CN105019059B - A kind of super soft hyperfine polyester fiber and preparation method thereof - Google Patents
A kind of super soft hyperfine polyester fiber and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to super soft hyperfine polyester fiber of one kind and preparation method thereof, super soft hyperfine polyester fiber is mainly polyester and is prepared by spinneret orifice melt spinning, oil agent and high-speed winding；The finish of the oil agent at least includes fluorochemical polyether, the 45% of the quality of quality >=finish of fluorochemical polyether；The fluorochemical polyether is the random copolymer of oxirane, [(1,1,2,2 tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane, and its structural formula is：
Description
Technical field
The present invention relates to super soft hyperfine polyester fiber of one kind and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) fiber since the advent of the world, has been obtained rapidly because of its excellent performance
Development, its yield has become the hat of world's synthetic fibers.Polyester fiber has fracture strength and modulus of elasticity height, and resilience is fitted
In, thermal finalization is excellent, and heat-resisting light resistance is good and a series of premium properties such as acid-fast alkali-proof corrosion resistance, and fabric have it is anti-
Wrinkle, the advantages of stiffness is good, so, polyester fiber is widely used in the fields such as clothes, home textile.
The drastically expansion and the change of international situation of polyester production capacity, comfort, feature, variation of the people to clothing
There is a higher requirement with security, the super soft superfine denier polyester production such as terylene 22dtex/48f, 22dtex/72f, 33dtex/72f
Product, its fabric is with the fine and smooth feel of particularly soft, comfortable ventilating, it is easy to the preferable superiority of texture of nursing and outward appearance, more next
More obtain the favor of user.
Produce super soft hyperfine polyester fiber polyester filament individual thread many, specific surface area is big, is difficult to oil, finish is in strand
Surface is difficult to attachment uniformly, and the coherent of tow is poor, and lousiness and broken end are also easy to produce in production process.By selecting Overseas New oil
Mouth, makes tow obtain the effect that preferably oils, while also properly increasing the oil content of FDY strands.Selected area update strategy diffusivity is good, profit
Moist good oil product, it is overall to improve super soft hyperfine polyester fiber and oil uniformity, to ensureing that the quality of product will play larger
Effect.
The content of the invention
It is an object of the invention to provide super soft hyperfine polyester fiber of one kind and preparation method thereof, the present invention is by using Gao Pin
It is fine that the polyester fondant of matter, the design of special spinneret orifice and the use of fluorine-containing finish and high speed spinning prepare super soft ultra-fine polyester
Dimension.The finish of the present invention is made up of mineral oil, fluorochemical polyether, phosphate kalium salt and sodium alkyl sulfonate, and the use of the finish is dense
Spend for 10~20wt%.The composition of the fluorochemical polyether ethylene oxide base monomer used in the present invention is moderate, introduces simultaneously
[(1,1,2,2- tetrafluoro ethyoxyl) methyl] oxirane, adds the hydrogen bond in system, the increase of hydrogen bond is conducive to cloud point
Improve, because of a little qualities for remaining to keep finish while the concentration of finish is being increased.The increase of finish concentration can
To greatly reduce the consumption of energy in finish drying process, energy is saved.
A kind of super soft hyperfine polyester fiber, mainly polyester passes through spinneret orifice melt spinning, oil agent and high-speed winding system
It is standby and obtain；The finish of the oil agent at least includes fluorochemical polyether, the 45% of the quality of quality >=finish of fluorochemical polyether；
The fluorochemical polyether is the random copolymerization of oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and expoxy propane
Thing, its structural formula is：
Wherein, m=10~20, n=20~30, k=1~3；
Fracture strength >=3.8cN/dtex of the super soft hyperfine polyester fiber, elongation at break is 35.0 ± 3.0%, single
Silk size is 0.20~0.50dtex.
The flexibility of super soft hyperfine polyester fiber is very thin mainly due to its filament number, and multifilament total fiber number also compared with and body
Existing, its fabric has the fine and smooth feel of particularly soft, and gloss is soft, comfortable ventilating.
The fluorochemical polyether can not only provide good smooth, emulsification and wetting function, additionally it is possible to be carried for finish system
For substantial amounts of hydrogen bond, cloud point is improved, is conducive to finish to use the raising of high concentration, energy is saved.Oxirane (EO)/epoxy third
Alkane (PO) ratio is one of most important index of polyethers, and the influence to polyethers performance is also very big.Pfpe molecule chain by multiple EO and
The arrangement of PO chain links is formed, and compared with EO, there is a side base on PO chain links, steric hindrance is larger.EO/PO is than increase, i.e. PO chain links
Reduce, pending methyl group quantity declines, intermolecular space steric hindrance is reduced, the hydrogen chain number formed between hydrone is more, so cloud point
Also raise.The presence of branched structure can reduce surface tension in pfpe molecule chain simultaneously, improve wetting speed, increase with EO/PO,
PO chain links containing branched chain methyl are reduced, thus surface tension rise, and wetting speed slows down, therefore must contain in polyethers macromolecular chain
There is a certain amount of PO.But polyethers relies primarily on the oxygen atom in ether with the hydrogen bond that hydrone is formed, so cloud point rise is limited,
The introducing of [(1,1,2,2- tetrafluoro ethyoxyl) methyl] oxirane, due to the presence of fluorine element, is formed between hydrone
It will increase more than hydrogen bond number, and can further improve the cloud point of polyether aqueous solution；Fluorine element will enter one all in branched positional simultaneously
The surface tension of step reduction polyethers.In finish formation oil film, fluorine element, due to the characteristic of fluorine element, can make in surface enrichment
The flatness of finish is further enhanced.
It is used as preferred technical scheme：
A kind of super soft hyperfine polyester fiber as described above, the relative molecular weight of the fluorochemical polyether is 1000~4000；
The cloud point of the fluorochemical polyether is 50~100 DEG C；25~40dyn/cm of surface tension of the fluorochemical polyether.
Also include mineral oil, phosphate kalium salt and alkane in a kind of super soft hyperfine polyester fiber as described above, the finish
Base sodium sulfonate；Mineral oil has good heat resistance, has good compatibility with other components, and it has uniform, the oil film that oils
The characteristics of intensity is high, moreover it is possible to the effective coefficient of friction for reducing fiber and metal, increases the cohesive force of fiber, is conducive to boundling.
Using anionic antistatic agent, surface hydrophilic can be realized, the heat resistance of phosphate kalium salt is relatively good, good is antistatic
Property, it is capable of the antistatic effect of reinforcing fiber, is conducive to the boundling of fiber.The addition of sodium alkyl sulfonate can improve oozing for finish
Saturating ability so that finish can be uniformly adhered on tow in the short period of time, can effectively reduce lousiness, broken end and go out
It is existing.
By weight：Mineral oil is 25~35 parts；Fluorochemical polyether is 50~70 parts；Phosphate kalium salt is 8~15 parts；Alkane
Base sodium sulfonate is 2~7 parts；
Described mineral oil is one kind in 9#~17# mineral oil；Described phosphate kalium salt is dodecylphosphoric acid
One kind in ester sylvite, isomerous tridecanol polyoxyethylene ether phosphate kalium salt and ten tetracosanol phosphate kalium salts；Described alkane
Base sodium sulfonate is one kind in dodecyl sodium sulfate, pentadecyl sulfonic acid sodium and sodium cetanesulfonate；
The finish when in use, the emulsion that oil concentration is 10~20wt% is configured to water.High speed spinning is to upper
Deep-fried twisted dough sticks part requires high, and the uniformity that oils directly influences the bar dry values and dyeing uniformity of fiber, and selected area update strategy diffusivity is good
Fluorine-containing oil product.
Super soft hyperfine polyester fiber as described above a kind of, the line density deviation ratio of the super soft hyperfine polyester fiber≤
0.5%, fracture strength CV value≤3.0%, extension at break CV value≤8.0%, yarn unevenness CV≤2.00%, boiling water shrinkage
7.5 ± 0.5%, oil content 1.00 ± 0.20%.
Present invention also offers a kind of preparation method of super soft hyperfine polyester fiber, by polyester through metering, extrusion, cooling,
Oil, stretch, thermal finalization and high-speed winding, super soft hyperfine polyester fiber is made；
The temperature of the extrusion is 290~295 DEG C；
The wind-warm syndrome of the cooling is 20~25 DEG C；
HT1：75~95 DEG C；
HT2：120~130 DEG C；
The high-speed winding speed is 4000~5000m/min；
The finish preparation method oiled：
Initiator and highly basic are blended, 105~125 DEG C are then heated to, add well mixed oxirane, [(1,
1,2,2- tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane, polymerisation is carried out under protective atmosphere, reaction pressure is small
In 0.4MPa, reach and fluorochemical polyether is obtained after predetermined molecular weight；
Then, fluorochemical polyether, phosphate kalium salt and sodium alkyl sulfonate normal temperature are well mixed, then fed the mixture into again
Into mineral oil, temperature control is 40-55 DEG C, stirs 1~3h, that is, obtains the finish；
By weight：
The finish when in use, the emulsion that oil concentration is 10~20wt% is configured to water.
A kind of super soft hyperfine polyester fiber as described above, the initiator is butanol, and the amount of the butanol is epoxy second
The 1-5 ‰ of alkane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and expoxy propane gross mass；The highly basic is hydroxide
Potassium or sodium hydroxide；The amount of the highly basic is oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and epoxy
The 1-5 ‰ of propane gross mass.
A kind of super soft hyperfine polyester fiber as described above, the oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) first
Base] consumption of oxirane and expoxy propane is 10~20 in molar ratio:1~3:20~30.
A kind of super soft hyperfine polyester fiber as described above, the protective atmosphere is nitrogen atmosphere or inert gas atmosphere；
The predetermined molecular weight refers to that the relative molecular weight of product is 1000~4000.
Super soft hyperfine polyester fiber as described above a kind of, the product reached after predetermined molecular weight also neutralized,
Absorption, vacuum dehydration, drying and filtering.
Super soft hyperfine polyester fiber as described above a kind of, the dyeing of the super soft hyperfine polyester fiber is：
Dyeing is Disperse Red 3B, disperse blue SE-2R with disperse dyes or disperses bright blue S-GL, and fiber is respectively in HTHP
Dyed in machine；Fiber nonionic surfactant is handled 30 minutes at 60 DEG C before dye；Dye dosage is 2.0% (o.w.f)；Point
Powder NNO1.2g/L, pH value is 5, and bath raio is 1:50,60 DEG C enter dye, are warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C of each constant temperature
Dye 1h.
A kind of super soft hyperfine polyester fiber of the present invention, because its filament number is very thin, its fabric is fine and smooth with particularly soft
Feel, gloss is soft, comfortable ventilating, it is easy to nursing and outward appearance the preferable superiority of texture, increasingly obtain the green grass or young crops of user
Look at.
Beneficial effect：
1st, super soft hyperfine polyester fiber, is the particular fabric raw material with unique aesthetic feeling and function.
2nd, using fluorine-containing finish, the composition of the polyethers ethylene oxide base monomer in finish is moderate, while introduce [(1,
1,2,2- tetrafluoro ethyoxyl) methyl] oxirane, the hydrogen bond in system is added, the increase of hydrogen bond is conducive to the raising of cloud point,
Therefore remain to keep the quality of finish while the concentration of finish is increased.
3rd, in spinning oil formation oil film, fluorine element, due to the characteristic of fluorine element, can make the flat of finish in surface enrichment
Slip is further enhanced, and reduces the damage of fiber in the process of running.Fluorine element will enter all in branched positional simultaneously
One step reduces the surface tension of finish.
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 of the invention lectured has been read, 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.
A kind of super soft hyperfine polyester fiber of the present invention, super soft hyperfine polyester fiber is mainly polyester and melted by spinneret orifice
Spinning, oil agent and high-speed winding are prepared；The finish of the oil agent at least includes fluorochemical polyether, the quality of fluorochemical polyether
The 45% of the quality of >=finish；The fluorochemical polyether is oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] epoxy
The random copolymer of ethane and expoxy propane, its structural formula is：
Wherein, m=10~20, n=20~30, k=1~3；
Fracture strength >=3.8cN/dtex of the super soft hyperfine polyester fiber, elongation at break is 35.0 ± 3.0%, single
Silk size is 0.20~0.50dtex.
Wherein, the relative molecular weight of the fluorochemical polyether is 1000~4000；The cloud point of the fluorochemical polyether is 50~100
℃；25~40dyn/cm of surface tension of the fluorochemical polyether；Also include mineral oil, phosphate kalium salt and alkyl in the finish
Sodium sulfonate；
By weight：Mineral oil is 25~35 parts；Fluorochemical polyether is 50~70 parts；Phosphate kalium salt is 8~15 parts；Alkane
Base sodium sulfonate is 2~7 parts；
Described mineral oil is one kind in 9#~17# mineral oil；Described phosphate kalium salt is dodecylphosphoric acid
One kind in ester sylvite, isomerous tridecanol polyoxyethylene ether phosphate kalium salt and ten tetracosanol phosphate kalium salts；Described alkane
Base sodium sulfonate is one kind in dodecyl sodium sulfate, pentadecyl sulfonic acid sodium and sodium cetanesulfonate；
The finish when in use, the emulsion that oil concentration is 10~20wt% is configured to water.
Line density deviation ratio≤0.5% of the super soft hyperfine polyester fiber of the present invention, fracture strength CV value≤3.0%,
Extension at break CV value≤8.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 1.00 ±
0.20%.
Embodiment 1
A kind of preparation method of super soft hyperfine polyester fiber, prepares the finish oiled first, and its specific preparation process is：
Initiator butanol and highly basic potassium hydroxide are blended, 105 DEG C are then heated to, add well mixed oxirane, [(1,
1,2,2- tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane, the amount of butanol is oxirane, [(1,1,2,2- tetrafluoro second
Epoxide) methyl] oxirane and expoxy propane gross mass 1 ‰, the amount of highly basic potassium hydroxide is oxirane, [(1,1,2,2-
Tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane gross mass 1 ‰, oxirane, [(1,1,2,2- tetrafluoro ethyoxyl)
Methyl] consumption of oxirane and expoxy propane is 10 in molar ratio:1:20, it is polymerize in the case where protective atmosphere is nitrogen atmosphere
Reaction, reaction pressure is 0.4MPa, reach relative molecular weight be 1000 after, that is, obtain fluorochemical polyether, its cloud point be 50 DEG C, its table
Face tension force 25dyn/cm；
Then, by fluorochemical polyether, phosphate kalium salt 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite and sodium alkyl sulfonate dodecyl sodium sulfonate
Sodium normal temperature is well mixed, and is then added mixture to again in mineral oil, and temperature control is 40 DEG C, stirs 1h, that is, obtains finish,
Finish when in use, the emulsion that oil concentration is 10wt% is configured to water；
By weight：
Then by polyester through measuring, extruding, cool down, oil, stretch, thermal finalization and high-speed winding, be made super soft ultra-fine poly-
Ester fiber；
The temperature of extrusion is 290 DEG C；
The wind-warm syndrome of cooling is 20 DEG C；
HT1：75℃
HT2：120℃
High-speed winding speed is 4000m/min；
The fracture strength of super soft hyperfine polyester fiber：3.8cN/dtex, elongation at break is 37.0%, and filament number is
0.50dtex；Line density deviation ratio：0.5%, fracture strength CV values：2.0%, extension at break CV values：6.0%, yarn unevenness
CV：1.00%, boiling water shrinkage 7.5%, oil content 1.00%.
The super soft hyperfine polyester fiber dyeing：
Dyeing is Disperse Red 3B with disperse dyes, and fiber is dyed in HTHP machine respectively；Fiber nonionic before dye
Surfactant is handled 30 minutes at 60 DEG C；Dye dosage is 2.0% (o.w.f)；Dispersant NNO1.2g/L, pH value is 5, bath
Than for 1:50,60 DEG C enter dye, are warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C of each constant temperature dyeing 1h.
Embodiment 2
A kind of preparation method of super soft hyperfine polyester fiber, prepares the finish oiled, it is concretely comprised the following steps first：Will starting
Agent butanol and the blending of highly basic sodium hydroxide, then heat to 125 DEG C, add well mixed oxirane, [(1,1,2,2-
Tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane, the amount of butanol is oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) first
Base] oxirane and expoxy propane gross mass 5 ‰, the amount of highly basic sodium hydroxide is oxirane, [(1,1,2,2- tetrafluoro second
Epoxide) methyl] oxirane and expoxy propane gross mass 5 ‰, oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) methyl] ring
The consumption of oxidative ethane and expoxy propane is 20 in molar ratio:3:30, in the case where protective atmosphere is inert gas atmosphere polymerize instead
Should, reaction pressure is 0.5MPa, and it is after 4000 to reach relative molecular weight, neutralized, adsorbed, vacuum dehydration, drying and filtering,
Fluorochemical polyether is obtained, its cloud point is 100 DEG C, its surface tension 32dyn/cm；
Then, by fluorochemical polyether, phosphate kalium salt isomerous tridecanol polyoxyethylene ether phosphate kalium salt and sodium alkyl sulfonate
Dodecyl sodium sulfate normal temperature is well mixed, and is then added mixture to again in mineral oil, and temperature control is 55 DEG C, stirring
3h, that is, obtain finish, and finish when in use, the emulsion that oil concentration is 20wt% is configured to water；
By weight：
Then by polyester through measuring, extruding, cool down, oil, stretch, thermal finalization and high-speed winding, be made super soft ultra-fine poly-
Ester fiber；
The temperature of extrusion is 295 DEG C；
The wind-warm syndrome of cooling is 25 DEG C；
HT1：95℃
HT2：130℃
High-speed winding speed is 5000m/min；
The fracture strength of super soft hyperfine polyester fiber：3.8cN/dtex, elongation at break is 36.0%, and filament number is
0.20dtex；Line density deviation ratio：0.5%, fracture strength CV values：3.0%, extension at break CV values：8.0%, yarn unevenness
CV：2.00%, boiling water shrinkage 7.5%, oil content 1.00%.
The super soft hyperfine polyester fiber dyeing：
Dyeing is disperse blue SE-2R with disperse dyes, and fiber is dyed in HTHP machine respectively；Dye before fiber with it is non-from
Sub- surfactant is handled 30 minutes at 60 DEG C；Dye dosage is 2.0% (o.w.f)；Dispersant NNO1.2g/L, pH value is 5,
Bath raio is 1:50,60 DEG C enter dye, are warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C of each constant temperature dyeing 1h.
Embodiment 3
A kind of preparation method of super soft hyperfine polyester fiber, prepares the finish oiled, it is concretely comprised the following steps first：Will starting
Agent butanol and the blending of highly basic sodium hydroxide, then heat to 115 DEG C, add well mixed oxirane, [(1,1,2,2-
Tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane, the amount of butanol is oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) first
Base] oxirane and expoxy propane gross mass 2 ‰, the amount of highly basic sodium hydroxide is oxirane, [(1,1,2,2- tetrafluoro second
Epoxide) methyl] oxirane and expoxy propane gross mass 1.5 ‰, oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) methyl]
The consumption of oxirane and expoxy propane is 12 in molar ratio:1:30, it is polymerize in the case where protective atmosphere is inert gas atmosphere
Reaction, reaction pressure is 0.8MPa, and it is after 3000 to reach relative molecular weight, neutralized, adsorbed, vacuum dehydration, drying and mistake
Filter, that is, obtain fluorochemical polyether, and its cloud point is 100 DEG C, its surface tension 40dyn/cm；
Then, by fluorochemical polyether, the tetracosanol phosphate kalium salt of phosphate kalium salt ten and sodium alkyl sulfonate cetyl sulphur
Sour sodium normal temperature is well mixed, and is then added mixture to again in mineral oil, and temperature control is 45 DEG C, stirs 2h, that is, obtains oil
Agent, finish when in use, the emulsion that oil concentration is 18wt% is configured to water；
By weight：
Then by polyester through measuring, extruding, cool down, oil, stretch, thermal finalization and high-speed winding, be made super soft ultra-fine poly-
Ester fiber；
The temperature of extrusion is 292 DEG C；
The wind-warm syndrome of cooling is 22 DEG C；
HT1：78℃
HT2：125℃
High-speed winding speed is 4200m/min；
The fracture strength of super soft hyperfine polyester fiber：4.2cN/dtex, elongation at break is 33.0%, and filament number is
0.30dtex；Line density deviation ratio：0.4%, fracture strength CV values：3.5%, extension at break CV values：7.0%, yarn unevenness
CV：1.00%, boiling water shrinkage 7.7%, oil content 0.90%.
The super soft hyperfine polyester fiber dyeing：
Dyeing disperse dyes are to disperse bright blue S-GL, and fiber is dyed in HTHP machine respectively；Fiber is with non-before dye
Ionic surface active agent is handled 30 minutes at 60 DEG C；Dye dosage is 2.0% (o.w.f)；Dispersant NNO1.2g/L, pH value is
5, bath raio is 1:50,60 DEG C enter dye, are warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C of each constant temperature dyeing 1h.
Embodiment 4
A kind of preparation method of super soft hyperfine polyester fiber, prepares the finish oiled, it is concretely comprised the following steps first：Will starting
Agent butanol and highly basic potassium hydroxide blending, then heat to 120 DEG C, add well mixed oxirane, [(1,1,2,2-
Tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane, the amount of butanol is oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) first
Base] oxirane and expoxy propane gross mass 4 ‰, the amount of highly basic potassium hydroxide is oxirane, [(1,1,2,2- tetrafluoro second
Epoxide) methyl] oxirane and expoxy propane gross mass 4 ‰, oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) methyl] ring
The consumption of oxidative ethane and expoxy propane is 20 in molar ratio:2:26, in the case where protective atmosphere is inert gas atmosphere polymerize instead
Should, reaction pressure is 0.8MPa, and it is after 2500 to reach relative molecular weight, neutralized, adsorbed, vacuum dehydration, drying and filtering,
Fluorochemical polyether is obtained, its cloud point is 80 DEG C, its surface tension 37dyn/cm；
Then, by fluorochemical polyether, phosphate kalium salt 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite and sodium alkyl sulfonate dodecyl sodium sulfonate
Sodium normal temperature is well mixed, and is then added mixture to again in mineral oil, and temperature control is 45 DEG C, stirs 2h, that is, obtains finish,
Finish when in use, the emulsion that oil concentration is 18wt% is configured to water；
By weight：
Then by polyester through measuring, extruding, cool down, oil, stretch, thermal finalization and high-speed winding, be made super soft ultra-fine poly-
Ester fiber；
The temperature of extrusion is 293 DEG C；
The wind-warm syndrome of cooling is 24 DEG C；
HT1：79℃
HT2：128℃
High-speed winding speed is 4700m/min；
The fracture strength of super soft hyperfine polyester fiber：4.4cN/dtex, elongation at break is 32.0%, and filament number is
0.40dtex；Line density deviation ratio：0.4%, fracture strength CV values：2.0%, extension at break CV values：7.0%, yarn unevenness
CV：1.00%, boiling water shrinkage 7.8%, oil content 1.20%.
The super soft hyperfine polyester fiber dyeing：
Dyeing is Disperse Red 3B with disperse dyes, and fiber is dyed in HTHP machine respectively；Fiber nonionic before dye
Surfactant is handled 30 minutes at 60 DEG C；Dye dosage is 2.0% (o.w.f)；Dispersant NNO1.2g/L, pH value is 5, bath
Than for 1:50,60 DEG C enter dye, are warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C of each constant temperature dyeing 1h.
Embodiment 5
A kind of preparation method of super soft hyperfine polyester fiber, prepares the finish oiled, it is concretely comprised the following steps first：Will starting
Agent butanol and highly basic potassium hydroxide blending, then heat to 125 DEG C, add well mixed oxirane, [(1,1,2,2-
Tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane, the amount of butanol is oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) first
Base] oxirane and expoxy propane gross mass 3 ‰, the amount of highly basic is oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) first
Base] oxirane and expoxy propane gross mass 3 ‰, oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) methyl] oxirane
Consumption with expoxy propane is 18 in molar ratio:2:20, carry out polymerisation, reaction pressure in the case where protective atmosphere is nitrogen atmosphere
For 0.9MPa, it is after 2500 to reach relative molecular weight, neutralized, adsorbed, vacuum dehydration, drying and filtering, that is, obtain fluorine-containing
Polyethers, its cloud point is 70 DEG C, its surface tension 29dyn/cm；
Then, by fluorochemical polyether, phosphate kalium salt isomerous tridecanol polyoxyethylene ether phosphate kalium salt and sodium alkyl sulfonate
Pentadecyl sulfonic acid sodium normal temperature is well mixed, and is then added mixture to again in mineral oil, and temperature control is 48 DEG C, stirring
1h, that is, obtain finish, and finish when in use, the emulsion that oil concentration is 15wt% is configured to water；
By weight：
Then by polyester through measuring, extruding, cool down, oil, stretch, thermal finalization and high-speed winding, be made super soft ultra-fine poly-
Ester fiber；
The temperature of extrusion is 294 DEG C；
The wind-warm syndrome of cooling is 23 DEG C；
HT1：85℃
HT2：126℃
High-speed winding speed is 4300m/min；
The fracture strength of super soft hyperfine polyester fiber：3.8cN/dtex, elongation at break is 37.0%, and filament number is
0.50dtex；Line density deviation ratio：0.5%, fracture strength CV values：3.0%, extension at break CV values：7.0%, yarn unevenness
CV：2.00%, boiling water shrinkage 7.9%, oil content 1.00%.
The super soft hyperfine polyester fiber dyeing：
Dyeing is disperse blue SE-2R with disperse dyes, and fiber is dyed in HTHP machine respectively；Dye before fiber with it is non-from
Sub- surfactant is handled 30 minutes at 60 DEG C；Dye dosage is 2.0% (o.w.f)；Dispersant NNO1.2g/L, pH value is 5,
Bath raio is 1:50,60 DEG C enter dye, are warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C of each constant temperature dyeing 1h.
Embodiment 6
A kind of preparation method of super soft hyperfine polyester fiber, prepares the finish oiled, it is concretely comprised the following steps first：Will starting
Agent butanol and the blending of highly basic sodium hydroxide, then heat to 123 DEG C, add well mixed oxirane, [(1,1,2,2-
Tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane, the amount of butanol is oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) first
Base] oxirane and expoxy propane gross mass 4 ‰, the amount of highly basic is oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) first
Base] oxirane and expoxy propane gross mass 2 ‰, oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) methyl] oxirane
Consumption with expoxy propane is 18 in molar ratio:2:26, carry out polymerisation, reaction pressure in the case where protective atmosphere is nitrogen atmosphere
For 1.0MPa, it is after 1600 to reach relative molecular weight, neutralized, adsorbed, vacuum dehydration, drying and filtering, that is, obtain fluorine-containing
Polyethers, its cloud point is 82 DEG C, its surface tension 33dyn/cm；
Then, by fluorochemical polyether, the tetracosanol phosphate kalium salt of phosphate kalium salt ten and sodium alkyl sulfonate cetyl sulphur
Sour sodium normal temperature is well mixed, and is then added mixture to again in mineral oil, and temperature control is 48 DEG C, stirs 2h, that is, obtains oil
Agent, finish when in use, the emulsion that oil concentration is 16wt% is configured to water；
By weight：
Then super soft hyperfine polyester fiber is made through measuring, extruding, cool down, oil and high-speed winding in polyester；
The temperature of extrusion is 295 DEG C；
The wind-warm syndrome of cooling is 20 DEG C；
The speed of winding is 6200m/min；
The draw ratio of spinneret orifice is 5, shear rate 3000s-1；
Spinneret back pressure 180kg/cm2。
Then by polyester through measuring, extruding, cool down, oil, stretch, thermal finalization and high-speed winding, be made super soft ultra-fine poly-
Ester fiber；
The temperature of extrusion is 294 DEG C；
The wind-warm syndrome of cooling is 23 DEG C；
HT1：82℃
HT2：128℃
High-speed winding speed is 4800m/min；
The fracture strength 4.6cN/dtex of super soft hyperfine polyester fiber, elongation at break is 32.0%, and filament number is
0.30dtex；Line density deviation ratio：0.5%, fracture strength CV values：3.0%, extension at break CV value 7.0%, yarn unevenness
CV：.00%, boiling water shrinkage 7.4%, oil content 1.00%.
The super soft hyperfine polyester fiber dyeing：
Dyeing disperse dyes are to disperse bright blue S-GL, and fiber is dyed in HTHP machine respectively；Fiber is with non-before dye
Ionic surface active agent is handled 30 minutes at 60 DEG C；Dye dosage is 2.0% (o.w.f)；Dispersant NNO1.2g/L, pH value is
5, bath raio is 1:50,60 DEG C enter dye, are warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C of each constant temperature dyeing 1h.
Claims (9)
1. a kind of super soft hyperfine polyester fiber, it is characterized in that：The super soft hyperfine polyester fiber is mainly polyester and passes through spinneret orifice
Melt spinning, oil agent and high-speed winding are prepared；The finish of the oil agent at least includes fluorochemical polyether, fluorochemical polyether
The 45% of the quality of quality >=finish；The fluorochemical polyether is oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl]
The random copolymer of oxirane and expoxy propane, its structural formula is：
Wherein, m=10~20, n=20~30, k=1~3；
The cloud point of the fluorochemical polyether is 50~100 DEG C；Surface tension 25~40dyn/cm of the fluorochemical polyether, it is described fluorine-containing
The relative molecular weight of polyethers is 1000~4000；
Fracture strength >=3.8cN/dtex of the super soft hyperfine polyester fiber, fracture strength CV value≤3.0%, elongation at break
For 35.0 ± 3.0%, extension at break CV value≤8.0%, oil content 1.00 ± 0.20%, filament number is 0.20~
0.50dtex。
2. the super soft hyperfine polyester fiber of one kind according to claim 1, it is characterised in that also include mineral in the finish
Oil, phosphate kalium salt and sodium alkyl sulfonate；
By weight：Mineral oil is 25~35 parts；Fluorochemical polyether is 50~70 parts；Phosphate kalium salt is 8~15 parts；Alkyl sulphur
Sour sodium is 2~7 parts；
Described mineral oil is one kind in 9#~17# mineral oil；Described phosphate kalium salt is 1-isobutyl-3,5-dimethylhexylphosphoric acid potassium
One kind in salt and isomerous tridecanol polyoxyethylene ether phosphate kalium salt；Described sodium alkyl sulfonate be dodecyl sodium sulfate,
One kind in pentadecyl sulfonic acid sodium and sodium cetanesulfonate；
The finish when in use, the emulsion that oil concentration is 10~20wt% is configured to water.
3. the super soft hyperfine polyester fiber of one kind according to claim 1, it is characterised in that the super soft hyperfine polyester fiber
Line density deviation ratio≤0.5%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%.
4. a kind of such as preparation method of super soft hyperfine polyester fiber according to any one of claims 1 to 3, it is characterized in that：Will
Polyester is through measuring, extruding, cool down, oil, stretch, thermal finalization and high-speed winding, and super soft hyperfine polyester fiber is made；
The temperature of the extrusion is 290~295 DEG C；
The wind-warm syndrome of the cooling is 20~25 DEG C；
HT1：75~95 DEG C；
HT2：120~130 DEG C；
The high-speed winding speed is 4000~5000m/min；
The finish preparation method oiled：
Butanol and highly basic are blended, 105~125 DEG C is then heated to, adds well mixed oxirane, [(1,1,2,2-
Tetrafluoro ethyoxyl) methyl] oxirane and expoxy propane, polymerisation is carried out under protective atmosphere, reaction pressure is less than
0.4MPa, reaches and fluorochemical polyether is obtained after predetermined molecular weight；
Then, fluorochemical polyether, phosphate kalium salt and sodium alkyl sulfonate normal temperature are well mixed, ore deposit is then added mixture to again
In thing oil, temperature control is 40~55 DEG C, stirs 1~3h, that is, obtains the finish；
By weight：
The finish when in use, the emulsion that oil concentration is 10~20wt% is configured to water.
5. the preparation method of a kind of super soft hyperfine polyester fiber according to claim 4, it is characterised in that the butanol
Measure as the 1-5 ‰ of oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and expoxy propane gross mass；It is described strong
Alkali is potassium hydroxide or sodium hydroxide；The amount of the highly basic is oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] epoxy
Ethane and the 1-5 of expoxy propane gross mass ‰.
6. a kind of preparation method of super soft hyperfine polyester fiber according to claim 4, it is characterised in that the epoxy second
The consumption of alkane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and expoxy propane is 10~20 in molar ratio:1~3:20
~30.
7. a kind of preparation method of super soft hyperfine polyester fiber according to claim 4, it is characterised in that the protection gas
Atmosphere is nitrogen atmosphere or inert gas atmosphere；The predetermined molecular weight refers to that the relative molecular weight of product is 1000~4000.
8. a kind of preparation method of super soft hyperfine polyester fiber according to claim 4, it is characterised in that it is described reach it is pre-
Determine the product after molecular weight also neutralized, adsorbed, vacuum dehydration, drying and filtering.
9. the preparation method of a kind of super soft hyperfine polyester fiber according to claim 4, it is characterised in that described super soft super
Carefully the dyeing of polyester fiber is：
Dyeing is Disperse Red 3B, disperse blue SE-2R with disperse dyes or disperses bright blue S-GL, and fiber is respectively in HTHP machine
Dyeing；Fiber nonionic surfactant is handled 30 minutes at 60 DEG C before dye；Dye dosage is 2.0%o.w.f；Dispersant
NNO1.2g/L, pH value is 5, and bath raio is 1:50,60 DEG C enter dye, are warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C of each constant temperature dyeings
1h。
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| CN105506775B (en) * | 2015-12-29 | 2018-05-18 | 江苏恒力化纤股份有限公司 | A kind of super soft ultrafine wire of low aberration polyester and preparation method thereof |
| CN105926061A (en) * | 2016-06-29 | 2016-09-07 | 浙江尤夫高新纤维股份有限公司 | Production method for polyester industrial filaments capable of improving cohesion property of stiff cord |
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| CN107893264B (en) * | 2017-12-14 | 2020-10-16 | 江苏恒力化纤股份有限公司 | Preparation method of high-uniformity military soft polyester industrial yarn |
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