CN104480567B - A kind of Wool-Like abnormal contraction composite filament and preparation method thereof - Google Patents
A kind of Wool-Like abnormal contraction composite filament and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Wool-Like abnormal contraction composite filament and preparation method thereof, described Wool-Like abnormal contraction composite filament is the composite filament of modified poly ester POY silk fibre mixed with modified poly ester FDY silk warp processing composition；Described modified poly ester is to be made up of with amino ethylene glycol fatty acid polyester, described amino ethylene glycol fatty acid is dispersed in the molecule interchain of described polyester, and the molecule interchain of described amino ethylene glycol fatty acid and described polyester has hydrogen bond action, described amino ethylene glycol fatty acid is made to fix with the relative position of the strand of described polyester；Described Wool-Like abnormal contraction composite filament is under the conditions of temperature is 90～130 DEG C, and the free volume space of fibrous inside molecule interchain increases 20～30v/v%.Fatty acid ester adds the free volume diffusion with increase dyestuff of polyester fiber, improves the dyeability of polyester fiber.Described Wool-Like abnormal contraction composite filament can use garment material, bedding adornment etc..
Description
Technical field
The invention belongs to fibre manufacturing technology field, relate to a kind of Wool-Like abnormal contraction composite filament and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) fiber, since coming out, has obtained rapidly because of the performance of its excellence
Development, its yield has become as the hat of world's synthetic fibers.Polyester fiber has fracture strength and elastic modelling quantity is high, and resilience is fitted
In, thermal finalization is excellent, and heat-resisting light resistance is good and a series of premium properties such as acid-fast alkali-proof corrosion resistance, and fabric has anti-
The advantages such as wrinkle, stiffness are good, so, polyester fiber is widely used in the field such as clothing, home textile.
PET belongs to symmetric straight chain macromolecular, and strand does not contains side-chain radical, and regularity is the best, its main chain
Phenyl ring containing rigidity and flexible alkyl, and the ester group being directly connected with phenyl ring and phenyl ring constitute the conjugated body of rigidity
System, thus constrain rotating freely of its soft segment.This structure is it will be evident that increase on the impact of glass transition temperature
The wall ridge of molecule segment motion, the glass transition temperature of PET is higher, need to dye at very high temperatures, promotes dyestuff
Molecule is to the diffusion of fibrous inside.It addition, the strand of PET is regular, good crystallinity, strand arrangement is tight, and strand
The upper polar group not having an effect with dye molecule, the colouring making polyester fiber is more difficult.
For the problem of solution PET dyeing difficulty, techniques or methods are now used mainly to be connect by introducing dye molecule
By base or the method for increase polyester amorphous regions amount, although the dyeability of polyester can be improved, destroy the segment rule of PET
Whole property, to reduce the performance of polyester fiber to obtain the raising of dyeability.Do not destroying polyester fiber crystallinity and permutation degree
In the case of, the method used at present has three kinds of colouring methods such as support methods, high temperature and high pressure method and high temperature thermosoling.
Wool-Like abnormal contraction composite filament is the long filament with different potential shrinkage, i.e. high-shrinkage filament POY and lower shrinkage
Silk FDY is through the composite filament of mixed fibre processing composition, the main feature of PET different contraction mixed fiber composite silk: high loft and soft hands
Sense.PET Wool-Like abnormal contraction composite filament outer existing the most similar with common long filament.Due to the difference of two component shrinkage factors, thermally treated
After, high convergency part forms clear-cut core filaments, becomes the skeleton of silk, and lower shrinkage part forms tiny wire ring and is wound on core filaments
Around, it is exactly like textured filament in appearance.Gloss is soft.Many due to the bulk and surface of PET Wool-Like abnormal contraction composite filament
Wire ring, eliminates the aurora defect of chemical fiber wire fabric.Excellent warmth retention property.The high loft of PET different contraction mixed fiber composite silk, increases
Space between big fiber.The air content in PET different contraction mixed fiber composite silk fabrics is caused to increase.
Summary of the invention
It is an object of the invention to provide a kind of Wool-Like abnormal contraction composite filament and preparation method thereof, the present invention utilizes aminolipid
Fat acid glycol ester is when uniform temperature condition, and the increasing degree of free volume is far longer than the characteristic of polyester macromolecule chain, logical
Cross the degree improving the entrance of disperse dyes molecule within polyester, improve the dyeability of polyester；Simultaneously because aminolipid
In the existence of the first amino in fat acid glycol ester molecule, increase the hydrogen bond action between itself and polyester macromolecule chain, add
Its compatibility with polyester and dispersion in the polyester, decrease migration to greatest extent.Simultaneously to polyester construction regularity,
Crystallinity is not destroyed, and maintains the premium properties of polyester.
A kind of Wool-Like abnormal contraction composite filament of the present invention, described Wool-Like abnormal contraction composite filament is modified poly ester POY silk
The composite filament formed through mixed fibre processing with modified poly ester FDY silk, described modified poly ester POY silk forms tiny wire ring and is centered around described
Around modified poly ester FDY silk；Described modified poly ester is made up of with amino ethylene glycol fatty acid polyester, described amino fatty acid second
Diol ester is dispersed in the molecule interchain of described polyester, and the molecule interchain of described amino ethylene glycol fatty acid and described polyester has
Hydrogen bond action, makes described amino ethylene glycol fatty acid fix with the relative position of the strand of described polyester；Described Wool-Like
Abnormal contraction composite filament under the conditions of temperature is 90～130 DEG C, the free volume space of fibrous inside molecule interchain increase 20～
30v/v%；Fracture strength >=the 2.1cN/dtex of described Wool-Like abnormal contraction composite filament, elongation at break is 15.0 ± 2.0%,
Crimp contraction is 2.50 ± 3.0%, and internet pricing is 90 ± 5/m.
The molecular structure of described amino ethylene glycol fatty acid is:
H2N(CH2)nCOOCH2CH2OOC(CH2)nNH2；
Wherein, n=10-50.
As preferred technical scheme:
Described a kind of Wool-Like abnormal contraction composite filament, described amino ethylene glycol fatty acid accounts for the different contraction of described Wool-Like
The percentage by weight of composite filament is 0.5～2.5%.
Described a kind of Wool-Like abnormal contraction composite filament, the line density deviation ratio of described Wool-Like abnormal contraction composite filament ±
2.5%, fracture strength CV value≤5.0%, extension at break CV value≤10.0%, boiling water shrinkage is 5.0 ± 1.0%, and curling is received
Shrinkage coefficient of variation CV value≤10.0%, oil content is 1.0 ± 0.2%, fiber number: 150-300dtex.Modified poly ester POY silk
Line density deviation ratio≤0.2%, fracture strength >=2.6cN/dtex, fracture strength CV value≤3.0%, elongation at break is 90.0
± 10.0%, extension at break CV value≤6.0%.；Line density deviation ratio≤0.5% of modified poly ester FDY silk, fracture strength >=
3.8cN/dtex, fracture strength CV value≤5.0%, elongation at break is 33.0 ± 3.0%, extension at break CV value≤10.0%,
Yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ± 0.20%.
Present invention also offers the preparation method of a kind of Wool-Like abnormal contraction composite filament, by polyester through metering, extrusion, cold
But, oil and wind, preparing POY silk,；By polyester slice through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, system
Obtain FDY silk；POY silk and FDY through plying network, adding hot-stretch, false twisting, thermal finalization and coiling and molding, to prepare the different contraction of Wool-Like multiple
Plying:
Modified poly ester POY yarn spinning technique:
Spinning temperature: 2860-290 DEG C；
Chilling temperature: 18-22 DEG C；
Winding speed: 3200-3600m/min；
Modified poly ester FDY yarn spinning technique:
Spinning temperature: 2860-290 DEG C；
Chilling 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 speed: 3600-3900m/min；
Two roll temperatures: 115-135 DEG C；
Winding speed: 3600-3800m/min；
Composite filament processing technique:
Spin speed 400-800m/min；
Sizing over feed rate(OFR) 3.5-5.50%；
Winding over feed rate(OFR) 2.5-5.0；
T1:180-220 DEG C；
T2:150-180 DEG C；
DR:1.6-1.8；
D/Y:1.6-2.0；
Network pressure: 0.05-0.3MPa；
Low heat setting temperature in the low elongation at break of POY, chilling temperature on the low side and the DTY course of processing is big fine
The imitative linen look abnormal contraction composite filament of degree provides technical support
The preparation process of described modified poly ester includes:
(1) preparation of amino ethylene glycol fatty acid:
1) binary of fatty acids is added in reactor with the amount of 1:1.5 mol ratio with methanol, under the catalysis of concentrated sulphuric acid, add
Heat is to 80～110 DEG C, and refuxing esterification, cooling, separating-purifying obtains binary of fatty acids mono-methyl；Described binary of fatty acids is 12
Alkane dicarboxylic acids is to the one in dopentacontane dicarboxylic acids；Reaction equation is:
HOOC(CH2)nCOOH+CH3OH→CH3OOC(CH2)NCOOH；
Wherein n=10～50
2) by described binary of fatty acids mono-methyl, lead tetraacetate and lithium bromide during 1:1:1 is dissolved in benzene in molar ratio, wherein two
The concentration of unit's fatty acid mono-methyl is 0.05～0.1mol/L, and under nitrogen atmosphere, 80～90 DEG C of reactions, backflow, when no longer
When having gas to produce, add a certain amount of dilute sulfuric acid and react 2～3 hours, be washed out, purify and be dried, obtain product bromo
Fatty acid；Reaction equation is:
3), by the ammonia of bromo fatty acid and 15～25wt% during 1:2 joins reactor in molar ratio, stirring, in room temperature
Lower reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is less than 70 DEG C, until nothing
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, by product
Vacuum drying obtains product amino fatty acid；Vacuum drying temperature can use 60～70 DEG C；Reaction equation is:
HOOC(CH2)nBr+NH3→HOOC(CH2)nNH2+NH4Br；
4) ethylene glycol and amino fatty acid are stirred for 1.1:2 in molar ratio, and press the hundred of amino fatty acid wt
/ mono-add concentration be 40～50wt% sulphuric acid be catalyst, carry out esterification, esterification reaction temperature is 160～220
DEG C, it is esterification terminal that esterification water quantity of distillate reaches more than the 90% of theoretical value；The separated purification of product obtains amino
Ethylene glycol fatty acid；Reaction equation is:
HOOC(CH2)nNH2+HOCH2CH2OH→
H2N(CH2)nCOOCH2CH2OOC(CH2)nNH2；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
Use p-phthalic acid and ethylene glycol as raw material, after being made into uniform sizing material, carry out esterification, obtain esterification and produce
Thing；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at normal pressure～0.3MPa, and temperature is at 250～260 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction coarse vacuum stage, esterification products adds catalyst and stabilizer, under conditions of negative pressure
Starting polycondensation reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature controls at 260～270 DEG C,
Response time is 30～50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino ethylene glycol fatty acid, and stir, generally stir
15～20 minutes；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275～280 DEG C, response time 50～90 minutes；
Prepare modified poly ester；
The preparation method of a kind of Wool-Like abnormal contraction composite filament as above, described ethylene glycol and described p-phthalic acid
Mol ratio be 1.2～2.0:1.
The preparation method of a kind of Wool-Like abnormal contraction composite filament as above, described catalyst selected from antimony oxide,
One in antimony glycol and antimony acetate, catalyst amount is the 0.01%～0.05% of described p-phthalic acid weight.
The preparation method of a kind of Wool-Like abnormal contraction composite filament as above, described stabilizer selected from triphenyl phosphate,
One in trimethyl phosphate and NSC 6513, stabilizing agent dosage be described p-phthalic acid weight 0.01%～
0.05%.
The preparation method of a kind of Wool-Like abnormal contraction composite filament as above, is washed with deionized water to without bromide ion
Employing silver nitrate solution detects.
The preparation method of a kind of Wool-Like abnormal contraction composite filament as above, described concentrated sulphuric acid refers to that mass concentration is 70
～the sulphuric acid of 80%, concentrated sulphuric acid addition is the 1～3wt% of binary of fatty acids；Described a certain amount of dilute sulfuric acid refers to that quality is dense
Degree is the sulphuric acid of 40～50%, and dilute sulfuric acid addition is the 1～3wt% of binary of fatty acids mono-methyl.
Polyester fiber is when dyeing, and the upper dye process of polyester fiber can be divided into the next stage by disperse dyes:
1) disperse dyes flowing with dye liquor in dye liquor moves closer to fiber interface；2) disperse dyes are near fiber interface
Adsorbed by fiber surface rapidly；3), after disperse dyes are adsorbed to fiber surface, in fiber, a concentration difference or inside and outside is produced
Dyestuff chemistry potential difference, dyestuff will spread to fibrous inside；4) disperse dyes diffusion velocity and fiber unformed area content, hole or
Free volume content is relevant, and therefore the dyeing speed of disperse dyes is in addition to dyestuff dissolubility in the solution, further depends on
When the structure of fiber is outer and dyes, the degree of swelling of fiber is relevant.
Polyster fibre is hydrophobic synthetic fibers, lacks as cellulose or protein fibre in terylene molecular structure
Energy and dyestuff occur combine active group, terylene molecules align must compare closely, only exist less space in fiber,
When dyeing under the conditions of humidity, polyester fiber will not can be by the most swelling and make space increase as cotton fiber, dyestuff divides
Son is difficult to see through fibrous inside.Therefore, raising will assist in the carrying out of dyeing to the free volume between fiber molecule.
The molecular chain structure of polyester is the linear macromolecule containing benzene ring structure, the functional group's marshalling on strand,
Unbranched, macromole chain flexibility is poor.The regularity of polyester is good and rigidity is the biggest simultaneously, and intermolecular active force is bigger.
Compared with other macromolecular materials, the strand generation sliding of polyester, rotation the most more difficulty, these characteristics hinder dyestuff and enter
Enter inside polyester, thus dyeability is poor.
It is main that amino ethylene glycol fatty acid is mainly with C-C, C-O key, has certain molecular weight simultaneously, i.e. has certain
The strand of length, strand flexibility is relatively big, linear big compared with benzene ring structure of the amount of crimp of amino ethylene glycol fatty acid
Molecule is bigger, simultaneously strong compared with the linear macromolecule containing benzene ring structure to the sensitivity of temperature.When the temperature is changed, amino fatty acid
Glycol ester moves prior to the linear macromolecule containing benzene ring structure, and the produced free volume of motion is far longer than containing phenyl ring
Produced by the linear macromolecule of structure.
Added the free volume diffusion with increase dyestuff of polyester fiber by fatty acid ester, improve polyester fiber
Dyeability, make fiber obtain high dye-uptake.
Oxygen in fatty acid ester can form hydrogen bond, but oxygen is when centre position, due to space steric effect and fat
The factors such as the curling of fat acid ester molecules reduce the quantity of itself and the hydrogen evolution hydrogen bond in polyester macromolecule chain；If amino is in α position
On, i.e. amino acids, owing to amino and carbonyl interact, also it is unfavorable for amino and the hydrogen evolution hydrogen in polyester macromolecule chain
Key；When end position at macromole of the amino of amino fatty acid ester, the curling of macromole is little on its impact, adds aminolipid
Amino in fat acid esters and the formation of the hydrogen evolution hydrogen bond in polyester macromolecule chain, improve amino fatty acid ester and polyester simultaneously
Active force between macromolecular chain, decreases sliding and the migration of amino fatty acid ester.
Add amino fatty acid ester and the compatibility of polyester and dispersion in the polyester, decrease to greatest extent and move
Move.Polyester construction regularity, crystallinity are not destroyed simultaneously, maintain the premium properties of polyester.
Beneficial effect:
The Wool-Like abnormal contraction composite filament of gained the most of the present invention, owing to amino ethylene glycol fatty acid is based on C-C, with
Time there is certain molecular weight, i.e. there is the strand of certain length, strand flexibility is relatively big, and amino adds the phase with polyester
Capacitive.The fiber of gained is good with the compatibility of amino ethylene glycol fatty acid.
2. due in amino ethylene glycol fatty acid molecule in the existence of the first amino, increase and it and polyester macromolecule chain
Between hydrogen bond action, add its compatibility with polyester and dispersion in the polyester, decrease migration to greatest extent.
The Wool-Like abnormal contraction composite filament of gained the most of the present invention, owing to the content of amino ethylene glycol fatty acid is less, right
Polyester construction regularity, crystallinity are not destroyed, and maintain the premium properties of polyester.
4. the amount of crimp of amino ethylene glycol fatty acid is bigger, simultaneously to temperature compared with the linear macromolecule of benzene ring structure
Sensitive strong compared with the linear macromolecule containing benzene ring structure.When the temperature is changed, transport prior to the linear macromolecule containing benzene ring structure
Dynamic, the produced free volume of motion of amino ethylene glycol fatty acid is far longer than the linear macromolecule institute containing benzene ring structure
Produce, increase the diffusion of additive, improve the functional of polyester.
5. fatty acid ester adds the free volume diffusion with increase dyestuff of polyester fiber, improves polyester fiber
Dyeability.
Many wire rings on the bulk and surface of the Wool-Like abnormal contraction composite filament of gained the most of the present invention, eliminate chemical fiber wire
The aurora defect of fabric, has the warmth retention property of excellence, and the high loft of Wool-Like abnormal contraction composite filament, increases between fiber
Space.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate this
Bright rather than limit the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, art technology
The present invention can be made various changes or modifications by personnel, and these equivalent form of values fall within the application appended claims equally and limited
Fixed scope.
A kind of Wool-Like abnormal contraction composite filament of the present invention, adds through mixed fibre with modified poly ester FDY silk for modified poly ester POY silk
The composite filament of work composition, described modified poly ester POY silk forms tiny wire ring and is centered around around described modified poly ester FDY silk；Described
Modified poly ester is made up of with amino ethylene glycol fatty acid polyester, and described amino ethylene glycol fatty acid is dispersed in described polyester
Molecule interchain, and the molecule interchain of described amino ethylene glycol fatty acid and described polyester has hydrogen bond action, makes described aminolipid
Fat acid glycol ester is fixed with the relative position of the strand of described polyester；Described Wool-Like abnormal contraction composite filament is 90 in temperature
～under the conditions of 130 DEG C, the free volume space of fibrous inside molecule interchain increases 20～30v/v%；The different contraction of described Wool-Like
Fracture strength >=the 2.1cN/dtex of composite filament, elongation at break is 15.0 ± 2.0%, and crimp contraction is 2.50 ± 3.0%,
Internet pricing is 90 ± 5/m.
The molecular structure of described amino ethylene glycol fatty acid is:
H2N(CH2)nCOOCH2CH2OOC(CH2)nNH2；
Wherein, n=10-50.
Described a kind of Wool-Like abnormal contraction composite filament, described amino ethylene glycol fatty acid accounts for the different contraction of described Wool-Like
The percentage by weight of composite filament is 0.5～2.5%.
Described a kind of Wool-Like abnormal contraction composite filament, the line density deviation ratio of described Wool-Like abnormal contraction composite filament ±
2.5%, fracture strength CV value≤5.0%, extension at break CV value≤10.0%, boiling water shrinkage is 5.0 ± 1.0%, and curling is received
Shrinkage coefficient of variation CV value≤10.0%, oil content is 1.0 ± 0.2%, fiber number: 150-300dtex.Modified poly ester POY silk
Line density deviation ratio≤0.2%, fracture strength >=2.6cN/dtex, fracture strength CV value≤3.0%, elongation at break is 90.0
± 10.0%, extension at break CV value≤6.0%.；Line density deviation ratio≤0.5% of modified poly ester FDY silk, fracture strength >=
3.8cN/dtex, fracture strength CV value≤5.0%, elongation at break is 33.0 ± 3.0%, extension at break CV value≤10.0%,
Yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ± 0.20%.
Colouring method: dyeing disperse dyes are Disperse Red 3B, the disperse blue SE-2R bright blue S-GL of dispersion, fiber exists respectively
High Temperature High Pressure machine dyes.Before dye, fiber nonionic surfactant processes 30 minutes at 60 DEG C.Dye dosage is 2.0%
(o.w.f)；Dispersant NNO1.2g/L, pH value is 5, and bath raio is 1:50,60 DEG C of people dye, be warming up to 90 DEG C, 100 DEG C, 110 DEG C,
120 DEG C of each constant temperature dyeing 1h.
Dye uptake uses residual liquid colorimetry to determine, draws appropriate dyeing stock solution and dyeing residual liquid, adds N, N-2 first
Base Methanamide (DMF) and distilled water, be that the ratio of the DMF in dye liquor to be measured and water is 70/30 (v/v), and dye liquor absorbance uses
Ultraviolet-visible spectrophotometer measures, and calculates dye uptake with following formula.
In above formula, A0 and A1 is respectively dyeing stock solution and the absorbance of dyeing residual liquid.
Embodiment 1
The preparation method of a kind of Wool-Like abnormal contraction composite filament, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) dodecanedicarboxylic acid is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 80 DEG C, refuxing esterification, cooling, separating-purifying obtains dodecanedicarboxylic acid mono-methyl；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of dodecanedicarboxylic acid；
2) described dodecanedicarboxylic acid mono-methyl, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Dodecanedicarboxylic acid mono-methyl concentration is 0.05mol/L, under nitrogen atmosphere, in 80 DEG C of reactions, backflow, produces when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2 hours, be washed out, purify and be dried, obtain product bromoundecane carboxylic acid；
Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40%, and dilute sulfuric acid addition is dodecanedicarboxylic acid mono-methyl
3wt%；
3), by the ammonia of bromoundecane carboxylic acid Yu 15wt% during 1:2 joins reactor in molar ratio, stirring, in room temperature
Lower reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, uses silver nitrate
Solution detects, and product vacuum drying is obtained product amino-undecanoic carboxylic acid；
4) ethylene glycol and amino-undecanoic carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino-undecanoic carboxylic acid
1% addition concentration of weight is the sulphuric acid of 40wt%, carries out esterification, and esterification reaction temperature is 160 DEG C, esterification water quantity of distillate
Reaching more than the 90% of theoretical value is esterification terminal；The separated purification of product obtains amino-undecanoic carboxylic acid ethylene glycol
Ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.2 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.3MPa, and temperature is 250 DEG C, esterification
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, three oxidations of the 0.01% of addition p-phthalic acid weight in esterification products
Two antimony and the triphenyl phosphate of p-phthalic acid weight 0.01%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Steadily be evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 260 DEG C, and the response time is 50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino-undecanoic carboxylic acid glycol ester, and stir 15 points
Clock；
Described amino-undecanoic carboxylic acid glycol ester, addition is the 0.5wt% of modified poly ester；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 90 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 15000；
(3) preparation of Wool-Like abnormal contraction composite filament:
By modified poly ester through measuring, extrude, cool down, oil and winding, prepare modified poly ester POY silk；Modified poly ester POY silk
Spinning technique:
Spinning temperature: 280 DEG C；
Chilling temperature: 20 DEG C；
Winding speed: 3600m/min；
The line density deviation ratio 0.2% of modified poly ester POY silk, fracture strength 2.6cN/dtex, fracture strength CV value
2.9%, elongation at break is 100.0%, extension at break CV value 6.0%.
By polyester slice through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique:
Spinning temperature: 280 DEG C；
Chilling temperature: 20 DEG C；
Network pressure: 0.30MPa；
One roller speed: 2600m/min；
One roll temperature: 85 DEG C；
Two roller speed: 3900m/min；
Two roll temperatures: 135 DEG C；
Winding speed: 3800m/min；
The line density deviation ratio 0.5% of modified poly ester FDY silk, fracture strength 3.8cN/dtex, fracture strength CV value
5.0%, elongation at break is 36.0%, extension at break CV value 9.9%, yarn unevenness CV2.00%, boiling water shrinkage
8.0%, oil content 1.1%.
Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, add hot-stretch, false twisting, thermal finalization and volume
Wool-Like abnormal contraction composite filament is prepared around molding；
Composite filament processing technique:
Spin speed 800m/min；
Sizing over feed rate(OFR) 5.50%；
Winding over feed rate(OFR) 5.0；
T1:220 DEG C；
T2:180 DEG C；
DR:1.8；
D/Y:2.0；
Network pressure: 0.3MPa；
Gained Wool-Like abnormal contraction composite filament is under the conditions of temperature is 90 DEG C, and the free volume of fibrous inside molecule interchain is empty
Between increase 20v/v%, line density deviation ratio 2.5%, fracture strength 2.1cN/dtex, fracture strength CV value 5.0%, extension at break
Rate is 17.0%, extension at break CV value 10.0%, and boiling water shrinkage is 6.0%, and crimp contraction is 5.5%, crimp contraction
Coefficient of variation CV value 10.0%, oil content is 1.2%, and internet pricing is 100/m, fiber number: 300dtex.
After described Wool-Like abnormal contraction composite filament is dyeed, it is thus achieved that dye uptake as shown in the table:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 51.2 | 83.8 | 92.2 | 93.0 | 92.6 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 53.9 | 88.3 | 93.0 | 93.8 | 94.6 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 46.9 | 75.0 | 87.7 | 88.9 | 91.2 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 2
The preparation method of a kind of Wool-Like abnormal contraction composite filament, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) dopentacontane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, in the catalysis of concentrated sulphuric acid
Under, it being heated to 110 DEG C, refuxing esterification, cooling, separating-purifying obtains dopentacontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to
Mass concentration is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of dopentacontane dicarboxylic acids；
2) described dopentacontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), its
Middle dopentacontane mono methyl dicarboxylate's concentration is 0.07mol/L, and under nitrogen atmosphere, 85 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 3 hours, be washed out, purify and be dried, obtain product bromo henpentacontane
Carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40%, and dilute sulfuric acid addition is dopentacontane dicarboxylic acids
The 3wt% of mono-methyl；
3), by the ammonia of bromo henpentacontane carboxylic acid Yu 25wt% during 1:2 joins reactor in molar ratio, stirring, in room
The lower reaction of temperature, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 62 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses nitric acid
Silver solution detection, obtains product amino henpentacontane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino henpentacontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino henpentacontane
2% addition concentration of carboxylic acid weight is the sulphuric acid of 45wt%, carries out esterification, and esterification reaction temperature is 220 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；The separated purification of product obtains amino henpentacontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:2.0 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.2MPa, and temperature, at 260 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, three oxidations of the 0.05% of addition p-phthalic acid weight in esterification products
Two antimony and the triphenyl phosphate of p-phthalic acid weight 0.05%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Steadily be evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 270 DEG C, and the response time is 30 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino henpentacontane carboxylic acid glycol ester, and stir 20 points
Clock；
Described amino henpentacontane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 2.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 280 DEG C, 50 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 30000；
(3) preparation of Wool-Like abnormal contraction composite filament:
By modified poly ester through measuring, extrude, cool down, oil and winding, prepare modified poly ester POY silk；
Modified poly ester POY yarn spinning technique:
Spinning temperature: 290 DEG C；
Chilling temperature: 20 DEG C；
Winding speed: 3150m/min；
The line density deviation ratio 0.19% of modified poly ester POY silk, fracture strength 2.7cN/dtex, fracture strength CV value
2.9%, elongation at break is 90.0%, extension at break CV value 5.9%；
By polyester slice through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique:
Spinning temperature: 290 DEG C；
Chilling temperature: 25 DEG C；
Network pressure: 0.20MPa；
One roller speed: 2200m/min；
One roll temperature: 75 DEG C；
Two roller speed: 3600m/min；
Two roll temperatures: 115 DEG C；
Winding speed: 3600m/min；
The line density deviation ratio 0.4% of modified poly ester FDY silk, fracture strength 3.9cN/dtex, fracture strength CV value
4.9%, elongation at break is 30.0%, extension at break CV value 9.8%, yarn unevenness CV1.95%, boiling water shrinkage
7.0%, oil content 0.70%；
Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, add hot-stretch, false twisting, thermal finalization and volume
Wool-Like abnormal contraction composite filament is prepared around molding；
Composite filament processing technique:
Spin speed 400m/min；
Sizing over feed rate(OFR) 3.5%；
Winding over feed rate(OFR) 2.5；
T1:190 DEG C；
T2:150 DEG C；
DR:1.6；
D/Y:1.6；
Network pressure: 0.05MPa；
Gained Wool-Like abnormal contraction composite filament under the conditions of temperature is 130 DEG C, the free volume space of interior molecules interchain
Increase 30v/v%, line density deviation ratio-2.5%, fracture strength 2.2cN/dtex, fracture strength CV value 4.9%, extension at break
Rate is 13.0%, extension at break CV value 9.9%, and boiling water shrinkage is 4.0%, and crimp contraction is-0.5%, crimp contraction
Coefficient of variation CV value 9.0%, oil content is 0.8%, and internet pricing is 85/m, fiber number: 150-300dtex.
After described Wool-Like abnormal contraction composite filament is dyeed, it is thus achieved that dye uptake as shown in the table:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 51.4 | 84.3 | 92.6 | 93.1 | 92.8 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 54.0 | 88.8 | 93.4 | 93.9 | 94.9 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 47.2 | 75.4 | 88.1 | 89.3 | 91.7 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 3
The preparation method of a kind of Wool-Like abnormal contraction composite filament, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) pentacosane dicarboxylic acid is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 85 DEG C, refuxing esterification, cooling, separating-purifying obtains pentacosane dicarboxylic acid mono-methyl；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of pentacosane dicarboxylic acid；
2) described pentacosane dicarboxylic acid mono-methyl, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Pentacosane dicarboxylic acid mono-methyl concentration is 0.08mol/L, under nitrogen atmosphere, in 90 DEG C of reactions, backflow, produces when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.5 hours, be washed out, purify and be dried, obtain product bromotetradecane carboxylic
Acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 50%, and dilute sulfuric acid addition is pentacosane dicarboxylic acid list first
The 3wt% of ester；
3), by the ammonia of bromotetradecane carboxylic acid Yu 20wt% during 1:2 joins reactor in molar ratio, stirring, in room temperature
Lower reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, uses silver nitrate
Solution detects, and product vacuum drying is obtained product amino tetradecane carboxylic acid；
4) ethylene glycol and amino tetradecane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino tetradecane carboxylic acid
2% addition concentration of weight is the sulphuric acid of 50wt%, carries out esterification, and esterification reaction temperature is 190 DEG C, esterification water quantity of distillate
Reaching more than the 90% of theoretical value is esterification terminal；The separated purification of product obtains amino tetradecane carboxylic acid ethylene glycol
Ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.6 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.3MPa, and temperature, at 255 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, three oxidations of the 0.03% of addition p-phthalic acid weight in esterification products
Two antimony and the triphenyl phosphate of p-phthalic acid weight 0.03%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Steadily be evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 265 DEG C, and the response time is 40 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino tetradecane carboxylic acid glycol ester, and stir 16 points
Clock；
Described amino tetradecane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 1.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 276 DEG C, 70 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 22500；
(3) preparation of Wool-Like abnormal contraction composite filament:
By modified poly ester through measuring, extrude, cool down, oil and winding, prepare modified poly ester POY silk；
Modified poly ester POY yarn spinning technique:
Spinning temperature: 286 DEG C；
Chilling temperature: 22 DEG C；
Winding speed: 3100m/min；
The line density deviation ratio 1.8% of modified poly ester POY silk, fracture strength 2.9cN/dtex, fracture strength CV value
2.7%, elongation at break is 100.0%, extension at break CV value 5.6%；
By polyester slice through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique:
Spinning temperature: 286 DEG C；
Chilling temperature: 22 DEG C；
Network pressure: 0.25MPa；
One roller speed: 2400m/min；
One roll temperature: 80 DEG C；
Two roller speed: 3750m/min；
Two roll temperatures: 125 DEG C；
Winding speed: 3700m/min；
The line density deviation ratio 0.43% of modified poly ester FDY silk, fracture strength 4.0cN/dtex, fracture strength CV value
4.8%, elongation at break is 33.0%, extension at break CV value 9.8%, yarn unevenness CV≤1.96%, boiling water shrinkage
7.5%, oil content 0.90%.
Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, add hot-stretch, false twisting, thermal finalization and volume
Wool-Like abnormal contraction composite filament is prepared around molding；
Composite filament processing technique:
Spin speed 600m/min；
Sizing over feed rate(OFR) 4.0%；
Winding over feed rate(OFR) 3.0；
T1:200 DEG C；
T2:180 DEG C；
DR:1.7；
D/Y:1.8；
Network pressure: 0.15MPa；
Gained Wool-Like abnormal contraction composite filament under the conditions of temperature is 100 DEG C, the free volume space of interior molecules interchain
Increase 20v/v%, line density deviation ratio 1.5%, fracture strength 2.5cN/dtex, fracture strength CV value 4.5%, elongation at break
Being 16.0%, extension at break CV value 9.6%, boiling water shrinkage is 5.5%, and crimp contraction is 4.5%, and crimp contraction makes a variation
Coefficient CV value 9.3%, oil content is 1.2%, and internet pricing is 91/m, fiber number: 180dtex.
After described Wool-Like abnormal contraction composite filament is dyeed, it is thus achieved that dye uptake as shown in the table:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 51.5 | 84.2 | 92.0 | 92.8 | 92.0 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 54.6 | 89.5 | 92.6 | 93.6 | 94.1 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 45.6 | 75.5 | 87.5 | 88.4 | 90.6 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 4
The preparation method of a kind of Wool-Like abnormal contraction composite filament, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) eicosane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 85 DEG C, refuxing esterification, cooling, separating-purifying obtains eicosane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of eicosane dicarboxylic acids；
2) described eicosane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Eicosane mono methyl dicarboxylate's concentration is 0.09mol/L, under nitrogen atmosphere, in 80 DEG C of reactions, backflow, produces when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.1 hours, be washed out, purify and be dried, obtain product bromo nonadecane carboxylic
Acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 43%, and dilute sulfuric acid addition is eicosane dicarboxylic acids list first
The 2wt% of ester；
3), by the ammonia of bromo nonadecane carboxylic acid Yu 16wt% during 1:2 joins reactor in molar ratio, stirring, in room temperature
Lower reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 69 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, uses silver nitrate
Solution detects, and product vacuum drying is obtained product amino nonadecane carboxylic acid；
4) ethylene glycol and amino nonadecane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino nonadecane carboxylic acid
2% addition concentration of weight is the sulphuric acid of 42wt%, carries out esterification, and esterification reaction temperature is 160 DEG C, esterification water quantity of distillate
Reaching more than the 90% of theoretical value is esterification terminal；The separated purification of product obtains amino nonadecane carboxylic acid ethylene glycol
Ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.2 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.15MPa, and temperature, at 251 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, three oxidations of the 0.02% of addition p-phthalic acid weight in esterification products
Two antimony and the triphenyl phosphate of p-phthalic acid weight 0.02%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Steadily be evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 262 DEG C, and the response time is 33 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino nonadecane carboxylic acid glycol ester, and stir 17 points
Clock；
Described amino nonadecane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 1.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 277 DEG C, 55 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 16000；
(3) preparation of Wool-Like abnormal contraction composite filament:
By modified poly ester through measuring, extrude, cool down, oil and winding, prepare modified poly ester POY silk；
Modified poly ester POY yarn spinning technique:
Spinning temperature: 287 DEG C；
Chilling temperature: 21 DEG C；
Winding speed: 3500m/min；
The line density deviation ratio 0.17% of modified poly ester POY silk, fracture strength 2.7cN/dtex, fracture strength CV value
2.6%, elongation at break is 80.0%, extension at break CV value 5.6%；
By polyester slice through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique:
Spinning temperature: 287 DEG C；
Chilling temperature: 21 DEG C；
Network pressure: 0.21MPa；
One roller speed: 2300m/min；
One roll temperature: 76 DEG C；
Two roller speed: 3650m/min；
Two roll temperatures: 117 DEG C；
Winding speed: 3650m/min；
The line density deviation ratio 0.45% of modified poly ester FDY silk, fracture strength 4.1cN/dtex, fracture strength CV value
4.4%, elongation at break is 35.0%, extension at break CV value 9.2%, yarn unevenness CV1.99%, boiling water shrinkage
7.9%, oil content 0.95%；
Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, add hot-stretch, false twisting, thermal finalization and volume
Wool-Like abnormal contraction composite filament is prepared around molding；
Composite filament processing technique:
Spin speed 500m/min；
Sizing over feed rate(OFR) 4.0%；
Winding over feed rate(OFR) 4.0；
T1:190 DEG C；
T2:160 DEG C；
DR:1.6；
D/Y:1.7；
Network pressure: 0.25MPa；
Gained Wool-Like abnormal contraction composite filament under the conditions of temperature is 105 DEG C, the free volume of fibrous inside molecule interchain
Space increases 21v/v%, and line density deviation ratio 1.0%, fracture strength 2.6cN/dtex, fracture strength CV value 4.3%, fracture is stretched
Long rate is 14.0%, extension at break CV value 9.4%, and boiling water shrinkage is 4.5%, and crimp contraction is 0.5%, crimp contraction
Coefficient of variation CV value 9.9%, oil content is 1.0%, and internet pricing is 88/m, fiber number: 250dtex.
After described Wool-Like abnormal contraction composite filament is dyeed, it is thus achieved that dye uptake as shown in the table:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 51.5 | 84.3 | 92.6 | 93.4 | 92.8 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 54.6 | 88.5 | 934 | 94.3 | 94.9 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 46.5 | 74.8 | 87.5 | 88.4 | 91.0 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 5
The preparation method of a kind of Wool-Like abnormal contraction composite filament, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) melissane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 90 DEG C, refuxing esterification, cooling, separating-purifying obtains melissane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of melissane dicarboxylic acids；
2) described melissane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Melissane mono methyl dicarboxylate's concentration be 0.10mol/L under nitrogen atmosphere, 85 DEG C of reactions, backflow, produce when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.3 hours, be washed out, purify and be dried, obtain product bromo nonacosane carboxylic
Acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40%, and dilute sulfuric acid addition is melissane dicarboxylic acids list first
The 3wt% of ester；
3), by the ammonia of bromo nonacosane carboxylic acid Yu 18wt% during 1:2 joins reactor in molar ratio, stirring, in room
The lower reaction of temperature, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 67 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses nitric acid
Silver solution detection, obtains product amino nonacosane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino nonacosane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino nonacosane
2% addition concentration of carboxylic acid weight is the sulphuric acid of 48wt%, carries out esterification, and esterification reaction temperature is 170 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；The separated purification of product obtains amino nonacosane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.5 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.3MPa, and temperature, at 254 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, the ethylene glycol of the 0.01% of addition p-phthalic acid weight in esterification products
Antimony and the trimethyl phosphate of p-phthalic acid weight 0.03%, under conditions of negative pressure start polycondensation reaction, this staged pressure by
Normal pressure is steadily evacuated to below absolute pressure 500Pa, and temperature controls at 266 DEG C, and the response time is 39 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino nonacosane carboxylic acid glycol ester, and stir 18 points
Clock；
Described amino nonacosane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 2.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 278 DEG C, 60 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 22000；
(3) preparation of Wool-Like abnormal contraction composite filament:
By modified poly ester through measuring, extrude, cool down, oil and winding, prepare modified poly ester POY silk；
Modified poly ester POY yarn spinning technique:
Spinning temperature: 285 DEG C；
Chilling temperature: 21 DEG C；
Winding speed: 3300m/min；
The line density deviation ratio 0.15% of modified poly ester POY silk, fracture strength 3.0cN/dtex, fracture strength CV value
2.9%, elongation at break is 98.0%, extension at break CV value 5.5%；
By polyester slice through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique:
Spinning temperature: 285 DEG C；
Chilling temperature: 23 DEG C；
Network pressure: 0.22MPa；
One roller speed: 2400m/min；
One roll temperature: 77 DEG C；
Two roller speed: 3800m/min；
Two roll temperatures: 119 DEG C；
Winding speed: 3750m/min；
The line density deviation ratio 0.44% of modified poly ester FDY silk, fracture strength 4.2cN/dtex, fracture strength CV value
4.3%, elongation at break is 34.0%, extension at break CV value 9.3%, yarn unevenness CV1.85%, boiling water shrinkage
7.8%, oil content 0.99%.
Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, add hot-stretch, false twisting, thermal finalization and volume
Wool-Like abnormal contraction composite filament is prepared around molding；
Composite filament processing technique:
Spin speed 700m/min；
Sizing over feed rate(OFR)-5.0%；
Winding is owed to feed rate 5.0；
T1:210 DEG C；
T2:170 DEG C；
DR:1.7；
D/Y:1.9；
Network pressure: 0.28MPa；
Gained Wool-Like abnormal contraction composite filament is under the conditions of temperature is 95 DEG C, and the free volume of fibrous inside molecule interchain is empty
Between increase 22v/v%, line density deviation ratio-1.0%, fracture strength 2.7cN/dtex, fracture strength CV value 4.4%, fracture is stretched
Long rate is 15.5%, extension at break CV value 9.2%, and boiling water shrinkage is 4.0%, and crimp contraction is 1.8%, crimp contraction
Coefficient of variation CV value 9.5%, oil content is 1.2%, and internet pricing is 94/m, fiber number: 260dtex.
After described Wool-Like abnormal contraction composite filament is dyeed, it is thus achieved that dye uptake as shown in the table:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 51.0 | 83.5 | 91.8 | 92.5 | 92.5 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 53.4 | 88.0 | 92.8 | 93.5 | 94.4 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 47.3 | 75.4 | 88.1 | 89.5 | 91.5 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 6
The preparation method of a kind of Wool-Like abnormal contraction composite filament, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) pentatriacontane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, in the catalysis of concentrated sulphuric acid
Under, it being heated to 95 DEG C, refuxing esterification, cooling, separating-purifying obtains pentatriacontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to matter
Amount concentration is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 2wt% of pentatriacontane dicarboxylic acids；
2) described pentatriacontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), its
Middle pentatriacontane mono methyl dicarboxylate's concentration be 0.09mol/L under nitrogen atmosphere, 90 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 2.6 hours, be washed out, purify and be dried, obtain product bromo 34
Alkane carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 45%, and dilute sulfuric acid addition is pentatriacontane dicarboxyl
The 1wt% of acid mono-methyl
3), by the ammonia of bromo tetratriacontane carboxylic acid Yu 20wt% during 1:2 joins reactor in molar ratio, stirring, in room
The lower reaction of temperature, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 69 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses nitric acid
Silver solution detection, obtains product amino tetratriacontane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino tetratriacontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino tetratriacontane
1% addition concentration of carboxylic acid weight is the sulphuric acid of 50wt%, carries out esterification, and esterification reaction temperature is 180 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；The separated purification of product obtains amino tetratriacontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.6 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.4MPa, and temperature, at 256 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, the antimony acetate of the 0.04% of addition p-phthalic acid weight in esterification products
With the NSC 6513 of p-phthalic acid weight 0.02%, under conditions of negative pressure start polycondensation reaction, this staged pressure by
Normal pressure is steadily evacuated to below absolute pressure 500Pa, and temperature controls at 267 DEG C, and the response time is 40 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino tetratriacontane carboxylic acid glycol ester, and stir 18 points
Clock；
Described amino tetratriacontane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 2.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 70 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 24000；
(3) preparation of Wool-Like abnormal contraction composite filament:
By modified poly ester through measuring, extrude, cool down, oil and winding, prepare modified poly ester POY silk；
Modified poly ester POY yarn spinning technique:
Spinning temperature: 287 DEG C；
Chilling temperature: 20 DEG C；
Winding speed: 3250m/min；
The line density deviation ratio 0.18% of modified poly ester POY silk, fracture strength 3.0cN/dtex, fracture strength CV value
3.1%, elongation at break is 95.0%, extension at break CV value 5.7%；
By polyester slice through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique:
Spinning temperature: 285 DEG C；
Chilling temperature: 21 DEG C
Network pressure: 0.20MPa；
One roller speed: 2600m/min；
One roll temperature: 77 DEG C
Two roller speed: 3800m/min；
Two roll temperatures: 120 DEG C；
Winding speed: 3700m/min；
The line density deviation ratio 0.44% of modified poly ester FDY silk, fracture strength 3.8cN/dtex, fracture strength CV value
4.8%, elongation at break is 36.0%, extension at break CV value 9.7%, yarn unevenness CV1.89%, boiling water shrinkage
7.7%, oil content 0.90%.
Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, add hot-stretch, false twisting, thermal finalization and volume
Wool-Like abnormal contraction composite filament is prepared around molding；
Composite filament processing technique:
Spin speed 800m/min；
Sizing over feed rate(OFR) 3.50%；
Winding is owed to feed rate 3.5；
T1:220 DEG C；
T2:170 DEG C；
DR:1.6；
D/Y:2.0；
Network pressure: 0.20MPa；
Gained Wool-Like abnormal contraction composite filament under the conditions of temperature is 110 DEG C, the free volume space of interior molecules interchain
Increase 24v/v%, line density deviation ratio 2.5%, fracture strength 2.3cN/dtex, fracture strength CV value 4.8%, elongation at break
Being 15.0%, extension at break CV value 9.7%, boiling water shrinkage is 5.0%, and crimp contraction is 2.50%, and crimp contraction becomes
Different coefficient CV value 9.3%, oil content is 1.0%, and internet pricing is 90/m, fiber number: 200dtex.
After described Wool-Like abnormal contraction composite filament is dyeed, it is thus achieved that dye uptake as shown in the table:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 51.0 | 83.4 | 92.0 | 92.9 | 92.0 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 53.5 | 87.8 | 92.8 | 93.4 | 94.1 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 46.4 | 74.9 | 87.5 | 88.5 | 90.8 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 7
The preparation method of a kind of Wool-Like abnormal contraction composite filament, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) tetracontane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid,
Being heated to 100 DEG C, refuxing esterification, cooling, separating-purifying obtains tetracontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of tetracontane dicarboxylic acids；
2) described tetracontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein
Tetracontane mono methyl dicarboxylate's concentration be 0.06mol/L under nitrogen atmosphere, 80 DEG C of reactions, backflow, produce when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.7 hours, be washed out, purify and be dried, obtain product bromo nonatriacontane carboxylic
Acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 48%, and dilute sulfuric acid addition is tetracontane dicarboxylic acids list first
The 2wt% of ester；
3), by the ammonia of bromo nonatriacontane carboxylic acid Yu 22wt% during 1:2 joins reactor in molar ratio, stirring, in room
The lower reaction of temperature, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses nitric acid
Silver solution detection, obtains product amino nonatriacontane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino nonatriacontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino nonatriacontane
2% addition concentration of carboxylic acid weight is the sulphuric acid of 46wt%, carries out esterification, and esterification reaction temperature is 190 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；The separated purification of product obtains amino nonatriacontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.8 and ethylene glycol, as raw material, are esterified after being made into uniform sizing material
Reaction, obtains esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.2MPa, and temperature, at 258 DEG C, is esterified
It is esterification terminal that water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, the antimony acetate of the 0.05% of addition p-phthalic acid weight in esterification products
With the trimethyl phosphate of p-phthalic acid weight 0.03%, starting polycondensation reaction under conditions of negative pressure, this staged pressure is by often
Flattening and be surely evacuated to below absolute pressure 500Pa, temperature controls at 268 DEG C, and the response time is 45 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino nonatriacontane carboxylic acid glycol ester, and stir 16 points
Clock；
Described amino nonatriacontane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 1.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 75 minutes response time；
Preparing modified poly ester, viscosity-average molecular weight is 25000；
(3) preparation of Wool-Like abnormal contraction composite filament:
By modified poly ester through measuring, extrude, cool down, oil and winding, prepare modified poly ester POY silk；
Modified poly ester POY yarn spinning technique:
Spinning temperature: 286 DEG C；
Chilling temperature: 20 DEG C；
Winding speed: 3400m/min；
The line density deviation ratio 0.17% of modified poly ester POY silk, fracture strength 3.0cN/dtex, fracture strength CV value
2.4%, elongation at break is 98%, extension at break CV value 5.8%；
By polyester slice through measuring, extrude, cool down, oil, stretching, thermal finalization and winding, prepare modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique:
Spinning temperature: 285 DEG C；
Chilling temperature: 22 DEG C；
Network pressure: 0.30MPa；
One roller speed: 2400m/min；
One roll temperature: 79 DEG C；
Two roller speed: 3650m/min；
Two roll temperatures: 123 DEG C；
Winding speed: 3700m/min；
The line density deviation ratio 4.5% of modified poly ester FDY silk, fracture strength 4.0cN/dtex, fracture strength CV value
4.6%, elongation at break is 32.0%, extension at break CV value 9.7%, yarn unevenness CV1.99%, boiling water shrinkage
7.3%, oil content 1.10%.
Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, add hot-stretch, false twisting, thermal finalization and volume
Wool-Like abnormal contraction composite filament is prepared around molding；
Composite filament processing technique:
Spin speed 400m/min；
Sizing over feed rate(OFR) 5.0%；
Winding is owed to feed rate 5.0；
T1:180 DEG C；
T2:170 DEG C；
DR:1.7；
D/Y:1.8；
Network pressure: 0.28MPa；
Gained Wool-Like abnormal contraction composite filament under the conditions of temperature is 120 DEG C, the free volume space of interior molecules interchain
Increase 27v/v%, line density deviation ratio-0.5%, fracture strength 2.8cN/dtex, fracture strength CV value 4.7%, extension at break
Rate is 14.5%, extension at break CV value 9.4.0%, and boiling water shrinkage is 5.3%, and crimp contraction is 3.5%, crimp contraction
Coefficient of variation CV value 9.2.0%, oil content is 0.9%, and internet pricing is 91/m, fiber number: 270dtex.
After described Wool-Like abnormal contraction composite filament is dyeed, it is thus achieved that dye uptake as shown in the table:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 51.4 | 83.5 | 92.6 | 93.4 | 92.8 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 54.9 | 87.3 | 93.5 | 93.3 | 94.4 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 46.5 | 75.6 | 87.5 | 89.4 | 91.5 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Claims (10)
1. a Wool-Like abnormal contraction composite filament, is characterized in that: described Wool-Like abnormal contraction composite filament be modified poly ester POY silk with
Modified poly ester FDY silk through the composite filament of mixed fibre processing composition, described modified poly ester POY silk formed tiny wire ring be centered around described in change
Around property polyester FDY silk；Modified poly ester is made up of with amino ethylene glycol fatty acid polyester, described amino ethylene glycol fatty acid
It is dispersed in the molecule interchain of described polyester, and the molecule interchain of described amino ethylene glycol fatty acid and described polyester has hydrogen bond to make
With, make described amino ethylene glycol fatty acid fix with the relative position of the strand of described polyester；The different contraction of described Wool-Like
Composite filament is under the conditions of temperature is 90～130 DEG C, and the free volume space of fibrous inside molecule interchain increases 20～30v/v%,
Fracture strength >=the 2.1cN/dtex of described Wool-Like abnormal contraction composite filament, elongation at break is 15.0 ± 2.0%, crimp shrinkage
Rate is 5.50 ± 3.0%, and internet pricing is 90 ± 5/m, fiber number: 150-300dtex；
The molecular structure of described amino ethylene glycol fatty acid is:
H2N(CH2)nCOOCH2CH2OOC(CH2)nNH2；
Wherein, n=10-50.
A kind of Wool-Like abnormal contraction composite filament the most according to claim 1, it is characterised in that the different contraction of described Wool-Like is multiple
Line density deviation ratio ± 2.5% of plying, fracture strength CV value≤5.0%, extension at break CV value≤10.0%, boiling water shrinkage
Being 5.0 ± 1.0%, crimp contraction coefficient of variation CV value≤10.0%, oil content is 1.0 ± 0.2%, fiber number: 150-
300dtex；Line density deviation ratio≤0.2% of modified poly ester POY silk, fracture strength >=2.6cN/dtex, fracture strength CV value
≤ 3.0%, elongation at break is 90.0 ± 10.0%, extension at break CV value≤6.0%；The line density of modified poly ester FDY silk is inclined
Rate≤0.5%, fracture strength >=3.8cN/dtex, fracture strength CV value≤5.0%, elongation at break is 33.0 ± 3.0%,
Extension at break CV value≤10.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ±
0.20%.
A kind of Wool-Like abnormal contraction composite filament the most according to claim 1, it is characterised in that described amino fatty acid second two
It is 0.5～2.5% that alcohol ester accounts for the percentage by weight of described Wool-Like abnormal contraction composite filament.
The preparation method of a kind of Wool-Like abnormal contraction composite filament the most as claimed in claim 1, is characterized in that: by modified poly ester warp
Measure, extrude, cool down, oil and wind, prepare modified poly ester POY silk；By polyester slice through measuring, extrude, cool down, oiling,
Stretching, thermal finalization and winding, prepare modified poly ester FDY silk；Then by modified poly ester POY silk and modified poly ester FDY silk through plying
Network, add hot-stretch, false twisting, thermal finalization and coiling and molding and prepare Wool-Like abnormal contraction composite filament；
Modified poly ester POY yarn spinning technique:
Spinning temperature: 280-290 DEG C；
Chilling temperature: 18-22 DEG C；
Winding speed: 2550-2880m/min；
Modified poly ester FDY yarn spinning technique:
Spinning temperature: 280-290 DEG C；
Chilling 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 speed: 3600-3900m/min；
Two roll temperatures: 115-135 DEG C；
Winding speed: 3600-3800m/min；
Wool-Like abnormal contraction composite filament processing technique:
Spin speed 400-800m/min；
Sizing over feed rate(OFR) 3.5-5.50%；
Winding over feed rate(OFR) 2.5-5.0；
T1:180-220 DEG C；
T2:150-180 DEG C；
DR:1.6-1.8；
D/Y:1.6-2.0；
Network pressure: 0.05-0.3MPa；
The preparation process of described modified poly ester includes:
(1) preparation of amino ethylene glycol fatty acid:
1) binary of fatty acids is added in reactor with the amount of 1:1.5 mol ratio with methanol, under the catalysis of concentrated sulphuric acid, be heated to
80～110 DEG C, refuxing esterification, cooling, separating-purifying obtains binary of fatty acids mono-methyl；Described binary of fatty acids is dodecane two
Carboxylic acid is to the one in dopentacontane dicarboxylic acids；
2) by described binary of fatty acids mono-methyl, lead tetraacetate and lithium bromide during 1:1:1 is dissolved in benzene in molar ratio, wherein binary fat
The concentration of fat acid mono-methyl is 0.05～0.1mol/L, and under nitrogen atmosphere, 80～90 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 2～3 hours, be washed out, purify and be dried, obtain product bromo fat
Acid；
3) by the ammonia of bromo fatty acid and 15～25wt% during 1:2 joins reactor in molar ratio, stirring, the most instead
Should, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is less than 70 DEG C,
Until bubble-free produces, i.e. stopping distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water and to without bromide ion is
Only, product vacuum drying is obtained product amino fatty acid；
4) ethylene glycol and amino fatty acid are stirred for 1.1:2 in molar ratio, and press the 1～3% of amino fatty acid wt
Adding the sulphuric acid that concentration is 40～50wt%, carry out esterification, esterification reaction temperature is 160～220 DEG C, esterification water quantity of distillate
Reaching more than the 90% of theoretical value is esterification terminal；The separated purification of product obtains amino ethylene glycol fatty acid；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
Use p-phthalic acid and ethylene glycol as raw material, carry out esterification after being made into uniform sizing material, obtain esterification products；
Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at normal pressure～0.3MPa, and temperature is at 250～260 DEG C, and esterification water evaporates
It is esterification terminal that output reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction coarse vacuum stage, esterification products adds catalyst and stabilizer, starts under conditions of negative pressure
Polycondensation reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature controls at 260～270 DEG C, reaction
Time is 30～50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino ethylene glycol fatty acid, and stir；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 275～280 DEG C, response time 50～90 minutes；
Prepare modified poly ester.
The preparation method of a kind of Wool-Like abnormal contraction composite filament the most according to claim 4, it is characterised in that described second two
Alcohol is 1.2～2.0:1 with the mol ratio of described p-phthalic acid.
The preparation method of a kind of Wool-Like abnormal contraction composite filament the most according to claim 4, it is characterised in that described catalysis
Agent one in antimony oxide, antimony glycol and antimony acetate, catalyst amount is described p-phthalic acid weight
0.01%～0.05%.
The preparation method of a kind of Wool-Like abnormal contraction composite filament the most according to claim 4, it is characterised in that described stable
Agent one in triphenyl phosphate, trimethyl phosphate and NSC 6513, stabilizing agent dosage is described p-phthalic acid
The 0.01%～0.05% of weight.
The preparation method of a kind of Wool-Like abnormal contraction composite filament the most according to claim 4, it is characterised in that add amino
Stirring after ethylene glycol fatty acid, the time is 15～20 minutes.
The preparation method of a kind of Wool-Like abnormal contraction composite filament the most according to claim 4, it is characterised in that use deionization
It is washed to without using silver nitrate solution detection till bromide ion.
The preparation method of a kind of Wool-Like abnormal contraction composite filament the most according to claim 4, it is characterised in that described dense
Sulphuric acid refers to the sulphuric acid that mass concentration is 70～80%, and concentrated sulphuric acid addition is the 1～3wt% of binary of fatty acids；Described necessarily
Amount dilute sulfuric acid refer to the sulphuric acid that mass concentration is 40～50%, dilute sulfuric acid addition be binary of fatty acids mono-methyl 1～
3wt%.
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| CN105648570B (en) * | 2015-12-29 | 2017-12-15 | 江苏恒力化纤股份有限公司 | A kind of low aberration polyester Wool-Like abnormal contraction composite filament and preparation method thereof |
| CN106245173B (en) * | 2016-08-19 | 2019-03-19 | 桐昆集团股份有限公司 | A kind of production method for terylene composite filament of trying to stop people from fighting each other |
| CN108048939B (en) * | 2017-12-14 | 2019-11-12 | 江苏恒力化纤股份有限公司 | One step spins elastic force composite filament and preparation method thereof |
| CN109402762A (en) * | 2018-10-19 | 2019-03-01 | 新凤鸣集团湖州中石科技有限公司 | A kind of preparation method of NEW TYPE OF COMPOSITE one step sprinning |
| CN109735979B (en) * | 2018-12-27 | 2020-11-06 | 江苏恒力化纤股份有限公司 | Preparation method of different-fineness and different-dye-uptake polyester low stretch yarn |
| CN109750372B (en) | 2018-12-27 | 2020-05-22 | 江苏恒力化纤股份有限公司 | Wool-like polyester filament and preparation method thereof |
| CN111534872B (en) * | 2020-04-30 | 2021-08-10 | 浙江佳宝聚酯有限公司 | Preparation method of novel composite wool-like fiber |
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