CN105002603B - A kind of super fine denier polyester fiber and preparation method thereof - Google Patents
A kind of super fine denier polyester fiber and preparation method thereof Download PDFInfo
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- CN105002603B CN105002603B CN201510465908.4A CN201510465908A CN105002603B CN 105002603 B CN105002603 B CN 105002603B CN 201510465908 A CN201510465908 A CN 201510465908A CN 105002603 B CN105002603 B CN 105002603B
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Abstract
The present invention relates to a kind of super fine denier polyester fiber and preparation method thereof, a kind of super fine denier polyester fiber, the super fine denier polyester fiber is mainly that polyester is prepared by spinneret orifice melt spinning, oil agent and high-speed winding；The finish of the oil agent comprises at least fluorochemical polyether, and 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 a kind of super fine denier polyester fiber 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 have 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 that stiffness is good, so, polyester fiber is widely used in the fields such as clothes, home textile.
With the continuous improvement of people's living standards, people propose to the comfortableness of clothing, feature, variation and grade
Higher require, polyester drawn yarns general fibre total linear density is typically in 30-150D or so at present, spatter property, drapability,
In terms of comfortableness, ordinary polyester fiber can not meet the requirement of high-grade fabric production.Fused mass directly spinning 10D (total linear densities
For 11dtex) serial ultra-fine denier polyester filament yarn has soft soft, high-flexibility, gloss, high water absorption oil absorption, high density
The good characteristics such as high-specific surface area, high heat preservation performance, and with weaving, the development of printing technology, its more potential characteristic
Also increasingly excavated.Its fabric has a soft fine and smooth feel, comfortable ventilating, is easy to the texture of nursing and outward appearance preferably etc.
Superiority.
But by production equipment and technology restriction, the line density of fiber is minimum to be accomplished domestic super fine denier product at present
15D or so, and product quality is generally unstable, drafting silk product total linear density can not further fine-denierization and industrialization production,
Fabric is strongly limit to more frivolous, soft, highly dense direction to develop.
Super fine denier polyester fiber is produced, because the total linear density of fiber is too low, is highly prone to damage in spinning, drawing process
Wound, while finish is difficult to attachment on the surface of strand uniformly, the coherent of tow is poor, and lousiness is also easy to produce in production process and is broken
Head.The oil product that selected area update strategy diffusivity is good, wetability is good, the overall super fine denier polyester fiber that improves oils uniformity, to ensureing to produce
The quality of product will play larger effect.
The content of the invention
It is an object of the invention to provide a kind of super fine denier polyester fiber and preparation method thereof, and the present invention is by using high-quality
Polyester fondant, special spinneret orifice design and the use of fluorine-containing finish and high speed spinning prepare super soft superfine fibre polyester
Fiber.The finish of the present invention is made up of mineral oil, fluorochemical polyether, phosphate kalium salt and sodium alkyl sulfonate, the use of the finish
Concentration is 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 advantageous to cloud point
Improve, because remaining to keep the quality of finish while the concentration of finish is being increased a bit.The increase of finish concentration can
To greatly reduce the consumption of energy in finish drying process, energy is saved.
A kind of super fine denier polyester fiber, mainly polyester are prepared by spinneret orifice melt spinning, oil agent and high-speed winding
And obtain；The finish of the oil agent comprises at least fluorochemical polyether, and the 45% of the quality of quality >=finish of fluorochemical polyether；Institute
State the random copolymerization that fluorochemical polyether is oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and expoxy propane
Thing, its structural formula are：
Wherein, m=10~20, n=20~30, k=1~3；
Fracture strength >=3.8cN/dtex of the superfine fibre polyester fiber, elongation at break are 30.0 ± 3.0%, always
Line density is 11dtex, and filament number is 0.40~1.50dtex.
11dtex super fine denier PFYs, it is good with frivolous, dyeability while with stronger flexibility, its fabric
With the softness as silk, can be used for doing the high-end textile products such as high-grade highly dense Polyester Taffeta.But due to the total linear density of fiber
It is too low, it is highly prone to damage in spinning, drawing process, the oil product that selected area update strategy diffusivity is good, wetability is good, overall raising is ultra-fine
Denier polyester fiber oils uniformity, to ensureing that the quality of product will play larger effect.
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 advantageous to the raising that finish uses high concentration, saves energy.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 forms, and compared with EO, there is a side base on PO chain links, and steric hindrance is larger.EO/PO is than increase, i.e. PO chain links
Reduce, pending methyl group quantity declines, and intermolecular space steric hindrance is reduced, and 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 raises, 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
Hydrogen bond number will increase more, can further improve the cloud point of polyether aqueous solution；Fluorine element will enter one all in branched positional simultaneously
Step reduces the surface tension of polyethers.When finish forms oil film, fluorine element, due to the characteristic of fluorine element, can make in surface enrichment
The flatness of finish is further enhanced.
As preferable technical scheme：
A kind of super fine denier polyester fiber as described above, the relative molecular weight of the fluorochemical polyether is 1000~4000；Institute
The cloud point for stating fluorochemical polyether is 50~100 DEG C；25~40dyn/cm of surface tension of the fluorochemical polyether.
A kind of super fine denier polyester fiber as described above, also include mineral oil, phosphate kalium salt and alkyl in the finish
Sodium sulfonate；Mineral oil has good heat resistance, has good compatibility with other components, and it, which has, oils uniformly, and oil film is strong
Spend the characteristics of high, moreover it is possible to the effective coefficient of friction for reducing fiber and metal, increase the cohesive force of fiber, be advantageous to boundling.Adopt
With anionic antistatic agent, surface hydrophilic can be realized, the heat resistance of phosphate kalium salt is relatively good, and good is antistatic
Property, it is capable of the antistatic effect of reinforcing fiber, is advantageous 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 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 is configured to the emulsion that oil concentration is 10~20wt% when in use, with 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.
A kind of super fine denier polyester fiber as described above, the line density deviation ratio of the super fine denier polyester fiber≤
1.0%, fracture strength CV value≤5.0%, extension at break CV value≤10.0%, yarn unevenness CV≤1.50%, boiling shrinkage
Rate 7.5 ± 0.5%, oil content 1.00 ± 0.10%.
Present invention also offers a kind of preparation method of super fine denier polyester fiber, by polyester through measuring, extruding, cooling down, on
Oil, stretching, thermal finalization and high-speed winding, are made super fine denier polyester fiber；
The temperature of the extrusion is 290~295 DEG C；
The wind-warm syndrome of the cooling is 20~25 DEG C；
HT1：75~85 DEG C；
HT2：120~128 DEG C；
The high-speed winding speed is 4000~5000m/min；
The finish preparation method to oil：
Initiator and highly basic are blended, then heat to 105~125 DEG C, 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, fluorochemical polyether is obtained after reaching 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 is configured to the emulsion that oil concentration is 10~20wt% when in use, with water.
A kind of super fine denier polyester fiber as described above, the initiator be butanol, the amount of the butanol be oxirane,
The 1-5 ‰ of [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and expoxy propane gross mass；The highly basic is potassium hydroxide
Or sodium hydroxide；The amount of the highly basic is oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and epoxy third
The 1-5 ‰ of alkane gross mass.
A kind of super fine denier polyester fiber as described above, the oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) methyl]
The dosage of oxirane and expoxy propane is 10~20 in molar ratio:1~3:20~30.
A kind of super fine denier polyester fiber as described above, the protective atmosphere is nitrogen atmosphere or inert gas atmosphere；Institute
State predetermined molecular weight and refer to that the relative molecular weight of product is 1000~4000.
A kind of super fine denier polyester fiber as described above, the product reached after predetermined molecular weight are also neutralized, inhaled
Attached, vacuum dehydration, drying and filtering.
A kind of super fine denier polyester fiber as described above, the dyeing of the super fine denier polyester fiber are：
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 5, bath raio 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 fine denier polyester fiber of the present invention, 10D series ultra-fine denier polyester filament yarns have soft, high flexible
Property, the good characteristic such as gloss is soft, high water absorption oil absorption, high density high-specific surface area, high heat preservation performance, and with weaving,
The development of printing technology, its more potential characteristic are also increasingly excavated.Beneficial effect：
1st, super fine denier polyester fiber, its fabric have a soft fine and smooth feel, comfortable ventilating, are easy to the matter of nursing and outward appearance
Feel the superiority such as preferable.
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 advantageous to the raising of cloud point,
Therefore remain to keep the quality of finish while the concentration of finish is increased.
3rd, when spinning oil forms 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 fine denier polyester fiber of the present invention, mainly polyester pass through spinneret orifice melt spinning, oil agent and high speed
Winding is prepared；The finish of the oil agent comprises at least fluorochemical polyether, the quality of quality >=finish of fluorochemical polyether
45%；The fluorochemical polyether is oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and expoxy propane
Random copolymer, its structural formula are：
Wherein, m=10~20, n=20~30, k=1~3；
Fracture strength >=3.8cN/dtex of the super fine denier polyester fiber, elongation at break are 30.0 ± 3.0%, bus
Density is 11dtex, and filament number is 0.40~1.50dtex.
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 is configured to the emulsion that oil concentration is 10~20wt% when in use, with water.
Line density deviation ratio≤1.0% of super fine denier polyester fiber of the present invention, fracture strength CV value≤5.0%, fracture
Elongation CV value≤10.0%, yarn unevenness CV≤1.50%, boiling water shrinkage 7.5 ± 0.5%, oil content 1.00 ±
0.10%.
Embodiment 1
A kind of preparation method of super fine denier polyester fiber, prepares the finish to oil first, and its specific preparation process is：Will
Initiator butanol and highly basic potassium hydroxide blending, then heat to 105 DEG C, add well mixed oxirane, [(1,1,
2,2- tetrafluoro ethyoxyls) methyl] oxirane and expoxy propane, the amount of butanol is oxirane, [(1,1,2,2- tetrafluoro ethoxy
Base) methyl] oxirane and expoxy propane gross mass 1 ‰, the amount of highly basic potassium hydroxide is oxirane, [(1,1,2,2- tetra-
Fluorine ethyoxyl) methyl] oxirane and expoxy propane gross mass 1 ‰, oxirane, [(1,1,2,2- tetrafluoro ethyoxyl) first
Base] dosage of oxirane and expoxy propane is 10 in molar ratio:1:20, in the case where protective atmosphere is nitrogen atmosphere polymerize instead
Should, reaction pressure 0.4MPa, reach relative molecular weight after 1000, that is, to obtain fluorochemical polyether, its cloud point is 50 DEG C, its surface
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 is configured to the emulsion that oil concentration is 10wt% when in use, with water；
By weight：
Then by polyester through measuring, extruding, cooling down, oiling, stretching, thermal finalization and high-speed winding, super fine denier polyester is made
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 index of the super fine denier polyester fiber：The fracture strength of super fine denier polyester fiber：3.8cN/dtex, elongation at break
For 30.0%, total linear density 11dtex, filament number 0.40dtex；Line density deviation ratio：1.0%, fracture strength CV values：
5.0%, extension at break CV values：10.0%, yarn unevenness CV：1.50%, boiling water shrinkage：7.5%, oil content 1.00%.
The super fine denier dyeing polyester fibers technique：
Dyeing is Disperse Red 3B with disperse dyes, and fiber dyes 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 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 fine denier polyester fiber, prepares the finish to oil, it is concretely comprised the following steps first：By initiator
Butanol and the blending of highly basic sodium hydroxide, then heat to 125 DEG C, add well mixed oxirane, [(1,1,2,2- tetra-
Fluorine 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 dosage 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 0.5MPa, reach relative molecular weight after 4000, to be neutralized, being 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 is configured to the emulsion that oil concentration is 20wt% when in use, with water；
By weight：
Then by polyester through measuring, extruding, cooling down, oiling, stretching, thermal finalization and high-speed winding, super fine denier polyester is made
Fiber；
The temperature of extrusion is 295 DEG C；
The wind-warm syndrome of cooling is 25 DEG C；
HT1：85℃
HT2：128℃
High-speed winding speed is 5000m/min.
The index of the super fine denier polyester fiber：The fracture strength of super fine denier polyester fiber：4.2cN/dtex, elongation at break
For 28.0%, total linear density 11dtex, filament number 0.8dtex；Line density deviation ratio：1.0%, fracture strength CV values：
4.0%, extension at break CV values：8.0%, yarn unevenness CV：1.00%, boiling water shrinkage 7.8%, oil content 1.00%.
The super fine denier dyeing polyester fibers technique：
Dyeing is disperse blue SE-2R with disperse dyes, and fiber dyes in HTHP machine respectively；Before dye 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 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 fine denier polyester fiber, prepares the finish to oil, it is concretely comprised the following steps first：By initiator
Butanol and the blending of highly basic sodium hydroxide, then heat to 115 DEG C, add well mixed oxirane, [(1,1,2,2- tetra-
Fluorine 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 dosage 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 0.8MPa, reach relative molecular weight after 3000, to be neutralized, being 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 are configured to the emulsion that oil concentration is 18wt% when in use, with water；
By weight：
Then by polyester through measuring, extruding, cooling down, oiling, stretching, thermal finalization and high-speed winding, super fine denier polyester is made
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 4500m/min.
The index of the super fine denier polyester fiber：The fracture strength of super fine denier polyester fiber:4.0cN/dtex, elongation at break
For 33.0%, total linear density 11dtex, filament number 1.00dtex；Line density deviation ratio：1.0%, fracture strength CV values
≤ 5.0%, extension at break CV values：8.0%, yarn unevenness CV；1.00%, boiling water shrinkage 7.0%, oil content 1.00%.
The super fine denier dyeing polyester fibers technique：
Dyeing disperse dyes are to disperse bright blue S-GL, and fiber dyes 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 are
5, bath raio 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 fine denier polyester fiber, prepares the finish to oil, it is concretely comprised the following steps first：By initiator
Butanol and highly basic potassium hydroxide blending, then heat to 120 DEG C, add well mixed oxirane, [(1,1,2,2- tetra-
Fluorine 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 dosage 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 0.8MPa, reach relative molecular weight after 2500, to be neutralized, being 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 is configured to the emulsion that oil concentration is 18wt% when in use, with water；
By weight：
Then by polyester through measuring, extruding, cooling down, oiling, stretching, thermal finalization and high-speed winding, super fine denier polyester is made
Fiber；
The temperature of extrusion is 293 DEG C；
The wind-warm syndrome of cooling is 22 DEG C；
HT1：78℃
HT2：125℃
High-speed winding speed is 4500m/min.
The index of the super fine denier polyester fiber：The fracture strength of super fine denier polyester fiber:3.9cN/dtex, elongation at break
For 33.0%, total linear density 11dtex, filament number 1.50dtex；Line density deviation ratio：1.0%, fracture strength CV values：
4.0%, extension at break CV value 9.0%, yarn unevenness CV：1.50%, boiling water shrinkage 7.5%, oil content 1.00%.
The super fine denier dyeing polyester fibers technique：
Dyeing is Disperse Red 3B with disperse dyes, and fiber dyes 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 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 fine denier polyester fiber, prepares the finish to oil, it is concretely comprised the following steps first：By initiator
Butanol and highly basic potassium hydroxide blending, then heat to 125 DEG C, add well mixed oxirane, [(1,1,2,2- tetra-
Fluorine 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
Dosage 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, reach relative molecular weight after 2500, to be neutralized, being adsorbed, vacuum dehydration, drying and filtering, that is, obtain fluorine-containing
Polyethers, its cloud point are 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 is configured to the emulsion that oil concentration is 15wt% when in use, with water；
By weight：
Then by polyester through measuring, extruding, cooling down, oiling, stretching, thermal finalization and high-speed winding, super fine denier polyester is made
Fiber；
The temperature of extrusion is 294 DEG C；
The wind-warm syndrome of cooling is 23 DEG C；
HT1：77℃
HT2：125℃
High-speed winding speed is 4500m/min.
The index of the super fine denier polyester fiber：The fracture strength of super fine denier polyester fiber:4.6cN/dtex, elongation at break
For 27.0%, total linear density 11dtex, filament number 1.00dtex；Line density deviation ratio：1.0%, fracture strength CV values：
4.0%, extension at break CV values：7.0%, yarn unevenness CV：1.50%, boiling water shrinkage 7.0%, oil content 1.00%.
The super fine denier dyeing polyester fibers technique：
Dyeing is disperse blue SE-2R with disperse dyes, and fiber dyes in HTHP machine respectively；Before dye 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 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 fine denier polyester fiber, prepares the finish to oil, it is concretely comprised the following steps first：By initiator
Butanol and the blending of highly basic sodium hydroxide, then heat to 123 DEG C, add well mixed oxirane, [(1,1,2,2- tetra-
Fluorine 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
Dosage 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, reach relative molecular weight after 1600, to be neutralized, being adsorbed, vacuum dehydration, drying and filtering, that is, obtain fluorine-containing
Polyethers, its cloud point are 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 are configured to the emulsion that oil concentration is 16wt% when in use, with water；
By weight：
Then by polyester through measuring, extruding, cooling down, oiling, stretching, thermal finalization and high-speed winding, super fine denier polyester is made
Fiber；
The temperature of extrusion is 293 DEG C；
The wind-warm syndrome of cooling is 23 DEG C；
HT1：78℃
HT2：126℃
High-speed winding speed is 4200m/min.
The index of the super fine denier polyester fiber：The fracture strength of super fine denier polyester fiber:3.8cN/dtex, elongation at break
For 30.0%, total linear density 11dtex, filament number 0.50dtex；Line density deviation ratio：1.0%, fracture strength CV values：
5.0%, extension at break CV values：8.0%, yarn unevenness CV：1.00%, boiling water shrinkage 7.0%, oil content 0.90%.
The super fine denier dyeing polyester fibers technique：
Dyeing disperse dyes are to disperse bright blue S-GL, and fiber dyes 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 are
5, bath raio 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 fine denier polyester fiber, it is characterized in that：The super fine denier polyester fiber is mainly that polyester is melted by spinneret orifice
Spinning, oil agent and high-speed winding are prepared；The finish of the oil agent comprises at least 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 are：
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 fine denier polyester fiber, elongation at break are 30.0 ± 3.0%, total linear density
For 11dtex, filament number is 0.40~1.50dtex.
2. a kind of super fine denier polyester fiber 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 is configured to the emulsion that oil concentration is 10~20wt% when in use, with water.
3. a kind of super fine denier polyester fiber according to claim 1, it is characterised in that the super fine denier polyester fiber
Line density deviation ratio≤1.0%, fracture strength CV value≤5.0%, extension at break CV value≤10.0%, yarn unevenness CV≤
1.50%, boiling water shrinkage 7.5 ± 0.5%, oil content 1.00 ± 0.10%.
4. a kind of such as preparation method of super fine denier polyester fiber according to any one of claims 1 to 3, it is characterized in that：Will be poly-
Ester is through measuring, extruding, cooling down, oiling, stretching, thermal finalization and high-speed winding, and super fine denier 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；
HT1：75~85 DEG C；
HT2：120~128 DEG C；
The high-speed winding speed is 4000~5000m/min；
The finish preparation method to oil：
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, fluorochemical polyether is obtained after reaching predetermined molecular weight；
Then, fluorochemical polyether, phosphate kalium salt and sodium alkyl sulfonate normal temperature are well mixed, then add mixture to ore deposit again
In thing oil, temperature control is 40-55 DEG C, stirs 1~3h, that is, obtains the finish；
By weight：
The finish is configured to the emulsion that oil concentration is 10~20wt% when in use, with water.
A kind of 5. preparation method of super fine denier polyester fiber according to claim 4, it is characterised in that the amount of the butanol
For the 1-5 ‰ of oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and expoxy propane gross mass；The highly basic
For potassium hydroxide or sodium hydroxide；The amount of the highly basic is oxirane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] epoxy second
1~the 5 ‰ of alkane and expoxy propane gross mass.
A kind of 6. preparation method of super fine denier polyester fiber according to claim 4, it is characterised in that the epoxy second
The dosage of alkane, [(1,1,2,2- tetrafluoros ethyoxyl) methyl] oxirane and expoxy propane is 10~20 in molar ratio:1~3:20
~30.
A kind of 7. preparation method of super fine denier polyester fiber according to claim 4, it is characterised in that the protective atmosphere
For nitrogen atmosphere or inert gas atmosphere；The predetermined molecular weight refers to that the relative molecular weight of product is 1000~4000.
8. the preparation method of a kind of super fine denier polyester fiber according to claim 4, it is characterised in that described to reach predetermined
Product after molecular weight is also neutralized, adsorbed, vacuum dehydration, drying and filtering.
9. the preparation method of a kind of super fine denier polyester fiber according to claim 4, it is characterised in that the super fine denier is gathered
The dyeing of ester 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 5, bath raio 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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