CN104562340B - Differential-shrinkage cotton-like composite filament and preparation method thereof - Google Patents
Differential-shrinkage cotton-like composite filament and preparation method thereof Download PDFInfo
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- CN104562340B CN104562340B CN201410850704.8A CN201410850704A CN104562340B CN 104562340 B CN104562340 B CN 104562340B CN 201410850704 A CN201410850704 A CN 201410850704A CN 104562340 B CN104562340 B CN 104562340B
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
- D02G3/045—Blended or other yarns or threads containing components made from different materials all components being made from artificial or synthetic material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/685—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen
- C08G63/6854—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6856—Dicarboxylic acids and dihydroxy compounds
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- 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
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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
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- 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
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- 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
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Abstract
The invention relates to a differential-shrinkage cotton-like composite filament and preparation method thereof; the differential-shrinkage cotton-like composite filament is a composite filament blended by a modified polyester POY filament and a modified polyester FDY filament; the modified polyester consists of polyester and aminoadipic acid glycol ester; the aminoadipic acid glycol ester is dispersed among the molecular chains of the polyester; and the aminoadipic acid glycol ester takes effect of hydrogen bond among the molecular chains of the polyester, so as to stabilize the positions of the aminoadipic acid glycol ester with respect to the molecular chains of the polyester; in condition of the temperature is 90-130 degrees centigrade, the free volume spaces among the molecular chains inside the fiber of the differential-shrinkage cotton-like composite filament are increased by 20-30v/v%. The aliphatic ester increases the free volume of the polyester fiber in order to increase the diffusion degree of the dye, thereby increasing the dyeing performance of the polyester fiber. The differential-shrinkage cotton-like composite filament is applicable to clothes fabric, bedding article, decoration article, and the like.
Description
Technical field
The invention belongs to fibre manufacturing technology field, it is related to a kind of imitative cotton abnormal contraction composite filament and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) fiber since the advent of the world, has obtained rapidly because of its excellent performance
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 have anti-
The advantages of wrinkle, stiffness are good, so, polyester fiber is widely used in the fields such as clothes, home textile.
PET belongs to symmetric straight chain macromolecular, and strand does not contain side-chain radical, and regularity is very good, its main chain
Phenyl ring containing rigidity and flexible alkyl, and the ester group being directly connected with phenyl ring constitutes rigid conjugated body with phenyl ring
System, thus constrain rotating freely of its soft segment.The impact to glass transition temperature for this structure is it will be evident that increasing
The wall ridge of molecule segment motion, the glass transition temperature of PET is higher, needs to dye at very high temperatures, promotes dyestuff
Molecule is to the diffusion of fibrous inside.In 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, makes the colouring of polyester fiber more difficult.
Difficult for solving the problems, such as PET dyeing, now mainly connect by introducing dye molecule using techniques or methods
By base or increase polyester amorphous regions amount method although the dyeability of polyester can be improved, destroy PET segment rule
Whole property, to obtain the raising of dyeability with the performance reducing polyester fiber.Do not destroying polyester fiber crystallinity and permutation degree
In the case of, the method adopting at present has three kinds of colouring methods such as support methods, high temperature and high pressure method and high temperature thermosoling.
Imitative cotton abnormal contraction composite filament is the long filament with different potential shrinkages, i.e. high-shrinkage filament POY and lower shrinkage
The composite filament through mixed fine processing composition for the silk FDY, the main feature of PET different contraction mixed fiber composite silk：High loft and soft hand
Sense.PET imitates the outer existing similar with common long filament of cotton abnormal contraction composite filament.Due to the difference of two component shrinkage factors, thermally treated
Afterwards, 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.Because PET imitates the many on the bulk and surface of cotton abnormal contraction composite filament
Wire ring, eliminates the aurora defect of chemical fibre silk fabrics.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.
Content of the invention
It is an object of the invention to provide a kind of imitative cotton abnormal contraction composite filament and preparation method thereof, the present invention utilizes aminolipid
In uniform temperature condition, the increasing degree of free volume is far longer than the characteristic of polyester macromolecule chain to fat acid glycol ester, leads to
Cross the degree improving within disperse dyes molecule entrance polyester, to improve the dyeability of polyester；Simultaneously because aminolipid
In the presence of the first amino in fat acid glycol ester molecule, increase itself hydrogen bond action and polyester macromolecule chain between, increased
It decreases migration to greatest extent with the compatibility of polyester and dispersion in the polyester.Simultaneously to polyester construction regularity,
Crystallinity is not destroyed, and maintains the premium properties of polyester.
A kind of imitative cotton abnormal contraction composite filament of the present invention, described imitative cotton abnormal contraction composite filament is modified poly ester POY silk
With the composite filament through mixed fine processing composition for the modified poly ester FDY silk, described modified poly ester POY silk formed tiny wire ring be 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 aliphatic acid second
Diol ester is dispersed in the molecule interchain of described polyester, and described amino ethylene glycol fatty acid is had with the molecule interchain of described polyester
Hydrogen bond action, makes described amino ethylene glycol fatty acid and the relative position of the strand of described polyester fix；Described imitative cotton
Abnormal contraction composite filament under the conditions of temperature is 90～130 DEG C, the free volume space of fibrous inside molecule interchain increases 20～
30v/v%；Fracture strength >=the 2.0cN/dtex of described imitative cotton abnormal contraction composite filament, elongation at break is 18.0 ± 3.0%,
Crimp contraction is 4.8 ± 3.0%, and internet pricing is 15 ± 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 imitative cotton abnormal contraction composite filament, described amino ethylene glycol fatty acid accounts for the different contraction of described imitative cotton
The percentage by weight of composite filament is 0.5～2.5%.
Described a kind of imitative cotton abnormal contraction composite filament, the fineness-unevenness rate CV value of described imitative cotton abnormal contraction composite filament
≤ 1.4%, fracture strength CV value≤7.0%, extension at break CV value≤9.0%, boiling water shrinkage is 3.0 ± 1.0%, and curling is received
Shrinkage coefficient of variation CV value≤9.0%, oil content is 3.0 ± 1.0%, fiber number：75-150dtex.The line of modified poly ester POY silk
Density variation rate≤0.2%, fracture strength >=2.6cN/dtex, fracture strength CV value≤3.0%, elongation at break is 100.0
± 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 a kind of preparation method of imitative cotton abnormal contraction composite filament, by polyester slice through metering, extrusion,
Cool down, oil and wind, prepared POY silk,；By polyester slice through measuring, extruding, cool down, oil, stretch, thermal finalization and winding,
Prepared FDY silk；POY silk and FDY are obtained imitative cotton through wire leading pipe, plying network, heating stretching, false twisting, thermal finalization and coiling and molding
Type abnormal contraction composite filament；
Modified poly ester POY yarn spinning technique：
Spinning temperature：280-290℃；
Chilling temperature：20-25℃；
Winding speed：2550-2880m/min；
Modified poly ester FDY yarn spinning technique：
Spinning temperature：280-290℃；
Chilling temperature：20-25℃；
Network pressure：0.20-0.30MPa；
One roller speed：2200-2600m/min；
One roll temperature：75-85℃；
Two roller speeds：3600-3900m/min；
Two roll temperatures：115-135℃；
Winding speed：3600-3800m/min；
Compound filament processing process：
Spin fast 400-800m/min；
Sizing over feed rate(OFR) 3.5-5.50%；
Winding over feed rate(OFR) 2.5-5.0；
T1：150-220℃；
T2：100-180℃；
DR：1.5-1.9；
D/Y:1.7-2.2；
Network pressure：0.05-0.3MPa；
The preparation process of described modified poly ester includes：
(1) preparation of amino ethylene glycol fatty acid：
1) by binary of fatty acids and methyl alcohol with 1:The amount of 1.5 mol ratios adds in reactor, under the catalysis of the concentrated sulfuric acid, plus
Heat to 80～110 DEG C, refuxing esterification, cooling, separating-purifying obtains binary of fatty acids mono-methyl；Described binary of fatty acids is 12
Alkane dicarboxylic acids is one of to 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 in molar ratio 1:1:1 is dissolved in benzene, and wherein two
The concentration of first aliphatic acid mono-methyl is 0.05～0.1mol/L, under nitrogen atmosphere, reacts at 80～90 DEG C, backflow, when no longer
When having gas to produce, add a certain amount of dilute sulfuric acid to react 2～3 hours, be washed out, purify and be dried, obtain product bromo
Aliphatic acid；Reaction equation is：
3) by the ammoniacal liquor of bromo binary of fatty acids and 15～25wt% in molar ratio 1:2 are added in reactor, stirring,
React under room temperature, then product is heated distillation, and absorb ammonia with cold water, the temperature of heating distillation is less than 70 DEG C, directly
Produce to bubble-free, that is, stop distillation, then cooled down and suction filtration, filter cake deionized water is washed till no till bromide ion, will
Product vacuum drying obtains product amino aliphatic acid；Vacuum drying temperature can adopt 60～70 DEG C；Reaction equation is：
HOOC(CH2)nBr+NH3→HOCO(CH2)nNH2+NH4Br；
4) by ethylene glycol and amino aliphatic acid in molar ratio for 1.1:2 stir, and press the hundred of amino fatty acid wt
/ mono- addition concentration is the sulfuric acid of 40～50wt% is catalyst, carries out esterification, and esterification reaction temperature is 160～220
DEG C, esterification water quantity of distillate reach theoretical value more than 90% be esterification terminal；The separated purification of product obtains amino
Ethylene glycol fatty acid；Reaction equation is：
(2) preparation of modified poly ester, including esterification and polycondensation reaction：
Described esterification：
Using terephthalic acid (TPA) 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 in normal pressure～0.3MPa, at 250～260 DEG C, esterification water evaporates temperature Stress control
Output reach theoretical value more than 90% be esterification terminal；
Described polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the described polycondensation reaction low vacuum stage, add catalyst and stabilizer in esterification products, under conditions of negative pressure
Start polycondensation reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature control at 260～270 DEG C,
Reaction time is 30～50 minutes；
Add amino ethylene glycol fatty acid after the described polycondensation reaction low vacuum stage terminates, and stir, generally stir
15～20 minutes；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275～280 DEG C, 50～90 minutes reaction time；
Prepared modified poly ester；
A kind of preparation method of imitative cotton abnormal contraction composite filament as above, described ethylene glycol and described terephthalic acid (TPA)
Mol ratio be 1.2～2.0:1.
A kind of preparation method of imitative cotton abnormal contraction composite filament as above, described catalyst be selected from antimony oxide,
One of antimony glycol and antimony acetate, catalyst amount is the 0.01%～0.05% of described terephthalic acid (TPA) weight.
A kind of preparation method of imitative cotton abnormal contraction composite filament as above, described stabilizer be selected from triphenyl phosphate,
One of trimethyl phosphate and Trimethyl phosphite, stabilizing agent dosage be described terephthalic acid (TPA) weight 0.01%～
0.05%.
A kind of preparation method of imitative cotton abnormal contraction composite filament as above, deionized water is washed till no till bromide ion
Using silver nitrate solution detection.
A kind of preparation method of imitative cotton abnormal contraction composite filament as above, the described concentrated sulfuric acid refers to that mass concentration is 70
～80% sulfuric acid, concentrated sulfuric acid addition is 1～3wt% of binary of fatty acids；Described a certain amount of dilute sulfuric acid refers to that quality is dense
Spend the sulfuric acid for 40～50%, dilute sulfuric acid addition is 1～3wt% of binary of fatty acids mono-methyl.
In dyeing, disperse dyes can be divided into the next stage polyester fiber to the upper dye process of polyester fiber：
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, produce a concentration difference or inside and outside in fiber
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, in addition to dyestuff solubility 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 exists less space in fiber,
Under the conditions of the humidity in dyeing, polyester fiber will not can be by acutely swelling and make space increase as cotton fiber, dyestuff divides
Son is difficult to see through fibrous inside.Therefore, improve the carrying out that the free volume between fiber molecule will be helpful to dye.
The molecular chain structure of polyester is the linear macromolecule containing benzene ring structure, the functional group's marshalling on strand,
Unbranched, macromolecular chain flexibility is poor.The regularity of polyester is good and rigidity is all larger simultaneously, and intermolecular active force is larger.
Compared with other macromolecular materials, the strand generation sliding of polyester, rotation are all more difficult, and these characteristics hinder dyestuff and enter
Enter inside polyester, thus dyeability is poor.
Amino ethylene glycol fatty acid, mainly with C-C, based on C-O key, has certain molecular weight simultaneously, that is, has certain
The strand of length, strand flexibility is larger, and the amount of crimp of amino ethylene glycol fatty acid is linearly big compared with benzene ring structure
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 aliphatic acid
Glycol ester moves prior to the linear macromolecule containing benzene ring structure, and free volume produced by motion is far longer than containing phenyl ring
Produced by the linear macromolecule of structure.
Increase the diffusion of dyestuff by the free volume that fatty acid ester increased polyester fiber, improve polyester fiber
Dyeability, make fiber obtain high dye-uptake.
Oxygen in fatty acid ester can form hydrogen bond, but oxygen when centre position, due to space steric effect and fat
The hydrogen that the factors such as the curling of fat acid ester molecules reduce in itself and polyester macromolecule chain forms the quantity of hydrogen bond；If amino is in α position
On, i.e. amino acids, because amino and carbonyl interact, also it is unfavorable for that amino forms hydrogen with the hydrogen in polyester macromolecule chain
Key；When the end position in macromolecular for the amino of amino fatty acid ester, the curling of macromolecular affects on it less, to increased aminolipid
Amino in fat acid esters and the formation of the formation hydrogen bond of the hydrogen 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.
Increased 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：
1. the imitative cotton abnormal contraction composite filament of gained of the present invention, because amino ethylene glycol fatty acid is based on C-C, with
When there is certain molecular weight, that is, there is the strand of certain length, strand flexibility is larger, and amino increased the phase with polyester
Capacitive.The fiber of gained is good with the compatibility of amino ethylene glycol fatty acid.
2., due to the presence in the first amino in amino ethylene glycol fatty acid molecule, increase with it with polyester macromolecule chain
Between hydrogen bond action, increased it with the compatibility of polyester and dispersion in the polyester, decrease migration to greatest extent.
3. the imitative cotton abnormal contraction composite filament of gained of the present invention, because 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 compared with the linear macromolecule of benzene ring structure, simultaneously to temperature
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, free volume produced by the motion of amino ethylene glycol fatty acid is far longer than the institute of the linear macromolecule containing benzene ring structure
Produce, increase the diffusion of additive, to improve the feature of polyester.
5. fatty acid ester increased the free volume of the polyester fiber diffusion to increase dyestuff, improves polyester fiber
Dyeability.
6. many wire rings on the bulk and surface of imitative cotton abnormal contraction composite filament of gained of the present invention, eliminate chemical fiber wire
The aurora defect of fabric, has excellent warmth retention property, and the high loft of different contraction mixed fiber composite silk, increases between fiber
Space.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It 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 of present invention instruction, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
A kind of imitative cotton abnormal contraction composite filament of the present invention, is that modified poly ester POY silk is added through mixed fibre with modified poly ester FDY 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 described amino ethylene glycol fatty acid has hydrogen bond action with the molecule interchain of described polyester, makes described aminolipid
The relative position of fat acid glycol ester and the strand of described polyester is fixed；Described imitative cotton 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 imitative cotton
Fracture strength >=the 2.0cN/dtex of composite filament, elongation at break is 18.0 ± 3.0%, and crimp contraction is 4.8 ± 3.0%,
Internet pricing is 15 ± 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 imitative cotton abnormal contraction composite filament, described amino ethylene glycol fatty acid accounts for the different contraction of described imitative cotton
The percentage by weight of composite filament is 0.5～2.5%.
Described a kind of imitative cotton abnormal contraction composite filament, the fineness-unevenness rate CV value of described imitative cotton abnormal contraction composite filament
≤ 1.4%, fracture strength CV value≤7.0%, extension at break CV value≤9.0%, boiling water shrinkage is 3.0 ± 1.0%, and curling is received
Shrinkage coefficient of variation CV value≤9.0%, oil content is 3.0 ± 1.0%, fiber number：75-150dtex.The line of modified poly ester POY silk
Density variation rate≤0.2%, fracture strength >=2.6cN/dtex, fracture strength CV value≤3.0%, elongation at break is 100.0
± 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, and disperse blue SE-2R disperses bright blue S-GL, and fiber exists respectively
Dye in HTHP machine.Before dye, fiber nonionic surfactant is processed 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 adopts raffinate colorimetric method to determine, draws appropriate dyeing stoste and dyeing residual liquid, adds N, N-2 first
Base formamide (DMF) and distilled water, are that the ratio of DMF in dye liquor to be measured and water is 70/30 (v/v), dye liquor absorbance adopts
Ultraviolet-visible spectrophotometer measures, and calculates dye uptake with following formula.
In above formula, A0 and A1 is respectively the absorbance dyeing stoste and dyeing residual liquid.
Embodiment 1
A kind of preparation method of imitative cotton abnormal contraction composite filament, comprises the following steps：
(1) preparation of amino ethylene glycol fatty acid：
1) by dodecanedicarboxylic acid and methyl alcohol with 1:The amount of 1.5 mol ratios adds in reactor, under the catalysis of the concentrated sulfuric acid,
It is heated to 80 DEG C, refuxing esterification, cooling, separating-purifying obtains dodecanedicarboxylic acid mono-methyl；The described concentrated sulfuric acid refers to that quality is dense
Spend the sulfuric acid for 70%, concentrated sulfuric 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, reacts at 80 DEG C, backflow, produces when no longer there being gas
When raw, add a certain amount of dilute sulfuric acid to 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 sulfuric acid that mass concentration is 40%, and dilute sulfuric acid addition is dodecanedicarboxylic acid mono-methyl
3wt%；
3) by the ammoniacal liquor of bromoundecane carboxylic acid and 15wt% in molar ratio 1:2 are added in reactor, and stirring, in room temperature
Lower reaction, then product is heated distillation, and absorb ammonia with cold water, the temperature of heating distillation is 60 DEG C, until bubble-free
Produce, that is, stop distillation, then cooled down and suction filtration, filter cake deionized water is washed till no till bromide ion, using silver nitrate
Solution detects, product vacuum drying is obtained product amino-undecanoic carboxylic acid；
4) by ethylene glycol and amino-undecanoic carboxylic acid in molar ratio for 1.1:2 stir, and press amino-undecanoic carboxylic acid
1% addition concentration of weight is the sulfuric acid of 40wt%, carries out esterification, 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：
It is 1 using mol ratio:1.2 terephthalic acid (TPA) 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 250 DEG C in 0.3MPa, temperature, esterification
Water quantity of distillate reach theoretical value more than 90% be esterification terminal；
Described polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the described polycondensation reaction low vacuum stage, esterification products add the 0.01% of terephthalic acid (TPA) weight three oxidations
Two antimony and the triphenyl phosphate of terephthalic acid (TPA) weight 0.01%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Below absolute pressure 500Pa is steadily evacuated to by normal pressure, at 260 DEG C, the reaction time is 50 minutes to temperature control；
Add amino-undecanoic carboxylic acid glycol ester after the described polycondensation reaction low vacuum stage terminates, 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 low vacuum stage, continues to vacuumize, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 90 minutes reaction time；
Prepared modified poly ester, viscosity average molecular weigh is 15000；
(3) imitate the preparation of cotton abnormal contraction composite filament：
By modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk；
Modified poly ester POY yarn spinning technique：
Spinning temperature：290℃；
Chilling temperature：25℃；
Winding speed：2550m/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, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique：
Spinning temperature：290℃；
Chilling temperature：25℃；
Network pressure：0.20MPa；
One roller speed：2200m/min；
One roll temperature：75℃；
Two roller speeds：3600m/min；
Two roll temperatures：115℃；
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, heating stretching, false twisting, thermal finalization and volume
Imitative cotton abnormal contraction composite filament is obtained around shaping；
Compound filament processing process：
Spin fast 400m/min；
Sizing over feed rate(OFR) 3.5%；
Winding over feed rate(OFR) 2.5；
T1：150℃；
T2：100℃；
DR：1.5；
D/Y:1.7；
Network pressure：0.05MPa；
Gained imitates cotton abnormal contraction composite filament under the conditions of temperature is 90 DEG C, and the free volume of fibrous inside molecule interchain is empty
Between increase 20v/v%, fineness-unevenness rate CV value 1.4%, fracture strength 2.0cN/dtex, fracture strength CV value 7.0%, rupture
Percentage elongation is 21.0%, extension at break CV value 9.0%, and boiling water shrinkage is 4.0%, and crimp contraction is 7.8%, crimp shrinkage
Rate coefficient of variation CV value 9.0%, oil content is 4.0%, fiber number：75dtex, internet pricing is 10/m.
After described imitative cotton abnormal contraction composite filament is dyeed, the dye uptake of acquisition is as shown in the table：
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 50.5 | 81.8 | 91.6 | 92.4 | 91.2 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 52.4 | 87.6 | 92.6 | 92.4 | 92.7 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 45.5 | 74.8 | 86.0 | 87.5 | 90.3 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 2
A kind of preparation method of imitative cotton abnormal contraction composite filament, comprises the following steps：
(1) preparation of amino ethylene glycol fatty acid：
1) by dopentacontane dicarboxylic acids and methyl alcohol with 1:The amount of 1.5 mol ratios adds in reactor, in the catalysis of the concentrated sulfuric acid
Under, it is heated to 110 DEG C, refuxing esterification, cooling, separating-purifying obtains dopentacontane mono methyl dicarboxylate；The described concentrated sulfuric acid refers to
Mass concentration is 70% sulfuric acid, and concentrated sulfuric 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, under nitrogen atmosphere, reacts at 85 DEG C, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid to 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 sulfuric acid that mass concentration is 40%, and dilute sulfuric acid addition is dopentacontane dicarboxylic acids
The 3wt% of mono-methyl；
3) by the ammoniacal liquor of bromo henpentacontane carboxylic acid and 25wt% in molar ratio 1:2 are added in reactor, and stirring, in room
Temperature is lower to react, then product is heated distillation, and absorbs ammonia with cold water, and the temperature of heating distillation is 62 DEG C, until no gas
Bubble produces, that is, stop distillation, then cooled down and suction filtration, and filter cake deionized water is washed till no till bromide ion, using nitric acid
Silver-colored solution detection, product vacuum drying is obtained product amino henpentacontane carboxylic acid；
4) by ethylene glycol and amino henpentacontane carboxylic acid in molar ratio for 1.1:2 stir, and press amino henpentacontane
2% addition concentration of carboxylic acid weight is the sulfuric acid of 45wt%, carries out esterification, esterification reaction temperature is 220 DEG C, and esterification water evaporates
Output reach theoretical value more than 90% be esterification terminal；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：
It is 1 using mol ratio:2.0 terephthalic acid (TPA) 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 in 0.2MPa, temperature, at 260 DEG C, is esterified Stress control
Water quantity of distillate reach theoretical value more than 90% be esterification terminal；
Described polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the described polycondensation reaction low vacuum stage, esterification products add the 0.05% of terephthalic acid (TPA) weight three oxidations
Two antimony and the triphenyl phosphate of terephthalic acid (TPA) weight 0.05%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Below absolute pressure 500Pa is steadily evacuated to by normal pressure, at 270 DEG C, the reaction time is 30 minutes to temperature control；
Add amino henpentacontane carboxylic acid glycol ester after the described polycondensation reaction low vacuum stage terminates, and stir 20 points
Clock；Described amino henpentacontane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 2.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 280 DEG C, 50 minutes reaction time；
Prepared modified poly ester, viscosity average molecular weigh is 30000；
(3) imitate the preparation of cotton abnormal contraction composite filament：
By modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk；
Modified poly ester POY yarn spinning technique：
Spinning temperature：280℃；
Chilling temperature：20℃；
Winding speed：2700m/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, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique：
Spinning temperature：280℃；
Chilling temperature：20℃；
Network pressure：0.25MPa；
One roller speed：2400m/min；
One roll temperature：80℃；
Two roller speeds：3750m/min；
Two roll temperatures：125℃；
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, heating stretching, false twisting, thermal finalization and volume
Imitative cotton abnormal contraction composite filament is obtained around shaping；
Compound filament processing process：
Spin fast 800m/min；
Sizing over feed rate(OFR) 5.50%；
Winding over feed rate(OFR) 5.0；
T1：220℃；
T2：180℃；
DR：1.9；
D/Y:2.2；
Network pressure：0.3MPa；
Gained imitates cotton abnormal contraction composite filament under the conditions of temperature is 130 DEG C, the free volume space of interior molecules interchain
Increase 30v/v%, fineness-unevenness rate CV value 1.3%, fracture strength 2.1cN/dtex, fracture strength CV value 6.9%, fracture is stretched
Long rate is 21.0%, extension at break CV value 8.9%, and boiling water shrinkage is 2.0%, and crimp contraction is 1.8%, crimp contraction
Coefficient of variation CV value 8.1%, oil content is 2.0%, fiber number：150dtex, internet pricing is 20/m.
After described imitative cotton abnormal contraction composite filament is dyeed, the dye uptake of acquisition is as shown in the table：
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 51.2 | 82.5 | 92.3 | 93.2 | 92.5 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 53.4 | 88.3 | 93.3 | 93.1 | 93.4 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 46.2 | 75.2 | 87.1 | 88.3 | 90.9 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 3
A kind of preparation method of imitative cotton abnormal contraction composite filament, comprises the following steps：
(1) preparation of amino ethylene glycol fatty acid：
1) by pentacosane dicarboxylic acid and methyl alcohol with 1:The amount of 1.5 mol ratios adds in reactor, under the catalysis of the concentrated sulfuric acid,
It is heated to 85 DEG C, refuxing esterification, cooling, separating-purifying obtains pentacosane dicarboxylic acid mono-methyl；The described concentrated sulfuric acid refers to that quality is dense
Spend the sulfuric acid for 70%, concentrated sulfuric 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, reacts at 90 DEG C, backflow, produces when no longer there being gas
When raw, add a certain amount of dilute sulfuric acid to 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 sulfuric acid that mass concentration is 50%, and dilute sulfuric acid addition is pentacosane dicarboxylic acid list first
The 3wt% of ester；
3) by the ammoniacal liquor of bromotetradecane carboxylic acid and 20wt% in molar ratio 1:2 are added in reactor, and stirring, in room temperature
Lower reaction, then product is heated distillation, and absorb ammonia with cold water, the temperature of heating distillation is 60 DEG C, until bubble-free
Produce, that is, stop distillation, then cooled down and suction filtration, filter cake deionized water is washed till no till bromide ion, using silver nitrate
Solution detects, product vacuum drying is obtained product amino tetradecane carboxylic acid；
4) by ethylene glycol and amino tetradecane carboxylic acid in molar ratio for 1.1:2 stir, and press amino tetradecane carboxylic acid
2% addition concentration of weight is the sulfuric acid of 50wt%, carries out esterification, 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：
It is 1 using mol ratio:1.6 terephthalic acid (TPA) 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 in 0.3MPa, temperature, at 255 DEG C, is esterified Stress control
Water quantity of distillate reach theoretical value more than 90% be esterification terminal；
Described polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the described polycondensation reaction low vacuum stage, esterification products add the 0.03% of terephthalic acid (TPA) weight three oxidations
Two antimony and the triphenyl phosphate of terephthalic acid (TPA) weight 0.03%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Below absolute pressure 500Pa is steadily evacuated to by normal pressure, at 265 DEG C, the reaction time is 40 minutes to temperature control；
Add amino tetradecane carboxylic acid glycol ester after the described polycondensation reaction low vacuum stage terminates, and stir 16 points
Clock；Described amino tetradecane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 1.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 276 DEG C, 70 minutes reaction time；
Prepared modified poly ester, viscosity average molecular weigh is 22500；
(3) imitate the preparation of cotton abnormal contraction composite filament：
By modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk；
Modified poly ester POY yarn spinning technique：
Spinning temperature：287℃；
Chilling temperature：23℃；
Winding speed：2880m/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 110.0%, extension at break CV value 6.0%；
By polyester slice through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique：
Spinning temperature：287℃；
Chilling temperature：23℃；
Network pressure：0.30MPa；
One roller speed：2600m/min；
One roll temperature：85℃；
Two roller speeds：3900m/min；
Two roll temperatures：135℃；
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, heating stretching, false twisting, thermal finalization and volume
Imitative cotton abnormal contraction composite filament is obtained around shaping；
Compound filament processing process：
Spin fast 600m/min；
Sizing over feed rate(OFR) 4.5%；
Winding over feed rate(OFR) 3.0；
T1：180℃；
T2：140℃；
DR：1.7；
D/Y:2.0；
Network pressure：0.15MPa；
Gained imitates cotton abnormal contraction composite filament under the conditions of temperature is 100 DEG C, the free volume space of interior molecules interchain
Increase 20v/v%, fineness-unevenness rate CV value 1.2%, fracture strength >=2.2cN/dtex, fracture strength CV value 6.8%, fracture
Percentage elongation is 18.0%, extension at break CV value 8.8%, and boiling water shrinkage is 3.0%, and crimp contraction is 4.8%, crimp shrinkage
Rate coefficient of variation CV value 8.2%, oil content is 3.0%, fiber number：105dtex, internet pricing is 15/m.Modified poly ester POY silk
Line density deviation ratio 0.2%, fracture strength 2.6cN/dtex, fracture strength CV value 2.9%, elongation at break is 110.0%, breaks
Split elongation CV value 6.0%.；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%.
After described imitative cotton abnormal contraction composite filament is dyeed, the dye uptake of acquisition is as shown in the table：
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 50.4 | 81.7 | 91.4 | 92.3 | 91.5 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 52.4 | 87.5 | 92.5 | 92.1 | 93.0 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 45.4 | 74.1 | 86.3 | 88.0 | 90.2 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 4
A kind of preparation method of imitative cotton abnormal contraction composite filament, comprises the following steps：
(1) preparation of amino ethylene glycol fatty acid：
1) by eicosane dicarboxylic acids and methyl alcohol with 1:The amount of 1.5 mol ratios adds in reactor, under the catalysis of the concentrated sulfuric acid,
It is heated to 85 DEG C, refuxing esterification, cooling, separating-purifying obtains eicosane mono methyl dicarboxylate；The described concentrated sulfuric acid refers to that quality is dense
Spend the sulfuric acid for 70%, concentrated sulfuric 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, reacts at 80 DEG C, backflow, produces when no longer there being gas
When raw, add a certain amount of dilute sulfuric acid to 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 sulfuric acid that mass concentration is 43%, and dilute sulfuric acid addition is eicosane dicarboxylic acids list first
The 2wt% of ester；
3) by the ammoniacal liquor of bromo nonadecane carboxylic acid and 16wt% in molar ratio 1:2 are added in reactor, and stirring, in room temperature
Lower reaction, then product is heated distillation, and absorb ammonia with cold water, the temperature of heating distillation is 69 DEG C, until bubble-free
Produce, that is, stop distillation, then cooled down and suction filtration, filter cake deionized water is washed till no till bromide ion, using silver nitrate
Solution detects, product vacuum drying is obtained product amino nonadecane carboxylic acid；
4) by ethylene glycol and amino nonadecane carboxylic acid in molar ratio for 1.1:2 stir, and press amino nonadecane carboxylic acid
2% addition concentration of weight is the sulfuric acid of 42wt%, carries out esterification, 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：
It is 1 using mol ratio:1.2 terephthalic acid (TPA) 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 in 0.15MPa, temperature, at 251 DEG C, is esterified Stress control
Water quantity of distillate reach theoretical value more than 90% be esterification terminal；
Described polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the described polycondensation reaction low vacuum stage, esterification products add the 0.02% of terephthalic acid (TPA) weight three oxidations
Two antimony and the triphenyl phosphate of terephthalic acid (TPA) weight 0.02%, start polycondensation reaction, this staged pressure under conditions of negative pressure
Below absolute pressure 500Pa is steadily evacuated to by normal pressure, at 262 DEG C, the reaction time is 33 minutes to temperature control；
Add amino nonadecane carboxylic acid glycol ester after the described polycondensation reaction low vacuum stage terminates, and stir 17 points
Clock；Described amino nonadecane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 1.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure
Power drops
It is less than 100Pa to absolute pressure, reaction temperature controls at 277 DEG C, 55 minutes reaction time；
Prepared modified poly ester, viscosity average molecular weigh is 16000；
(3) imitate the preparation of cotton abnormal contraction composite filament：
By modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk；
Modified poly ester POY yarn spinning technique：
Spinning temperature：287℃；
Chilling temperature：21℃；
Winding speed：2650m/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 109.0%, extension at break CV value 5.6%；
By polyester slice through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique：
Spinning temperature：287℃；
Chilling temperature：21℃；
Network pressure：0.21MPa；
One roller speed：2300m/min；
One roll temperature：76℃；
Two roller speeds：3650m/min；
Two roll temperatures：117℃；
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, heating stretching, false twisting, thermal finalization and volume
Imitative cotton abnormal contraction composite filament is obtained around shaping；
Compound filament processing process：
Spin fast 500m/min；
Sizing over feed rate(OFR) 4.0%；
Winding over feed rate(OFR) 3.0；
T1：160℃；
T2：110℃；
DR：1.6；
D/Y:1.8；
Network pressure：0.10MPa；
Gained imitates cotton abnormal contraction composite filament under the conditions of temperature is 100 DEG C, the free volume of fibrous inside molecule interchain
Space increases 22v/v%, fineness-unevenness rate CV value 1.1%, fracture strength 2.4cN/dtex, fracture strength CV value 6.5%, breaks
Splitting percentage elongation is 19.0%, extension at break CV value 8.2%, and boiling water shrinkage is 3.5%, and crimp contraction is 6.8%, and curling is received
Shrinkage coefficient of variation CV value 8.8%, oil content is 3.5%, fiber number：80dtex, internet pricing is 16/m.
After described imitative cotton abnormal contraction composite filament is dyeed, the dye uptake of acquisition is as shown in the table：
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 50.2 | 81.8 | 91.5 | 92.5 | 91.1 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 53.1 | 88.5 | 93.4 | 92.9 | 93.5 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 45.8 | 75.0 | 86.8 | 88.4 | 90.7 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 5
A kind of preparation method of imitative cotton abnormal contraction composite filament, comprises the following steps：
(1) preparation of amino ethylene glycol fatty acid：
1) by melissane dicarboxylic acids and methyl alcohol with 1:The amount of 1.5 mol ratios adds in reactor, under the catalysis of the concentrated sulfuric acid,
It is heated to 90 DEG C, refuxing esterification, cooling, separating-purifying obtains melissane mono methyl dicarboxylate；The described concentrated sulfuric acid refers to that quality is dense
Spend the sulfuric acid for 70%, concentrated sulfuric 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 for 0.10mol/L under nitrogen atmosphere, is reacted at 85 DEG C, backflow, produces when no longer there being gas
When raw, add a certain amount of dilute sulfuric acid to 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 sulfuric acid that mass concentration is 40%, and dilute sulfuric acid addition is melissane dicarboxylic acids list first
The 3wt% of ester；
3) by the ammoniacal liquor of bromo nonacosane carboxylic acid and 18wt% in molar ratio 1:2 are added in reactor, and stirring, in room
Temperature is lower to react, then product is heated distillation, and absorbs ammonia with cold water, and the temperature of heating distillation is 67 DEG C, until no gas
Bubble produces, that is, stop distillation, then cooled down and suction filtration, and filter cake deionized water is washed till no till bromide ion, using nitric acid
Silver-colored solution detection, product vacuum drying is obtained product amino nonacosane carboxylic acid；
4) by ethylene glycol and amino nonacosane carboxylic acid in molar ratio for 1.1:2 stir, and press amino nonacosane
2% addition concentration of carboxylic acid weight is the sulfuric acid of 48wt%, carries out esterification, esterification reaction temperature is 170 DEG C, and esterification water evaporates
Output reach theoretical value more than 90% be esterification terminal；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：
It is 1 using mol ratio:1.5 terephthalic acid (TPA) 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 in 0.3MPa, temperature, at 254 DEG C, is esterified Stress control
Water quantity of distillate reach theoretical value more than 90% be esterification terminal；
Described polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the described polycondensation reaction low vacuum stage, esterification products add the 0.01% of terephthalic acid (TPA) weight ethylene glycol
Antimony and the trimethyl phosphate of terephthalic acid (TPA) 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 at 266 DEG C, the reaction time is 39 minutes to temperature control；
Add amino nonacosane carboxylic acid glycol ester after the described polycondensation reaction low vacuum stage terminates, and stir 18 points
Clock；Described amino nonacosane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 2.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 278 DEG C, 60 minutes reaction time；
Prepared modified poly ester, viscosity average molecular weigh is 22000；
(3) imitate the preparation of cotton abnormal contraction composite filament：
By modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk；
Modified poly ester POY yarn spinning technique：
Spinning temperature：285℃；
Chilling temperature：23℃；
Winding speed：2800m/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 108.0%, extension at break CV value 5.5%；
By polyester through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique：
Spinning temperature：285℃；
Chilling temperature：23℃；
Network pressure：0.22MPa；
One roller speed：2400m/min；
One roll temperature：77℃；
Two roller speeds：3800m/min；
Two roll temperatures：119℃；
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, heating stretching, false twisting, thermal finalization and volume
Imitative cotton abnormal contraction composite filament is obtained around shaping；
Compound filament processing process：
Spin fast 700m/min；
Sizing over feed rate(OFR) 5.0%；
Winding over feed rate(OFR) 4.5；
T1：210℃；
T2：170℃；
DR：1.8；
D/Y:2.1；
Network pressure：0.25MPa；
Gained imitates cotton abnormal contraction composite filament under the conditions of temperature is 90 DEG C, and the free volume of fibrous inside molecule interchain is empty
Between increase 23v/v%, fineness-unevenness rate CV value 1.1%, fracture strength 2.5cN/dtex, fracture strength CV value 6.7%, rupture
Percentage elongation is 16.0%, extension at break CV value 8.6%, and boiling water shrinkage is 2.5%, and crimp contraction is 2.5%, crimp shrinkage
Rate coefficient of variation CV value 8.4%, oil content is 3.7%, fiber number：140dtex, internet pricing is 19/m.
After described imitative cotton abnormal contraction composite filament is dyeed, the dye uptake of acquisition is as shown in the table：
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 51.2 | 82.9 | 92.1 | 93.4 | 92.5 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 53.0 | 88.1 | 93.4 | 92.8 | 93.5 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 45.3 | 74.5 | 86.0 | 87.4 | 90.3 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 6
A kind of preparation method of modified poly ester, comprises the following steps：
(1) preparation of amino ethylene glycol fatty acid：
1) by pentatriacontane dicarboxylic acids and methyl alcohol with 1:The amount of 1.5 mol ratios adds in reactor, in the catalysis of the concentrated sulfuric acid
Under, it is heated to 95 DEG C, refuxing esterification, cooling, separating-purifying obtains pentatriacontane mono methyl dicarboxylate；The described concentrated sulfuric acid refers to matter
Amount concentration is 70% sulfuric acid, and concentrated sulfuric 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, react at 90 DEG C, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid to 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 sulfuric acid that mass concentration is 45%, and dilute sulfuric acid addition is pentatriacontane dicarboxyl
The 1wt% of sour mono-methyl
3) by the ammoniacal liquor of bromo tetratriacontane carboxylic acid and 20wt% in molar ratio 1:2 are added in reactor, and stirring, in room
Temperature is lower to react, then product is heated distillation, and absorbs ammonia with cold water, and the temperature of heating distillation is 69 DEG C, until no gas
Bubble produces, that is, stop distillation, then cooled down and suction filtration, and filter cake deionized water is washed till no till bromide ion, using nitric acid
Silver-colored solution detection, product vacuum drying is obtained product amino tetratriacontane carboxylic acid；
4) by ethylene glycol and amino tetratriacontane carboxylic acid in molar ratio for 1.1:2 stir, and press amino tetratriacontane
1% addition concentration of carboxylic acid weight is the sulfuric acid of 50wt%, carries out esterification, esterification reaction temperature is 180 DEG C, and esterification water evaporates
Output reach theoretical value more than 90% be esterification terminal；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：
It is 1 using mol ratio:1.6 terephthalic acid (TPA) 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 in 0.4MPa, temperature, at 256 DEG C, is esterified Stress control
Water quantity of distillate reach theoretical value more than 90% be esterification terminal；
Described polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the described polycondensation reaction low vacuum stage, esterification products add the 0.04% of terephthalic acid (TPA) weight antimony acetate
With the Trimethyl phosphite of terephthalic acid (TPA) 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 at 267 DEG C, the reaction time is 40 minutes to temperature control；
Add amino tetratriacontane carboxylic acid glycol ester after the described polycondensation reaction low vacuum stage terminates, and stir 18 points
Clock；Described amino tetratriacontane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 2.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 70 minutes reaction time；
Prepared modified poly ester, viscosity average molecular weigh is 24000；
(3) imitate the preparation of cotton abnormal contraction composite filament：
By modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk；
Modified poly ester POY yarn spinning technique：
Spinning temperature：287℃；
Chilling temperature：23℃；
Winding speed：2550m/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 105.0%, extension at break CV value 5.7%；
By polyester slice through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique：
Spinning temperature：285℃；
Chilling temperature：21℃；
Network pressure：0.20MPa；
One roller speed：2600m/min；
One roll temperature：77℃；
Two roller speeds：3800m/min；
Two roll temperatures：120℃；
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, heating stretching, false twisting, thermal finalization and volume
Imitative cotton abnormal contraction composite filament is obtained around shaping；
Compound filament processing process：
Spin fast 400m/min；
Sizing over feed rate(OFR) 5.50%；
Winding over feed rate(OFR) 4.0；
T1：200℃；
T2：130℃；
DR：1.7；
D/Y:1.9；
Network pressure：0.20MPa；
Gained imitates cotton abnormal contraction composite filament under the conditions of temperature is 110 DEG C, the free volume space of interior molecules interchain
Increase 24v/v%, fineness-unevenness rate CV value 0.9%, fracture strength 2.8cN/dtex, fracture strength CV value 6.1%, fracture is stretched
Long rate is 17.5%, extension at break CV value 8.9%, and boiling water shrinkage is 3.0%, and crimp contraction is 6.8%, crimp contraction
Coefficient of variation CV value 8.1%, oil content is 3.5%, fiber number：120dtex, internet pricing is 14/m.
After described imitative cotton abnormal contraction composite filament is dyeed, the dye uptake of acquisition is as shown in the table：
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 50.1 | 82.4 | 92.6 | 92.5 | 92.2 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 52.3 | 87.9 | 93.4 | 92.4 | 93.4 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 45.4 | 74.0 | 86.0 | 87.8 | 90.8 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Embodiment 7
A kind of preparation method of modified poly ester, comprises the following steps：
(1) preparation of amino ethylene glycol fatty acid：
1) by tetracontane dicarboxylic acids and methyl alcohol with 1:The amount of 1.5 mol ratios adds in reactor, under the catalysis of the concentrated sulfuric acid,
It is heated to 100 DEG C, refuxing esterification, cooling, separating-purifying obtains tetracontane mono methyl dicarboxylate；The described concentrated sulfuric acid refers to that quality is dense
Spend the sulfuric acid for 70%, concentrated sulfuric 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 for 0.06mol/L under nitrogen atmosphere, is reacted at 80 DEG C, backflow, produces when no longer there being gas
When raw, add a certain amount of dilute sulfuric acid to 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 sulfuric acid that mass concentration is 48%, and dilute sulfuric acid addition is tetracontane dicarboxylic acids list first
The 2wt% of ester；
3) by the ammoniacal liquor of bromo nonatriacontane carboxylic acid and 22wt% in molar ratio 1:2 are added in reactor, and stirring, in room
Temperature is lower to react, then product is heated distillation, and absorbs ammonia with cold water, and the temperature of heating distillation is 60 DEG C, until no gas
Bubble produces, that is, stop distillation, then cooled down and suction filtration, and filter cake deionized water is washed till no till bromide ion, using nitric acid
Silver-colored solution detection, product vacuum drying is obtained product amino nonatriacontane carboxylic acid；
4) by ethylene glycol and amino nonatriacontane carboxylic acid in molar ratio for 1.1:2 stir, and press amino nonatriacontane
2% addition concentration of carboxylic acid weight is the sulfuric acid of 46wt%, carries out esterification, esterification reaction temperature is 190 DEG C, and esterification water evaporates
Output reach theoretical value more than 90% be esterification terminal；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：
It is 1 using mol ratio:1.8 terephthalic acid (TPA) 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 in 0.2MPa, temperature, at 258 DEG C, is esterified Stress control
Water quantity of distillate reach theoretical value more than 90% be esterification terminal；
Described polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the described polycondensation reaction low vacuum stage, esterification products add the 0.05% of terephthalic acid (TPA) weight antimony acetate
With the trimethyl phosphate of terephthalic acid (TPA) weight 0.03%, start polycondensation reaction under conditions of negative pressure, this staged pressure is by normal
Flatten and be surely evacuated to below absolute pressure 500Pa, at 268 DEG C, the reaction time is 45 minutes to temperature control；
Add amino nonatriacontane carboxylic acid glycol ester after the described polycondensation reaction low vacuum stage terminates, and stir 16 points
Clock；Described amino nonatriacontane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 1.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure
Power is down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 75 minutes reaction time；
Prepared modified poly ester, viscosity average molecular weigh is 25000；
(3) imitate the preparation of cotton abnormal contraction composite filament：
By modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk；
Modified poly ester POY yarn spinning technique：
Spinning temperature：286℃；
Chilling temperature：23℃；
Winding speed：2800m/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, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk；
Modified poly ester FDY yarn spinning technique：
Spinning temperature：285℃；
Chilling temperature：22℃；
Network pressure：0.30MPa；
One roller speed：2400m/min；
One roll temperature：79℃；
Two roller speeds：3650m/min；
Two roll temperatures：123℃；
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, heating stretching, false twisting, thermal finalization and volume
Imitative cotton abnormal contraction composite filament is obtained around shaping；
Compound filament processing process：
Spin fast 600m/min；
Sizing over feed rate(OFR) 3.5%；
Winding over feed rate(OFR) 3.0；
T1：190℃；
T2：140℃；
DR：1.5；
D/Y:2.2；
Network pressure：0.10MPa；
Gained imitates cotton abnormal contraction composite filament under the conditions of temperature is 120 DEG C, the free volume space of interior molecules interchain
Increase 27v/v%, fineness-unevenness rate CV value 1.0%, fracture strength 2.7cN/dtex, fracture strength CV value 6.3%, fracture is stretched
Long rate is 14.0%, extension at break CV value 8.8%, and boiling water shrinkage is 3.8%, and crimp contraction is 5.5%, crimp contraction
Coefficient of variation CV value 8.4%, oil content is 2.7%, fiber number：135dtex, internet pricing is 12/m.
After described imitative cotton abnormal contraction composite filament is dyeed, the dye uptake of acquisition is as shown in the table：
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 50.8 | 82.1 | 91.8 | 92.7 | 91.8 |
| General fibre | 29.1 | 48.4 | 80.3 | 84.2 | 90.7 | |
| Disperse blue SE-2R | Modified fibre | 52.9 | 87.7 | 93.0 | 92.7 | 93.1 |
| General fibre | 16.3 | 38.2 | 76.9 | 89.7 | 92.6 | |
| Disperse bright blue S-GL | Modified fibre | 45.7 | 74.8 | 86.5 | 88.0 | 90.6 |
| General fibre | 14.3 | 39.2 | 73.4 | 76.7 | 84.6 |
Claims (9)
1. a kind of imitative cotton abnormal contraction composite filament, is characterized in that：Described imitative cotton abnormal contraction composite filament be modified poly ester POY silk with
The composite filament through mixed fine processing composition for the modified poly ester FDY silk, described modified poly ester POY silk formed tiny wire ring be centered around described in change
Around property polyester FDY silk；Described modified poly ester is made up of with amino ethylene glycol fatty acid polyester, described amino aliphatic acid second two
Alcohol ester is dispersed in the molecule interchain of described polyester, and described amino ethylene glycol fatty acid has hydrogen with the molecule interchain of described polyester
Key acts on, and so that described amino ethylene glycol fatty acid and the relative position of the strand of described polyester is fixed；Described imitative cotton is different
Under the conditions of temperature is 90～130 DEG C, the free volume space of fibrous inside molecule interchain increases 10～30v/ to contraction composite filament
V%；Fracture strength >=the 2.0cN/dtex of described imitative cotton abnormal contraction composite filament, elongation at break is 18.0 ± 3.0%, curling
Shrinkage factor is 4.8 ± 3.0%, and internet pricing is 15 ± 5/m；
The percentage by weight that described amino ethylene glycol fatty acid accounts for described imitative cotton abnormal contraction composite filament is 0.5～2.5%, institute
The molecular structure stating amino ethylene glycol fatty acid is：
H2N(CH2)nCOOCH2CH2OOC(CH2)nNH2；
Wherein, n=10-50.
2. a kind of imitative cotton abnormal contraction composite filament according to claim 1 is it is characterised in that the different contraction of described imitative cotton is multiple
Fineness-unevenness rate CV value≤1.4% of plying, fracture strength CV value≤7.0%, extension at break CV value≤9.0%, boiling water is received
Shrinkage is 3.0 ± 1.0%, crimp contraction coefficient of variation CV value≤9.0%, and oil content is 3.0 ± 1.0%, fiber number：75-
150dtex；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 100.0 ± 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%.
3. a kind of preparation method of imitative cotton abnormal contraction composite filament as claimed in claim 1, it is characterized in that by polyester through metering,
Extrude, cool down, oil and wind, prepared POY silk；By polyester slice through measuring, extruding, cool down, oil, stretch, thermal finalization and
Winding, prepared FDY silk；POY silk and FDY are obtained imitative cotton through plying network, heating stretching, false twisting, thermal finalization and coiling and molding
Abnormal contraction composite filament；
Modified poly ester POY yarn spinning technique：
Spinning temperature：280-290℃；
Chilling temperature：20-25℃；
Winding speed：2550-2880m/min；
Modified poly ester FDY yarn spinning technique：
Spinning temperature：280-290℃；
Chilling temperature：20-25℃；
Network pressure：0.20-0.30MPa；
One roller speed：2200-2600m/min；
One roll temperature：75-85℃；
Two roller speeds：3600-3900m/min；
Two roll temperatures：115-135℃；
Winding speed：3600-3800m/min；
Compound filament processing process：
Spin fast 400-800m/min；
Sizing over feed rate(OFR) 3.5-5.50%；
Winding over feed rate(OFR) 2.5-5.0%；
Heating-up temperature：150-220℃；
Heat setting temperature：100-180℃；
Draw ratio：1.5-1.9；
The superficial velocity of frictional disk and strand leave the ratio of the speed of scroll tube:1.7-2.2；
Network pressure：0.05-0.3MPa；
The preparation process of described modified poly ester includes：
(1) preparation of amino ethylene glycol fatty acid：
1) by binary of fatty acids and methyl alcohol with 1:The amount of 1.5 mol ratios adds in reactor, under the catalysis of the concentrated sulfuric acid, is 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 one of to dopentacontane dicarboxylic acids；
2) by described binary of fatty acids mono-methyl, lead tetraacetate and lithium bromide in molar ratio 1:1:1 is dissolved in benzene, wherein binary fat
The concentration of fat acid mono-methyl is 0.05～0.1mol/L, under nitrogen atmosphere, reacts at 80～90 DEG C, backflow, when no longer there being gas
When body produces, add the sulfuric acid reaction that mass concentration is 40～50% 2～3 hours, be washed out, purify and be dried, produced
Thing bromo aliphatic acid；
3) by the ammoniacal liquor of bromo aliphatic acid and 15～25wt% in molar ratio 1:2 are added in reactor, stirring, at room temperature instead
Should, then product is heated distillation, and absorb ammonia with cold water, the temperature of heating distillation is less than 70 DEG C, until bubble-free
Produce, that is, stop distillation, then cooled down and suction filtration, filter cake deionized water is washed till no till bromide ion, by product vacuum
It is dried to obtain product amino aliphatic acid；
4) by ethylene glycol and amino aliphatic acid in molar ratio for 1.1:2 stir, and press the 1～3% of amino fatty acid wt
The sulfuric acid adding concentration to be 40～50wt%, carries out esterification, and 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：
Using terephthalic acid (TPA) and ethylene glycol as raw material, carry out esterification after being made into uniform sizing material, obtain esterification products；Ester
Change reaction to pressurize in nitrogen atmosphere, in normal pressure～0.3MPa, at 250～260 DEG C, esterification water quantity of distillate reaches temperature Stress control
It is esterification terminal to more than the 90% of theoretical value；
Described polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the described polycondensation reaction low vacuum stage, in esterification products, add catalyst and stabilizer, start under conditions of negative pressure
Polycondensation reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature control, at 260～270 DEG C, is reacted
Time is 30～50 minutes；
Add amino ethylene glycol fatty acid after the described polycondensation reaction low vacuum stage terminates, and stir；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and so that reaction pressure is dropped
It is less than 100Pa to absolute pressure, reaction temperature controls at 275～280 DEG C, 50～90 minutes reaction time；
Prepared modified poly ester.
4. a kind of preparation method of imitative cotton abnormal contraction composite filament according to claim 3 is it is characterised in that described second two
Alcohol is 1.2～2.0 with the mol ratio of described terephthalic acid (TPA):1.
5. a kind of preparation method of imitative cotton abnormal contraction composite filament according to claim 3 is it is characterised in that described catalysis
Agent is selected from one of antimony oxide, antimony glycol and antimony acetate, and catalyst amount is described terephthalic acid (TPA) weight
0.01%～0.05%.
6. a kind of preparation method of imitative cotton abnormal contraction composite filament according to claim 3 is it is characterised in that described stable
Agent is selected from one of triphenyl phosphate, trimethyl phosphate and Trimethyl phosphite, and stabilizing agent dosage is described terephthalic acid (TPA)
The 0.01%～0.05% of weight.
7. a kind of preparation method of imitative cotton abnormal contraction composite filament according to claim 3 is it is characterised in that add amino
Stirring after ethylene glycol fatty acid, the time is 15～20 minutes.
8. a kind of preparation method of imitative cotton abnormal contraction composite filament according to claim 3 is it is characterised in that use deionization
It is washed to no till bromide ion, described bromide ion adopts silver nitrate solution to detect.
9. a kind of preparation method of imitative cotton abnormal contraction composite filament according to claim 3 is it is characterised in that described dense sulphur
Acid refers to the sulfuric acid that mass concentration is 70～80%, and concentrated sulfuric acid addition is 1～3wt% of binary of fatty acids；Described dilute sulfuric acid
Addition is 1～3wt% of binary of fatty acids mono-methyl.
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| CN105506774B (en) * | 2015-12-29 | 2017-12-12 | 江苏恒力化纤股份有限公司 | A kind of low aberration polyester abnormal contraction composite filament and preparation method thereof |
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| 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 |
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| JPS6245720A (en) * | 1985-08-26 | 1987-02-27 | Kuraray Co Ltd | Production of polyester yarn having improved fastness to light |
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| CN101575745A (en) * | 2008-05-07 | 2009-11-11 | 东丽纤维研究所（中国）有限公司 | Heavy denier polyester fiber and production method thereof |
| CN101906678A (en) * | 2010-08-19 | 2010-12-08 | 中国纺织科学研究院 | Modified polyester complex fiber and preparation method thereof |
| CN103320923A (en) * | 2013-05-22 | 2013-09-25 | 浙江恒逸高新材料有限公司 | Method for producing cationic type composite cotton yarn imitation threads |
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| JPS581133B2 (en) * | 1974-05-20 | 1983-01-10 | 東レ株式会社 | High quality polyester |
| JPS6245720A (en) * | 1985-08-26 | 1987-02-27 | Kuraray Co Ltd | Production of polyester yarn having improved fastness to light |
| CN1940156A (en) * | 2005-09-30 | 2007-04-04 | 厦门翔鹭化纤股份有限公司 | Production of wool-imitated special silk |
| CN101575745A (en) * | 2008-05-07 | 2009-11-11 | 东丽纤维研究所（中国）有限公司 | Heavy denier polyester fiber and production method thereof |
| CN101906678A (en) * | 2010-08-19 | 2010-12-08 | 中国纺织科学研究院 | Modified polyester complex fiber and preparation method thereof |
| CN103320923A (en) * | 2013-05-22 | 2013-09-25 | 浙江恒逸高新材料有限公司 | Method for producing cationic type composite cotton yarn imitation threads |
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| CN104562340A (en) | 2015-04-29 |
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