CN108048940A - Soft type polyester fiber and preparation method thereof - Google Patents
Soft type polyester fiber and preparation method thereof Download PDFInfo
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- CN108048940A CN108048940A CN201711341960.4A CN201711341960A CN108048940A CN 108048940 A CN108048940 A CN 108048940A CN 201711341960 A CN201711341960 A CN 201711341960A CN 108048940 A CN108048940 A CN 108048940A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
- D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- 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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- Medicinal Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to a kind of soft type polyester fibers and preparation method thereof, and preparation method is：By modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, thermal finalization and winding soft type polyester fiber is made, crown ether is contained in the finish to oil, and the content of crown ether is 67.30~85.58wt%.The material of soft type polyester fiber obtained includes the modified poly ester of terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment for strand, initial modulus≤80cN/dtex, fiber number is 75~300dtex, fracture strength >=3.6cN/dtex, elongation at break is 45.0 ± 3.0%, fracture strength CV value≤5.0%, extension at break CV value≤10.0%, boiling water shrinkage is 7.5 ± 0.5%, and oil content is 0.90 ± 0.20%.Preparation method of the present invention is simple, and the polyester fiber of acquisition has preferable softness, and application prospect is very considerable.
Description
Technical field
The invention belongs to fiber preparation fields, are related to a kind of flexibility polyester fiber and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) is a kind of polymer of function admirable, and PET is high, strong with modulus because of it
The advantages that degree is high, conformality is good and barrier property is good is widely used in the fields such as fiber, bottle packaging, film and sheet material, yield
Cumulative year after year, position in industry are obviously improved.
It, must in spinning process since the dielectric constant of most of PET fiber is smaller, regain is relatively low and coefficient of friction is higher
Spinning oil must be used.The main component of finish is surfactant, can form oriented attachment layer on chemical fibre surface, i.e., oily
Film, on the one hand, the hydrophilic radical of oil film can adsorb the moisture in air, form continuous water on the fiber surface towards space
Film makes charged ion that migration occur on it, reduces between fiber because of the accumulation of electrostatic charge caused by friction, so as to reduce
The sheet resistance of fiber adds the electric conductivity of fiber, and on the other hand, oil film isolation fiber again can generate fiber certain
Affinity makes it be not at random there are certain convergence, and in addition, oil film also imparts certain smooth of fiber
Property, fiber is made not to be damaged in friction process, and with good feel, can be passed through in spinning winding, stretching,
The operational sequences such as dry, eliminate the electrostatic interaction during textile process, will not occur bad around apron, roller, cylinder etc.
Phenomenon reduces the generation of lousiness and broken end, ensures the quality of fiber product.
After being ruptured due to the oil film of fiber surface under high temperature, high speed and certain pressure, the friction behavior of fiber can be changed,
Frictional force is caused to increase, fiber is caused the other problems such as lousiness, broken end occur, film strength is higher, is more not easily broken, more favourable
In the spinnability of fiber, when finish equably adsorbs on the fiber surface, surface forms the oil film of distribution uniform, and oil film exists
Fiber is rapid after being stretched and uniformly extends, if the viscosity of finish is excessively high, is unfavorable for the scattered of finish, forms uniform oil
Film.And with the development of the high speed of polyester filament, ultrahigh speed and Mobyneb fiber, develop that a kind of heat resistance is good, viscosity
The great realistic meaning of finish low, that film strength is high, Lubricity is good and antistatic property is strong.
The flexibility of fabric, which is people, is stroking, is grabbing a kind of subjective feeling when pinching fabric, and flexibility is one for fiber
Critically important performance, the good fibre fineness of flexibility it is thin and uniformly, intensity is big and high resilience, soft texture, feel slide it is glutinous
Exquisiteness, and the fabric being spun into has characteristic soft and that dress is graceful.And the finish used in the prior art is difficult to
Meet the condition needed for production fine count fiber, obtained fiber quality is not high, and flexibility is often nor very good.
Therefore, how to overcome the shortcomings of the prior art, it is good and there is flexibility simultaneously to prepare a kind of mechanical property
Polyester fiber becomes a technical problem to be solved urgently.
The content of the invention
The purpose of the invention is to overcome the problems, such as that polyester fiber flexibility of the prior art is poor, one kind is provided
Soft type polyester fiber with preferable flexibility and preparation method thereof.The use of present invention finish containing crown ether, improves finish
Heat resistance and lubricity, improve the quality of fiber；The use of adipic acid of the present invention improves the flexibility of fiber.
In order to achieve the above object, the technical solution adopted by the present invention is：
Soft type polyester fiber, the material of soft type polyester fiber is modified poly ester；
The strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment, adipic acid segment
It is longer aliphatic chain, the polyester that can make rigidly declines, so as to be effectively improved the flexibility of fiber；
Initial modulus≤80cN/dtex of soft type polyester fiber.
As preferred technical solution：
Soft type polyester fiber as described above, the fiber number of the soft type polyester fiber is 75~300dtex, and fracture is strong
Degree >=3.6cN/dtex, elongation at break are 45.0 ± 3.0%, fracture strength CV value≤5.0%, extension at break CV values≤
10.0%, boiling water shrinkage is 7.5 ± 0.5%, and oil content is 0.90 ± 0.20%.
Soft type polyester fiber as described above, the number-average molecular weight 20000~27000 of the modified poly ester, molecular weight
Profile exponent is 1.8~2.2, and the molecular weight of modified poly ester produced by the present invention is higher, and molecular weight distribution is relatively narrow, disclosure satisfy that
The demand of spinning processing, and be conducive to the excellent fiber of processability；
The molar content of adipic acid segment is the 5~8% of terephthalic acid (TPA) segment molar content in the modified poly ester, this
The molar content of adipic acid segment is relatively low in the modified poly ester of invention, is conducive to keep the excellent performance of polyester itself, and then makes
It obtains crystallinity to decline, initial modulus is less than normal polyester.
Soft type polyester fiber as described above, the preparation method of the modified poly ester are：By terephthalic acid (TPA), ethylene glycol
Successively esterification is carried out with adipic acid after mixing and polycondensation reaction obtains modified poly ester；It is as follows：
(1) esterification；
Terephthalic acid (TPA), ethylene glycol and adipic acid are made into slurry, catalyst, delustering agent and stabilizer is added in and is uniformly mixed
Afterwards, pressurization carries out esterification in nitrogen atmosphere, and moulding pressure is normal pressure~0.3MPa, the temperature of esterification for 250~
260 DEG C, be esterification terminal when the water quantity of distillate in esterification reaches more than the 90% of theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, the staged pressure 30~
Steadily is evacuated to by normal pressure below absolute pressure 500Pa in 50min, reaction temperature is 260~270 DEG C, the reaction time for 30~
50min then proceedes to vacuumize, and carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure
Below 100Pa, reaction temperature are 275~285 DEG C, and the reaction time is 50~90min, and modified poly ester is made.
Soft type polyester fiber as described above, in step (1), the molar ratio of terephthalic acid (TPA), ethylene glycol and adipic acid
For 1:1.2~2.0:0.03~0.06, the addition of the catalyst is the 0.01~0.05% of terephthalic acid (TPA) weight, described
The addition of delustering agent is the 0.20~0.25% of terephthalic acid (TPA) weight, and the addition of the stabilizer is terephthalic acid (TPA) weight
The 0.01~0.05% of amount；
The catalyst be antimony oxide, antimony glycol or antimony acetate, the delustering agent be titanium dioxide, the stabilization
Agent is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite.
The present invention also provides a kind of method for preparing soft type polyester fiber as described above, by the modified poly ester through meter
It measures, squeeze out, cooling down, oiling, stretching, soft type polyester fiber is made in thermal finalization and winding；
Contain crown ether in the finish to oil, and the content of crown ether is 67.30~85.58wt%.
Crown ether is a kind of heterocyclic organic compounds, includes multiple ether groups, the wettability of crown ether-like surfactant
Bigger than corresponding open chain compound, crown ether has preferable solubilising, and solubility of the salt compounds in organic compound is relatively low,
But the addition of crown ether can be improved solubility of the salt compounds in organic matter.Conventional polyester class or polyethers in finish
Class compound, since molecular weight is larger and the effect of hydrogen bond, intermolecular effect is larger, and it is larger to show as kinematic viscosity, adds in
After crown ether, crown ether can be preferably compatible in polyesters or the finish system of polyether compound, into polyesters or polyethers
Between the strand of compound, the active force between strand is shielded, is reduced so as to cause the viscosity of finish system, while chemical fibre
The antistatic agent of finish is broadly divided into anionic, cationic and amphoteric surfactant, mostly containing metal ion or
Person exists in a salt form, this all makes antistatic agent and polyesters in finish or the phase tolerance of polyether compound, and crown ether adds
Enter, due to salting in effect, improve antistatic agent and polyesters or the compatibility of polyether compound, and then improve finish oil
Film strength, this has larger meaning to the stability and the product amount of holding of spinning.The index of finish is the body of a composite factor
It is existing, thus certain restriction is proposed to the addition of crown ether, the too low heat resistance and film strength to finish of addition it is excellent
Gesture embodies not enough, other excessive indexs can be restricted.
As preferred technical solution：
Method as described above, thermal weight loss is less than 15wt% after the finish heats 2h at 200 DEG C, and crown ether has more
High volatilization point and excellent heat-resistant stability, the heat resistance of the finish introduced after crown ether are also obviously improved；
For the finish at (50 ± 0.01) DEG C, kinematic viscosity is 27.5~30.1mm2/ s, the finish are configured to water
Kinematic viscosity after the lotion that concentration is 10wt% is 0.93~0.95mm2/ s, the viscosity that crown ether can reduce finish are mainly
Since crown ether oneself viscosity is relatively low and is pearl small molecule, after introducing crown ether in finish system, crown ether can be preferably compatible to
In polyesters compound or polyether compound finish system, while enter polyesters compound or polyether compound strand
Between, the active force between strand is shielded, so as to reduce the viscosity of finish system；
The film strength of the finish is 121~127N, and the film strength of finish is relatively low in the prior art, generally in 110N
Left and right, the antistatic agent this is mainly due to preparation medium mostly exist containing metal ion or in a salt form, cause to resist
Electrostatic agent can improve film strength and be mainly with polyesters compound or the poor compatibility of polyether compound in finish, crown ether
Salting in effect can be generated after being added in due to crown ether, improves antistatic agent and polyesters compound or the compatibility of polyethers,
And then improve finish oil film strength；
The surface tension of the finish is 23.2~26.8cN/cm, and specific resistance is 1.0 × 108~1.8 × 108Ω·cm；
After oiling, confficient of static friction between fiber and fiber is 0.250~0.263, the coefficient of kinetic friction for 0.262~
0.273；
After oiling, confficient of static friction between fiber and metal is 0.202~0.210, the coefficient of kinetic friction for 0.320~
0.332。
Method as described above, the crown ether are 2- methylols -12-crown-4,15- crown ethers -5 or 2- methylol -15- crown-s
5；
Also contain mineral oil, phosphate kalium salt, trimethylolpropane laurate and sodium alkyl sulfonate in the finish；
The mineral oil is one kind in the mineral oil of 9#~17#；
The phosphate kalium salt is 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite, isomerous tridecanol polyoxyethylene ether phosphate kalium salt or ten
Tetracosanol phosphate kalium salt；
The sodium alkyl sulfonate is dodecyl sodium sulfate, pentadecyl sulfonic acid sodium or sodium cetanesulfonate；
The finish is configured to the emulsion that concentration is 10~20wt% when in use, with water；
The preparation method of the finish is：By crown ether and phosphate kalium salt, trimethylolpropane laurate and alkyl sulphur
Sour sodium is added in mineral oil after mixing is uniformly mixing to obtain finish；It counts in parts by weight, the addition of each component is as follows：
The mixing carries out at normal temperatures, and the temperature of the stirring is 40~55 DEG C, and the time is 1~3h.
Method as described above, the spinning technology parameter of the soft type polyester fiber are as follows：
Spinning temperature：280~290 DEG C；
Cooling temperature：20~25 DEG C；
Network pressure：0.20~0.30MPa；
One roller speed：2200~2600m/min
One roll temperature：75~85 DEG C；
Two roller speeds：3600~3900m/min；
Two roll temperatures：135~165 DEG C；
The speed of winding：3580~3840m/min.
Invention mechanism：
The present invention has been made that a kind of viscosity is low, heat resistance is good and film strength is higher by introducing crown ether in finish
Finish.The viscosity of finish is higher mainly due to containing conventional polyester class compound or polyethers chemical combination in finish in the prior art
Object, for such compound since molecular weight is larger and the effect of hydrogen bond, the intermolecular larger kinematic viscosity that shows as of effect is larger,
Thus cause the viscosity of finish higher, the viscosity of finish can significantly reduce after addition crown ether, mainly since crown ether itself is viscous
To spend relatively low and for pearl small molecule, crown ether can be preferably compatible in polyesters compound or polyethers finish system, while into
Enter between polyesters compound or polyether compound strand, the active force between strand is shielded, so as to reduce finish body
The viscosity of system.The film strength of finish is relatively low mainly since the antistatic agent of preparation medium mostly contains metal in the prior art
Ion exists in a salt form, causes antistatic agent and the poor compatibility of polyesters compound or polyethers in finish, hat
Ether, which can be improved after film strength is mainly added in due to crown ether, can generate salting in effect, improve antistatic agent and polyesters
The compatibility of compound or polyethers, and then improve finish oil film strength.In addition, crown ether has higher volatilization point and excellent
Good heat-resistant stability, the heat resistance of the finish introduced after crown ether are also obviously improved, since crown ether is more conventional flat
Lubrication prescription with lower viscosity, higher volatilization point, smaller coefficient of friction and with more excellent heat-resistant stability, from
And the processing performance of fiber is improved, reduce the appearance of fiber lousiness and a phenomenon of floaing so that the flexibility of fiber is more preferable.
Advantageous effect：
(1) soft type polyester fiber of the invention, preparation flow advantages of simple, soft type polyester fiber obtained have good
Good flexibility, great popularization；
(2) preparation method of soft type polyester fiber of the invention by introducing ethanedioic acid segment in modified poly ester, changes
The rigidity of polyester is become, so as to significantly improve the softness of fiber；
(3) preparation method of soft type polyester fiber of the invention, oil the oil agent containing crown ether used in the process
Have the characteristics that viscosity is low, heat resistance is good, film strength is high, Lubricity is good and antistatic property is strong, improve spinning
The processing performance of stability and fiber.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It is to 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 scope.
Embodiment 1
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；
It is 1 by molar ratio:1.2:0.03 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry, adds in three oxidations two
After mixing, the pressurization progress esterification in nitrogen atmosphere, moulding pressure is normal for antimony, titanium dioxide and triphenyl phosphate
Pressure, the temperature of esterification is 250 DEG C, is that esterification is whole when the water quantity of distillate in esterification reaches the 90% of theoretical value
The addition of point, wherein antimony oxide is the 0.01% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is terephthaldehyde
The 0.20% of sour weight, the addition of triphenyl phosphate are the 0.05% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 30min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 500Pa, and reaction temperature is 260 DEG C, and reaction time 40min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 100Pa, and reaction temperature is 275 DEG C, instead
It is 70min between seasonable, modified poly ester strand, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment, number
Average molecular weight 20000, molecular weight distributing index 2.0, the molar content of adipic acid segment is terephthalic acid (TPA) in modified poly ester
The 3% of segment molar content；
(2) oil and prepared with finish：By 2- methylols -12-crown-4 and 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite, trimethylolpropane
Laurate and dodecyl sodium sulfate are added to after mixing at normal temperatures in 9# mineral oil and in 40 DEG C of uniform stirring 1h
Obtain finish；It counts in parts by weight, the addition of each component is as follows：2 parts of 9# mineral oil；Trimethylolpropane laurate 10
Part；2- methylols -90 parts of 12-crown-4；8 parts of 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite；3 parts of dodecyl sodium sulfate.The finish prepared
The content of middle crown ether is 79.6wt%, and the high temperature resistance of finish is excellent, and thermal weight loss is after heating 2h at 200 DEG C
14.5wt%；The viscosity of finish is relatively low, at (50 ± 0.01) DEG C, kinematic viscosity 29.6mm2/ s, being configured to concentration with water is
Kinematic viscosity after the lotion of 10wt% is 0.93mm2/s；The film strength of finish is higher, film strength 125N, finish
Surface tension is 24.8cN/cm, and specific resistance is 1.3 × 108Ω cm, after oiling, the static friction between fiber and fiber (F/F)
Coefficient (μs) it is 0.255, the coefficient of kinetic friction (μd) it is 0.266, the confficient of static friction (μ between fiber and metal (F/M)s) be
0.203, the coefficient of kinetic friction (μd) it is 0.320, the finish of preparation is configured to the emulsification that concentration is 15wt% when in use, with water
Liquid；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 80cN/dtex, fiber number 80dtex, and fracture strength is
3.6cN/dtex, elongation at break 42.0%, fracture strength CV values are 4.7%, and extension at break CV values are 9.8%, and boiling water is received
Shrinkage is 7.5%, oil content 1.10%.
Embodiment 2
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；
It is 1 by molar ratio:1.4:0.05 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry, adds in antimony acetate, two
Titanium oxide and Trimethyl phosphite after mixing, pressurize in nitrogen atmosphere and carry out esterification, moulding pressure 0.1MPa,
The temperature of esterification is 252 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 92% of theoretical value,
Wherein the addition of antimony acetate is the 0.03% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is terephthalic acid (TPA) weight
0.23%, the addition of Trimethyl phosphite is the 0.01% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 40min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 495Pa, and reaction temperature is 263 DEG C, and reaction time 45min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 95Pa, and reaction temperature is 278 DEG C, instead
It is 60min between seasonable, modified poly ester strand, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment, number
Average molecular weight 21000, molecular weight distributing index 2.2, the molar content of adipic acid segment is terephthalic acid (TPA) in modified poly ester
The 4% of segment molar content；
(2) oil and prepared with finish：By 15- crown ethers -5 and isomerous tridecanol polyoxyethylene ether phosphate kalium salt, three hydroxyl first
Base propane laurate and pentadecyl sulfonic acid sodium be added to after mixing at normal temperatures in 10# mineral oil and 43 DEG C uniformly
Stirring 1.5h obtains finish；It counts in parts by weight, the addition of each component is as follows：2 parts of 10# mineral oil；The trimethylolpropane moon
15 parts of cinnamic acid ester；- 5 70 parts of 15- crown ethers；10 parts of isomerous tridecanol polyoxyethylene ether phosphate kalium salt；Pentadecyl sulfonic acid sodium 7
Part.The content of crown ether is 67.30wt% in the finish prepared, and the high temperature resistance of finish is excellent, heats 2h at 200 DEG C
Thermal weight loss is 13wt% afterwards, and the viscosity of finish is relatively low, at (50 ± 0.01) DEG C, kinematic viscosity 28.1mm2/ s, is configured with water
The kinematic viscosity after lotion for being 10wt% into concentration is 0.93mm2/ s, the film strength of finish is higher, is 123N, finish
Surface tension is 25.1cN/cm, and specific resistance is 1.5 × 108Ω cm, after oiling, the static friction between fiber and fiber (F/F)
Coefficient (μs) it is 0.257, the coefficient of kinetic friction (μd) it is 0.265, after oiling, the confficient of static friction between fiber and metal (F/M)
(μs) it is 0.205, the coefficient of kinetic friction (μd) it is 0.323, when in use, it is 14wt%'s to be configured to concentration with water to the finish of preparation
Emulsion；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 79cN/dtex, fiber number 120dtex, fracture strength
For 3.8cN/dtex, elongation at break 45.0%, fracture strength CV values are 4.7%, and extension at break CV values are 9.9%, boiling water
Shrinking percentage is 7.0%, oil content 1.10%.
Embodiment 3
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；It is 1 by molar ratio:1.4:0.05 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry,
Add in antimony acetate, titanium dioxide and Trimethyl phosphite after mixing, pressurization progress esterification, pressurization in nitrogen atmosphere
Pressure is 0.1MPa, and the temperature of esterification is 252 DEG C, is when the water quantity of distillate in esterification reaches the 92% of theoretical value
The addition of esterification terminal, wherein antimony acetate is the 0.03% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is pair
The 0.23% of phthalic acid weight, the addition of Trimethyl phosphite are the 0.01% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 40min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 495Pa, and reaction temperature is 263 DEG C, and reaction time 45min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 95Pa, and reaction temperature is 278 DEG C, instead
It is 60min between seasonable, the strand of modified poly ester, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment,
Number-average molecular weight 21000, molecular weight distributing index 2.2, the molar content of adipic acid segment is terephthaldehyde in modified poly ester
The 4% of sour segment molar content；
(2) oil and prepared with finish：By 2- methylol -15- crown-s 5 and ten tetracosanol phosphate kalium salts, trihydroxy methyl third
Alkane laurate and pentadecyl sulfonic acid sodium are added to after mixing at normal temperatures in 11# mineral oil and in 48 DEG C of uniform stirrings
3h obtains finish；It counts in parts by weight, the addition of each component is as follows：8 parts of 11# mineral oil；Trimethylolpropane laurate
10 parts；585 parts of 2- methylol -15- crown-s；Ten 11 parts of tetracosanol phosphate kalium salts；5 parts of pentadecyl sulfonic acid sodium.It prepares
The content of crown ether is 70.83wt% in finish, and the high temperature resistance of finish is excellent, and thermal weight loss is after heating 2h at 200 DEG C
11wt%, the viscosity of finish is relatively low, at (50 ± 0.01) DEG C, kinematic viscosity 30.1mm2/ s, being configured to concentration with water is
Kinematic viscosity after the lotion of 10wt% is 0.94mm2/ s, the film strength of finish is higher, is 125N.The surface tension of finish
For 23.2cN/cm, specific resistance is 1.8 × 108Ω cm, after oiling, the confficient of static friction (μ between fiber and fiber (F/F)s)
For 0.250, the coefficient of kinetic friction (μd) it is 0.272, after oiling, the confficient of static friction (μ between fiber and metal (F/M)s) be
0.209, the coefficient of kinetic friction (μd) it is 0.329, the finish of preparation is configured to the emulsification that concentration is 15wt% when in use, with water
Liquid；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 77cN/dtex, fiber number 250dtex, fracture strength
For 3.9cN/dtex, elongation at break 48.0%, fracture strength CV values are 4.7%, and extension at break CV values are 9.6%, boiling water
Shrinking percentage is 8.0%, oil content 0.90%.
Embodiment 4
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；It is 1 by molar ratio:1.5:0.06 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry,
Add in antimony oxide, titanium dioxide and triphenyl phosphate after mixing, pressurization progress esterification, adds in nitrogen atmosphere
Pressure pressure is 0.3MPa, and the temperature of esterification is 255 DEG C, when the water quantity of distillate in esterification reaches the 95% of theoretical value
For esterification terminal, the wherein addition of antimony oxide is the 0.04% of terephthalic acid (TPA) weight, the addition of titanium dioxide
It measures as the 0.25% of terephthalic acid (TPA) weight, the addition of triphenyl phosphate is the 0.01% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 50min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 400Pa, and reaction temperature is 265 DEG C, and reaction time 33min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 90Pa, and reaction temperature is 280 DEG C, instead
It is 50min between seasonable, the strand of modified poly ester, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment,
Number-average molecular weight 23000, molecular weight distributing index 1.9, the molar content of adipic acid segment is terephthaldehyde in modified poly ester
The 3.5% of sour segment molar content；
(2) oil and prepared with finish：By 2- methylols -12-crown-4 and 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite, trimethylolpropane
Laurate and sodium cetanesulfonate are added to after mixing at normal temperatures in 12# mineral oil and in 40 DEG C of uniform stirrings
2.5h obtains finish；It counts in parts by weight, the addition of each component is as follows：5 parts of 12# mineral oil；2- methylols -12-crown-4 95
Part；9 parts of 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite；2 parts of sodium cetanesulfonate.The content of crown ether is in the finish prepared
85.58wt%, the high temperature resistance of finish is excellent, and it is 9wt% to heat thermal weight loss after 2h at 200 DEG C, the viscosity of finish compared with
It is low, at (50 ± 0.01) DEG C, kinematic viscosity 29.5mm2/ s, the movement being configured to water after the lotion that concentration is 10wt%
Viscosity is 0.93mm2/ s, the film strength of finish is higher, is 121N, the surface tension of finish is 24.3cN/cm, and specific resistance is
1.0×108Ω cm, after oiling, the confficient of static friction (μ between fiber and fiber (F/F)s) it is 0.260, the coefficient of kinetic friction
(μd) it is 0.263, after oiling, the confficient of static friction (μ between fiber and metal (F/M)s) it is 0.202, the coefficient of kinetic friction (μd) be
0.330, the finish of preparation is configured to the emulsion that concentration is 16wt% when in use, with water；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 80cN/dtex, fiber number 190dtex, fracture strength
For 4.0cN/dtex, elongation at break 44.0%, fracture strength CV values are 5.0%, and extension at break CV values are 9.3%, boiling water
Shrinking percentage is 7.4%, oil content 0.80%.
Embodiment 5
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；
It is 1 by molar ratio:1.6:0.03 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry, add in antimony glycol,
Titanium dioxide and trimethyl phosphate after mixing, in nitrogen atmosphere pressurization carry out esterification, moulding pressure is normal pressure, ester
Change the temperature of reaction as 257 DEG C, be esterification terminal when the water quantity of distillate in esterification reaches the 92% of theoretical value,
The addition of middle antimony glycol is the 0.05% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is terephthalic acid (TPA) weight
0.20%, the addition of trimethyl phosphate is the 0.04% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 33min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 450Pa, and reaction temperature is 270 DEG C, and reaction time 30min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 95Pa, and reaction temperature is 275 DEG C, instead
It is 60min between seasonable, the strand of modified poly ester, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment,
Number-average molecular weight 25000, molecular weight distributing index 2.1, the molar content of adipic acid segment is terephthaldehyde in modified poly ester
The 5% of sour segment molar content；
(2) oil and prepared with finish：By 15- crown ethers -5 and isomerous tridecanol polyoxyethylene ether phosphate kalium salt, three hydroxyl first
Base propane laurate and dodecyl sodium sulfate be added to after mixing at normal temperatures in 13# mineral oil and 52 DEG C uniformly
Stirring 2h obtains finish；It counts in parts by weight, the addition of each component is as follows：10 parts of 13# mineral oil；Trimethylolpropane bay
5 parts of acid esters；- 5 70 parts of 15- crown ethers；8 parts of isomerous tridecanol polyoxyethylene ether phosphate kalium salt；6 parts of dodecyl sodium sulfate.System
Content for crown ether in the finish gone out is 70.70wt%, and the high temperature resistance of finish is excellent, the heat after 200 DEG C of heating 2h
Weightlessness is 13.5wt%, and the viscosity of finish is relatively low, at (50 ± 0.01) DEG C, kinematic viscosity 28.6mm2/ s, is configured to water
Kinematic viscosity after the lotion that concentration is 10wt% is 0.95mm2/ s, the film strength of finish is higher, for 126N, the table of finish
Face tension is 24.9cN/cm, and specific resistance is 1.2 × 108Ω cm, after oiling, the static friction system between fiber and fiber (F/F)
Number (μs) it is 0.251, the coefficient of kinetic friction (μd) it is 0.262, after oiling, the confficient of static friction (μ between fiber and metal (F/M)s)
For 0.202, the coefficient of kinetic friction (μd) it is 0.332, the finish of preparation is configured to the emulsification that concentration is 15wt% when in use, with water
Liquid；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 75cN/dtex, fiber number 130dtex, fracture strength
For 4.4cN/dtex, elongation at break 43.2%, fracture strength CV values are 4.8%, and extension at break CV values are 9.5%, boiling water
Shrinking percentage is 7.8%, oil content 1.00%.
Embodiment 6
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；
It is 1 by molar ratio:1.7:0.05 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry, adds in antimony acetate, two
Titanium oxide and Trimethyl phosphite after mixing, pressurize in nitrogen atmosphere and carry out esterification, moulding pressure 0.2MPa,
The temperature of esterification is 253 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 96% of theoretical value,
Wherein the addition of antimony acetate is the 0.01% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is terephthalic acid (TPA) weight
0.20%, the addition of Trimethyl phosphite is the 0.05% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 38min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 480Pa, and reaction temperature is 262 DEG C, and reaction time 38min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 98Pa, and reaction temperature is 279 DEG C, instead
It is 80min between seasonable, the strand of modified poly ester, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment,
Number-average molecular weight 27000, molecular weight distributing index 2.2, the molar content of adipic acid segment is terephthaldehyde in modified poly ester
The 4% of sour segment molar content；
(2) oil and prepared with finish：By 2- methylol -15- crown-s 5 and ten tetracosanol phosphate kalium salts, trihydroxy methyl third
Alkane laurate and pentadecyl sulfonic acid sodium are added to after mixing at normal temperatures in 14# mineral oil and in 55 DEG C of uniform stirrings
1h obtains finish；It counts in parts by weight, the addition of each component is as follows：3 parts of 14# mineral oil；Trimethylolpropane laurate
10 parts；5 75 parts of 2- methylol -15- crown-s；Ten 14 parts of tetracosanol phosphate kalium salts；7 parts of pentadecyl sulfonic acid sodium.It prepares
Finish in crown ether content for 68.80wt%, the high temperature resistance of finish is excellent, heats thermal weight loss after 2h at 200 DEG C
For 12wt%, the viscosity of finish is relatively low, at (50 ± 0.01) DEG C, kinematic viscosity 27.5mm2/ s, being configured to concentration with water is
Kinematic viscosity after the lotion of 10wt% is 0.95mm2/ s, the film strength of finish is higher, is 126N.The surface tension of finish
For 25.4cN/cm, specific resistance is 1.6 × 108Ω cm, after oiling, the confficient of static friction (μ between fiber and fiber (F/F)s)
For 0.255, the coefficient of kinetic friction (μd) it is 0.267, after oiling, the confficient of static friction (μ between fiber and metal (F/M)s) be
0.203, the coefficient of kinetic friction (μd) it is 0.330, the finish of preparation is configured to the emulsification that concentration is 17wt% when in use, with water
Liquid；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 71cN/dtex, fiber number 75dtex, and fracture strength is
3.7cN/dtex, elongation at break 45.5%, fracture strength CV values are 4.9%, and extension at break CV values are 10.0%, and boiling water is received
Shrinkage is 7.3%, oil content 0.92%.
Embodiment 7
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；
It is 1 by molar ratio:1.8:0.03 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry, adds in three oxidations two
After mixing, pressurization progress esterification, moulding pressure are in nitrogen atmosphere for antimony, titanium dioxide and triphenyl phosphate
0.3MPa, the temperature of esterification is 250 DEG C, is that esterification is anti-when the water quantity of distillate in esterification reaches the 90% of theoretical value
Terminal is answered, the wherein addition of antimony oxide is the 0.03% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is to benzene
The 0.24% of dioctyl phthalate weight, the addition of triphenyl phosphate are the 0.02% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 42min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 455Pa, and reaction temperature is 264 DEG C, and reaction time 45min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 85Pa, and reaction temperature is 285 DEG C, instead
It is 75min between seasonable, the strand of modified poly ester, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment,
Number-average molecular weight 26500, molecular weight distributing index 2.2, the molar content of adipic acid segment is terephthaldehyde in modified poly ester
The 4.5% of sour segment molar content；
(2) oil and prepared with finish：By 15- crown ethers -5 and 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite, trimethylolpropane lauric acid
Ester and sodium cetanesulfonate are added in 15# mineral oil and obtain oil in 41 DEG C of uniform stirring 2h after mixing at normal temperatures
Agent；It counts in parts by weight, the addition of each component is as follows：8 parts of 15# mineral oil；20 parts of trimethylolpropane laurate；15-
100 parts of crown ether -5；15 parts of 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite；2 parts of sodium cetanesulfonate.Crown ether contains in the finish prepared
It measures as 68.97wt%, the high temperature resistance of finish is excellent, and thermal weight loss is 8.5wt% after heating 2h at 200 DEG C, finish
Viscosity is relatively low, at (50 ± 0.01) DEG C, kinematic viscosity 28.4mm2/ s, after the lotion that concentration is 10wt% is configured to water
Kinematic viscosity be 0.94mm2/ s, the film strength of finish is higher, is 122N.The surface tension of finish is 26.8cN/cm, than
Resistance is 1.8 × 108Ω cm, after oiling, the confficient of static friction (μ between fiber and fiber (F/F)s) it is 0.263, dynamic friction
Coefficient (μd) it is 0.268, after oiling, the confficient of static friction (μ between fiber and metal (F/M)s) it is 0.210, the coefficient of kinetic friction
(μd) it is 0.320, the finish of preparation is configured to the emulsion that concentration is 16wt% when in use, with water；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 72cN/dtex, fiber number 72dtex, and fracture strength is
3.7cN/dtex, elongation at break 45.0%, fracture strength CV values are 4.9%, and extension at break CV values are 10.0%, and boiling water is received
Shrinkage is 7.0%, oil content 0.90%.
Embodiment 8
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；
It is 1 by molar ratio:1.9:0.04 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry, add in antimony glycol,
Titanium dioxide and trimethyl phosphate after mixing, pressurize in nitrogen atmosphere and carry out esterification, moulding pressure 0.3MPa,
The temperature of esterification is 260 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 93% of theoretical value,
Wherein the addition of antimony glycol is the 0.04% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is terephthalic acid (TPA) weight
0.21%, the addition of trimethyl phosphate is the 0.03% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 45min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 475Pa, and reaction temperature is 265 DEG C, and reaction time 48min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 88Pa, and reaction temperature is 283 DEG C, instead
It is 80min between seasonable, the strand of modified poly ester, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment,
Number-average molecular weight 23000, molecular weight distributing index 2.0, the molar content of adipic acid segment is terephthaldehyde in modified poly ester
The 3% of sour segment molar content；
(2) oil and prepared with finish：By 2- methylols -12-crown-4 and ten tetracosanol phosphate kalium salts, trihydroxy methyl third
Alkane laurate and pentadecyl sulfonic acid sodium are added to after mixing at normal temperatures in 16# mineral oil and in 45 DEG C of uniform stirrings
3h obtains finish；It counts in parts by weight, the addition of each component is as follows：9 parts of 16# mineral oil；2- methylols -12-crown-4 80
Part；Ten 12 parts of tetracosanol phosphate kalium salts；5 parts of pentadecyl sulfonic acid sodium.The content of crown ether is in the finish prepared
83.33wt%, the high temperature resistance of finish is excellent, and it is 14wt% to heat thermal weight loss after 2h at 200 DEG C, the viscosity of finish compared with
It is low, at (50 ± 0.01) DEG C, kinematic viscosity 30.0mm2/ s, the movement being configured to water after the lotion that concentration is 10wt%
Viscosity is 0.93mm2/ s, the film strength of finish is higher, is 127N.The surface tension of finish is 23.5cN/cm, and specific resistance is
1.5×108Ω cm, after oiling, the confficient of static friction (μ between fiber and fiber (F/F)s) it is 0.262, the coefficient of kinetic friction
(μd) it is 0.273, after oiling, the confficient of static friction (μ between fiber and metal (F/M)s) it is 0.208, the coefficient of kinetic friction (μd) be
0.328, the finish of preparation is configured to the emulsion that concentration is 18wt% when in use, with water；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 80cN/dtex, fiber number 200dtex, fracture strength
For 3.8cN/dtex, elongation at break 42.0%, fracture strength CV values are 4.2%, and extension at break CV values are 9.5%, boiling water
Shrinking percentage is 8.0%, oil content 0.90%.
Embodiment 9
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；
It is 1 by molar ratio:2.0:0.05 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry, adds in antimony acetate, two
After mixing, the pressurization progress esterification in nitrogen atmosphere, moulding pressure is normal pressure MPa for titanium oxide and trimethyl phosphate,
The temperature of esterification is 251 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 96% of theoretical value,
Wherein the addition of antimony acetate is the 0.05% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is terephthalic acid (TPA) weight
0.22%, the addition of trimethyl phosphate is the 0.04% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 30min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 420Pa, and reaction temperature is 267 DEG C, and reaction time 50min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 80Pa, and reaction temperature is 280 DEG C, instead
It is 90min between seasonable, the strand of modified poly ester, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment,
Number-average molecular weight 24000, molecular weight distributing index 2.2, the molar content of adipic acid segment is terephthaldehyde in modified poly ester
The 4% of sour segment molar content；
(2) oil and prepared with finish：By 2- methylol -15- crown-s 5 and 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite, trimethylolpropane
Laurate and dodecyl sodium sulfate obtain finish after mixing and in 55 DEG C of uniform stirring 3h at normal temperatures；By weight
Number meter, the addition of each component are as follows：15 parts of trimethylolpropane laurate；5 90 parts of 2- methylol -15- crown-s；Dodecane
8 parts of base phosphate kalium salt；7 parts of dodecyl sodium sulfate.The content of crown ether is 81.81wt% in the finish prepared, finish
High temperature resistance is excellent, and thermal weight loss is 10wt% after heating 2h at 200 DEG C, and the viscosity of finish is relatively low, in (50 ± 0.01)
DEG C when, kinematic viscosity 29.7mm2/ s, the kinematic viscosity being configured to water after the lotion that concentration is 10wt% is 0.94mm2/ s,
The film strength of finish is higher, is 126N.The surface tension of finish is 24.8cN/cm, and specific resistance is 1.8 × 108Ω cm, on
After oil, the confficient of static friction (μ between fiber and fiber (F/F)s) it is 0.250, the coefficient of kinetic friction (μd) it is 0.264, after oiling,
Confficient of static friction (μ between fiber and metal (F/M)s) it is 0.210, the coefficient of kinetic friction (μd) it is 0.321, the finish of preparation exists
In use, it is configured to the emulsion that concentration is 17wt% with water；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 76cN/dtex, fiber number 240dtex, fracture strength
For 3.9cN/dtex, elongation at break 42.0%, fracture strength CV values are 5.0%, and extension at break CV values are 9.4%, boiling water
Shrinking percentage is 7.0%, oil content 0.70%.
Embodiment 10
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；
It is 1 by molar ratio:1.2:0.06 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry, add in antimony glycol,
After mixing, pressurization progress esterification, moulding pressure are in nitrogen atmosphere for titanium dioxide and Trimethyl phosphite
0.1MPa, the temperature of esterification is 255 DEG C, is that esterification is anti-when the water quantity of distillate in esterification reaches the 92% of theoretical value
Terminal is answered, the wherein addition of antimony glycol is the 0.01% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is to benzene two
The 0.20% of formic acid weight, the addition of Trimethyl phosphite are the 0.01% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 50min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 490Pa, and reaction temperature is 269 DEG C, and reaction time 30min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 100Pa, and reaction temperature is 281 DEG C, instead
It is 55min between seasonable, the strand of modified poly ester, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment,
Number-average molecular weight 20000, molecular weight distributing index 1.9, the molar content of adipic acid segment is terephthaldehyde in modified poly ester
The 3.5% of sour segment molar content；
(2) oil and prepared with finish：By 2- methylol -15- crown-s 5 and 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite, trimethylolpropane
Laurate and dodecyl sodium sulfate obtain finish after mixing and in 55 DEG C of uniform stirring 3h at normal temperatures；By weight
Number meter, the addition of each component are as follows：15 parts of trimethylolpropane laurate；5 90 parts of 2- methylol -15- crown-s；Dodecane
8 parts of base phosphate kalium salt；7 parts of dodecyl sodium sulfate.The content of crown ether is 81.81wt% in the finish prepared, finish
High temperature resistance is excellent, and thermal weight loss is 10wt% after heating 2h at 200 DEG C, and the viscosity of finish is relatively low, in (50 ± 0.01)
DEG C when, kinematic viscosity 29.7mm2/ s, the kinematic viscosity being configured to water after the lotion that concentration is 10wt% is 0.94mm2/ s,
The film strength of finish is higher, is 126N, the surface tension of finish is 24.8cN/cm, and specific resistance is 1.8 × 108Ω cm, on
After oil, the confficient of static friction (μ between fiber and fiber (F/F)s) it is 0.250, the coefficient of kinetic friction (μd) it is 0.264, after oiling,
Confficient of static friction (μ between fiber and metal (F/M)s) it is 0.210, the coefficient of kinetic friction (μd) it is 0.321, the finish of preparation exists
In use, it is configured to the emulsion that concentration is 16wt% with water；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 74cN/dtex, fiber number 150dtex, fracture strength
For 4.5cN/dtex, elongation at break 48.0%, fracture strength CV values are 4.4%, and extension at break CV values are 9.7%, boiling water
Shrinking percentage is 7.5%, oil content 0.70%.
Embodiment 11
A kind of preparation method of soft type polyester fiber, is as follows：
(1) preparation of modified poly ester：
(a) esterification；
It is 1 by molar ratio:2.0:0.03 terephthalic acid (TPA), ethylene glycol and adipic acid is made into slurry, adds in antimony acetate, two
Titanium oxide and Trimethyl phosphite after mixing, pressurize in nitrogen atmosphere and carry out esterification, moulding pressure 0.2MPa,
The temperature of esterification is 250 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 97% of theoretical value,
Wherein the addition of antimony acetate is the 0.01% of terephthalic acid (TPA) weight, and the addition of titanium dioxide is terephthalic acid (TPA) weight
0.23%, the addition of Trimethyl phosphite is the 0.05% of terephthalic acid (TPA) weight；
(b) polycondensation reaction；
After esterification, under condition of negative pressure start the low vacuum stage polycondensation reaction, in 45min by pressure by
Normal pressure is steadily evacuated to absolute pressure as 500Pa, and reaction temperature is 260 DEG C, and reaction time 40min then proceedes to vacuumize, into
The polycondensation reaction of row high vacuum stage of Fig makes reaction pressure be further reduced to absolute pressure as 92Pa, and reaction temperature is 277 DEG C, instead
It is 80min between seasonable, the strand of modified poly ester, which is made, includes terephthalic acid (TPA) segment, ethylene glycol segment and 3 adipic acid segments,
Number-average molecular weight 25500, molecular weight distributing index 1.8, the molar content of adipic acid segment is terephthaldehyde in modified poly ester
The 5% of sour segment molar content.
(2) oil and prepared with finish：By 2- methylols -12-crown-4 and 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite, trimethylolpropane
Laurate and dodecyl sodium sulfate are added to after mixing at normal temperatures in 9# mineral oil and in 40 DEG C of uniform stirring 1h
Obtain finish；It counts in parts by weight, the addition of each component is as follows：2 parts of 9# mineral oil；Trimethylolpropane laurate 10
Part；2- methylols -90 parts of 12-crown-4；8 parts of 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite；3 parts of dodecyl sodium sulfate.The finish prepared
The content of middle crown ether is 79.6wt%, and the high temperature resistance of finish is excellent, and thermal weight loss is after heating 2h at 200 DEG C
14.5wt%, the viscosity of finish is relatively low, at (50 ± 0.01) DEG C, kinematic viscosity 29.6mm2/ s, being configured to concentration with water is
Kinematic viscosity after the lotion of 10wt% is 0.93mm2/ s, the film strength of finish is higher, film strength 125N, finish
Surface tension is 24.8cN/cm, and specific resistance is 1.3 × 108Ω cm, after oiling, the static friction between fiber and fiber (F/F)
Coefficient (μs) it is 0.255, the coefficient of kinetic friction (μd) it is 0.266, after oiling, the confficient of static friction between fiber and metal (F/M)
(μs) it is 0.203, the coefficient of kinetic friction (μd) it is 0.320, when in use, it is 15wt%'s to be configured to concentration with water to the finish of preparation
Emulsion；
(3) by modified poly ester through measuring, squeezing out, cooling down, oiling, stretching, that soft type polyester is made in thermal finalization and winding is fine
Dimension, the main spinning technology parameter of soft type polyester fiber are shown in Table 1.
The initial modulus of final obtained soft type polyester fiber is 79cN/dtex, fiber number 300dtex, fracture strength
For 3.8cN/dtex, elongation at break 48.0%, fracture strength CV values are 4.7%, and extension at break CV values are 9.9%, boiling water
Shrinking percentage is 8.0%, oil content 1.10%.
Table 1
Claims (9)
1. soft type polyester fiber, it is characterized in that：The material of soft type polyester fiber is modified poly ester；
The strand of modified poly ester includes terephthalic acid (TPA) segment, ethylene glycol segment and adipic acid segment；
Initial modulus≤80cN/dtex of soft type polyester fiber.
2. soft type polyester fiber according to claim 1, which is characterized in that the fiber number of the soft type polyester fiber is
75~300dtex, fracture strength >=3.6cN/dtex, elongation at break are 45.0 ± 3.0%, fracture strength CV value≤5.0%,
Extension at break CV value≤10.0%, boiling water shrinkage are 7.5 ± 0.5%, and oil content is 0.90 ± 0.20%.
3. soft type polyester fiber according to claim 1 or 2, which is characterized in that the equal molecule of number of the modified poly ester
Amount 20000~27000, molecular weight distributing index are 1.8~2.2；
The molar content of adipic acid segment is the 5~8% of terephthalic acid (TPA) segment molar content in the modified poly ester.
4. soft type polyester fiber according to claim 3, which is characterized in that the preparation method of the modified poly ester is：
Terephthalic acid (TPA), ethylene glycol and adipic acid are successively subjected to esterification after mixing and polycondensation reaction obtains modified poly ester；
It is as follows：
(1) esterification；
Terephthalic acid (TPA), ethylene glycol and adipic acid are made into slurry, add in catalyst, delustering agent and stabilizer after mixing,
Pressurization carries out esterification in nitrogen atmosphere, and moulding pressure is normal pressure~0.3MPa, and the temperature of esterification is 250~260
DEG C, it is esterification terminal when the water quantity of distillate in esterification reaches more than the 90% of theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, the staged pressure is in 30~50min
Interior to be steadily evacuated to by normal pressure below absolute pressure 500Pa, reaction temperature is 260~270 DEG C, and the reaction time is 30~50min, so
After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure made to be further reduced to below absolute pressure 100Pa,
Reaction temperature is 275~285 DEG C, and the reaction time is 50~90min, and modified poly ester is made.
5. soft type polyester fiber according to claim 4, which is characterized in that in step (1), terephthalic acid (TPA), second two
The molar ratio of alcohol and adipic acid is 1:1.2~2.0:0.03~0.06, the addition of the catalyst is terephthalic acid (TPA) weight
0.01~0.05%, the addition of the delustering agent is the 0.20~0.25% of terephthalic acid (TPA) weight, the stabilizer
Addition is the 0.01~0.05% of terephthalic acid (TPA) weight；
The catalyst is antimony oxide, antimony glycol or antimony acetate, and the delustering agent is titanium dioxide, and the stabilizer is
Triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite.
6. the method such as Claims 1 to 5 any one of them soft type polyester fiber is prepared, it is characterized in that：By the modification
Polyester is through measuring, squeezing out, cooling down, oiling, stretching, soft type polyester fiber is made in thermal finalization and winding；
Contain crown ether in the finish to oil, and the content of crown ether is 67.30~85.58wt%.
7. according to the method described in claim 6, it is characterized in that, thermal weight loss is small after the finish heats 2h at 200 DEG C
In 15wt%；
For the finish at (50 ± 0.01) DEG C, kinematic viscosity is 27.5~30.1mm2/ s, the finish are configured to concentration with water
It is 0.93~0.95mm for the kinematic viscosity after the lotion of 10wt%2/s；
The film strength of the finish is 121~127N；
The surface tension of the finish is 23.2~26.8cN/cm, and specific resistance is 1.0 × 108~1.8 × 108Ω·cm；
After oiling, the confficient of static friction between fiber and fiber is 0.250~0.263, and the coefficient of kinetic friction is 0.262~0.273；
After oiling, the confficient of static friction between fiber and metal is 0.202~0.210, and the coefficient of kinetic friction is 0.320~0.332.
8. the method according to the description of claim 7 is characterized in that the crown ether is 2- methylols -12-crown-4,15- crown ethers -5
Or 2- methylol -15- crown-s 5；
Also contain mineral oil, phosphate kalium salt, trimethylolpropane laurate and sodium alkyl sulfonate in the finish；
The mineral oil is one kind in the mineral oil of 9#~17#；
The phosphate kalium salt is 1-isobutyl-3,5-dimethylhexylphosphoric acid sylvite, isomerous tridecanol polyoxyethylene ether phosphate kalium salt or 12
Tetrol phosphate kalium salt；
The sodium alkyl sulfonate is dodecyl sodium sulfate, pentadecyl sulfonic acid sodium or sodium cetanesulfonate；
The finish is configured to the emulsion that concentration is 10~20wt% when in use, with water；
The preparation method of the finish is：By crown ether and phosphate kalium salt, trimethylolpropane laurate and sodium alkyl sulfonate
It is added to after mixing in mineral oil and is uniformly mixing to obtain finish；It counts in parts by weight, the addition of each component is as follows：
The mixing carries out at normal temperatures, and the temperature of the stirring is 40~55 DEG C, and the time is 1~3h.
9. according to claim 6~8 any one of them method, which is characterized in that the spinning work of the soft type polyester fiber
Skill parameter is as follows：
Spinning temperature：280~290 DEG C；
Cooling temperature：20~25 DEG C；
Network pressure：0.20~0.30MPa；
One roller speed：2200~2600m/min
One roll temperature：75~85 DEG C；
Two roller speeds：3600~3900m/min；
Two roll temperatures：135~165 DEG C；
The speed of winding：3580~3840m/min.
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