CN106400164A - Porous flax-like polyester fiber and preparation method thereof - Google Patents
Porous flax-like polyester fiber and preparation method thereof Download PDFInfo
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- CN106400164A CN106400164A CN201610779088.0A CN201610779088A CN106400164A CN 106400164 A CN106400164 A CN 106400164A CN 201610779088 A CN201610779088 A CN 201610779088A CN 106400164 A CN106400164 A CN 106400164A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
- D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention relates to a porous flax-like polyester fiber and a preparation method thereof. The porous flax-like polyester fiber is prepared by spinning modified polyester by using a porous spinneret plate, wherein spinneret holes in the porous spinneret plate are elliptically arrayed; i.e., the centers of the spinneret holes are located on concentric ellipses which are series ellipses, the long axes of all the ellipses are collinear, and the short axes of all the ellipses are also collinear. The porous flax-like polyester fiber is prepared from modified polyester POY yarns and modified polyester FDY yarns through process. A preparation method for the modified polyester comprises the following steps: reacting terephthalic acid with glycol to prepare ethylene terephthalate; adding dihydric alcohol terephthalate prepared through reaction of terephthalic acid with propylene glycol containing a branched chain; and continuing reaction so as to obtain the modified polyester. The fiber prepared in the invention has following excellent properties: a linear density deviation ratio of no more than 2.0%, a breaking tenacity CV value of no more than 4.0%, a breaking elongation CV value of no more than 8.0%, and a crimp contraction variation coefficient CV value of no more than 8.0%.
Description
Technical field
The invention belongs to field of polyester fiber, it is related to a kind of porous and imitates fiber crops polyester fiber and preparation method thereof.
Background technology
Polyethylene terephthalate (PET or polyester fiber) fiber since the advent of the world, have fracture strength and
Elastic modelling quantity is high, and resilience is moderate, and thermal finalization is excellent, and heat-resisting light resistance is good and acid-fast alkali-proof corrosion resistance etc. is a series of excellent
Performance, is widely used in the fields such as clothing, home textile.But because the degree of crystallinity of PET is high, on compact structure, and strand not with
The functional group that dyestuff combines, causes dye molecule to hardly enter fibrous inside, dyeing is difficult.Cause the former of PET dyeing difficulty
Because PET belongs to symmetric straight chain macromolecular, strand does not contain side-chain radical, and regularity is very good, and its main chain contains
The phenyl ring of rigidity and flexible alkyl, and the ester group being directly connected with phenyl ring constitutes rigid conjugated system with phenyl ring,
Thus constraining rotating freely of its soft segment.Such a structure increases the wall ridge of molecule segment motion, lead to the glass of PET
Change transition temperature higher, need to promote the diffusion to fibrous inside for the dye molecule under very high temperature conditionss, complete dyeing step
Suddenly.In addition, the strand of PET is regular, good crystallinity, molecule chain alignment closely, and is not sent out with dye molecule on strand
The polar group of raw effect, makes the colouring of PET more difficult.
Therefore, under the general High Temperature High Pressure of the dyeing of common PET, select disperse dyeing, when temperature reaches PET
When fiber obtains more than vitrification point, between PET polymer molecule, space increases, but the degree that its free volume increases is little,
Dyeing rate is not high, but the energy consumption brought of high temperature and high pressure method and dye-uptake low be the subject matter facing now.In addition,
PET melt viscosity is higher, is unfavorable for processing.Melt spinning method is conventional process in current commercial production application, and melting is spun
Many parameters are had, these parameters determine the course of fiberizing and spin structure and the performance of fiber, in production just during silk
It is the fiber of desired properties to be obtained by controlling these parameters.Main spinning parameter can be summarized as melting according to technical process
Condition, spinning conditions, condition of cure, wrapping wire condition etc., wherein strand cooling and solidifying condition has decision to fibre structure and performance
Property impact, for controlling the rate of cooling of polyester fondant thread and its uniformity, in production, generally take cooling blowing, can accelerate to melt
The rate of cooling of body thread, is conducive to improving spinning speed；Strengthen the convection current of strand surrounding air, so that ectonexine strand is cooled down all
Even, it is that condition is created using porous spinneret；Cooling blowing can make as-spun fibre Quality advance, and tensile property improves, favorably
In the production capacity improving equipment.
Ring blowing device not only possesses the uniform advantage of every synnema wind-engaging, and energy consumption is compared relatively low, effectively solves
The wind energy loss problem that cross air blasting causes because blowing area is big.In spinning process, although ring blowing have significantly excellent
Gesture, but still have problems：Because spun silk is after circular spinneret is extruded, by ring wind quenching, due to circular jetting
The filament plate number of turns is more so that ring blowing hardly enters innermost layer, leads to that the silk of innermost layer can after cooling in outermost silk
Can be also uncolled, thus the silk of gained occurs, and fiber number is irregular, intensity is irregular, the problems such as uneven dyeing, causes and subsequently silk is entered
Difficulty in one step processing.
Imitative linen look abnormal contraction composite filament is the long filament with different potential shrinkages, i.e. lower shrinkage silk POY and high convergency
The composite filament through mixed fine processing composition for the silk FDY, the main feature of PET different contraction mixed fiber composite silk：High loft and soft handss
Sense.PET imitates the outer existing similar with common long filament of linen look abnormal contraction composite filament.Due to the difference of two component shrinkage factors, thermally treated
Afterwards, high convergency part forms clear-cut core filaments, becomes the skeleton of silk, and lower shrinkage part forms tiny wire ring and is wound on core filaments
Around, it is exactly like textured filament in appearance.Gloss is soft.Because PET imitates the many on the bulk and surface of linen look abnormal contraction composite filament
Wire ring, eliminates the aurora defect of chemical fibre silk fabrics.Excellent warmth retention property.The high loft of PET different contraction mixed fiber composite silk, increases
Space between big fiber.The air content in PET different contraction mixed fiber composite silk fabrics is caused to increase.
Content of the invention
The purpose of the present invention is to overcome the problems such as existing dyeing polyester fibers are irregular, mechanical property is poor, realizes extensive
The production spinning changed, provides a kind of porous to imitate fiber crops polyester fiber and preparation method thereof.The raw material of the polyester fiber of the present invention is to change
Property polyester, introduce the propylene glycol segment containing side chain in the strand of modified poly ester, the porous of modified polyester preparation imitates fiber crops polyester
Fiber, under the conditions of uniform temperature, the increasing degree that porous imitates the spatial joint clearance of fiber crops polyester fiber interior molecules interchain is far longer than
Unbranched conventional polyester fiber at equal temperature, is conducive to the degree within the entrance of the molecules such as stain, improves dyeing
Speed；The melt viscosity that porous imitates fiber crops polyester fiber reduces, and reduces processing temperature, reduces degradation rate, is conducive to processing；In addition
The structural regularity that propylene glycol segment containing side chain imitates fiber crops polyester fiber to porous does not have big destruction, maintains polyester fiber
Premium properties.Adopt the spinneret of spinneret orifice oval shaped arrangements in spinning process of the present invention, be conducive to fiber in spinning process
Uniform, sufficiently cool, performance between fiber and structure difference less, improve dyeing uniformity and the mechanical property of fiber
Energy.
For reaching above-mentioned purpose, the technical solution used in the present invention is：
A kind of porous imitates fiber crops polyester fiber, and the material that described porous imitates fiber crops polyester fiber is modified poly ester, described modified poly-
Ester is made up of p-phthalic acid segment, ethylene glycol segment and the propylene glycol segment containing side chain, the described propylene glycol segment containing side chain
Refer to that side chain is located on one of propylene glycol segment non-end group carbon and side chain is the linear carbon chain containing 5-10 carbon atom
Propylene glycol segment；
The fiber number that described porous imitates fiber crops polyester fiber is 75-150dtex, initial moduluss≤85cN/dtex, fracture strength >=
3.0cN/dtex, elongation at break is 40.0 ± 3.0%, and crimp contraction is 3.50 ± 2.0%, and internet pricing is 95 ± 5/m；
Described porous imitates fiber crops polyester fiber at temperature is 80～130 DEG C, and the spatial joint clearance of fibrous inside molecule interchain increases 10～
30v/v%；Described porous imitates line density deviation ratio≤2.0% of fiber crops polyester fiber, fracture strength CV value≤4.0%, and fracture is stretched
Long CV value≤8.0%, crimp contraction coefficient of variation CV value≤8.0%, boiling water shrinkage is 10.0 ± 1.0%.
Present invention also offers a kind of porous imitates the preparation method of fiber crops polyester fiber, modified poly ester is adopted porous spinneret
Spinning is obtained porous and imitates fiber crops polyester fiber；On described porous spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, described ellipse
Circular arrangement refers to that the hole of spinneret orifice is centrally located on concentration ellipse, and described concentration ellipse is that series is oval, all oval length
Axle is conllinear, and short axle is conllinear；
Described porous imitate fiber crops polyester fiber preparation method be：By modified poly ester through measuring, extruding, cool down, oil and roll up
Around prepared modified poly ester POY silk；By Modified polyester chips through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, system
Obtain modified poly ester FDY silk；Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, heating stretching, false twisting, heat
Sizing and coiling and molding are obtained porous and imitate fiber crops polyester fiber；
The preparation process of described modified poly ester is：
(1) preparation of p-phthalic acid binary alcohol esters；
P-phthalic acid is made into after slurry with the propylene glycol containing side chain, under the catalytic action of concentrated sulphuric acid, is esterified
Reaction obtains p-phthalic acid binary alcohol esters；It is non-that the described propylene glycol containing side chain refers to that side chain is located at one of propylene glycol segment
On end group carbon and side chain is the dihydroxylic alcohols of the linear carbon chain containing 5-10 carbon atom；
For the propylene glycol containing side chain, its side chain is alkyl, is electron withdraw group, in the presence of side chain, makes strand
Spatial volume increases, and solvation diminishes, and in dihydroxylic alcohols, proton is difficult to dissociate so that containing propylene glycol and the terephthaldehyde of side chain
The reactivity of acid is less than ethylene glycol, according to the mixing of same ethylene glycol and terephthaldehyde's acid reaction, can cause the third two containing side chain
Alcohol reaction is imperfect, thus ratio in polyester macromolecule for the propylene glycol containing side chain for the impact, and then affect the performance of polyester.This
Using first the propylene glycol containing side chain being carried out esterification with p-phthalic acid under the catalytic action of sulphuric acid, its product exists for invention
Ethylene glycol and p phthalic acid esterification add it is ensured that containing the stability of the propylene glycol proportioning of side chain after terminating；
(2) preparation of ethylene glycol terephthalate；
P-phthalic acid and ethylene glycol are made into after slurry, carry out esterification, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stir
Mix mixing, in the presence of catalyst and stabilizer, under conditions of negative pressure, carry out successively the coarse vacuum stage polycondensation reaction and
The polycondensation reaction of high vacuum stage of Fig, prepared modified poly ester.
As preferred technical scheme：
A kind of porous imitates the preparation method of fiber crops polyester fiber, the concrete preparation process of described modified poly ester as above
For：
(1) preparation of p-phthalic acid binary alcohol esters；
P-phthalic acid is made into slurry with the propylene glycol containing side chain, under the catalytic action of concentrated sulphuric acid, carries out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure～0.3MPa, and temperature is 180～240 DEG C, works as ester
It is esterification terminal that water quantity of distillate in change reaction reaches during more than the 90% of theoretical value, obtains p-phthalic acid dihydroxylic alcohols
Ester；
(2) preparation of ethylene glycol terephthalate；
P-phthalic acid and ethylene glycol are made into after slurry, carry out esterification, esterification is pressurizeed in nitrogen atmosphere
Reaction, moulding pressure is normal pressure～0.3MPa, and temperature is 250～260 DEG C, when the water quantity of distillate in esterification reaches theoretical value
More than 90% when be esterification terminal, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stir
Mix mixing 15-20 minute, in the presence of catalyst and stabilizer, the polycondensation starting the coarse vacuum stage under conditions of negative pressure is anti-
Should, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and at 260～270 DEG C, the response time is temperature control
30～50 minutes；Then proceed to evacuation, carry out the polycondensation reaction of high vacuum stage of Fig, make reaction pressure be down to absolute pressure and be less than
100Pa, reaction temperature controls at 275～280 DEG C, 50～90 minutes response time, prepared modified poly ester；
The main spinning technology parameter of described modified poly ester POY silk is：
Spinning temperature：280-290℃；Chilling temperature：23-27℃；Winding speed：2300-2500m/min；
The main spinning technology parameter of described modified poly ester FDY silk is：
Spinning temperature：280-290℃；Chilling temperature：20-25℃；Network pressure：0.20-0.30MPa；One roller speed：
2200-2600m/min；One roll temperature：75-85℃；Two roller speeds：3650-3850m/min；Two roll temperatures：115-
135℃；
Winding speed：3600-3800m/min；
Described porous imitate fiber crops polyester fiber main spinning technology parameter be：
Spin speed：400-800m/min；Sizing over feed rate(OFR)：3.5-5.50%；Winding over feed rate(OFR)：2.5-5.0%；
T1：160-220℃；T2：180-220℃；DR：1.6-1.8；D/Y:1.6-2.0；Network pressure：0.05-
0.3MPa.
As above a kind of porous imitate fiber crops polyester fiber preparation method, in step (1), p-phthalic acid with containing side chain
Propylene glycol mol ratio be 1:1.3-1.5；Concentrated sulphuric acid addition is the 0.3-0.5% of p-phthalic acid weight；Described dense sulfur
The concentration of acid is 50-60wt%；
In step (2), p-phthalic acid is 1 with the mol ratio of ethylene glycol:1.2～2.0；
In step (3), described p-phthalic acid binary alcohol esters are 2 with the Mole percent ratio of ethylene glycol terephthalate
～5%；Described catalyst is antimony oxide, antimony glycol or antimony acetate, and catalyst charge is p-phthalic acid gross weight
0.01%～0.05%；Described stabilizer is triphenyl phosphate, trimethyl phosphate or NSC 6513, stabilizer addition
For described p-phthalic acid gross weight 0.01%～0.05%；
The number-average molecular weight of described modified poly ester is 15000～30000.
As above a kind of porous imitate fiber crops polyester fiber preparation method, the described propylene glycol containing side chain be 2- amyl group-
1,3 propylene glycol, 2- hexyl -1,3 propylene glycol, 2- heptyl -1,3 propylene glycol, 2- octyl group -1,3 propylene glycol, 2- nonyl -1,3 propylene glycol
One or more of or 2- decyl -1,3 propylene glycol.
As above a kind of porous imitate fiber crops polyester fiber preparation method, described spinneret orifice be arranged as major axis and/or
Short axle is symmetrical.
A kind of porous imitates the preparation method of fiber crops polyester fiber as above, and oval major axis with the ratio of 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 1.5mm.Effective area when spinneret
Mutually simultaneously as the girth of ellipse is more than circular girth, the number of plies of spinneret orifice oval shaped arrangements is less than the layer of circular arrangement
Number, the hole count of spinneret orifice oval shaped arrangements is more than the hole count of circular arrangement, and therefore, spinneret orifice oval shaped arrangements are conducive to ring to dry
Cooling, improve the cooling effectiveness of ring blowing, the fibre property of preparation is also more excellent.Major axis is more connect with the ratio of minor axis length
It is bordering on 1, ellipse is more similar to justify, and the difference of cooling effectiveness and cooling effect is little；Major axis is 1.3 with the ratio of minor axis length
When, cooling effect significantly improves, and individual pen hole count is corresponding to increase by 16%；When the ratio of major axis and minor axis length is 1.8, cooling effect
Improve larger, individual pen hole count is corresponding to increase by 33%, in the case of identical hole count, and the oval shaped arrangements of the present invention are than conventional concentric circle row
The number of turns of row reduces it is easy to cooling wind thoroughly, makes the fiber cooling condition of Internal and external cycle evenly；Major axis and the ratio of minor axis length
During more than 1.8, ellipse is partial to form flat shape, is difficult to punch, cooling no longer raises.Therefore, series is ellipse
The major axis of circle is 1.3～1.8 with the ratio of minor axis length, can reach higher cooling effectiveness and preferable cooling effect.
A kind of porous imitates the preparation method of fiber crops polyester fiber as above, and described spinneret is circular spinneret or ellipse
Shape spinneret；The diameter of described circle spinneret is more than 10mm, described ellipse with the difference of the oval maximum long axis length of series
Shape spinneret is more than 10mm with the difference of the oval maximum long axis length of series.
A kind of porous imitates the preparation method of fiber crops polyester fiber as above, and the guide hole of described spinneret orifice is a diameter of 1.5～
2.5mm；The spray webbing hole count of described spinneret is more than or equal to 192.
A kind of porous imitates the preparation method of fiber crops polyester fiber, the cross section of the spinneret orifice of described spinneret as above
Generally circular in shape, square, rhombus, yi word pattern, triangular form, trilobal cross, hollow type or platypelloid type.
The principle of the present invention is：
For unbranched polyester fiber, its molecular chain structure is the linear macromolecule containing benzene ring structure, on strand
Functional group's marshalling, regularity is good, flexible poor；When temperature raises, its free volume increments is little, and these characteristics hinder
Hinder dyestuff to enter inside polyester fiber, thus dyeability is poor.
The raw material of the polyester fiber of the present invention is modified poly ester, the propylene glycol containing side chain containing in modified poly ester macromole
Segment, when temperature is higher than vitrification point, side chain, prior to backbone motion, makes the increasing degree of free volume be far longer than and no props up
The characteristic of the polyester macromolecule chain of chain, the increase of free volume improves the degree within molecule entrance polyester, modified
The free volume of the polyester fiber of polyester preparation is far longer than unbranched polyester fiber at equal temperature, increases the diffusion of dyestuff
Degree, improves the dyeability of polyester fiber.Meanwhile, the polyester fiber of modified poly ester preparation advantageously reduces melt viscosity, has
It is beneficial to improve its processing characteristics.The introducing of the propylene glycol segment containing side chain does not have big destruction to polyester fiber structures regularity,
Maintain the premium properties of polyester fiber.
When the effective area phase of spinneret is simultaneously as the girth of ellipse is more than circular girth, spinneret orifice is oval
The number of plies of arrangement is less than the number of plies of circular arrangement, and the hole count of spinneret orifice oval shaped arrangements is more than the hole count of circular arrangement, using spray
The spinneret of silk hole oval shaped arrangements enables to that fiber is quick, uniformly cools down, and between fiber, the difference of structure and performance is less,
Be conducive to improving the even dyeing rate of fiber and the performance of fiber.
Beneficial effect：
1) on the spinneret of the present invention, the arrangement mode of spinneret orifice is oval shaped arrangements, and the effective area of spinneret is identical
When, the number of plies of spinneret orifice oval shaped arrangements is less than the number of plies of circular arrangement, and ring blowing is easier to blow through dynamic analysis of spinning, dynamic analysis of spinning
Cooling effect more preferably, the fibre property of preparation is also more excellent.
2) on the spinneret of the present invention, the arrangement mode of spinneret orifice is oval shaped arrangements, and the effective area of spinneret is identical
When, the hole count of spinneret orifice oval shaped arrangements is more than the hole count of circular arrangement, and oval shaped arrangements are capable of greatly cooling down,
Significantly improve cooling effectiveness.
3) material that the porous that the present invention is obtained imitates fiber crops polyester fiber is modified poly ester, contains in modified poly ester macromole
Propylene glycol segment containing side chain, when temperature is higher than vitrification point, side chain, prior to backbone motion, makes the increase width of free volume
Degree is far longer than the characteristic of unbranched polyester macromolecule chain, and the increase of free volume improves molecule and enters inside polyester
Degree, increase the diffusion of dyestuff by the free volume that side chain increased polyester fiber, improve the dye of polyester fiber
Color performance.
4) porous that the present invention is obtained imitates fiber crops polyester fiber, and the increase of polyester fiber free volume advantageously reduces melt and glues
Degree, is conducive to improving its processing characteristics.The porous that the present invention is obtained imitates fiber crops polyester fiber, the introducing of the propylene glycol segment containing side chain
To the structural regularity of polyester fiber there is no big destruction, maintain the premium properties of polyester fiber.
5) porous that the present invention is obtained imitates fiber crops dyeing polyester fibers performance and good mechanical performance, initial moduluss≤85cN/
Dtex, line density deviation ratio≤2.0% of porous imitative fiber crops polyester fiber, fracture strength CV value≤4.0%, extension at break CV value≤
8.0%, crimp contraction coefficient of variation CV value≤8.0%.
Brief description
Fig. 1 is the oval shaped arrangements figure of 374 spinneret orifices, and the aperture of spinneret orifice is 2.0mm, the length of transverse and short axle
Degree ratio is 1.3；
Fig. 2 is the circular arrangement figure of 370 spinneret orifices, and the aperture of spinneret orifice is 2.0mm；
Fig. 3 is the oval shaped arrangements figure of 382 spinneret orifices, and the aperture of spinneret orifice is 2.0mm, the length of transverse and short axle
Degree ratio is 1.6.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate this
Bright rather than limit the scope of the present invention.In addition, it is to be understood that after having read the content of present invention instruction, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
Embodiment 1
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.3 p-phthalic acid and 2- amyl group -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 50wt%, and addition is under the catalytic action of 0.3% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure, and temperature is 180 DEG C, when the water in esterification distillates
It is esterification terminal that amount reaches during the 90% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.2 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure, and temperature is 250 DEG C, when the water in esterification distillates
It is esterification terminal that amount reaches during the 90% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 2% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 15 minutes is adding
Measure for p-phthalic acid weight 0.01% the catalytic antimony trioxide and addition be p-phthalic acid weight 0.01%
Stabilizer triphenyl phosphate in the presence of, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure
Steadily being evacuated to absolute pressure by normal pressure is 500Pa, and at 260 DEG C, the response time is 30 minutes to temperature control；Then proceed to take out very
Sky, carries out the polycondensation reaction of high vacuum stage of Fig, and making reaction pressure be down to absolute pressure is 100Pa, and reaction temperature controls 275
DEG C, 50 minutes response time, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 15000, by p-phthalic acid
Segment, ethylene glycol segment and 2- amyl group -1,3 propylene glycol segment compositions, 2- amyl group -1,3 propylene glycol segments and ethylene glycol segment
Mole percent ratio is 2%.
Embodiment 2
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.38 p-phthalic acid and 2- hexyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.32% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.13MPa, and temperature is 181 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 91% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.3 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.12MPa, and temperature is 251 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 91% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 2.1% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 16 minutes is adding
Entering 0.011% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.02% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 262 DEG C, the response time is 31 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 99Pa, and reaction temperature controls at 276 DEG C,
51 minutes response time, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 16000, by p-phthalic acid chain
Section, ethylene glycol segment and 2- hexyl -1,3 propylene glycol segment compositions, 2- hexyl -1,3 propylene glycol segments are rubbed with ethylene glycol segment
Your percent value is 2.1%.
Embodiment 3
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.33 p-phthalic acid and 2- heptyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.33% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.12MPa, and temperature is 183 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.31 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.31MPa, and temperature is 252 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 2.2% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 16 minutes is adding
Entering 0.03% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.02% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 498Pa by normal pressure, and at 263 DEG C, the response time is 32 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 80Pa, and reaction temperature controls at 277 DEG C,
57 minutes response time, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 15900, by p-phthalic acid chain
Section, ethylene glycol segment and 2- heptyl -1,3 propylene glycol segment compositions, 2- heptyl -1,3 propylene glycol segments are rubbed with ethylene glycol segment
Your percent value is 2.2%.
Embodiment 4
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.34 p-phthalic acid and 2- octyl group -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of 0.34% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.13MPa, and temperature is 184 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 93% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.32 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.33MPa, and temperature is 253 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 93% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 2.3% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 17 minutes is adding
Entering 0.033% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.023% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
It is 497Pa that section pressure is steadily evacuated to absolute pressure by normal pressure, and at 264 DEG C, the response time is 33 minutes to temperature control；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, and making reaction pressure be down to absolute pressure is 80Pa, and reaction temperature controls
278 DEG C, 58 minutes response time, prepared modified poly ester, number-average molecular weight is 15800, by p-phthalic acid segment, glycol chain
Section and 2- octyl group -1,3 propylene glycol segments form, 2- octyl group -1, and 3 propylene glycol segments with the Mole percent ratio of ethylene glycol segment are
2.3%.
Embodiment 5
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.35 p-phthalic acid and 2- nonyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.36% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.14MPa, and temperature is 185 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 93.2% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.33 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.14MPa, and temperature is 254 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 93.2% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 2.4% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 17 minutes is adding
Entering 0.034% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.024% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and at 265 DEG C, the response time is 34 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, and making reaction pressure be down to absolute pressure is 70Pa, and reaction temperature controls 277
DEG C, 59 minutes response time, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 15900, by p-phthalic acid
Segment, ethylene glycol segment and 2- nonyl -1,3 propylene glycol segment compositions, 2- nonyl -1,3 propylene glycol segments and ethylene glycol segment
Mole percent ratio is 2.4%.
Embodiment 6
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.36 p-phthalic acid and 2- decyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 50wt%, and addition is under the catalytic action of 0.37% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.15MPa, and temperature is 186 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 93.3% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.34 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.15MPa, and temperature is 255 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 93.3% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 2.5% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Entering 0.035% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.025% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 266 DEG C, the response time is 35 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, and making reaction pressure be down to absolute pressure is 70Pa, and reaction temperature controls 278
DEG C, 60 minutes response time, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 16000, by p-phthalic acid
Segment, ethylene glycol segment and 2- decyl -1,3 propylene glycol segment compositions, 2- decyl -1,3 propylene glycol segments and ethylene glycol segment
Mole percent ratio is 2.5%.
Embodiment 7
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.37 p-phthalic acid and 2- amyl group -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of 0.38% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.16MPa, and temperature is 187 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 93.4% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.36 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.16MPa, and temperature is 256 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 93.4% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 2.6% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 19 minutes is adding
Entering 0.036% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.025% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and at 267 DEG C, the response time is 36 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, and making reaction pressure be down to absolute pressure is 70Pa, and reaction temperature controls 278
DEG C, 61 minutes response time, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 16000, by p-phthalic acid
Segment, ethylene glycol segment and 2- amyl group -1,3 propylene glycol segment compositions, 2- amyl group -1,3 propylene glycol segments and ethylene glycol segment
Mole percent ratio is 2.6%.
Embodiment 8
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.38 p-phthalic acid and 2- hexyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.39% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.17MPa, and temperature is 188 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 93.5% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.37 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.17MPa, and temperature is 257 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 93.5% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 2.7% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 19 minutes is adding
Entering 0.036% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.025% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and at 267 DEG C, the response time is 36 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, and making reaction pressure be down to absolute pressure is 60Pa, and reaction temperature controls 278
DEG C, 61 minutes response time, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 17000, by p-phthalic acid
Segment, ethylene glycol segment and 2- hexyl -1,3 propylene glycol segment compositions, 2- hexyl -1,3 propylene glycol segments and ethylene glycol segment
Mole percent ratio is 2.7%.
Embodiment 9
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.39 p-phthalic acid and 2- heptyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 50wt%, and addition is under the catalytic action of 0.4% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.17MPa, and temperature is 188 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 93.5% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.37 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.17MPa, and temperature is 257 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 93.5% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 2.8% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 16 minutes is adding
Entering 0.04% catalyst glycol antimony that amount is p-phthalic acid weight and addition is the 0.026% of p-phthalic acid weight
Stabilizer trimethyl phosphate in the presence of, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure
Absolute pressure 497Pa is steadily evacuated to by normal pressure, at 268 DEG C, the response time is 38 minutes to temperature control；Then proceed to evacuation,
Carry out the polycondensation reaction of high vacuum stage of Fig, making reaction pressure be down to absolute pressure is 50Pa, and reaction temperature controls at 279 DEG C, instead
62 minutes between seasonable, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester be 18000, by p-phthalic acid segment,
Ethylene glycol segment and 2- heptyl -1,3 propylene glycol segments compositions, 2- heptyl -1, moles the hundred of 3 propylene glycol segments and ethylene glycol segment
Ratio is divided to be 2.8%.
Embodiment 10
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.4 p-phthalic acid and 2- octyl group -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.4% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.17MPa, and temperature is 188 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 93.5% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.38 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.18MPa, and temperature is 257.8 DEG C, when in esterification
Water quantity of distillate reach theoretical value 93.6% when be esterification terminal, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 3% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 17 minutes is adding
Measure for p-phthalic acid weight 0.03% catalyst glycol antimony and addition be the 0.027% of p-phthalic acid weight
In the presence of stabilizer trimethyl phosphate, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure by
Normal pressure is steadily evacuated to absolute pressure 498Pa, and at 269 DEG C, the response time is 39 minutes to temperature control；Then proceed to evacuation, enter
The polycondensation reaction of row high vacuum stage of Fig, making reaction pressure be down to absolute pressure is 50Pa, and reaction temperature controls at 278 DEG C, reaction
64 minutes time, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 19000, by p-phthalic acid segment, second
Glycol segment and 2- octyl group -1,3 propylene glycol segment compositions, 2- octyl group -1, the Mole percent of 3 propylene glycol segments and ethylene glycol segment
Ratio is 3%.
Embodiment 11
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.4 p-phthalic acid and 2- nonyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.4% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.18MPa, and temperature is 189 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 93.6% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.39 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.19MPa, and temperature is 258.8 DEG C, when in esterification
Water quantity of distillate reach theoretical value 94% when be esterification terminal, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Measure for p-phthalic acid weight 0.04% catalyst glycol antimony and addition be the 0.03% of p-phthalic acid weight
In the presence of stabilizer trimethyl phosphate, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure by
Normal pressure is steadily evacuated to absolute pressure 497Pa, and at 260 DEG C, the response time is 40 minutes to temperature control；Then proceed to evacuation, enter
The polycondensation reaction of row high vacuum stage of Fig, making reaction pressure be down to absolute pressure is 40Pa, and reaction temperature controls at 277 DEG C, reaction
63 minutes time, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 20000, by p-phthalic acid segment, second
Glycol segment and 2- nonyl -1,3 propylene glycol segment compositions, 2- nonyl -1, the Mole percent of 3 propylene glycol segments and ethylene glycol segment
Ratio is 4%.
Embodiment 12
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.4 p-phthalic acid and 2- nonyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.4% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.2MPa, and temperature is 200 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 94% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.6 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.2MPa, and temperature is 256 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 94% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.5% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Enter that amount is 0.038% catalyst acetic acid antimony of p-phthalic acid weight and addition is p-phthalic acid weight 0.03%
Under conditions of negative pressure, in the presence of stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, this staged pressure
Absolute pressure 497Pa is steadily evacuated to by normal pressure, at 265 DEG C, the response time is 42 minutes to temperature control；Then proceed to evacuation,
Carry out the polycondensation reaction of high vacuum stage of Fig, making reaction pressure be down to absolute pressure is 40Pa, and reaction temperature controls at 277 DEG C, instead
70 minutes between seasonable, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester be 26000, by p-phthalic acid segment,
Ethylene glycol segment and 2- decyl -1,3 propylene glycol segments compositions, 2- decyl -1, moles the hundred of 3 propylene glycol segments and ethylene glycol segment
Ratio is divided to be 4%.
Embodiment 13
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.5 p-phthalic acid and 2- decyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of 0.5% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.3MPa, and temperature is 240 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:2.0 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.3MPa, and temperature is 260 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 5% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 20 minutes is adding
Measure for p-phthalic acid weight 0.05% catalyst acetic acid antimony and addition be p-phthalic acid weight 0.05% steady
In the presence of determining agent NSC 6513, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure by
It is 450Pa that normal pressure is steadily evacuated to absolute pressure, and at 270 DEG C, the response time is 50 minutes to temperature control；Then proceed to evacuation,
Carry out the polycondensation reaction of high vacuum stage of Fig, making reaction pressure be down to absolute pressure is 30Pa, and reaction temperature controls at 280 DEG C, instead
90 minutes between seasonable, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester be 30000, by p-phthalic acid segment,
Ethylene glycol segment and 2- decyl -1,3 propylene glycol segments compositions, 2- decyl -1, moles the hundred of 3 propylene glycol segments and ethylene glycol segment
Ratio is divided to be 5%.
Embodiment 14
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.47 p-phthalic acid and 2- nonyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of 0.47% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 220 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Measure for p-phthalic acid weight 0.04% catalyst glycol antimony and addition be the 0.04% of p-phthalic acid weight
In the presence of stabilizer trimethyl phosphate, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure by
Normal pressure is steadily evacuated to absolute pressure 460Pa, and at 263 DEG C, the response time is 47 minutes to temperature control；Then proceed to evacuation, enter
The polycondensation reaction of row high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 278 DEG C, during reaction
Between 85 minutes, prepared modified poly ester.The number-average molecular weight of prepared modified poly ester is 28000, by p-phthalic acid segment, second two
Alcohol segment and 2- nonyl -1,3 propylene glycol segment compositions, 2- nonyl -1, the molar percentage of 3 propylene glycol segments and ethylene glycol segment
It is worth for 4%.
Embodiment 15
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.46 p-phthalic acid and 2- octyl group -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of 0.49% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 233 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 259 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.5% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 19 minutes is adding
Entering 0.044% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.046% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 269 DEG C, the response time is 48 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 279 DEG C,
87 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, pungent by p-phthalic acid segment, ethylene glycol segment and 2-
Base -1,3 propylene glycol segment compositions, 2- octyl group -1,3 propylene glycol segments are 4.5% with the Mole percent ratio of ethylene glycol segment.
Embodiment 16
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.49 p-phthalic acid and 2- heptyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of 0.48% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 230 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.7% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 19 minutes is adding
Entering 0.048% catalyst glycol antimony that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.047% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 460Pa by normal pressure, and at 267 DEG C, the response time is 48 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 279 DEG C,
83 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 27000, by p-phthalic acid segment, ethylene glycol segment and 2- heptan
Base -1,6 hexanediol segment compositions, 2- heptyl -1,6 hexanediol segments are 4.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 17
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.467 p-phthalic acid and 2- hexyl -1,3 propylene glycol are made into slurry and add in reactor,
It is 60wt% in concentration, addition is under the catalytic action of 0.47% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 236 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.89 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 258 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.3% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Entering 0.04% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.041% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 268 DEG C, the response time is 48 minutes to temperature control；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, reaction temperature controls 278
DEG C, 85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, own by p-phthalic acid segment, ethylene glycol segment and 2-
Base -1,3 propylene glycol segment compositions, 2- hexyl -1,3 propylene glycol segments are 4.3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 18
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.48 p-phthalic acid and 2- amyl group -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.46% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 230 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.88 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 256 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.7% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Entering 0.047% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.047% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 480Pa by normal pressure, and at 265 DEG C, the response time is 47 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 279 DEG C,
85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 28000, by p-phthalic acid segment, ethylene glycol segment and 2- penta
Base -1,3 propylene glycol segment compositions, 2- amyl group -1,3 propylene glycol segments are 4.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 19
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.46 p-phthalic acid and 2- decyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.47% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 238 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.9 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 259 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during more than the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.7% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 19 minutes is adding
Entering the 0.046% catalyst acetic acid antimony that amount is p-phthalic acid weight and addition is the 0.048% of p-phthalic acid weight
Stabilizer NSC 6513 in the presence of, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this stage press
It is 446Pa that power is steadily evacuated to absolute pressure by normal pressure, and at 267 DEG C, the response time is 49 minutes to temperature control；Then proceed to take out very
Sky, carries out the polycondensation reaction of high vacuum stage of Fig, and making reaction pressure be down to absolute pressure is 40Pa, and reaction temperature controls at 278 DEG C,
87 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, by p-phthalic acid segment, ethylene glycol segment and the 2- last of the ten Heavenly stems
Base -1,3 propylene glycol segment compositions, 2- decyl -1,3 propylene glycol segments are 4.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 20
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.46 p-phthalic acid and 2- nonyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of 0.46% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.26MPa, and temperature is 221 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.89 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.25MPa, and temperature is 259 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.1% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Entering 0.041% catalyst glycol antimony that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.042% stabilizer trimethyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 460Pa by normal pressure, and at 265 DEG C, the response time is 47 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 278 DEG C,
85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 28000, by p-phthalic acid segment, ethylene glycol segment and 2- nonyl
Base -1,3 propylene glycol segment compositions, 2- nonyl -1,3 propylene glycol segments are 4.1% with the Mole percent ratio of ethylene glycol segment.
Embodiment 21
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.43 p-phthalic acid and 2- octyl group -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of 0.47% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 235 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.78 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.26MPa, and temperature is 255 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.3% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 17 minutes is adding
Entering 0.043% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.049% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 268 DEG C, the response time is 46 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls at 275 DEG C,
85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 28000, pungent by p-phthalic acid segment, ethylene glycol segment and 2-
Base -1,3 propylene glycol segment compositions, 2- octyl group -1,3 propylene glycol segments are 4.3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 22
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.43 p-phthalic acid and 2- heptyl -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.45% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.29MPa, and temperature is 235 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.87 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 255 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.6% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Entering 0.047% catalyst glycol antimony that amount is p-phthalic acid weight and addition is the 0.04% of p-phthalic acid weight
Stabilizer triphenyl phosphate in the presence of, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure
Absolute pressure 470Pa is steadily evacuated to by normal pressure, at 268 DEG C, the response time is 45 minutes to temperature control；Then proceed to evacuation,
Carry out the polycondensation reaction of high vacuum stage of Fig, make reaction pressure be down to absolute pressure 40Pa, reaction temperature controls at 279 DEG C, reaction
83 minutes time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, by p-phthalic acid segment, ethylene glycol segment and 2- heptan
Base -1,3 propylene glycol segment compositions, 2- heptyl -1,3 propylene glycol segments are 4.6% with the Mole percent ratio of ethylene glycol segment.
Embodiment 23
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.457 p-phthalic acid and 2- hexyl -1,3 propylene glycol are made into slurry and add in reactor,
It is 55% in concentration, addition is under the catalytic action of 0.46% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 239 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.81 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 255 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.41% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 19 minutes,
Addition is 0.042% the catalytic antimony trioxide of p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.048% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the response time is 45 minutes to temperature control；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 275
DEG C, 85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 28000, own by p-phthalic acid segment, ethylene glycol segment and 2-
Base -1,3 propylene glycol segment compositions, 2- hexyl -1,3 propylene glycol segments are 4.41% with the Mole percent ratio of ethylene glycol segment.
Embodiment 24
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.47 p-phthalic acid and 2- amyl group -1,3 propylene glycol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of 0.48% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 245 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.81 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 259 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.67% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 19 minutes,
Addition is 0.041% the catalytic antimony trioxide of p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.042% stabilizer triphenyl phosphate, start the polycondensation reaction in coarse vacuum stage, this rank
Section pressure is steadily evacuated to absolute pressure 485Pa by normal pressure, and at 268 DEG C, the response time is 46 minutes to temperature control；Then proceed to take out
Vacuum, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, and reaction temperature controls at 275 DEG C,
89 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, by p-phthalic acid segment, ethylene glycol segment and 2- penta
Base -1,3 propylene glycol segment compositions, 2- amyl group -1,3 propylene glycol segments are 4.67% with the Mole percent ratio of ethylene glycol segment.
Embodiment 25
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.45 p-phthalic acid and 2- hexyl -1,3 propylene glycol and 2- amyl group -1,3 propylene glycol mixed
Compound is made into slurry and adds in reactor, wherein 2- hexyl -1,3 propylene glycol and 2- amyl group -1, and the mol ratio of 3 propylene glycol is 3:1,
It is 55% in concentration, addition is under the catalytic action of 0.49% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.26MPa, and temperature is 236 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.4% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Entering 0.042% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.047% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the response time is 49 minutes to temperature control；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 278
DEG C, 88 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester be 29000, by p-phthalic acid segment, ethylene glycol segment, 2- hexyl-
1,3 propylene glycol segment and 2- amyl group -1,3 propylene glycol segments compositions, 2- hexyl -1,3 propylene glycol segments and 2- amyl group -1,3 the third two
The summation of alcohol segment is 4.4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 26
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:2- octyl group -1,3 propylene glycol of 1.45 p-phthalic acid sum and 2- amyl group -1,3 propylene glycol
Mixture is made into slurry and adds in reactor, wherein 2- octyl group -1,3 propylene glycol and 2- amyl group -1, and the mol ratio of 3 propylene glycol is 3:
2, it is 60% in concentration, addition is under the catalytic action of 0.45% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 239 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.84 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification anti-
Should, esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.29MPa, and temperature is 255 DEG C, when in esterification
It is esterification terminal that water quantity of distillate reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.6% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Entering 0.0423% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.045% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the response time is 45 minutes to temperature control；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 278
DEG C, 85 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester be 28000, by p-phthalic acid segment, ethylene glycol segment, 2- octyl group-
1,3 propylene glycol segment and 2- amyl group -1,3 propylene glycol segments compositions, 2- octyl group -1,3 propylene glycol segments and 2- amyl group -1,3 the third two
Alcohol segment is 4.6% with the Mole percent ratio of ethylene glycol segment.
Embodiment 27
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.45 p-phthalic acid and 2- hexyl -1,3 propylene glycol and 2- amyl group -1,3 propylene glycol mixed
Compound is made into slurry and adds in reactor, wherein 2- hexyl -1,3 propylene glycol and 2- amyl group -1, and the mol ratio of 3 propylene glycol is 3:1,
It is 55% in concentration, addition is under the catalytic action of 0.49% concentrated sulphuric acid of p-phthalic acid weight, carries out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.26MPa, and temperature is 236 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 96% of theoretical value, obtains p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.28MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.4% with the Mole percent ratio of ethylene glycol terephthalate, and stirring mixing 18 minutes is adding
Entering 0.042% the catalytic antimony trioxide that amount is p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.047% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and at 265 DEG C, the response time is 49 minutes to temperature control；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 278
DEG C, 88 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester be 29000, by p-phthalic acid segment, ethylene glycol segment, 2- hexyl-
1,3 propylene glycol segment and 2- amyl group -1,3 propylene glycol segments compositions, 2- hexyl -1,3 propylene glycol segments and 2- amyl group -1,3 the third two
The summation of alcohol segment is 4.4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 28
A kind of preparation method of modified poly ester, specifically includes following steps：
(1) preparation of p-phthalic acid binary alcohol esters：
Mol ratio is 1:1.45 p-phthalic acid is own with 2- octyl group -1,3 propylene glycol, 2- amyl group -1,3 propylene glycol and 2-
Base -1, the mixture of 3 propylene glycol is made into slurry and adds in reactor, wherein 2- octyl group -1,3 propylene glycol, 2- amyl group -1, and 3 the third two
The mol ratio of alcohol and 2- hexyl -1,3 propylene glycol is 3:2:1, it is 60% in concentration, addition is p-phthalic acid weight
Under the catalytic action of 0.47% concentrated sulphuric acid, carry out esterification, esterification compressive reaction in nitrogen atmosphere, moulding pressure
For 0.29MPa, temperature is 235 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 92% of theoretical value,
Obtain p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate：
Mol ratio is 1:1.8 p-phthalic acids and ethylene glycol add in reactor after being made into slurry, carry out esterification,
Esterification compressive reaction in nitrogen atmosphere, moulding pressure is 0.27MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal that output reaches during the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester：
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters are 4.71% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes,
Addition is 0.04% the catalytic antimony trioxide of p-phthalic acid weight and addition is p-phthalic acid weight
Under conditions of negative pressure, in the presence of 0.041% stabilizer NSC 6513, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and at 268 DEG C, the response time is 49 minutes to temperature control；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, reaction temperature controls 277
DEG C, 84 minutes response time, prepared modified poly ester.
The number-average molecular weight of prepared modified poly ester is 29000, by p-phthalic acid segment, ethylene glycol segment, band side chain
Glycol segment composition, wherein branched glycol segment be 2- octyl group -1,3 propylene glycol segments, 2- amyl group -1,3 propylene glycol chains
Section and 2- hexyl -1,3 propylene glycol segments form, and branched glycol segment with the Mole percent ratio of ethylene glycol segment is
4.71%.
Embodiment 29
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
As shown in figure 1, the major axis of ellipse is 1.3 with the ratio of minor axis length, the spacing of adjacent spinneret orifice is equal to spinneret orifice
Guide hole diameter add 1.5mm, spinneret is circular spinneret, the diameter of circular spinneret oval maximum long axial length with series
The difference of degree is 11mm, a diameter of 2.0mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 374, the spinneret orifice of spinneret
Shape of cross section be circle.
By the prepared modified poly ester of embodiment 1 through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk,
The spinning temperature of modified poly ester POY silk is 285 DEG C, and chilling temperature is 25 DEG C, and winding speed is 2400m/min；By modified poly ester
Section is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk, modified poly ester FDY silk
Spinning temperature is 285 DEG C, and chilling temperature is 25 DEG C, and network pressure is 0.25MPa, and a roller speed is 2400m/min, a roll temperature
For 80 DEG C, two roller speeds are 3800m/min, and two roll temperatures are 120 DEG C, and winding speed is 3750m/min；Then by modified poly ester
POY silk and modified poly ester FDY silk are obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitate fiber crops polyester
Fiber, the spinning speed that porous imitates fiber crops polyester fiber is 600m/min, and sizing over feed rate(OFR) is 4.50%, and winding over feed rate(OFR) is 4.0%, T1
For 200 DEG C, T2 is 200 DEG C, and DR is 1.7, D/Y is 1.8, and network pressure is 0.15MPa.
The fiber number that prepared porous imitates fiber crops polyester fiber is 120tex, initial moduluss 83cN/dtex, and fracture strength is
4.7cN/dtex, elongation at break is 41.7%, and crimp contraction is 4.53%, and internet pricing is 95/m；Porous imitates fiber crops polyester
At temperature is 80 DEG C, the spatial joint clearance of fibrous inside molecule interchain increases 15v/v% to fiber；Porous imitates the line of fiber crops polyester fiber
Density variation rate is 1.7%, and fracture strength CV value is 3.2%, and extension at break CV value is 6.9%, the crimp contraction coefficient of variation
CV value is 7.2%, and boiling water shrinkage is 10.5%.
Embodiment 30
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
As shown in figure 3, the major axis of ellipse is 1.6 with the ratio of minor axis length, the spacing of adjacent spinneret orifice is equal to spinneret orifice
Guide hole diameter add 1.5mm, spinneret is circular spinneret, the diameter of circular spinneret oval maximum long axial length with series
The difference of degree is 11mm, a diameter of 2.0mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 382, the spinneret orifice of spinneret
Shape of cross section be circle.
By the prepared modified poly ester of embodiment 1 through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk,
The spinning temperature of modified poly ester POY silk is 285 DEG C, and chilling temperature is 25 DEG C, and winding speed is 2400m/min；By modified poly ester
Section is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk, modified poly ester FDY silk
Spinning temperature is 285 DEG C, and chilling temperature is 25 DEG C, and network pressure is 0.25MPa, and a roller speed is 2400m/min, a roll temperature
For 80 DEG C, two roller speeds are 3800m/min, and two roll temperatures are 120 DEG C, and winding speed is 3750m/min；Then by modified poly ester
POY silk and modified poly ester FDY silk are obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitate fiber crops polyester
Fiber, the spinning speed that porous imitates fiber crops polyester fiber is 600m/min, and sizing over feed rate(OFR) is 4.50%, and winding over feed rate(OFR) is 4.0%, T1
For 200 DEG C, T2 is 200 DEG C, and DR is 1.7, D/Y is 1.8, and network pressure is 0.15MPa.
The fiber number that prepared porous imitates fiber crops polyester fiber is 140dtex, initial moduluss 85cN/dtex, and fracture strength is
5.2cN/dtex, elongation at break is 42.6%, and crimp contraction is 4.77%, and internet pricing is 98/m；Porous imitates fiber crops polyester
At temperature is 80 DEG C, the spatial joint clearance of fibrous inside molecule interchain increases 15v/v% to fiber；Porous imitates the line of fiber crops polyester fiber
Density variation rate is 1.2%, and fracture strength CV value is 3.1%, and extension at break CV value is 5.3%, the crimp contraction coefficient of variation
CV value is 4.9%, and boiling water shrinkage is 10.6%.
Comparative example 1
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is circular arrangement, and circular arrangement refers to that the hole of spinneret orifice is centrally located on concentric circular, with one heart
Circle is circular for series.As shown in Fig. 2 the guide hole diameter that the spacing of adjacent spinneret orifice is equal to spinneret orifice adds 1.5mm, spinneret is
Circular spinneret, the diameter of circular spinneret is 11mm with the difference of the circular maximum diameter of series, the guide hole diameter of spinneret orifice
For 2.0mm, the spray webbing hole count of spinneret is 370, and the shape of cross section of the spinneret orifice of spinneret is circle.
By the prepared modified poly ester of embodiment 1 through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk,
The spinning temperature of modified poly ester POY silk is 285 DEG C, and chilling temperature is 25 DEG C, and winding speed is 2400m/min；By modified poly ester
Section is through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, prepared modified poly ester FDY silk, modified poly ester FDY silk
Spinning temperature is 285 DEG C, and chilling temperature is 25 DEG C, and network pressure is 0.25MPa, and a roller speed is 2400m/min, a roll temperature
For 80 DEG C, two roller speeds are 3800m/min, and two roll temperatures are 120 DEG C, and winding speed is 3750m/min；Then by modified poly ester
POY silk and modified poly ester FDY silk are obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitate fiber crops polyester
Fiber, the spinning speed that porous imitates fiber crops polyester fiber is 600m/min, and sizing over feed rate(OFR) is 4.50%, and winding over feed rate(OFR) is 4.0%, T1
For 200 DEG C, T2 is 200 DEG C, and DR is 1.7, D/Y is 1.8, and network pressure is 0.15MPa.
The fiber number that prepared porous imitates fiber crops polyester fiber is 70dtex, initial moduluss 80cN/dtex, and fracture strength is
2.7cN/dtex, elongation at break is 36.1%, and crimp contraction is 5.6%, and internet pricing is 87/m；It is fine that porous imitates fiber crops polyester
At temperature is 80 DEG C, the spatial joint clearance of fibrous inside molecule interchain increases 15v/v% to dimension；The line that porous imitates fiber crops polyester fiber is close
Degree deviation ratio is 2.6%, and fracture strength CV value is 4.5%, and extension at break CV value is 8.2%, crimp contraction coefficient of variation CV
It is worth for 8.5%, boiling water shrinkage is 9.1%.
When identical with the effective area that embodiment 29 contrast can be seen that spinneret, (circular arrangement when spray webbing hole count is close
Spray webbing hole count is 370, and oval shaped arrangements spray webbing hole count is 374), the spinneret orifice number of plies of oval shaped arrangements is 6, less than circular arrangement
The spinneret orifice number of plies 8, cooling effect is more preferable；When identical with the effective area that embodiment 30 contrast can be seen that spinneret, oval
The spinneret orifice number of plies of shape arrangement is 5, and less than the spinneret orifice number of plies 8 of circular arrangement, cooling effect is more preferable, the spray webbing of oval shaped arrangements
The hole count 382 in hole is more than the hole count 370 of the spinneret orifice of circular arrangement, and cooling effectiveness is higher.The comparing result of fibre property shows,
Fiber linear density deviation ratio, fracture strength CV value, extension at break CV value and evenness fault that embodiment 29 and embodiment 30 are obtained
Rate CV value is less than comparative example 1, under the conditions of same process is described, using the prepared fibroids of the spinneret of spinneret orifice oval shaped arrangements
Can be better than the spinneret using spinneret circular arrangement.
Embodiment 31～33
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as long axial symmetry, oval major axis is 1.4 with the ratio of minor axis length, between adjacent spinneret orifice
Add 1.6mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series
The difference of maximum long axis length is 12mm, a diameter of 1.5mm of guide hole of spinneret orifice, the spinneret orifice numerical digit 192 of spinneret, spray webbing
The shape of cross section of the spinneret orifice of plate is square.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk
Spinning temperature is 280 DEG C, and chilling temperature is 23 DEG C, and winding speed is 2300m/min；By Modified polyester chips through metering, extrusion,
Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 280 DEG C,
Chilling temperature is 20 DEG C, and network pressure is 0.20MPa, and a roller speed is 2200m/min, and a roll temperature is 75 DEG C, two roller speeds
For 3650m/min, two roll temperatures are 115 DEG C, and winding speed is 3600m/min；Then by modified poly ester POY silk and modified poly ester
FDY silk is obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitates fiber crops polyester fiber, and it is poly- that porous imitates fiber crops
The spinning speed of ester fiber is 400m/min, and sizing over feed rate(OFR) is 3.50%, and winding over feed rate(OFR) is that 2.5%, T1 is 160 DEG C, and T2 is 180
DEG C, DR is 1.6, D/Y is 1.6, and network pressure is 0.05MPa.The boiling water shrinkage that prepared porous imitates fiber crops polyester fiber is 9.0
～9.7, the mechanical performance data such as following table of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 80 DEG C.
Embodiment 34～36
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that short axle is symmetrical, oval major axis is 1.4 with the ratio of minor axis length, between adjacent spinneret orifice
Add 1.7mm away from the guide hole diameter equal to spinneret orifice, spinneret is elliptical spinneret plate, elliptical spinneret plate is with serial ellipse
The difference of big long axis length is 12mm, a diameter of 1.8mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 200, spinneret
Spinneret orifice shape of cross section be rhombus.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk
Spinning temperature is 282 DEG C, and chilling temperature is 23 DEG C, and winding speed is 2350m/min；By Modified polyester chips through metering, extrusion,
Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 281 DEG C,
Chilling temperature is 21 DEG C, and network pressure is 0.21MPa, and a roller speed is 2250m/min, and a roll temperature is 77 DEG C, two roller speeds
For 3680m/min, two roll temperatures are 116 DEG C, and winding speed is 3630m/min；Then by modified poly ester POY silk and modified poly ester
FDY silk is obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitates fiber crops polyester fiber, and it is poly- that porous imitates fiber crops
The spinning speed of ester fiber is 450m/min, and sizing over feed rate(OFR) is 3.9%, and winding over feed rate(OFR) is that 2.9%, T1 is 170 DEG C, and T2 is 185
DEG C, DR is 1.6, D/Y is 1.6, and network pressure is 0.15MPa.The boiling water shrinkage that porous imitates fiber crops polyester fiber is 9.1～9.6,
The mechanical performance data such as following table of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 90 DEG C.
Embodiment 37～39
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that major axis and short axle are symmetrical, oval major axis is 1.4 with the ratio of minor axis length, adjacent spray webbing
The guide hole diameter that the spacing in hole is equal to spinneret orifice adds 1.8mm, and spinneret is circular spinneret, the diameter of circular spinneret be
The difference of the oval maximum long axis length of row is 13mm, a diameter of 2.5mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is
200, the shape of cross section of the spinneret orifice of spinneret is yi word pattern.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk
Spinning temperature is 283 DEG C, and chilling temperature is 24 DEG C, and winding speed is 2400m/min；By Modified polyester chips through metering, extrusion,
Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 284 DEG C,
Chilling temperature is 23 DEG C, and network pressure is 0.25MPa, and a roller speed is 2300m/min, and a roll temperature is 78 DEG C, two roller speeds
For 3700m/min, two roll temperatures are 125 DEG C, and winding speed is 3650m/min；Then by modified poly ester POY silk and modified poly ester
FDY silk is obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitates fiber crops polyester fiber, and it is poly- that porous imitates fiber crops
The spinning speed of ester fiber is 470m/min, and sizing over feed rate(OFR) is 4.50%, and winding over feed rate(OFR) is that 3.5%, T1 is 180 DEG C, and T2 is 190
DEG C, DR is 1.6, D/Y is 1.7, and network pressure is 0.17MPa.Porous imitate fiber crops polyester fiber boiling water shrinkage be 9.6～
10.0, the mechanical performance data such as following table of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 100 DEG C.
Embodiment 40～42
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that major axis and short axle are symmetrical, oval major axis is 1.7 with the ratio of minor axis length, adjacent spray webbing
The spacing in hole be equal to spinneret orifice guide hole diameter add 1.9mm, spinneret be elliptical spinneret plate, elliptical spinneret plate with series
The difference of oval maximum long axis length is 14mm, a diameter of 1.5mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 210,
The shape of cross section of the spinneret orifice of spinneret is triangular form.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk
Spinning temperature is 283 DEG C, and chilling temperature is 27 DEG C, and winding speed is 2500m/min；By Modified polyester chips through metering, extrusion,
Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 284 DEG C,
Chilling temperature is 22 DEG C, and network pressure is 0.23MPa, and a roller speed is 2500m/min, and a roll temperature is 79 DEG C, two roller speeds
For 3850m/min, two roll temperatures are 124 DEG C, and winding speed is 3800m/min；Then by modified poly ester POY silk and modified poly ester
FDY silk is obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitates fiber crops polyester fiber, and it is poly- that porous imitates fiber crops
The spinning speed of ester fiber is 600m/min, and sizing over feed rate(OFR) is 4.70%, and winding over feed rate(OFR) is that 5.0%, T1 is 175 DEG C, and T2 is 200
DEG C, DR is 1.8, D/Y is 2.0, and network pressure is 0.18MPa.Porous imitate fiber crops polyester fiber boiling water shrinkage be 10.4～
11.0, the mechanical performance data such as following table of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 110 DEG C.
Embodiment 43～45
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that short axle is symmetrical, oval major axis is 1.8 with the ratio of minor axis length, between adjacent spinneret orifice
Add 1.5mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series
The difference of maximum long axis length is 15mm, a diameter of 1.8mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 240, spray webbing
The shape of cross section of the spinneret orifice of plate is trilobal cross.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk
Spinning temperature is 287 DEG C, and chilling temperature is 26 DEG C, and winding speed is 2450m/min；By Modified polyester chips through metering, extrusion,
Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 284 DEG C,
Chilling temperature is 23 DEG C, and network pressure is 0.23MPa, and a roller speed is 2600m/min, and a roll temperature is 85 DEG C, two roller speeds
For 3790m/min, two roll temperatures are 135 DEG C, and winding speed is 3740m/min；Then by modified poly ester POY silk and modified poly ester
FDY silk is obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitates fiber crops polyester fiber, and it is poly- that porous imitates fiber crops
The spinning speed of ester fiber is 560m/min, and sizing over feed rate(OFR) is 4.50%, and winding over feed rate(OFR) is that 3.5%, T1 is 190 DEG C, and T2 is 210
DEG C, DR is 1.7, D/Y is 1.7, and network pressure is 0.19MPa.The boiling water shrinkage that porous imitates fiber crops polyester fiber is 9.4～9.7,
The mechanical performance data such as following table of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 120 DEG C.
Embodiment 46～49
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as long axial symmetry, oval major axis is 1.8 with the ratio of minor axis length, between adjacent spinneret orifice
Add 1.6mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series
The difference of maximum long axis length is 16mm, a diameter of 2.2mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 250, spray webbing
The shape of cross section of the spinneret orifice of plate is hollow type.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk
Spinning temperature is 290 DEG C, and chilling temperature is 26 DEG C, and winding speed is 2470m/min；By Modified polyester chips through metering, extrusion,
Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 290 DEG C,
Chilling temperature is 23 DEG C, and network pressure is 0.30MPa, and a roller speed is 2460m/min, and a roll temperature is 79 DEG C, two roller speeds
For 3780m/min, two roll temperatures are 124 DEG C, and winding speed is 3730m/min；Then by modified poly ester POY silk and modified poly ester
FDY silk is obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitates fiber crops polyester fiber, and it is poly- that porous imitates fiber crops
The spinning speed of ester fiber is 610m/min, and sizing over feed rate(OFR) is 4.3%, and winding over feed rate(OFR) is that 4.1%, T1 is 180 DEG C, and T2 is 220
DEG C, DR is 1.7, D/Y is 1.8, and network pressure is 0.30MPa.The boiling water shrinkage that prepared porous imitates fiber crops polyester fiber is 9.2
～9.8, the mechanical performance data such as following table of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 130 DEG C.
Embodiment 50～53
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as that short axle is symmetrical, oval major axis is 1.8 with the ratio of minor axis length, between adjacent spinneret orifice
Add 1.8mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series
The difference of maximum long axis length is 15mm, a diameter of 2.5mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 260, spray webbing
The shape of cross section of the spinneret orifice of plate is platypelloid type.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, spinning temperature be 286
DEG C, chilling temperature is 24 DEG C, and winding speed is 2430m/min；By Modified polyester chips through measuring, extruding, cool down, oil, draw
Stretch, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 282 DEG C, and chilling temperature is 22
DEG C, network pressure is 0.23MPa, and a roller speed is 2460m/min, and a roll temperature is 75-85 DEG C, and two roller speeds are 3760m/
Min, two roll temperatures are 121 DEG C, and winding speed is 3710m/min；Then by modified poly ester POY silk and modified poly ester FDY silk warp
Plying network, heating stretching, false twisting, thermal finalization and coiling and molding are obtained porous and imitate fiber crops polyester fiber, and porous imitates fiber crops polyester fiber
Spinning speed be 800m/min, sizing over feed rate(OFR) is 5.5%, and winding over feed rate(OFR) is that 4.6%, T1 is 180 DEG C, and T2 is 190 DEG C, and DR is
1.6, D/Y is 1.8, and network pressure is 0.21MPa.The boiling water shrinkage that porous imitates fiber crops polyester fiber is 10.0～10.7,100
The mechanical performance data such as following table of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at DEG C.
Embodiment 54～57
A kind of porous imitates the preparation method of fiber crops polyester fiber, and porous is imitated fiber crops polyester fiber and adopts porous spinneret to be obtained, spray
On filament plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refer to that the hole of spinneret orifice is centrally located at concentration ellipse
On, concentration ellipse is that series is oval, and all oval major axis are conllinear, and short axle is conllinear.
Spinneret orifice be arranged as long axial symmetry, oval major axis is 1.8 with the ratio of minor axis length, between adjacent spinneret orifice
Add 1.5mm away from the guide hole diameter equal to spinneret orifice, spinneret is circular spinneret, the diameter of circular spinneret is oval with series
The difference of maximum long axis length is 16mm, a diameter of 1.8mm of guide hole of spinneret orifice, and the spray webbing hole count of spinneret is 300, spray webbing
The shape of cross section of the spinneret orifice of plate is hollow type.
Modified poly ester through measuring, extruding, cool down, oil and wind, prepared modified poly ester POY silk, modified poly ester POY silk
Spinning temperature is 281 DEG C, and chilling temperature is 26 DEG C, and winding speed is 2460m/min；By Modified polyester chips through metering, extrusion,
Cool down, oil, stretching, thermal finalization and winding, prepared modified poly ester FDY silk, the spinning temperature of modified poly ester FDY silk is 283 DEG C,
Chilling temperature is 25 DEG C, and network pressure is 0.23MPa, and a roller speed is 2480m/min, and a roll temperature is 78 DEG C, two roller speeds
For 3690m/min, two roll temperatures are 124 DEG C, and winding speed is 3640m/min；Then by modified poly ester POY silk and modified poly ester
FDY silk is obtained porous through plying network, heating stretching, false twisting, thermal finalization and coiling and molding and imitates fiber crops polyester fiber, and it is poly- that porous imitates fiber crops
The spinning speed of ester fiber is 590m/min, and sizing over feed rate(OFR) is 4.60%, and winding over feed rate(OFR) is that 3.7%, T1 is 190 DEG C, and T2 is 220
DEG C, DR is 1.6, D/Y is 1.7, and network pressure is 0.23MPa.Porous imitate fiber crops polyester fiber boiling water shrinkage be 9.6～
10.3, the mechanical performance data such as following table of the spatial joint clearance Magnification of fibrous inside molecule interchain and fiber at 120 DEG C.
Embodiment 58
Porous imitates the dyeing of fiber crops polyester fiber：
The porous imitative fiber crops polyester fiber of embodiment 29 preparation is dyeed in High Temperature High Pressure machine, actual conditions is：Dye
Before color, porous is imitated fiber crops polyester fiber nonionic surfactant and is processed 30 minutes at 60 DEG C, is subsequently adding in dyeing liquor, dyeing
Disperse dyes consumption in liquid is 2.0% (o.w.f)；Dispersant NNO, concentration 1.2g/L of dispersant NNO；PH value is 5, bath raio
For 1:50, enter dye at 60 DEG C, then heat to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C and 130 DEG C of each constant temperature dyeing 1h.
Using identical dyeing condition, general fibre is dyeed.Porous after dyed imitates the upper dye of fiber crops polyester fiber
Percentage rate obtains by the following method：
Dye uptake adopts residual liquid colorimetry to determine, draws appropriate dyeing stock solution and dyeing residual liquid, adds N, N-2 first
Base Methanamide (DMF) and distilled water, the DMF in dye liquor to be measured and the ratio of water are 70/30 (v/v), and dye liquor absorbance is using purple
Outward-visible spectrophotometer measures, and calculates dye uptake with following formula.
In above formula, A0 and A1 is respectively the absorbance dyeing stock solution and dyeing residual liquid.
When disperse dyes are Disperse Red 3B, disperse blue SE-2R or when disperseing bright blue S-GL, porous imitates fiber crops polyester fiber and general
The dye uptake result such as following table of perforating fiber：
The Color contrast of fiber crops polyester fiber and general fibre is imitated it can be seen that porous imitates fiber crops polyester fiber by porous
Color be substantially better than general fibre, also contain the modified poly ester macromole of present invention preparation from side illustration contains
The propylene glycol segment of side chain, makes the increasing degree of free volume be far longer than the characteristic of unbranched polyester macromolecule chain, freely
The increase of volume improves the degree within molecule entrance polyester, the free volume of the polyester fiber of modified polyester preparation
It is far longer than unbranched polyester fiber at equal temperature, increases the diffusion of dyestuff, improve the dyeability of polyester fiber.
Embodiment 59
Porous imitates the dyeing of fiber crops polyester fiber：
The porous imitative fiber crops polyester fiber of embodiment 31 preparation is dyeed by embodiment 58, adopts identical to dye simultaneously
Condition dyes to general fibre.Porous imitates the dye uptake result such as following table of fiber crops polyester fiber and general fibre：
Contrasted by Color it can be seen that the Color that porous imitates fiber crops polyester fiber is substantially better than general fibre.
Claims (10)
1. a kind of porous imitates fiber crops polyester fiber, it is characterized in that：The material that described porous imitates fiber crops polyester fiber is modified poly ester, described
Modified poly ester form by p-phthalic acid segment, ethylene glycol segment and containing the propylene glycol segment of side chain, described containing side chain the third two
Alcohol segment refers to that side chain is located on one of propylene glycol segment non-end group carbon and side chain is the straight chain containing 5-10 carbon atom
The propylene glycol segment of carbochain；
The fiber number that described porous imitates fiber crops polyester fiber is 75-150dtex, initial moduluss≤85cN/dtex, fracture strength >=
3.0cN/dtex, elongation at break is 40.0 ± 3.0%, and crimp contraction is 3.50 ± 2.0%, and internet pricing is 95 ± 5/m；
Described porous imitates fiber crops polyester fiber at temperature is 80～130 DEG C, and the spatial joint clearance of fibrous inside molecule interchain increases 10～
30v/v%；Described porous imitates line density deviation ratio≤2.0% of fiber crops polyester fiber, fracture strength CV value≤4.0%, and fracture is stretched
Long CV value≤8.0%, crimp contraction coefficient of variation CV value≤8.0%, boiling water shrinkage is 10.0 ± 1.0%；Described divides
Spatial joint clearance between subchain increases the right of the spatial joint clearance referring to modified poly ester and normal polyester in mutually synthermal molecule interchain
Than.
2. a kind of porous imitates the preparation method of fiber crops polyester fiber as claimed in claim 1, it is characterized in that：Modified poly ester is adopted
Porous spinneret spinning is obtained porous and imitates fiber crops polyester fiber；On described porous spinneret, the arrangement mode of spinneret orifice is oval row
Row, described oval shaped arrangements refer to that the hole of spinneret orifice is centrally located on concentration ellipse, and described concentration ellipse is that series is oval, owns
Oval major axis is conllinear, and short axle is conllinear；
Described porous imitate fiber crops polyester fiber preparation method be：By modified poly ester through measuring, extruding, cool down, oil and wind, system
Obtain modified poly ester POY silk；By Modified polyester chips through measuring, extruding, cool down, oil, stretch, thermal finalization and winding, be obtained and change
Property polyester FDY silk；Then by modified poly ester POY silk and modified poly ester FDY silk through plying network, heating stretching, false twisting, thermal finalization
Porous is obtained with coiling and molding and imitates fiber crops polyester fiber；
The preparation process of described modified poly ester is：
(1) preparation of p-phthalic acid binary alcohol esters；
P-phthalic acid is made into after slurry with the propylene glycol containing side chain, under the catalytic action of concentrated sulphuric acid, carries out esterification
Obtain p-phthalic acid binary alcohol esters；The described propylene glycol containing side chain refers to that side chain is located at the non-end group of one of propylene glycol segment
On carbon and side chain is the dihydroxylic alcohols of the linear carbon chain containing 5-10 carbon atom；
(2) preparation of ethylene glycol terephthalate；
P-phthalic acid and ethylene glycol are made into after slurry, carry out esterification, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stirring is mixed
Close, in the presence of catalyst and stabilizer, under conditions of negative pressure, carry out polycondensation reaction and the Gao Zhen in coarse vacuum stage successively
The polycondensation reaction in empty stage, prepared modified poly ester.
3. a kind of porous according to claim 2 imitates the preparation method of fiber crops polyester fiber it is characterised in that described modification is poly-
The concrete preparation process of ester is：
(1) preparation of p-phthalic acid binary alcohol esters；
P-phthalic acid is made into slurry with the propylene glycol containing side chain, under the catalytic action of concentrated sulphuric acid, carries out esterification, ester
Change reaction compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure～0.3MPa, temperature is 180～240 DEG C, works as esterification
In water quantity of distillate reach theoretical value more than 90% when be esterification terminal, obtain p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate；
P-phthalic acid and ethylene glycol are made into after slurry, carry out esterification, esterification compressive reaction in nitrogen atmosphere,
Moulding pressure is normal pressure～0.3MPa, and temperature is 250～260 DEG C, when the water quantity of distillate in esterification reaches theoretical value
It is esterification terminal when more than 90%, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester；
After the esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stirring is mixed
Close 15-20 minute, under conditions of negative pressure, in the presence of catalyst and stabilizer, start the polycondensation reaction in coarse vacuum stage,
This staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature control at 260～270 DEG C, the response time be 30～
50 minutes；Then proceed to evacuation, carry out the polycondensation reaction of high vacuum stage of Fig, make reaction pressure be down to absolute pressure and be less than
100Pa, reaction temperature controls at 275～280 DEG C, 50～90 minutes response time, prepared modified poly ester；
The main spinning technology parameter of described modified poly ester POY silk is：
Spinning temperature：280-290℃；
Chilling temperature：23-27℃；
Winding speed：2300-2500m/min；
The main spinning technology parameter of described modified poly ester FDY silk is：
Spinning temperature：280-290℃；
Chilling temperature：20-25℃；
Network pressure：0.20-0.30MPa；
One roller speed：2200-2600m/min；
One roll temperature：75-85℃；
Two roller speeds：3650-3850m/min；
Two roll temperatures：115-135℃；
Winding speed：3600-3800m/min；
Described porous imitate fiber crops polyester fiber main spinning technology parameter be：
Spin speed：400-800m/min；
Sizing over feed rate(OFR)：3.5-5.50%；
Winding over feed rate(OFR)：2.5-5.0%；
T1：160-220℃；
T2：180-220℃；
DR：1.6-1.8；
D/Y:1.6-2.0；
Network pressure：0.05-0.3MPa.
4. a kind of porous according to claim 2 imitates the preparation method of fiber crops polyester fiber it is characterised in that in step (1),
P-phthalic acid is 1 with the mol ratio of the propylene glycol containing side chain:1.3-1.5；Concentrated sulphuric acid addition is p-phthalic acid weight
0.3-0.5%；The concentration of described concentrated sulphuric acid is 50-60wt%；
In step (2), p-phthalic acid is 1 with the mol ratio of ethylene glycol:1.2～2.0；
In step (3), the Mole percent ratio of described p-phthalic acid binary alcohol esters and ethylene glycol terephthalate is 2～
5%；Described catalyst is antimony oxide, antimony glycol or antimony acetate, and catalyst charge is p-phthalic acid gross weight
0.01%～0.05%；Described stabilizer is triphenyl phosphate, trimethyl phosphate or NSC 6513, and stabilizer addition is
The 0.01%～0.05% of described p-phthalic acid gross weight；
The number-average molecular weight of described modified poly ester is 15000～30000.
5. a kind of porous according to claim 2 imitate fiber crops polyester fiber preparation method it is characterised in that described containing side chain
Propylene glycol be 2- amyl group -1,3 propylene glycol, 2- hexyl -1,3 propylene glycol, 2- heptyl -1,3 propylene glycol, 2- octyl group -1,3 the third two
One or more of alcohol, 2- nonyl -1,3 propylene glycol or 2- decyl -1,3 propylene glycol.
6. a kind of porous according to claim 2 imitates the preparation method of fiber crops polyester fiber it is characterised in that described spinneret orifice
Be arranged as major axis and/or short axle is symmetrical.
7. a kind of porous according to claim 2 imitates the preparation method of fiber crops polyester fiber it is characterised in that the major axis of ellipse
Ratio with 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 1.5mm.
8. a kind of porous according to claim 2 imitates the preparation method of fiber crops polyester fiber it is characterised in that described spinneret
For circular spinneret or elliptical spinneret plate；The diameter of described circle spinneret and the difference of the oval maximum long axis length of series
More than 10mm, described elliptical spinneret plate is more than 10mm with the difference of the oval maximum long axis length of series.
9. a kind of porous according to claim 2 imitates the preparation method of fiber crops polyester fiber it is characterised in that described spinneret orifice
The a diameter of 1.5～2.5mm of guide hole；The spray webbing hole count of described spinneret is more than or equal to 192.
10. a kind of porous according to claim 2 imitates the preparation method of fiber crops polyester fiber it is characterised in that described spray webbing
The shape of cross section of the spinneret orifice of plate is circle, square, rhombus, yi word pattern, triangular form, trilobal cross, hollow type or flat
Type.
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| CN108035006A (en) * | 2017-12-14 | 2018-05-15 | 江苏恒力化纤股份有限公司 | A kind of hygroscopic fibre and preparation method thereof |
| CN108130624A (en) * | 2017-12-14 | 2018-06-08 | 江苏恒力化纤股份有限公司 | A kind of polyester imitates linen look abnormal contraction composite filament and preparation method thereof |
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| CN110344128A (en) * | 2019-07-17 | 2019-10-18 | 军事科学院系统工程研究院军需工程技术研究所 | A kind of micropore imitates the preparation method of flaxen fiber |
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