
A little characteristics hinder the reduction of fusing point, thus melting temperature is high.
A series of side reaction has occurred in esterification and polycondensation process in polyester, generates a series of by-product,
It is middle to influence maximum by-product for acetaldehyde.By-product of the acetaldehyde as polymerization reaction, can not completely eliminate, therefore such as in polymerization
What reduces the difficult point that the content of acetaldehyde in low melting point polyester fiber is production process.
The preparation method of low melting point polyester fiber of the invention, using the cooling circular blow of twice during ring wind quenching
Wind makes acetaldehyde is as much as possible to volatilize away, and the boiling point of acetaldehyde is 20.8 DEG C, volatile, first of 50 DEG C of circular blow wind-warm syndrome~
At 80 DEG C, the residence time of polyester fiber at relatively high temperatures is extended, the volatile quantity of acetaldehyde is increased, in second circular blow wind
At 14 DEG C~20 DEG C of temperature, on the one hand makes tow cooling, on the other hand further acetaldehyde is made to volatilize.Add 5% in oil bath simultaneously
On the one hand~10% sodium sulfite absorbs acetaldehyde using sodium sulfite, in another aspect oil bath tow due to stretching action,
Fiber attenuates, and surface area increases, so that acetaldehyde and the degree of sodium sulfite reaction further increase, is fully absorbed acetaldehyde,
Thus increase the acetaldehyde diffusion outside from fibrous inside；And the addition of rinsing bowl can wash away the Asia that tow is stained in oil bath
Sodium sulphate；Through the above process, make the acetaldehyde < 0.5ppm in fiber；
The raw material of polyester is terephthalic acid (TPA) and ethylene glycol, and M-phthalic acid, diethylene glycol (DEG), monoacid series are added wherein
Molecular structure is destroyed, it is made to become unordered chaotic structure from the ordered structure of high-sequential, the addition of M-phthalic acid changes
Ratio and size between the different sub- macro crystallization forms of polyester, keep crystallizing polyester difficult, are intended to unformed mode
In the presence of；The addition of diethylene glycol (DEG) increases the flexibility of copolyesters macromolecular chain, reduces fusing point；The addition of molecular weight regulator increases low
The molecular weight of melt polyester, in 5 DEG C/min of heating rate, more than fusing point in the range of 20 DEG C, low-melting point polyester melts journey
Degree >=63% shows as melting speed and accelerates；And conventional low-melting point polyester is under same Elevated Temperature Conditions, this temperature range
Interior melting degree≤20%；The present invention, which reduces low-melting point polyester part macromolecular weight, can reduce softening and flowing temperature
Degree is conducive to low melting point infiltration adherend, increases bond effect；By M-phthalic acid segment, diethylene glycol (DEG) segment and molecular weight
Prepared low-melting point polyester is added in the modified components such as regulator end-capping group, has had melting temperature is low, and melting speed is fast etc.
Advantage.
The utility model has the advantages that
(1) it is dried in a kind of preparation method of low melting point polyester fiber of the invention using twice cooling ring, uses up acetaldehyde
May more than volatilization go out, the boiling point of acetaldehyde is 20.8 DEG C, volatile, at first at 50 DEG C~80 DEG C of circular blow wind-warm syndrome, acetaldehyde
It can largely volatilize, at 14 DEG C~20 DEG C of second circular blow wind-warm syndrome, on the one hand make tow cooling, on the other hand further make acetaldehyde
Volatilization.
(2) add the Asia of 5%~10wt% in a kind of preparation method of low melting point polyester fiber of the invention in oil bath
On the one hand sodium sulphate absorbs acetaldehyde using sodium sulfite, the surface area of tow is big in another aspect oil bath, so that acetaldehyde and Asia
The degree of sodium sulphate reaction further increases, and is fully absorbed acetaldehyde.
(3) raw material of low-melting point polyester produced by the present invention is terephthalic acid (TPA) segment and ethylene glycol segment, in macromolecular
Containing M-phthalic acid segment, diethylene glycol (DEG) segment and molecular weight regulator end-capping group, prepared low-melting point polyester has
The advantages that melting temperature is low, and melting speed is fast.
(4) raw material of low-melting point polyester produced by the present invention is terephthalic acid (TPA) and ethylene glycol, and molecular weight regulator adds
Enter to widen the molecular weight distribution of high polymer, when relative molecular weight distribution broadens, the flowing temperature of polyester fondant declines, this be by
It broadens in the temperature range that relative displacement occurs for strand at this time, especially low relative molecular mass component plays internally plasticized
Effect makes polyester fondant that the temperature decline of flowing take place, therefore low-melting point polyester is enable to melt rapidly at corresponding temperature
Melt, improves the melting behaviour of low-melting point polyester.In 5 DEG C/min of heating rate, more than fusing point in the range of 20 DEG C, eutectic
Point polyester melt degree >=63% shows as melting speed and accelerates；And conventional low-melting point polyester is under same Elevated Temperature Conditions,
Melting degree≤20% in this temperature range；Softening and stream can be reduced by reducing low-melting point polyester part macromolecular weight
Dynamic temperature is conducive to low melting point infiltration adherend, increases 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
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 low melting point polyester fiber:
A) low-melting point polyester polymerize；
(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 are normal pressure, and temperature is 230 DEG C, when the quantity of distillate of the water in esterification reaches
Theoretical value 90% or more when be esterification terminal, obtain esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid, two sweet
The molar ratio of alcohol and ethylene glycol is 1:0.4:0.1:1.8；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；
Preceding spin uses core-sheath spinning technique, using low-melting point polyester as cortex, using PET as sandwich layer；It spins afterwards and uses drawing-off-
Washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.
The main technologic parameters of spinning are as follows:
Spinning temperature: 262 DEG C of cortex, 280 DEG C of sandwich layer, spinning speed: 500m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 50 DEG C, and circular blow wind wind speed is 1.0m/s；Described second
Circular blow wind-warm syndrome in road is 14 DEG C, and circular blow wind wind speed is 2.0m/s；Twice cooling ring blowing interval 30cm；
Drawing-off uses oil bath drawing-off, and 5 sodium sulfite is added in oil bath, and the temperature of oil bath is 65 DEG C；The temperature of washing is
65℃；
Drafting multiple is 2.5 times；
It 50 DEG C of coiling temperature, crimps main pressure 0.4MPa, crimps back pressure 0.2MPa, 8/25mm of crispation number, crimpness 11%,
Drying temperature is 65 DEG C, time 10min.
The low melting point polyester fiber prepared through the above steps is skin-core structure；Cortex in skin-core structure is poly- for low melting point
Ester；Sandwich layer in skin-core structure is PET；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, glycol chain
Section, diethylene glycol (DEG) segment, benzoic acid end-capping group section composition；Benzoic acid end-capping group is phthalic acid segment molal quantity
0.01%, the fusing point of low-melting point polyester is at 100 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 80%；The number-average molecular weight of low-melting point polyester is 15000, low-melting point polyester
Molecular weight distributing index D=2.5.The content of acetaldehyde is 0.49ppm, the monofilament of low melting point polyester fiber in low melting point polyester fiber
Fiber number is 1.5dtex, breaking strength 3.00cN/dtex；The core-skin area ratio of skin-core structure is 40:60.
Embodiment 2
A kind of preparation method of low melting point polyester fiber:
A) low-melting point polyester polymerize；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), p-methylbenzoic acid are made into slurry, it is esterified
It reacts, under nitrogen atmosphere compressive reaction, moulding pressure 0.3MPa, temperature is 250 DEG C, when distillating for the water in esterification
Amount is esterification terminal when reaching 90% of theoretical value or more, obtains esterification products；Wherein, terephthalic acid (TPA), isophthalic diformazan
The molar ratio of acid, diethylene glycol (DEG) and ethylene glycol is 1:0.6:0.3:2.5；The additional amount of p-methylbenzoic acid is phthalic acid molal quantity
0.5%.
(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；
Preceding spin uses core-sheath spinning technique, using low-melting point polyester as cortex, using PET as sandwich layer；It spins afterwards and uses drawing-off-
Washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.
The main technologic parameters of spinning are as follows:
Spinning temperature: 275 DEG C of cortex, 288 DEG C of sandwich layer, spinning speed: 1100m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 80 DEG C, and circular blow wind wind speed is 3.0m/s；Described second
Circular blow wind-warm syndrome in road is 20 DEG C, and circular blow wind wind speed is 4.0m/s；Twice cooling ring blowing interval 50cm；
Drawing-off uses oil bath drawing-off, and the sodium sulfite of 10wt% is added in oil bath, and the temperature of oil bath is 75 DEG C；The temperature of washing
Degree is 75 DEG C；
Drafting multiple is 2.7 times；
60 DEG C of coiling temperature, main pressure 0.6MPa is crimped, crimps back pressure 0.4MPa, 10/25mm of crispation number, crimpness
13%, drying temperature is 75 DEG C, time 20min.
The low melting point polyester fiber prepared through the above steps is skin-core structure；Cortex in skin-core structure is poly- for low melting point
Ester；Sandwich layer in skin-core structure is PET；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, glycol chain
Section, diethylene glycol (DEG) segment, p-methylbenzoic acid end-capping group composition；P-methylbenzoic acid end-capping group is phthalic acid segment mole
Several 0.5%, 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 20000, and low melting point is poly-
The molecular weight distributing index D=3 of ester.The content of acetaldehyde is 0.3ppm, the list of low melting point polyester fiber in low melting point polyester fiber
Silk size is 3.0dtex, breaking strength 3.50cN/dtex；The core-skin area ratio of skin-core structure is 60:40.
Embodiment 3
A kind of preparation method of low melting point polyester fiber:
A) low-melting point polyester polymerize；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), p-ethylbenzoic acid are made into slurry, it is esterified
It reacts, under nitrogen atmosphere compressive reaction, moulding pressure 0.1MPa, temperature is 240 DEG C, when distillating for the water in esterification
Amount is esterification terminal when reaching 90% of theoretical value or more, obtains esterification products；Wherein, terephthalic acid (TPA), isophthalic diformazan
The molar ratio of acid, diethylene glycol (DEG) and ethylene glycol is 1:0.5:0.2:2；The additional amount of p-ethylbenzoic acid is phthalic acid molal quantity
0.1%.
(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；
Preceding spin uses core-sheath spinning technique, using low-melting point polyester as cortex, using PET as sandwich layer；It spins afterwards and uses drawing-off-
Washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.
The main technologic parameters of spinning are as follows:
Spinning temperature: 265 DEG C of cortex, 285 DEG C of sandwich layer, spinning speed: 1000m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 60 DEG C, and circular blow wind wind speed is 2.0m/s；Described second
Circular blow wind-warm syndrome in road is 16 DEG C, and circular blow wind wind speed is 3.0m/s；Twice cooling ring blowing interval 40cm；
Drawing-off uses oil bath drawing-off, and the sodium sulfite of 6wt% is added in oil bath, and the temperature of oil bath is 70 DEG C；The temperature of washing
Degree is 70 DEG C；
Drafting multiple is 2.6 times；
It 55 DEG C of coiling temperature, crimps main pressure 0.5MPa, crimps back pressure 0.3MPa, 9/25mm of crispation number, crimpness 12%,
Drying temperature is 70 DEG C, time 15min.
The low melting point polyester fiber prepared through the above steps is skin-core structure；Cortex in skin-core structure is poly- for low melting point
Ester；Sandwich layer in skin-core structure is PET；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, glycol chain
Section, diethylene glycol (DEG) segment, p-ethylbenzoic acid end-capping group composition；P-ethylbenzoic acid end-capping group is phthalic acid segment mole
Several 0.1%, 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
In the range of when, the melting degree of low-melting point polyester is 82%；The number-average molecular weight of low-melting point polyester is 25000, and low melting point is poly-
The molecular weight distributing index D=4 of ester.The content of acetaldehyde is 0.4ppm, the list of low melting point polyester fiber in low melting point polyester fiber
Silk size is 2.0dtex, breaking strength 3.20cN/dtex；The core-skin area ratio of skin-core structure is 50:50.
Embodiment 4
A kind of preparation method of low melting point polyester fiber:
A) low-melting point polyester polymerize；
(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 0.2MPa, temperature is 245 DEG C, when the quantity of distillate of the water in esterification reaches
To theoretical value 90% or more when be esterification terminal, obtain esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid, two
The molar ratio of glycol and ethylene glycol is 1:0.5:0.25:2.2；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；
Preceding spin uses core-sheath spinning technique, using low-melting point polyester as cortex, using PET as sandwich layer；It spins afterwards and uses drawing-off-
Washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.
The main technologic parameters of spinning are as follows:
Spinning temperature: 270 DEG C of cortex, 284 DEG C of sandwich layer, spinning speed: 700m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 70 DEG C, and circular blow wind wind speed is 2.5m/s；Described second
Circular blow wind-warm syndrome in road is 18 DEG C, and circular blow wind wind speed is 2.5m/s；Twice cooling ring blowing interval 45cm；
Drawing-off uses oil bath drawing-off, and the sodium sulfite of 8wt% is added in oil bath, and the temperature of oil bath is 72 DEG C；The temperature of washing
Degree is 68 DEG C；
Drafting multiple is 2.55 times；
55 DEG C of coiling temperature, main pressure 0.55MPa is crimped, crimps back pressure 0.25MPa, 9/25mm of crispation number, crimpness
12%, drying temperature is 72 DEG C, time 16min.
The low melting point polyester fiber prepared through the above steps is skin-core structure；Cortex in skin-core structure is poly- for low melting point
Ester；Sandwich layer in skin-core structure is PET；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, glycol chain
Section, diethylene glycol (DEG) segment, pelargonic acid end-capping group composition；Pelargonic acid end-capping group is the 0.2% of phthalic acid segment molal quantity, 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 content of acetaldehyde is 0.35ppm in low melting point polyester fiber, and the filament number of low melting point polyester fiber is
2.4dtex, breaking strength 3.60cN/dtex；The core-skin area ratio of skin-core structure is 45:55.
Embodiment 5
A kind of preparation method of low melting point polyester fiber:
A) low-melting point polyester polymerize；
(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 0.1MPa, temperature is 245 DEG C, when the quantity of distillate of the water in esterification reaches
Theoretical value 90% or more when be esterification terminal, obtain esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid, two sweet
The molar ratio of alcohol and ethylene glycol is 1:0.5:0.15:2.3；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；
Preceding spin uses core-sheath spinning technique, using low-melting point polyester as cortex, using PET as sandwich layer；It spins afterwards and uses drawing-off-
Washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.
The main technologic parameters of spinning are as follows:
Spinning temperature: 274 DEG C of cortex, 285 DEG C of sandwich layer, spinning speed: 900m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 75 DEG C, and circular blow wind wind speed is 1.8m/s；Described second
Circular blow wind-warm syndrome in road is 17 DEG C, and circular blow wind wind speed is 3.5m/s；Twice cooling ring blowing interval 44cm；
Drawing-off uses oil bath drawing-off, and the sodium sulfite of 8wt% is added in oil bath, and the temperature of oil bath is 70 DEG C；The temperature of washing
Degree is 72 DEG C；
Drafting multiple is 2.6 times；
55 DEG C of coiling temperature, main pressure 0.55MPa is crimped, crimps back pressure 0.3MPa, 10/25mm of crispation number, crimpness
13%, drying temperature is 75 DEG C, time 10min.
The low melting point polyester fiber prepared through the above steps is skin-core structure；Cortex in skin-core structure is poly- for low melting point
Ester；Sandwich layer in skin-core structure is PET；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, glycol chain
Section, diethylene glycol (DEG) segment, capric acid end-capping group composition；Capric acid end-capping group is the 0.4% of phthalic acid segment molal quantity, low melting point
The fusing point of polyester is at 120 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 82%；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 content of acetaldehyde is 0.4ppm in low melting point polyester fiber, and the filament number of low melting point polyester fiber is 1.9dtex,
Breaking strength is 3.30cN/dtex；The core-skin area ratio of skin-core structure is 55:45.
Embodiment 6
A kind of preparation method of low melting point polyester fiber:
A) low-melting point polyester polymerize；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), benzoic acid formicester are made into slurry, be esterified anti-
It answers, under nitrogen atmosphere compressive reaction, moulding pressure 0.3MPa, temperature is 250 DEG C, when the quantity of distillate of the water in esterification
It is esterification terminal when reaching 90% or more of theoretical value, obtains esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid,
The molar ratio of diethylene glycol (DEG) and ethylene glycol is 1:0.4:0.3:1.8；The additional amount of benzoic acid formicester is phthalic acid molal quantity
0.09%.
(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；
Preceding spin uses core-sheath spinning technique, using low-melting point polyester as cortex, using PET as sandwich layer；It spins afterwards and uses drawing-off-
Washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.
The main technologic parameters of spinning are as follows:
Spinning temperature: 268 DEG C of cortex, 283 DEG C of sandwich layer, spinning speed: 600m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 60 DEG C, and circular blow wind wind speed is 2.0m/s；Described second
Circular blow wind-warm syndrome in road is 18 DEG C, and circular blow wind wind speed is 3.0m/s；Twice cooling ring blowing interval 45cm；
Drawing-off uses oil bath drawing-off, and the sodium sulfite of 8wt% is added in oil bath, and the temperature of oil bath is 70 DEG C；The temperature of washing
Degree is 70 DEG C；
Drafting multiple is 2.5 times；
It 60 DEG C of coiling temperature, crimps main pressure 0.4MPa, crimps back pressure 0.4MPa, 9/25mm of crispation number, crimpness 12%,
Drying temperature is 70 DEG C, time 20min.
The low melting point polyester fiber prepared through the above steps is skin-core structure；Cortex in skin-core structure is poly- for low melting point
Ester；Sandwich layer in skin-core structure is PET；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, glycol chain
Section, diethylene glycol (DEG) segment, benzoic acid formicester end-capping group composition；Benzoic acid formicester end-capping group 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 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 84%；The number-average molecular weight of low-melting point polyester is 20000, low-melting point polyester
Molecular weight distributing index D=3.The content of acetaldehyde is 0.38ppm in low melting point polyester fiber, and the monofilament of low melting point polyester fiber is fine
Degree is 2.5dtex, breaking strength 3.30cN/dtex；The core-skin area ratio of skin-core structure is 48:52.
Embodiment 7
A kind of preparation method of low melting point polyester fiber:
A) low-melting point polyester polymerize；
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG), benzoic acid second rouge are made into slurry, be esterified anti-
It answers, 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 90% or more when be esterification terminal, obtain esterification products；Wherein, terephthalic acid (TPA), M-phthalic acid, two
The molar ratio of glycol and ethylene glycol is 1:0.4:0.3:1.8；The additional amount of benzoic acid second rouge is phthalic acid molal quantity
0.5%.
(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；
Preceding spin uses core-sheath spinning technique, using low-melting point polyester as cortex, using PET as sandwich layer；It spins afterwards and uses drawing-off-
Washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.
The main technologic parameters of spinning are as follows:
Spinning temperature: 262 DEG C of cortex, 288 DEG C of sandwich layer, spinning speed: 1100m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 80 DEG C, and circular blow wind wind speed is 1.0m/s；Described second
Circular blow wind-warm syndrome in road is 20 DEG C, and circular blow wind wind speed is 2.0m/s；Twice cooling ring blowing interval 50cm；
Drawing-off uses oil bath drawing-off, and the sodium sulfite of 10wt% is added in oil bath, and the temperature of oil bath is 70 DEG C；The temperature of washing
Degree is 65 DEG C；
Drafting multiple is 2.7 times；
55 DEG C of coiling temperature, main pressure 0.5MPa is crimped, crimps back pressure 0.3MPa, 10/25mm of crispation number, crimpness
11%, drying temperature is 75 DEG C, time 20min.
The low melting point polyester fiber prepared through the above steps is skin-core structure；Cortex in skin-core structure is poly- for low melting point
Ester；Sandwich layer in skin-core structure is PET；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, glycol chain
Section, diethylene glycol (DEG) segment, benzoic acid second rouge end-capping group composition；Benzoic acid second rouge end-capping group is phthalic acid segment molal quantity
0.5%, the fusing point of low-melting point polyester is at 175 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 20000, low-melting point polyester
Molecular weight distributing index D=3.8.The content of acetaldehyde is 0.4ppm, the monofilament of low melting point polyester fiber in low melting point polyester fiber
Fiber number is 2.3dtex, breaking strength 3.50cN/dtex；The core-skin area ratio of skin-core structure is 55:45.
Embodiment 8-31
A kind of preparation method of 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) and ethylene glycol molar ratio be 1:0.4~0.6:0.1~0.3:1.8~
2.5；The additional amount of molecular weight regulator is the 0.01%~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 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；
Preceding spin uses core-sheath spinning technique, using low-melting point polyester as cortex, using PET as sandwich layer；It spins afterwards and uses drawing-off-
Washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.
The main technologic parameters of spinning are as follows:
Spinning temperature: 265 DEG C of cortex, 288 DEG C of sandwich layer, spinning speed: 1000m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 80 DEG C, and circular blow wind wind speed is 1.0m/s；Described second
Circular blow wind-warm syndrome in road is 20 DEG C, and circular blow wind wind speed is 3.0m/s；Twice cooling ring blowing interval 50cm；
Drawing-off uses oil bath drawing-off, and the sodium sulfite of 7wt% is added in oil bath, and the temperature of oil bath is 70 DEG C；The temperature of washing
Degree is 65 DEG C；
Drafting multiple is 2.6 times；
It 55 DEG C of coiling temperature, crimps main pressure 0.5MPa, crimps back pressure 0.3MPa, 9/25mm of crispation number, crimpness 12%,
Drying temperature is 75 DEG C, time 20min.
The low melting point polyester fiber prepared through the above steps is skin-core structure；Cortex in skin-core structure is poly- for low melting point
Ester；Sandwich layer in skin-core structure is PET；Low-melting point polyester is by terephthalic acid (TPA) segment, M-phthalic acid segment, glycol chain
Section, diethylene glycol (DEG) segment, molecular weight regulator end-capping group composition；Low-melting point polyester is 5 DEG C/min in heating rate, and low melting point is poly-
When more than ester fusing point in the range of 20 DEG C, melting degree >=80% of low-melting point polyester.Acetaldehyde contains in low melting point polyester fiber
< 0.5ppm is measured, the filament number of low melting point polyester fiber is 1.5~3.0dtex, breaking strength >=3.00cN/dtex；Core-skin
The core-skin area ratio of structure is 40~60:60~40.
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 low melting point polyester fiber, filament number, breaking strength and skin-core structure
The particular product performance parameters such as core-skin area ratio are as shown in the table:
Claims (9)
1. a kind of low melting point polyester fiber, it is characterized in that: the low melting point polyester fiber is skin-core structure；In the skin-core structure
Cortex be 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 and molecule
Measure regulator end-capping group composition；
The fusing point of the low-melting point polyester is between 100 DEG C~180 DEG C；It is 5 DEG C/min in heating rate, 20 DEG C more than fusing point
In the range of when, low-melting point polyester melting degree >=63%；
The corresponding molecular weight regulator of the molecular weight regulator end-capping group is specially benzoic acid, p-methylbenzoic acid or to second
Yl benzoic acid is perhaps the methyl esters or ethyl ester corresponding to them or methyl esters or ethyl ester for saturated fatty acid or corresponding to it；
The saturated fatty acid refers to that carbon atom number is the fatty acid of 9-30；
The content < 0.5ppm of acetaldehyde in the low melting point polyester fiber.
2. a kind of low melting point polyester fiber according to claim 1, which is characterized in that the list of the low melting point polyester fiber
Silk size is 1.5~3.0dtex, breaking strength >=3.00cN/dtex；The core-skin area ratio of the skin-core structure is 40~60:
60~40.
3. a kind of low melting point polyester fiber according to claim 1, which is characterized in that the number of the low-melting point polyester is divided equally
Son amount is 15000-35000, molecular weight distributing index D=2.5~4.5 of the low-melting point polyester.
4. a kind of low melting point polyester fiber according to claim 1, which is characterized in that the molecular weight regulator END CAPPED GROUP
Group is the 0.01%~0.5% of phthalic acid segment molal quantity.
5. the preparation method of the low melting point polyester fiber as described in claim 1-4 is any, it is characterized in that: comprising steps of
A) low-melting point polyester polymerize；
(1) terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG) and molecular weight regulator are subjected to esterification；
(2) then, polycondensation reaction is carried out, low-melting point polyester is made；
B) spinning；
Preceding spin uses core-sheath spinning technique, using the low-melting point polyester as cortex, using PET as sandwich layer；It spins afterwards and uses drawing-off-
Washing process；Through curling, cutting and dry acquisition low melting point polyester fiber.
6. a kind of preparation method of low melting point polyester fiber according to claim 5, which is characterized in that terephthalic acid (TPA),
The molar ratio of M-phthalic acid, diethylene glycol (DEG) and ethylene glycol is 1:0.4~0.6:0.1~0.3:1.8~2.5；The molecular weight tune
The content for saving agent is the 0.01%~0.5% of phthalic acid molal quantity.
7. a kind of preparation method of low melting point polyester fiber according to claim 5, which is characterized in that low-melting point polyester is poly-
The specific steps of conjunction are as follows:
(1) esterification；
After terephthalic acid (TPA), M-phthalic acid, ethylene glycol, diethylene glycol (DEG) and molecular weight regulator are made into slurry, be esterified anti-
It answers, under nitrogen atmosphere compressive reaction, moulding pressure is normal pressure~0.3MPa, and temperature is 230 DEG C~250 DEG C, works as esterification
In the quantity of distillate of water be esterification terminal when reaching 90% of theoretical value or more, obtain 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 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.
8. a kind of preparation method of low melting point polyester fiber according to claim 5, which is characterized in that the master of the spinning
Want technological parameter are as follows:
Spinning temperature: 262-275 DEG C of cortex, 280-288 DEG C of sandwich layer, spinning speed: 500-1100m/min；
Blowing is that twice cooling ring is dried；First of circular blow wind-warm syndrome is 50 DEG C~80 DEG C, and circular blow wind wind speed is 1.0m/s~3.0m/
s；Second circular blow wind-warm syndrome is 14 DEG C~20 DEG C, and circular blow wind wind speed is 2.0m/s~4.0m/s；Twice cooling ring blowing interval 30
~50cm；
Drawing-off uses oil bath drawing-off, and the sodium sulfite of 5~10wt% is added in oil bath, and the temperature of the oil bath is 65 DEG C~75
℃；The temperature of washing is 65 DEG C~75 DEG C；
Drafting multiple is 2.5~2.7 times；
50-60 DEG C of coiling temperature, main pressure 0.4-0.6MPa is crimped, crimps back pressure 0.2-0.4MPa, 8-10/25mm of crispation number,
Crimpness 11-13%.
9. a kind of preparation method of low melting point polyester fiber according to claim 7, which is characterized in that the catalyst is
Antimony oxide, antimony glycol or antimony acetate, catalyst charge are the 0.01%~0.05% of phthalic acid total weight；It is described
Stabilizer is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite, and stabilizer additional amount is phthalic acid total weight
0.01%~0.05%.
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| CN109853082B (en) * | 2018-12-27 | 2020-08-14 | 江苏恒力化纤股份有限公司 | Sheath-core thermal fuse and preparation method thereof |
| CN110952161B (en) * | 2019-12-16 | 2021-06-29 | 扬州富威尔复合材料有限公司 | Low-melting-point elastic polyester fiber and preparation method thereof |
| CN110952168B (en) * | 2019-12-16 | 2021-05-28 | 扬州富威尔复合材料有限公司 | Low-content organic volatile matter and low-melting-point polyester fiber and preparation method thereof |
| CN111441100A (en) * | 2020-05-26 | 2020-07-24 | 无锡佳成纤维有限公司 | Spinning forming process of low-melting-point polyester chip |
| CN114262954B (en) * | 2021-12-30 | 2023-07-25 | 扬州富威尔复合材料有限公司 | Preparation of low-melting-point polyester fiber and application of low-melting-point polyester fiber in natural fiber adhesion |
| CN115142150A (en) * | 2022-07-18 | 2022-10-04 | 盛谷(苏州)环保材料有限公司 | Low-melting-point polyester fiber and preparation method thereof |
| 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 |
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