CN106381551A - Porous soft flax-like polyester fiber and preparation method thereof - Google Patents

Porous soft flax-like polyester fiber and preparation method thereof Download PDF

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Publication number
CN106381551A
CN106381551A CN201610788731.6A CN201610788731A CN106381551A CN 106381551 A CN106381551 A CN 106381551A CN 201610788731 A CN201610788731 A CN 201610788731A CN 106381551 A CN106381551 A CN 106381551A
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Prior art keywords
phthalic acid
modified poly
preparation
poly ester
porous
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CN106381551B (en
Inventor
范红卫
马文平
沈建根
王锋宾
孙晓华
杨超明
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Jiangsu Hengli Chemical Fiber Co Ltd
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Jiangsu Hengli Chemical Fiber Co Ltd
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16—Dicarboxylic acids and dihydroxy compounds
    • C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/181—Acids containing aromatic rings
    • C08G63/183—Terephthalic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78—Preparation processes
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D4/00—Spinnerette packs; Cleaning thereof
    • D01D4/02—Spinnerettes
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/08—Melt spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Polyesters Or Polycarbonates (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention relates to a porous soft flax-like polyester fiber and a preparation method thereof; the porous soft flax-like polyester fiber is prepared by spinning modified polyester through a porous spinneret plate; an arrangement way of spinneret holes in the porous spinneret plate is in oval arrangement, that is to say, a hole center of the spinneret holes is located in concentric ellipses, the concentric ellipses are a series of ellipses, the long axes of all the ellipses are collinear, and the short axes are collinear. The porous soft flax-like polyester fiber is prepared by processing modified polyester POY filaments and modified polyester FDY filaments, wherein a preparation method for the modified polyester comprises the steps: carrying out a reaction of terephthalic acid and ethylene glycol to prepare ethylene glycol terephthalate, adding terephthalic acid and branched chain-containing dihydric alcohol, carrying out a reaction to prepare dihydric alcohol terephthalate, and continuing to carry out reaction to obtain the modified polyester. The prepared fiber is excellent in properties, the linear density deviation rate is less than or equal to 2.0%, the CV value of breaking strength is less than or equal to 4.0%, the CV value of elongation at break is less than or equal to 8.0%, and the CV value of the crimp shrinking percentage variation coefficient is less than or equal to 8.0%.

Description

Soft imitative fiber crops polyester fiber of a kind of porous and preparation method thereof
Technical field
The invention belongs to field of polyester fiber, it is related to soft imitative fiber crops polyester fiber of a kind of porous and preparation method thereof.
Background technology
Polyethylene terephthalate (PET or polyester fiber) fiber since the advent of the world, have fracture strength and Elastic modelling quantity is high, and resilience is moderate, and thermal finalization is excellent, and heat-resisting light resistance is good and acid-fast alkali-proof corrosion resistance etc. is a series of excellent Performance, and fabric has wash and wear, the advantages of stiffness is good, is widely used in the fields such as clothing, home textile.
But because the degree of crystallinity of PET is high, the functional group that compact structure, and strand are not combined with dyestuff, cause Dye molecule hardly enters fibrous inside, and dyeing is difficult.People cannot be met to bright-coloured beautiful, unique style fabric demand.
PET dyeing is caused to belong to symmetric straight chain macromolecular for PET the reason difficult, strand does not contain side chain radical Group, regularity is very good, and its main chain contains rigid phenyl ring and flexible alkyl, and the ester group being directly connected with phenyl ring and Phenyl ring constitutes rigid conjugated system again, thus constraining rotating freely of its soft segment.Such a structure increases molecule The wall ridge of sub-chain motion, leads to the glass transition temperature of PET higher, needs to promote dye molecule under very high temperature conditionss To the diffusion of fibrous inside, complete staining procedure.In addition, the strand of PET is regular, good crystallinity, molecule chain alignment is tight, and And the polar group not having an effect with dye molecule on strand, make the colouring of PET more difficult.
Therefore, under the general High Temperature High Pressure of the dyeing of common PET, select disperse dyeing, when temperature reaches PET When fiber obtains more than vitrification point, between PET polymer molecule, space increases, but the degree that its free volume increases is little, Dyeing rate is not high, but the energy consumption brought of high temperature and high pressure method and dye-uptake low be the subject matter facing now.In addition, PET melt viscosity is higher, is unfavorable for processing.
The method of preparation PET is a lot, and wherein melt spinning method is more one kind in current commercial production application.Molten Melt and in spinning process, have many parameters, these parameters determine the course of fiberizing and spin structure and the performance of fiber, produce Upper is exactly the fiber of desired properties to be obtained by controlling these parameters.The main spinning that can control in producing according to technical process Silk summary of parameters.An is melting condition, spinning conditions, condition of cure, wrapping wire condition etc., and wherein strand cooling and solidifying condition is to fiber Structure and performance have conclusive impact, for controlling rate of cooling and its uniformity of polyester fondant thread, generally adopt in production Take cooling blowing.Cooling blowing can accelerate the rate of cooling of melt stream, is conducive to improving spinning speed；Strengthen empty around strand The convection current of gas, makes ectonexine strand cool down uniformly, is to create condition using porous spinneret；Cooling blowing can make as-spun fibre Quality advance, tensile property improves, and is conducive to the production capacity of raising equipment.
Experimental branch line all adopts cross air blasting as the type of cooling for a long time, and energy resource consumption accounts for long filament production cost very Major part, increasingly improves to chemical fibre performance and quality requirements with people, and the exploitation of chemical-fibres filaments new product is to high added value The cooling blowing condition it is desirable to higher is developed in fibre in differentiation direction, then proposes ring blowing device.Ring blowing device is not only Possess the uniform advantage of every synnema wind-engaging, and energy consumption is compared relatively low, effectively solves cross air blasting because blowing area is big The wind energy loss problem causing.
In spinning process, although ring blowing has obvious advantage, still have problems：Due to spun silk from After circular spinneret extrusion, by ring wind quenching, due to the circular spinneret number of turns more so that ring blowing hardly enter interior Layer, leads to that the silk of innermost layer may be also uncolled after cooling in outermost silk, thus the silk of gained fiber number irregular, Intensity is irregular, the problems such as uneven dyeing, cause follow-up to silk be processed further difficulty occurs.
Imitative linen look abnormal contraction composite filament is the long filament with different potential shrinkages, i.e. lower shrinkage silk POY and high convergency 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 handss Sense.PET imitates the outer existing similar with common long filament of linen look 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 linen look 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
The purpose of the present invention is to overcome the problems such as existing dyeing polyester fibers are irregular, mechanical property is poor, realizes extensive The production spinning changed, provides soft imitative fiber crops polyester fiber of a kind of porous and preparation method thereof.The raw material of the polyester fiber of the present invention For modified poly ester, in the strand of modified poly ester, introduce the dihydroxylic alcohols segment containing side chain, the porous of modified polyester preparation is soft Imitative fiber crops polyester fiber, under the conditions of uniform temperature, the increase of the spatial joint clearance of the soft imitative fiber crops polyester fiber interior molecules interchain of porous Amplitude is far longer than unbranched conventional polyester fiber at equal temperature, is conducive to the journey within the entrance of the molecules such as stain Degree, improves dyeing rate；The melt viscosity of the soft imitative fiber crops polyester fiber of porous reduces, and reduces processing temperature, reduces degradation rate, Be conducive to processing；The structural regularity of the other dihydroxylic alcohols segment imitative fiber crops polyester fiber soft to porous containing side chain does not have big breaking Bad, maintain the premium properties of polyester fiber.The spinneret of spinneret orifice oval shaped arrangements is adopted, favorably in spinning process of the present invention Uniform, sufficiently cool in spinning process in fiber, performance between fiber and structure difference less, improve the dye of fiber Color uniformity and mechanical property.
For reaching above-mentioned purpose, the technical solution used in the present invention is：
A kind of soft imitative fiber crops polyester fiber of porous, the material of the soft imitative fiber crops polyester fiber of described porous is modified poly ester, institute State modified poly ester form by p-phthalic acid segment, ethylene glycol segment and containing the dihydroxylic alcohols segment of side chain, described containing side chain two First alcohol segment refers to that side chain is located on one of dihydroxylic alcohols segment non-end group carbon and side chain is straight containing 5-10 carbon atom The dihydroxylic alcohols segment of chain carbochain；
The fiber number of the soft imitative fiber crops polyester fiber of described porous is 75-150dtex, initial moduluss≤80cN/dtex, and fracture is strong Degree >=3.0cN/dtex, elongation at break is 40.0 ± 3.0%, and crimp contraction is 3.50 ± 2.0%, and internet pricing is 95 ± 5 Individual/m；At temperature is 80～130 DEG C, the spatial joint clearance of fibrous inside molecule interchain increases the soft imitative fiber crops polyester fiber of described porous Big 10～30v/v%；Line density deviation ratio≤2.0% of the soft imitative fiber crops polyester fiber of described porous, fracture strength CV value≤ 4.0%, extension at break CV value≤8.0%, crimp contraction coefficient of variation CV value≤8.0%, boiling water shrinkage be 10.0 ± 1.0%.
Present invention also offers a kind of preparation method of the soft imitative fiber crops polyester fiber of porous, modified poly ester is adopted porous to spray Filament plate spinning is obtained the soft imitative fiber crops polyester fiber of porous；On described porous spinneret, the arrangement mode of spinneret orifice is oval row Row, described oval shaped arrangements refer to that the hole of spinneret orifice is centrally located on concentration ellipse, and described concentration ellipse is that series is oval, owns Oval major axis is conllinear, and short axle is conllinear；
The preparation method of the soft imitative fiber crops polyester fiber of described porous is：By modified poly ester through measuring, extruding, cool down, oil And winding, prepared modified poly ester POY silk；By Modified polyester chips through measuring, extruding, cool down, oil, stretch, thermal finalization and volume Around prepared modified poly ester FDY silk；Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, heating stretching, vacation Twist with the fingers, thermal finalization and coiling and molding are obtained the soft imitative fiber crops polyester fiber of porous；
The preparation process of described modified poly ester is：
(1) preparation of p-phthalic acid binary alcohol esters；
P-phthalic acid is made into after slurry with the dihydroxylic alcohols containing side chain, under the catalytic action of concentrated sulphuric acid, is esterified Reaction obtains p-phthalic acid binary alcohol esters；It is non-that the described dihydroxylic alcohols containing side chain refer to that side chain is located at one of dihydroxylic alcohols segment On end group carbon and side chain is the dihydroxylic alcohols of the linear carbon chain containing 5-10 carbon atom；
For the dihydroxylic alcohols containing side chain, its side chain is alkyl, is electron withdraw group, in the presence of side chain, makes strand Spatial volume increases, and solvation diminishes, and in dihydroxylic alcohols, proton is difficult to dissociate so that containing dihydroxylic alcohols and the terephthaldehyde of side chain The reactivity of acid is less than ethylene glycol, according to the mixing of same ethylene glycol and terephthaldehyde's acid reaction, can cause the binary containing side chain Alcohol reaction is imperfect, thus ratio in polyester macromolecule for the dihydroxylic alcohols containing side chain for the impact, and then affect the performance of polyester.This Using first the dihydroxylic alcohols containing side chain being carried out esterification with p-phthalic acid under the catalytic action of sulphuric acid, its product exists for invention Ethylene glycol and p phthalic acid esterification add it is ensured that containing the stability of the dihydroxylic alcohols proportioning of side chain after terminating；
(2) preparation of ethylene glycol terephthalate；
P-phthalic acid and ethylene glycol are made into after slurry, carry out esterification, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stir Mix mixing, in the presence of catalyst and stabilizer, under conditions of negative pressure, carry out successively the coarse vacuum stage polycondensation reaction and The polycondensation reaction of high vacuum stage of Fig, prepared modified poly ester.
As preferred technical scheme：
The preparation method of the soft imitative fiber crops polyester fiber of a kind of porous as above, the concrete preparation step of described modified poly ester Suddenly it is：
(1) preparation of p-phthalic acid binary alcohol esters；
P-phthalic acid is made into slurry with the dihydroxylic alcohols containing side chain, under the catalytic action of concentrated sulphuric acid, carries out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure～0.3MPa, and temperature is 180～240 DEG C, works as ester It is esterification terminal that water quantity of distillate in change reaction reaches during more than the 90% of theoretical value, obtains p-phthalic acid dihydroxylic alcohols Ester；
(2) preparation of ethylene glycol terephthalate；
P-phthalic acid and ethylene glycol are made into after slurry, carry out esterification, esterification is pressurizeed in nitrogen atmosphere Reaction, moulding pressure is normal pressure～0.3MPa, and temperature is 250～260 DEG C, when the water quantity of distillate in esterification reaches theoretical value More than 90% when be esterification terminal, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stir Mix mixing 15-20 minute, in the presence of catalyst and stabilizer, the polycondensation starting the coarse vacuum stage under conditions of negative pressure is anti- Should, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 260～270 DEG C, the response time is temperature control 30～50 minutes；Then proceed to evacuation, carry out the polycondensation reaction of high vacuum stage of Fig, make reaction pressure be down to absolute pressure and be less than 100Pa, reaction temperature controls at 275～280 DEG C, 50～90 minutes response time, prepared modified poly ester；
The main spinning technology parameter of described modified poly ester POY silk is：
Spinning temperature：280-290℃；
Chilling temperature：23-27℃；
Winding speed：2300-2500m/min；
The main spinning technology parameter of described modified poly ester FDY silk is：
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：3650-3850m/min；
Two roll temperatures：115-135℃；
Winding speed：3600-3800m/min；
The main spinning technology parameter of the soft imitative fiber crops polyester fiber of described porous is：
Spin speed：400-800m/min；
Sizing over feed rate(OFR)：3.5-5.50%；
Winding over feed rate(OFR)：2.5-5.0%；
T1：160-220℃；
T2：180-220℃；
DR：1.6-1.8；
D/Y:1.6-2.0；
Network pressure：0.05-0.3MPa.
The preparation method of the soft imitative fiber crops polyester fiber of a kind of porous as above, in step (1), p-phthalic acid with contain The mol ratio of the dihydroxylic alcohols of side chain is 1:1.3-1.5；Concentrated sulphuric acid addition is the 0.3-0.5% of p-phthalic acid weight；Described The concentration of concentrated sulphuric acid is 50-60wt%；
In step (2), p-phthalic acid is 1 with the mol ratio of ethylene glycol:1.2～2.0；
In step (3), described p-phthalic acid binary alcohol esters are 2 with the Mole percent ratio of ethylene glycol terephthalate ～5%；Described catalyst is antimony oxide, antimony glycol or antimony acetate, and catalyst charge is p-phthalic acid gross weight 0.01%～0.05%；Described stabilizer is triphenyl phosphate, trimethyl phosphate or NSC 6513, stabilizer addition For described p-phthalic acid gross weight 0.01%～0.05%；
The number-average molecular weight of described modified poly ester is 15000～30000.
The preparation method of the soft imitative fiber crops polyester fiber of a kind of porous as above, the described dihydroxylic alcohols containing side chain are 2- penta Base -1,4 butanediol, 2- hexyl -1,4 butanediol, 2- heptyl -1,4 butanediol, 2- octyl group -1,4 butanediol, 2- nonyl -1,4 fourth Glycol, 2- decyl -1,4 butanediol, 2- amyl group -1,5 pentanediol, 2- hexyl -1,5 pentanediol, 2- heptyl -1,5 pentanediol, 2- are pungent One or more of base -1,5 pentanediol, 2- nonyl -1,5 pentanediol or 2- decyl -1,5 pentanediol.
The preparation method of the soft imitative fiber crops polyester fiber of a kind of porous as above, described spinneret orifice be arranged as major axis And/or short axle is symmetrical.
The preparation method of the soft imitative fiber crops polyester fiber of a kind of porous as above, the ratio of oval major axis and minor axis length It is worth for 1.3～1.8；The guide hole diameter that the spacing of adjacent spinneret orifice is more than or equal to spinneret orifice adds 1.5mm.Effective when spinneret Simultaneously as the girth of ellipse is more than circular girth, the number of plies of spinneret orifice oval shaped arrangements is less than circular arrangement to area phase The number of plies, the hole count of spinneret orifice oval shaped arrangements is more than the hole count of circular arrangement, and therefore, spinneret orifice oval shaped arrangements are conducive to ring The cooling of blowing, improves the cooling effectiveness of ring blowing, and the fibre property of preparation is also more excellent.Major axis and the ratio of minor axis length It is closer to 1, ellipse is more similar to justify, and the difference of cooling effectiveness and cooling effect is little；Major axis with the ratio of minor axis length is When 1.3, cooling effect significantly improves, and individual pen hole count is corresponding to increase by 16%；When the ratio of major axis and minor axis length is 1.8, cooling Effect improves larger, the corresponding increase by 33% of individual pen hole count, and in the case of identical hole count, the oval shaped arrangements of the present invention compare conventional concentric The number of turns of circle best-fit reduces it is easy to cooling wind thoroughly, makes the fiber cooling condition of Internal and external cycle evenly；Major axis and minor axis length When ratio is more than 1.8, ellipse is partial to form flat shape, is difficult to punch, cooling no longer raises.Therefore, it is The oval major axis of row is 1.3～1.8 with the ratio of minor axis length, can reach higher cooling effectiveness and preferable cooling effect Really.
The preparation method of the soft imitative fiber crops polyester fiber of a kind of porous as above, described spinneret be circular spinneret or Elliptical spinneret plate；The diameter of described circle spinneret is more than 10mm with the difference of the oval maximum long axis length of series, described Elliptical spinneret plate is more than 10mm with the difference of the oval maximum long axis length of series.
The preparation method of the soft imitative fiber crops polyester fiber of a kind of porous as above, the guide hole of described spinneret orifice is a diameter of 1.5～2.5mm；The spray webbing hole count of described spinneret is more than or equal to 192.
The preparation method of the soft imitative fiber crops polyester fiber of a kind of porous as above, the horizontal stroke of the spinneret orifice of described spinneret Cross sectional shape is circle, square, rhombus, yi word pattern, triangular form, trilobal cross, hollow type or platypelloid type.
The principle of the present invention is：
For unbranched polyester fiber, its molecular chain structure is the linear macromolecule containing benzene ring structure, on strand Functional group's marshalling, regularity is good, flexible poor；When temperature raises, its free volume increments is little, and these characteristics hinder Hinder dyestuff to enter inside polyester fiber, thus dyeability is poor.
The raw material of the polyester fiber of the present invention is modified poly ester, the dihydroxylic alcohols containing side chain containing in modified poly ester macromole Segment, when temperature is higher than vitrification point, side chain, prior to backbone motion, makes the increasing degree of free volume be far longer than and no props up The characteristic of the polyester macromolecule chain of chain, the increase of free volume improves the degree within molecule entrance polyester, modified The free volume of the polyester fiber of polyester preparation is far longer than unbranched polyester fiber at equal temperature, increases the diffusion of dyestuff Degree, improves the dyeability of polyester fiber.Meanwhile, the polyester fiber of modified poly ester preparation advantageously reduces melt viscosity, has It is beneficial to improve its processing characteristics.The introducing of the dihydroxylic alcohols segment containing side chain does not have big destruction to polyester fiber structures regularity, Maintain the premium properties of polyester fiber.
When the effective area phase of spinneret is simultaneously as the girth of ellipse is more than circular girth, spinneret orifice is oval The number of plies of arrangement is less than the number of plies of circular arrangement, and the hole count of spinneret orifice oval shaped arrangements is more than the hole count of circular arrangement, using spray The spinneret of silk hole oval shaped arrangements enables to that fiber is quick, uniformly cools down, and between fiber, the difference of structure and performance is less, Be conducive to improving the even dyeing rate of fiber and the performance of fiber.
Beneficial effect：
1) on the spinneret of the present invention, the arrangement mode of spinneret orifice is oval shaped arrangements, and the effective area of spinneret is identical When, the number of plies of spinneret orifice oval shaped arrangements is less than the number of plies of circular arrangement, and ring blowing is easier to blow through dynamic analysis of spinning, dynamic analysis of spinning Cooling effect more preferably, the fibre property of preparation is also more excellent.
2) on the spinneret of the present invention, the arrangement mode of spinneret orifice is oval shaped arrangements, and the effective area of spinneret is identical When, the hole count of spinneret orifice oval shaped arrangements is more than the hole count of circular arrangement, and oval shaped arrangements are capable of greatly cooling down, Significantly improve cooling effectiveness.
3) material of the soft imitative fiber crops polyester fiber of porous that the present invention is obtained is modified poly ester, contains in modified poly ester macromole The dihydroxylic alcohols segment containing side chain having, when temperature is higher than vitrification point, side chain, prior to backbone motion, makes the increasing of free volume Plus amplitude is far longer than the characteristic of unbranched polyester macromolecule chain, the increase of free volume improves molecule and enters polyester Internal degree, increases the diffusion of dyestuff by the free volume that side chain increased polyester fiber, improves polyester fiber Dyeability.
4) the soft imitative fiber crops polyester fiber of the present invention is obtained porous, the increase of polyester fiber free volume advantageously reduces molten Body viscosity, is conducive to improving its processing characteristics.
5) the soft imitative fiber crops polyester fiber of the present invention is obtained porous, the introducing of the dihydroxylic alcohols segment containing side chain to polyester fine The structural regularity of dimension does not have big destruction, maintains the premium properties of polyester fiber.
6) present invention is obtained the soft imitative fiber crops dyeing polyester fibers performance of porous and good mechanical performance, initial moduluss≤ 80cN/dtex, line density deviation ratio≤2.0% of the soft imitative fiber crops polyester fiber of porous, fracture strength CV value≤4.0%, fracture Elongation CV value≤8.0%, crimp contraction coefficient of variation CV value≤8.0%.
Brief description
Fig. 1 is the oval shaped arrangements figure of 374 spinneret orifices, and the aperture of spinneret orifice is 2.0mm, the length of transverse and short axle Degree ratio is 1.3；
Fig. 2 is the circular arrangement figure of 370 spinneret orifices, and the aperture of spinneret orifice is 2.0mm；
Fig. 3 is the oval shaped arrangements figure of 382 spinneret orifices, and the aperture of spinneret orifice is 2.0mm, the length of transverse and short axle Degree ratio is 1.6.
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.
Embodiment 1
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.3 p-phthalic acid and 2- amyl group-Isosorbide-5-Nitrae butanediol are made into slurry and add in reactor, Concentration is 50wt%, and addition is under the catalytic action of 0.3% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure, and temperature is 180 DEG C, when the water in esterification distillates It is esterification terminal that amount reaches during the 90% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.2 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure, and temperature is 250 DEG C, when the water in esterification distillates It is esterification terminal that amount reaches during the 90% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 2% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 15 minutes is adding Measure for p-phthalic acid weight 0.01% the catalytic antimony trioxide and addition be p-phthalic acid weight 0.01% Stabilizer triphenyl phosphate in the presence of, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure Steadily being evacuated to absolute pressure by normal pressure is 500Pa, and at 260 DEG C, the response time is 30 minutes to temperature control；Then proceed to take out very Sky, carries out the polycondensation reaction of high vacuum stage of Fig, and making reaction pressure be down to absolute pressure is 100Pa, and reaction temperature controls 275 DEG C, 50 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 15000, by p-phthalic acid segment, ethylene glycol segment and 2- penta Base-Isosorbide-5-Nitrae butanediol segment composition, 2- amyl group-Isosorbide-5-Nitrae butanediol segment is 2% with the Mole percent ratio of ethylene glycol segment.
Table 1：Embodiment 2-12 important technological parameters
Embodiment 2
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 2；In step (3), after adding p-phthalic acid binary alcohol esters, stirring mixing 16 minutes, is p-phthalic acid gross weight in addition 0.011% the catalytic antimony trioxide and addition are the stabilizer triphenyl phosphate of the 0.02% of p-phthalic acid gross weight In the presence of, start the polycondensation reaction in coarse vacuum stage under conditions of negative pressure, this staged pressure is steadily evacuated to definitely by normal pressure Pressure 490Pa, at 262 DEG C, the response time is 31 minutes to temperature control；Then proceed to evacuation, carry out the contracting of high vacuum stage of Fig Poly- reaction, makes reaction pressure be down to absolute pressure 90Pa, reaction temperature controls at 276 DEG C, in 51 minutes response time, modification is obtained Polyester.
The number-average molecular weight of modified poly ester is 16000, and modified poly ester is own by p-phthalic acid segment, ethylene glycol segment and 2- Base-Isosorbide-5-Nitrae butanediol segment composition, 2- hexyl-Isosorbide-5-Nitrae butanediol segment is 2.1% with the Mole percent ratio of ethylene glycol segment.
Embodiment 3
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 3；In step (3), after adding p-phthalic acid binary alcohol esters, stirring mixing 16 minutes, is the 0.03% of p-phthalic acid gross weight in addition The catalytic antimony trioxide and addition be p-phthalic acid gross weight 0.02% stabilizer triphenyl phosphate effect Under, start the polycondensation reaction in coarse vacuum stage under conditions of negative pressure, this staged pressure is steadily evacuated to absolute pressure by normal pressure 498Pa, at 263 DEG C, the response time is 32 minutes to temperature control；Then proceed to evacuation, the polycondensation carrying out high vacuum stage of Fig is anti- Should, make reaction pressure be down to absolute pressure 90Pa, reaction temperature controls at 277 DEG C, in 57 minutes response time, be obtained modified poly- Ester.
The number-average molecular weight of modified poly ester is 15900, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2- heptan Base-Isosorbide-5-Nitrae butanediol segment composition, 2- heptyl-Isosorbide-5-Nitrae butanediol segment is 2.2% with the Mole percent ratio of ethylene glycol segment.
Embodiment 4
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 4；In step (3), after adding p-phthalic acid binary alcohol esters, stirring mixing 17 minutes, is p-phthalic acid gross weight in addition 0.033% the catalytic antimony trioxide and addition are the stabilizer phosphoric acid triphen of the 0.023% of p-phthalic acid gross weight Under conditions of negative pressure, in the presence of ester, start the polycondensation reaction in coarse vacuum stage, this staged pressure is steadily evacuated to absolutely by normal pressure It is 497Pa to pressure, at 264 DEG C, the response time is 33 minutes to temperature control；Then proceed to evacuation, carry out high vacuum stage of Fig Polycondensation reaction, make reaction pressure be down to absolute pressure be 80Pa, reaction temperature controls at 278 DEG C, 58 minutes response time, system Obtain modified poly ester.
The number-average molecular weight of modified poly ester is 15800, and modified poly ester is pungent by p-phthalic acid segment, ethylene glycol segment and 2- Base-Isosorbide-5-Nitrae butanediol segment composition, 2- octyl group-Isosorbide-5-Nitrae butanediol segment is 2.3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 5
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 5；In step (3), after adding p-phthalic acid binary alcohol esters, stirring mixing 17 minutes, is p-phthalic acid gross weight in addition 0.034% the catalytic antimony trioxide and addition are the stabilizer phosphoric acid triphen of the 0.024% of p-phthalic acid gross weight Under conditions of negative pressure, in the presence of ester, start the polycondensation reaction in coarse vacuum stage, this staged pressure is steadily evacuated to absolutely by normal pressure To pressure 496Pa, at 265 DEG C, the response time is 34 minutes to temperature control；Then proceed to evacuation, carry out high vacuum stage of Fig Polycondensation reaction, making reaction pressure be down to absolute pressure is 80Pa, and reaction temperature controls at 277 DEG C, 59 minutes response time, is obtained Modified poly ester.
The number-average molecular weight of modified poly ester is 15900, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2- nonyl Base-Isosorbide-5-Nitrae butanediol segment composition, 2- nonyl-Isosorbide-5-Nitrae butanediol segment is 2.4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 6
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 6；In step (3), after adding p-phthalic acid binary alcohol esters, stirring mixing 18 minutes, is p-phthalic acid gross weight in addition 0.035% the catalytic antimony trioxide and addition are the stabilizer phosphoric acid triphen of the 0.025% of p-phthalic acid gross weight Under conditions of negative pressure, in the presence of ester, start the polycondensation reaction in coarse vacuum stage, this staged pressure is steadily evacuated to absolutely by normal pressure To pressure 495Pa, at 266 DEG C, the response time is 35 minutes to temperature control；Then proceed to evacuation, carry out high vacuum stage of Fig Polycondensation reaction, making reaction pressure be down to absolute pressure is 70Pa, and reaction temperature controls at 278 DEG C, 60 minutes response time, is obtained Modified poly ester.
The number-average molecular weight of modified poly ester is 16000, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and the 2- last of the ten Heavenly stems Base-Isosorbide-5-Nitrae butanediol segment composition, 2- decyl-Isosorbide-5-Nitrae butanediol segment is 2.5% with the Mole percent ratio of ethylene glycol segment.
Embodiment 7
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 7；In step (3), after adding p-phthalic acid binary alcohol esters, stirring mixing 19 minutes, is p-phthalic acid gross weight in addition 0.036% the catalytic antimony trioxide and addition are the stabilizer phosphoric acid triphen of the 0.025% of p-phthalic acid gross weight Under conditions of negative pressure, in the presence of ester, start the polycondensation reaction in coarse vacuum stage, this staged pressure is steadily evacuated to absolutely by normal pressure To pressure 496Pa, at 267 DEG C, the response time is 36 minutes to temperature control；Then proceed to evacuation, carry out high vacuum stage of Fig Polycondensation reaction, making reaction pressure be down to absolute pressure is 70Pa, and reaction temperature controls at 278 DEG C, 61 minutes response time, is obtained Modified poly ester.
The number-average molecular weight of modified poly ester is 16000, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2- penta Base-Isosorbide-5-Nitrae butanediol segment composition, 2- amyl group-Isosorbide-5-Nitrae butanediol segment is 2.6% with the Mole percent ratio of ethylene glycol segment.
Embodiment 8
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 8；In step (3), after adding p-phthalic acid binary alcohol esters, stirring mixing 19 minutes, is p-phthalic acid gross weight in addition 0.036% the catalytic antimony trioxide and addition are the stabilizer phosphoric acid triphen of the 0.025% of p-phthalic acid gross weight Under conditions of negative pressure, in the presence of ester, start the polycondensation reaction in coarse vacuum stage, this staged pressure is steadily evacuated to absolutely by normal pressure To pressure 496Pa, at 267 DEG C, the response time is 36 minutes to temperature control；Then proceed to evacuation, carry out high vacuum stage of Fig Polycondensation reaction, making reaction pressure be down to absolute pressure is 70Pa, and reaction temperature controls at 278 DEG C, 61 minutes response time, is obtained Modified poly ester.
The number-average molecular weight of modified poly ester is 17000, and modified poly ester is own by p-phthalic acid segment, ethylene glycol segment and 2- Base-Isosorbide-5-Nitrae butanediol segment composition, 2- hexyl-Isosorbide-5-Nitrae butanediol segment is 2.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 9
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 9；In step (3), after adding p-phthalic acid binary alcohol esters, stirring mixing 16 minutes, is the 0.04% of p-phthalic acid gross weight in addition Catalyst glycol antimony and addition be p-phthalic acid gross weight 0.026% stabilizer trimethyl phosphate effect Under, start the polycondensation reaction in coarse vacuum stage under conditions of negative pressure, this staged pressure is steadily evacuated to absolute pressure by normal pressure 497Pa, at 268 DEG C, the response time is 38 minutes to temperature control；Then proceed to evacuation, the polycondensation carrying out high vacuum stage of Fig is anti- Should, making reaction pressure be down to absolute pressure is 60Pa, and reaction temperature controls at 279 DEG C, 62 minutes response time, is obtained modified poly- Ester.
The number-average molecular weight of modified poly ester is 17000, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2- heptan Base -1,3 propylene glycol segment compositions, 2- heptyl -1,3 propylene glycol segments are 2.8% with the Mole percent ratio of ethylene glycol segment.
Embodiment 10
, with embodiment 1, wherein main technical parameter is referring to table 1 for the modified poly ester preparation process of embodiment 10；In step (3), after adding p-phthalic acid binary alcohol esters, stirring mixing 17 minutes, is the 0.03% of p-phthalic acid gross weight in addition Catalyst glycol antimony and addition be p-phthalic acid gross weight 0.027% stabilizer trimethyl phosphate effect Under, start the polycondensation reaction in coarse vacuum stage under conditions of negative pressure, this staged pressure is steadily evacuated to absolute pressure by normal pressure 498Pa, at 269 DEG C, the response time is 39 minutes to temperature control；Then proceed to evacuation, the polycondensation carrying out high vacuum stage of Fig is anti- Should, making reaction pressure be down to absolute pressure is 60Pa, and reaction temperature controls at 278 DEG C, 64 minutes response time, is obtained modified poly- Ester.
The number-average molecular weight of modified poly ester is 17000, and modified poly ester is pungent by p-phthalic acid segment, ethylene glycol segment and 2- Base-Isosorbide-5-Nitrae butanediol segment composition, 2- octyl group-Isosorbide-5-Nitrae butanediol segment is 3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 11
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 11；In step Suddenly, after (3) add p-phthalic acid binary alcohol esters, stirring mixing 18 minutes, is p-phthalic acid gross weight in addition 0.04% catalyst glycol antimony and addition are 0.03% stabilizer trimethyl phosphate of p-phthalic acid gross weight Under conditions of negative pressure, under effect, start the polycondensation reaction in coarse vacuum stage, this staged pressure is steadily evacuated to absolute pressure by normal pressure Power 497Pa, at 260 DEG C, the response time is 40 minutes to temperature control；Then proceed to evacuation, carry out the polycondensation of high vacuum stage of Fig Reaction, making reaction pressure be down to absolute pressure is 60Pa, and reaction temperature controls at 277 DEG C, 63 minutes response time, and modification is obtained Polyester.
The number-average molecular weight of modified poly ester is 18000, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2- nonyl Base-Isosorbide-5-Nitrae butanediol segment composition, 2- nonyl-Isosorbide-5-Nitrae butanediol segment is 4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 12
, with embodiment 1, wherein main technical parameter is referring to table 1 for the preparation process of the modified poly ester of embodiment 12；In step Suddenly, after (3) add p-phthalic acid binary alcohol esters, stirring mixing 18 minutes, is p-phthalic acid weight in addition 0.038% catalyst acetic acid antimony and addition are the work of 0.03% stabilizer NSC 6513 of p-phthalic acid weight With under, start the polycondensation reaction in coarse vacuum stage under conditions of negative pressure, this staged pressure is steadily evacuated to absolute pressure by normal pressure 497Pa, at 265 DEG C, the response time is 42 minutes to temperature control；Then proceed to evacuation, the polycondensation carrying out high vacuum stage of Fig is anti- Should, making reaction pressure be down to absolute pressure is 40Pa, and reaction temperature controls at 277 DEG C, 70 minutes response time, is obtained modified poly- Ester.
The number-average molecular weight of prepared modified poly ester is 26000, by p-phthalic acid segment, ethylene glycol segment and the 2- last of the ten Heavenly stems Base-Isosorbide-5-Nitrae butanediol segment composition, 2- decyl-Isosorbide-5-Nitrae butanediol segment is 4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 13
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.5 p-phthalic acid and 2- decyl -1,5 pentanediols are made into slurry and add in reactor, Concentration is 60wt%, and addition is under the catalytic action of 0.5% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.3MPa, and temperature is 240 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:2.0 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.3MPa, and temperature is 260 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 5% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 20 minutes is adding Measure for p-phthalic acid weight 0.05% catalyst acetic acid antimony and addition be p-phthalic acid weight 0.05% steady In the presence of determining agent NSC 6513, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure by It is 450Pa that normal pressure is steadily evacuated to absolute pressure, and at 270 DEG C, the response time is 50 minutes to temperature control；Then proceed to evacuation, Carry out the polycondensation reaction of high vacuum stage of Fig, making reaction pressure be down to absolute pressure is 30Pa, and reaction temperature controls at 280 DEG C, instead 90 minutes between seasonable, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 30000, by p-phthalic acid segment, ethylene glycol segment and the 2- last of the ten Heavenly stems Base -1,5 pentanediol segment compositions, 2- decyl -1,5 pentanediol segments are 5% with the Mole percent ratio of ethylene glycol segment.
Embodiment 14
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.47 p-phthalic acid and 2- nonyl -1,5 pentanediols are made into slurry and add in reactor, Concentration is 60wt%, and addition is under the catalytic action of 0.47% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 220 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 258 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding Measure for p-phthalic acid weight 0.04% catalyst glycol antimony and addition be the 0.04% of p-phthalic acid weight In the presence of stabilizer trimethyl phosphate, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure by Normal pressure is steadily evacuated to absolute pressure 460Pa, and at 263 DEG C, the response time is 47 minutes to temperature control；Then proceed to evacuation, enter The polycondensation reaction of row high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 278 DEG C, during reaction Between 85 minutes, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 28000, by p-phthalic acid segment, ethylene glycol segment and 2- nonyl Base -1,5 pentanediol segment compositions, 2- nonyl -1,5 pentanediol segments are 4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 15
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.46 p-phthalic acid and 2- octyl group -1,5 pentanediols are made into slurry and add in reactor, Concentration is 60wt%, and addition is under the catalytic action of 0.49% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 233 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 259 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.5% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 19 minutes is adding Entering 0.044% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.046% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 269 DEG C, the response time is 48 minutes to temperature control；Then proceed to take out Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 279 DEG C, 87 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, pungent by p-phthalic acid segment, ethylene glycol segment and 2- Base -1,5 pentanediol segment compositions, 2- octyl group -1,5 pentanediol segments are 4.5% with the Mole percent ratio of ethylene glycol segment.
Embodiment 16
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.49 p-phthalic acid and 2- heptyl -1,5 pentanediols are made into slurry and add in reactor, Concentration is 60wt%, and addition is under the catalytic action of 0.48% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 230 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 258 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.7% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 19 minutes is adding Entering 0.048% catalyst glycol antimony that amount is p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.047% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank Section pressure is steadily evacuated to absolute pressure 460Pa by normal pressure, and at 267 DEG C, the response time is 48 minutes to temperature control；Then proceed to take out Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 279 DEG C, 83 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 27000, by p-phthalic acid segment, ethylene glycol segment and 2- heptan Base -1,5 pentanediol segment compositions, 2- heptyl -1,5 pentanediol segments are 4.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 17
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.467 p-phthalic acid and 2- hexyl -1,5 pentanediols are made into slurry and add in reactor, It is 60wt% in concentration, addition is under the catalytic action of 0.47% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 236 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.89 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 258 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.3% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding Entering 0.04% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.041% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should Staged pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 268 DEG C, the response time is 48 minutes to temperature control；Then proceed to Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, reaction temperature controls 278 DEG C, 85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, own by p-phthalic acid segment, ethylene glycol segment and 2- Base -1,5 pentanediol segment compositions, 2- hexyl -1,5 pentanediol segments are 4.3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 18
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.48 p-phthalic acid and 2- amyl group -1,5 pentanediols are made into slurry and add in reactor, Concentration is 55wt%, and addition is under the catalytic action of 0.46% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 230 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.88 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 256 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.7% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding Entering 0.047% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.047% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank Section pressure is steadily evacuated to absolute pressure 480Pa by normal pressure, and at 265 DEG C, the response time is 47 minutes to temperature control；Then proceed to take out Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 279 DEG C, 85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 28000, by p-phthalic acid segment, ethylene glycol segment and 2- penta Base -1,5 pentanediol segment compositions, 2- amyl group -1,5 pentanediol segments are 4.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 19
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.46 p-phthalic acid and 2- decyl -1,5 pentanediols are made into slurry and add in reactor, Concentration is 55wt%, and addition is under the catalytic action of 0.47% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 238 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.9 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 259 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during more than the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.7% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 19 minutes is adding Entering the 0.046% catalyst acetic acid antimony that amount is p-phthalic acid weight and addition is the 0.048% of p-phthalic acid weight Stabilizer NSC 6513 in the presence of, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this stage press It is 446Pa that power is steadily evacuated to absolute pressure by normal pressure, and at 267 DEG C, the response time is 49 minutes to temperature control；Then proceed to take out very Sky, carries out the polycondensation reaction of high vacuum stage of Fig, and making reaction pressure be down to absolute pressure is 40Pa, and reaction temperature controls at 278 DEG C, 87 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, by p-phthalic acid segment, ethylene glycol segment and the 2- last of the ten Heavenly stems Base -1,5 pentanediol segment compositions, 2- decyl -1,5 pentanediol segments are 4.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 20
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.46 p-phthalic acid and 2- nonyl -1,5 pentanediols are made into slurry and add in reactor, Concentration is 60wt%, and addition is under the catalytic action of 0.46% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.26MPa, and temperature is 221 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.89 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.25MPa, and temperature is 259 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.1% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding Entering 0.041% catalyst glycol antimony that amount is p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.042% stabilizer trimethyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank Section pressure is steadily evacuated to absolute pressure 460Pa by normal pressure, and at 265 DEG C, the response time is 47 minutes to temperature control；Then proceed to take out Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 278 DEG C, 85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 28000, by p-phthalic acid segment, ethylene glycol segment and 2- nonyl Base -1,5 pentanediol segment compositions, 2- nonyl -1,5 pentanediol segments are 4.1% with the Mole percent ratio of ethylene glycol segment.
Embodiment 21
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.43 p-phthalic acid and 2- octyl group -1,5 pentanediols are made into slurry and add in reactor, Concentration is 60wt%, and addition is under the catalytic action of 0.47% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 235 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.78 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.26MPa, and temperature is 255 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.3% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 17 minutes is adding Entering 0.043% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.049% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 268 DEG C, the response time is 46 minutes to temperature control；Then proceed to take out Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 275 DEG C, 85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 28000, pungent by p-phthalic acid segment, ethylene glycol segment and 2- Base -1,5 pentanediol segment compositions, 2- octyl group -1,5 pentanediol segments are 4.3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 22
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.43 p-phthalic acid and 2- heptyl -1,5 pentanediols are made into slurry and add in reactor, Concentration is 55wt%, and addition is under the catalytic action of 0.45% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.29MPa, and temperature is 235 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.87 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 255 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.6% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding Entering 0.047% catalyst glycol antimony that amount is p-phthalic acid weight and addition is the 0.04% of p-phthalic acid weight Stabilizer triphenyl phosphate in the presence of, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure Absolute pressure 470Pa is steadily evacuated to by normal pressure, at 268 DEG C, the response time is 45 minutes to temperature control；Then proceed to evacuation, Carry out the polycondensation reaction of high vacuum stage of Fig, make reaction pressure be down to absolute pressure 40Pa, reaction temperature controls at 279 DEG C, reaction 83 minutes time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, by p-phthalic acid segment, ethylene glycol segment and 2- heptan Base -1,5 pentanediol segment compositions, 2- heptyl -1,5 pentanediol segments are 4.6% with the Mole percent ratio of ethylene glycol segment.
Embodiment 23
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.457 p-phthalic acid and 2- hexyl -1,5 pentanediols are made into slurry and add in reactor, It is 55% in concentration, addition is under the catalytic action of 0.46% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 239 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.81 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 255 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.41% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 19 minutes, Addition is 0.042% the catalytic antimony trioxide of p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.048% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the response time is 45 minutes to temperature control；Then proceed to Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 275 DEG C, 85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 28000, own by p-phthalic acid segment, ethylene glycol segment and 2- Base -1,5 pentanediol segment compositions, 2- hexyl -1,5 pentanediol segments are 4.41% with the Mole percent ratio of ethylene glycol segment.
Embodiment 24
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.47 p-phthalic acid and 2- amyl group -1,5 pentanediols are made into slurry and add in reactor, Concentration is 55wt%, and addition is under the catalytic action of 0.48% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 245 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.81 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 259 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.67% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 19 minutes, Addition is 0.041% the catalytic antimony trioxide of p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.042% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank Section pressure is steadily evacuated to absolute pressure 485Pa by normal pressure, and at 268 DEG C, the response time is 46 minutes to temperature control；Then proceed to take out Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, and reaction temperature controls at 275 DEG C, 89 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, by p-phthalic acid segment, ethylene glycol segment and 2- penta Base -1,5 pentanediol segment compositions, 2- amyl group -1,5 pentanediol segments are 4.67% with the Mole percent ratio of ethylene glycol segment.
Embodiment 25
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.45 p-phthalic acid and 2- hexyl -1,5 pentanediol and 2- amyl group -1,4 butanediol mixed Compound is made into slurry and adds in reactor, wherein 2- hexyl -1, and the mol ratio of 5 pentanediols and 2- amyl group-Isosorbide-5-Nitrae butanediol is 3:1, It is 55% in concentration, addition is under the catalytic action of 0.49% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.26MPa, and temperature is 236 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 258 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.4% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding Entering 0.042% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.047% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the response time is 49 minutes to temperature control；Then proceed to Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 278 DEG C, 88 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester be 29000, by p-phthalic acid segment, ethylene glycol segment, 2- hexyl- 1,5 pentanediol segment and 2- amyl group-Isosorbide-5-Nitrae butanediol segment composition, 2- hexyl -1,5 pentanediol segments and 2- amyl group-Isosorbide-5-Nitrae fourth two The summation of alcohol segment is 4.4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 26
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:2- octyl group -1,5 pentanediol of 1.45 p-phthalic acid sum and 2- amyl group -1,5 pentanediol Mixture is made into slurry and adds in reactor, wherein 2- octyl group -1,6 hexanediol and 2- amyl group -1, and the mol ratio of 5 pentanediols is 3: 2, it is 60% in concentration, addition is under the catalytic action of 0.45% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 239 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.84 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti- Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.29MPa, and temperature is 255 DEG C, when in esterification It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.6% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding Entering 0.0423% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.045% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the response time is 45 minutes to temperature control；Then proceed to Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 278 DEG C, 85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester be 28000, by p-phthalic acid segment, ethylene glycol segment, 2- octyl group- 1,5 pentanediol segment and 2- amyl group -1,5 pentanediol segment compositions, 2- octyl group -1,5 pentanediol segments and 2- amyl group -1,5 penta 2 Alcohol segment is 4.6% with the Mole percent ratio of ethylene glycol segment.
Embodiment 27
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.45 p-phthalic acid and 2- hexyl -1,5 pentanediol and 2- amyl group -1,4 butanediol mixed Compound is made into slurry and adds in reactor, wherein 2- hexyl -1, and the mol ratio of 5 pentanediols and 2- amyl group-Isosorbide-5-Nitrae butanediol is 3:1, It is 55% in concentration, addition is under the catalytic action of 0.49% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.26MPa, and temperature is 236 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 96% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 258 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.4% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding Entering 0.042% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.047% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the response time is 49 minutes to temperature control；Then proceed to Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 278 DEG C, 88 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester be 29000, by p-phthalic acid segment, ethylene glycol segment, 2- hexyl- 1,5 pentanediol segment and 2- amyl group-Isosorbide-5-Nitrae butanediol segment composition, 2- hexyl -1,5 pentanediol segments and 2- amyl group-Isosorbide-5-Nitrae fourth two The summation of alcohol segment is 4.4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 28
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.45 p-phthalic acid is own with 2- octyl group -1,5 pentanediol, 2- amyl group -1,4 butanediol and 2- Base -1, the mixture of 5 pentanediols is made into slurry and adds in reactor, wherein 2- octyl group -1,5 pentanediols, 2- amyl group-Isosorbide-5-Nitrae fourth two The mol ratio of alcohol and 2- hexyl -1,5 pentanediol is 3:2:1, it is 60% in concentration, addition is p-phthalic acid weight Under the catalytic action of 0.47% concentrated sulphuric acid, carry out esterification, esterification compressive reaction in nitrogen atmosphere, moulding pressure For 0.29MPa, temperature is 235 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 92% of theoretical value, Obtain p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 258 DEG C, when the water in esterification evaporates It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right Phthalic acid binary alcohol esters are 4.71% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes, Addition is 0.04% the catalytic antimony trioxide of p-phthalic acid weight and addition is p-phthalic acid weight Under conditions of negative pressure, in the presence of 0.041% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should Staged pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 268 DEG C, the response time is 49 minutes to temperature control；Then proceed to Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 277 DEG C, 84 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, by p-phthalic acid segment, ethylene glycol segment, band side chain Glycol segment composition, wherein branched glycol segment be 2- octyl group -1,5 pentanediol segments, 2- amyl group-Isosorbide-5-Nitrae butanediol chain Section and 2- hexyl -1,5 pentanediol segments form, and branched glycol segment with the Mole percent ratio of ethylene glycol segment is 4.71%.
Embodiment 29
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
As shown in figure 1, the major axis of ellipse is 1.3 with the ratio of minor axis length, the spacing of adjacent spinneret orifice is equal to spinneret orifice Guide hole diameter add 1.5mm, spinneret is circular spinneret, the diameter of circular spinneret oval maximum long axial length with series The difference of degree is 11mm, a diameter of 2.0mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 374, the spinneret orifice of spinneret Shape of cross section be circle.
By the prepared modified poly ester of embodiment 1 through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, The spinning temperature of modified poly ester POY silk is 285 DEG C, and chilling temperature is 25 DEG C, and winding speed is 2400m/min；By modified poly ester Section is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk, modified poly ester FDY silk Spinning temperature is 285 DEG C, and chilling temperature is 25 DEG C, and network pressure is 0.25MPa, and a roller speed is 2400m/min, a roll temperature For 80 DEG C, two roller speeds are 3800m/min, and two roll temperatures are 120 DEG C, and winding speed is 3750m/min；Then by modified poly ester POY silk and modified poly ester FDY silk are obtained the soft imitative fiber crops of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding Polyester fiber, the spinning speed of the soft imitative fiber crops polyester fiber of porous is 600m/min, and sizing over feed rate(OFR) is 4.50%, and winding over feed rate(OFR) is 4.0%, T1 are 200 DEG C, and T2 is 200 DEG C, and DR is 1.7, D/Y is 1.8, and network pressure is 0.15MPa.
The fiber number of the soft imitative fiber crops polyester fiber of prepared porous is 120tex, initial moduluss 78cN/dtex, and fracture strength is 4.7cN/dtex, elongation at break is 41.7%, and crimp contraction is 4.53%, and internet pricing is 95/m；The soft imitative fiber crops of porous At temperature is 80 DEG C, the spatial joint clearance of fibrous inside molecule interchain increases 15v/v% to polyester fiber；Porous imitates fiber crops polyester fiber Line density deviation ratio be 1.7%, fracture strength CV value is 3.2%, and extension at break CV value is 6.9%, crimp contraction make a variation Coefficient CV value is 7.2%, and boiling water shrinkage is 10.5%.
Embodiment 30
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
As shown in figure 3, the major axis of ellipse is 1.6 with the ratio of minor axis length, the spacing of adjacent spinneret orifice is equal to spinneret orifice Guide hole diameter add 1.5mm, spinneret is circular spinneret, the diameter of circular spinneret oval maximum long axial length with series The difference of degree is 11mm, a diameter of 2.0mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 382, the spinneret orifice of spinneret Shape of cross section be circle.
By the prepared modified poly ester of embodiment 1 through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, The spinning temperature of modified poly ester POY silk is 285 DEG C, and chilling temperature is 25 DEG C, and winding speed is 2400m/min；By modified poly ester Section is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk, modified poly ester FDY silk Spinning temperature is 285 DEG C, and chilling temperature is 25 DEG C, and network pressure is 0.25MPa, and a roller speed is 2400m/min, a roll temperature For 80 DEG C, two roller speeds are 3800m/min, and two roll temperatures are 120 DEG C, and winding speed is 3750m/min；Then by modified poly ester POY silk and modified poly ester FDY silk are obtained the soft imitative fiber crops of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding Polyester fiber, the spinning speed of the soft imitative fiber crops polyester fiber of porous is 600m/min, and sizing over feed rate(OFR) is 4.50%, and winding over feed rate(OFR) is 4.0%, T1 are 200 DEG C, and T2 is 200 DEG C, and DR is 1.7, D/Y is 1.8, and network pressure is 0.15MPa.
The fiber number of the soft imitative fiber crops polyester fiber of prepared porous is 140dtex, initial moduluss 80cN/dtex, fracture strength For 5.2cN/dtex, elongation at break is 42.6%, and crimp contraction is 4.77%, and internet pricing is 98/m；Porous is soft imitative At temperature is 80 DEG C, the spatial joint clearance of fibrous inside molecule interchain increases 15v/v% to numb polyester fiber；It is fine that porous imitates fiber crops polyester The line density deviation ratio of dimension is 1.2%, and fracture strength CV value is 3.1%, and extension at break CV value is 5.3%, and crimp contraction becomes Different coefficient CV value is 4.9%, and boiling water shrinkage is 10.6%.
Comparative example 1
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is circular arrangement, circular arrangement refers to that the hole of spinneret orifice is centrally located at concentric circular On, concentric circular is that series is circular.As shown in Fig. 2 the guide hole diameter that the spacing of adjacent spinneret orifice is equal to spinneret orifice adds 1.5mm, Spinneret is circular spinneret, and the diameter of circular spinneret is 11mm with the difference of the circular maximum diameter of series, spinneret orifice The a diameter of 2.0mm of guide hole, the spray webbing hole count of spinneret is 370, and the shape of cross section of the spinneret orifice of spinneret is circle.
By the prepared modified poly ester of embodiment 1 through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, The spinning temperature of modified poly ester POY silk is 285 DEG C, and chilling temperature is 25 DEG C, and winding speed is 2400m/min；By modified poly ester Section is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk, modified poly ester FDY silk Spinning temperature is 285 DEG C, and chilling temperature is 25 DEG C, and network pressure is 0.25MPa, and a roller speed is 2400m/min, a roll temperature For 80 DEG C, two roller speeds are 3800m/min, and two roll temperatures are 120 DEG C, and winding speed is 3750m/min；Then by modified poly ester POY silk and modified poly ester FDY silk are obtained the soft imitative fiber crops of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding Polyester fiber, the spinning speed of the soft imitative fiber crops polyester fiber of porous is 600m/min, and sizing over feed rate(OFR) is 4.50%, and winding over feed rate(OFR) is 4.0%, T1 are 200 DEG C, and T2 is 200 DEG C, and DR is 1.7, D/Y is 1.8, and network pressure is 0.15MPa.
The fiber number of the soft imitative fiber crops polyester fiber of prepared porous is 75dtex, initial moduluss 73cN/dtex, and fracture strength is 2.7cN/dtex, elongation at break is 37.6%, and crimp contraction is 5.4%, and internet pricing is 87/m；The soft imitative fiber crops of porous are poly- At temperature is 80 DEG C, the spatial joint clearance of fibrous inside molecule interchain increases 15v/v% to ester fiber；Porous imitates fiber crops polyester fiber Line density deviation ratio is 2.6%, and fracture strength CV value is 4.5%, and extension at break CV value is 8.2%, crimp contraction Variation Lines Number CV value is 8.5%, and boiling water shrinkage is 9.1%.
When identical with the effective area that embodiment 29 contrast can be seen that spinneret, (circular arrangement when spray webbing hole count is close Spray webbing hole count is 370, and oval shaped arrangements spray webbing hole count is 374), the spinneret orifice number of plies of oval shaped arrangements is 6, less than circular arrangement The spinneret orifice number of plies 8, cooling effect is more preferable；When identical with the effective area that embodiment 30 contrast can be seen that spinneret, oval The spinneret orifice number of plies of shape arrangement is 5, and less than the spinneret orifice number of plies 8 of circular arrangement, cooling effect is more preferable, the spray webbing of oval shaped arrangements The hole count 382 in hole is more than the hole count 370 of the spinneret orifice of circular arrangement, and cooling effectiveness is higher.The comparing result of fibre property shows, Fiber linear density deviation ratio, fracture strength CV value, extension at break CV value and evenness fault that embodiment 29 and embodiment 30 are obtained Rate CV value is less than comparative example 1, under the conditions of same process is described, using the prepared fibroids of the spinneret of spinneret orifice oval shaped arrangements Can be better than the spinneret using spinneret circular arrangement.
Embodiment 31～33
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as long axial symmetry, oval major axis is 1.4 with the ratio of minor axis length, between adjacent spinneret orifice Add 1.6mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series The difference of maximum long axis length is 12mm, a diameter of 1.5mm of guide hole of spinneret orifice, the spinneret orifice numerical digit 192 of spinneret, spray webbing The shape of cross section of the spinneret orifice of plate is square.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk Spinning temperature is 280 DEG C, and chilling temperature is 23 DEG C, and winding speed is 2300m/min；By Modified polyester chips through metering, extrusion, Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 280 DEG C, Chilling temperature is 20 DEG C, and network pressure is 0.20MPa, and a roller speed is 2200m/min, and a roll temperature is 75 DEG C, two roller speeds For 3650m/min, two roll temperatures are 115 DEG C, and winding speed is 3600m/min；Then by modified poly ester POY silk and modified poly ester FDY silk is obtained the soft imitative fiber crops polyester fiber of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding, and porous is soft The spinning speed of soft imitative fiber crops polyester fiber is 400m/min, and sizing over feed rate(OFR) is 3.50%, and winding over feed rate(OFR) is 2.5%, T1 is 160 DEG C, T2 is 180 DEG C, and DR is 1.6, D/Y is 0.05MPa for 1.6 network pressures.The boiling of the soft imitative fiber crops polyester fiber of prepared porous Water shrinkage factor is 9.0～9.7, the mechanical property of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 80 DEG C Data such as following table.
Embodiment 34～36
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that short axle is symmetrical, oval major axis is 1.4 with the ratio of minor axis length, between adjacent spinneret orifice Add 1.7mm away from the guide hole diameter equal to spinneret orifice, spinneret is elliptical spinneret plate, elliptical spinneret plate is with serial ellipse The difference of big long axis length is 12mm, a diameter of 1.8mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 200, spinneret Spinneret orifice shape of cross section be rhombus.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk Spinning temperature is 282 DEG C, and chilling temperature is 23 DEG C, and winding speed is 2350m/min；By Modified polyester chips through metering, extrusion, Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 281 DEG C, Chilling temperature is 21 DEG C, and network pressure is 0.21MPa, and a roller speed is 2250m/min, and a roll temperature is 77 DEG C, two roller speeds For 3680m/min, two roll temperatures are 116 DEG C, and winding speed is 3630m/min；Then by modified poly ester POY silk and modified poly ester FDY silk is obtained the soft imitative fiber crops polyester fiber of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding, and porous is soft The spinning speed of soft imitative fiber crops polyester fiber is 450m/min, and sizing over feed rate(OFR) is 3.9%, and winding over feed rate(OFR) is that 2.9%, T1 is 170 DEG C, T2 is 185 DEG C, and DR is 1.6, D/Y is 1.6, and network pressure is 0.15MPa.The boiling water of the soft imitative fiber crops polyester fiber of prepared porous Shrinkage factor is 9.1～9.6, the mechanical property number of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 90 DEG C According to such as following table.
Embodiment 37～39
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that major axis and short axle are symmetrical, oval major axis is 1.4 with the ratio of minor axis length, adjacent spray webbing The guide hole diameter that the spacing in hole is equal to spinneret orifice adds 1.8mm, and spinneret is circular spinneret, the diameter of circular spinneret be The difference of the oval maximum long axis length of row is 13mm, a diameter of 2.5mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 200, the shape of cross section of the spinneret orifice of spinneret is yi word pattern.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk Spinning temperature is 283 DEG C, and chilling temperature is 24 DEG C, and winding speed is 2400m/min；By Modified polyester chips through metering, extrusion, Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 284 DEG C, Chilling temperature is 23 DEG C, and network pressure is 0.30MPa, and a roller speed is 2300m/min, and a roll temperature is 78 DEG C, two roller speeds For 3700m/min, two roll temperatures are 125 DEG C, and winding speed is 3650m/min；Then by modified poly ester POY silk and modified poly ester FDY silk is obtained the soft imitative fiber crops polyester fiber of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding, and porous is soft The spinning speed of soft imitative fiber crops polyester fiber is 470m/min, and sizing over feed rate(OFR) is 5.50%, and winding over feed rate(OFR) is 3.5%, T1 is 180 DEG C, T2 is 190 DEG C, and DR is 1.6, D/Y is 1.7, and network pressure is 0.30MPa.The soft imitative fiber crops polyester fiber of prepared porous Boiling water shrinkage is 9.6～10.0, the mechanics of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 100 DEG C Performance data such as following table.
Embodiment 40～42
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that major axis and short axle are symmetrical, oval major axis is 1.7 with the ratio of minor axis length, adjacent spray webbing The spacing in hole be equal to spinneret orifice guide hole diameter add 1.9mm, spinneret be elliptical spinneret plate, elliptical spinneret plate with series The difference of oval maximum long axis length is 14mm, a diameter of 1.5mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 210, The shape of cross section of the spinneret orifice of spinneret is triangular form.
By the prepared modified poly ester of embodiment 1 through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, The spinning temperature of modified poly ester POY silk is 283 DEG C, and chilling temperature is 24 DEG C, and winding speed is 2400m/min；By modified poly ester Section is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk, modified poly ester FDY silk Spinning temperature is 284 DEG C, and chilling temperature is 22 DEG C, and network pressure is 0.23MPa, and a roller speed is 2500m/min, a roll temperature For 85 DEG C, two roller speeds are 3800m/min, and two roll temperatures are 135 DEG C, and winding speed is 3750m/min；Then by modified poly ester POY silk and modified poly ester FDY silk are obtained the soft imitative fiber crops of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding Polyester fiber, the spinning speed of the soft imitative fiber crops polyester fiber of porous is 600m/min, and sizing over feed rate(OFR) is 4.70%, and winding over feed rate(OFR) is 4.1%, T1 are 175 DEG C, and T2 is 200 DEG C, and DR is 1.7, D/Y is 1.8, and network pressure is 0.18MPa.Prepared porous is soft imitative The boiling water shrinkage of numb polyester fiber is 10.4～11.0, the spatial joint clearance Magnification of fibrous inside molecule interchain at 110 DEG C And the mechanical performance data of fiber such as following table.
Embodiment 43～45
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that short axle is symmetrical, oval major axis is 1.8 with the ratio of minor axis length, between adjacent spinneret orifice Add 1.5mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series The difference of maximum long axis length is 15mm, a diameter of 1.8mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 240, spray webbing The shape of cross section of the spinneret orifice of plate is trilobal cross.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk Spinning temperature is 287 DEG C, and chilling temperature is 26 DEG C, and winding speed is 2450m/min；By Modified polyester chips through metering, extrusion, Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 284 DEG C, Chilling temperature is 23 DEG C, and network pressure is 0.23MPa, and a roller speed is 2450m/min, and a roll temperature is 76 DEG C, two roller speeds For 3790m/min, two roll temperatures are 125 DEG C, and winding speed is 3740m/min；Then by modified poly ester POY silk and modified poly ester FDY silk is obtained the soft imitative fiber crops polyester fiber of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding, and porous is soft The spinning speed of soft imitative fiber crops polyester fiber is 560m/min, and sizing over feed rate(OFR) is 4.50%, and winding over feed rate(OFR) is 3.5%, T1 is 190 DEG C, T2 is 210 DEG C, and DR is 1.8, D/Y is 2.0, and network pressure is 0.19MPa.The soft imitative fiber crops polyester fiber of prepared porous Boiling water shrinkage is 9.4～9.7, the mechanics of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 120 DEG C Performance data such as following table.
Embodiment 46～49
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as long axial symmetry, oval major axis is 1.8 with the ratio of minor axis length, between adjacent spinneret orifice Add 1.6mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series The difference of maximum long axis length is 16mm, a diameter of 2.2mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 250, spray webbing The shape of cross section of the spinneret orifice of plate is hollow type.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk Spinning temperature is 288 DEG C, and chilling temperature is 27 DEG C, and winding speed is 2470m/min；By Modified polyester chips through metering, extrusion, Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 284 DEG C, Chilling temperature is 23 DEG C, and network pressure is 0.240MPa, and a roller speed is 2460m/min, and a roll temperature is 79 DEG C, two roller speeds For 3780m/min, two roll temperatures are 124 DEG C, and winding speed is 3730m/min；Then by modified poly ester POY silk and modified poly ester FDY silk is obtained the soft imitative fiber crops polyester fiber of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding, and porous is soft The spinning speed of soft imitative fiber crops polyester fiber is 610m/min, and sizing over feed rate(OFR) is 4.3%, and winding over feed rate(OFR) is that 4.1%, T1 is 170 DEG C, T2 is 193 DEG C, and DR is 1.7, D/Y is 1.8, and network pressure is 0.24MPa.The boiling water of the soft imitative fiber crops polyester fiber of prepared porous Shrinkage factor is 9.2～9.8, the mechanical property of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 130 DEG C Data such as following table.
Embodiment 50～53
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that short axle is symmetrical, oval major axis is 1.8 with the ratio of minor axis length, between adjacent spinneret orifice Add 1.8mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series The difference of maximum long axis length is 15mm, a diameter of 2.5mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 260, spray webbing The shape of cross section of the spinneret orifice of plate is platypelloid type.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk Spinning temperature is 286 DEG C, and chilling temperature is 24 DEG C, and winding speed is 2430m/min；By Modified polyester chips through metering, extrusion, Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 282 DEG C, Chilling temperature is 22 DEG C, and network pressure is 0.23MPa, and a roller speed is 2600m/min, and a roll temperature is 75-85 DEG C, two roller speed Spend for 3760m/min, two roll temperatures are 121 DEG C, winding speed is 3710m/min；Then modified poly ester POY silk and modification are gathered Ester FDY silk is obtained the soft imitative fiber crops polyester fiber of porous, porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding The spinning speed of soft imitative fiber crops polyester fiber is 800m/min, and sizing over feed rate(OFR) is 4.1%, and winding over feed rate(OFR) is 5.0%, T1 is 220 DEG C, T2 is 220 DEG C, and DR is 1.6, D/Y is 1.8, and network pressure is 0.21MPa.The soft imitative fiber crops polyester fiber of prepared porous Boiling water shrinkage is 10.0～10.7, the power of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 100 DEG C Learn performance data such as following table.
Embodiment 54～57
A kind of preparation method of the soft imitative fiber crops polyester fiber of porous, the soft imitative fiber crops polyester fiber of porous adopts porous spinneret It is obtained, on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, it is same that oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at On heart ellipse, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as long axial symmetry, oval major axis is 1.8 with the ratio of minor axis length, between adjacent spinneret orifice Add 1.5mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series The difference of maximum long axis length is 16mm, a diameter of 1.8mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 300, spray webbing The shape of cross section of the spinneret orifice of plate is hollow type.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk Spinning temperature is 290 DEG C, and chilling temperature is 26 DEG C, and winding speed is 2500m/min；By Modified polyester chips through metering, extrusion, Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 290 DEG C, Chilling temperature is 25 DEG C, and network pressure is 0.23MPa, and a roller speed is 2480m/min, and a roll temperature is 78 DEG C, two roller speeds For 3850m/min, two roll temperatures are 124 DEG C, and winding speed is 3800m/min；Then by modified poly ester POY silk and modified poly ester FDY silk is obtained the soft imitative fiber crops polyester fiber of porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding, and porous is soft The spinning speed of soft imitative fiber crops polyester fiber is 590m/min, and sizing over feed rate(OFR) is 4.60%, and winding over feed rate(OFR) is 3.7%, T1 is 190 DEG C, T2 is 220 DEG C, and DR is 1.6, D/Y is 1.7, and network pressure is 0.23MPa.The soft imitative fiber crops polyester fiber of prepared porous Boiling water shrinkage is 9.6～10.3, the mechanics of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 120 DEG C Performance data such as following table.
Embodiment 58
The dyeing of the soft imitative fiber crops polyester fiber of porous：
The soft imitative fiber crops polyester fiber of porous of embodiment 29 preparation is dyeed in High Temperature High Pressure machine, actual conditions For：Before dyeing, the soft imitative fiber crops polyester fiber nonionic surfactant of porous is processed 30 minutes at 60 DEG C, is subsequently adding dyeing In liquid, the disperse dyes consumption in dyeing liquor is 2.0% (o.w.f)；Dispersant NNO, concentration 1.2g/L of dispersant NNO；pH It is worth for 5, bath raio is 1:50, enter dye at 60 DEG C, then heat to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C and 130 DEG C of each constant temperature dyes Color 1h.
Using identical dyeing condition, general fibre is dyeed.The soft imitative fiber crops polyester fiber of porous after dyed Dye uptake obtains by the following method：
Dye uptake adopts 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, the DMF in dye liquor to be measured and the ratio of water are 70/30 (v/v), and dye liquor absorbance is using purple Outward-visible spectrophotometer measures, and calculates dye uptake with following formula.
In above formula, A0 and A1 is respectively the absorbance dyeing stock solution and dyeing residual liquid.
When disperse dyes are Disperse Red 3B, when disperse blue SE-2R or the bright blue S-GL of dispersion, the soft imitative fiber crops polyester fiber of porous Dye uptake result such as following table with general fibre：
Contrasted it can be seen that porous is soft imitative numb by the Color of the soft imitative numb polyester fiber of porous and general fibre The Color of polyester fiber is substantially better than general fibre, also the modified poly ester macromole of present invention preparation from side illustration The dihydroxylic alcohols segment containing side chain containing, makes the increasing degree of free volume be far longer than the spy of unbranched polyester macromolecule chain Property, the increase of free volume improves molecule and enters the internal degree of polyester, polyester fiber prepared by modified polyester Free volume is far longer than unbranched polyester fiber at equal temperature, increases the diffusion of dyestuff, improves polyester fiber Dyeability.
Embodiment 59
The dyeing of the soft imitative fiber crops polyester fiber of porous：
The soft imitative fiber crops polyester fiber of porous of embodiment 31 preparation is dyeed in High Temperature High Pressure machine, actual conditions For：Before dyeing, the soft imitative fiber crops polyester fiber nonionic surfactant of porous is processed 30 minutes at 60 DEG C, is subsequently adding dyeing In liquid, the disperse dyes consumption in dyeing liquor is 2.0% (o.w.f)；Dispersant NNO, concentration 1.2g/L of dispersant NNO；pH It is worth for 5, bath raio is 1:50, enter dye at 60 DEG C, then heat to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C and 130 DEG C of each constant temperature dyes Color 1h.
Using identical dyeing condition, general fibre is dyeed.The soft imitative fiber crops polyester fiber of porous after dyed Dye uptake obtains by the following method：
Dye uptake adopts 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, the DMF in dye liquor to be measured and the ratio of water are 70/30 (v/v), and dye liquor absorbance is using purple Outward-visible spectrophotometer measures, and calculates dye uptake with following formula.
In above formula, A0 and A1 is respectively the absorbance dyeing stock solution and dyeing residual liquid.
When disperse dyes are Disperse Red 3B, when disperse blue SE-2R or the bright blue S-GL of dispersion, the soft imitative fiber crops polyester fiber of porous Dye uptake result such as following table with general fibre：
Contrasted it can be seen that porous is soft imitative numb by the Color of the soft imitative numb polyester fiber of porous and general fibre The Color of polyester fiber is substantially better than general fibre, also the modified poly ester macromole of present invention preparation from side illustration The dihydroxylic alcohols segment containing side chain containing, makes the increasing degree of free volume be far longer than the spy of unbranched polyester macromolecule chain Property, the increase of free volume improves molecule and enters the internal degree of polyester, polyester fiber prepared by modified polyester Free volume is far longer than unbranched polyester fiber at equal temperature, increases the diffusion of dyestuff, improves polyester fiber Dyeability.

Claims (10)

1. a kind of soft imitative fiber crops polyester fiber of porous, is characterized in that：The material of the soft imitative fiber crops polyester fiber of described porous is modification Polyester, described modified poly ester form by p-phthalic acid segment, ethylene glycol segment and containing the dihydroxylic alcohols segment of side chain, described containing The dihydroxylic alcohols segment of chain refers to that side chain is located on one of dihydroxylic alcohols segment non-end group carbon and side chain is former containing 5-10 carbon The dihydroxylic alcohols segment of the linear carbon chain of son；
The fiber number of the soft imitative fiber crops polyester fiber of described porous is 75-150dtex, initial moduluss≤80cN/dtex, fracture strength >= 3.0cN/dtex, elongation at break is 40.0 ± 3.0%, and crimp contraction is 3.50 ± 2.0%, and internet pricing is 95 ± 5/m； At temperature is 80～130 DEG C, the spatial joint clearance of fibrous inside molecule interchain increases 10 to the soft imitative fiber crops polyester fiber of described porous ～30v/v%；Line density deviation ratio≤2.0% of the soft imitative fiber crops polyester fiber of described porous, fracture strength CV value≤4.0%, Extension at break CV value≤8.0%, crimp contraction coefficient of variation CV value≤8.0%, boiling water shrinkage is 10.0 ± 1.0%；Institute The spatial joint clearance increase of the molecule interchain stated refers to modified poly ester and normal polyester between the space of mutually synthermal molecule interchain The contrast of gap.
2. a kind of porous softness imitates the preparation method of fiber crops polyester fiber as claimed in claim 1, it is characterized in that：By modified poly ester The soft imitative fiber crops polyester fiber of porous is obtained using porous spinneret spinning；On described porous spinneret, the arrangement mode of spinneret orifice is Oval shaped arrangements, described oval shaped arrangements refer to that the hole of spinneret orifice is centrally located on concentration ellipse, and described concentration ellipse is series Ellipse, all oval major axis are conllinear, and short axle is conllinear；
The preparation method of the soft imitative fiber crops polyester fiber of described porous is：By modified poly ester through measuring, extruding, cool down, oil and roll up Around prepared modified poly ester POY silk；By Modified polyester chips through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, system Obtain modified poly ester FDY silk；Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, heating stretching, false twisting, heat Sizing and coiling and molding are obtained the soft imitative fiber crops polyester fiber of porous；
The preparation process of described modified poly ester is：
(1) preparation of p-phthalic acid binary alcohol esters；
P-phthalic acid is made into after slurry with the dihydroxylic alcohols containing side chain, under the catalytic action of concentrated sulphuric acid, carries out esterification Obtain p-phthalic acid binary alcohol esters；The described dihydroxylic alcohols containing side chain refer to that side chain is located at the non-end group of one of dihydroxylic alcohols segment On carbon and side chain is the dihydroxylic alcohols of the linear carbon chain containing 5-10 carbon atom；
(2) preparation of ethylene glycol terephthalate；
P-phthalic acid and ethylene glycol are made into after slurry, carry out esterification, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stirring is mixed Close, in the presence of catalyst and stabilizer, under conditions of negative pressure, carry out polycondensation reaction and the Gao Zhen in coarse vacuum stage successively The polycondensation reaction in empty stage, prepared modified poly ester.
3. a kind of soft preparation method imitating fiber crops polyester fiber of porous according to claim 2 is it is characterised in that described change The concrete preparation process of property polyester is：
(1) preparation of p-phthalic acid binary alcohol esters；
P-phthalic acid is made into slurry with the dihydroxylic alcohols containing side chain, under the catalytic action of concentrated sulphuric acid, carries out esterification, ester Change reaction compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure～0.3MPa, temperature is 180～240 DEG C, works as esterification In water quantity of distillate reach theoretical value more than 90% when be esterification terminal, obtain p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate；
P-phthalic acid and ethylene glycol are made into after slurry, carry out esterification, esterification compressive reaction in nitrogen atmosphere, Moulding pressure is normal pressure～0.3MPa, and temperature is 250～260 DEG C, when the water quantity of distillate in esterification reaches theoretical value It is esterification terminal when more than 90%, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stirring is mixed Close 15-20 minute, under conditions of negative pressure, in the presence of catalyst and stabilizer, start the polycondensation reaction in coarse vacuum stage, This staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature control at 260～270 DEG C, the response time be 30～ 50 minutes；Then proceed to evacuation, carry out the polycondensation reaction of high vacuum stage of Fig, make reaction pressure be down to absolute pressure and be less than 100Pa, reaction temperature controls at 275～280 DEG C, 50～90 minutes response time, prepared modified poly ester；
The main spinning technology parameter of described modified poly ester POY silk is：
Spinning temperature：280-290℃；
Chilling temperature：23-27℃；
Winding speed：2300-2500m/min；
The main spinning technology parameter of described modified poly ester FDY silk is：
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：3650-3850m/min；
Two roll temperatures：115-135℃；
Winding speed：3600-3800m/min；
The main spinning technology parameter of the soft imitative fiber crops polyester fiber of described porous is：
Spin speed：400-800m/min；
Sizing over feed rate(OFR)：3.5-5.50%；
Winding over feed rate(OFR)：2.5-5.0%；
T1：160-220℃；
T2：180-220℃；
DR：1.6-1.8；
D/Y:1.6-2.0；
Network pressure：0.05-0.3MPa.
4. a kind of preparation method of the soft imitative fiber crops polyester fiber of porous according to claim 2 is it is characterised in that step (1), in, p-phthalic acid is 1 with the mol ratio of the dihydroxylic alcohols containing side chain:1.3-1.5；Concentrated sulphuric acid addition is p-phthalic acid The 0.3-0.5% of weight；The concentration of described concentrated sulphuric acid is 50-60wt%；
In step (2), p-phthalic acid is 1 with the mol ratio of ethylene glycol:1.2～2.0；
In step (3), the Mole percent ratio of described p-phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2～ 5%；Described catalyst is antimony oxide, antimony glycol or antimony acetate, and catalyst charge is p-phthalic acid gross weight 0.01%～0.05%；Described stabilizer is triphenyl phosphate, trimethyl phosphate or NSC 6513, and stabilizer addition is The 0.01%～0.05% of described p-phthalic acid gross weight；
The number-average molecular weight of described modified poly ester is 15000～30000.
5. a kind of soft preparation method imitating fiber crops polyester fiber of porous according to claim 2 is it is characterised in that described contain The dihydroxylic alcohols of side chain are 2- amyl group -1,4 butanediol, 2- hexyl -1,4 butanediol, 2- heptyl -1,4 butanediol, 2- octyl group -1,4 fourth Glycol, 2- nonyl -1,4 butanediol, 2- decyl -1,4 butanediol, 2- amyl group -1,5 pentanediol, 2- hexyl -1,5 pentanediol, 2- heptan One or more of base -1,5 pentanediol, 2- octyl group -1,5 pentanediol, 2- nonyl -1,5 pentanediol or 2- decyl -1,5 pentanediol.
6. a kind of preparation method of the soft imitative fiber crops polyester fiber of porous according to claim 2 is it is characterised in that described spray Silk hole be arranged as major axis and/or short axle is symmetrical.
7. a kind of preparation method of porous according to claim 2 soft imitative fiber crops polyester fiber is it is characterised in that ellipse Major axis is 1.3～1.8 with the ratio of minor axis length；The guide hole diameter that the spacing of adjacent spinneret orifice is more than or equal to spinneret orifice adds 1.5mm.
8. a kind of preparation method of the soft imitative fiber crops polyester fiber of porous according to claim 2 is it is characterised in that described spray Filament plate is circular spinneret or elliptical spinneret plate；The diameter of described circle spinneret and the oval maximum long axis length of series Difference is more than 10mm, and described elliptical spinneret plate is more than 10mm with the difference of the oval maximum long axis length of series.
9. a kind of preparation method of the soft imitative fiber crops polyester fiber of porous according to claim 2 is it is characterised in that described spray A diameter of 1.5～the 2.5mm of guide hole in silk hole；The spray webbing hole count of described spinneret is more than or equal to 192.
10. a kind of preparation method of the soft imitative fiber crops polyester fiber of porous according to claim 2 is it is characterised in that described The shape of cross section of the spinneret orifice of spinneret be circle, square, rhombus, yi word pattern, triangular form, trilobal cross, hollow type or Platypelloid type.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108130624A (en) * 2017-12-14 2018-06-08 江苏恒力化纤股份有限公司 A kind of polyester imitates linen look abnormal contraction composite filament and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102030893A (en) * 2009-09-29 2011-04-27 东丽纤维研究所（中国）有限公司 Copolyester as well as preparation method and application thereof
CN102851757A (en) * 2011-06-30 2013-01-02 江苏华亚化纤有限公司 Special-shaped spinneret plate for spinning heavy denier yarns
CN102797054B (en) * 2012-09-03 2014-10-01 江苏恒力化纤股份有限公司 Manufacturing method of high-strength, high-modulus and low-shrinkage polyester industrial yarn
JP2014189933A (en) * 2013-03-28 2014-10-06 Toray Ind Inc Normal pressure dispersion-dyeable polyester ultra-fine fiber
CN104499080A (en) * 2014-12-31 2015-04-08 江苏恒力化纤股份有限公司 High-strength activated polyester industry yarn and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102030893A (en) * 2009-09-29 2011-04-27 东丽纤维研究所（中国）有限公司 Copolyester as well as preparation method and application thereof
CN102851757A (en) * 2011-06-30 2013-01-02 江苏华亚化纤有限公司 Special-shaped spinneret plate for spinning heavy denier yarns
CN102797054B (en) * 2012-09-03 2014-10-01 江苏恒力化纤股份有限公司 Manufacturing method of high-strength, high-modulus and low-shrinkage polyester industrial yarn
JP2014189933A (en) * 2013-03-28 2014-10-06 Toray Ind Inc Normal pressure dispersion-dyeable polyester ultra-fine fiber
CN104499080A (en) * 2014-12-31 2015-04-08 江苏恒力化纤股份有限公司 High-strength activated polyester industry yarn and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108130624A (en) * 2017-12-14 2018-06-08 江苏恒力化纤股份有限公司 A kind of polyester imitates linen look abnormal contraction composite filament and preparation method thereof
CN108130624B (en) * 2017-12-14 2020-05-05 江苏恒力化纤股份有限公司 Polyester linen-like different-shrinkage composite yarn and preparation method thereof

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