CN106283260B - Porous super flexible polyester fiber FDY of one kind and preparation method thereof - Google Patents

Porous super flexible polyester fiber FDY of one kind and preparation method thereof Download PDF

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Publication number
CN106283260B
CN106283260B CN201610783891.1A CN201610783891A CN106283260B CN 106283260 B CN106283260 B CN 106283260B CN 201610783891 A CN201610783891 A CN 201610783891A CN 106283260 B CN106283260 B CN 106283260B
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tpa
terephthalic acid
esterification
preparation
spinneret
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CN106283260A (en
Inventor
范红卫
王山水
李文刚
熊克
杨超明
张元华
张烨
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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
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16—Dicarboxylic acids and dihydroxy compounds
    • C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/181—Acids containing aromatic rings
    • C08G63/183—Terephthalic acids
    • 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
    • D01D5/08—Melt spinning methods
    • D01D5/088—Cooling filaments, threads or the like, leaving the 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
    • D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties

Abstract

The present invention relates to a kind of porous super flexible polyester fibers FDY and preparation method thereof, and porous super flexible polyester fiber FDY is made using porous spinneret spinning in modified poly ester；The arrangement mode of spinneret orifice is oval shaped arrangements on porous spinneret, i.e. the hole center of spinneret orifice is located on concentration ellipse, and concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.Porous super flexible polyester fiber FDY by Modified polyester chips through metering, extrusion, cooling, oil, stretch, thermal finalization and winding are made, the preparation method of modified poly ester is：Ethylene glycol terephthalate is made with glycol reaction in terephthalic acid (TPA), and terephthalic acid (TPA) is added and reacts terephthalic acid (TPA) binary alcohol esters obtained with the hexylene glycol containing branch, the reaction was continued obtains.Fibre property produced by the present invention is excellent, line density deviation ratio≤0.5%, fracture strength CV value≤4.0%, extension at break CV value≤8.0%, yarn unevenness CV≤2.0%.

Description

Porous super flexible polyester fiber FDY of one kind and preparation method thereof
Technical field
The invention belongs to field of polyester fiber, are related to porous super flexible polyester fiber FDY of one kind and preparation method thereof.
Background technology
Polyethylene terephthalate (PET fiber or polyester fiber) fiber since the advent of the world, have fracture strength and Elasticity modulus 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 many advantages, such as wash and wear, stiffness is good, is widely used in the fields such as clothes, home textile.
But due to the crystallinity of PET height, compact structure, and the functional group not being combined with dyestuff on strand cause Dye molecule hardly enters fibrous inside, and dyeing is difficult.People be cannot be satisfied to bright-coloured beautiful, unique style fabric demand.
The reason for causing PET dyeing difficult is the straight chain macromolecular that PET belongs to symmetry, and strand does not contain side chain radical Group, regularity is very good, its main chain contains rigid phenyl ring and alkyl flexible, and the ester group being directly connected with phenyl ring with Phenyl ring constitutes rigid conjugated system again, to constrain rotating freely for its soft segment.Such a structure increases molecules The wall ridge of sub-chain motion, causes the glass transition temperature of PET higher, needs to promote dye molecule under very high temperature condition Staining procedure is completed in diffusion to fibrous inside.In addition, the strand of PET is regular, good crystallinity, strand arrangement is close, and And the polar group not having an effect with dye molecule on strand, keep the colouring of PET fiber more difficult.
Therefore, under the general high temperature and pressure of the dyeing of common PET fiber, disperse dyeing is selected, when temperature reaches PET When fiber obtains glass transition temperature or more, gap increases between PET fiber polymer molecule, but the increased degree of its free volume is small, Dyeing rate is not high, but it is the main problem faced now that energy consumption and dye-uptake caused by high temperature and high pressure method are low.In addition, PET fiber melt viscosity is higher, is unfavorable for processing.
There are many method for preparing PET fiber, and wherein melt spinning method is one kind more in current industrial production application.It is molten Melt many of spinning process parameter, these parameters determine the course of fiberizing and spin the structure and performance of fiber, production Upper is exactly the fiber for being made by controlling these parameters required performance.The main spinning that can will be controlled in production according to technical process Silk summary of parameters.An is melting condition, spinning conditions, condition of cure, wrapping wire condition etc., and wherein strand cools and solidifies condition to fiber Structure has conclusive influence with performance, and the cooling velocity and its uniformity of polyester fondant thread, are generally adopted in production in order to control Take cooling blowing.Cooling blowing can accelerate the cooling velocity of melt stream, be conducive to improve spinning speed；Reinforce empty around strand The convection current of gas keeps the cooling of ectonexine strand uniform, to create condition using porous spinneret；Cooling blowing can make as-spun fibre Quality advance, tensile property improve, and are conducive to the production capacity for improving equipment.
Experimental branch line all uses cross air blasting as the type of cooling for a long time, and energy consumption accounts for long filament production cost very Most of, as people increasingly improve chemical fibre performance and quality requirements, the exploitation of chemical-fibres filaments new product is to high added value Fibre in differentiation direction is developed, it is desirable that higher cooling blowing condition then proposes ring blowing device.Ring blowing device is not only Have a uniform advantage of every synnema wind-engaging, and energy consumption is compared to relatively low, effective solution cross air blasting since blowing area is big and Caused by wind energy lose problem.
In spinning process, although ring blowing has apparent advantage, problem is still remained：Due to spun silk from After round spinneret squeezes out, by ring wind quenching, since the round spinneret number of turns is more so that ring blowing hardly enters most interior Layer, leads to that the silk of innermost layer may be also uncolled after cooling in outermost silk, so that fiber number occur irregular for the silk of gained, The problems such as intensity is irregular, uneven dyeing causes the further processing subsequently to silk difficulty occur.
Invention content
The purpose of the present invention is overcoming the problems such as existing dyeing polyester fibers are irregular, mechanical property is poor, realize extensive The production spinning of change provides porous super flexible polyester fiber FDY of one kind and preparation method thereof.The original of the polyester fiber of the present invention Material is modified poly ester, and the hexylene glycol segment containing branch is introduced in the strand of modified poly ester, and modified polyester is prepared porous super Flexible polyester fiber FDY, under the conditions of certain temperature, between the space of porous super FDY interior molecules interchains of flexible polyester fiber The increasing degree of gap is far longer than conventional polyester fiber unbranched at same temperature, is conducive to the entrance of the molecules such as coloring agent Internal degree improves dyeing rate；The melt viscosity of porous super flexible polyester fiber FDY reduces, and reduces processing temperature, subtracts Few degradation rate, is conducive to process；In addition the hexylene glycol segment containing branch advises the structure of porous super flexible polyester fiber FDY The not big destruction of whole property, maintains the excellent performance of polyester fiber.It is arranged using spinneret orifice ellipse in spinning process of the present invention The spinneret of row, be conducive to fiber in spinning process it is uniform, be fully cooled, performance between fiber and structure difference compared with It is small, improve the dyeing uniformity and mechanical property of fiber.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
The material of a kind of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is modified poly- Ester, the modified poly ester are made of terephthalic acid (TPA) segment, ethylene glycol segment and hexylene glycol segment containing branch, described to contain branch Hexylene glycol segment refer on a non-end group carbon that branch is located in hexylene glycol segment and branch is containing 5-10 carbon atom Linear carbon chain hexylene glycol segment；
The filament number of porous super flexible polyester fiber FDY is 0.3~2.0dtex, initial modulus≤70cN/ Dtex, fracture strength >=3.8cN/dtex, elongation at break are 33.0 ± 3.0%；Porous super flexible polyester fiber FDY In the case where temperature is 80~130 DEG C, the spatial joint clearance of fibrous inside molecule interchain increases 10~30v/v%, at 260~290 DEG C, Melt viscosity declines 10~20%；Line density deviation ratio≤0.5% of porous super flexible polyester fiber FDY, fracture are strong Spend CV value≤4.0%, extension at break CV value≤8.0%, yarn unevenness CV≤2.0%.
The present invention also provides a kind of preparation methods of porous super flexible polyester fiber FDY, by modified poly ester using more Porous super flexible polyester fiber FDY is made in hole spinneret spinning；The arrangement mode of spinneret orifice is ellipse on the porous spinneret Circular arrangement, the oval shaped arrangements refer to that the hole center of spinneret orifice is located on concentration ellipse, and the concentration ellipse is that series is ellipse Circle, all elliptical long axis are conllinear, and short axle is conllinear；
The preparation method of porous super flexible polyester fiber FDY is：Modified poly ester obtains modified poly ester through pelletizing and cuts Piece, Modified polyester chips through metering, extrusion, cooling, oil, stretch, modified poly ester FDY is made in thermal finalization and winding；
The preparation process of the modified poly ester is：
(1) preparation of terephthalic acid (TPA) binary alcohol esters；
After terephthalic acid (TPA) and the hexylene glycol containing branch are made into slurry, under the catalytic action of the concentrated sulfuric acid, it is esterified Terephthalic acid (TPA) binary alcohol esters are obtained by the reaction；The hexylene glycol containing branch refers to that be located in hexylene glycol segment one of branch is non- On end group carbon and branch be the linear carbon chain containing 5-10 carbon atom dihydric alcohol；
For the hexylene glycol containing branch, branch is alkyl, is electron-withdrawing group, in the presence of branch, makes strand Spatial volume increases, and solvation becomes smaller, and proton is not easy to dissociate in dihydric alcohol so that the hexylene glycol containing branch and terephthaldehyde The reactivity of acid is less than ethylene glycol, mixes according to same ethylene glycol and reacts with terephthalic acid (TPA), can cause containing branch oneself two Alcohol reaction is imperfect, to influence ratio of the hexylene glycol containing branch in polyester macromolecule, and then influences the performance of polyester.This Using the hexylene glycol containing branch is first carried out esterification under the catalytic action of sulfuric acid with terephthalic acid (TPA), product exists for invention It is added after ethylene glycol and p phthalic acid esterification, ensure that the stability of the hexylene glycol proportioning containing branch；
(2) preparation of ethylene glycol terephthalate；
After terephthalic acid (TPA) and ethylene glycol are made into slurry, esterification is carried out, ethylene glycol terephthalate is obtained；
(3) preparation of modified poly ester；
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, stir Mix mixing, under the action of catalyst and stabilizer, under conditions of negative pressure, successively carry out low vacuum stage polycondensation reaction and Modified poly ester is made in the polycondensation reaction of high vacuum stage of Fig.
As preferred technical solution：
A kind of preparation method of porous super flexible polyester fiber FDY as described above, the specific system of the modified poly ester It is for step：
(1) preparation of terephthalic acid (TPA) binary alcohol esters；
Terephthalic acid (TPA) and the hexylene glycol containing branch are made into slurry, under the catalytic action of the concentrated sulfuric acid, be esterified anti- It answers, 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 to change when the water quantity of distillate in reaction reaches 90% of theoretical value or more, obtains terephthalic acid (TPA) dihydric alcohol Ester；
(2) preparation of ethylene glycol terephthalate；
After terephthalic acid (TPA) and ethylene glycol are made into slurry, esterification is carried out, esterification is pressurizeed in nitrogen atmosphere Reaction, moulding pressure are normal pressure~0.3MPa, and temperature is 250~260 DEG C, when the water quantity of distillate in esterification reaches theoretical value 90% or more when be esterification terminal, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, stir Mixing 15-20 minutes is mixed, under the action of catalyst and stabilizer, the polycondensation for starting low vacuum stage under conditions of negative pressure is anti- It answers, which by normal pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 260~270 DEG C, and the reaction time is 30~50 minutes；It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure and be less than Modified poly ester is made in 275~280 DEG C, 50~90 minutes reaction time in 100Pa, reaction temperature control；
The main spinning technology parameter of porous super flexible polyester fiber FDY is：
The temperature of extrusion：280~290 DEG C；
Cooling wind-warm syndrome：20~25 DEG C；
The speed of winding：4000~4600m/min.
A kind of preparation method of porous super flexible polyester fiber FDY as described above, in step (1), terephthalic acid (TPA) Molar ratio with the hexylene glycol containing branch is 1:1.3-1.5；Concentrated sulfuric acid addition is the 0.3-0.5% of terephthalic acid (TPA) weight； A concentration of 50-60wt% of the concentrated sulfuric acid；
In step (2), the molar ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2~2.0；
In step (3), the Mole percent ratio of the terephthalic acid (TPA) binary alcohol esters and ethylene glycol terephthalate is 2 ~5%；The catalyst is antimony oxide, antimony glycol or antimony acetate, and catalyst charge is terephthalic acid (TPA) total weight 0.01%~0.05%；The stabilizer is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite, stabilizer addition It is the 0.01%~0.05% of the terephthalic acid (TPA) total weight；
The number-average molecular weight of the modified poly ester is 15000~30000.
A kind of preparation method of porous super flexible polyester fiber FDY as described above, the hexylene glycol containing branch are 2- amyls -1,6 hexylene glycol, 2- hexyl -1,6 hexylene glycols, 2- heptyl -1,6 hexylene glycol, 2- octyls -1,6 hexylene glycol, nonyl -1 2-, One or more of -1,6 hexylene glycol of 6 hexylene glycols or 2- decyls.
A kind of preparation method of porous super flexible polyester fiber FDY as described above, the spinneret orifice are arranged as growing Axis and/or short axle are symmetrical.
A kind of preparation method of porous super flexible polyester fiber FDY as described above, elliptical long axis and minor axis length Ratio be 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.When spinneret For effective area phase simultaneously as the perimeter of ellipse is more than circular perimeter, the number of plies of spinneret orifice oval shaped arrangements is less than circle The number of plies of arrangement, the hole count of spinneret orifice oval shaped arrangements are more than the hole count of circular arrangement, and therefore, spinneret orifice oval shaped arrangements are advantageous In the cooling of ring blowing, the cooling efficiency of ring blowing is improved, the fibre property of preparation is also more excellent.Long axis and minor axis length Ratio is closer to 1, and ellipse is more similar to justify, and the difference of cooling efficiency and cooling effect is little；The ratio of long axis and minor axis length When value is 1.3, cooling effect significantly improves individual pen hole count and accordingly increases by 16%；It is cold when long axis and the ratio of minor axis length are 1.8 But effect improves larger, the accordingly increase by 33% of individual pen hole count, and in the case of identical hole count, oval shaped arrangements of the invention are more same than conventional The number of turns of heart circle best-fit is reduced, and is easy to cooling wind and is blown through, makes the fiber cooling condition of Internal and external cycle evenly；Long axis and minor axis length Ratio be more than 1.8 when, ellipse be partial to form flat shape, be not easy to punch, cooling no longer increases.Therefore, The elliptical long axis of series and the ratio of minor axis length are 1.3~1.8, can reach higher cooling efficiency and preferable cooling is imitated Fruit.
A kind of preparation method of porous super flexible polyester fiber FDY as described above, the spinneret are round spinneret Plate or elliptical spinneret plate；The diameter of the circle spinneret and the difference of the oval maximum long axis length of series are more than 10mm, The elliptical spinneret plate and the difference of the oval maximum long axis length of series are more than 10mm.
A kind of preparation method of porous super flexible polyester fiber FDY as described above, the guide hole diameter of the spinneret orifice For 1.5~2.5mm；The spinneret hole count of the spinneret is more than or equal to 192.
A kind of preparation method of porous super flexible polyester fiber FDY as described above, the spinneret orifice of the spinneret Cross-sectional shape be circle, square, diamond shape, "-" type, triangular form, trilobal cross, hollow type or platypelloid type.
The principle of the present invention is：
For unbranched polyester fiber, molecular chain structure is the linear macromolecule containing benzene ring structure, on strand Functional group's marshalling, regularity is good, flexible poor；Its free volume increments is small when the temperature rises, the resistance of these characteristics Dyestuff has been hindered 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 hexylene glycol containing branch contained in modified poly ester macromolecular Segment, when temperature is higher than glass transition temperature, branch makes the increasing degree of free volume be far longer than no branch prior to backbone motion The characteristic of the polyester macromolecule chain of chain, the increase of free volume improves molecule and enters degree inside polyester, modified The free volume of polyester fiber prepared by polyester is far longer than polyester fiber unbranched at same temperature, increases the diffusion of dyestuff Degree improves the dyeability of polyester fiber.Meanwhile polyester fiber prepared by modified poly ester advantageously reduces melt viscosity, has Conducive to its processing performance of improvement.The introducing of hexylene glycol segment containing the branch destruction not big to polyester fiber structures regularity, Maintain the excellent performance of polyester fiber.
When the effective area phase of spinneret is simultaneously as the perimeter of ellipse is more than circular perimeter, spinneret orifice ellipse 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 wire hole oval shaped arrangements enables to fiber quick, uniformly cooling, and the difference of structure and performance is smaller between fiber, Be conducive to improve the performance of the even dyeing rate and fiber of fiber.
Advantageous effect：
1) arrangement mode of spinneret orifice is oval shaped arrangements on spinneret of the invention, 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 it is more preferable, the fibre property of preparation is also more excellent.
2) arrangement mode of spinneret orifice is oval shaped arrangements on spinneret of the invention, 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 can realize a greater degree of cooling, Significantly improve cooling efficiency.
3) material of porous super flexible polyester fiber FDY produced by the present invention is modified poly ester, modified poly ester macromolecular In the hexylene glycol segment containing branch that contains, when temperature is higher than glass transition temperature, branch makes free volume prior to backbone motion Increasing degree be far longer than the characteristic of unbranched polyester macromolecule chain, the increase of free volume improves molecule entrance Degree inside polyester increases the free volume of polyester fiber by branch to increase the diffusion of dyestuff, improves polyester The dyeability of fiber.
4) porous super flexible polyester fiber FDY produced by the present invention, the increase of polyester fiber free volume is conducive to drop Low melt viscosity is conducive to improve its processing performance.
5) porous super flexible polyester fiber FDY produced by the present invention, the introducing of the hexylene glycol segment containing branch is to gathering The not big destruction of the structural regularity of ester fiber, maintains the excellent performance of polyester fiber.
6) porous FDY dyeabilities of super flexible polyester fiber and good mechanical performance produced by the present invention, initial modulus ≤ 70cN/dtex, line density deviation ratio≤0.5% of porous super flexible polyester fiber FDY, fracture strength CV value≤4.0%, Extension at break CV value≤8.0%, yarn unevenness CV≤2.0%.
Description of the drawings
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 It is 1.3 to spend ratio；
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 It is 1.6 to spend ratio.
Specific implementation mode
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Fixed range.
Embodiment 1
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.3 terephthalic acid (TPA) is made into slurry with 2- amyl -1,6 hexylene glycols and is added in reactor, A concentration of 50wt%, addition are to carry out esterification under the catalytic action of 0.3% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure are normal pressure, and temperature is 180 DEG C, when the water in esterification distillates Amount is esterification terminal when reaching the 90% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.2 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure are normal pressure, and temperature is 250 DEG C, when the water in esterification distillates Amount is esterification terminal when reaching the 90% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2%, is stirred 15 minutes, is being added Amount is 0.01% the catalytic antimony trioxide of terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight 0.01% Stabilizer triphenyl phosphate under the action of, under conditions of negative pressure start low vacuum stage polycondensation reaction, the staged pressure It is 500Pa that absolute pressure is steadily evacuated to by normal pressure, and at 260 DEG C, the reaction time is 30 minutes for temperature control；It then proceedes to take out true Sky carries out the polycondensation reaction of high vacuum stage of Fig, and it is 100Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled 275 DEG C, modified poly ester was made in 50 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 15000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- penta Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- amyl -1,6 hexylene glycol segments and ethylene glycol segment is 2%.
Embodiment 2
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.38 terephthalic acid (TPA) is made into slurry with 2- hexyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.32% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.13MPa, temperature is 181 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 91% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.3 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.12MPa, temperature is 251 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 91% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2.1%, is stirred 16 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.011% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.02% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 262 DEG C, the reaction time is 31 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be down to absolute pressure 99Pa, and reaction temperature is controlled at 276 DEG C, Modified poly ester was made in 51 minutes reaction time.
The number-average molecular weight of modified poly ester obtained be 16000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- oneself Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- hexyl -1,6 hexylene glycol segments and ethylene glycol segment is 2.1%.
Embodiment 3
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.33 terephthalic acid (TPA) is made into slurry with 2- heptyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.33% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.12MPa, temperature is 183 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.31 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.31MPa, temperature is 252 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2.2%, is stirred 16 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.03% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.02% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 498Pa by normal pressure, and at 263 DEG C, the reaction time is 32 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be down to absolute pressure 80Pa, and reaction temperature is controlled at 277 DEG C, Modified poly ester was made in 57 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 15900, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- heptan Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- heptyl -1,6 hexylene glycol segments and ethylene glycol segment is 2.2%.
Embodiment 4
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.34 terephthalic acid (TPA) is made into slurry with 2- octyl -1,6 hexylene glycols and is added in reactor, A concentration of 60wt%, addition are to carry out esterification under the catalytic action of 0.34% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.13MPa, temperature is 184 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 93% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.32 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.33MPa, temperature is 253 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 93% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2.3%, is stirred 17 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.033% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.023% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure It is 497Pa that section pressure, which is steadily evacuated to absolute pressure by normal pressure, and at 264 DEG C, the reaction time is 33 minutes for temperature control；It then proceedes to It vacuumizes, carries out the polycondensation reaction of high vacuum stage of Fig, it is 80Pa so that reaction pressure is down to absolute pressure, and reaction temperature control exists 278 DEG C, modified poly ester was made in 58 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 15800, pungent by terephthalic acid (TPA) segment, ethylene glycol segment and 2- Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- octyl -1,6 hexylene glycol segments and ethylene glycol segment is 2.3%.
Embodiment 5
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.35 terephthalic acid (TPA) is made into slurry with 2- nonyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.36% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.14MPa, temperature is 185 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 93.2% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.33 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.14MPa, temperature is 254 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 93.2% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2.4%, is stirred 17 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.034% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.024% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and at 265 DEG C, the reaction time is 34 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and it is 70Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled 277 DEG C, modified poly ester was made in 59 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 15900, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- nonyls Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- nonyl -1,6 hexylene glycol segments and ethylene glycol segment is 2.4%.
Embodiment 6
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.36 terephthalic acid (TPA) is made into slurry with 2- decyl -1,6 hexylene glycols and is added in reactor, A concentration of 50wt%, addition are to carry out esterification under the catalytic action of 0.37% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.15MPa, temperature is 186 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 93.3% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.34 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.15MPa, temperature is 255 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 93.3% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2.5%, is stirred 18 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.035% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.025% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 266 DEG C, the reaction time is 35 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and it is 70Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled 278 DEG C, modified poly ester was made in 60 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 16000, by terephthalic acid (TPA) segment, ethylene glycol segment and the 2- last of the ten Heavenly stems Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- decyl -1,6 hexylene glycol segments and ethylene glycol segment is 2.5%.
Embodiment 7
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.37 terephthalic acid (TPA) is made into slurry with 2- amyl -1,6 hexylene glycols and is added in reactor, A concentration of 60wt%, addition are to carry out esterification under the catalytic action of 0.38% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.16MPa, temperature is 187 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 93.4% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.36 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.16MPa, temperature is 256 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 93.4% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2.6%, is stirred 19 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.036% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.025% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and at 267 DEG C, the reaction time is 36 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and it is 70Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled 278 DEG C, modified poly ester was made in 61 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 16000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- penta Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- amyl -1,6 hexylene glycol segments and ethylene glycol segment is 2.6%.
Embodiment 8
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.38 terephthalic acid (TPA) is made into slurry with 2- hexyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.39% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.17MPa, temperature is 188 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 93.5% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.37 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.17MPa, temperature is 257 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 93.5% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2.7%, is stirred 19 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.036% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.025% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and at 267 DEG C, the reaction time is 36 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and it is 60Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled 278 DEG C, modified poly ester was made in 61 minutes reaction time.
The number-average molecular weight of modified poly ester obtained be 17000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- oneself Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- hexyl -1,6 hexylene glycol segments and ethylene glycol segment is 2.7%.
Embodiment 9
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.39 terephthalic acid (TPA) is made into slurry with 2- heptyl -1,6 hexylene glycols and is added in reactor, A concentration of 50wt%, addition are to carry out esterification under the catalytic action of 0.4% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.17MPa, temperature is 188 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 93.5% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.37 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.17MPa, temperature is 257 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 93.5% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2.8%, is stirred 16 minutes, is adding Enter 0.04% catalyst glycol antimony that amount is terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight 0.026% Stabilizer trimethyl phosphate under the action of, under conditions of negative pressure start low vacuum stage polycondensation reaction, the staged pressure Absolute pressure 497Pa is steadily evacuated to by normal pressure, at 268 DEG C, the reaction time is 38 minutes for temperature control；It then proceedes to vacuumize, The polycondensation reaction for carrying out high vacuum stage of Fig, it is 50Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled at 279 DEG C, instead 62 minutes between seasonable, modified poly ester is made.
The number-average molecular weight of modified poly ester obtained is 18000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- heptan Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- heptyl -1,6 hexylene glycol segments and ethylene glycol segment is 2.8%.
Embodiment 10
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.4 terephthalic acid (TPA) is made into slurry with 2- octyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.4% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.17MPa, temperature is 188 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 93.5% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.38 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.18MPa, temperature is 257.8 DEG C, when in esterification Water quantity of distillate be esterification terminal when reaching the 93.6% of theoretical value, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 3%, is stirred 17 minutes, is being added Amount is 0.03% catalyst glycol antimony of terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight 0.027% Under the action of stabilizer trimethyl phosphate, under conditions of negative pressure start low vacuum stage polycondensation reaction, the staged pressure by Normal pressure is steadily evacuated to absolute pressure 498Pa, and at 269 DEG C, the reaction time is 39 minutes for temperature control；It then proceedes to vacuumize, into The polycondensation reaction of row high vacuum stage of Fig, it is 50Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled at 278 DEG C, reaction Modified poly ester was made in 64 minutes time.
The number-average molecular weight of modified poly ester obtained is 19000, pungent by terephthalic acid (TPA) segment, ethylene glycol segment and 2- Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- octyl -1,6 hexylene glycol segments and ethylene glycol segment is 3%.
Embodiment 11
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.4 terephthalic acid (TPA) is made into slurry with 2- nonyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.4% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.18MPa, temperature is 189 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 93.6% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.39 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.19MPa, temperature is 258.8 DEG C, when in esterification Water quantity of distillate be esterification terminal when reaching the 94% of theoretical value, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4%, is stirred 18 minutes, is being added Amount is 0.04% catalyst glycol antimony of terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight 0.03% Under the action of stabilizer trimethyl phosphate, under conditions of negative pressure start low vacuum stage polycondensation reaction, the staged pressure by Normal pressure is steadily evacuated to absolute pressure 497Pa, and at 260 DEG C, the reaction time is 40 minutes for temperature control；It then proceedes to vacuumize, into The polycondensation reaction of row high vacuum stage of Fig, it is 40Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled at 277 DEG C, reaction Modified poly ester was made in 63 minutes time.
The number-average molecular weight of modified poly ester obtained is 20000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- nonyls Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- nonyl -1,6 hexylene glycol segments and ethylene glycol segment is 4%.
Embodiment 12
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.4 terephthalic acid (TPA) is made into slurry with 2- nonyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.4% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.2MPa, temperature is 200 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 94% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.6 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.2MPa, temperature is 256 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 94% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.5%, is stirred 18 minutes, is adding Enter the 0.038% catalyst acetic acid antimony that amount is terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight 0.03% Under the action of stabilizer Trimethyl phosphite, start the polycondensation reaction of low vacuum stage, the staged pressure under conditions of negative pressure Absolute pressure 497Pa is steadily evacuated to by normal pressure, at 265 DEG C, the reaction time is 42 minutes for temperature control；It then proceedes to vacuumize, The polycondensation reaction for carrying out high vacuum stage of Fig, it is 40Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled at 277 DEG C, instead 70 minutes between seasonable, modified poly ester is made.
The number-average molecular weight of modified poly ester obtained is 26000, by terephthalic acid (TPA) segment, ethylene glycol segment and the 2- last of the ten Heavenly stems Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- decyl -1,6 hexylene glycol segments and ethylene glycol segment is 4%.
Embodiment 13
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.5 terephthalic acid (TPA) is made into slurry with 2- decyl -1,6 hexylene glycols and is added in reactor, A concentration of 60wt%, addition are to carry out esterification under the catalytic action of 0.5% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.3MPa, temperature is 240 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:2.0 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.3MPa, temperature is 260 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 5%, is stirred 20 minutes, is being added Amount be 0.05% catalyst acetic acid antimony of terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight 0.05% it is steady Under the action of determining agent Trimethyl phosphite, under conditions of negative pressure start low vacuum stage polycondensation reaction, the staged pressure by It is 450Pa that normal pressure, which is steadily evacuated to absolute pressure, and at 270 DEG C, the reaction time is 50 minutes for temperature control；It then proceedes to vacuumize, The polycondensation reaction for carrying out high vacuum stage of Fig, it is 30Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled at 280 DEG C, instead 90 minutes between seasonable, modified poly ester is made.
The number-average molecular weight of modified poly ester obtained is 30000, by terephthalic acid (TPA) segment, ethylene glycol segment and the 2- last of the ten Heavenly stems Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- decyl -1,6 hexylene glycol segments and ethylene glycol segment is 5%.
Embodiment 14
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.47 terephthalic acid (TPA) is made into slurry with 2- nonyl -1,6 hexylene glycols and is added in reactor, A concentration of 60wt%, addition are to carry out esterification under the catalytic action of 0.47% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 220 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.8 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.27MPa, temperature is 258 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4%, is stirred 18 minutes, is being added Amount is 0.04% catalyst glycol antimony of terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight 0.04% Under the action of stabilizer trimethyl phosphate, under conditions of negative pressure start low vacuum stage polycondensation reaction, the staged pressure by Normal pressure is steadily evacuated to absolute pressure 460Pa, and at 263 DEG C, the reaction time is 47 minutes for temperature control；It then proceedes to vacuumize, into The polycondensation reaction of row high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature is controlled at 278 DEG C, reaction Between 85 minutes, be made modified poly ester.
The number-average molecular weight of modified poly ester obtained is 28000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- nonyls Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- nonyl -1,6 hexylene glycol segments and ethylene glycol segment is 4%.
Embodiment 15
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.46 terephthalic acid (TPA) is made into slurry with 2- octyl -1,6 hexylene glycols and is added in reactor, A concentration of 60wt%, addition are to carry out esterification under the catalytic action of 0.49% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 233 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.8 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 259 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.5%, is stirred 19 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.044% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.046% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 269 DEG C, the reaction time is 48 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be down to absolute pressure 40Pa, and reaction temperature is controlled at 279 DEG C, Modified poly ester was made in 87 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 29000, pungent by terephthalic acid (TPA) segment, ethylene glycol segment and 2- Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- octyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.5%.
Embodiment 16
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.49 terephthalic acid (TPA) is made into slurry with 2- heptyl -1,6 hexylene glycols and is added in reactor, A concentration of 60wt%, addition are to carry out esterification under the catalytic action of 0.48% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 230 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.8 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 258 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.7%, is stirred 19 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.048% catalyst glycol antimony that amount is terephthalic acid (TPA) weight and addition Under the action of 0.047% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 460Pa by normal pressure, and at 267 DEG C, the reaction time is 48 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be down to absolute pressure 40Pa, and reaction temperature is controlled at 279 DEG C, Modified poly ester was made in 83 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 27000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- heptan Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- heptyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.7%.
Embodiment 17
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.467 terephthalic acid (TPA) is made into slurry with 2- hexyl -1,6 hexylene glycols and is added in reactor, In a concentration of 60wt%, addition is be esterified anti-under the catalytic action of 0.47% concentrated sulfuric acid of terephthalic acid (TPA) weight It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.27MPa, temperature is 236 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.89 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 258 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.3%, is stirred 18 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.04% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.041% stabilizer Trimethyl phosphite, start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should Staged pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 268 DEG C, the reaction time is 48 minutes for temperature control；It then proceedes to It vacuumizes, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be down to absolute pressure 40Pa, reaction temperature is controlled 278 DEG C, modified poly ester was made in 85 minutes reaction time.
The number-average molecular weight of modified poly ester obtained be 29000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- oneself Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- hexyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.3%.
Embodiment 18
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.48 terephthalic acid (TPA) is made into slurry with 2- amyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.46% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 230 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.88 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 256 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.7%, is stirred 18 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.047% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.047% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 480Pa by normal pressure, and at 265 DEG C, the reaction time is 47 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be down to absolute pressure 40Pa, and reaction temperature is controlled at 279 DEG C, Modified poly ester was made in 85 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 28000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- penta Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- amyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.7%.
Embodiment 19
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.46 terephthalic acid (TPA) is made into slurry with 2- decyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.47% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 238 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.9 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 259 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching 92% of theoretical value or more, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.7%, is stirred 19 minutes, is adding Enter the 0.046% catalyst acetic acid antimony that amount is terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight 0.048% Stabilizer Trimethyl phosphite under the action of, under conditions of negative pressure start low vacuum stage polycondensation reaction, the stage pressure It is 446Pa that power, which is steadily evacuated to absolute pressure by normal pressure, and at 267 DEG C, the reaction time is 49 minutes for temperature control；It then proceedes to take out true Sky carries out the polycondensation reaction of high vacuum stage of Fig, and it is 40Pa so that reaction pressure is down to absolute pressure, and reaction temperature is controlled at 278 DEG C, Modified poly ester was made in 87 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 29000, by terephthalic acid (TPA) segment, ethylene glycol segment and the 2- last of the ten Heavenly stems Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- decyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.7%.
Embodiment 20
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.46 terephthalic acid (TPA) is made into slurry with 2- nonyl -1,6 hexylene glycols and is added in reactor, A concentration of 60wt%, addition are to carry out esterification under the catalytic action of 0.46% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.26MPa, temperature is 221 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.89 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.25MPa, temperature is 259 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.1%, is stirred 18 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.041% catalyst glycol antimony that amount is terephthalic acid (TPA) weight and addition Under the action of 0.042% stabilizer trimethyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 460Pa by normal pressure, and at 265 DEG C, the reaction time is 47 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be down to absolute pressure 40Pa, and reaction temperature is controlled at 278 DEG C, Modified poly ester was made in 85 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 28000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- nonyls Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- nonyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.1%.
Embodiment 21
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.43 terephthalic acid (TPA) is made into slurry with 2- octyl -1,6 hexylene glycols and is added in reactor, A concentration of 60wt%, addition are to carry out esterification under the catalytic action of 0.47% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.27MPa, temperature is 235 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.78 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.26MPa, temperature is 255 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.3%, is stirred 17 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.043% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.049% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 268 DEG C, the reaction time is 46 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be down to absolute pressure 40Pa, and reaction temperature is controlled at 275 DEG C, Modified poly ester was made in 85 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 28000, pungent by terephthalic acid (TPA) segment, ethylene glycol segment and 2- Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- octyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.3%.
Embodiment 22
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.43 terephthalic acid (TPA) is made into slurry with 2- heptyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.45% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.29MPa, temperature is 235 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.87 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.27MPa, temperature is 255 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.6%, is stirred 18 minutes, is adding Enter 0.047% catalyst glycol antimony that amount is terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight 0.04% Stabilizer triphenyl phosphate under the action of, under conditions of negative pressure start low vacuum stage polycondensation reaction, the staged pressure Absolute pressure 470Pa is steadily evacuated to by normal pressure, at 268 DEG C, the reaction time is 45 minutes for temperature control；It then proceedes to vacuumize, The polycondensation reaction for carrying out high vacuum stage of Fig makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature is controlled at 279 DEG C, reaction Modified poly ester was made in 83 minutes time.
The number-average molecular weight of modified poly ester obtained is 29000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- heptan Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- heptyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.6%.
Embodiment 23
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.457 terephthalic acid (TPA) is made into slurry with 2- hexyl -1,6 hexylene glycols and is added in reactor, A concentration of 55%, addition is to carry out esterification under the catalytic action of 0.46% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 239 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.81 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.27MPa, temperature is 255 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.41%, is stirred 19 minutes, Addition is 0.042% the catalytic antimony trioxide of terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight Under the action of 0.048% stabilizer Trimethyl phosphite, start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the reaction time is 45 minutes for temperature control；It then proceedes to It vacuumizes, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be down to absolute pressure 50Pa, reaction temperature is controlled 275 DEG C, modified poly ester was made in 85 minutes reaction time.
The number-average molecular weight of modified poly ester obtained be 28000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- oneself Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- hexyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.41%.
Embodiment 24
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.47 terephthalic acid (TPA) is made into slurry with 2- amyl -1,6 hexylene glycols and is added in reactor, A concentration of 55wt%, addition are to carry out esterification under the catalytic action of 0.48% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.27MPa, temperature is 245 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.81 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.27MPa, temperature is 259 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.67%, is stirred 19 minutes, Addition is 0.041% the catalytic antimony trioxide of terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight Under the action of 0.042% stabilizer triphenyl phosphate, start the polycondensation reaction of low vacuum stage, the rank under conditions of negative pressure Section pressure is steadily evacuated to absolute pressure 485Pa by normal pressure, and at 268 DEG C, the reaction time is 46 minutes for temperature control；It then proceedes to take out Vacuum carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be down to absolute pressure 50Pa, and reaction temperature is controlled at 275 DEG C, Modified poly ester was made in 89 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 29000, by terephthalic acid (TPA) segment, ethylene glycol segment and 2- penta Base -1,6 hexylene glycol segment forms, and the Mole percent ratio of 2- amyl -1,6 hexylene glycol segments and ethylene glycol segment is 4.67%.
Embodiment 25
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.45 terephthalic acid (TPA) is mixed with -1,6 hexylene glycol of -1,6 hexylene glycol of 2- hexyls and 2- amyls It closes object to be made into slurry addition reactor, wherein the molar ratio of 2- hexyls -1,6 hexylene glycol and 2- amyl -1,6 hexylene glycols is 3:1, A concentration of 55%, addition is to carry out esterification under the catalytic action of 0.49% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.26MPa, temperature is 236 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.8 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 258 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.4%, is stirred 18 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.042% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.047% stabilizer Trimethyl phosphite, start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the reaction time is 49 minutes for temperature control；It then proceedes to It vacuumizes, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be down to absolute pressure 50Pa, reaction temperature is controlled 278 DEG C, modified poly ester was made in 88 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 29000, by terephthalic acid (TPA) segment, ethylene glycol segment, 2- hexyls- 1,6 hexylene glycol segment and 2- amyl -1,6 hexylene glycol segments composition, 2- hexyl -1,6 hexylene glycol segments and 2- amyls -1,6 oneself 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 terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.45 terephthalic acid (TPA) and -1,6 hexylene glycol of 2- octyls and -1,6 hexylene glycol of 2- amyls Mixture is made into slurry and is added in reactor, and the molar ratio of wherein 2- octyls -1,6 hexylene glycol and 2- amyl -1,6 hexylene glycols is 3: 2, a concentration of 60%, addition is be esterified anti-under the catalytic action of 0.45% concentrated sulfuric acid of terephthalic acid (TPA) weight It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 239 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.84 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, be esterified anti- It answers, esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.29MPa, temperature is 255 DEG C, when in esterification Water quantity of distillate is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.6%, is stirred 18 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.0423% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.045% stabilizer Trimethyl phosphite, start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the reaction time is 45 minutes for temperature control；It then proceedes to It vacuumizes, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be down to absolute pressure 50Pa, reaction temperature is controlled 278 DEG C, modified poly ester was made in 85 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 28000, by terephthalic acid (TPA) segment, ethylene glycol segment, 2- octyls- 1,6 hexylene glycol segment and 2- amyl -1,6 hexylene glycol segments composition, 2- octyl -1,6 hexylene glycol segments and 2- amyls -1,6 oneself two The Mole percent ratio of alcohol segment and ethylene glycol segment is 4.6%.
Embodiment 27
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.45 terephthalic acid (TPA) is mixed with -1,6 hexylene glycol of -1,6 hexylene glycol of 2- hexyls and 2- amyls It closes object to be made into slurry addition reactor, wherein the molar ratio of 2- hexyls -1,6 hexylene glycol and 2- amyl -1,6 hexylene glycols is 3:1, A concentration of 55%, addition is to carry out esterification under the catalytic action of 0.49% concentrated sulfuric acid of terephthalic acid (TPA) weight, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.26MPa, temperature is 236 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 96% of theoretical value, obtains terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.8 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.28MPa, temperature is 258 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.4%, is stirred 18 minutes, is adding It is terephthalic acid (TPA) weight to enter 0.042% the catalytic antimony trioxide that amount is terephthalic acid (TPA) weight and addition Under the action of 0.047% stabilizer Trimethyl phosphite, start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the reaction time is 49 minutes for temperature control；It then proceedes to It vacuumizes, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be down to absolute pressure 50Pa, reaction temperature is controlled 278 DEG C, modified poly ester was made in 88 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 29000, by terephthalic acid (TPA) segment, ethylene glycol segment, 2- hexyls- 1,6 hexylene glycol segment and 2- amyls-Isosorbide-5-Nitrae butanediol segment composition, 2- hexyl -1,6 hexylene glycol segments and 2- amyls-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 terephthalic acid (TPA) binary alcohol esters：
It is 1 by molar ratio:1.45 terephthalic acid (TPA) and -1,6 hexylene glycol of 2- octyls, -1,6 hexylene glycol of 2- amyls and 2- oneself The mixture of base -1,6 hexylene glycol is made into slurry and is added in reactor, wherein 2- octyls -1,3 propylene glycol, 2- amyls-Isosorbide-5-Nitrae fourth two The molar ratio of -1,6 hexylene glycol of alcohol and 2- hexyls is 3:2:1, a concentration of 60%, addition is terephthalic acid (TPA) weight Under the catalytic action of 0.47% concentrated sulfuric acid, esterification, esterification compressive reaction in nitrogen atmosphere, moulding pressure are carried out 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 terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
It is 1 by molar ratio:1.8 terephthalic acid (TPA)s and ethylene glycol are added after being made into slurry in reactor, carry out esterification, Esterification compressive reaction in nitrogen atmosphere, moulding pressure 0.27MPa, temperature is 258 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, it is right The Mole percent ratio of phthalic acid binary alcohol esters and ethylene glycol terephthalate is 4.71%, is stirred 18 minutes, Addition is 0.04% the catalytic antimony trioxide of terephthalic acid (TPA) weight and addition is terephthalic acid (TPA) weight Under the action of 0.041% stabilizer Trimethyl phosphite, start the polycondensation reaction of low vacuum stage under conditions of negative pressure, it should Staged pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 268 DEG C, the reaction time is 49 minutes for temperature control；It then proceedes to It vacuumizes, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be down to absolute pressure 50Pa, reaction temperature is controlled 277 DEG C, modified poly ester was made in 84 minutes reaction time.
The number-average molecular weight of modified poly ester obtained is 29000, by terephthalic acid (TPA) segment, ethylene glycol segment, band branch Glycol segment composition, wherein branched glycol segment be 2- octyl -1,6 hexylene glycols segment, 2- amyl -1,6 hexylene glycol chains Section and 2- hexyl -1,6 hexylene glycol segments composition, the Mole percent ratio of branched glycol segment and ethylene glycol segment are 4.71%.
Embodiment 29
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
As shown in Figure 1, elliptical long axis and the ratio of minor axis length are 1.3, the spacing of adjacent spinneret orifice is equal to spinneret orifice Guide hole diameter add 1.5mm, spinneret is round spinneret, diameter and the oval maximum long axial length of series of round spinneret The difference of degree is 11mm, and the spinneret hole count of a diameter of 2.0mm of guide hole of spinneret orifice, spinneret are 374, the spinneret orifice of spinneret Cross-sectional shape be circle.
By modified modified polyester made from embodiment 1, Modified polyester chips are obtained through pelletizing；Again through metering, extrusion, cold But it, oils, stretch, thermal finalization and winding, being made FDY, the temperature of FDY extrusions is 285 DEG C, and cooling wind-warm syndrome is 25 DEG C, the speed of winding is 4500m/min；
The filament number of porous super flexible polyester fiber FDY is 1.4dtex, initial modulus 68cN/dtex, fracture strength For 4.7cN/dtex, elongation at break 34.7%；Porous super flexible polyester fiber FDY is in the case where temperature is 80 DEG C, in fiber Spatial joint clearance between the subchain of part increases 15v/v%, and at 289 DEG C, melt viscosity declines 16%；Porous super flexible polyester fiber FDY line density deviation ratios are 0.4%, and fracture strength CV values are 3.2%, and extension at break CV values are 6.9%, yarn unevenness CV values are 1.8%.
Embodiment 30
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
As shown in figure 3, elliptical long axis and the ratio of minor axis length are 1.6, the spacing of adjacent spinneret orifice is equal to spinneret orifice Guide hole diameter add 1.5mm, spinneret is round spinneret, diameter and the oval maximum long axial length of series of round spinneret The difference of degree is 11mm, and the spinneret hole count of a diameter of 2.0mm of guide hole of spinneret orifice, spinneret are 382, the spinneret orifice of spinneret Cross-sectional shape be circle.
By modified modified polyester made from embodiment 1, Modified polyester chips are obtained through pelletizing；Again through metering, extrusion, cold But it, oils, stretch, thermal finalization and winding, being made FDY, the temperature of FDY extrusions is 285 DEG C, and cooling wind-warm syndrome is 25 DEG C, the speed of winding is 4500m/min；
The filament number of porous super flexible polyester fiber FDY obtained is 1.7dtex, initial modulus 70cN/dtex, is broken Resistance to spalling is 5.4cN/dtex, elongation at break 35.2%；Porous super flexible polyester fiber FDY in the case where temperature is 80 DEG C, The spatial joint clearance of fibrous inside molecule interchain increases 15v/v%, and at 289 DEG C, melt viscosity declines 16%；It is porous super soft poly- The line density deviation ratio of ester fiber FDY is 0.2%, and fracture strength CV values are 2.2%, and extension at break CV values are 5.9%, and item is dry Irregularity CV values are 1.4%.
Comparative example 1
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is circular arrangement on spinneret, and circular arrangement refers to that the hole center of spinneret orifice is located at On concentric circles, concentric circles is that series is round.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 are round spinneret, and the diameter of round spinneret and the difference of the round maximum diameter of series are 11mm, spray The spinneret hole count of a diameter of 2.0mm of guide hole of wire hole, spinneret are 370, and the cross-sectional shape of the spinneret orifice of spinneret is circle Shape.
By modified modified polyester made from embodiment 1, Modified polyester chips are obtained through pelletizing；Again through metering, extrusion, cold But it, oils, stretch, thermal finalization and winding, being made FDY, the temperature of FDY extrusions is 285 DEG C, and cooling wind-warm syndrome is 25 DEG C, the speed of winding is 4500m/min；
The filament number of porous super flexible polyester fiber FDY obtained is 1.0dtex, initial modulus 65cN/dtex, is broken Resistance to spalling is 3.8cN/dtex, elongation at break 36.0%；Porous super flexible polyester fiber FDY in the case where temperature is 80 DEG C, The spatial joint clearance of fibrous inside molecule interchain increases 15v/v%, and at 289 DEG C, melt viscosity declines 16%；It is porous super soft poly- The line density deviation ratio of ester fiber FDY is 0.7%, and fracture strength CV values are 5.2%, and extension at break CV values are 9.1%, and item is dry Irregularity CV values are 2.8%.
With embodiment 29 comparison as can be seen that the effective area of spinneret it is identical when, (circular arrangement when spinneret hole count is close Spinneret hole count is 370, and oval shaped arrangements spinneret hole count is that 374), the spinneret orifice number of plies of oval shaped arrangements is 6, is less than circular arrangement The spinneret orifice number of plies 8, cooling effect is more preferable；It is oval with the comparison of embodiment 30 as can be seen that when the identical effective area of spinneret The spinneret orifice number of plies of shape arrangement is 5, is less than the spinneret orifice number of plies 8 of circular arrangement, cooling effect is more preferable, the spinneret of oval shaped arrangements The hole count 382 in hole is more than the hole count 370 of the spinneret orifice of circular arrangement, cooling efficiency higher.The comparing result of fibre property shows Fiber linear density deviation ratio made from embodiment 29 and embodiment 30, fracture strength CV values, extension at break CV values and evenness fault Rate CV values are less than comparative example 1, under the conditions of illustrating same process, fibroid made from the spinneret using spinneret orifice oval shaped arrangements It can be better than the spinneret using spinneret circular arrangement.
Embodiment 31~33
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
Spinneret orifice is arranged as long axial symmetry, and the ratio of elliptical long axis and minor axis length is 1.4, between adjacent spinneret orifice 1.6mm is added away from the guide hole diameter equal to spinneret orifice, spinneret is round spinneret, and the diameter and series of round spinneret are oval 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, spinneret The cross-sectional shape of the spinneret orifice of plate is square.
Modified poly ester obtains Modified polyester chips through pelletizing；Again through metering, extrusion, cooling, oil, stretch, thermal finalization and Winding is made FDY, and the temperature of FDY extrusions is 280 DEG C, and cooling wind-warm syndrome is 20 DEG C, and the speed of winding is 4000m/ min；The spatial joint clearance of the super fibrous inside molecule interchain at 80 DEG C of flexible polyester fiber FDY of porous porous obtained increases Rate, the mechanical performance data of the melt viscosity rate of descent and fiber such as following table at 260 DEG C.
Embodiment 34~36
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
Spinneret orifice is arranged as that short axle is symmetrical, and the ratio of elliptical long axis and minor axis length is 1.4, between adjacent spinneret orifice 1.7mm is added away from the guide hole diameter equal to spinneret orifice, spinneret is elliptical spinneret plate, and elliptical spinneret plate is oval most with series The difference of big long axis length is 12mm, and the spinneret hole count of a diameter of 1.8mm of guide hole of spinneret orifice, spinneret are 200, spinneret Spinneret orifice cross-sectional shape be diamond shape.
Modified poly ester obtains Modified polyester chips through pelletizing；Again through metering, extrusion, cooling, oil, stretch, thermal finalization and Winding is made FDY, and the temperature of FDY extrusions is 283 DEG C, and cooling wind-warm syndrome is 22 DEG C, and the speed of winding is 4300m/ min；The spatial joint clearance of the super fibrous inside molecule interchain at 130 DEG C of flexible polyester fiber FDY of porous porous obtained increases Rate, the mechanical performance data of the melt viscosity rate of descent and fiber such as following table at 289 DEG C.
Embodiment 37~39
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as long axis and short axle is symmetrical, the ratio of elliptical long axis and minor axis length is 1.4, adjacent spinneret The guide hole diameter that the spacing in hole is equal to spinneret orifice adds 1.8mm, and spinneret is round spinneret, the diameter of round 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 spinneret hole count of spinneret is 200, the cross-sectional shape of the spinneret orifice of spinneret is "-" type.
Modified poly ester obtains Modified polyester chips through pelletizing；Again through metering, extrusion, cooling, oil, stretch, thermal finalization and Winding is made FDY, and the temperature of FDY extrusions is 286 DEG C, and cooling wind-warm syndrome is 21 DEG C, and the speed of winding is 4400m/ min；The spatial joint clearance of the super fibrous inside molecule interchain at 100 DEG C of flexible polyester fiber FDY of porous porous obtained increases Rate, the mechanical performance data of the melt viscosity rate of descent and fiber such as following table at 290 DEG C.
Embodiment 40~42
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as long axis and short axle is symmetrical, the ratio of elliptical long axis and minor axis length is 1.7, adjacent spinneret The guide hole diameter that the spacing in hole is equal to spinneret orifice adds 1.9mm, and spinneret is elliptical spinneret plate, elliptical spinneret plate and series The difference of oval maximum long axis length is 14mm, and the spinneret hole count of a diameter of 1.5mm of guide hole of spinneret orifice, spinneret are 210, The cross-sectional shape of the spinneret orifice of spinneret is triangular form.
Modified poly ester obtains Modified polyester chips through pelletizing；Again through metering, extrusion, cooling, oil, stretch, thermal finalization and Winding is made FDY, and the temperature of FDY extrusions is 281 DEG C, and cooling wind-warm syndrome is 24 DEG C, and the speed of winding is 4340m/ min；The spatial joint clearance of the super fibrous inside molecule interchain at 110 DEG C of flexible polyester fiber FDY of porous porous obtained increases Rate, the mechanical performance data of the melt viscosity rate of descent and fiber such as following table at 289 DEG C.
Embodiment 43~45
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
Spinneret orifice is arranged as that short axle is symmetrical, and the ratio of elliptical long axis and minor axis length is 1.8, between adjacent spinneret orifice 1.5mm is added away from the guide hole diameter equal to spinneret orifice, spinneret is round spinneret, and the diameter and series of round spinneret are oval The difference of maximum long axis length is 15mm, and the spinneret hole count of a diameter of 1.8mm of guide hole of spinneret orifice, spinneret are 240, spinneret The cross-sectional shape of the spinneret orifice of plate is trilobal cross.
Modified poly ester obtains Modified polyester chips through pelletizing；Again through metering, extrusion, cooling, oil, stretch, thermal finalization and Winding is made FDY, and the temperature of FDY extrusions is 284 DEG C, and cooling wind-warm syndrome is 23 DEG C, and the speed of winding is 4390m/ min；The spatial joint clearance of the super fibrous inside molecule interchain at 120 DEG C of flexible polyester fiber FDY of porous porous obtained increases Rate, the mechanical performance data of the melt viscosity rate of descent and fiber such as following table at 270 DEG C.
Embodiment 46~49
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
Spinneret orifice is arranged as long axial symmetry, and the ratio of elliptical long axis and minor axis length is 1.8, between adjacent spinneret orifice 1.6mm is added away from the guide hole diameter equal to spinneret orifice, spinneret is round spinneret, and the diameter and series of round spinneret are oval The difference of maximum long axis length is 16mm, and the spinneret hole count of a diameter of 2.2mm of guide hole of spinneret orifice, spinneret are 250, spinneret The cross-sectional shape of the spinneret orifice of plate is hollow type.
Modified poly ester obtains Modified polyester chips through pelletizing；Again through metering, extrusion, cooling, oil, stretch, thermal finalization and Winding is made FDY, and the temperature of FDY extrusions is 286 DEG C, and cooling wind-warm syndrome is 25 DEG C, and the speed of winding is 4600m/ min；The spatial joint clearance of the super fibrous inside molecule interchain at 80 DEG C of flexible polyester fiber FDY of porous porous obtained increases Rate, the mechanical performance data of the melt viscosity rate of descent and fiber such as following table at 275 DEG C.
Embodiment 50~53
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
Spinneret orifice is arranged as that short axle is symmetrical, and the ratio of elliptical long axis and minor axis length is 1.8, between adjacent spinneret orifice 1.8mm is added away from the guide hole diameter equal to spinneret orifice, spinneret is round spinneret, and the diameter and series of round spinneret are oval The difference of maximum long axis length is 15mm, and the spinneret hole count of a diameter of 2.5mm of guide hole of spinneret orifice, spinneret are 260, spinneret The cross-sectional shape of the spinneret orifice of plate is platypelloid type.
Modified poly ester obtains Modified polyester chips through pelletizing；Again through metering, extrusion, cooling, oil, stretch, thermal finalization and Winding is made FDY, and the temperature of FDY extrusions is 285 DEG C, and cooling wind-warm syndrome is 23 DEG C, and the speed of winding is 4550m/ min；The spatial joint clearance of the super fibrous inside molecule interchain at 80 DEG C of flexible polyester fiber FDY of porous porous obtained increases Rate, the mechanical performance data of the melt viscosity rate of descent and fiber such as following table at 289 DEG C.
Embodiment 54~57
A kind of preparation method of porous super flexible polyester fiber FDY, porous super flexible polyester fiber FDY is using porous Spinneret is made, and the arrangement mode of spinneret orifice is oval shaped arrangements on spinneret, and oval shaped arrangements refer to the hole center of spinneret orifice On concentration ellipse, concentration ellipse is that series is oval, and all elliptical long axis are conllinear, and short axle is conllinear.
Spinneret orifice is arranged as long axial symmetry, and the ratio of elliptical long axis and minor axis length is 1.8, between adjacent spinneret orifice 1.5mm is added away from the guide hole diameter equal to spinneret orifice, spinneret is round spinneret, and the diameter and series of round spinneret are oval The difference of maximum long axis length is 16mm, and the spinneret hole count of a diameter of 1.8mm of guide hole of spinneret orifice, spinneret are 300, spinneret The cross-sectional shape of the spinneret orifice of plate is hollow type.
Modified poly ester obtains Modified polyester chips through pelletizing；Again through metering, extrusion, cooling, oil, stretch, thermal finalization and Winding is made FDY, and the temperature of FDY extrusions is 290 DEG C, and cooling wind-warm syndrome is 25 DEG C, and the speed of winding is 4600m/ min；The spatial joint clearance of the super fibrous inside molecule interchain at 130 DEG C of flexible polyester fiber FDY of porous porous obtained increases Rate, the mechanical performance data of the melt viscosity rate of descent and fiber such as following table at 260 DEG C.
Embodiment 58
The dyeing of porous super flexible polyester fiber FDY：
Porous porous super flexible polyester fiber FDY prepared to embodiment 29 dyes in high temperature and pressure machine, has Concrete conditions in the establishment of a specific crime is：Before dyeing, porous super flexible polyester fiber FDY silks nonionic surfactant handles 30 minutes at 60 DEG C, so It is added in dyeing liquor afterwards, the disperse dyes dosage in dyeing liquor is 2.0% (o.w.f)；Dispersant NNO, the concentration of dispersant NNO 1.2g/L；PH value is 5, bath raio 1:50, it is contaminated in 60 DEG C of tripping in, then heats to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C and 130 DEG C each constant temperature dyeing 1h.
General fibre is dyed using identical dyeing condition.The super flexible polyester fiber of porous porous after dyed FDY dye uptakes obtain by the following method：
Dye uptake is determined using raffinate colorimetric method, draws suitable dyeing stoste and dyeing residual liquid, and N, N-2 first is added The ratio of base formamide (DMF) and distilled water, DMF and water in dye liquor to be measured is 70/30 (v/v), and dye liquor absorbance is using purple Outside-visible spectrophotometer measures, and dye uptake is calculated with following formula.
In above formula, A0 and A1 are respectively the absorbance for dyeing stoste and dyeing residual liquid.
When disperse dyes are Disperse Red 3B, disperse blue SE-2R or the bright blue S-GL of dispersion, the super flexible polyester of porous porous is fine The dye uptake result such as following table of dimension FDY and general fibre：
Surpass flexible polyester fiber FDY by porous porous and the coloring of general fibre compares, it can be seen that is porous The coloring of super flexible polyester fiber FDY is substantially better than general fibre, also from the side illustration modification of the invention prepared The hexylene glycol segment containing branch contained in polyester macromolecule, makes the increasing degree of free volume be far longer than unbranched polyester The characteristic of macromolecular chain, the increase of free volume improve molecule and enter degree inside polyester, prepared by modified polyester The free volume of polyester fiber be far longer than polyester fiber unbranched at same temperature, increase the diffusion of dyestuff, carry The dyeability of superpolyester fiber.
Embodiment 59
The dyeing of porous super flexible polyester fiber FDY：
Porous porous super flexible polyester fiber FDY prepared to embodiment 31 dyes in high temperature and pressure machine, has Concrete conditions in the establishment of a specific crime is：Before dyeing, porous super flexible polyester fiber FDY silks nonionic surfactant handles 30 minutes at 60 DEG C, so It is added in dyeing liquor afterwards, the disperse dyes dosage in dyeing liquor is 2.0% (o.w.f)；Dispersant NNO, the concentration of dispersant NNO 1.2g/L；PH value is 5, bath raio 1:50, it is contaminated in 60 DEG C of tripping in, then heats to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C and 130 DEG C each constant temperature dyeing 1h.
General fibre is dyed using identical dyeing condition.The super flexible polyester fiber of porous porous after dyed FDY dye uptakes obtain by the following method：
Dye uptake is determined using raffinate colorimetric method, draws suitable dyeing stoste and dyeing residual liquid, and N, N-2 first is added The ratio of base formamide (DMF) and distilled water, DMF and water in dye liquor to be measured is 70/30 (v/v), and dye liquor absorbance is using purple Outside-visible spectrophotometer measures, and dye uptake is calculated with following formula.
In above formula, A0 and A1 are respectively the absorbance for dyeing stoste and dyeing residual liquid.
When disperse dyes are Disperse Red 3B, disperse blue SE-2R or the bright blue S-GL of dispersion, the super flexible polyester of porous porous is fine The dye uptake result such as following table of dimension FDY and general fibre：
It is compared by porous super flexible polyester fiber FDY and the coloring of general fibre, it can be seen that porous super soft Soft polyester fiber FDY colorings are substantially better than general fibre, also from the side illustration modified poly ester of the invention prepared The hexylene glycol segment containing branch contained in macromolecular makes the increasing degree of free volume be far longer than unbranched polyester and divides greatly The characteristic of subchain, the increase of free volume improve molecule and enter degree inside polyester, and modified polyester is prepared poly- The free volume of ester fiber is far longer than polyester fiber unbranched at same temperature, increases the diffusion of dyestuff, improves poly- The dyeability of ester fiber.

Claims (9)

1. a kind of porous super flexible polyester fiber FDY, it is characterized in that：The material of porous super flexible polyester fiber FDY For modified poly ester, the modified poly ester is made of terephthalic acid (TPA) segment, ethylene glycol segment and hexylene glycol segment containing branch；Contain The hexylene glycol of branch be 2- amyls -1,6 hexylene glycol, 2- hexyl -1,6 hexylene glycols, 2- heptyl -1,6 hexylene glycol, 2- octyls -1,6 oneself One or more of -1,6 hexylene glycol of glycol, -1,6 hexylene glycol of 2- nonyls or 2- decyls；
The filament number of porous super flexible polyester fiber FDY be 0.3~2.0dtex, initial modulus≤70cN/dtex, Fracture strength >=3.8cN/dtex, elongation at break are 33.0 ± 3.0%；Porous super flexible polyester fiber FDY is in temperature Degree is at 80~130 DEG C, and the spatial joint clearance of fibrous inside molecule interchain increases 10~30v/v%, at 260~290 DEG C, melt Viscosity declines 10~20%；Line density deviation ratio≤0.5% of porous super flexible polyester fiber FDY, fracture strength CV Value≤4.0%, extension at break CV value≤8.0%, yarn unevenness CV≤2.0%.
2. a kind of preparation method of porous super flexible polyester fiber FDY as described in claim 1, it is characterized in that：It will be modified Porous super flexible polyester fiber FDY is made using porous spinneret spinning in polyester；The row of spinneret orifice on the porous spinneret Row mode is oval shaped arrangements, and the oval shaped arrangements refer to that the hole center of spinneret orifice is located on concentration ellipse, described ellipse with one heart Circle is oval for series, and all elliptical long axis are conllinear, and short axle is conllinear；
The preparation method of porous super flexible polyester fiber FDY is：Modified poly ester obtains Modified polyester chips through pelletizing, changes Property polyester slice through metering, extrusion, cooling, oil, stretch, modified poly ester FDY is made in thermal finalization and winding；
The preparation process of the modified poly ester is：
(1) preparation of terephthalic acid (TPA) binary alcohol esters；
After terephthalic acid (TPA) and the hexylene glycol containing branch are made into slurry, under the catalytic action of the concentrated sulfuric acid, esterification is carried out Obtain terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate；
After terephthalic acid (TPA) and ethylene glycol are made into slurry, esterification is carried out, ethylene glycol terephthalate is obtained；
(3) preparation of modified poly ester；
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, stirring is mixed It closes, under the action of catalyst and stabilizer, under conditions of negative pressure, carries out polycondensation reaction and the Gao Zhen of low vacuum stage successively Modified poly ester is made in the polycondensation reaction in empty stage.
3. a kind of preparation method of porous super flexible polyester fiber FDY according to claim 2, which is characterized in that institute The specific preparation process for stating modified poly ester is：
(1) preparation of terephthalic acid (TPA) binary alcohol esters；
Terephthalic acid (TPA) and the hexylene glycol containing branch are made into slurry, under the catalytic action of the concentrated sulfuric acid, carry out esterification, ester Change reaction compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure~0.3MPa, and temperature is 180~240 DEG C, works as esterification In water quantity of distillate be esterification terminal when reaching 90% of theoretical value or more, obtain terephthalic acid (TPA) binary alcohol esters；
(2) preparation of ethylene glycol terephthalate；
After terephthalic acid (TPA) and ethylene glycol are made into slurry, progress 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 90% or more, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After esterification in step (2), the terephthalic acid (TPA) binary alcohol esters prepared in step (1) are added, stirring is mixed It closes 15-20 minutes, under the action of catalyst and stabilizer, starts the polycondensation reaction of low vacuum stage under conditions of negative pressure, The staged pressure by normal pressure is steadily evacuated to absolute pressure 500Pa hereinafter, temperature control is at 260~270 DEG C, and the reaction time is 30~ 50 minutes；It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is down to absolute pressure and be less than Modified poly ester is made in 275~280 DEG C, 50~90 minutes reaction time in 100Pa, reaction temperature control；
The main spinning technology parameter of porous super flexible polyester fiber FDY is：
The temperature of extrusion：280~290 DEG C；
Cooling wind-warm syndrome：20~25 DEG C；
The speed of winding：4000~4600m/min.
4. a kind of preparation method of porous super flexible polyester fiber FDY according to claim 2, which is characterized in that step Suddenly in (1), the molar ratio of terephthalic acid (TPA) and the hexylene glycol containing branch is 1:1.3-1.5；Concentrated sulfuric acid addition is terephthaldehyde The 0.3-0.5% of sour weight；A concentration of 50-60wt% of the concentrated sulfuric acid；
In step (2), the molar ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2~2.0；
In step (3), the Mole percent ratio of the terephthalic acid (TPA) binary alcohol esters and ethylene glycol terephthalate is 2~ 5%；The catalyst is antimony oxide, antimony glycol or antimony acetate, and catalyst charge is terephthalic acid (TPA) total weight 0.01%~0.05%；The stabilizer is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite, and stabilizer addition is The 0.01%~0.05% of the terephthalic acid (TPA) total weight；
The number-average molecular weight of the modified poly ester is 15000~30000.
5. a kind of preparation method of porous super flexible polyester fiber FDY according to claim 2, which is characterized in that institute State spinneret orifice be arranged as long axis and/or short axle is symmetrical.
6. a kind of preparation method of porous super flexible polyester fiber FDY according to claim 2, which is characterized in that ellipse The ratio of round long axis and minor axis length is 1.3~1.8；The guide hole diameter that the spacing of adjacent spinneret orifice is more than or equal to spinneret orifice adds Upper 1.5mm.
7. a kind of preparation method of porous super flexible polyester fiber FDY according to claim 2, which is characterized in that institute It is round spinneret or elliptical spinneret plate to state spinneret；The diameter of the circle spinneret and the oval maximum long axial length of series The difference of degree is more than 10mm, and the elliptical spinneret plate and the difference of the oval maximum long axis length of series are more than 10mm.
8. a kind of preparation method of porous super flexible polyester fiber FDY according to claim 2, which is characterized in that institute State a diameter of 1.5~2.5mm of guide hole of spinneret orifice；The spinneret hole count of the spinneret is more than or equal to 192.
9. a kind of preparation method of porous super flexible polyester fiber FDY according to claim 2, which is characterized in that institute The cross-sectional shape for stating the spinneret orifice of spinneret is circle, square, diamond shape, "-" type, triangular form, trilobal cross, hollow type Or platypelloid type.
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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
CN108048940B (en) * 2017-12-14 2020-10-13 江苏恒力化纤股份有限公司 Soft polyester fiber and preparation method thereof
CN109735920B (en) * 2018-12-27 2020-07-07 江苏恒力化纤股份有限公司 Soft polyester fiber and preparation method thereof
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