CN105506775B - A kind of super soft ultrafine wire of low aberration polyester and preparation method thereof - Google Patents
A kind of super soft ultrafine wire of low aberration polyester and preparation method thereof Download PDFInfo
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- CN105506775B CN105506775B CN201511017992.XA CN201511017992A CN105506775B CN 105506775 B CN105506775 B CN 105506775B CN 201511017992 A CN201511017992 A CN 201511017992A CN 105506775 B CN105506775 B CN 105506775B
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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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/83—Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, or compounds thereof
- C08G63/866—Antimony or compounds thereof
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/16—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
- D06P3/54—Polyesters using dispersed dyestuffs
Abstract
The present invention relates to super soft ultrafine wires of a kind of low aberration polyester and preparation method thereof, the super soft ultrafine wire of low aberration polyester is obtained by Direct-spinning of PET Fiber, fracture strength >=3.8cN/dtex of the super soft ultrafine wire of high dye-uptake polyester fiber, elongation at break is 35.0 ± 3.0%, filament number is 0.20~0.50dtex, aberration Δ E is less than 0.200, ethylene glycol magnesium in the present invention is milder, its thermal degradation coefficient very little, the side reaction triggered during the reaction is less, reduces the generation of oligomer in process；The reduction of oligomer in polymerization process, oligomer is further reduced during dissolveing and washing away so that in dyeing polyester fibers and post-processing heat setting, oligomer is reduced out of fiber to the amount of external migration, reduce color spot and item flower occurs, ensure that fiber level-dyeing property and crock fastness.The flexibility of super soft hyperfine polyester fiber since its filament number is very thin, and multifilament total fiber number also compared with and embody, fabric have particularly soft exquisiteness feel, gloss is soft, comfortable ventilating.
Description
Technical field
The invention belongs to polyester preparing technical fields, are related to super soft ultrafine wire of a kind of low aberration polyester and preparation method thereof, special
Be not a kind of polycondensation catalyst through water and dissolves and washes away agent 120 using the mixture and polyester slice of ethylene glycol magnesium and antimony glycol
~130 DEG C, brew under the conditions of 0.2~0.3MPa, the super soft ultrafine wire of low aberration polyester and preparation method thereof of washing.
Background technology
Polyethylene terephthalate (PET) is a kind of polymer of function admirable, PET with its modulus is high, intensity is high,
It is well-pressed, conformality is good, pure health, barrier property are good etc., be widely used in fiber, the fields such as bottle is packed, film and sheet material,
Yield cumulative year after year, position in industry are obviously improved.
PET belongs to the straight chain macromolecular of symmetry, and strand does not contain side-chain radical, and regularity is very good, this structure
Glass transition temperature it is higher, it is necessary to dye at very high temperatures, promote diffusion of the dye molecule to fibrous inside.Separately
Outside, the strand of PET is regular, good crystallinity, and strand arrangement is close, and does not have an effect on strand with dye molecule
Polar group, the colouring for making polyester fiber is more difficult.Due to not having hydrophilic radical in its molecule, hygroscopicity is very poor, this leads
The dyeing for causing terylene is relatively difficult.The main high-temperature and high pressure dyeing process method of terylene disperse dyeing
Oligomer in polyester fiber is the ester or ether of a kind of low molecular weight, is primarily referred to as the oligomerisation that the degree of polymerization is less than 10
Object, diethylene glycol (DEG) are to generate as a by-product.Wherein oligomer is divided into linear oligomerization object and cyclic oligomer, wherein with ring
Shape aggressiveness particularly cyclic trimer is in the majority, and oligomer is mainly concerned with heterogeneous nucleation, spinning processing, dyeing etc., to polyester
Performance and the processing of rear road cause certain harmful effect.Ethylene glycol terephthalate polymer (PET) is greatly containing about oligomer 3-
4%, it will make troubles when oligomer occurs in fiber surface to dyeing and post-processing.Diffusing out for oligomer is easiest to occur
Temperature control heating and holding stage in dyeing.When cooling since oligomer solubility in water is with temperature as dyestuff
Degree is reduced and strongly reduced, therefore can crystallize precipitation, and the dyestuff and oligomer of precipitation are attached to fiber surface and are very unlikely to wash away, from
And bringing many troubles to dyeing and post-processing, in dyeing course, the dyestuff and oligomer of aggregation are adhered to fiber surface, occur
Phenomena such as dyestuff color dot, spot, dyeing defect.It is deposited in the pipeline and valve of overflow dyeing machine, hinders liquid stream Xun Huan, cause dyeing tired
It is difficult.Oligomer key is eliminated to be to eliminate oligomer cyclic trimer and diethylene glycol (DEG), be on the one hand reduce in the course of the polymerization process it is low
On the other hand the generation of polymers is removed before dyeing or in dyeing.
The drastically expansion and the variation of international situation of polyester production capacity, people are to the comfort of clothing, functionality, variation
There is the super soft superfine denier polyester production such as higher requirement, terylene 22dtex/48f, 22dtex/72f, 33dtex/72f with security
Product, fabric is easy to the preferable superiority of texture of nursing and appearance with the feel of particularly soft exquisiteness, comfortable ventilating, more next
More obtain the favor of user.
The content of the invention
The object of the present invention is to provide super soft ultrafine wires of a kind of low aberration polyester and preparation method thereof, are a kind of polycondensation catalysis
Agent is using polyester and the super soft ultrafine wire of low aberration polyester of ethylene glycol magnesium and the mixture of antimony glycol and preparation method thereof.This
Invention uses the mixture of ethylene glycol magnesium and antimony glycol as polycondensation catalyst, and thermal degradation is reduced to minimum and polyester cuts
Piece is through water and dissolves and washes away agent at 130 DEG C, brew, washing under the conditions of 0.3MPa；It is super to polyester soft super to reduce oligomer, diethylene glycol content
The influence of filament dyeing.
A kind of super soft ultrafine wire of low aberration polyester of the present invention is terephthalic acid (TPA) and ethylene glycol through esterification for the polyester
With the mixture through catalytic of ethylene glycol magnesium and antimony glycol effect under polycondensation, be granulated and dissolve and wash away after spinning be made；
In the section of the industry polyester, oligomer mass percentage content is less than 0.5%, the quality percentage of diethylene glycol (DEG)
It is less than 0.5% than content；
The molecular formula of the ethylene glycol magnesium is Mg (OCH2CH2OH)2；
Described dissolve and wash away refers to that the section after being granulated is boiled with dissolveing and washing away agent under the conditions of 120~130 DEG C with 0.2~0.3MPa through water
Bubble and washing.
The super soft ultrafine wire of low aberration polyester is dissolved and washed away rear spinning by polyester and is obtained, the super soft ultrafine wire of low aberration polyester
Fracture strength >=3.8cN/dtex, elongation at break are 35.0 ± 3.0%, and filament number is 0.20~0.50dtex, aberration Δ E
Less than 0.200, the flexibility of super soft hyperfine polyester fiber is very thin mainly due to its filament number, and multifilament total fiber number also compared with and
It embodies, fabric has the feel of particularly soft exquisiteness, and gloss is soft, comfortable ventilating.
In dyeing polyester fibers and post-processing, influence surface oligomers precipitation factor it is very much, mainly have temperature and when
Between etc. factors.The migration that dyeing temperature will aggravate oligomer is improved, in the presence of particularly ought having some auxiliary agents or dyestuff, migration speed
Degree improves faster.The time of dye liquor circulation continuous is longer, and oligomer increases out of fiber to the amount of external migration, frequent cold cycling
And the presence of some auxiliary agents, dyestuff can aggravate removal and the deposition of oligomer significantly.The temperature and time of heat setting simultaneously
Have a significant impact to oligomer migration speed and the amount of migration.Heat setting is one of crucial importance for synthetic fibers dyeing and finishing processing
Process, its main purpose be eliminate fabric on existing fine wrinkle and improve fabric dimensional stability and improve fabric it is strong
The performances such as power, feel, pilling and surfacing.But the phenomenon that so often occurs in yarn dyed fabric shaping process, i.e.,
Fabric surface after heat setting is susceptible to color spot and item flower, and level-dyeing property and crock fastness are also remarkably decreased, especially for super
Thin dacron influences to be particularly acute, and migration of the oligomer under heat effect from inside to outside is one of the main reasons.Existing skill
Art all concentrates on dyeing link to solve influence of the oligomer to dyeing, this is that one kind controls calibration method, only from source
Solution be only effect a permanent cure it is basic.
Using ethylene glycol magnesium and antimony glycol mixture as polycondensation catalyst, ethylene glycol magnesium belongs to comparatively gentle one
Class, thermal degradation coefficient very little, the side reaction triggered during the reaction is less, reduces the production of oligomer in process
It is raw.The principal element for causing thermal degradation is high mild catalyst, and high temperature is that response intensity is excessively high, and degradation is caused to accelerate, is generated
End carboxyl, while also increase cyclic oligomer；Catalyst is then related to the degradation reaction constant of catalyst, in polycondensation process
In, the effect of catalyst, which is not only in that, can be catalyzed generation main reaction, so as to influence the rate and yield of reaction, while can also be catalyzed
Thermal degradation and ehter bond generation increase the content of cyclic oligomer and diethylene glycol (DEG).
A kind of line density deviation ratio≤0.5% of the super soft ultrafine wire of low aberration polyester as described above, fracture strength CV values
≤ 3.0%, extension at break CV value≤8.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content
1.00 ± 0.20%.
In the mixture of a kind of super soft ultrafine wire of low aberration polyester as described above, the ethylene glycol magnesium and antimony glycol,
Ethylene glycol magnesium is 2~3 with antimony glycol mass ratio:1.
The present invention also provides a kind of preparation method of the super soft ultrafine wire of low aberration polyester, a kind of low aberration polyester is super soft super
The preparation method of filament is that terephthalic acid (TPA) and ethylene glycol are made through esterification and in the mixture through catalytic of ethylene glycol magnesium and antimony glycol
Polyester is made with lower polycondensation, then polyester slice is obtained through pelletizing, polyester is made after then polyester slice is dissolved and washed away；Again through meter
It measures, squeeze out, cooling down, oiling and high-speed winding, the super soft ultrafine wire of low aberration polyester fiber is made；Main technique is：
(1) preparation of catalyst glycol magnesium：
In single-cell for electrolyzation plus ethylene glycol, supporting electrolyte are magnesium chloride, and metal MAG block is anode, and cathode is graphite；
Logical direct current, 6~10VV of starting voltage, cathode-current density are 150~200mA, when electrolysis 10~12 is small at 50~60 DEG C, electricity
Electrode is taken out after solution, obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, and second two is obtained after dry
Magnesium alkoxide；
(2) preparation of polyester, including esterification and polycondensation reaction：
The esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, anti-ether agent is added in, esterification is carried out after being made into uniform sizing material,
Obtain esterification products；Esterification is pressurizeed in nitrogen atmosphere, and pressure is controlled in normal pressure~0.3MPa, and temperature is 250~260
DEG C, esterification water quantity of distillate reaches more than the 90% of theoretical value for esterification terminal；
The polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
The polycondensation reaction low vacuum stage adds in catalyst and stabilizer, under conditions of negative pressure in esterification products
Start polycondensation reaction, which is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature is controlled at 260~270 DEG C,
Reaction time is 30~50 minutes；The catalyst is ethylene glycol magnesium and the mixture of antimony glycol；
The polycondensation reaction high vacuum stage of Fig after the polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure
Power is down to absolute pressure less than 100Pa, and reaction temperature control is at 275~280 DEG C, 50~90 minutes reaction time；
Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
The polyester slice is through water and dissolves and washes away agent when brew 3-5 is small under the conditions of 120~130 DEG C with 0.2~0.3MPa, after
It is washed；Obtain polyester.
(4) spinning main technologic parameters：
The temperature of the extrusion is 290~295 DEG C；
The wind-warm syndrome of the cooling is 20~25 DEG C；
HT1：75-95℃；
HT2：120-130℃；
The high-speed winding speed is 4000~5000m/min.
A kind of preparation method of the super soft ultrafine wire of low aberration polyester as described above, the ethylene glycol and the terephthaldehyde
The molar ratio of acid is 1.2~2.0:1.
A kind of preparation method of the super soft ultrafine wire of low aberration polyester as described above, the ethylene glycol magnesium and antimony glycol
In mixture, ethylene glycol magnesium is 2~3 with antimony glycol mass ratio:1；The catalyst amount is the terephthalic acid (TPA) quality
0.01%~0.05%.
A kind of preparation method of the super soft ultrafine wire of low aberration polyester as described above, the stabilizer are selected from phosphoric acid triphen
One kind in ester, trimethyl phosphate and Trimethyl phosphite, stabilizing agent dosage for the terephthalic acid (TPA) weight 0.01%~
0.05%.For stabilizer mainly based on phosphate, main function is the free radical that catching reaction generates in the course of the polymerization process, is reduced
Side reaction.
A kind of preparation method of the super soft ultrafine wire of low aberration polyester as described above, the water and the mass ratio for dissolveing and washing away agent
For 100:3~4, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio is 1:5-10；It is described to dissolve and wash away agent as one second of ethylene glycol
One kind in ether, propyl cellosolve and ethylene glycol monobutyl ether (EGMBE), what addition was a small amount of in water dissolves and washes away agent, dissolves and washes away agent and is dissolved in water, together
When also can dissolve most of low molecular ethers and ester, be conducive to improve washing effect and oligomer reduction.
A kind of preparation method of the super soft ultrafine wire of low aberration polyester as described above, polyester is cut after the washing refers to brew
70~80 DEG C of 10~15min of hot water wash of piece, are then cleaned, Drying and cooling is spare with cold water.
A kind of preparation method of the super soft ultrafine wire of low aberration polyester as described above, the anti-ether agent are sodium acetate and acetic acid
One kind in calcium, anti-ether agent dosage are the 0.01%~0.05% of the terephthalic acid (TPA) weight.Anti- ether agent is a small amount of by adding in
NaAc reduces the generation of ether in acid condition, so as to reduce the activity of glycol reaction generation diethylene glycol (DEG).
The object of the present invention is to provide a kind of super soft ultrafine wire of low aberration polyester, using relatively mild a kind of polycondensation catalyst
Ethylene glycol magnesium, the less side reaction triggered during the reaction is less and process in less thermal degradation, reduce
The generation of oligomer in process.Polyester slice is through water and dissolves and washes away agent at 130 DEG C, and brew is conducive to improve under the conditions of 0.3MPa
The effect of washing and the reduction of oligomer.The reduction of oligomer so that in dyeing polyester fibers and post-processing heat setting, oligomer
It is reduced out of fiber to the amount of external migration, reduces color spot and item flower occurs, ensure that fiber level-dyeing property and crock fastness.
Advantageous effect：
● using ethylene glycol magnesium and antimony glycol mixture as polycondensation catalyst, ethylene glycol magnesium belongs to comparatively gentle one
Class, thermal degradation coefficient very little, the side reaction triggered during the reaction is less, reduces end carboxyl in process and low
The generation of polymers.
● the oligomer mass percentage content of polyester slice is less than 0.5%, and the mass percentage content of diethylene glycol (DEG) is less than
0.5%, be conducive to further improve the quality of fiber.
● polyester slice through water with dissolve and wash away agent brew under the conditions of 120~130 DEG C with 0.2~0.3MPa be conducive to improve wash
The effect washed and the reduction of oligomer.
● anti-ether agent reduces the generation of ether in acid condition by adding in a small amount of NaAc, so as to reduce glycol reaction
Generate the activity of diethylene glycol (DEG).
● the reduction of oligomer in polymerization process, oligomer is further reduced during dissolveing and washing away so that dyeing polyester fibers
And in post-processing heat setting, oligomer is reduced out of fiber to the amount of external migration, reduces color spot and item flower occurs, ensure that fibre
Tie up level-dyeing property and crock fastness.
● fiber of the invention since its filament number is very thin, fabric with the feel of particularly soft exquisiteness, gloss is soft,
Comfortable ventilating is easy to the preferable superiority of texture of nursing and appearance, increasingly obtains the favor of user.
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.
A kind of super soft ultrafine wire of low aberration polyester of the present invention, the super soft ultrafine wire of low aberration polyester are spun by polyester after dissolveing and washing away
Silk and obtain, fracture strength >=3.8cN/dtex of the super soft ultrafine wire of low aberration polyester, elongation at break be 35.0 ±
3.0%, filament number is 0.20~0.50dtex, and aberration Δ E is less than 0.200, and polyester is terephthalic acid (TPA) and ethylene glycol through ester
Change and the polycondensation under the effect of the mixture through catalytic of ethylene glycol magnesium and antimony glycol, then obtain polyester slice through pelletizing；Industry is used poly-
In the section of ester, oligomer mass percentage content is less than 0.5%, and the mass percentage content of diethylene glycol (DEG) is less than 0.5%；Second two
The molecular formula of magnesium alkoxide is Mg (OCH2CH2OH)2；It dissolves and washes away and refers to the section after being granulated through water and dissolve and wash away agent at 120~130 DEG C and 0.2
Brew and washing under the conditions of~0.3MPa.
Wherein line density deviation ratio≤0.5% of the super soft ultrafine wire of low aberration polyester, fracture strength CV value≤3.0% break
It splits and extends CV value≤8.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 1.00 ±
0.20%.
Wherein, in the mixture of ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium is 2~3 with antimony glycol mass ratio:1.
A kind of preparation method of the super soft ultrafine wire of low aberration polyester of the present invention, terephthalic acid (TPA) and ethylene glycol through esterification and
Polyester is made in polycondensation under the effect of the mixture through catalytic of ethylene glycol magnesium and antimony glycol, then obtains polyester slice through pelletizing, then
Polyester is made after polyester slice is dissolved and washed away；Again through measuring, squeezing out, cooling down, oiling and high-speed winding, it is fine that low aberration polyester is made
Tie up super soft ultrafine wire.
1st, dyestuff：
Disperse brilliant blue 2BLN, 5% (o.w.f)
2nd, dyeing：
Fiber enters dye 10~15min of heat preservation, 1.0~2.0 DEG C/min of heating rate, 120~130 DEG C of heat preservations at 70~80 DEG C
40~60min, cooling, 70~80 DEG C of 20~30min of reduction cleaning.
3rd, the measure of dye uptake
It is dyed by above-mentioned technique, and draws liquid before dye respectively, each 2ml of Liquid Residue adds in third in 10ml volumetric flasks
Ketone 4ml, makes dyestuff fully dissolve.Scale is diluted to distilled water, then λ is measured with spectrophotometricmax, when dyeing before and after dyestuff
Absorbance A 0, A1 are then：
Dye uptake (%)=(mono- A1/A0 of l) × 100%
In formula：The absorbance of liquid before A0--- dyes
The absorbance of A1--- Liquid Residues
4th, the measure of dyefastness
It is tested by GB3920-83, GB251-64, GB3921-83
5th, tinctorial yield and the measure of aberration
It is tested using color measurement and color match instrument.
6th, the measure of apparent colour depth (K/S)
It is calculated using storehouse Bell card-Munch (kubelka-munk) function：In K/S=(1-R) 2//2R. formulas, K is quilt
Survey the absorption coefficient of object；S is the scattering coefficient of testee；Reflectivity when R is testee infinite thickness.Using SF600X
Datacolor color measurement and color matches instrument is tested, and is tested 5 times in different zones per sample, is taken its mathematical mean.
Embodiment 1
A kind of preparation method of the super soft ultrafine wire of low aberration polyester, main technique include：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and cathode is stone
Ink；Logical direct current, starting voltage 6V, cathode-current density 150mA when electrolysis 10 is small at 50 DEG C, take out electricity after electrolysis
Pole obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, and ethylene glycol magnesium is obtained after dry；
(2) preparation of polyester, including esterification and polycondensation reaction：
Esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, the molar ratio of ethylene glycol and terephthalic acid (TPA) is 1.2:1, it adds in
Anti- ether agent sodium acetate, sodium acetate dosage are the 0.01% of terephthalic acid (TPA) weight, carry out esterification after being made into uniform sizing material, obtain
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, and pressure is controlled in normal pressure, and at 250 DEG C, esterification water quantity of distillate reaches temperature
It is esterification terminal to the 91% of theoretical value；
Polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the polycondensation reaction low vacuum stage, catalyst and stabilizer triphenyl phosphate are added in esterification products, catalyst is used
It measures as the 0.01% of terephthalic acid (TPA) quality, triphenyl phosphate dosage is the 0.01% of terephthalic acid (TPA) weight, in the item of negative pressure
Start polycondensation reaction under part, which is steadily evacuated to absolute pressure 498Pa by normal pressure, and temperature is controlled at 260 DEG C, reaction
Between be 30 minutes；Catalyst is ethylene glycol magnesium and the mixture of antimony glycol, and ethylene glycol magnesium is 2 with antimony glycol mass ratio:1；
Polycondensation reaction high vacuum stage of Fig after the polycondensation reaction low vacuum stage, continues to vacuumize, reaction pressure is made to be down to absolutely
To pressure 96Pa, reaction temperature control is at 275 DEG C, 50 minutes reaction time；Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
Polyester slice is through water and dissolves and washes away agent ethylene glycol monoethyl ether when brew 3 is small under the conditions of 120 DEG C with 0.2MPa, by washing
It washs, i.e., 70 DEG C of hot water wash 10min of polyester slice, are then cleaned, Drying and cooling is spare with cold water after brew；Obtain polyester, water
Mass ratio with dissolveing and washing away agent is 100:3, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio is 1:5.
(4) spinning main technologic parameters：
The temperature of extrusion is 290 DEG C；
The wind-warm syndrome of cooling is 20 DEG C；
HT1：75℃；
HT2：120℃；
High-speed winding speed is 4000m/min.
The fracture strength 3.9cN/dtex of the super soft ultrafine wire of low aberration polyester, elongation at break 37.5%, monofilament is made
Fiber number is 0.25dtex；Line density deviation ratio 0.4%, fracture strength CV values 2.8%, extension at break CV values 7.8%, evenness fault
Rate CV1.92%, boiling water shrinkage 7.6%, oil content 1.15%.
(5) dye
Embodiment 2
A kind of preparation method of the super soft ultrafine wire of low aberration polyester, main technique include：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and cathode is stone
Ink；Logical direct current, starting voltage 10V, cathode-current density 200mA when electrolysis 12 is small at 60 DEG C, take out electricity after electrolysis
Pole obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, and ethylene glycol magnesium is obtained after dry；
(2) preparation of polyester, including esterification and polycondensation reaction：
Esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, the molar ratio of ethylene glycol and terephthalic acid (TPA) is 2.0:1, it adds in
Anti- ether agent calcium acetate, calcium acetate dosage are the 0.05% of terephthalic acid (TPA) weight, carry out esterification after being made into uniform sizing material, obtain
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, and pressure control is in 0.3MPa, and temperature is at 260 DEG C, esterification water quantity of distillate
Reach the 92% of theoretical value for esterification terminal；
Polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the polycondensation reaction low vacuum stage, catalyst and stabilizer trimethyl phosphate are added in esterification products, catalyst is used
It measures as the 0.05% of terephthalic acid (TPA) quality, trimethyl phosphate dosage is the 0.05% of terephthalic acid (TPA) weight, in the item of negative pressure
Start polycondensation reaction under part, which is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature is controlled at 270 DEG C, reaction
Between be 50 minutes；Catalyst is ethylene glycol magnesium and the mixture of antimony glycol, and ethylene glycol magnesium is 3 with antimony glycol mass ratio:1；
Polycondensation reaction high vacuum stage of Fig after the polycondensation reaction low vacuum stage, continues to vacuumize, reaction pressure is made to be down to absolutely
To pressure 95Pa, reaction temperature control is at 280 DEG C, 90 minutes reaction time；Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
Polyester slice is through water and dissolves and washes away agent propyl cellosolve when brew 5 is small under the conditions of 130 DEG C with 0.3MPa, by washing
It washs, i.e., 80 DEG C of hot water wash 15min of polyester slice, are then cleaned, Drying and cooling is spare with cold water after brew；Obtain polyester, water
Mass ratio with dissolveing and washing away agent is 100:4, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio is 1:10.
(4) spinning main technologic parameters：
The temperature of extrusion is 295 DEG C；
The wind-warm syndrome of cooling is 25 DEG C；
HT1：95℃；
HT2：1130℃；
High-speed winding speed is 5000m/min.
The fracture strength 3.8cN/dtex of the super soft ultrafine wire of low aberration polyester, elongation at break 37% is made；Low aberration
The line density deviation ratio 0.18% of the super soft ultrafine wire of polyester, fracture strength CV values 2.8%, extension at break CV values 5.8%.
(5) dye
Embodiment 3
A kind of preparation method of the super soft ultrafine wire of low aberration polyester, main technique include：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and cathode is stone
Ink；Logical direct current, starting voltage 7V, cathode-current density 160mA when electrolysis 11 is small at 55 DEG C, take out electricity after electrolysis
Pole obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, and ethylene glycol magnesium is obtained after dry；
(2) preparation of polyester, including esterification and polycondensation reaction：
Esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, the molar ratio of ethylene glycol and terephthalic acid (TPA) is 1.5:1, it adds in
Anti- ether agent sodium acetate, sodium acetate dosage are the 0.02% of terephthalic acid (TPA) weight, carry out esterification after being made into uniform sizing material, obtain
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, and pressure control is in 0.2MPa, and temperature is at 255 DEG C, esterification water quantity of distillate
Reach the 92% of theoretical value for esterification terminal；
Polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
The polycondensation reaction low vacuum stage adds in catalyst and stabilizer Trimethyl phosphite, catalyst in esterification products
Dosage is the 0.02% of terephthalic acid (TPA) quality, and Trimethyl phosphite dosage is the 0.02% of terephthalic acid (TPA) weight, in negative pressure
Under conditions of start polycondensation reaction, which is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature is controlled at 265 DEG C, instead
It is 35 minutes between seasonable；Catalyst is ethylene glycol magnesium and the mixture of antimony glycol, and ethylene glycol magnesium is with antimony glycol mass ratio
3:1；
Polycondensation reaction high vacuum stage of Fig after the polycondensation reaction low vacuum stage, continues to vacuumize, reaction pressure is made to be down to absolutely
To pressure 98Pa, reaction temperature control is at 277 DEG C, 60 minutes reaction time；Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
Polyester slice is through water and dissolves and washes away agent ethylene glycol monobutyl ether (EGMBE) when brew 3 is small under the conditions of 125 DEG C with 0.2MPa, by washing
It washs, i.e., 70 DEG C of hot water wash 15min of polyester slice, are then cleaned, Drying and cooling is spare with cold water after brew；Obtain polyester, water
Mass ratio with dissolveing and washing away agent is 100:4, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio is 1:10.
(4) spinning main technologic parameters：
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 4000~5000m/min.
The fracture strength 3.8cN/dtex of the super soft ultrafine wire of low aberration polyester, elongation at break 36% is made；Low aberration
The line density deviation ratio 0.19% of the super soft ultrafine wire of polyester, fracture strength CV values 2.8%, extension at break CV values 5.6%.
(5) dye
Embodiment 4
A kind of preparation method of the super soft ultrafine wire of low aberration polyester, main technique include：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and cathode is stone
Ink；Logical direct current, starting voltage 7V, cathode-current density 170mA when electrolysis 11 is small at 58 DEG C, take out electricity after electrolysis
Pole obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, and ethylene glycol magnesium is obtained after dry；
(2) preparation of polyester, including esterification and polycondensation reaction：
Esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, the molar ratio of ethylene glycol and the terephthalic acid (TPA) is 1.8:1,
Anti- ether agent sodium acetate is added in, sodium acetate dosage is the 0.02% of terephthalic acid (TPA) weight, after being made into uniform sizing material be esterified instead
Should, obtain esterification products；Esterification is pressurizeed in nitrogen atmosphere, and pressure control is in 0.3MPa, and temperature is at 250 DEG C, esterification water
Quantity of distillate reaches the 98% of theoretical value for esterification terminal；
Polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the polycondensation reaction low vacuum stage, catalyst and stabilizer triphenyl phosphate are added in esterification products, catalyst is used
It measures as the 0.02% of the terephthalic acid (TPA) quality, triphenyl phosphate dosage is the 0.02% of terephthalic acid (TPA) weight, in negative pressure
Under conditions of start polycondensation reaction, which is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature is controlled at 264 DEG C, instead
It is 38 minutes between seasonable；Catalyst is ethylene glycol magnesium and the mixture of antimony glycol, and ethylene glycol magnesium is with antimony glycol mass ratio
3:1；
Polycondensation reaction high vacuum stage of Fig after the polycondensation reaction low vacuum stage, continues to vacuumize, reaction pressure is made to be down to absolutely
To pressure 99Pa, reaction temperature control is at 280 DEG C, 90 minutes reaction time；Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
Polyester slice is through water and dissolves and washes away agent ethylene glycol monoethyl ether when brew 3 is small under the conditions of 120 DEG C with 0.3MPa, by washing
It washs, i.e., 70 DEG C of hot water wash 15min of polyester slice, are then cleaned, Drying and cooling is spare with cold water after brew；Obtain polyester, water
Mass ratio with dissolveing and washing away agent is 100:4, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio is 1:8.
(4) spinning main technologic parameters：
The temperature of extrusion is 292 DEG C；
The wind-warm syndrome of cooling is 23 DEG C；
HT1：90℃；
HT2：128℃；
High-speed winding speed is 4500m/min.
The fracture strength 3.9cN/dtex of the super soft ultrafine wire of low aberration polyester, elongation at break 38% is made；Low aberration
The line density deviation ratio 0.18% of the super soft ultrafine wire of polyester, fracture strength CV values 2.6%, extension at break CV values 5.2%.
(5) dye
Claims (9)
1. a kind of super soft ultrafine wire of low aberration polyester, it is characterized in that：The super soft ultrafine wire of low aberration polyester is by polyester through dissolveing and washing away
Afterwards spinning and obtain, fracture strength >=3.8cN/dtex of the super soft ultrafine wire of low aberration polyester, elongation at break for 35.0 ±
3.0%, filament number is 0.20~0.50dtex, and aberration Δ E is less than 0.200, and the polyester is terephthalic acid (TPA) and ethylene glycol
Polyester slice is obtained through esterification and the polycondensation under the effect of the mixture through catalytic of ethylene glycol magnesium and antimony glycol, then through pelletizing；
In the polyester slice, oligomer mass percentage content is less than 0.5%, and the mass percentage content of diethylene glycol (DEG) is less than
0.5%；
The molecular formula of the ethylene glycol magnesium is Mg (OCH2CH2OH)2；
In the mixture of the ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium is 2~3 with antimony glycol mass ratio:1；
Described dissolve and wash away refers to the section after being granulated through water and dissolves and washes away agent under the conditions of 120~130 DEG C with 0.2~0.3MPa after brew
Washing.
2. the super soft ultrafine wire of a kind of low aberration polyester according to claim 1, which is characterized in that the low aberration polyester surpasses
Line density deviation ratio≤0.5% of soft ultrafine wire, fracture strength CV value≤3.0%, extension at break CV value≤8.0%, item are done not
Even rate CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 1.00 ± 0.20%.
3. such as a kind of preparation method of the super soft ultrafine wire of low aberration polyester according to any one of claims 1 to 2, feature
It is：Polycondensation is made poly- through esterification and under the effect of the mixture through catalytic of ethylene glycol magnesium and antimony glycol for terephthalic acid (TPA) and ethylene glycol
Ester, then polyester slice is obtained through pelletizing, polyester is made after then polyester slice is dissolved and washed away；Again through measuring, squeezing out, cooling down, on
The super soft ultrafine wire of low aberration polyester fiber is made in oil and high-speed winding.
A kind of 4. preparation method of the super soft ultrafine wire of low aberration polyester according to claim 3, which is characterized in that main technique bag
It includes：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and cathode is graphite；It is logical
Direct current, 6~10V of starting voltage, cathode-current density are 150~200mA, when electrolysis 10~12 is small at 50~60 DEG C, electrolysis
After take out electrode, obtain white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, and ethylene glycol is obtained after dry
Magnesium；
(2) preparation of polyester, including esterification and polycondensation reaction：
The esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, anti-ether agent is added in, esterification is carried out after being made into uniform sizing material, obtains
Esterification products；Esterification is pressurizeed in nitrogen atmosphere, and pressure control is in normal pressure~0.3MPa, and temperature is at 250~260 DEG C, ester
Change water quantity of distillate and reach more than the 90% of theoretical value for esterification terminal；
The polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
The polycondensation reaction low vacuum stage adds in catalyst and stabilizer in esterification products, starts under conditions of negative pressure
Polycondensation reaction, the staged pressure are steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature is controlled at 260~270 DEG C, reaction
Time is 30~50 minutes；The catalyst is ethylene glycol magnesium and the mixture of antimony glycol；
The polycondensation reaction high vacuum stage of Fig after the polycondensation reaction low vacuum stage, continues to vacuumize, drops reaction pressure
It is less than 100Pa to absolute pressure, reaction temperature control is at 275~280 DEG C, 50~90 minutes reaction time；
Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
The polyester slice is through water and dissolves and washes away agent when brew 3-5 is small under the conditions of 120~130 DEG C with 0.2~0.3MPa, by washing
It washs to obtain polyester；
(4) spinning main technologic parameters：
The temperature of the extrusion is 290~295 DEG C；
The wind-warm syndrome of the cooling is 20~25 DEG C；
HT1：75-95℃；
HT2：120-130℃；
The high-speed winding speed is 4000~5000m/min.
A kind of 5. preparation method of the super soft ultrafine wire of low aberration polyester according to claim 3 or 4, which is characterized in that institute
The molar ratio for stating ethylene glycol and the terephthalic acid (TPA) is 1.2~2.0:1.
A kind of 6. preparation method of the super soft ultrafine wire of low aberration polyester according to claim 4, which is characterized in that the second
In the mixture of two magnesium alkoxides and antimony glycol, ethylene glycol magnesium is 2~3 with antimony glycol mass ratio:1；The catalyst amount is
The 0.01%~0.05% of the terephthalic acid (TPA) quality；The stabilizer is selected from triphenyl phosphate, trimethyl phosphate and phosphorous
One kind in sour trimethyl, stabilizing agent dosage are the 0.01%~0.05% of the terephthalic acid (TPA) weight.
A kind of 7. preparation method of the super soft ultrafine wire of low aberration polyester according to claim 4, which is characterized in that the water
Mass ratio with dissolveing and washing away agent is 100:3~4, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio is 1:5~10；Institute
It states and dissolves and washes away agent as one kind in ethylene glycol monoethyl ether, propyl cellosolve and ethylene glycol monobutyl ether (EGMBE).
8. the preparation method of the super soft ultrafine wire of a kind of low aberration polyester according to claim 4, which is characterized in that described to wash
It washs and refers to 70~80 DEG C of 10~15min of hot water wash of polyester slice after brew, then cleaned with cold water, Drying and cooling is spare.
9. the preparation method of the super soft ultrafine wire of a kind of low aberration polyester according to claim 4, which is characterized in that described anti-
Ether agent is one kind in sodium acetate and calcium acetate, and anti-ether agent dosage is the 0.01%~0.05% of the terephthalic acid (TPA) weight.
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